Solvent pulping process
Abstract
Solvent pulping of wood chips or other fibrous plant material is effected using an aqueous solution of a lower aliphatic alcohol in a plurality of batch extraction vessels. The charge in each vessel is heated rapidly to pulping temperature by recirculation of a primary extraction liquor having a relatively high dissolved solids content, and thereafter the charge is subjected to a series of once-through extractions or washes with successively cleaner liquors, including a final extraction or wash with fresh liquor. The extraction liquor from one extraction stage in one vessel is used in another extraction stage in another vessel. Upon completion of the extraction, the liquor is drained from the vessel, the vessel is depressurized to a solvent condenser, and the remaining solvent is steam stripped from the charge and recovered. The used extraction liquor is treated in an alcohol recovery system by flash vaporization, condensation of the solvent vapors, and vacuum stripping of the residual liquor with steam. The alcohol-free extract is then treated to recover a concentrated aqueous lignin suspension and a concentrated aqueous carbohydrate solution.

Term
No projected expiry on record.
- Priority
- Filed
- Granted
- Today
9 claims: 1 independent, 8 dependent
- 1Patentkrav 1. Fremgangsmåte ved oppslutning ved hjelp av oppløsningsmiddelekstraksjon, hvor lignin ekstraheres fra et oppdelt, fiberholdig plantemateriale i en rekke satsvis arbeidende ekstraksjonsapparater ved i hvert av disse å innføre en charge av det nevnte materiale og å bringe chargen i kontakt med en oppløsningsmiddelvæske for oppslutning omfattende en vandig oppløsning av en lavere alifatisk alkohol ved en oppslutningstemperatur av 160-220°C og et oppslutningstrykk av 10-50 atm., og hvor rå cellulosemasse fjernes fra ekstraksjonsapparatet, karakterisert ved at (a) et første ekstraksjonsapparat som inneholder en første charge av det nevnte materiale, fylles med en første væske for å fortrenge luft fra det første ekstraksjonsapparat, (b) den første væske erstattes med en annen væske med forholdsvis høyt innhold av oppløst faststoff, og den annen væske resirkuleres med forholdsvis høy hastighet gjennom det første ekstraksjonsapparat og gjennom en ekstern varmeveksler for å bevirke hurtig oppvarming av den første charge til oppslutningstemperatur i løpet av ikke over 10 minutter, og fortrinnsvis ikke over 5 minutter, idet det som den annen væske anvendes væske fra det nedenfor beskrevne trinn (d) erholdt under oppslutning av en annen chargé av det nevnte materiale i et annet ekstraksjonsapparat, (c) resirkuleringen av den annen væske fortsettes for å bevirke en opprinneliq ekstraksjon av den første charge, hvoretter den annen væske fjernes fra det første ekstraksjonsapparat , (d) innføring av en ytterligere væske slik at den strømmer gjennom den første charge i det første ekstraksjonsapparat på basis av ett enkelt gjennomløp for å bevirke ytterligere ekstraksjon av den første charge, idet det som den ytterligere væske anvendes en væske med et lavere innhold av oppløste faststoffer enn den annen væske, og idet den ytter' s ’ Ligere væske tas fra det nedenfor beskrevne trinn (e) ( erholdt under oppslutning av ytterligere en annen charge ·- \ av materialet i et tredje ekstraksjonsapparat, og (e) på forhånd oppvarmet fersk oppslutningsvæske bringes til å strømme gjennom den første charge i det første ekstraksjonsapparat på basis av ett enkelt gjennomløp for å bevirke sluttekstraksjon av den første charge.
- 2Fremgangsmåte ifølge krav 1, karakterisert ved at væske dreneres fra det første ekstraksjonsapparat, at trykket oppheves i det første ekstraksjonsapparat ved å frigjøre oppløsningsmiddeldampene i dette til en kondensator, at kondensert oppløsningsmiddel gjenvinnes som er egnet for fornyet anvendelse som den nevnte ferske oppslutningsvæske i trinn (e), og at damp ledes gjennom det første ekstraksjonsapparat for å strippe gjenværende oppløsningsmiddel fra den første charge, og de strippede oppløsningsmiddeldamper kondenseres for oppnåelse av et kondensat som er egnet for fornyet anvendelse som den nevnte ferske oppslutningsvæske i trinn (e).
- 3Fremgangsmåte ifølge krav 1 eller 2, karakterisert v ed at (f) den annen væske som er blitt fjernet fra trinn (c) utsettes for trykkopphevelse for å bevirke en delvis flashfordampning av oppløsningsmidlet, at de erholdte oppløsningsmiddeldamper separeres fra gjenværende væske' som er egnet for fornyet anvendelse som den nevnte første væske i trinn (a), og at (g) oppløsningsmiddeldampene kondenseres for erholdelse av et kondensat som er egnet for fornyet anvendelse som den nevnte ferske oppslutningsvæske i trinn (e).
