CN104368290A - Method for preparing aqueous solution of titanium tetrachloride, and apparatus thereof - Google Patents
Method for preparing aqueous solution of titanium tetrachloride, and apparatus thereof Download PDFInfo
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- CN104368290A CN104368290A CN201310357522.2A CN201310357522A CN104368290A CN 104368290 A CN104368290 A CN 104368290A CN 201310357522 A CN201310357522 A CN 201310357522A CN 104368290 A CN104368290 A CN 104368290A
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- titanium tetrachloride
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- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 title claims abstract description 96
- 239000007864 aqueous solution Substances 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 81
- 239000008367 deionised water Substances 0.000 claims abstract description 42
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000010521 absorption reaction Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims description 26
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 10
- 238000002242 deionisation method Methods 0.000 claims description 9
- 230000001105 regulatory effect Effects 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 7
- 239000000376 reactant Substances 0.000 claims description 5
- 238000004891 communication Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 230000007062 hydrolysis Effects 0.000 abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 15
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 15
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 15
- 239000007789 gas Substances 0.000 description 13
- 239000000243 solution Substances 0.000 description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 9
- 235000010215 titanium dioxide Nutrition 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 229910003074 TiCl4 Inorganic materials 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- UFNOKFQJIDUZIU-UHFFFAOYSA-J ethene titanium(4+) tetrachloride Chemical group C=C.[Cl-].[Cl-].[Cl-].[Cl-].[Ti+4] UFNOKFQJIDUZIU-UHFFFAOYSA-J 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00099—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor the reactor being immersed in the heat exchange medium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00177—Controlling or regulating processes controlling the pH
Abstract
The invention relates to a method for preparing aqueous solution of titanium tetrachloride, and an apparatus thereof. The apparatus includes a deionized water tank, the deionized water tank is connected with into a reaction kettle through a deionized water pipeline, a titanium tetrachloride tank is connected to the reaction kettle through a blanking pipeline, the deionized water pipeline is provided with a deionized water valve, the blanking pipeline is provided with a blanking valve, a stirrer is arranged in the reaction kettle, the bottom of the reaction kettle is connected to an aqueous solution tank through an aqueous solution pipeline, the aqueous solution pipeline is provided with an aqueous solution pump, the reaction kettle jacket is provided with a jacket, the jacket is provided with a chilled water inlet tube and a chilled water outlet tube, the apparatus also comprises a negative pressure tank, the bottom of the negative pressure tank is connected with the top of the reaction kettle through a circulating tube, a connecting tube with a valve is arranged between the top of the negative pressure tank and the circulating tube, a water absorption tube is arranged between the connecting tube and the top of the reaction kettle, and the connecting tube is provided with a vacuum jet pump. The apparatus for preparing the aqueous solution of titanium tetrachloride has the advantages of stable quality, low hydrolysis rate and high production efficiency.
Description
Technical field
The present invention relates to titanium tetrachloride Liquid-phase hydrolysis and produce high purity titanium white powder and Nano titanium dioxide technical field, more specifically, relate to a kind of compound method of efficient, pollution-free, low energy consumption titanium tetrachloride aqueous solution, and the required device of preparation and retracting device.
Background technology
At present, high purity titanium white powder and nano grade titanium white powder have extensive use in the fields such as electronic component, coating, automotive paints, photocatalyst, cosmetics, and production process is all mainly adopt titanium tetrachloride Liquid-phase hydrolysis explained hereafter.And important step is exactly the preparation of titanium tetrachloride aqueous solution in production process, titanium tetrachloride and water react conversion process: the carboxylic chloride → carboxyl complex compound → multinuclear carboxyl complex compound → metatitanic acid ion → hydrated titanium dioxide of titanium tetrachloride → titanium, the factor wherein affecting reaction is mainly reaction temperature and reactant liquor acidity.Prove that the pH value of solution to aqueous solution quality influence is by production practices: during PH 1.26-1.99, solution is yellow, clear; During PH 1.99-2.87, solution is pale yellow transparent, clarification; Slight white opacity during PH 2.88-4.21.Temperature is greater than 35 DEG C and starts to occur a small amount of precipitation, is less than 10 DEG C of solution and becomes sticky thick.The titanium tetrachloride aqueous solution concentration of described titanium tetrachloride aqueous solution preparation method gained counts 35%-50% with TiCl4, in titanium tetrachloride aqueous solution, if this concentration is less than 35% in TiCl4 wherein, then in titanium tetrachloride aqueous solution, slowly can separate out precipitation; If concentration is greater than 50% also may occur floccule.This process for preparation is particularly important, badly can produce white or pale yellow precipitate, directly will affect the granularity, specific area etc. of titanium dioxide if control.Titanium tetrachloride has intense hydrolysis tendency and meets water and kickback can occur release large calorimetric, and evaporates with a large amount of titanium tetrachloride and HCl gas, and environment, equipment are caused to corrosion and pollutes.Existing most of producer compound method all has difference, and main method adopts deionized water and refined titanic chloride to react, and adopts ice cube or graphite cooler cooling, controls temperature of reaction system≤30 DEG C.What hydrolytic process adopted is manually regulate and control charging rate and system temperature, and precision is low can not well control whole course of reaction.The gas simultaneously volatilized during preparation adopts water or alkali lye spray-absorption, neutralizes discharge later up to standard.Ye You producer reduces to reduce the wastage the titanium tetrachloride gases that negative pressure is taken away in reactor, does not adopt tail gas absorber and directly that Volatile Gas is emptying.But the method causes severe contamination to environment, also serious harm health simultaneously.
