CN1724595A - White minera powder TiO2 composite white pigment and its preparation method - Google Patents
White minera powder TiO2 composite white pigment and its preparation method Download PDFInfo
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Abstract
The invention supplies a method to manufacture compound white dyestuff that has the characteristic of titanium dioxide dyestuff. It uses white mineral powder as covering center basal material, and uses TiO2 as covering material. In the grinding system of waterproof superfine, by using the method of grain to grain covering and modifying, the white mineral dyestuff-TiO2 compound white dyestuff that has the characteristic of titanium dioxide dyestuff would be made. The invention has the advantages of simple technology, low cost, and so on. It could improve the capability of the product and reduce the cost.
Description
Technical field the present invention relates to the production technical field of composite white pigment, specifically, relates to white mineral powder-TiO
2The preparation method of composite white pigment.
Background technology titanium dioxide (being pigmentary titanium dioxide) is people's color superfine white pigment of generally acknowledging up to now, it has good opacifying power, tinting strength, photostabilization and chemical stability, be widely used in industrial sectors such as coating, papermaking, chemical industry, pottery and building material, become important chemical material in the development of the national economy.In the last few years, because of the construction industry of factors such as Economic development, social progress and people's living standard raising drive and the fast development of relevant paint industry, the demand of white pigment titanium dioxide was grown with each passing day.And on the other hand, the shortage day by day of world's high-quality titanium resource, the resources processing process complications, the environmental protection requirement strictness, these all cause the titanium white production cost to increase, and price raises up.The problems referred to above constantly increase the weight of titanium white consumption industry such as coating burden, and therefore industry development is restricted.
Adopting the compound technology of preparing preparation composite product similar and with low cost to the titanium white performance of inorganic materials is to solve in-problem effective way in titanium white production and the consumption.By inorganic surfaces coating modification mode, coat TiO at inorganic material surfaces such as non-metallic mineralss
2Layer and form composite white pigment and receive concern both domestic and external always with TiO 2 pigment character, though relevant technical study has obtained certain achievement, but also there is more problem in aspects such as preparation method, product performance and utilisation technology, mainly show as:
1. adopt simple hybrid mode to prepare composite product.This method TiO
2Coat relatively poor, so the composite product part character of simple analog titanium dioxide within the specific limits can't satisfy bulk users' such as coating requirement.The SiO that makes as Japan
2Composite titanium dioxide pigment is mainly used in the synthon goods, and the talcum base composite titanium dioxide of Britain and France only part is used for paper industry etc.And they are to be applied in the mode that low ratio substitutes titanium white, and its effect that reduces the application product cost is very limited.
2. prepare composite product with inorganic precipitation reaction-thermal treatment crystallization process.The hydrated titanium dioxide that the titanium salt hydrolysis is generated precipitates the non-metallic minerals particle surface that is coated on as matrix, and the mode by roasting makes titanium dioxide crystalization then, forms the composite pigment that the surface has the crystal titanium dioxide modified layer.The problem that this method exists mainly contains: the inducing action of mineral substance bag nuclear matrix causes the hydrated titanium dioxide throw out to be difficult to generate rutile titanium dioxide by follow-up crystallization; Be subjected to the restriction of hydrolytic process titanium salt concentration and solid content, coat TiO
2Amount and degree of uniformity are restricted, and the pigment performance of product does not generally reach requirement; The removal of impurity such as titanium salt hydrolysis and iron ion produces a large amount of acid waste waters, contaminate environment.
3. dry method grain-grain coating modification mode is made the titanium white surrogate.This method bag nuclear matrix and TiO
2Degree of scatter relatively poor, what lack the firmly effect that produces between matrix and the titanium white excites external force and binding groups, the mixture pigment performance is limited and unstable.Summary of the invention the purpose of this invention is to provide a kind of with the firm crystallization TiO that coats in solid bag nuclear composition granule surface
2Particle is feature, have pigmentary titanium dioxide character and composite white pigment with low cost.
The present invention has realized crystallization TiO in the composite pigment by following measure
2Particle coats firmly and uniformly on solid bag nuclear composition granule surface:
(1) adopt the wet ultra-fine grinding method will be as the solid particulate of bag nuclear thing with as the crystallization TiO of coating thing
2Particle is refined to the size range that both are complementary respectively, i.e. bag nuclear composition granule diameter: TiO
2Particle diameter is about 5-8: 1;
(2) make solid bag nuclear composition granule produce the mechanical force activating effect by extra-fine grinding, promote itself and TiO with this
2Between reaction bonded;
(3) solid bag nuclear composition granule and TiO
2Each self-forming surface functional group in reaction system is realized the alternate reaction of two particulate by the chemical bonding between functional group;
The composite pigment of the present invention's preparation is because of particle surface TiO
2Strong dissemination that the high refractive index of coating layer, heterogeneous particulate material cause and high scattering process, and wrap up the strong covering effect that more air dielectric causes when forming coating and have the pigment property of similar titanium dioxide.
