CN106186055A - A kind of preparation method producing hydrolysis crystal seed in titanium dioxide technique and the delustering agent titanium dioxide of the method manufacture - Google Patents
A kind of preparation method producing hydrolysis crystal seed in titanium dioxide technique and the delustering agent titanium dioxide of the method manufacture Download PDFInfo
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- CN106186055A CN106186055A CN201610504442.9A CN201610504442A CN106186055A CN 106186055 A CN106186055 A CN 106186055A CN 201610504442 A CN201610504442 A CN 201610504442A CN 106186055 A CN106186055 A CN 106186055A
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- titanium dioxide
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- 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
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
- C01G23/0534—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts in the presence of seeds
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The present invention refers to titanyl sulfate solution and Na3PO4Solution reaction prepares the method for hydrolysis crystal seed.Concrete grammar uses and is added to Na according to certain mass ratio by the titanyl sulfate solution under uniform temperature3PO4In solution, stirring ripening is until the stability of crystal seed drops to the requirement of regulation and get final product, and thus method generation obtains the titanium dioxide product as delustering agent.The present invention has the advantage such as excellent whiteness, aqueous dispersion ability is strong, extinction capability good, impurity content is few, moderate in grain size and narrow particle size distribution with regard to this titanium dioxide of obtaining of hydrolysis, is suitable for use as delustering agent.
Description
Technical field
The present invention relates to the preparation method of hydrolysis crystal seed in a kind of sulfuric acid method titanium pigment production process, and the method manufacture
Delustering agent titanium dioxide, belong to titanium dioxide manufacture field.
Background technology
Titanium dioxide is mainly used as delustering agent in chemical fibre industry, estimates that global Year's consumption is at 80,000 tons～10 at present
About ten thousand tons, domestic it is used to about about 10,000 tons.Owing to titanium dioxide has special optics and thing in all of Chinese white
Rationality energy, it is considered to be the optimal extinction material of chemical fibre, is widely used to the production of chemical fibre as delustering agent
In.The good dispersion that chemical fibre requires in water with titanium dioxide, there is also a need at the solution such as ethylene glycol, sodium rhodanate for some kind
In have preferable dispersive property, do not react with these chemical substances.Additionally, impurity content to be required is low,
The outward appearance whiteness that can guarantee that fiber is good, the good dispersion of titanium dioxide.
The operating process of plus seed Hydrolyze method is fairly simple, and its technology key is the matter of method and the crystal seed preparing crystal seed
Amount.So-called crystal seed is exactly a kind of colloid titanium hydroxide solution that titanyl sulfate solution prepares through not exclusively neutralizing, and it is at water
Playing a part hydrated titanium dioxide nucleus of crystal during solution, it can not only accelerate hydrolysis, shorten the hydrolysis cycle, and to water
Solve the particle diameter of precipitated product, particle diameter distribution and end product quality and have large effect.In hydrolytic process, titanyl sulfate is adding
The effect of induction of heat and crystal seed issues unboiled water solution, as long as there being the surface of sufficient amount of crystal seed in titanium liquid, and programming rate, stirs
Mix speed, dilute proper, then generated hydrated titanium dioxide all precipitatings, on these nucleus of crystals, will not occur new crystallization
Center, the most not only hydrolysis carries out completely, and the particle diameter ratio of hydrated titanium dioxide is more uniform, and it is excellent to obtain pigment performance
TiO more2, filter washing and be also easier, wear filter loss few.
Plus seed Hydrolyze method is commonly used in existing industry usually will count concentration for 190-200g/L sulphuric acid with titanium dioxide
Oxygen titanium solution and the sodium hydroxide solution that concentration is 7.8% are separately heated to 90 DEG C, then by sodium hydroxide and titanyl sulfate (with
TiO2Meter) mix with the ratio of mass ratio 7: 1, it is neutralized, after neutralization, is warming up to 96 DEG C, survey crystal seed stability and reach 100-130.
But learn through practice, its particle diameter of the hydrolysis crystal seed thus prepared complete hydrolysis that is unfavorable for the most uniform, of low quality, hydrolysis
The hydrated titanium dioxide particle generated is thicker, although be easier to wash, but the broad particle distribution of products obtained therefrom (1.0-2.0 μm),
Impurity content higher (100ppm) causes reducing power low, and finished product is of poor quality, and is unfavorable in ethylene glycol (high temperature 300 DEG C) dividing
Dissipate property to reach the requirement of delustering agent titanium dioxide, also make that relevant delustering agent product quality is low, the market competitiveness is low.
