Process for sorbent obtaining

Description:

The invention relates to the food industry, in particular to a process for obtaining sorbent for clearing and stabilizing must, juice, wine and other beverages.

The process of enhancing the clarification efficiency and stabilizing the sorbent by activating it with 10% H2SO4 solution is known [1].

The disadvantages of the process are the partial decomposition of the sorbent, the use of high acid concentration and the difficulties presented by the control of the degree of decomposition of the mineral.

There is also known a process for the treatment of bentonite which is used in the vinification industry with 0.3 ... 0.5 kg citric acid and 5 ... 35 kg Na₂COs per 1 ton of sorbent [2].

The disadvantages of the process are the use of citric acid, which is deficient and expensive and the use of large quantities of Na₂CCh.

Also known is the process of obtaining the sorbent suspension (bentonite, palagorskit), which consists in sanding and dispersing it in iron or aluminum salt solution with a concentration of 5 ... 50% depending on the exchange capacity of of the metal cations of the sorbent, keeping for 1 ... 2 hours and dehydrating it [3].

The disadvantage of the process is the use of the salt of iron or aluminum which in considerable concentrations can be found in the menfionaph sorbets. In addition, enrichment of the sorbent with iron or aluminum cations negatively affects the organoleptic characteristics and the stability of the treated product.

It is also known the process of obtaining the bentonite suspension used for clearing and treating the juice, must or wine which includes dispersing the sorbent, activating it by ultrasonic treatment

120 ... 150 Hz or 170 ... 200 Hz [4].

But the process is expensive, it requires special facilities to treat the sorbent with ultrasound.

Closer to the technical process than the requested process is the process of obtaining the sorbent, which includes bentonite softening in sodium carbonate solution, keeping for 10 to 12 hours. To the obtained mixture is added concentrated hydrochloric acid (36%) and boiled for 8 hours under phlegm. After the mixture is cooled, it is treated with acid solution or phosphoric acid salt which contributes to the passage of iron or aluminum into insoluble substances. The soluble fraction is separated from the liquid, the substances are added which prevent the aggregation of the glomeruli and are dried for 10 hours at 150 ° C [5].

The disadvantages of the process are: complicated and costly production technology, huge costs of electricity, phosphoric acid or phosphoric acid salts.

The problem solved by the present invention is to increase the active surface of the sorbent, increasing its ability to clarify and stabilize.

The process according to the invention removes the disadvantages mentioned above in that it includes bentonite milling, washing with water, treating with chemical agents, subsequent washing and decanting the mixture, plasticizing the obtained sorbent, drying and milling it. The proposed procedure requires that the treatment of bentonite with chemical agents be carried out in two stages: at the first stage - with 0.25 ... 5.00% hydrochloric acid solution at a mineral ratio: 1:20 solution for 2 ... 4 hours, after which the sorbent is washed with softened water and decanted, and in the second step - with saturated sodium carbonate solution heated to 4O ... 5O ° C in a dose of 0.8 ... 1.3% by weight of the mineral until the pH of the solution reaches 8.5 ... 9.2 with intense stirring for 3 ... 4 hours and the plasticization of the obtained sorbent for 3 ... 4 days.

Treatment of bentonite with hydrochloric acid leads to its enrichment with montmorillonite, removal of impurities, increase of the number of active centers on its surface and partial replacement of alkaline cations by hydrogen cations. At this о easy treatment the structure of the montmorillonite relay will not be destroyed.

At the same time, the treatment with saturated sodium carbonate solution leads to the substitution of the different cations in the mineral with the sodium cations that increase the active surface, intensify the dispersion effect and consequently increase the efficiency of clarification and stabilization of the sorbent.

The changes that occurred following the treatment of bentonite with chemical agents were controlled using the roentgen methods, of thermography and physico-chemical analyzes.