Summary of the invention
The object of the invention is to overcome preparation method and the device that above-mentioned deficiency provides a kind of titanium tetrachloride aqueous solution, this preparation method can obtain steady quality, percent hydrolysis is low, production efficiency is high, titanium tetrachloride utilization rate is high and free from environmental pollution, and this device can realize that automation is reinforced in addition, regulating and controlling temperature and feeding quantity.
For achieving the above object, the present invention is by the following technical solutions:
A kind of device preparing titanium tetrachloride aqueous solution, comprise aqueous solution storage tank, de-ionized water tank, titanium tetrachloride groove and reactor, de-ionized water tank passes through deionized water pipeline communication in reactor, titanium tetrachloride groove is communicated in reactor by blanking pipe, ionized water pipeline is provided with deionization water valve, blanking pipe is provided with baiting valve, agitator is provided with in reactor, be communicated on aqueous solution storage tank by aqueous solution pipeline bottom reactor, aqueous solution pipeline is provided with water-soluble liquid pump, chuck is arranged with outside reactor, chuck is provided with chilled water water inlet pipe and chilled water outlet pipe, also be provided with negative-pressure cup, negative-pressure cup is outside equipped with chuck, chuck is provided with chilled water water inlet pipe and chilled water outlet pipe, the bottom of negative-pressure cup is communicated with reactor top by circulation pipe, circulation pipe is provided with circulating valve and circulating pump, communicating pipe is provided with between negative-pressure cup top and circulation pipe, communicating pipe is provided with valve, communicating pipe between valve and negative-pressure cup and be also provided with absorption tube between reactor top, communicating pipe is provided with vacuum jet pump with absorption tube attaching parts, negative-pressure cup is also provided with deionized water water inlet pipe.
The above-mentioned device preparing titanium tetrachloride aqueous solution, also comprise control unit, deionization water valve is magnetic valve, deionized water pipeline is also provided with water speed sensor, deionization water valve, water speed sensor is all connected with control unit with agitator, baiting valve is magnetic valve, blanking pipe is also provided with blanking velocity sensor, baiting valve is all connected with control unit with blanking velocity sensor, be provided with temperature sensor in a kettle., pH sensor and concentration sensor, also temperature sensor is provided with in negative-pressure cup, pH sensor and concentration sensor, all temperature sensors, pH sensor is all connected with control unit with concentration sensor, circulating valve on circulation pipe and the valve on communicating pipe are all magnetic valves, circulating valve and valve are all electrically connected with control unit.
The above-mentioned device preparing titanium tetrachloride aqueous solution, chilled water water inlet pipe and the chilled water outlet pipe of reactor and negative-pressure cup are provided with the temperature sensor be connected with control unit.
