CN103131212A - Preparation method of special titanium dioxide for oily system - Google Patents
Preparation method of special titanium dioxide for oily system Download PDFInfo
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- CN103131212A CN103131212A CN2013100634905A CN201310063490A CN103131212A CN 103131212 A CN103131212 A CN 103131212A CN 2013100634905 A CN2013100634905 A CN 2013100634905A CN 201310063490 A CN201310063490 A CN 201310063490A CN 103131212 A CN103131212 A CN 103131212A
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Abstract
The invention discloses a preparation method of a special titanium dioxide for an oily system. The method comprises the following steps: 1, pulping to prepare a titanium dioxide suspension slurry, adding a dispersant, dispersing, and grinding; 2, diluting the ground titanium dioxide suspension slurry, and filtering; 3, adding a zirconium compound, curing, and depositing; 4, adding an aluminum compound, curing, and depositing; 5, adjusting the pH value, and curing; and 6, washing, drying, and carrying out airflow crushing. The method allows the surface of a titanium dioxide particle to be respectively coated with a zirconium oxide film and an alumina film inside out and a silane coupling agent hydrolysate to be adopted to carry out organic treatment, so the special titanium dioxide has the advantages of substantially-increased weather resistance, lipophilicity and luster, low oil absorption, good dispersity, realization of the hiding capability same to import titanium dioxide, high contrast rate, good temperature resistance, and no ink layer yellowing.
Description
Technical field
The present invention relates to a kind of preparation method of titanium dioxide, especially a kind of oil number is low, the preparation method of the oiliness system special titanium pigment of good dispersity good weatherability, belongs to chemical material technical field.
Background technology
Titanium dioxide is a kind of white inorganic pigment, it is water insoluble, slightly acidic, and good heat resistance, have nontoxic, best opacity, best whiteness and luminance brightness, be widely used in the industries such as coating, plastics, papermaking, printing-ink, chemical fibre, rubber, makeup.For different application industries, titanium dioxide generally all needs the processing through mineral compound, to improve the performances such as its oil number, weathering resistance, opacifying power, dispersiveness and glossiness.Present domestic titanium dioxide adopts the general purpose grade titanium dioxide usually, and general purpose grade titanium dioxide oil number is often higher, bring disadvantageous effect for oiliness coating and printing ink industry user, ordinary titanium powder is when oil paint and the use of printing ink industry, and whiteness and dispersiveness are stable not.
Application number is that 201010208549.1 Chinese invention patent has been announced a kind of titanium dioxide organic film-coating technique for oil paint, it is to use one or more organic silicon compound things, act on the titanium dioxide particle by disintegrating apparatus such as wet method or dry method titanium dioxide is carried out surface modification treatment, can improve rate of dispersion and the dispersion stabilization of titanium dioxide in oleoresin, improve the heat resistance of titanium dioxide in oil paint.Organic coated improvement is more the dispersiveness that can improve the titanium white product, and can't improve the weathering resistance of product.
Application number is that 201010231162.8 Chinese invention patent has been announced a kind of titanium dioxide pigment for ink and preparation method thereof, the technical scheme that it provides, to be coated with coated fertilizer at the titanium dioxide particle surface, coated fertilizer is aluminum oxide, specifically first add certain alkaline aluminum oxide stirring, slaking, deposition, then add the stirring of acidic aluminum oxide compound, slaking, deposition.After washing, drying, pulverizing, when micronizing, add TriMethylolPropane(TMP) to carry out organic process.The weak point of this technology is to adopt monobasic aluminium to coat, and its product weathering resistance is relatively lower slightly, adopts the TriMethylolPropane(TMP) organic process, and organic process technique is simple, and the temperature tolerance of titanium white product is not high enough, can cause China ink layer xanthochromia during the poor quality.
Summary of the invention
The purpose of this invention is to provide that a kind of, good dispersity low in oiliness system oil number, opacifying power are high, the titanium dioxide manufacture method of good weatherability.