Summary of the invention
Present invention aim at providing the preparation method of hydrolysis crystal seed in a kind of new plus seed method, and utilize the method
Prepare delustering agent titanium dioxide, to overcome existing delustering agent titanium dioxide particle size distribution width, impurity content higher and at (high temperature 300
DEG C) problem such as bad dispersibility in ethylene glycol, thus improve Related product quality, enhance one's market competitiveness.
The present invention realizes the drip irrigation device of above-mentioned purpose, uses Na3PO4The method system replacing traditional NaOH
Standby crystal seed, to reach control crystallite grain size and ensure the purposes such as crystal seed uniform particle sizes.
Technical scheme is as follows, will be with TiO2Titanyl sulfate solution and the concentration of meter 190-200g/L are the Na of 5%-7%3PO4
Solution, according to the ratio of mass ratio 5: 1-7: 1, is separately heated to 90 DEG C, then titanyl sulfate solution is joined Na3PO4Solution
In be neutralized, coutroi velocity is to ensure that the response time controlled in 6-8 minute.It is warming up to 96 DEG C after neutralizing reaction, measures crystalline substance
Kind of stability reaches 100-130, quickly puts in preheated Hydrolysis of Titanium liquid, the titanium dioxide of high-quality.Why use
Concentration is the Na of 5%-7%3PO4Substitute NaOH, be because in practical operation finding, solution exists certain density PO4 3-
Ion is more conducive to TiO2The dispersion of colloidal sol thus obtain particle diameter hydrolysis crystal seed evenly, in follow-up hydrolytic process
The nucleus of crystal of uniform particle sizes can be obtained, thus control the aspects such as the particle diameter of finished product, particle size distribution, form moral character excellent
Titanium dioxide.Wherein the method for testing of crystal seed stability is for measuring 10ml crystal seed, add water the hydrolysis until solution bleaches time consumed
The volume of water.
Preferably, Na3PO4Solution concentration is 6%；
Preferably, with TiO2The titanyl sulfate solution of meter 190-200g/L and Na3PO4Solution, according to the ratio of mass ratio 6: 1
Example carries out subsequent reactions, obtains the described titanium dioxide for delustering agent.
Beneficial effect:
1. the present invention uses the Na of 5-7%3PO4Solution substitutes 7.8%NaOH solution, according to 5: the ratio of 1-7: 1 is with clean
Titanyl sulfate reaction prepare crystal seed, centralized particle diameter, in later stage calcine technology, be difficult to agglomeration, be beneficial to obtain grain
Footpath is little and the product of narrow diameter distribution, and its quality is significantly better than and uses NaOH to prepare crystal seed to hydrolyze the product quality obtained.
2. using crystal seed preparation method of the present invention to hydrolyze the metatitanic acid obtained, washing speed is accelerated than prior art
50%, shorten the production time.
3. avoid using strong basicity NaOH, require to reduce to equipment corrosion resistance, extend the use of production equipment accordingly
Life-span thus reduce dirt produce equipment cost.
4. the titanium dioxide using the crystal seed preparation method of the present invention to produce have excellent whiteness, aqueous dispersion ability strong,
The advantages such as extinction capability is good, impurity content is few, moderate in grain size and narrow particle size distribution.
5., when being used for cutting photo etching use, unit are consumption is greatly reduced, and cuts light effect constant.And be conducive to extending accordingly
Produce service life of equipment etc., such that it is able to reduce production cost.When spraying uses, it is not easily blocked nozzle, extends shower nozzle and use
Life-span.
6. the titanium dioxide dispersive property in high temperature glycol (300 DEG C) using the crystal seed preparation method of the present invention to produce is steady
Fixed, reach the requirement of delustering agent titanium dioxide, product quality improves, and enhances the market competitiveness.
Detailed description of the invention
The present invention will be described in detail by the specific embodiment of following exemplary, but the spirit of the present invention and right are wanted
The protection domain seeking book is not limited by these specific embodiments.
