Method for preparing mixed crystal nanometer titanium dioxide suspension from double precursors

Method for and pilot body and nanometer crystal titanium dioxide suspension

technical field

[0001] The invention relates to a inorganic material and preparation method thereof, particularly refers to the double pilot body and nanometer crystal titanium dioxide suspension method, belonging to the technical field.

[0002]

background technology

[0003] Of 1972. A Fjishima and K. Hindan the η is arranged on the semiconductor device of electrode discovers the light water of the cracking photoelectricity catalytic cracking phenomenon,Since 1976, scientist heating Carey are in a conducted with the grinding of degradation to the violently poisonous sand multi-chlorine biphenyl through the nanometer titanium dioxide, multiple scientific grinding workers invest of the photocatalytic performance for nanometre titanium dioxide the grinding applied in the environment-friendly, the different photocatalytic technology with aroused the centre-free of grinding worker. TiO2 because of with a photocatalytic activeness is high, stability bar, a human body non-toxic, the lower plate and a merits component, wherein the multiple semiconductor photochemical blooming, the application field provided with a degradation and a to paper, the air purifying, wherein, the whole heavy metal of an organic wastewater and engaged with numerous aspects. Photocatalytic performance of the nanometer titanium dioxide is not can only degrade of the organic material of the biology the water and air is unable to degrade, wherein degradation is H2O and CO2; moreover of the existing inorganic metal ions in water deposits, therefore the nanometer titanium dioxide is applied in the organic dye sewage, the air toxic gas, inorganic heavy metal ions and a pollution environment-friendly of governments. The recent years, the grinding discovered of with high photocatalytic active T^2 multiple and anatase dealt with a rutile the mixed crystal structure; to the catalytic movable Degussa P25 TiO2 is a Anatase (80%) +Rutile (20%) of the crystallizer. The mixed crystal with high-activity is because of the effect of, wherein the anatase the surface door-shaped of crystal the light rutile the crystallizing layer, a sleeve can turn to the anatase crystal to photoproduction the electronic hole is fixed to the separation, and two bulk phase the compound probability, and improving the electronic the diffusion speed. Multiple people are simple in the middle development the grinding process, which is inexpensive, and with industrial and production method for preparing high photocatalytic active nanometre titanium dioxide.

[0004] The gift, a nanometre titanium dioxide preparation method of for gaseous phase synthesis and high-pressure water heat - seal arranged on one sol gel method and carbon dioxide. The although gaseous phase bottle capable of high-grade with nanometre titanium dioxide powder, and a gas phase reaction to be a material head, the energy consumption of high. In addition, the gas phase reaction device according of the high-temperature blade instantaneously, and in with a high claim to form, material; the material through-port port and reactor, with a group of claims a questions. High-pressure water heat - seal arranged on without requirement the high-temperature coating to obtain the crystal bar nanometre titanium dioxide directly, when presenting avoided the high-temperature coating layer of hard reunion. The method of operation, and has high to the claim device. A preparation method of use raw material multiple and high purity alkoxide titanium and titanium inorganic salt, part production cost with higher questions.

[0005]

The invention

[0006] That of the insufficient, An objective of the present invention claims a process of the existing technology exists is simple, feasible, comprising a to the claim device, which is inexpensive, and with the upper photocatalytic activeness to degrade the organic material can effectively method for preparing stable nanometre titanium dioxide suspension.

[0007] The invention solves the middle technical goes technological means to realize to the:

Method for and pilot body and nanometer crystal titanium dioxide suspension, wherein preparing steps: (1) Compounds the TiCl4 storing and TiCl3 cooling liquid close to the deionized water o°c, and dry pipette to move to take the ration TiCl4, a TiCl4 with a funnel pipe slowly to the ice water tank, and a deionized water of a stirring, obtains the colorless transparent TiCl4 solution, before the winding titanium ion and 0. 5-1.0 mOl/L,0°C preservation spare;

Taking the ration TiCl3, dilutes with the deionized water agent, compounds the density 0. 5-1. mol/L 0 TiCl3 introduced;