Above-mentioned utilization prepares the device of titanium tetrachloride aqueous solution to prepare the method for titanium tetrachloride aqueous solution, comprises the following steps:
A. react in a kettle. with the titanium tetrachloride in the deionized water in de-ionized water tank and titanium tetrachloride groove;
B. the TiCl volatilized in course of reaction
4enter in negative-pressure cup after being reclaimed by absorption tube with HCl gas and form absorbing liquid;
C. control the mass percentage of HCl in absorbing liquid below 20%, absorbing liquid is squeezed into reactor by circulating pump again and is regulated pH value in reactor, and the pH value in reactor controls below 2.87;
D. the temperature of reactor is cooled by the chilled water in chuck, and the temperature in reactor controls below 30 DEG C;
E. prepare titanium tetrachloride aqueous solution, wherein the mass percentage of titanium tetrachloride is 30%-50%.
Above-mentioned utilization prepares the device of titanium tetrachloride aqueous solution to prepare the method for titanium tetrachloride aqueous solution, utilize the pH sensor in reactor and negative-pressure cup and temperature sensor that the pH value in reactor and temperature information are fed back to control unit, control unit controls the magnetic valve on deionized water pipeline and the magnetic valve on blanking pipe, regulate the inlet amount and the amount of deionized water that add titanium tetrachloride, regulate mixing speed simultaneously, on the other hand by regulating the magnetic valve on circulation pipe, what regulate absorbing liquid adds speed and addition, thus the pH value in control reactor, what control unit controlled chilled water adds speed and addition to control the temperature of reactant liquor and absorbing liquid in reactor and negative-pressure cup.
Adopt technique scheme, the present invention has following advantage: the present invention is effective, by regulating the pH value of deionized water in advance, issuable white or pale yellow precipitate in titanium tetrachloride aqueous solution process for preparation can directly be dissolved, reclaim HCl, TiCl4 gas evaporated in process for preparation as pH value regulator solution, resource is able to Appropriate application, and titanium tetrachloride utilization rate is up to more than 99% simultaneously, improve environment simultaneously, and achieve automated production.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Detailed description of the invention
A kind of device preparing titanium tetrachloride aqueous solution as shown in Figure 1, comprise aqueous solution storage tank 11, de-ionized water tank 5, titanium tetrachloride groove 6 and reactor 1, de-ionized water tank passes through deionized water pipeline communication in reactor, titanium tetrachloride groove 6 is communicated in reactor by blanking pipe, ionized water pipeline is provided with deionization water valve 18, blanking pipe is provided with baiting valve 7, agitator 10 is provided with in reactor 1, be communicated on aqueous solution storage tank 11 by aqueous solution pipeline bottom reactor, aqueous solution pipeline is provided with water-soluble liquid pump 12, chuck 9 is arranged with outside reactor, chuck 9 is provided with chilled water water inlet pipe 14 and chilled water outlet pipe 15, also be provided with negative-pressure cup 2, agitator is provided with in negative-pressure cup, negative-pressure cup is outside equipped with chuck, chuck is provided with chilled water water inlet pipe and chilled water outlet pipe, the bottom of negative-pressure cup 2 is communicated with reactor top by circulation pipe 23, circulation pipe 23 is provided with circulating valve 16 and circulating pump 13, communicating pipe 25 is provided with between negative-pressure cup top and circulation pipe, be provided with valve 17 communicating pipe 25, communicating pipe between valve and negative-pressure cup and be also provided with absorption tube 24 between reactor top, communicating pipe 25 is provided with vacuum jet pump 3 with absorption tube 24 attaching parts, negative-pressure cup 2 is also provided with deionized water water inlet pipe.The present invention also comprises control unit 4, deionization water valve 18 is magnetic valves, deionized water pipeline is also provided with water speed sensor 19, deionization water valve, water speed sensor is all connected with control unit with agitator, baiting valve 7 is magnetic valves, blanking pipe is also provided with blanking velocity sensor 20, baiting valve is all connected with control unit with blanking velocity sensor, be provided with temperature sensor 8 in a kettle., pH sensor 21 and concentration sensor 22, also temperature sensor is provided with in negative-pressure cup, pH sensor and concentration sensor, all temperature sensors, pH sensor is all connected with control unit with concentration sensor, circulating valve 16 on circulation pipe and the valve on communicating pipe 17 are all magnetic valves, circulating valve 16 and valve 17 are all electrically connected with control unit.Chilled water water inlet pipe and the chilled water outlet pipe of reactor and negative-pressure cup are provided with the temperature sensor be connected with control unit.
