CN105152210A - Substitution reaction method of titanium dioxide - Google Patents
Substitution reaction method of titanium dioxide Download PDFInfo
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- CN105152210A CN105152210A CN201510694978.7A CN201510694978A CN105152210A CN 105152210 A CN105152210 A CN 105152210A CN 201510694978 A CN201510694978 A CN 201510694978A CN 105152210 A CN105152210 A CN 105152210A
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- Prior art keywords
- titanium dioxide
- titanium
- hydrolysis
- substitution reaction
- water
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 136
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 64
- 238000006467 substitution reaction Methods 0.000 title claims abstract description 23
- RTAQQCXQSZGOHL-UHFFFAOYSA-N titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 39
- 239000010936 titanium Substances 0.000 claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 35
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 238000004061 bleaching Methods 0.000 claims abstract description 7
- 238000009835 boiling Methods 0.000 claims abstract description 4
- 239000000413 hydrolysate Substances 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 8
- 241000218218 Ficus <angiosperm> Species 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 24
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 238000004458 analytical method Methods 0.000 abstract description 4
- LLZRNZOLAXHGLL-UHFFFAOYSA-J Titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 239000011780 sodium chloride Substances 0.000 abstract 1
- 235000010215 titanium dioxide Nutrition 0.000 description 60
- 238000000034 method Methods 0.000 description 14
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J Titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- -1 and meanwhile Substances 0.000 description 1
- 238000005039 chemical industry Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001475 halogen functional group Chemical group 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 230000003287 optical Effects 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
Abstract
The invention discloses a substitution reaction method of titanium dioxide. The method includes the steps that 1, metered titanium liquid is preheated to above 60 DEG C in a semi-closed preheating pot for use; 2, metered water is preheated to above 60 DEG C in a water preheating pot for use; 3, the water preheated in the step2 is added into a semi-closed hydrolysis pot, then the titanium liquid preheated in the step1 is added into the semi-closed hydrolysis pot, the mixture is heated to above 90 DEG C within 40 min but kept below the boiling point, heat preservation is performed for 1-4 h, the temperature is lowered to 70 DEG C, and a hydrolysis product is obtained after hydrolysis is finished, wherein the volume ratio of the titanium liquid to the water is 3-6:1; 4, analysis is performed after the hydrolysis product obtained in the step3 is subjected to washing, bleaching, secondary washing, salt treatment and calcination. By means of the method, the size of particles (titanic acid or tetrabutyl titanate) is effectively controlled, and manufacturing of high-quality titanium dioxide is facilitated; under the micro-negative pressure technological condition, escaping of hydrochloric acid is prevented, and recycling of hydrochloric acid is facilitated.
Description
Technical field
The invention belongs to titanium dioxide technical field, especially relate to a kind of substitution reaction method of titanium dioxide.
Background technology
At present, the production of whole world titanium dioxide all adopts sulfuric acid process or chlorination process.Sulfate process titanium dioxide manufacture adopts sulfuric acid solution titanium ore or titanium slag, produces titanium liquid (titanyl sulfate), then through series of process process, produce titanium dioxide; Titanium Dioxide Produced by Chloride Procedure manufacture utilizes chlorine to produce titanium tetrachloride, then through series of process process, produce titanium dioxide; The manufacture of hydrochloric acid method titanium dioxide is through the exploration of decades, also do not have industrialization at present, major cause is: A, technique are immature, and the substitution reaction of titanium liquid (is called hydrolysis in titanium dioxide industry, hereinafter referred to as substitution reaction for being hydrolyzed) poor quality, cannot produce coating level titanium white; The recycling of B, hydrochloric acid is not thorough, not environmentally; C, impurity removal process imperfection.
In the production process of titanium dioxide, have to pass through the techniques such as acidolysis, removal of impurities, hydrolysis, calcining, and hydrolysis process is a step of most critical in titanium dioxide technical process, it directly determines the size (in theory, the best particle of titanium dioxide is the half-wavelength of visible light wave) of titanium dioxide particle.In the production of titanium dioxide, the purity of titanium dioxide and the association of attribute degree of titanium dioxide are large, but do not determine the quality of titanium dioxide, and real what determine titanium dioxide quality is the size of titanium dioxide particle.The optical property of titanium dioxide is determined by its particle dia, and in theory, when particle dia reaches the half-wavelength of visible ray, the reflection of titanium dioxide to light reaches optimum value.In fact, particle is excessive, and reflection reduces, titanium dioxide reflect red BELAND light intensity, the partially red phase of titanium dioxide; Particle is too small, and reflection reduces, and titanium dioxide reflect blue is stronger than ruddiness, the partially blue phase of titanium dioxide, and meanwhile, particle is too small, light generation diffraction, and the covering performance of titanium dioxide declines fast.Therefore, the particle of titanium dioxide should be slightly more longer than the half-wavelength of visible ray, and the wavelength of visible ray is 350-700 nanometer, and particle dia the best of rutile titanium white powder is 300 ran.