(2) And the nanometre preparing titanium dioxide wet type as the ration the deionized water circulating, the inorganic alkaline liquid to obtain the inorganic is deionized water storing, wherein the situation of stirring, (1) compounds the end of the TiCl4 storing and TiCl3 liquid according to Ti4+: Ti3+ is 9:1-1 5: proportion mixing and a to the plates of the inorganic is deionized water storing, - section of the liquid PH value is 1. Or/. 5th, Constant temperature 2-10h comprising a 50-100°C the condition, obtains the white depositing product; the filtering and function, obtains the nanometer titanium dioxide wet type;

(3) And the configuration nanometre titanium dioxide suspension the nanometer titanium dioxide wet type the step (2) made system, a circulating the amount of deionized water dilution, type 10-30 middle layer, namely of the stable the nanometer crystal titanium dioxide suspension and.

[0008] The step (2) and inorganic alkaline liquid for ammonia water or the sodium hydroxide or a sodium potash liquid.

[0009] Preferably carry out the carrying is: The density of step (1) TiCl4 storing and TiCl3 liquid is 0. 5 mol/L-SHAPED; The step (2) TiCl4 storing and TiCl3 liquid plates (of plates Ti4+: Ti3+ is 4:1); when being the speed of dropping ld/s to the inorganic alkaline solution, - section of the liquid PH value and stopping 1.5, wherein! 95: the constant temperature crystallizes 4 h.

[0010] Compares the existing technology, the invention has the following beneficial effect:

(1). The invention uses the lower lukewarm hot water comprising a method for nanometre preparing titanium dioxide, two hard reunion is avoided the high-temperature calcine y, and a speed and energy consumption to production device according, and uses the inexpensive inorganic titanium salt of the raw material; the method's process is less simple, feasible, is a to the claim device, the raw material is inexpensive; one end of which is low, easy to realize the large industrialization production.

[0011] (2). The invention uses the TiCl4 storing and TiCl3 liquid feeding of the reaction of the opposition dropping method to the spray layers; the reaction production the grain size of nanometer titanium dioxide is less, the photocatalytic capability is stronger, compounds the suspension is stabler, wherein a subside.

[0012] (3). The invention without passes through the nanometer titanium dioxide of the system made of dry, further provided with a wet type preparation suspension, capable of reducing and prevent the reunion directly; the suspension thins, without need to ultrasonic disperse and uniformly, convenient to use.

[0013] (4). To the organic pollutant with good degradation capability is titanium dioxide according we law system made with, so long function to the environment-friendly improved, and used for sewage, waste gas processing and a aspects, further - of applying the coating, textile and a domains made from cleaning material.

[0014]

Carry out the chute specifically

[0015] The invention taking titanium tetrachloride and titanium trichloride and raw material; the dilution dissolved and chemical reaction precipitation, a control PH value, the heating, comprising a filter washing, results in the nanometer titanium dioxide wet type on the system; A taking the synthesis the nanometer titanium dioxide wet type as raw material, by the ration the deionized water; the ultrasonic dispersion, making the stable nanometre titanium dioxide suspension. The specific steps as follows:

(1) Compounds the TiCl4 storing and TiCl3 cooling liquid close to the deionized water o°c, and dry pipette to move to take the ration TiCl4, with a funnel pipe slowly to the ice water tank, and a deionized water of a stirring, obtains the colorless transparent TiCl4 solution, before the winding titanium ion and 0.5-1.0, mol/L (TC preservation spare. The solvent deionized water of the ice water - bath, therefore according to TiCl4 liquid of the preparation method of

4) Is hydrolisis.

[0016] Taking the ration TiCl3, dilutes with the deionized water agent, compounds density 0.5-1.0 mol/L 11 (: 13 Introduced.

[0017] (2) And the nanometre preparing titanium dioxide wet type as the ration the deionized water circulating, the inorganic alkaline liquid (4b ammonia water or sodium or for hydroxide solution) obtains the inorganic is deionized water storing, wherein the situation of mechanical agitation, according to the proportion mixed making the TiCl4 storing and TiCl3 liquid of the step (1) compounds Ti4+: Ti3+=9: 1-1: 5, for drop composed of multiple speed, the adjusting mechanism PH value to 1.0-2.5, stopping adding of, is 50-100!: Constant-temperature comprising 2-10h, obtains the white depositing product; the filtering and function, obtains the nanometer titanium dioxide wet type.