Titanium tetrachloride preparation method embodiment 1 of the present invention: comprise the following steps:
A. react in a kettle. with the titanium tetrachloride in the deionized water in de-ionized water tank and titanium tetrachloride groove;
B. the TiCl volatilized in course of reaction
4enter in negative-pressure cup after being reclaimed by absorption tube with HCl gas and form absorbing liquid;
C. the mass percentage of HCl in absorbing liquid is controlled below 20%, absorbing liquid is squeezed into reactor by circulating pump again and is regulated pH value in reactor, pH value in reactor controls below 2.87, this process can be carried out continuously, regulate baiting valve opening degree and deionized water addition simultaneously, keep material turnover balance;
D. the temperature of reactor is cooled by the chilled water in chuck, and the temperature in reactor controls below 30 DEG C;
E. prepare titanium tetrachloride aqueous solution, wherein the mass percentage of titanium tetrachloride is 30%-50%.
The present invention is also provided with control unit, utilize the pH sensor in reactor and negative-pressure cup and temperature sensor that the pH value in reactor and temperature information are fed back to control unit, control unit controls the magnetic valve on deionized water pipeline and the magnetic valve on blanking pipe, regulate the inlet amount and the amount of deionized water that add titanium tetrachloride, regulate mixing speed simultaneously, on the other hand by regulating the magnetic valve on circulation pipe, what regulate absorbing liquid adds speed and addition, thus the pH value in control reactor, what control unit controlled chilled water adds speed and addition to control the temperature of reactant liquor and absorbing liquid in reactor and negative-pressure cup.
In the present invention, by the running of vacuum jet pump, circulating pump, the titanium tetrachloride evaporated in titanium tetrachloride aqueous solution process for preparation, hydrogen chloride gas are absorbed, then absorbing liquid is proceeded in reactor regulates its pH value, make the utilization rate of titanium tetrachloride reach more than 99%.Titanium tetrachloride groove 6, aqueous solution storage tank 11, reactor 1 are all connected to vacuum jet pump side, by the work of vacuum jet pump, make all aobvious negative pressure in each position, thus can prevent TiCl4, HCl gaseous volatilization in process for preparation and to environment.
Chilled water pipeline is arranged around reactor 1 and negative-pressure cup 2 in the present invention, described temperature sensor measurement reactor 1, chilled water water inlet pipe 14, chilled water outlet pipe 15, negative-pressure cup 2 temperature, described magnetic valve regulates the charging rate of titanium tetrachloride and the opening degree of absorbing liquid circulating valve 16, the solution acidity in described acidity test instrument test reaction still 1 and negative-pressure cup 2.Control unit of the present invention is not limited thereto, but automatically can regulate the addition of titanium tetrachloride and Ethylene recov according to the material acidity in reactor 1, variations in temperature feedback information, arrives the device that reaction end also has feedback.
Preparation method's embodiment 2 of the present invention: comprise the following steps: by deionized water and titanium tetrachloride reaction, regulate the acidity of deionized water with the titanium tetrachloride volatilized, absorbing hydrogen chloride gas liquid simultaneously, control PH≤2.87, reaction temperature chilled water controls not higher than 30 DEG C, utilization measures pH from pH sensor and temperature sensor and temperature gives feedback, after obtaining feedback information, control unit controls to adjust charging rate and turns liquid measure.In the process that titanium tetrachloride and water react, temperature strictly controls, and the temperature stabilization of reaction system controls not higher than 30 DEG C.Acidity PH≤2.87 Yin Wendu can be suppressed to raise or acidity low and make to produce white or pale yellow precipitate and affect the effect preparing titanium dioxide in reaction system.
Preparation method's embodiment 3 of the present invention: in titanium tetrachloride Ethylene recov, hydrogen chloride mass percentage is lower than 20%, in absorption process, continuity joins in reactant liquor, in negative-pressure cup, supplement deionized water simultaneously, mend amount of deionized water=preparation titanium tetrachloride institute water requirement, titanium tetrachloride and hydrogen chloride gas utilization rate in process for preparation can be made like this to increase, and the gas of more than 99% is recycled utilization.
Preparation method's embodiment 4 of the present invention: use the device preparing titanium tetrachloride aqueous solution as shown in Figure 1, the titanium tetrachloride mass percent concentration in titanium tetrachloride groove is with wherein TiCl
4the titanium tetrachloride aqueous solution counting 30% enters reactor, appropriate amount of deionized water is added again in reactor, the absorbing liquid of hydrogen chloride content 20% is used to carry out pH value adjustment, in mixed process, reaction temperature is controlled to be in 30 DEG C, control charging rate and solution pH value by control unit, the concentration obtained subsequently is with wherein TiCl
4count the titanium tetrachloride aqueous solution of 33%, after testing, not containing solid formation in this titanium tetrachloride aqueous solution, outward appearance light yellow transparent liquid, reclaims TiCl
4about 3%.