Although some achievements in research of relevant hydrochloric acid method titanium white are own through occurring, do not reach industrial requirement all the time.What disclosed in Sichuan University, patent CN102602991A adopted is the hydrolysis of micro emulsion method, and organic phase and hydrolysate are difficult to be separated, and cannot realize industrialization.Patent CN1217298 disclosed in the Hua Changji development corporation, Ltd. of Guangzhou adopts mixing water solution, cannot removal of impurities, cannot the titanium dioxide of production high-quality.Yibin Tianyuan Group Co., Ltd's disclosed " hydrochloric acid method titanium white production technique " (" chemical industry for making chlorine and alkali ", 2014,50 (4): 36-39) adopt spraying hydrolysis, the spraying hydrolysis of one ton of titanium dioxide needs consumption 23 tons of steam, and energy consumption is too high.Patent CN1766137A disclosed in Chen Zean adopts and adds polymer substance hydrolysis, and hydrolysate washing difficulty, and the particle dia 5 μm of product titanium dioxide, much larger than the particle dia (about 0.3 μm) that coating titanium dioxide requires.Chengdu Chemical Pharmaceutical Factory once produced non-coating titanium dioxide by hydrochloric acid method, but the production of hydrochloric acid method coating level titanium dioxide does not also realize industrialization at present.
Summary of the invention
For above-mentioned technical problem, the object of the present invention is to provide a kind of substitution reaction method of titanium dioxide, with production high-quality coating titanium dioxide, be beneficial to the suitability for industrialized production of hydrochloric acid method titanium dioxide, be beneficial to the recycling of hydrochloric acid.
The technical solution used in the present invention is:
A substitution reaction method for titanium dioxide, comprises the following steps:
(1) in the foreheater of semi closed, by the titanium liquid measured, described titanium liquid is greater than 80 grams per liters containing titanium dioxide, and free acid is greater than 100 grams per liters, is preheating to more than 60 DEG C, for subsequent use;
(2) in water preheat pot, by the water preheat that measures to more than 60 DEG C, for subsequent use;
(3) in the hydrolyzer of semi closed, first add water preheated in step (2), then, add titanium liquid preheated in step (1) within 20 minutes, the volume ratio of titanium liquid and water is 3-6:1; Be heated to more than 90 DEG C, below boiling point in 40 minutes, insulation 1-4 hour, reduces the temperature to 70 DEG C, and hydrolysis replaces end, obtains hydrolysate;
(4) in step (3), hydrolysate, after washing, bleaching, secondary washing, Ficus caricaL, calcination, is analyzed.
The substitution reaction method of titanium dioxide of the present invention, wherein, described titanium liquid is 80-170 grams per liter containing titanium dioxide, and free acid is 100-200 grams per liter.
The substitution reaction method of titanium dioxide of the present invention, wherein, in step (3), the joining day of titanium liquid is 10-15 minute.
The substitution reaction method of titanium dioxide of the present invention, wherein, in step (1), the preheating temperature of titanium liquid and the middle water of step (2) is 60-100 DEG C.
The substitution reaction method of titanium dioxide of the present invention, wherein, the HCL that in step (1), the preheating of titanium liquid and the middle hydrolysis of step (3) produce or hydrochloric acid enter retrieving arrangement.
The substitution reaction method of titanium dioxide of the present invention, mainly utilize titanium liquid oneself to produce crystal seed under certain condition, then, utilize this automatic growing crystal species to induce titanium liquid to be hydrolyzed, under the condition ensureing some amount crystal seed, utilize the quantity of crystal seed to control the particle dia of titanium hydrolysis.Number of seeds Halo is more, and hydrolysis particle is thinner; Crystal seed quantity is fewer, and hydrolysis particle is larger.And the particle of titanium dioxide must control within the specific limits (about 0.3 μm), therefore, the quantity of crystal seed must be controlled within the specific limits, and crystal seed quantity will be controlled, the condition that crystal seed of must controlling well produces.