The composite pigment of the present invention's preparation is owing to wherein only contain part TiO
2, and solid bag nuclear thing is cheap powder body material, so its cost is compared with titanium dioxide and is greatly diminished.
The final white mineral powder-TiO that forms of the present invention
2The composition of composite white pigment with consist of: white mineral powder (lime carbonate or kaolin, or calcined kaolin, or barite) 50%-80%, crystallization TiO
2(anatase titanium dioxide or rutile-type) 20%-50%.
Realize white mineral powder-TiO of the present invention
2The concrete preparation method of composite white pigment is:
Raw material selection:
1. white mineral powder (lime carbonate or kaolin, or calcined kaolin, or barite), powder fineness 200-400 order, mineral purity is greater than 98%;
2. anatase titanium dioxide or Rutile type Titanium Dioxide industrial goods (crystallization TiO
2), whiteness is greater than 95%;
3. Sodium hexametaphosphate 99 (the above rank of technical pure) is mixed with the aqueous solution with deionized water, and strength of solution 20% is added use as grinding aid when the fine grinding of white mineral powder wet method;
4. service water glass (modulus 3) is mixed with the aqueous solution with deionized water, and strength of solution 10% is at homogenizing TiO
2Grind with superfine white mineral mixture slurry, be i.e. add use as wedding agent in the process that the two realization response coats;
The concrete steps of principle production process are:
1, presses white mineral powder (lime carbonate or kaolin, or calcined kaolin, or barite) forms the requirement of solid content 50%～70% in the suspensoid with water, take by weighing white mineral powder, water and account for the Sodium hexametaphosphate 99 of dry powder amount 0.5%-1.2%, place wet type to stir in the extra-fine grinding system of mill, stir to make by stirrer and treat the extra-fine grinding slurry with high-speed stirring effect;
2, by crystallization TiO
2(anatase titanium dioxide or rutile-type) and water form the requirement of solid content 50%～70% in the suspensoid, take by weighing TiO
2, water and account for the Sodium hexametaphosphate 99 of dry powder amount 1%-2%, place in the stirrer with high-speed stirring effect and stir, make slurry;
3, start the extra-fine grinding system that wet type stirs mill, the slurry that white mineral powder and water are made carries out grinding operation, makes levigate product granularity be less than 2 μ m content 60%～85%;
4. with superfine white mineral slurry and TiO
2Slurry mixes, and both blending ratios (dry powder weight) are pressed TiO
2/ (white mineral+TiO
2The requirement of)=20%-50% is determined, adds the water glass that accounts for dry powder amount 0.5%-1.5% then and carries out high-speed stirring together to realize the homogenizing of mixture slurry;
5, start the extra-fine grinding system that wet type stirs mill, to the TiO of homogenizing
2Slurry and superfine white mineral mixture slurry carry out grinding operation, make levigate product granularity be less than 2 μ m content 80%～92%, and importing has in the stirred pot of medium stirring intensity;
6, to superfine Ti O is housed
2With add water in the stirred pot of superfine white mineral mixture slurry, make it be diluted to solid content 20%-35%, and stir.Use the ultra-fine hydroclassifier of GSDF-10 (Φ 10) type that it is carried out classification then, make the classification overflow granularity be less than 2 μ m content 92%～94%.