- 4Fremgangsmåte ifølge krav 3, •karakterisert ved at (h) i det minste en del av den gjenværende væsken fra trinn (f) strippes med damp ved underatmosfærisk trykk, at de strippede oppløsningsmiddeldåmper fjernes og kondenseres for erholdelse av et kondensat som er egnet for fornyet anvendelse som den nevnte ferske oppslutningsvæske i trinn (e), og at den erholdte oppslemning som inneholder ligninfaststoffer og oppløste kullhydrater separeres.
- 5Fremgangsmåte ifølge krav 4, karakterisert v ed at den gjenværende oppslemning får avsettes for erholdelse av en fortykket ligninoppslemning og en overliggende væske, at den fortykkede oppslemning sentrifugeres for å skille et ligninslam fra en annen overliggende væske, at de nevnte overliggende væsker kombineres, og at de kombinerte væsker konsentreres ved inndampning for erholdelse av et kullhydratkonsentrat.
- 6Fremgangsmåte ifølge krav 5, karakterisert ved at varmen som avgis ved kondenseringen av oppløsningsmiddeldampene i trinn (g), anvendes for delvis tilførsel av den varme som er nødvendig for inndampningen.
- 7Fremgangsmåte ifølge krav 1, karakterisert ved at det som oppløsningsmiddelvæske for oppslutning anvendes en vandig oppløsning av ethanol, methanol eller blandinger derav i en konsentrasjon av 20-80 vekt%.
- 8Fremgangsmåte ifølge krav 7, karakterisert ved at alkoholen anvendes i en konsentrasjon av 40-60 vekt%.
- 9Fremgangsmåte ifølge krav 1, karakterisert ved at det anvendes en oppslutningstemperatur av 180-2L0°C og et oppslutningstrykk av 20-35 atm. I
Independent claims9
85 paragraphs in 3 sections, as filed
(74) Agent
Tandbergs Patentkontor AS, Oslo.
(56) Cited publications
US Patent No. 1856567, 3588104
<img file="NO149115B_D0001.tif" />
The invention relates to improvements in the preparation of cellulose pulp from wood or other fibrous plant materials using a solvent as a suspending agent.
The principle of separating lignin from cellulose using solvents is well known in the art, and methods have been proposed to utilize this in the essential analytical aid for the preparation of commercial pulp, e.g. in U.S. Patent No. 1856567 and U.S. Patent No. 3585104. However, such processes have been subject to severe limitations as to the removal of lignin, the quality and bleaching of the raw pulp, and the difficulties in recovering solvents and the separation of the lignin-containing fraction from them.
However, by means of the present method, it is possible to obtain a separation and recovery of the cellulose and lignin fractions in a very efficient manner, so that no significant air or water drag contaminants or solid waste from the process is present. In addition, the organic solvent is recovered very efficiently and can be recycled to the process, thereby overcoming a major obstacle to the practical utilization of digestion by a solvent.
Although a variety of solvents can be used to remove lignin from cellulose, aqueous mixtures or solutions of any of the lower aliphatic alcohols, such as methanol, ethanol, isopropanol, n-propanol or butanol, are used for the purpose of the present process. At it
In the preferred embodiment of the present process, ethanol is used because it is relatively easy to recover and because there is essentially no reaction between the ethanol and the tree or other fibrous plant material. Some methanol is formed by the digestion process, and the recycled solvent may be a mixture of methanol and ethanol, or methanol alone may advantageously be used.
The invention thus provides a method of digestion by means of solvent extraction, in which lignin is extracted from a divided fibrous plant material in a series of batch-extracting extractors by introducing in each of them a charge of said material and contacting the charge with
In a solvent for digestion comprising an aqueous solution of a lower aliphatic alcohol at a digestion temperature of 160-220 ° C and a digestion pressure of 10-50 atm, and wherein crude cellulose pulp is removed from the extraction apparatus, and the process is characterized in that (a) a first extraction apparatus containing a first charge of said material is filled with a first liquid to displace air from the first extraction apparatus, (b) replacing the first liquid with a second liquid having a relatively high dissolved solids content, and the second liquid being recycled at a relatively high rate through the first extraction apparatus and through an external heat exchanger to effect rapid heating of the first charge to the digestion temperature during of not more than 10 minutes, and preferably not more than 5 minutes, wherein, like the second liquid, liquid from the step (d) described below obtained during dissolution of a second charge of said material in another extraction apparatus is used, (c) the recycling of the second liquid is continued to effect an initial extraction of the first charge, after which the second liquid is removed from the first extraction apparatus, (d) introducing an additional liquid so that it flows through the first charge of the first extraction apparatus on the basis of a single passageway to effect further extraction of the first charge, being that of the additional liquid
<td></td><td>a liquid having a lower content of dissolved solids is reversed than the other liquid, and the additional liquid is taken from it.</td>
<td>*> / ί</td><td>The step (s) described below are obtained during the digestion of yet another charge of the material in a third extraction apparatus, and (e) pre-heated fresh containment liquid is caused to flow through the first charge of the first extraction apparatus on the basis of a single pass-through to effect final extraction of the first charge. To avoid adverse effects on both the rate and extent of the lignin extraction, the wood chips or other fibrous plant material should be heated to extraction or digestion temperature in the first extraction step within not more than 10 minutes, preferably not more than 5 minutes. In order to ensure a maximum amount of lignin extraction with a minimum amount of deposited undesirable polymerized fractions, the extraction vessel should be so designed that there is minimal channel formation and / or mixing of the solvent of alcohol and water. Thus, the container may have a high height-to-diameter ratio of 4: 1-15: 1, preferably approx. 10: 1. Solvent extraction. can be carried out using a variety of concentrations of alcohol as a solvent (in aqueous solution), from as little as 20% by weight to as much as 80% by weight. However, a preferred range of conditions comprises an alcohol concentration in water of 40-60% by weight, a pressure of 20-35 atmospheres and a temperature of 180-210 ° C. In order to provide wood chips or other fibrous plant material to the solvent and water pressure system with minimal solvent loss and to achieve a minimal back-mixing and maximum extraction, the invention utilizes a number of batch extraction containers in series.</td>
follow, so that solvent from one extraction step in one container is used for another extraction step in another container, as further described below.
