CN103450712B - Illite-based composite titanium dioxide and preparation method thereof - Google Patents
Illite-based composite titanium dioxide and preparation method thereof Download PDFInfo
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- CN103450712B CN103450712B CN201310367913.2A CN201310367913A CN103450712B CN 103450712 B CN103450712 B CN 103450712B CN 201310367913 A CN201310367913 A CN 201310367913A CN 103450712 B CN103450712 B CN 103450712B
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Abstract
The invention provides illite-based composite titanium dioxide and a preparation method thereof. The composite titanium dioxide is obtained by coating the surface of illite with nano titanium dioxide particles, and is prepared from the following components in parts by weight: 60-80 parts of illite, 15-35 parts of titanium dioxide and 0.5-5 parts of dispersing agents. The preparation method comprises the steps of depositing, washing and filtering and calcining. The prepared composite titanium dioxide has the characteristics of low cost, high whiteness, strong covering power, low oil absorption and low water-soluble salt value.
Description
Technical field
The present invention relates to a kind of composite titanium dioxide and preparation method thereof.
Background technology
Titanium dioxide (TiO
2), English name Titanium dioxide is a kind of important Inorganic Chemicals, nontoxic to health, harmless.When titanium dioxide is as being referred to as titanium white (Titanium dioxide white pigment, Titanium white) during white pigment, titanium white is most important white pigment, accounts for 80% of whole white pigment usage quantity.Titanium resource 90% for the production of titanium dioxide, all the other 10% produce metal titanium, titanium alloy and potteries etc.Titanium dioxide has become one of three kinds of maximum commodity of sales volume in world's inorganic chemical product, is only second to synthetic ammonia and phosphoric acid.TiO
2as white pigment, there is high opaqueness and excellent optical property, pigment property.Therefore be widely used in the industries such as coating, ink, plastics, rubber, papermaking, chemical fibre and daily cosmetics.
The industrial process of current titanium dioxide comprises sulfuric acid process and chlorination process, accounts for 47% and 53% of global titanium white production respectively, in China, about has the enterprise of 95% to adopt sulfuric acid process.Sulfuric acid process is raw material with ilmenite, adopts 85% sulfuric acid to decompose, and makes titanium compound in ore deposit be transformed into titanium liquid, and the hydrolysis after purification of titanium liquid is transformed into hydrated titanium dioxide, then obtains titanium dioxide finished product through washing, calcining and aftertreatment.Sulfuric acid process is complicated, and long flow path, produces a large amount of spent acid, acid waste water and waste residue in production process, environmental pollution is extremely serious.Chlorination process is that titaniferous ore (or artificial rutile) is made titanium tetrachloride through high-temp chlorination, and titanium tetrachloride is at high temperature oxidized and generates titanium dioxide and chlorine after purifying, and the chlorine of generation returns titanium chloride material.Technical process is short, and automatization level is high, and product specification is high.But produce the waste residue containing radioactive substance and toxic chlorinated thing in chloride process titanium dioxide production process, be difficult to administer and utilize, pollution hazard is very big.Along with continuing to increase of the day by day in short supply of Mineral Resources in China and national environmental protection dynamics, production cost and environmental problem have become the bottleneck of restriction titanium powder industry in China development.
The pigment performance of titanium dioxide particle embodies mainly through optical property, and optical property depends primarily on TiO
2the surface properties of particle, therefore, TiO
2check optical property in particle almost not contribute.If a kind of white material cheap and easy to get can be used to replace TiO
2particle kernel, then titanium dioxide cost will reduce greatly.
Composite titanium dioxide passes through to adopt cheap mineral as kernel, at its Surface coating one deck TiO just
2particle and obtaining.Current each state is all studying and is exploring composite titanium dioxide, to reduce its cost.
Application number is 02135086.8, and denomination of invention is " Nano-meter CaCO3
3/ TiO
2composite particles and preparation method thereof " Chinese patent application, disclose adopt Ti (OH) 4 colloidal solution be deposited on Nano-meter CaCO3
3particle prepares Nano-meter CaCO3
3/ TiO
2the method of composite particles, but the method goes out Ti (OH) because needs are previously prepared
4colloid, makes complex process, and cost is higher, the TiO simultaneously deposited
2very limited, make composite particles pigment performance poor.
