CN100365207C - Composite titania material and its prepn and application - Google Patents
Composite titania material and its prepn and application Download PDFInfo
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- CN100365207C CN100365207C CNB2006100239639A CN200610023963A CN100365207C CN 100365207 C CN100365207 C CN 100365207C CN B2006100239639 A CNB2006100239639 A CN B2006100239639A CN 200610023963 A CN200610023963 A CN 200610023963A CN 100365207 C CN100365207 C CN 100365207C
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- carrier
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- titanium dioxide
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 133
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims description 32
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 48
- 239000011248 coating agent Substances 0.000 claims abstract description 16
- 238000000576 coating method Methods 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims description 124
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 49
- 239000007787 solid Substances 0.000 claims description 32
- 239000000203 mixture Substances 0.000 claims description 29
- 239000012065 filter cake Substances 0.000 claims description 25
- 238000001914 filtration Methods 0.000 claims description 24
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 23
- 238000010009 beating Methods 0.000 claims description 23
- 229910052726 zirconium Inorganic materials 0.000 claims description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 22
- 229910052710 silicon Inorganic materials 0.000 claims description 22
- 239000010703 silicon Substances 0.000 claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 16
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000004411 aluminium Substances 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 239000000945 filler Substances 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 8
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 7
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 6
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 5
- 239000005995 Aluminium silicate Substances 0.000 claims description 4
- 241000276489 Merlangius merlangus Species 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 235000012211 aluminium silicate Nutrition 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 4
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 4
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 4
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 4
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 claims description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- 229960000892 attapulgite Drugs 0.000 claims description 3
- 239000000440 bentonite Substances 0.000 claims description 3
- 229910000278 bentonite Inorganic materials 0.000 claims description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- 229940043237 diethanolamine Drugs 0.000 claims description 3
- 239000010445 mica Substances 0.000 claims description 3
- 229910052618 mica group Inorganic materials 0.000 claims description 3
- 229910052625 palygorskite Inorganic materials 0.000 claims description 3
- 229940088417 precipitated calcium carbonate Drugs 0.000 claims description 3
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 3
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 3
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 3
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 2
- CENHPXAQKISCGD-UHFFFAOYSA-N trioxathietane 4,4-dioxide Chemical compound O=S1(=O)OOO1 CENHPXAQKISCGD-UHFFFAOYSA-N 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000007796 conventional method Methods 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000011247 coating layer Substances 0.000 abstract 9
- 239000002344 surface layer Substances 0.000 abstract 2
- 238000011049 filling Methods 0.000 abstract 1
- 238000002955 isolation Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 abstract 1
- 239000002346 layers by function Substances 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 39
- 239000008367 deionised water Substances 0.000 description 38
- 229910021641 deionized water Inorganic materials 0.000 description 38
- 235000019353 potassium silicate Nutrition 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 229910000989 Alclad Inorganic materials 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 229920001131 Pulp (paper) Polymers 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 238000005253 cladding Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- SMYKVLBUSSNXMV-UHFFFAOYSA-K aluminum;trihydroxide;hydrate Chemical compound O.[OH-].[OH-].[OH-].[Al+3] SMYKVLBUSSNXMV-UHFFFAOYSA-K 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Abstract
The present invention discloses titanium dioxide composite material and a preparation method thereof and an application thereof. The core of the titanium dioxide composite material is a granular carrier; the outside of the carrier is a first coating layer; the outside of the first coating layer is coated with a second coating layer; the outside of the second coating layer can be coated with a third coating layer or can not be coated with the third coating layer. The first coating layer is a dense isolation layer for preventing that impurity elements in the carrier can not migrate into titanium dioxide lattices at a surface layer in a calcination process, so the perfection of the titanium dioxide lattices is guaranteed; the second coating layer is a functional layer with the component of titanium dioxide, and the high whiteness and the high refractive index of the titanium dioxide are used; the third coating layer has the functions of passivating the titanium dioxide at the surface layer, eliminating the photocatalysis of the titanium dioxide and increasing the weatherability and the surface gloss of the titanium dioxide. The titanium dioxide composite material of the present invention is mainly used for filling and coating paper; the added weight of the titanium dioxide composite material is far lower than that of titanium dioxide prepared by the conventional method, so the production cost is greatly reduced.
Description
Technical field
The present invention relates to a kind of composite titania material and technology of preparing thereof, specifically, is a kind of composite that is used for the inorganic powder material surface cladding titanium dioxide of papermaking filler and coating pigment, and the technology for preparing this material.