Beneficial effect of the present invention:
The substitution reaction method of titanium dioxide of the present invention, tiny structure reaction in semi closed hydrolyzer and foreheater, the processing condition of tiny structure, prevent escaping of hydrochloric acid, are conducive to the recovery of hydrochloric acid; By controlled hydrolysis condition, thus the size of controlled hydrolysis particle (metatitanic acid or positive metatitanic acid) effectively; By acid hydrolysate after washing, bleaching, secondary washing, Ficus caricaL and calcining, coating type rutile titanium white powder can be produced; This hydrolysis is reacted below boiling point, and energy consumption is low, thus is conducive to the manufacture of high quality titanium white powder.
The substitution reaction method of titanium dioxide of the present invention, the HCL that in step (1), the preheating of titanium liquid and the middle hydrolysis of step (3) produce or hydrochloric acid enter retrieving arrangement, efficiently solve the recovery problem of hydrochloric acid.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment
Embodiment 1
A substitution reaction method for titanium dioxide, comprises the following steps:
(1) in the semi closed foreheater of 50 liters, add 30 liters of titanium liquid, described titanium liquid contains titanium dioxide 85.2 grams per liter, titanous 0.5 grams per liter, and free acid 102.7 grams per liter, is preheating to 70 DEG C, obtains preheated titanium liquid, for subsequent use; HCL or the HCL solution escaped during heating sends into retrieving arrangement;
(2) in the water preheat pot of 50 liters, add 8 premium on currency, be preheating to 70 DEG C, obtain preheated water, for subsequent use;
(3) in the hydrolyzer of semi closed, first add water preheated in step (2), then in 15 minutes, add titanium liquid preheated in step (1); Within 30 minutes, be heated to 103 DEG C, be incubated 1 hour; During hydrolysis, HCL or the HCL solution that hydrolysis produces constantly is sent into retrieving arrangement by pipeline; Be cooled to 70 DEG C, hydrolysis terminates, and obtains hydrolysate;
(4) in step (3), hydrolysate, after washing, bleaching, secondary washing, Ficus caricaL, calcination, is analyzed.
Hydrolysis particle analytical results: D502.53 μm; Calcining particle analysis: D500.34 μm.
Embodiment 2
A substitution reaction method for titanium dioxide, comprises the following steps:
(1) in the semi closed foreheater of 50 liters, add 30 liters of titanium liquid, described titanium liquid contains titanium dioxide 165.2 grams per liter, titanous 0.6 grams per liter, and free acid 160.7 grams per liter, is preheating to 88 DEG C, obtains preheated titanium liquid, for subsequent use; HCL or the HCL solution escaped during heating sends into retrieving arrangement;
(2) in the water preheat pot of 50 liters, add 10 premium on currency, be preheating to 85 DEG C, obtain preheated water, for subsequent use;
(3) in the hydrolyzer of semi closed, first add water preheated in step (2), then in 12 minutes, add titanium liquid preheated in step (1); Within 30 minutes, be heated to 101 DEG C, be incubated 70 minutes; During hydrolysis, HCL or the HCL solution that hydrolysis produces constantly is sent into retrieving arrangement by pipeline; Be cooled to 70 DEG C, hydrolysis terminates, and obtains hydrolysate;
(4) in step (3), hydrolysate, after washing, bleaching, secondary washing, Ficus caricaL, calcination, is analyzed.
Hydrolysis particle analytical results: D502.09 μm; Calcining particle analysis: D500.33 μm.
Embodiment 3
A substitution reaction method for titanium dioxide, comprises the following steps:
(1) in the semi closed foreheater of 50 liters, add 30 liters of titanium liquid, described titanium liquid contains titanium dioxide 145.5 grams per liter, titanous 0.5 grams per liter, and free acid 151.7 grams per liter, is preheating to 88 DEG C, obtains preheated titanium liquid, for subsequent use; HCL or the HCL solution escaped during heating sends into retrieving arrangement;
(2) in the water preheat pot of 50 liters, add 10 premium on currency, be heated to 85 DEG C, obtain preheated water, for subsequent use;
(3) in the hydrolyzer of semi closed, first add water preheated in step (2), then in 15 minutes, add titanium liquid preheated in step (1); Within 30 minutes, be heated to 97 DEG C, be incubated 4 hours; During hydrolysis, HCL or the HCL solution that hydrolysis produces constantly is sent into retrieving arrangement by pipeline; Be cooled to 70 DEG C, hydrolysis terminates, and obtains hydrolysate;
(4) in step (3), hydrolysate, after washing, bleaching, secondary washing, Ficus caricaL, calcination, is analyzed.