Application number is 200510080497.3, denomination of invention is the Chinese patent application of " white mineral powder-TiO2 composite white pigment and preparation method thereof ", disclose and use white mineral powder, if calcium carbonate, kaolin, calcined kaolin and barite etc. are bag core matrix, crystal TiO
2for coating thing, in wet ultra-fine grinding system, by grain-grain coating modification mode, realize TiO
2coated and the modifying and decorating in the reaction of bag core matrix surface, preparation has the white mineral powder-TiO of pigmentary titanium dioxide character thus
2the method of composite white pigment.But the method is owing to existing, and bonding force is strong, grain-grain is coated is the quality problems such as to carry out on secondary agglomeration particle, can only obtain appropriateness application, and cost is higher in low and middle-grade products of part industry.
The application number of Nittetsu Mining Co., Ltd. of Japan is the Chinese patent application of 01813600.1, disclose employing carbonating process, prepare and a kind ofly can present the method for titanium dioxide natural characteristics as the titanium dioxide calcium carbonate composite particles of height opacity, the method adds the TiO 2 particles with median size 0.1 ~ 0.5 μm in carbonation step, typically under agitation, the mixture of introducing carbon dioxide gas and air in calcium hydroxide slurry, carry out carbonation reaction, and the pH that continuation importing gaseous mixture makes reaction proceed to slurry is 7.Final acquisition relates to containing combination above-mentioned composite particles ground composite composition wherein, can be applicable to coating and the pigment of paper grade (stock), and matrix material such as paper, plastic shaping material and rubber-moulding material etc.The method utilizes the existing calcium carbonate technological process of production, suitability for industrialized production can be realized after increasing process portion, as long as composite pigment meets use properties requirement, application prospect is very good, but the combination of the calcium carbonate of composite titanium dioxide prepared by the method and titanium dioxide is firm not, opacifying power is strong not, and weathering resistance is not high.
Summary of the invention
In view of this, the first object of the present invention is to provide a kind of composite titanium dioxide of with low cost, better performances, and the second object of the present invention is to provide a kind of method preparing composite titanium dioxide.
In first aspect, the invention provides a kind of composite titanium dioxide, described composite titanium dioxide obtains by illite Surface coating titanium dioxide nanoparticle, described composite titanium dioxide is prepared by the component of following ratio of weight and number: illite 60 ~ 80 parts, titanium dioxide 15 ~ 35 parts, dispersion agent 0.5 ~ 5 part.
Described dispersion agent is at least one in Sodium hexametaphosphate 99, water glass, trolamine, citric acid, oleic acid, sodium oleate in the present invention.
Preferably, in the present invention described illite is the powder of 1250 orders or more.
Preferably, in the present invention described illitic Hunter whiteness is 80 ~ 95.
Preferably, in the present invention illitic Hunter whiteness is 86 ~ 90.
Prepare a method for described illite based composite titanium white powder, comprise the steps:
(1) deposit: by the illite of 1250 orders or more, adding water and being mixed with concentration is 100 ~ 500g/L slurries, stir and add dispersion agent, then add precipitation agent and stir, add pH adjusting agent, regulate slurry pH value to be 1.0 ~ 3.0, make the composite titanium dioxide slurries of surface deposition Nano titanium dioxide; Wherein, described precipitation agent is the one in titanium sulfate, titanium tetrachloride, titanyl sulfate;
(2) washing and filtering: the composite titanium dioxide slurries obtained by deposition step carry out washing and filter, and obtain filter cake;
(3) calcine: the filter cake after the washing obtain washing and filtering step is calcined 6 ~ 10 hours under 500 ~ 800 degree, pulverizes after calcining, namely obtains illite based composite titanium white powder.
In the preparation method of illite based composite titanium white powder, described pH adjusting agent is middle strong acid or strongly-acid material and/or alkaline matter.
Preferably, the preparation method of illite based composite titanium white powder, comprises the steps:
(1) pulp: add water illite stirring, and being mixed with concentration is 100 ~ 500g/L slurries, adds dispersion agent, obtains slurries;
(2) wet method sand milling: the slurries obtained by slurry step proceed in sand mill, carries out wet method sand milling, the illite of obtained 1250 orders or more;
(3) deposit: the illite obtained by wet method sanding step, adds precipitation agent and stir, adding pH adjusting agent, regulates slurry pH value to be 1.0 ~ 3.0, makes the composite titanium dioxide slurries of surface deposition Nano titanium dioxide; Wherein, described precipitation agent is the one in titanium sulfate, titanium tetrachloride, titanyl sulfate;
(4) washing and filtering: the composite titanium dioxide slurries obtained by deposition step carry out washing and filter, and obtain filter cake;
(5) calcine: the filter cake after the washing obtain washing and filtering step is calcined 6 ~ 10 hours under 600 ~ 800 degree, pulverizes after calcining, namely obtains illite based composite titanium white powder.