Background technology
In recent years, the development of digital printed technology, office automation and personal computer, to propose to upgrade with paper, higher requirement, the annual requirement of paper plays crucial effect just with double-digit speed increment in the development of the national economy.Influence the paper product quality except the paper pulp fiber quality, a filler and the face coat that very important factor is a paper.It requires paper that certain glossiness, smoothness and printing adaptability are arranged.Therefore, the filler of paper and coating pigment play very crucial effect.
In paper industry, for the output that reduces waste material with reduce cost of transportation, tend to reduce the weight of paper.The reduction of paper weight can weigh, make the paper thinning by reduction or reduce the amount of filler of mixing and reach.But can cause the opacity of paper to descend like this.In order to increase opacity, need to add various fillers or dispose special coating.
The material that is used as the paper industry filler also comprises: kaolin, talcum powder, titanium dioxide, silica or the like except that powdered whiting and precipitated calcium carbonate.These materials have different characteristics, according to the desired quality of papermaking, can be used alone or as a mixture.Wherein, titanium dioxide has the highest refractive index, is the most effective for the opacity that increases paper.
Using under the situation of titanium dioxide as filler or coated paper, flocculation can take place and cause TiO 2 particles skewness in the paper in TiO 2 particles, and the effect of the increase opacity that titanium dioxide is intrinsic can not demonstrate fully.Therefore, when titanium dioxide is the flocculation attitude, in order to obtain desirable opacity, the consumption of titanium dioxide must strengthen, because titanium dioxide is compared the price height with other pigment and than great, is caused cost to rise so on the one hand with filler, also opposing with the lighting of paper on the one hand.So, reach desired opacity by the titanium dioxide that uses minimum.In addition, trickle TiO 2 particles is difficult for attached on the paper pulp fiber, and part can be lost in the waste water of paper machine, and productive rate is reduced.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of composite titania material and its production and application, to overcome the above-mentioned defective that prior art exists, satisfy the needs of field of papermaking.
Composite titania material of the present invention comprises graininess core as carrier, is coated on first clad of carrier outside and is coated on the second outer clad of first clad;
Said carrier is selected from one or more the mixture in talcum powder, kaolin, precipitated calcium carbonate, powdered whiting, mica, white carbon black, bentonite or the attapulgite;
The material of said first clad comprises one or more the mixture in silica, hydrated SiO 2, aluminium oxide, hydrated alumina, zirconia or the hydrous zirconium oxide(HZO);
The material of said second clad comprises one or more the mixture in titanium dioxide or the hydrated titanium dioxide;
The average grain diameter 0.3-2.0 μ m of said carrier;
The weight of first clad is the 0.1-25% (wt) of vehicle weight, and the weight of second clad is the 0.1-20% (wt) of vehicle weight;
According to the preferred scheme of the present invention, be coated with the 3rd clad at second clad, the 3rd layer material comprises one or more the mixture in silica, hydrated SiO 2, aluminium oxide, hydrated alumina, zirconia or the hydrous zirconium oxide(HZO);
The weight of described the 3rd clad is the 0.1-20% (wt) of vehicle weight;
Prepare the method for composite titania material of the present invention, comprise the steps:
(1) mixture of carrier, water and dispersant is pulled an oar together, the weight concentration of carrier is 30-80% during making beating, and the addition of dispersant is the 0.1-10% of carrier dry weight, obtains the carrier slurry;
(2) thin up to solid content is 50g/L-250g/L then, be heated to 60～95 ℃, silicon source and/or aluminium source and/or zirconium source are joined in the carrier slurry, add acid or alkali in the time of adding, the pH value of the hierarchy of control is 2-11, and silicon source and/or aluminium source and/or zirconium source are deposited on the carrier.Coat two kinds or when above, the addition sequence in silicon source, aluminium source, zirconium source is simultaneously: when coating silicon source, aluminium source, bag silicon source, alclad source more earlier; When coating silicon source, zirconium source, the zirconium source is wrapped in bag silicon source more earlier; When metallized aluminum source, zirconium source, the zirconium source is wrapped in first alclad source again; When coating silicon source, aluminium source, zirconium source, wrap the silicon source earlier, the zirconium source is wrapped in the alclad source more then.Slurries filtration, filter cake are dry under 90～150 ℃, obtain to be coated with the carrier of first clad;
(3) carrier and the dispersant that will be coated with first clad pulled an oar with the mixture of water, the weight concentration that is coated with the carrier of first clad is 30-80%, the addition of dispersant is for coating the 0.1-5% of back carrier dry weight, be diluted with water to solid content 50g/L-200g/L, under 40～95 ℃ temperature, be 10-500g TiO with concentration