It is a further feature of the invention that the present process is carried out so that after the extraction of lignin has been completed in a given extraction vessel, the remainder of the solution of alcohol and water is discharged from the vessel, the pressure is reduced by means of a condensation system for alcohol and water, and the remaining solvent is then removed from the crude cellulose residue using water vapor or another suitable stripper, while the crude cellulose is still in the extraction vessel, removing the stripped vapors from the extraction vessel and into the condensation system for alcohol and water. The crude cellulose mass is then discharged from the extraction vessel by displacement with water. The raw material is not only liberated from lignin, but it is also washed thoroughly and is essentially completely liberated from solvent. The raw material is of high quality and, after defibration, constitutes a mass which is easily bleached by conventional methods to obtain high quality bleached pulp suitable for a variety of applications.
For further solvent recovery, the final extract solution from the solvent extraction section of the process is subjected to a stripping to remove and recover the alcohol from the aqueous extract solution. In order to achieve this separation while minimizing the formation of tar or highly polymerized solid forms of lignin which would have been prone to fouling the equipment, the separation is carried out under vacuum after the extract solution has first been subjected to an equilibrium flash evaporation. This vacuum should be as low as possible, but in practice it may be 0.1-0.8 atmosphere, preferably 0.5 atmosphere, and at this pressure the temperature obtained will be such that the lignin-containing precipitate which forms as the alcohol stripped will be passed through the stripping unit in the form of a suspension.
After the alcohol has been evaporated from the extract solution, the aqueous residual slurry of lignin can be treated in the usual manner. However, improved results are obtained by first adding lignin-nopp149115
<img file="NO149115B_D0002.tif" />
the slurry bottom deposit to then concentrate the thickened lignin slurry in a separator, such as a solid centrifuge bowl, and the resulting lignin sludge or lignin cake obtained is suitable for combustion as fuel in conventional furnaces and for conventional boilers. The overlying aqueous liquid containing substantially sugars, hemicellulose, organic acids and small amounts of low molecular weight lignin fractions is then evaporated in the usual manner. The evaporation does not substantially result in deposits or soiling of the equipment due to the absence of high molecular weight lignins or lignin polymers.
The sugar-carbohydrate concentrate containing 50-70% solids, preferably approx. 60% solids can be sold as a by-product for use as animal feed or it can be converted into other chemical or biological products. If the use of such a by-product is not practical, the concentrate may also be incinerated in a conventional furnace or for a conventional boiler for recovery of the by-product's calorific value in the form of water vapor which may be used in the above alcohol stripping step. The combustion of the lignin sludge and of the aqueous sugar concentrate can be accomplished by mixing the two streams which will thereby produce a mixture having similar properties as that of a light fuel oil, except for a lower calorific value. However, combustion of the mixture will not result in the formation of undesirable pollutant combustion products, such as sulfur compounds, chlorides and similar compounds, nor will any significant problems common to conventional digestion methods occur, since the only solid obtained by combustion is a solids determined by the relatively low ash content of the tree or other fibrous plant material that is decomposed.
Thus, the improved digestion process by alcohol of the invention not only results in a high quality mass which can be easily bleached, but if the lignin and / or sugar carbohydrate fractions are not commercially available as by-products, they can be used as fuels so that the present process will become essentially energy self-sustaining. The substantially complete avoidance of contaminants by the incineration of the wreckage materials from the backing is another major advantage of the method. The modest content of BOD in the condensate from the evaporator can be easily treated by a conventional secondary
14911 5 treatment so that a substantially pollution-free digestion process is obtained. '' '
A particular example of an embodiment of the present method is shown in the drawings, of which fig. 1 is a flow chart showing the solvent extraction steps of the present process; and FIG. 2 is a flowchart which is a continuation of the flowchart of FIG. 1 and showing the solvent recovery step of the present process and, moreover, a preferred method of handling the waste products.