Illite based composite titanium white powder provided by the invention, has following advantage:
1, cost is low, whiteness is high;
2, strong covering power, can be used as high covering power pigment and uses;
3, oil-absorption(number) is low;
4, water-soluble salt figure is low.
Embodiment
Word " exemplary " special here means " as example, embodiment or illustrative ".Here need not be interpreted as being better than or being better than other embodiment as any embodiment illustrated by " exemplary ".
In addition, in order to better the present invention is described, in embodiment hereafter, give numerous details.It will be appreciated by those skilled in the art that do not have these details, the present invention can implement equally.In other example, known method, means and material are not described in detail, so that highlight purport of the present invention.
Embodiment 1
Take the illite 60g that granularity is 1250 orders, Hunter whiteness is 86, add water 600g, is mixed with 100g/L slurries, adds the sodium hexametaphosphate solution 15g that massfraction is 20% simultaneously, and stir.Keep whipped state, add 100g/L titanium sulfate solution 210ml, regulate slurry pH value to be 1.0, make the composite titanium dioxide slurries of surface deposition Nano titanium dioxide.
Under 40-50 DEG C of condition, carrying out making beating washing with deionized water by depositing the composite titanium dioxide slurries obtained, after filtration, obtaining filter cake;
The filter cake obtained by washing and filtering is calcined 6 hours under 700 degree, pulverizes after calcining, namely obtains illite based composite titanium white powder.
Embodiment 2
Take the illite 70g that granularity is 2000 orders, Hunter whiteness is 89, add water 350g, is mixed with 200g/L slurries, adds the sodium silicate solution 1.75g that massfraction is 20% simultaneously, and stir.Keep whipped state, add 200g/L titanium tetrachloride solution 68ml, regulate slurry pH value to be 2.0, make the composite titanium dioxide slurries of surface deposition Nano titanium dioxide.
Under 40-50 DEG C of condition, carrying out making beating washing with deionized water by depositing the composite titanium dioxide slurries obtained, after filtration, obtaining filter cake;
Filter cake after the washing obtained by washing and filtering is calcined 8 hours under 800 degree, pulverizes after calcining, namely obtains illite based composite titanium white powder.
Embodiment 3
Take the illite 65g that granularity is 1500 orders, Hunter whiteness is 87, add water 130g, is mixed with 500g/L slurries, adds the sodium hexametaphosphate solution 6.5g that massfraction is 20% simultaneously, and stir.Keep whipped state, add 100g/L titanyl sulfate solution 220ml, regulate slurry pH value to be 3.0, make the composite titanium dioxide slurries of surface deposition Nano titanium dioxide.
Under 40-50 DEG C of condition, carrying out making beating washing with deionized water by depositing the composite titanium dioxide slurries obtained, after filtration, obtaining filter cake;
The filter cake obtained by washing and filtering is calcined 10 hours under 700 degree, pulverizes after calcining, namely obtains illite based composite titanium white powder.
Embodiment 4
Take the illite 70g that granularity is 1500 orders, Hunter whiteness is 88, add water 200g, is mixed with 350g/L slurries, adds the triethanolamine solution 35g that massfraction is 20% simultaneously, and stir.Keep whipped state, add 100g/L titanyl sulfate solution 140ml, regulate slurry pH value to be 3.0, make the composite titanium dioxide slurries of surface deposition Nano titanium dioxide.
Under 40-50 DEG C of condition, carrying out making beating washing with deionized water by depositing the composite titanium dioxide slurries obtained, after filtration, obtaining filter cake;
The filter cake obtained by washing and filtering is calcined 10 hours under 600 degree, pulverizes after calcining, namely obtains illite based composite titanium white powder.