Hydrolysis particle analytical results: D502.69 μm; Calcining particle analysis: D500.41 μm.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (5)
1. a substitution reaction method for titanium dioxide, is characterized in that: comprise the following steps:
(1) in the foreheater of semi closed, by the titanium liquid measured, described titanium liquid is greater than 80 grams per liters containing titanium dioxide, and free acid is greater than 100 grams per liters, is preheating to more than 60 DEG C, for subsequent use;
(2) in water preheat pot, by the water preheat that measures to more than 60 DEG C, for subsequent use;
(3) in the hydrolyzer of semi closed, first add water preheated in step (2), then, add titanium liquid preheated in step (1) within 20 minutes, the volume ratio of titanium liquid and water is 3-6:1; Be heated to more than 90 DEG C, below boiling point in 40 minutes, insulation 1-4 hour, reduces the temperature to 70 DEG C, and hydrolysis terminates, and obtains hydrolysate;
(4) in step (3), hydrolysate, after washing, bleaching, secondary washing, Ficus caricaL, calcination, is analyzed.
2. the substitution reaction method of Ju titanium dioxide according to claim 1, is characterized in that: described titanium liquid is 80-170 grams per liter containing titanium dioxide, and free acid is 100-200 grams per liter.
3. the substitution reaction method of Ju titanium dioxide according to claim 1, is characterized in that: in step (3), the joining day of titanium liquid is 10-15 minute.
4. the substitution reaction method of Ju titanium dioxide according to claim 1, is characterized in that: in step (1), the preheating temperature of titanium liquid and the middle water of step (2) is 60-100 DEG C.
5. the substitution reaction method of the titanium dioxide piece described in Ju claim 1-4 any one, is characterized in that: the HCL that in step (1), in the preheating of titanium liquid and step (3), hydrolysis produces or hydrochloric acid enter retrieving arrangement.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510694978.7A CN105152210A (en) | 2015-10-23 | 2015-10-23 | Substitution reaction method of titanium dioxide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510694978.7A CN105152210A (en) | 2015-10-23 | 2015-10-23 | Substitution reaction method of titanium dioxide |
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| CN105152210A true CN105152210A (en) | 2015-12-16 |
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| CN201510694978.7A Pending CN105152210A (en) | 2015-10-23 | 2015-10-23 | Substitution reaction method of titanium dioxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112694123A (en) * | 2020-12-30 | 2021-04-23 | 福州钛发科技有限公司 | Preparation method of titanium dioxide for delustering dacron chemical fiber |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62278125A (en) * | 1986-05-27 | 1987-12-03 | Sumitomo Metal Mining Co Ltd | Production of fine particles of crystalline titanium oxide |
| CN101367546A (en) * | 2008-09-27 | 2009-02-18 | 攀钢集团研究院有限公司 | Method for preparing titanium liquid and method for preparing titanium dioxide |
| CN101555038A (en) * | 2009-04-28 | 2009-10-14 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium pigment by hydrolysis |
| CN101700807A (en) * | 2009-11-20 | 2010-05-05 | 无锡海鸿制艇有限公司 | Release structure of free fall style lifeboat |
| CN102050488A (en) * | 2011-01-10 | 2011-05-11 | 攀钢集团重庆钛业有限公司 | Hydrolysis process |
| CN102515267A (en) * | 2011-11-03 | 2012-06-27 | 攀枝花鼎星钛业有限公司 | Production method of high-resistivity titanium dioxide |
-
2015
- 2015-10-23 CN CN201510694978.7A patent/CN105152210A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62278125A (en) * | 1986-05-27 | 1987-12-03 | Sumitomo Metal Mining Co Ltd | Production of fine particles of crystalline titanium oxide |
| CN101367546A (en) * | 2008-09-27 | 2009-02-18 | 攀钢集团研究院有限公司 | Method for preparing titanium liquid and method for preparing titanium dioxide |
| CN101555038A (en) * | 2009-04-28 | 2009-10-14 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium pigment by hydrolysis |
| CN101700807A (en) * | 2009-11-20 | 2010-05-05 | 无锡海鸿制艇有限公司 | Release structure of free fall style lifeboat |
| CN102050488A (en) * | 2011-01-10 | 2011-05-11 | 攀钢集团重庆钛业有限公司 | Hydrolysis process |
| CN102515267A (en) * | 2011-11-03 | 2012-06-27 | 攀枝花鼎星钛业有限公司 | Production method of high-resistivity titanium dioxide |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112694123A (en) * | 2020-12-30 | 2021-04-23 | 福州钛发科技有限公司 | Preparation method of titanium dioxide for delustering dacron chemical fiber |
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