The present invention is achieved by the following technical programs:
A kind of preparation method of oiliness system special titanium pigment comprises the following steps:
(1) titanium dioxide is joined in deionized water, make the suspension slurry that concentration is 500～800g/l, add the making beating dispersion agent in suspension slurry, after stirring, adjusting suspension slurry pH value with inorganic alkali solution is 9～11, again the titanium dioxide suspension slurry is carried out milled processed, the dispersion agent weight of wherein pulling an oar is 0.1～0.5% of titanium dioxide weight.
(2) adopt the titanium dioxide suspension slurry after deionized water will grind to be diluted to 200～400g/l, then the suspension slurry after diluting filter by Vibrationsifter.
(3) the titanium dioxide suspension slurry after filtering is warming up to 40～60 ℃, and adjust pH is 5～7, add zirconium compounds in the titanium dioxide suspension slurry in pH value 5～7 scopes, then with titanium dioxide suspension slurry slaking 1～2 hour, make the titanium dioxide particle surface form one deck zirconium white rete, wherein zirconium compounds weight is 0.8～1.5% of titanium dioxide weight, and the mode that adds is and alkali and stream.
(4) the titanium dioxide suspension slurry is continued to be warmed up to 60～80 ℃, adding alkali, progressively to adjust the pH value be 8～10, in being 8～10 scopes, the pH value adds aluminum compound in the titanium dioxide suspension slurry, then with titanium dioxide suspension slurry slaking 1～3 hour, make titanium dioxide particulate zirconium oxide film surface form one deck aluminum oxide rete, wherein aluminum compound weight is 1～4% of titanium dioxide weight, and the mode that adds is and alkali and stream.
(5) adjusting titanium dioxide suspension slurry pH value with mineral acid is 5～7, and slaking 0.5～2 hour.
(6) the titanium dioxide suspension slurry is washed, dry, comminution by gas stream, and add organic agent to carry out organic process in crushing process, obtain final titanium dioxide particle.
Purpose of the present invention can also further realize by following technical measures.
The preparation method of aforesaid oiliness system special titanium pigment, wherein in step (1), the concentration of suspension slurry is 650～700g/l, the making beating dispersion agent is Sodium hexametaphosphate 99 or water glass, making beating dispersion agent weight is 0.3～0.4% of titanium dioxide weight, after stirring, adjusting slurry pH value with sodium hydroxide solution is 10～10.5.
The preparation method of aforesaid oiliness system special titanium pigment, wherein in step (2), the concentration after the dilution of titanium dioxide suspension slurry is 300～350g/l.
The preparation method of aforesaid oiliness system special titanium pigment, wherein in step (3), the titanium dioxide suspension slurry is warming up to 50～55 ℃, and adjust pH is 5～5.5, add zirconium sulfate or zirconyl chloride in above-mentioned pH value scope, zirconium sulfate or zirconyl chloride weight are 1.0% of titanium dioxide weight, and the mode that adds is and sodium hydroxide solution and stream that the curing time is 1 hour.
The preparation method of aforesaid oiliness system special titanium pigment, wherein in step (4), the titanium dioxide suspension slurry is warming up to 65～70 ℃, adding alkali, progressively to adjust the pH value be 8.5～9, add sodium metaaluminate or Tai-Ace S 150 in above-mentioned pH value scope, sodium metaaluminate or Tai-Ace S 150 weight are 2～2.5% of titanium dioxide weight, and the mode that adds is and sodium hydroxide solution and stream that the curing time is 2 hours.
The preparation method of aforesaid oiliness system special titanium pigment, wherein in step (5), adjusting the titanium white slurry pH value with sulphuric acid soln is 6～6.5,1 hour curing time.
The preparation method of aforesaid oiliness system special titanium pigment, wherein said organic agent is the silane coupling agent hydrolyzed solution of concentration 3～10%, the weight that adds the silane coupling agent hydrolyzed solution is 0.3～1% of titanium dioxide weight.