In FIG. 1, the solvent extraction portion of the present process is shown, using a variety of batch extraction vessels. As an example of a commercial embodiment of the present process, 9 such containers can be used, and each container is operated in a cover-to-cover cycle of 3 hours and used sequentially so that a finished batch of raw cellulose pulp is removed from one of the containers every twenty minute. For convenience, only three such containers are shown in FIG. 1 in the form of long tubular extractors 10, 11 and 12. In order to avoid problems with duct formation and / or fluid back-mixing, the ratio of the height and diameter of the extractors should be relatively high, as mentioned above.
Each extractor is used for a sequence of steps which can be briefly described as (1) tile filling, (2) displacement of air, (3) rapid heating of primary extraction fluid recycling, (4) at least one wash with used liquid, (5) final washing. with freshly added liquid, (6) pressure lift and water vapor treatment, and (7) depletion of pulp. It will be understood that at any given time, each extraction apparatus will be at a different stage of the process, and the sequence of steps in each extraction apparatus may be performed automatically by ordinary control and instrumentation. Although the necessary wiring system for operating the three extraction apparatus 10, 11 and 12 is shown in FIG. 1, it will suffice to describe a complete operating cycle for only one of the extractors.
Thus, the extractor 10 is first filled with wood chips which can be pneumatically transported through a supply distribution line and a branch line 14 to the extractor 10. After the chip has been filled, air is flushed out of the extractor 10 by a suitable relatively cold backing or extraction liquid. According to the illustrated embodiment, a relatively cold spent containment or extraction fluid is introduced into the bottom of the extraction apparatus 10 from a supply distribution line, 16, a sub-conduit 17 with a valve 18 and an inlet manifold 18. Ί in accordance with the commonly used cellulose pulping process. terminology, this fluid will then be referred to as black liquor. The displaced air flows from the upper part of the closure apparatus 10 through an outlet manifold 26, a branch line 27 with a valve 28 and a return manifold 29 to a cold storage tank 31 (FIG. 2). From the tank 31, the air flows via a conduit 25 to a capacitor 24 and is discharged there into the atmosphere by a suitable discharge device (not shown).
The air displacement from the extractor is necessary to prevent serious flashing when a high temperature and high pressure extraction fluid is later introduced into the extractor. As explained below, the storage tank 31 (Fig. 2) is a suitable source of cold black liquor for the air displacement step and from which the liquor is removed.<sub>e</sub>d a relatively low temperature, e.g. about. 80 ° C, by means of a pump 32 and supplied to the manifold 16. However, any suitable liquid can be used to flush air out of the extraction apparatus, e.g. a pure solvent of alcohol and water which can be supplied from the fresh tank 106 (described below). As a result of the air displacement step, the tile in the extractor is briefly immersed in and impregnated with the cold displacement fluid.
Once the extractor 10 has been filled, the valve 18 is closed to interrupt the flow of cold black liquor through the extractor, and a primary extraction liquid comprising a used solvent mixture having a relatively high solids content and the desired extraction temperature and the desired extraction pressure, the bottom of the extractor 10. D. A primary extraction fluid is supplied from a collection device 33 via a conduit 34, a pump 36, a conduit 37, a supply distribution conduit 38, a
149115 '.8 branch line 39 with a valve 41 and the inlet manifold 19. When the extraction apparatus is filled with cold black liquor, it will immediately be pressurized with little or no flashing. The cold black liquor is displaced and returned from the top of the extraction apparatus 10 via the collection line 26, line 27 and collection line 29 to the black liquor storage tank 31. At this stage, the valve 28 is closed and the outlet flow is changed so that the primary extraction fluid flows from the extraction apparatus 10 through the manifold 26. a branch line 42 with a valve 43 and a connecting line 44 to a peak load heater 46. From the heater 46, the primary extraction liquid is returned via a line 47 to the collecting device 33.
During the first part of the period when the primary extractor liquid is recycled through the extractor 10 and the heater 46 in succession, the circulation is performed at high flow rate and with high heat supply from the heater 46 to bring the chip edge in the extractor to boiling temperature over a very short time. The flow rate and heat input are e.g. such that the preferred extraction temperature of 180-210<sup>o</sup>Preferably, C is obtained in the extraction apparatus within not more than 5 minutes, and at least within not more than 10 minutes. Once the chips have been brought to the boiling temperature, the recycle of the primary extraction liquid is continued at high flow rate for the remainder of the primary extraction period, but with a greatly reduced heat supply from the heater 46. The heat supply during this time will usually be sufficient to replace heat loss, so that substantially isothermal extraction conditions are maintained in the extractor 10. Thus, a very uniform boiling condition is obtained during the primary extraction period, and a very high rate of removal of lignin is removed. the result is that 70-80% of the total removal of lignin from the tile is achieved during the primary extraction period. Towards the end of the primary extraction period, valve 43 closes and the extraction fluid effluent from the extraction apparatus flows from the outlet manifold 26 and via a conduit 48 with a valve 49 to an outlet manifold 51 which is connected to a recovery device 52 for recovery of supply. As described below, the spent extraction liquid is continuously supplied under pressure from the collection device 52 via a conduit 53 with a valve 54 to the alcohol recovery system.