Embodiment 1
Will be with TiO2Titanyl sulfate solution and the concentration of meter 190-200g/L are the Na of 6%3PO4Solution is according to mass ratio 7: 1
Ratio, be separately heated to 90 DEG C, then titanyl sulfate solution joined Na3PO4Solution is neutralized, coutroi velocity with
Ensure that the response time controlled in 6-8 minute.It is warming up to 96 DEG C altogether after neutralizing reaction, measures crystal seed stability and reach 100-130, soon
Speed is put in preheated Hydrolysis of Titanium liquid.Wherein the method for testing of crystal seed stability is: measure 10ml crystal seed, adds water until molten
Liquid bleach hydrolysis time the volume of water that consumed.It was verified that solution exists certain density PO4 3-Ion is more conducive to TiO2
The dispersion of colloidal sol thus obtain the washing process of particle diameter hydrolysis crystal seed evenly, the most beneficially later stage, to wear filter loss few, also
It is beneficial to obtain the TiO that pigment performance is superior2Finished product, gives full play to the effect of delustering agent.
Embodiment 2
Will be with TiO2Titanyl sulfate solution and the concentration of meter 190-200g/L are the Na of 6%3PO4Solution is according to mass ratio 6: 1
Ratio, be separately heated to 90 DEG C, then titanyl sulfate solution joined Na3PO4Solution is neutralized, coutroi velocity with
Ensure that the response time controlled in 6-8 minute.It is warming up to 96 DEG C altogether after neutralizing reaction, measures crystal seed stability and reach 100-130, soon
Speed is put in preheated Hydrolysis of Titanium liquid.It was verified that solution exists certain density PO4 3-Ion is more conducive to TiO2Molten
The dispersion of glue thus obtain the washing process of particle diameter hydrolysis crystal seed evenly, the most beneficially later stage, to wear filter loss few, also profit
In obtaining the TiO that pigment performance is superior2Finished product, gives full play to the effect of delustering agent.
Embodiment 3
Will be with TiO2Titanyl sulfate solution and the concentration of meter 190-200g/L are the Na of 5%3PO4Solution is according to mass ratio 6: 1
Ratio, be separately heated to 90 DEG C, then titanyl sulfate solution joined Na3PO4Solution is neutralized, coutroi velocity with
Ensure that the response time controlled in 6-8 minute.It is warming up to 96 DEG C altogether after neutralizing reaction, measures crystal seed stability and reach 100-130, soon
Speed is put in preheated Hydrolysis of Titanium liquid.It was verified that solution exists certain density PO4 3-Ion is more conducive to TiO2Molten
The dispersion of glue thus obtain the washing process of particle diameter hydrolysis crystal seed evenly, the most beneficially later stage, to wear filter loss few, also profit
In obtaining the TiO that pigment performance is superior2Finished product, gives full play to the effect of delustering agent.
Embodiment 4
Will be with TiO2Titanyl sulfate solution and the concentration of meter 190-200g/L are the Na of 7%3PO4Solution is according to mass ratio 6: 1
Ratio, be separately heated to 90 DEG C, then titanyl sulfate solution joined Na3PO4Solution is neutralized, coutroi velocity with
Ensure that the response time controlled in 6-8 minute.It is warming up to 96 DEG C altogether after neutralizing reaction, measures crystal seed stability and reach 100-130, soon
Speed is put in preheated Hydrolysis of Titanium liquid.It was verified that solution exists certain density PO4 3-Ion is more conducive to TiO2Molten
The dispersion of glue thus obtain the washing process of particle diameter hydrolysis crystal seed evenly, the most beneficially later stage, to wear filter loss few, also profit
In obtaining the TiO that pigment performance is superior2Finished product, gives full play to the effect of delustering agent.The index of above-described embodiment products obtained therefrom
As shown in the table:
| Two wash after titanyl sulfate iron content | ＜ 10ppm |
| P2O5 | 0.6-0.65% |
| TiO2 | >=98% |
| Color, reducing power (with standard specimen ratio) | >=100% |
| 105 DEG C of volatile matters | ≤ 0.5% |
| Water-soluble substance | ≤ 0.35% |
| Water slurry pH value | 7.2 |
| Oil absorption | 22g/100g |
| Residue on sieve (45 μm sieve aperture) | ≤ 0.01 (%) |
| Water dispersible | >=94% |
| Water extract resistivity | ≥30Ω.cm |
| Fe2O3 | ≤10ppm |
| Ethylene glycol dispersibility | >=92% |
| The apparent whiteness of powder body | ≥97.0 |
| L | ≥98.0 |
| a | ≤0.15 |
| b | ≤0.30 |
| D50 | 0.27-0.29μm |
| D90 | ≤0.4μm |
Claims (5)
1. the preparation method being used for producing the hydrolysis crystal seed of titanium dioxide, it is characterised in that with TiO2It is calculated as 190-200g/L sulfur
Acid oxygen titanium is raw material and Na3PO4Solution reacts according to certain mass ratio.