The preparation method of aforesaid oiliness system special titanium pigment, the compound method of wherein said silane coupling agent hydrolyzed solution is: with the silane coupling agent thin up, then add HAc to make hydrolyst, be hydrolyzed 5 minutes, adjusting the pH value is 3.5～4.5.
The present invention coats respectively zirconium white rete and aluminum oxide rete from inside to outside at the titanium dioxide particle surface, and adopt the silane coupling agent hydrolyzed solution to carry out organic process, weathering resistance, lipophilicity and the glossiness of titanium dioxide have greatly been improved, the titanium dioxide oil number is low, good dispersity, opacifying power is suitable with the import titanium dioxide simultaneously, has higher contrast ratio, the product temperature tolerance is good, can not cause China ink layer xanthochromia.
Advantage and disadvantage of the present invention will be for illustration and explanation by the non-limitative illustration of following preferred embodiment, and these embodiment only provide as an example with reference to accompanying drawing.
Description of drawings
Fig. 1 is schematic flow sheet of the present invention.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment one
(1) the 400g titanium dioxide is joined in deionized water, make the suspension slurry that concentration is 650g/l, add Sodium hexametaphosphate 99 as the making beating dispersion agent in suspension slurry, adding weight is 0.3% of titanium dioxide weight, after stirring, adjusting slurry pH value with the 100g/l sodium hydroxide solution is 10, the titanium dioxide suspension slurry is pumped into the anti-sand mill of speeding of testing laboratory grind.
(2) the titanium dioxide suspension slurry after adopting deionized water with sand milling is diluted to 300g/l, and slurries are by 325 order Vibrationsifters, with the crude product titanium white macroparticle of removing the pettiness that may exist and chip and other impurity of sand milling mill pearl.
(3) above-mentioned titanium dioxide suspension slurry is warmed up to 50 ℃ and adjust pH 5～5.5, add zirconium sulfate or zirconyl chloride in this pH value scope, the present embodiment preferably sulfuric acid zirconium, it is 1.0% of titanium dioxide weight that zirconium sulfate adds weight, the mode that adds is and sodium hydroxide solution and stream, after adding, with titanium white slurries slaking 1 hour, make the titanium dioxide particle surface form one deck hydrous zirconium oxide rete, hydrous zirconium oxide rete by deposition, can improve the weathering resistance of product, and can be combined well with the titanium dioxide granule surface, make follow-up aqua oxidation aluminum membranous layer coat closelyr.
(4) the titanium dioxide slurries are warmed up to 67 ℃, add alkali and progressively adjust pH value to 8.5～9, add sodium metaaluminate or Tai-Ace S 150 in this pH value scope, the preferred sodium metaaluminate of the present embodiment, the sodium metaaluminate add-on is 2% of titanium dioxide weight, the mode that adds is and sodium hydroxide solution and stream, after adding, with titanium white slurries slaking 2 hours, make titanium dioxide particle hydrous zirconium oxide film surface form one deck aqua oxidation aluminum membranous layer, can improve lipophilicity, weathering resistance, the gloss of product by the aqua oxidation aluminum membranous layer of deposition.
(5) adjust titanium white slurry pH value to 6～6.5 with the 100g/l sulphuric acid soln, slaking 1 hour makes it fully stable until the pH value remains unchanged.
(6) with above-mentioned titanium white aqueous suspension slurries, carry out suction filtration, washing, drying, comminution by gas stream.
Embodiment two
Embodiment two steps (1) are basic identical to step (6) and embodiment one, and difference is, the sodium silicate solution that adopts 100g/l in embodiment two steps (1) is as the sand milling dispersion agent of pulling an oar.
Embodiment three
Embodiment three steps (1) are identical with embodiment one to step (6), at last in the comminution by gas stream stage, add 0.5% TriMethylolPropane(TMP) to carry out organic process.