7, utilize whizzer or vacuum filter that the classification overflow is filtered and form filter cake;
8, filter cake is placed the drying machine of 90 ℃-120 ℃ of temperature be dried to moisture below 3%;
9, dried material is sent in the beater handled, make it to form even-grained powder;
Embodiment
Embodiment 1:
1. calcined kaolin powder (300 order) 400kg, deionized water 400kg are placed wet type to stir in the extra-fine grinding system of mill, stir 10min by stirrer with high-speed stirring effect, add the solution (strength of solution 20% that contains the 4kg Sodium hexametaphosphate 99 then, add this solution 20kg), restir 30min makes and treats the extra-fine grinding slurry;
2. start the extra-fine grinding system that wet type stirs mill, the slurry of calcined kaolin powder and water being made according to the circulation grinding mode grinds and makes levigate product granularity be less than 2 μ m content 70%;
3. with crystallization TiO
2(Rutile type Titanium Dioxide) 133kg, deionized water 133kg place and stir 10min in the stirred pot with high-speed stirring effect, add the solution (strength of solution 20% adds this solution 10kg) that contains the 2kg Sodium hexametaphosphate 99 then, and restir 30min makes slurry;
4. with the levigate slurry 300kg of calcined kaolin, TiO
2The water glass solution 20kg of slurry 100kg, concentration 10% mixes, and high-speed stirring 40min is to realize the homogenizing of mixture slurry;
5. start the extra-fine grinding system that wet type stirs mill, according to the circulation grinding mode to the TiO of homogenizing
2Slurry and superfine calcined kaolin mixture slurry carry out grinding operation, make levigate product granularity be less than 2 μ m content 90%, and importing has in the stirred pot of medium stirring intensity;
6. to superfine Ti O is housed
2With add water 408kg in the stirred pot of superfine white mineral mixture slurry 350kg, and stir.Use the ultra-fine hydroclassifier of GSDF-10 (Φ 10) type that it is carried out classification then, make the classification overflow granularity be less than 2 μ m content 93%.
7, utilize Φ 800 type tripod pendulum type batch centrifugals that the classification overflow is filtered and form filter cake;
8, filter cake is placed the drying machine of 90 ℃-120 ℃ of temperature be dried to moisture below 3%;
9, dried material is sent in the beater handled, make it to form even-grained powder;
Embodiment 2:
1. calcined kaolin powder (300 order) 400kg, deionized water 400kg are placed wet type to stir in the extra-fine grinding system of mill, stir 10min by stirrer with high-speed stirring effect, add the solution (strength of solution 20% that contains the 4kg Sodium hexametaphosphate 99 then, add this solution 20kg), restir 30min makes and treats the extra-fine grinding slurry;
2. start the extra-fine grinding system that wet type stirs mill, the slurry of calcined kaolin powder and water being made according to the circulation grinding mode grinds and makes levigate product granularity be less than 2 μ m content 70%;
3. with crystallization TiO
2(anatase thpe white powder) 133kg, deionized water 133kg place and stir 10min in the stirred pot with high-speed stirring effect, add the solution (strength of solution 20% adds this solution 10kg) that contains the 2kg Sodium hexametaphosphate 99 then, and restir 30min makes slurry;
4. with calcined kaolin slurry 300kg, TiO
2The water glass solution 20kg of slurry 100kg, concentration 10% mixes, and high-speed stirring 40min is to realize the homogenizing of mixture slurry;
5. start the extra-fine grinding system that wet type stirs mill, according to the circulation grinding mode to the TiO of homogenizing
2Slurry and superfine calcined kaolin mixture slurry carry out grinding operation, make levigate product granularity be less than 2 μ m content 90%, and importing has in the stirred pot of medium stirring intensity;
6. to superfine Ti O is housed
2With add water 408kg in the stirred pot of superfine white mineral mixture slurry 350kg, and stir.Use the ultra-fine hydroclassifier of GSDF-10 (Φ 10) type that it is carried out classification then, make the classification overflow granularity be less than 2 μ m content 93%.
7, utilize Φ 800 type tripod pendulum type batch centrifugals that the classification overflow is filtered and form filter cake;
8, filter cake is placed the drying machine of 90 ℃-120 ℃ of temperature be dried to moisture below 3%;
9, dried material is sent in the beater handled, make it to form even-grained powder;
Two kinds of white mineral powder-TiO that make respectively by embodiment 1 and embodiment 2
2The performance of composite white pigment is listed in table 1, the performance of the internal wall emulsion coating of the composite white pigment preparation made from embodiment 2 and list in table 2 with the contrast of titanium dioxide.The result shows white mineral powder-TiO
2Composite white pigment has the pigment performance similar with titanium dioxide.