2. according to the preparation method of a kind of hydrolysis crystal seed for producing titanium dioxide described in claim 1, it is characterised in that
With TiO2Being calculated as 190-200g/L titanyl sulfate is raw material and concentration is 5%-7%Na3PO4Solution, is separately heated to 90 DEG C, so
After according to 5: titanyl sulfate solution is joined Na by the mass ratio of 1-7: 13PO4Solution is neutralized；Coutroi velocity is to ensure
Response time controlled in 6-8 minute；96 DEG C it are warming up to altogether after neutralizing reaction；Measure crystal seed stability and reach 100-130, obtain institute
Need hydrolysis crystal seed.
3. according to the preparation method of a kind of hydrolysis crystal seed for producing titanium dioxide described in claim 2, it is characterised in that
Na3PO4Solution concentration is 6%.
4. according to the preparation method of a kind of hydrolysis crystal seed for producing titanium dioxide described in claim 2, it is characterised in that
Titanyl sulfate and Na3PO4It is 6: 1 titanyl sulfate solution to be joined Na according to mass ratio3PO4Solution is neutralized.
5. the titanium dioxide produced by method described in claim 1, cuts the purposes in photo etching manufacturing.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678202A (en) * | 2019-01-25 | 2019-04-26 | 衡阳师范学院 | A kind of surface modified titanium preparation method and its surface modifying apparatus |
| CN112457691A (en) * | 2020-11-26 | 2021-03-09 | 海宁澜钛新材料有限公司 | Low-photocatalytic-activity delustering agent and preparation method and application thereof |
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| CN1834019A (en) * | 2006-04-05 | 2006-09-20 | 江苏太白集团有限公司 | Prepn. method of hydrolytic crystal seeds for producing titanium pigment |
| CN1850619A (en) * | 2006-05-12 | 2006-10-25 | 南京钛白化工有限责任公司 | Method for preparing anatase chemical fiber special titanium pigment |
| CN101049556A (en) * | 2007-05-15 | 2007-10-10 | 河北师范大学 | Method for preparing high heat stability titanium dichloride in anatase type |
| CN103183377A (en) * | 2013-03-04 | 2013-07-03 | 广西金茂钛业有限公司 | Method for hydrolyzing low-concentration self-generating crystal seed in process of preparing titanium dioxide by sulfuric acid method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1834019A (en) * | 2006-04-05 | 2006-09-20 | 江苏太白集团有限公司 | Prepn. method of hydrolytic crystal seeds for producing titanium pigment |
| CN1850619A (en) * | 2006-05-12 | 2006-10-25 | 南京钛白化工有限责任公司 | Method for preparing anatase chemical fiber special titanium pigment |
| CN101049556A (en) * | 2007-05-15 | 2007-10-10 | 河北师范大学 | Method for preparing high heat stability titanium dichloride in anatase type |
| CN103183377A (en) * | 2013-03-04 | 2013-07-03 | 广西金茂钛业有限公司 | Method for hydrolyzing low-concentration self-generating crystal seed in process of preparing titanium dioxide by sulfuric acid method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678202A (en) * | 2019-01-25 | 2019-04-26 | 衡阳师范学院 | A kind of surface modified titanium preparation method and its surface modifying apparatus |
| CN112457691A (en) * | 2020-11-26 | 2021-03-09 | 海宁澜钛新材料有限公司 | Low-photocatalytic-activity delustering agent and preparation method and application thereof |
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Address after: 543399 Tengxian Chemical Industry Zone, Wuzhou City, Guangxi Zhuang Autonomous Region Patentee after: Guangxi Jinmao Titanium Industry Co.,Ltd. Address before: 543300 Tengxian Chemical Industry Park, Guangxi (Pingzheng Village, Tengzhou Town, the original plant area of Tengxian Resin Factory) Patentee before: GUANGXI JINMAO TITANIUM Co.,Ltd. |
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Denomination of invention: A preparation method for hydrolyzed crystal seeds in the production process of titanium dioxide and titanium dioxide powder for matting agent manufactured by the method Effective date of registration: 20230822 Granted publication date: 20181113 Pledgee: Tengxian Rural Credit Cooperative Association Pledgor: Guangxi Jinmao Titanium Industry Co.,Ltd. Registration number: Y2023980053145 |
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