Embodiment four
Step in embodiment four (1) is identical with embodiment one to step (6), at last in the comminution by gas stream stage, adds the silane coupling agent hydrolyzed solution to carry out organic process, and add-on is 0.6% of titanium dioxide weight.
Silane coupling agent hydrolyzed solution compound method: with the silane coupling agent thin up, then add HAc or salt to make hydrolyst, be hydrolyzed 5 minutes, and the pH value is transferred to 4.0, under this pH the silane coupling agent alcoholysis the fastest, condensation is the slowest, be hydrolyzed after 5 minutes, namely generate the hydrolyzate that contains Si-OH.The silane coupling agent hydrolyzed solution concentration of preparation is 5%.
Embodiment five
Embodiment five is identical to step (6) with embodiment two steps (1), at last in the comminution by gas stream stage, adds the silane coupling agent hydrolyzed solution to carry out organic process, and add-on is 0.6% of titanium dioxide weight.Silane coupling agent hydrolyzed solution compound method is identical with compound method in embodiment four.
Titanium white powder pigment with embodiment one to embodiment five preparation compares with commercially available titanium dioxide pigment, and wherein contrasting sample 1 is to adopt sial to coat, and contrast sample 2 is to adopt aluminium to coat.
Comparing result is as follows:
By comparing result as can be known, what the present invention prepared processes titanium dioxide pigment with silane coupling agent, owing to adopting remarkable inorganic and organic process technique, product has high dispersiveness, glossiness and extremely low oil number in the oiliness system, opacifying power is suitable with the import titanium dioxide simultaneously, has higher contrast ratio.
In addition to the implementation, the present invention can also have other embodiments, and all employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop in the protection domain of requirement of the present invention.
Claims (8)
1. the preparation method of an oiliness system special titanium pigment is characterized in that comprising the following steps:
(1) titanium dioxide is joined in deionized water, make the suspension slurry that concentration is 500～800g/l, add the making beating dispersion agent in suspension slurry, after stirring, adjusting suspension slurry pH value with inorganic alkali solution is 9～11, again the titanium dioxide suspension slurry is carried out milled processed, the dispersion agent weight of wherein pulling an oar is 0.1～0.5% of titanium dioxide weight;
(2) adopt the titanium dioxide suspension slurry after deionized water will grind to be diluted to 200～400g/l, then the suspension slurry after diluting filter by Vibrationsifter;
(3) the titanium dioxide suspension slurry after filtering is warming up to 40～60 ℃, and adjust pH is 5～7, add zirconium compounds in the titanium dioxide suspension slurry in pH value 5～7 scopes, then with titanium dioxide suspension slurry slaking 1～2 hour, make the titanium dioxide particle surface form one deck zirconium white rete, wherein zirconium compounds weight is 0.8～1.5% of titanium dioxide weight, and the mode that adds is and alkali and stream;
(4) the titanium dioxide suspension slurry is continued to be warmed up to 60～80 ℃, adding alkali, progressively to adjust the pH value be 8～10, in being 8～10 scopes, the pH value adds aluminum compound in the titanium dioxide suspension slurry, then with titanium dioxide suspension slurry slaking 1～3 hour, make titanium dioxide particulate zirconium oxide film surface form one deck aluminum oxide rete, wherein aluminum compound weight is 1～4% of titanium dioxide weight, and the mode that adds is and alkali and stream;
(5) adjusting titanium dioxide suspension slurry pH value with mineral acid is 5～7, and slaking 0.5～2 hour;
(6) the titanium dioxide suspension slurry is washed, dry, comminution by gas stream, and add organic agent to carry out organic process in crushing process, obtain final titanium dioxide particle.
2. the preparation method of oiliness system special titanium pigment as claimed in claim 1, it is characterized in that: in step (1), the concentration of suspension slurry is 650～700g/l, the making beating dispersion agent is Sodium hexametaphosphate 99 or water glass, making beating dispersion agent weight is 0.3～0.4% of titanium dioxide weight, after stirring, adjusting slurry pH value with sodium hydroxide solution is 10～10.5.