White mineral powder-TiO
2The performance table 1 of composite white pigment
| Sequence number | Project | Index | |
| Embodiment 1 product | Embodiment 2 products | ||
| 1 | TiO 2Content, % | 25 | 25 |
| 2 | Granularity is less than 2 μ m content, % | 95.63 | 94.57 |
| 3 | Whiteness, % | 96 | 94.6 |
| 4 | Density, g/m 3 | 3.2 | 3.0 |
| 5 | The slurry contrast ratio, % | 99.67 | 98.89％ |
| 6 | Opacifying power, g/m 2 | 22.4 | 22.8 |
| 7 | Oil number, g/100g | 27.5 | 28.5 |
| 8 | 105 ℃ of volatile matters, % | 0.05 | 0.05％ |
| 9 | The aqeous suspension pH value | 8.9 | 8.8 |
| 10 | Screenings (45 μ m sieve aperture), % | 0 | 0 |
Composite white pigment (embodiment 2) and anatase thpe white powder prepare interior wall coating performance test results table 2
| Sequence number | Test item | Detected result | GB GB/T9756-2001 requires (salable product) | The comparative evaluation | |
| Composite white pigment | Anatase thpe white powder | ||||
| 1 | Condition in container | No lump is uniform state after the stirring | No lump is uniform state after the stirring | No lump is uniform state after the stirring | Meet |
| 2 | Application property | It is accessible to brush two roads | It is accessible to brush two roads | It is accessible to brush two roads | Meet |
| 3 | Low-temperature stability | Never degenerate | Never degenerate | Never degenerate | Meet |
| 4 | Time of drying (surface drying), h | 1 | 1 | ≤2 | Meet |
| 5 | Appearance of film | Normally | Normally | Normally | Meet |
| 6 | Contrast ratio (white or light color) | 0.91 | 0.92 | ≥0.90 | Meet |
| 7 | Alkali resistance | 24h is no abnormal | 24h is no abnormal | 24h is no abnormal | Meet |
| 8 | Abrasion resistance, inferior | ≥200 | ≥200 | ≥200 | Meet |
Claims (3)
1. white mineral powder-TiO
2Composite white pigment is characterized in that: with white mineral powders such as lime carbonate, kaolin, calcined kaolin and barites is bag nuclear matrix, crystallization TiO
2(anatase titanium dioxide and rutile-type) is the coating thing, adopts white mineral powder wet ultra-fine grinding and white mineral powder and crystallization TiO
2Approach is ground in the wet method blend, and the modes such as grain-grain coating modification reaction that refinement, surface hydroxylation transformation and Mechanochemical Effect cause of cutting apart by solid particulate are prepared from.
White mineral powder-TiO
2The fineness of composite white pigment is less than 2 μ m content 90%～94%, and each component ratio of components by weight is: white mineral powder (lime carbonate or kaolin, or calcined kaolin, or barite) 50%-80%, crystallization TiO
2(anatase titanium dioxide or rutile-type) 20%-50%.
2. white mineral powder-TiO
2Composite white pigment, its preparation technology and method feature are:
A, press white mineral powder (lime carbonate or kaolin, or calcined kaolin, or barite) forms the requirement of solid content 50%～70% in the suspensoid with water, take by weighing white mineral powder, water and account for the Sodium hexametaphosphate 99 of dry powder amount 0.5%-1.2%, place wet type to stir in the extra-fine grinding system of mill, stir to make by stirrer and treat the extra-fine grinding slurry with high-speed stirring effect;
B, by crystallization TiO
2(anatase titanium dioxide or rutile-type) and water form the requirement of solid content 50%～70% in the suspensoid, take by weighing TiO
2, water and account for the Sodium hexametaphosphate 99 of dry powder amount 1%-2%, place in the stirrer with high-speed stirring effect and stir, make slurry;
C, start the extra-fine grinding system that wet type stirs mill, the slurry that white mineral powder and water are made carries out grinding operation, makes levigate product granularity be less than 2 μ m content 60%～85%, and with itself and TiO
2Slurry mixes stirring, and both blending ratios (dry powder weight) are pressed TiO
2/ (white mineral+TiO
2The requirement of)=20%-50% is determined.Add the water glass that accounts for dry powder amount 0.5%-1.5% simultaneously, then mixture slurry is stirred homogenizing;
D, start the extra-fine grinding system that wet type stirs mill, to the TiO of homogenizing
2Slurry and superfine white mineral mixture slurry carry out grinding operation, make levigate product granularity be less than 2 μ m content 80%～92%, and importing has in the stirred pot of medium stirring intensity;
E, to superfine Ti O is housed
2With add water in the stirred pot of superfine white mineral mixture slurry, make it be diluted to solid content 20%-35%, and stir.Use the ultra-fine hydroclassifier of GSDF-10 (Ф 10) type that it is carried out classification then, make the classification overflow granularity be less than 2 μ m content 92%～94%.
F, utilize whizzer or vacuum filter that the classification overflow is filtered to form filter cake;
G, place the drying machine of 90 ℃-120 ℃ of temperature to be dried to moisture below 3% filter cake;
H, dried material sent in the beater handle, make it to form even-grained powder.