Embodiment 5
Be the illite 40g of 87 by Hunter whiteness, add water 200g, is mixed with 200g/L slurries, adds the sodium hexametaphosphate solution 2g that massfraction is 20% simultaneously, and stir, obtain slurries;
Slurries pulp obtained proceed in sand mill, carry out wet method sand milling, obtained 1250 object illite slurries;
Keep whipped state, add 100g/L titanyl sulfate solution 100ml, regulate slurry pH value to be 2.0, make the composite titanium dioxide slurries of surface deposition Nano titanium dioxide.
Under 40-50 DEG C of condition, carrying out making beating washing with deionized water by depositing the composite titanium dioxide slurries obtained, after filtration, obtaining filter cake;
The filter cake obtained by washing and filtering is calcined 8 hours under 800 degree, pulverizes after calcining, namely obtains illite based composite titanium white powder.
About pH adjusting agent, the pH according to slurries selects, and can be middle strong acid or strongly-acid material and/or alkaline matter.Can be sulfuric acid, hydrochloric acid, oxalic acid, highly basic etc.
Comparative example 1
Commercially available titanium dioxide (certain sulfuric acid method titanium pigment manufacturer product domestic)
Comparative example 2
Commercially available composite titanium dioxide.
The performance index of table 1 composite titanium dioxide of the present invention and common commercially available titanium dioxide and commercially available composite titanium dioxide contrast
Can draw from upper table, the whiteness of illite based composite titanium white powder of the present invention is not less than or higher than commercially available ordinary titanium powder, commercially available composite titanium dioxide.Opacifying power is better than ordinary titanium powder, suitable with commercially available composite titanium dioxide, can be used as high covering power pigment and uses.Oil-absorption(number) is lower than commercially available composite titanium dioxide.The more commercially available common white powder of water-soluble salt, commercially available composite titanium dioxide are low, in application system, have advantage.
Composite titanium dioxide manufacturing cost provided by the invention not only lower than ordinary titanium powder, also lower than existing commercially available composite titanium dioxide.Existing composite titanium dioxide, the matrix kernel adopted has light calcium carbonate, calcium carbonate, kaolin, calcined kaolin, barite etc., these matrixes have plenty of to be needed through complex process, has plenty of matrix and causes more greatly product particle comparatively large, have plenty of cost higher.The present invention uses illite for matrix kernel.Illite is the new mineral of one of China, is common a kind of clay mineral, has rich potassium, high alumina, low iron and superior chemistry, the physicals such as smooth, bright, fine and smooth, heat-resisting.Illitic cost is very low.
Illitic whiteness own is general not high, and be 80 ~ 95, common illite whiteness is between 85 ~ 90.The present invention, when the whiteness of matrix kernel own is not high, provides a kind of composite titanium dioxide being equivalent to commercially available ordinary titanium powder, commercially available composite titanium dioxide whiteness, has good parameter and lower cost simultaneously.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; change can be expected easily or replace, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should described be as the criterion with the protection domain of claim.
Claims (6)
1. an illite based composite titanium white powder, it is characterized in that, obtain at illite Surface coating titanium dioxide nanoparticle, described composite titanium dioxide is made up of the component of following ratio of weight and number: illite 60 ~ 80 parts, titanium dioxide 15 ~ 35 parts, dispersion agent 0.5 ~ 5 part; The preparation method of described composite titanium dioxide comprises the steps:
Deposition: being added water by illite and being mixed with concentration is 100 ~ 500g/L slurries, stir and add dispersion agent, then add precipitation agent and stir, adding pH adjusting agent, regulate slurry pH value to be 1.0 ~ 3.0, make the composite titanium dioxide slurries of surface deposition Nano titanium dioxide; Wherein, described precipitation agent is the one in titanium sulfate, titanium tetrachloride, titanyl sulfate;
Washing and filtering: the composite titanium dioxide slurries obtained by deposition step carry out washing and filter, and obtain filter cake;
Calcining: filter cake washing and filtering step obtained is calcined 6 ~ 10 hours at 500 ~ 800 DEG C, pulverizes after calcining, namely obtains illite based composite titanium white powder.
2. illite based composite titanium white powder according to claim 1, is characterized in that, described dispersion agent is one or more in Sodium hexametaphosphate 99, water glass, trolamine, citric acid, oleic acid, sodium oleate.
3. illite based composite titanium white powder according to claim 1, is characterized in that, described illite is the powder of 1250 orders or more.
4. illite based composite titanium white powder according to claim 3, is characterized in that, described illitic Hunter whiteness is 80 ~ 95.