[0018] (3) And the configuration nanometre titanium dioxide suspension of the step (2) and a wet type made by, the ration the deionized water, type 10-30 middle layer, namely of the stable nanometre titanium dioxide suspension. The clutch number of deionized water need for guaranteeing the nanometer titanium dioxide suspension with multiple density, and convenient for use in parallel dilutes according to the requirement; therefore wants the density on thinly clip.

[0019] The experiment are of the nanometer titanium dioxide suspension of the method for preparing obtains with good effect degradation to the organic material.

[0020] Principle of the invention: The alkaline solution, the different valent controlling titanium ion for producing deposition, and liquid value of pH, the heating in water - bath crystallizes, a out of the low temperature is provided with a preparation of high photocatalytic active nanometre titanium dioxide.

[0021] The following and a preparation the implementation carrying to form.

[0022] (1) Compounds the TiCl4 storing and TiCl3 liquid cooling water deionized to 0°C, and dry pipette to move to take AND m1.5 TiCl4 (analytically cleaner, M=189. 68th P, =1. G/ml 726), which a funnel pipe slowly to the ice water tank, and a deionized water of a stirring, obtains the colorless transparent TiCl4 solution, a constant winding to 1000 ml a flasks, making the density is 0. mol/L 5 TiCl4 said that 0°C preservation

[0023]A TiCl3 (analytically cleaner, M=156. 26, =1 P. G/ml 192, w=16_18% 100) is m1.5, the agent dilutes, a constant winding to 250 ml a flasks, making the density is 0. mol/L 5 TiCl3 said that spare.

[0024] (2) For preparing mixed nanometre crystal titanium dioxide wet type claim 100 ml deionized water feeding, 15 ml ammonia water (analytically cleaner, M=35, w=2548%); the situation of mechanical agitation, taking the step (1) preparation TiCl4 liquid 80 ml and TiCl3 liquid 20 ml agent (of plates are Ti4+: Ti3+ is 4:1), for drop of the ld/s speed, when the solution pH value is 1.5; a on electric 4 h of 95 +, obtains the white depositing product; the filter, washing machine is a drop 0 to a filter. the AgNO3 liquid non-sediment production of 1 mol/L, obtains the nanometer titanium dioxide wet type. Obtains a through the XRD detecting the sample anatase titanium dioxide and rutile titanium dioxide content respectively is 60. 4% and 39. 6% ο

[0025] (3) Preparation nanometre titanium dioxide suspension of the step (2) and a wet type, made of multiple water deionized, type middle 20 min, of the stable nanometre titanium dioxide suspension. Obtains the solid content according to GB/T2793-1995 The Adhesive Non-Volatile Content a Built-is 2 to 11%. .

[0026] By detecting carrying: A nanometre titanium dioxide suspension of the upper implementation carrying preparing 10. g 42 and 3 mmol/L Rodin composite introduced are 2. 00 ml, compounds of the catalyst made of whose aperture ratio is 0. 1% Rodin and bright B dye of whose aperture ratio is 0.03 mmol/L suspension liquid 200 (g taking P =1. G/ml 0), taking the liquid with pipette are to 6 inner diameter of 7.5 cm culture dishes each 25 ml layers; the liquid is formed is 1 cm, without by the ultraviolet degradation, wherein culture 5 dishes position is apart from low pressure mercury lamp tube vertical distance 10 cm seat; each other 10 min take out a culture disc, determines the Rodin composite B and ultraviolet spectrophotometer when 553 nm seat extinctions, 50 min the liquid 88. 5% Rodin composite B are degraded. And the whole process, suspension is sleeved at the fixed and is provided with a sediment production. The experiment are of the nanometer titanium dioxide suspension of the invention can preparation degrade the organic material can effectively, and suspension is less stable will not with the sedimentation.

[0027] The upper implementation carrying out of the invention merely for example according to explain the invention is; it to the invention the inhibit movement of implementation chute. Of steel domain's common technical personnel, capable of the channel and a speed change of different sides of the base of the explanation. Here is unable to exhaust to an implementation chute. Everything belonged to the obvious change or a gear according invention's technical solution is expanded kettle the invention) of protecting.