3. white mineral powder-TiO according to claim 2
2The preparation technology of composite white pigment and method are characterised in that:
A, the requirement that accounts for white mineral powder 1% by white mineral powder/(white mineral powder+water)=65%, Sodium hexametaphosphate 99, in wet type stirred the extra-fine grinding system of mill, the stirrer by the high-speed stirring effect stirs to make by what white mineral powder, water and Sodium hexametaphosphate 99 formed treated the extra-fine grinding slurry.The white mineral powder is meant lime carbonate or kaolin, or calcined kaolin, or barite;
B, by crystallization TiO
2(anatase titanium dioxide or rutile-type) and water form the requirement of solid content 65% in the suspensoid, take by weighing TiO
2, water and account for the Sodium hexametaphosphate 99 of dry powder amount 1.5%, place in the stirrer with high-speed stirring effect and stir, make slurry;
C, start the extra-fine grinding system that wet type stirs mill, the slurry that white mineral powder and water are made carries out grinding operation, makes levigate product granularity be less than 2 μ m content 70%, then with itself and TiO
2Slurry is pressed TiO
2/ (white mineral+TiO
2The requirement that)=35%, adding simultaneously account for the water glass of dry powder amount 1.2% mixes homogenizing;
D, utilize wet type to stir the extra-fine grinding system of mill, to the TiO of homogenizing
2Grind with superfine white mineral mixture slurry and make levigate product granularity be less than 2 μ m content 90%;
E, add water to superfine Ti O
2Be diluted to solid content 30% with superfine white mineral mixture slurry, dispersed with stirring evenly back is carried out classification with the ultra-fine hydroclassifier of GSDF-10 (Φ 10) type, makes the classification overflow granularity be less than 2 μ m content 92%;
F, utilize whizzer or vacuum filter that the classification overflow is filtered to form filter cake;
G, to place the drying machine of 100 ℃ of temperature to be dried to filter cake moisture below 3%;
H, dried material sent in the beater handle, make it to form even-grained powder.
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| CN102260422B (en) * | 2010-05-25 | 2014-04-02 | 中国地质大学（北京） | Method for preparing TiO2/powdered quartz composite powder material |
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| CN105754378A (en) * | 2016-03-23 | 2016-07-13 | 南召鑫泰钙业有限公司 | Calcium-based titanium dioxide and preparation process thereof |
| CN105754378B (en) * | 2016-03-23 | 2018-11-09 | 河南鑫泰钙业有限公司 | A kind of calcium base titanium dioxide and its preparation process |
| CN106479247A (en) * | 2016-08-18 | 2017-03-08 | 徐英豪 | The application on coating of barium sulfate and titanium white compound powder |
| CN106479247B (en) * | 2016-08-18 | 2018-09-14 | 西藏亚吐克工贸有限公司 | The application of barium sulfate and titanium white compound powder on coating |
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| CN106542573A (en) * | 2016-10-17 | 2017-03-29 | 中国科学院过程工程研究所 | A kind of method for preparing pigmentary titanium dioxide |
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| CN106590062A (en) * | 2016-12-06 | 2017-04-26 | 大连环球矿产股份有限公司 | Preparation method of composite titanium dioxide pigment with wollastonite coated with titanium dioxide |
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| CN108003661A (en) * | 2017-11-28 | 2018-05-08 | 广西雅照钛白有限公司 | A kind of composite titanium dioxide |
| CN109679379A (en) * | 2018-12-12 | 2019-04-26 | 东升新材料（山东）有限公司 | A kind of black composite pigment and preparation method thereof |
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| CN112592606A (en) * | 2020-09-14 | 2021-04-02 | 沈阳化工大学 | Preparation method of barite/TiO 2 composite material |
| CN113248942A (en) * | 2021-03-12 | 2021-08-13 | 吉林大学 | Nano TiO for improving paper performance2Preparation method and application of opal compound |
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| CN113234255B (en) * | 2021-05-07 | 2022-12-02 | 江苏群鑫粉体科技股份有限公司 | Ultraviolet screening agent and preparation method and application thereof |
| CN113105784A (en) * | 2021-05-10 | 2021-07-13 | 华东理工大学 | Method for producing pigment for coating from papermaking white mud |
| CN114410130A (en) * | 2021-11-23 | 2022-04-29 | 江西广源化工有限责任公司 | Modified wollastonite and preparation method and application thereof |
| CN115819003A (en) * | 2022-12-29 | 2023-03-21 | 湖南蒙源精细化工有限公司 | Core titanium dioxide and preparation method thereof |
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