In the tab. 1 are the physico-chemical indices of the sorbent obfinufa following the treatment of bentonite with HC1 and Na₂CCh in different doses. As can be seen from the table, the content of montmorillonite and protein sorption, the main indices that characterize the efficacy of bentonite are higher than those provided by the technical norms (OCT 18-49-71). Using solution of HC1 in the treatment of bentonite with concentration less than 0.25% does not completely remove the calcite impurities from the mineral, due to which the activity on the surface of the sorbent is low. When the concentration greater than 5% is used, the structure of montmorillonite is destroyed and the sorption efficiency of the proteins is reduced. The use of sodium carbonate in a dose of 0.8 ... 1.3% by weight of bentonite ensures the sorbent is obtained with pH 8.5 ... 9.2.

The physico-chemical indices of the sorbent were determined according to OCT-18-49-71 "Бентониты для винодельческой промышленности".

Table 1

<td rowspan="3">Physical and chemical indices</td><td colspan="4">The value of indices</td>

<td rowspan="2">Conformable OCT 18-49-71</td><td colspan="3">Sorbenfi obfinufi according to the requested invention</td>

<td>0.25% HC1 pH 8.5</td><td>0.5% HC1 pH 9.2</td><td>HC1 5% pH 9.0</td>

<td>Organoleptic characteristic</td><td>no smell</td><td>no smell</td><td>no smell</td><td>no smell</td>

<td>Inflate,%</td><td>not less than 90.0</td><td> 90,0</td><td> 96,0</td><td> 98,0</td>

<td>Protein Sorption,%</td><td>greater than 25.0</td><td> 26,0</td><td> 38,0</td><td> 38,4</td>

<td>pH of bentonite suspension</td><td>not more than 9.0</td><td> 8,5</td><td> 9,2</td><td> 9,0</td>

<td>The contents of my world 11 times on it</td><td>not less than 0.4</td><td> 0,41</td><td> 0,52</td><td> 0,54</td>

<td>Iron concentration, mg</td><td>not more than 8.0</td><td> 0,7</td><td> 0,8</td><td> 0,7</td>

<td>Arsenium concentration</td><td>missing</td><td>missing</td><td>missing</td><td>missing</td>

<td>Sand content,%</td><td>not more than 1,0</td><td> 0,5</td><td> 0,5</td><td> 0,5</td>

According to the above, we obtain a new result - increasing the active surface of the sorbent, increasing its ability to clear and stabilize.

The procedure is performed as follows:

In the industrial processing units equipped with the necessary equipment bentonite from Larguța or Căciulia village, it is minced until 20x20x10 dispersion, washed with softened water to remove gravel and sand. Thereafter, a solution of hydrochloric acid with a concentration of 0.25 ... 5.00% at a bentonite ratio: a solution of 1:20. Mix well and leave to stand for 2 to 4 hours. The sorbent is then washed with softened water to a negative reaction with chlorine ions and the liquid fraction decanted.

The solid fraction (about 36%) is treated with intense stirring for 3 to 4 hours with a warm solution of 4O ... 5O ° C saturated with sodium carbon until the pH of the suspension reaches 8.5 ... 9.2 and is left to rest for 3 to 4 days. For the bentonite suspension to reach pH

8.5 .. .9.2 requires a dose of sodium carbonate of 0.8 ... 1.3% by weight of the mineral or 0.6 ... 0.65 dm³ saturated solution of NazCCh to 1 kg of mineral. The obtained wet sorbent can be used directly in the treatment of must, wine or juice or it can be dried, shredded, packed in special bags and used as needed.

The drying is carried out at a temperature of 12O ... 125 ° C for 8 ... 10 hours, and the grinding until

100 .. .200 pm in tum-diffuser dryer.

Example 1

Bentonite from Largufa or Căciulia village is air-dried, minced until 20x20x10 dispersion, passed through softened water to clean up impurities. 0.25% hydrochloric acid solution was dissolved with a mineralolysis ratio of 1:20. Mix well and leave to stand for 2 hours. The sorbent is washed with softened water until the reaction with chlorine ions is negative. The solid fraction is separated from the liquid by decanting and with intense stirring for 3 hours it is mixed with hot saturated solution of 40 ° C sodium carbonate at a dose of 0.8% by weight of the mineral until the pH of the suspension reaches value 8.5 and is left idle for 3 days.