3. the preparation method of oiliness system special titanium pigment as claimed in claim 1 is characterized in that: in step (2), the concentration after the dilution of titanium dioxide suspension slurry is 300～350g/l.
4. the preparation method of oiliness system special titanium pigment as claimed in claim 1, it is characterized in that: in step (3), the titanium dioxide suspension slurry is warming up to 50～55 ℃, and adjust pH is 5～5.5, add zirconium sulfate or zirconyl chloride in above-mentioned pH value scope, zirconium sulfate or zirconyl chloride weight are 1.0% of titanium dioxide weight, and the mode that adds is and sodium hydroxide solution and stream that the curing time is 1 hour.
5. the preparation method of oiliness system special titanium pigment as claimed in claim 1, it is characterized in that: in step (4), the titanium dioxide suspension slurry is warming up to 65～70 ℃, adding alkali, progressively to adjust the pH value be 8.5～9, add sodium metaaluminate or Tai-Ace S 150 in above-mentioned pH value scope, sodium metaaluminate or Tai-Ace S 150 weight are 2～2.5% of titanium dioxide weight, and the mode that adds is and sodium hydroxide solution and stream that the curing time is 2 hours.
6. the preparation method of oiliness system special titanium pigment as claimed in claim 1 is characterized in that: in step (5), adjusting the titanium white slurry pH value with sulphuric acid soln is 6～6.5,1 hour curing time.
7. the preparation method of oiliness system special titanium pigment as claimed in claim 1, it is characterized in that: described organic agent is the silane coupling agent hydrolyzed solution of concentration 3～10%, the weight that adds the silane coupling agent hydrolyzed solution is 0.3～1% of titanium dioxide weight.
8. the preparation method of oiliness system special titanium pigment as claimed in claim 7, it is characterized in that: the compound method of described silane coupling agent hydrolyzed solution is: with the silane coupling agent thin up, then add HAc to make hydrolyst, be hydrolyzed 5 minutes, adjusting the pH value is 3.5～4.5.
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| CN104107764A (en) * | 2014-07-22 | 2014-10-22 | 四川龙蟒钛业股份有限公司 | Method for improving flatness and glossiness of titanium dioxide film |
| CN104119702A (en) * | 2014-07-22 | 2014-10-29 | 四川龙蟒钛业股份有限公司 | Process for coating aluminum and zirconium on rutile-type titanium dioxide with high gloss and high weather resistance |
| CN105860591A (en) * | 2016-05-05 | 2016-08-17 | 中钛集团洛阳市裕星化工有限公司 | Preparation method of novel zirconium-aluminum coated titanium dioxide |
| CN106006724A (en) * | 2016-05-18 | 2016-10-12 | 云南林缘香料有限公司 | Reacting and washing process and equipment for production of metatitanic acid from titanium dioxide slurry |
| CN106280572A (en) * | 2016-07-18 | 2017-01-04 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method improving titanium dioxide dispersibility |
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| CN108864770A (en) * | 2018-09-05 | 2018-11-23 | 襄阳龙蟒钛业有限公司 | A kind of preparation method of low oil absorption ferric titanium dioxide |
| CN109054453A (en) * | 2018-09-05 | 2018-12-21 | 襄阳龙蟒钛业有限公司 | A kind of low oil absorption ferric titanium dioxide |
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| CN110256874A (en) * | 2019-05-24 | 2019-09-20 | 江苏大学 | The process of zirconium silicon compound adhesive cyst membrane coated red schorl type titanium dioxide |