Preparation method's embodiment 5 of the present invention: use the device preparing titanium tetrachloride aqueous solution as shown in Figure 1, the titanium tetrachloride mass percent concentration in titanium tetrachloride groove is with wherein TiCl
4the titanium tetrachloride aqueous solution counting 35% enters reactor, appropriate deionized water is added again in reactor, then adjustment pH=2.5 is carried out with the absorbing liquid that hydrogen chloride content is 15%, in mixed process, temperature of reaction system is controlled to be in 20 DEG C, by automatic control system charging rate and solution pH value.Subsequently, concentration is obtained with wherein TiCl
4count the titanium tetrachloride aqueous solution of 37%, after testing, not containing solid formation in this titanium tetrachloride aqueous solution, outward appearance light yellow transparent liquid, reclaims TiCl
4about 2%, there is very considerable economic worth.
Preparation method's embodiment 6 of the present invention: use the device preparing titanium tetrachloride aqueous solution as shown in Figure 1, the titanium tetrachloride mass percent concentration in titanium tetrachloride groove is with wherein TiCl
4the titanium tetrachloride aqueous solution counting 45% enters reactor, appropriate deionized water is added again in reactor, then the Ethylene recov of hydrogen chloride content 20% is used to carry out adjustment pH=2.87, within reaction temperature being controlled to be 15 DEG C in mixed process, by automatic controlling system charging rate and solution ph, obtain mass concentration subsequently with wherein TiCl
4count the titanium tetrachloride aqueous solution of 48.5%.After testing, this TiCl
4not containing solid formation in the aqueous solution, outward appearance pale yellow transparent, reclaims TiCl
4about 4.5%, there is very considerable economic worth.
In sum, the present invention prepares the method for titanium tetrachloride aqueous solution and device can make preparation process automatically control and continuously, simultaneously environmentally safe again, has accomplished cleaner production, obtained titanium tetrachloride aqueous solution steady quality deposit-free, the TiCl simultaneously will volatilized in process for preparation
4reclaimed with HCl gas, the rate of recovery is up to more than 99%.In preparation titanium tetrachloride aqueous solution process traditional at present, TiCl
4loss about 3%-5%, compared with the method for preparation titanium tetrachloride aqueous solution traditional at present, has very considerable economic worth.
Claims (5)
1. prepare the device of titanium tetrachloride aqueous solution for one kind, comprise aqueous solution storage tank (11), de-ionized water tank (5), titanium tetrachloride groove (6) and reactor (1), de-ionized water tank passes through deionized water pipeline communication in reactor, titanium tetrachloride groove (6) is communicated in reactor by blanking pipe, ionized water pipeline is provided with deionization water valve (18), blanking pipe is provided with baiting valve (7), agitator (10) is provided with in reactor (1), be communicated on aqueous solution storage tank (11) by aqueous solution pipeline bottom reactor, aqueous solution pipeline is provided with water-soluble liquid pump (12), it is characterized in that: outside reactor, be arranged with chuck (9), chuck (9) is provided with chilled water water inlet pipe (14) and chilled water outlet pipe (15), also be provided with negative-pressure cup (2), negative-pressure cup is outside equipped with chuck, chuck is provided with chilled water water inlet pipe and chilled water outlet pipe, the bottom of negative-pressure cup (2) is communicated with reactor top by circulation pipe (23), circulation pipe (23) is provided with circulating valve (16) and circulating pump (13), communicating pipe (25) is provided with between negative-pressure cup top and circulation pipe, be provided with valve (17) communicating pipe (25), communicating pipe between valve and negative-pressure cup and be also provided with absorption tube (24) between reactor top, in communicating pipe (25), upper and absorption tube (24) attaching parts are provided with vacuum jet pump (3), negative-pressure cup (2) is also provided with deionized water water inlet pipe.