As mentioned above, in the recycling of spent extraction liquid with a relatively high content of dissolved solids, a substantial proportion of the lignin removal is obtained during the primary extraction period. Thereafter, the chip joint is subjected to one or more extractions or washes at a one-time pass, ie. without recirculation, and each such wash on a once-through-feed basis is carried out with a liquid having a progressively lower dissolved solids content, until the final wash based on one-time feed is carried out with freshly added, substantially lignin-free liquid. In the particular embodiment disclosed herein, after the primary extraction period when the liquor is recycled at high speed, the chip joint is subjected to an intermediate one-time passage wash with a dissolved solids content liquid, and then to a one-time final passage wash with new liquid. However, it will be appreciated that any desired number of intermediate disposable passageways can be performed.
Thus, while the extractor 10 is in its primary extraction period, as described above, the extraction apparatus 11 is in its intermediate single-pass extraction or washing period and the extraction apparatus 12 in its final single-extraction or washing period. Fresh solvent or fresh extraction fluid is supplied via a conduit 56 from the alcohol recovery system, as described below, to a fresh extraction fluid collection device 57. The fresh liquid is removed via a conduit 58 by means of the pump 59 and fed through a conduit 61 to a collection conduit 62 and then through a branch conduit 63 with a valve 64 to an inlet conduit 66 and upward through the extraction apparatus 12 containing a second chip joint. The wastewater with a relatively low content of dissolved solids leaves the top of extractor 12 via an outlet manifold 67 and a branch line 68 with a valve 69 to a manifold 71. From the manifold 71, the liquid flows through a line 72 to another manifold 73 and thence through a branch line. 74 with a valve 76 to an inlet manifold 77 which communicates with the bottom of the extraction apparatus 11 which contains a further different chip batch. The spent liquid with an increased content of dissolved solids leaves the top of the extractor 11 via an outlet manifold 78 and flows through a branch line 79 with a valve 81 to the manifold 44 in which the liquid is fed with the recirculating wastewater from the extractor 10. Thus, it is seen that fresh liquid flows in sequence through the extraction apparatus 12 and 11 and then forms part of the primary extraction fluid which is recycled through the extraction apparatus 10 and the heating apparatus 46. The liquid thus supplied to the collecting device 33 compensates for the proportion of the primary extraction liquid is branched to the feed liquid recovery device 52 towards the end of the primary extraction period.
With continued reference to the flow through the extraction apparatus 10, the setting of the necessary valves is changed at the end of the above-described primary extraction period, so that fresh liquid from the manifold 62 now flows through a branch line 82 with a valve 83 to the inlet manifold 77 and then through the extraction apparatus 11. . The effluent from the extractor 11 flows through the outlet manifold 78, a manifold 84 with a valve 86, the manifold 71, conduit 72, the manifold 73, a manifold 87 with a valve 88, and the manifold 19 into the bottom of the extractor 10. From the top of the extractor 10, the effluent flows through the outlet manifold 26 and the branch line 42 to the manifold 44 as part of the recirculating primary extraction fluid now supplied from the manifold 38 to another extraction apparatus in the system which is in its primary extraction period. The flow rate through the extraction apparatus 10 during subsequent disposable extraction or washing periods is substantially less than during the primary extraction period or recycling extraction period, and although the lignin removal continues during the secondary extraction period at a rapidly decreasing rate, the main effect is the the diffusion of dissolved solids into the tile into the percolating wash liquid under the influence of the applied concentration gradient. Towards the end of the secondary extraction or washing period, the flow of fresh liquid to the extractor 11 is stopped and the liquid in the extractor
<img file="NO149115B_D0003.tif" />
is discharged through a conduit 89 with a valve 91 to a conduit 92 and then through a conduit 93 to a pump 94 which, via a conduit 96, communicates with the conduit 73. From the conduit 73, the liquid flows through conduit 87 and the conduit 19 to the extractor apparatus 10 and thence through the conduit 26 and conduit 42 to the primary fluid circuit described above.
By adjusting the valve appropriately, the extractor 10 now enters its final extraction or washing period where fresh liquid is used. Thus, fresh liquid is now supplied from the collecting device 57 via the conduit 62, a branch line 97 with a valve 98 and the conduit 19 to the bottom of the extraction apparatus 10. Wastewater from the top of the extractor 10 flows through the manifold 26, a branch line 99 with a valve 101, the manifold 71 and the manifold 72 of the manifold 73, from which the liquid flows through another extraction apparatus in the system which is in its secondary extraction or washing period. The removal of lignin proceeds to a lesser extent during the final extraction period, but the main effect obtained is again the leaching of dissolved solids from the tile, so that towards the end of the final extraction period the residual solids content in the tile is quite low.