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| CN113583480A (en) * | 2021-07-30 | 2021-11-02 | 龙佰集团股份有限公司 | Preparation method of high-end universal titanium dioxide |
| CN115746582A (en) * | 2022-11-30 | 2023-03-07 | 攀钢集团研究院有限公司 | Method for reducing oil absorption of titanium dioxide |
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| CN104119702A (en) * | 2014-07-22 | 2014-10-29 | 四川龙蟒钛业股份有限公司 | Process for coating aluminum and zirconium on rutile-type titanium dioxide with high gloss and high weather resistance |
| CN104119702B (en) * | 2014-07-22 | 2015-11-18 | 四川龙蟒钛业股份有限公司 | The zirconium aluminium coating process of a kind of high gloss, high-weatherability Rutile type Titanium Dioxide |
| CN104107764A (en) * | 2014-07-22 | 2014-10-22 | 四川龙蟒钛业股份有限公司 | Method for improving flatness and glossiness of titanium dioxide film |
| CN105860591B (en) * | 2016-05-05 | 2018-05-18 | 焦作市裕盛钛业有限公司 | A kind of preparation method of novel zirconium-aluminum-ctitanium titanium dioxide |
| CN105860591A (en) * | 2016-05-05 | 2016-08-17 | 中钛集团洛阳市裕星化工有限公司 | Preparation method of novel zirconium-aluminum coated titanium dioxide |
| CN106006724A (en) * | 2016-05-18 | 2016-10-12 | 云南林缘香料有限公司 | Reacting and washing process and equipment for production of metatitanic acid from titanium dioxide slurry |
| CN106006724B (en) * | 2016-05-18 | 2017-07-21 | 云南林缘香料有限公司 | The reaction washing process and equipment of titanium dioxide slurry production metatitanic acid |
| CN106280572B (en) * | 2016-07-18 | 2018-08-14 | 成都先进金属材料产业技术研究院有限公司 | A method of improving titanium dioxide dispersibility |
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| CN107828249A (en) * | 2017-11-28 | 2018-03-23 | 钦州学院 | Plastics titanium dioxide Organic surface treatment method |
| CN107955414A (en) * | 2017-12-01 | 2018-04-24 | 江苏镇钛化工有限公司 | The preparation method of water-based Diamond Search ink special titanium pigment |
| CN108864770A (en) * | 2018-09-05 | 2018-11-23 | 襄阳龙蟒钛业有限公司 | A kind of preparation method of low oil absorption ferric titanium dioxide |
| CN109054453A (en) * | 2018-09-05 | 2018-12-21 | 襄阳龙蟒钛业有限公司 | A kind of low oil absorption ferric titanium dioxide |
| CN109535775B (en) * | 2018-12-24 | 2020-11-24 | 攀钢集团重庆钛业有限公司 | Preparation method of titanium dioxide special for printing ink |
| CN109535775A (en) * | 2018-12-24 | 2019-03-29 | 攀钢集团重庆钛业有限公司 | The preparation method of ink tailored version titanium dioxide |
| CN110256874A (en) * | 2019-05-24 | 2019-09-20 | 江苏大学 | The process of zirconium silicon compound adhesive cyst membrane coated red schorl type titanium dioxide |
| CN112759948A (en) * | 2020-12-30 | 2021-05-07 | 攀枝花东方钛业有限公司 | Special titanium dioxide for road sign paint and preparation method thereof |
| CN112759948B (en) * | 2020-12-30 | 2022-05-10 | 攀枝花东方钛业有限公司 | Special titanium dioxide for road sign paint and preparation method thereof |
| CN112759994A (en) * | 2021-01-22 | 2021-05-07 | 安徽天锦云节能防水科技有限公司 | Heat-insulation heat-preservation cold-insulation coating and preparation method thereof |
| CN113583480A (en) * | 2021-07-30 | 2021-11-02 | 龙佰集团股份有限公司 | Preparation method of high-end universal titanium dioxide |
| CN115746582A (en) * | 2022-11-30 | 2023-03-07 | 攀钢集团研究院有限公司 | Method for reducing oil absorption of titanium dioxide |
| CN115850999A (en) * | 2022-11-30 | 2023-03-28 | 攀钢集团研究院有限公司 | Preparation method of titanium dioxide for high-gloss high-dispersion ink |
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Application publication date: 20130605 |