2. the device preparing titanium tetrachloride aqueous solution according to claim 1, it is characterized in that: also comprise control unit (4), deionization water valve (18) is magnetic valve, deionized water pipeline is also provided with water speed sensor (19), deionization water valve, water speed sensor is all connected with control unit with agitator, baiting valve (7) is magnetic valve, blanking pipe is also provided with blanking velocity sensor (20), baiting valve is all connected with control unit with blanking velocity sensor, be provided with temperature sensor (8) in a kettle., pH sensor (21) and concentration sensor (22), also temperature sensor is provided with in negative-pressure cup, pH sensor and concentration sensor, all temperature sensors, pH sensor is all connected with control unit with concentration sensor, circulating valve (16) on circulation pipe and the valve on communicating pipe (17) are all magnetic valves, circulating valve (16) and valve (17) are all electrically connected with control unit.
3. the device preparing titanium tetrachloride aqueous solution according to claim 1 and 2, is characterized in that: on chilled water water inlet pipe and the chilled water outlet pipe of reactor and negative-pressure cup, be provided with the temperature sensor be connected with control unit.
4. utilize the device preparing titanium tetrachloride aqueous solution described in claim 1 to prepare a method for titanium tetrachloride aqueous solution, comprise the following steps:
A. react in a kettle. with the titanium tetrachloride in the deionized water in de-ionized water tank and titanium tetrachloride groove;
B. the TiCl volatilized in course of reaction
4enter in negative-pressure cup after being reclaimed by absorption tube with HCl gas and form absorbing liquid;
C. control the mass percentage of HCl in absorbing liquid below 20%, absorbing liquid is squeezed into reactor by circulating pump again and is regulated pH value in reactor, and the pH value in reactor controls below 2.87;
D. the temperature of reactor is cooled by the chilled water in chuck, and the temperature in reactor controls below 30 DEG C;
E. prepare titanium tetrachloride aqueous solution, wherein the mass percentage of titanium tetrachloride is 30%-50%.
5. utilize the device preparing titanium tetrachloride aqueous solution to prepare the method for titanium tetrachloride aqueous solution according to claim 4, it is characterized in that: utilize the pH sensor in reactor and negative-pressure cup and temperature sensor that the pH value in reactor and temperature information are fed back to control unit, control unit controls the magnetic valve on deionized water pipeline and the magnetic valve on blanking pipe, regulate the inlet amount and the amount of deionized water that add titanium tetrachloride, regulate mixing speed simultaneously, on the other hand by regulating the magnetic valve on circulation pipe, what regulate absorbing liquid adds speed and addition, thus the pH value in control reactor, what control unit controlled chilled water adds speed and addition to control the temperature of reactant liquor and absorbing liquid in reactor and negative-pressure cup.
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| CN107469753A (en) * | 2017-09-25 | 2017-12-15 | 河南师范大学 | A kind of new chemical experimental robot |
| CN108183141A (en) * | 2017-12-28 | 2018-06-19 | 成都中建材光电材料有限公司 | A kind of cadmium telluride thin-film battery of new structure and preparation method thereof |
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| CN108854617A (en) * | 2018-06-06 | 2018-11-23 | 杭州弗沃德精细化工有限公司 | A kind of titanium tetrachloride aqueous solution device for formulating and method |
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| CN107469753A (en) * | 2017-09-25 | 2017-12-15 | 河南师范大学 | A kind of new chemical experimental robot |
| CN108183141A (en) * | 2017-12-28 | 2018-06-19 | 成都中建材光电材料有限公司 | A kind of cadmium telluride thin-film battery of new structure and preparation method thereof |
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| CN108854617B (en) * | 2018-06-06 | 2020-09-15 | 杭州弗沃德精细化工有限公司 | Titanium tetrachloride aqueous solution preparation device and method |
| CN108795105A (en) * | 2018-07-18 | 2018-11-13 | 黄山幻彩颜料科技有限公司 | A kind of stable quality, efficiently, the hydrolysis process of the production pearlescent pigment of environmental protection |
| CN109111340A (en) * | 2018-10-26 | 2019-01-01 | 浙江众成包装材料股份有限公司 | Serialization prepares the high pressure reaction assembly of 1- (1- bromoethyl) -4- chloromethylbenzene |
| CN109364787A (en) * | 2018-11-19 | 2019-02-22 | 云南昆船环保技术有限公司 | A kind of alcohol concentration auto-scheduling system and its concocting method |
| CN111253795A (en) * | 2020-01-17 | 2020-06-09 | 营口盼盼硅藻材料集团有限公司 | Production process and device of purifying material |
| CN113731329A (en) * | 2021-08-31 | 2021-12-03 | 沈阳工程学院 | Titanium tetrachloride aqueous solution preparation device |
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