Towards the end of the final extraction period, the flow of fresh liquid to the extractor 10 is stopped, and the liquid in the extractor 10 is discharged through a conduit 102 with a valve 103 to the conduit 92 and is supplied thereto via conduit 93, pump 94, conduit 96 and conduit extraction 73 to the subsequent extraction conduit. in the system and which are in their secondary extraction or washing period.
The tile in the extractor apparatus 10 which has been subjected to a primary recirculating extraction step and two consecutive disposable passageways, respectively. used liquid and fresh liquid, is now ready for discharge from the extractor 10. First, however, the extractor is subjected to a regulated pressure cancellation where the solvent vapors in the extraction pore 10 are discharged via a branch line 21 with a valve 22 to a discharge distribution line 23 and then to that in FIG. 2 showed recycling system. It can be seen from this that the alcohol-rich vapors leaving the extraction apparatus flow through the blow-down capacitor 24 to form a condensate flowing through a conduit 104 to a fresh liquid storage tank 106. After the pressure lift, the tile is subjected to water vapor stripping in the extractor 10 by introducing low pressure water vapor from a supply distribution line 107 and via a branch line 108 with a valve 109 at the bottom of the extractor. 10. The water vapor flows upwardly through the chip joint, thereby evaporating the residual alcohol, and the mixture of water vapor and alcohol vapor flows through line 120 and collection line 23 to the blow-off capacitor 24, in exactly the same way as during the pressure lifting step. Water vapor treatment continues until «only trace amounts of alcohol are left in the tile.
After the water vapor treatment is completed, the extractor 10 is pumped full of water (by means of a device not shown), and then the mixture of water and raw material is discharged from the bottom of the extractor through a branch line 111 with a valve 112 to an outlet collection line 113 and thence to a pump ( not shown) which transfers the raw material to ordinary papermaking steps. Nozzles for injecting water may be provided in the extraction apparatus at appropriate locations to ensure complete discharge of the pulp from the extraction apparatus. After the extraction apparatus has been emptied, it is ready to be filled again with chips and for further containment treatment as described above.
Although the schedule may be varied to meet the requirements of a particular solvent-based digestion, a typical plan for a single extraction apparatus operated after a 3 hour cover-to-cover cycle is presented in Table I below:
<img file="NO149115B_D0004.tif" />
TABLE I
<img file="NO149115B_D0005.tif" />
<td>T</td><td>Time (min)</td><td colspan="2">Operation</td>
<td>'Φ' '' '</td><td> 0-15</td><td>(A)</td><td>Fill with tile.</td>
<td></td><td> 15-20</td><td>(B)</td><td>Replacement of air with cold black liquor.</td>
<td></td><td> 20-25</td><td>(C)</td><td>Replacement of cold black liquor and recirculation of primary extraction fluid for rapid heating.</td>
<td></td><td> 25-40</td><td>(D)</td><td>Recirculation of primary extraction fluid at digestion temperature, and branching of primary extraction fluid to collection device for recovery of feed liquid.</td>
<td></td><td> 40-53</td><td>(E)</td><td>One-time passage washing with secondary extraction liquid.</td>
<td></td><td> 53-60</td><td>(F)</td><td>Continuation of (E) with secondary extraction fluid discharged from the preceding extraction apparatus.</td>
<td></td><td> 60-7 3</td><td>(G)</td><td>One-time passage washing with fresh extraction liquid.</td>
<td></td><td> 73-80</td><td>(H)</td><td>Extraction of extracted liquid.</td>
<td></td><td> 80-110</td><td>(IN)</td><td>Press Repeal.</td>
<td></td><td> 110-165</td><td>(J)</td><td>Evaporation with water vapor.</td>
<td></td><td> 165-180</td><td>(K)</td><td>Fill with water and drain mixture</td>
water and plenty out.