5. the illite based composite titanium white powder according to claim 3 or 4, is characterized in that, described illitic Hunter whiteness is 86 ~ 90.
6. the preparation method of illite based composite titanium white powder according to claim 1, is characterized in that, comprise the steps:
(1) pulp: add water illite stirring, and being mixed with concentration is 100 ~ 500g/L slurries, adds dispersion agent, obtains slurries;
(2) wet method sand milling: the slurries obtained by slurry step proceed in sand mill, carries out wet method sand milling, the illite of obtained 1250 orders or more;
(3) deposit: the illite obtained by wet method sanding step, adds precipitation agent and stir, adding pH adjusting agent, regulates slurry pH value to be 1.0 ~ 3.0, makes the composite titanium dioxide slurries of surface deposition Nano titanium dioxide; Wherein, described precipitation agent is the one in titanium sulfate, titanium tetrachloride, titanyl sulfate;
(4) washing and filtering: the composite titanium dioxide slurries obtained by deposition step carry out washing and filter, and obtain filter cake;
(5) calcine: the filter cake after the washing obtain washing and filtering step is calcined 6 ~ 10 hours at 600 ~ 800 DEG C, pulverizes after calcining, namely obtains illite based composite titanium white powder.
7. the preparation method of the illite based composite titanium white powder according to claim 1 or 6, is characterized in that, described pH adjusting agent is middle strong acid or strongly-acid material and/or alkaline matter.
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| CN106082320B (en) * | 2016-06-23 | 2017-07-07 | 吉林大学 | A kind of hydrothermal synthesis method of Erie's ground mass anatase compound |
| CN106189374A (en) * | 2016-07-05 | 2016-12-07 | 承德人和矿业有限责任公司 | A kind of composite granule and preparation method thereof |
| CN106280573B (en) * | 2016-08-03 | 2018-08-07 | 江苏大学 | A method of enhancing rutile type titanium white substance whiteness and brightness |
| CN109504136B (en) * | 2018-11-21 | 2020-09-18 | 延边大学 | Nano TiO (titanium dioxide)2Interior wall coating of silica complex based on illite and preparation method thereof |
| CN110564179B (en) * | 2019-08-21 | 2021-06-01 | 中国科学院过程工程研究所 | Method for preparing composite titanium dioxide by using waste silicon slag discharged in zirconium oxychloride production |
| CN111206454B (en) * | 2020-02-10 | 2022-01-25 | 成都工业学院 | Silicon-aluminum-titanium-based composite material and preparation method and application thereof |
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| GB1073338A (en) * | 1965-07-21 | 1967-06-21 | British Titan Products | Mixed coating process |
| US4416699A (en) * | 1982-01-21 | 1983-11-22 | E. I. Du Pont De Nemours & Co. | Alumina coated TiO2 |
| SE501035C2 (en) * | 1993-03-15 | 1994-10-24 | Small Particle Technology Gbg | Pigments with great light scattering ability and way of making the same |
| CN1056395C (en) * | 1998-07-03 | 2000-09-13 | 吉林大学 | Preparation of nanometer Tio/ore powder composite titanium dioxide |
| JP3600855B2 (en) * | 2001-01-31 | 2004-12-15 | 独立行政法人産業技術総合研究所 | Method for producing fine hollow glass spheres coated with titanium oxide |
| CN1464011A (en) * | 2002-06-20 | 2003-12-31 | 石家庄市友利经贸开发公司 | Process for preparing composite titanium dioxide |
| CN1724595A (en) * | 2005-07-07 | 2006-01-25 | 北京天之岩健康科技有限公司 | White minera powder TiO2 composite white pigment and its preparation method |
| CN101062475B (en) * | 2006-04-29 | 2014-04-30 | 宝山钢铁股份有限公司 | Metasilicate hole material assembled nano titanium oxide composite material and preparation method thereof |
| CN101245198B (en) * | 2008-03-13 | 2011-03-23 | 常州市美伦钛业有限公司 | Coated titanium dioxide manufacture method |
| CN101302359B (en) * | 2008-06-30 | 2011-07-20 | 攀枝花学院 | Composite titanium pigment and preparation thereof |
| JP5513777B2 (en) * | 2009-06-02 | 2014-06-04 | 奥多摩工業株式会社 | Pigment composition for paint |
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