The wet fraction of bentonite with the pH value 8.5 was used directly for the clarification of the wort, preventively dissolving with softened water up to the concentration of 20%.

The must obtained from the Aligote vine variety is sliced ​​into 4 cylinders of 500 cm each³, add bentonite suspension in 0.5 doses; 1.0; 1.5; 2.0 g / dm³, shake and leave to stand to clear the must. The clarified must decant from the sediment and proceed to fermentation.

Table 2

<td>Bentonite dose, g / dm³</td><td>Clarifying the must</td><td>Sediment volume,%</td><td>Volume of clarified fraction,%</td>

<td>control</td><td> 2,6</td><td> 40</td><td> 60</td>

<td> 0,5</td><td> 1,9</td><td> 38</td><td> 62</td>

<td>it a</td><td> 0,9</td><td> 35</td><td> 65</td>

<td> 1,5</td><td> 0,8</td><td> 42</td><td> 58</td>

<td> 2,0</td><td> 0,7</td><td> 46</td><td> 54</td>

The must was cleared using the turbidimetric method.

The data in the tab. 2 shows that the wort following the treatment with bentonite starting from the dose of 1.0 g / dm³ clear well, the clearing coefficient is 0.7 ... 0.9, but considering the volume of sediment and the volume of the clear fraction we conclude that the optimal treatment dose is 1.0 g / dm³. Increase the dose of bentonite above 1.0 g / dm³ it leads to an increase in sediment volume, but the efficiency of the clearing changes not significantly.

Example 2

Bentonite preparation and activation is performed as in ex. 1, except that the bentonite is treated with 5.0% hydrochloric acid solution for 4 hours and with saturated solution heated to 50 ° C sodium carbonate at 1.3% by weight of the mineral shaking 4 hours until the pH of the suspension reaches 9.2 and the plasticization for 4 days.

After that, the liquid fraction is removed from the solid fraction by decanting and the last fraction is dried.

The dehydration of the sorbent is carried out in the drying tower tower at 125 ° C for 8 hours. The dehydrated sorbent is ground to a particle dispersion of 100 µm and packed in special bags of 50 kg each.

Preventing treatment, bentonite suspension with a concentration of 20% is prepared. For this 20 g of bentonite is mixed well with 80 g of hot water, left to swell for 20 ... 24 hours. After this the suspension is stirred, heated to boiling and after cooling it is brought with water to the level of 100 cm³. For treatment, 5 cylinders of 500 cm each are taken³, pour dry white wine Sovignion and administer bentonite suspension starting with 0.5 dose; 1.0; 1.5; 2.5 g / dm³. The samples are stirred well and allowed to stand for 1 day for wine clarification. The clarified wine is filtered.

Table 3

<td rowspan="2">Bentonite dose, g / dm³</td><td rowspan="2">Wine clarification after 24 hours</td><td colspan="3">Resistance to disorders</td>

<td>protein</td><td>crystalline</td><td>albumin concentration, mg / dm³</td>

<td> 0,5</td><td>troubled</td><td>unstable</td><td>stable</td><td> 28,0</td>

<td>it a</td><td>opalescent</td><td>unstable</td><td>stable</td><td> 20,0</td>

<td> 1,5</td><td>opalescent puffin</td><td>stable</td><td>stable</td><td> 10,0</td>

<td> 2,0</td><td> —</td><td> —</td><td>unstable</td><td> 7,0</td>

<td> 2,5</td><td> —</td><td> —</td><td> —</td><td> 5,0</td>

The data presented in the tab. 3 shows that the optimal treatment dose of wine with bentonite suspension is 1.5 g / dm³. Treating wine with such a concentration of bentonite decreases the concentration of albumin to 28.0 mg / dm³ at 10.0 mg / dm³.

It becomes stable in protein and crystalline disorders. Bentonite dose increase decreases albumin concentration to 1.5 g / dm³, but crystalline cascades appear.