Based on the schedule of each operation listed in the table
You are the one. complete cycle plan for a system of 9 extractors shown in Table II below:
<td></td><td>o Ύ</td><td>o co 1—1 1</td><td colspan="2">o OJ 1</td><td colspan="2">o <r 1</td><td colspan="2">o kD 1</td><td colspan="3">o CO 1</td><td>oo r- < 1</td><td>o OJ H</td><td>o <r 1</td>
<td></td><td></td><td>m</td><td></td><td>H</td><td>LT »</td><td></td><td>□ n</td><td></td><td></td><td>un</td><td></td><td>un</td><td>un</td><td>un</td>
<td>'-s</td><td></td><td></td><td></td><td></td><td>OJ</td><td></td><td><r</td><td></td><td></td><td>Ό</td><td></td><td> 00</td><td>o</td><td>Beer</td>
<td></td><td> 1—1</td><td>i-4</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td>1 "in</td><td></td>
<td></td><td>UD</td><td>H</td><td></td><td>O</td><td></td><td>o</td><td></td><td>o</td><td></td><td></td><td></td><td></td><td>un</td><td>un</td>
<td></td><td><r</td><td>queue</td><td></td><td>CO</td><td>UD</td><td>co</td><td>un</td><td>co</td><td></td><td>un</td><td></td><td>un</td><td>o</td><td>OJ</td>
<td></td><td>t- *</td><td>r)</td><td>IFJ</td><td> 1—1</td><td>OJ</td><td>rh</td><td><r</td><td>1 in</td><td></td><td>kD</td><td></td><td> 00</td><td>ride</td><td></td>
<td></td><td> 1</td><td> 1</td><td> 1</td><td></td><td></td><td> 1</td><td> 1</td><td></td><td></td><td></td><td></td><td> 1</td><td></td><td> 1</td>
<td></td><td>o</td><td>o</td><td>o</td><td>o</td><td>o</td><td>o</td><td>o</td><td>o</td><td></td><td>o</td><td></td><td>o</td><td>o</td><td>o</td>
<td></td><td>σ></td><td> <—4</td><td></td><td>m</td><td></td><td>un</td><td></td><td>o "</td><td></td><td> 1—1</td><td></td><td>cn</td><td>un</td><td>Γ--</td>
<td></td><td></td><td>r - 4</td><td></td><td>| -u</td><td></td><td>IN-</td><td></td><td>r-1</td><td></td><td></td><td></td><td></td><td></td><td></td>
<td></td><td></td><td>o</td><td></td><td>O</td><td>o</td><td></td><td>o</td><td></td><td></td><td></td><td>O</td><td></td><td></td><td></td>
<td></td><td>o</td><td>in-U</td><td></td><td>m</td><td>UD</td><td></td><td></td><td></td><td>o</td><td></td><td> 00</td><td>c</td><td>o</td><td>O</td>
<td></td><td>σ></td><td>t <</td><td></td><td>in 1</td><td>r-1</td><td></td><td></td><td></td><td></td><td></td><td>in 1</td><td>m</td><td>un</td><td>r-</td>
<td></td><td> 1</td><td> 1</td><td></td><td> 1</td><td> 1</td><td></td><td> 1</td><td></td><td></td><td></td><td> 1</td><td> 1</td><td></td><td> 1</td>
<td></td><td>o</td><td>o</td><td></td><td>o</td><td>o</td><td></td><td>o</td><td></td><td>o</td><td></td><td>o</td><td>o</td><td>o</td><td>o</td>
<td></td><td> <0</td><td>co</td><td></td><td>o</td><td>OJ</td><td></td><td></td><td></td><td></td><td></td><td>kD</td><td></td><td>OJ</td><td><r</td>
<td></td><td></td><td></td><td></td><td>r-1</td><td>s ~ 4</td><td></td><td> 1—1</td><td></td><td></td><td></td><td>in 1</td><td></td><td></td><td></td>
TABLE II
Time interval (m ± n) for each operation
ICE
It can be seen from FIG. 2 shows that the spent extraction fluid flows under pressure from the collecting arrangement 52 via the conduit 53 to a liquid flash drum 121 in which the pressure is reduced so as to obtain a partial evaporation of the alcohol solvent and cooling of the residual liquid. A portion of the remaining black liquor having a relatively low temperature, e.g. about. 80 ° C, can be passed through a conduit 120 with a valve 122 to the cold black liquor storage tank 31 which is vented to the capacitor 24 via a conduit 25. As described above, the cold black liquor, when selected to flush air out of the extractors, is supplied from the container 31 via a conduit 30 and a pump 32 to the supply distribution conduit 16, and the liquid is returned to the container 31 via conduit 29. The evaporated solvent flows from the flash drum 121 in
via a conduit 123 to a boiler for reheating or a heat exchanger 12'4 which communicates with a first power evaporator 126. The alcohol vapors are condensed in the heat exchanger 124 and the condensate flows via conduit 127 and a conduit 128 to the storage tank of fresh liquid.
The major portion of the cold residual black liquor flows from the flash tank 121 via a conduit 129 with a valve 131 and is introduced into the upper part of a vacuum stripping tower 133. It is desired to use a vacuum to lower the slurry temperature so that the precipitated lignin will not adhere to and deposit on the turret surface folds. If desired, the liquid removed from the flash tank 121 can be cleared to remove any precipitated lignin before the liquid is transferred to the stripping tower 133. Water vapor is supplied at the bottom of the vacuum stripping tower 133 via a conduit 134 from an evaporator 166 which is described below, and a conduit 136. 128 to the fresh liquid storage tank 106. Although not shown in the drawings, it will be appreciated that a portion of the condensate from the condensing apparatus 138 may be returned to the top of the stripping tower 133 if a rectification section is desired at the top of the tower.
It can be seen that the fresh liquid supply in the tank 106 comprises the top vapor condensate from the extraction apparatus and introduced via line 104, the condensed vapors from the flash drum 121 and introduced via lines 127 and 128, and the condensed top vapors \ from tower 133 and introduced via line 128. substitute alcohol can be added to the fresh liquid supply via a conduit 139. Fresh liquid is removed from the storage tank 106 via a conduit 141 by means of a pump 142 and discharged via a conduit 143 into a heater 144 heated by water vapor from conduit 134 and conduit 146. The heated fresh fluid then flows through conduit 56 to the collecting device. 57 for the fresh liquid.
A bottom stream is removed from the tower 133 via a conduit 147. This stream consists of a water slurry containing precipitated solids (essentially lignin) and dissolved materials which are mainly of the carbohydrate type. The aqueous slurry flows from conduit 147 to a thickening apparatus or bottom deposition apparatus 148, wherein the precipitated lignin is deposited with a dry matter content of 5-15% leaving a clear aqueous solution of carbohydrate as the overlying layer. A bottom slurry is removed from the clarifier 148 via a conduit 149 by means of a pump 141 and discharged via a conduit 152 into a centrifuge 153 in which the solids content of the slurry is increased e.g. to 30-40%. A concentrated aqueous lignin suspension is removed from the centrifuge 153 via line 154.
The clear stream from the centrifuge 153 is removed via a conduit 156 and combined with the overlying clear liquid flowing from the top of the clarifier 148 via a conduit 157. The combined liquids are pumped by means of a pump 158 through a conduit 159 to the first power evaporator 126. Heat / is supplied to the evaporator 126 by recirculating a portion of the concentrated liquid via a conduit 161 and a conduit 126 through the boiler for renewed heating 124 and thence via a conduit 163 back to the evaporator apparatus 126. The remainder of the concentrated liquid from the first evaporator apparatus 126 flows via line 162 and line 164 to a second power evaporator 166 in which a concentrate is obtained containing 40-50% solids. The concentrated liquid is removed via a conduit 167 by the pump 168, and a portion of this liquid is recycled via a conduit 169 and a conduit 171 to a boiler 172 for reheating and from there via a conduit 173 back to
- -ήτΠιΐή'ΐΓ- vaporizer apparatus 166. The boiler 17 for renewed heating is heated by means of top vapor flowing from the first vaporizer 161 through a conduit 174. The remainder of the concentrated stream from the vaporizer 166 is removed via line Ϋ. 169 in the form of an aqueous carbohydrate concentrate. The water vapor removed from the second power vaporizer 166 via conduit 134 will generally suffice to meet the requirements of stripping column 133 and heater 144, but if necessary, replacement water vapor may be supplied via conduit 176.
From the above system for handling waste products, it will be seen that the aqueous lignin suspension and the aqueous carbohydrate solution are concentrated separately, thereby avoiding soiling of the evaporator apparatus tubes with lignin. If it is economically desired to handle lignin and carbohydrate by-products, the streams removed via lines 154 and 169 may be further processed. The two streams can otherwise be brought together and into a boiler for the incineration of waste products, in which their energy content is recovered in the form of process water vapor.
Contents3
7 sheets
Sheet 1 Sheet 2 Sheet 3 Sheet 4 Sheet 5 Sheet 6 Sheet 7
18 members in 9 offices
Priority claims3
| Document | Office | Kind | Date |
|---|---|---|---|
| 238294 | Canada | A | |
| 238294 | – | – | – |
| CA19750238294 | – | – | – |
Members18
| Document | Office | Kind | |
|---|---|---|---|
| FI762745A | Finland | A | |
| FI762745A7 | Finland | A7 | |
| SE7611648L | Sweden | L | |
| NO763603L | Norway | L | |
| DE2637449A1 | Germany | A1 | |
| JPS5259702A | Japan | A | |
| US4100016A | United States of America | A | |
| ATA706376A | Austria | A | |
| CH617476A5 | Switzerland | A5 | |
| CA1079008A | Canada | A | |
| AT369801B | Austria | B | |
| SE428028B | Sweden | B | |
| NO149115BThis record | Norway | B | |
| FI65290B | Finland | B | |
| NO149115C | Norway | C | |
| FI65290C | Finland | C | |
| JPS616193B2 | Japan | B2 | |
| DE2637449C2 | Germany | C2 |
Numbers
- Publication, DOCDB
- 149115
- Publication, EPODOC
- NO149115B
- Application
- 763603
- Application, DOCDB
- 763603
- Application, EPODOC
- NO19760003603
Titles2
- Norwegian
- FREMGANGSMAATE VED OPPSLUTNING AV FIBERHOLDIG, VEGETABILSK MATERIALE VED EKSTRAKSJON MED VANDIG OPPLOESNINGSMIDDELHOLDIG OPPSLUTNINGSVAESKE
- English
- PROCEDURE FOR THE CONSUMPTION OF FIBER-CONTAINED VEGETABLE MATERIALS FOR EXTRACTION WITH Aqueous SOLVENT CONSUMPING FLUID
Classification
- CPC, 1
- D21C3/20
- IPC, 4
- B01D11 02
- D21C3 00
- D21C3 18
- D21C3 20