2The aqueous solution in the titanium source of/L and weight concentration are that the aqueous alkali of 5-50% joins in the slurry, the pH value of the hierarchy of control is 6-11, slurries filtration, filter cake is dry down at 90～150 ℃, dried material obtains to be coated with the carrier of second clad 500--1000 ℃ temperature lower calcination 0.5-10 hour;
(4) further, the mixture that is coated with carrier, dispersant and the water of second layer clad is pulled an oar together, the weight concentration that is coated with the carrier of the second layer clad during making beating is 30-80%, the addition of dispersant is the 0.1-8% of weight that is coated with the carrier of second layer clad, be diluted with water to solid content 50g/L-250g/L then, under 60--95 ℃ temperature, add silicon source and/or aluminium source and/or zirconium source, add acid or alkali when adding, the pH value of the hierarchy of control is 2-11, and silicon source and/or aluminium source and/or zirconium source are deposited on the carrier.Coat two kinds or when above, the addition sequence in silicon source, aluminium source, zirconium source is simultaneously: when coating silicon source, aluminium source, bag silicon source, alclad source more earlier; When coating silicon source, zirconium source, the zirconium source is wrapped in bag silicon source more earlier; When metallized aluminum source, zirconium source, the zirconium source is wrapped in first alclad source again; When coating silicon source, aluminium source, zirconium source, wrap the silicon source earlier, the zirconium source is wrapped in the alclad source more then.Filter then, filter cake is dry under 90--150 ℃ temperature, obtains to be coated with the carrier of the 3rd clad;
Described dispersant is one or more the mixture in Sodium Polyacrylate, calgon, sodium pyrophosphate, sodium polyphosphate, triethanolamine or the diethanol amine;
Described silicon source is one or more the mixture in sodium metasilicate, waterglass, Ludox or the ethyl orthosilicate;
Described aluminium source is one or more the mixture in aluminium chloride, aluminum sulfate, sodium aluminate or the aluminium isopropoxide;
Described zirconium source is one or more the mixture in zirconium oxychloride, zirconium sulfate or the zirconium oxysulfate;
Described titanium source is one or more the mixture in titanyl sulfate, titanium sulfate, titanium tetrachloride, tetrabutyl titanate or the isopropyl titanate;
Described acid is one or more the mixture in sulfuric acid, hydrochloric acid, nitric acid or the acetic acid;
Described alkali is one or more the mixture in NaOH, sodium carbonate, sodium bicarbonate, potassium hydroxide or the ammoniacal liquor.
The inventor finds that at the carrier surface cladding titanium dioxide, the product of coating must just can make the crystal formation of titanium dioxide grow more completely through calcining, could bring into play the opacity that the titanium dioxide high index of refraction is embodied better like this.But titanium dioxide directly is coated on carrier surface, and in calcination process, the impurity element in the carrier can be moved in the titanium dioxide lattice on top layer, causes titanium dioxide to produce lattice defect, and loses original whiteness and gloss.Because of titanium dioxide to impurity element sensitivity very, a spot of impurity will make the titanium dioxide flavescence or become ash, surpasses 100ppm as the rutile titanium dioxide iron-holder, will obviously turn to be yellow.So before the cladding titanium dioxide layer, necessary in carrier surface coating one deck compact isolating layer, impurity element in the carrier can not be moved in calcination process in the titanium dioxide lattice on top layer, thereby guarantee the titanium dioxide perfection of lattice, make titanium dioxide bring into play its original high whiteness and high index of refraction.
Titanium dioxide has stronger photocatalytic again in addition, can be under ultraviolet irradiation, produce electron-hole pair, thus to around the matrix organic matter produce photocatalytic Degradation, cause the matrix variable color, become fragile, intensity decreases.Concerning paper, can cause the paper flavescence, tarnish.To the less demanding paper of weatherability, the titanium dioxide that can use surperficial unpassivated to handle, but, must carry out Passivation Treatment to top layer titanium dioxide to the paper that weatherability is had relatively high expectations.The method of passivation is to coat one deck compact isolating layer again at titanium dioxide surface, this layer compact isolating layer is first coated silica, silica outside coated aluminum oxide also has in the outside of aluminium oxide to coat zirconia again, with its weatherability of further raising and lustrous surface.
Adopt the composite titania material of method for preparing, can be used as papermaking filler, using method is identical with conventional titanium dioxide, but it adds weight and is generally 5～10% of paper weight, be significantly less than the titanium dioxide of conventional method preparation, thereby greatly reduce production cost, make paper obtain whiteness and opacity preferably simultaneously.
Below the invention will be further described and provide embodiment.Embodiment only is better explanation the present invention, does not limit the present invention.
The specific embodiment
Among the embodiment, adopt standard GB/T 5950-1996 to measure the whiteness of material; Measure the reducing power of material according to standard GB 5211.16-88.
Embodiment 1
In average grain diameter is to add the 150g deionized water in the 100g talcum powder of 0.3 μ m, adds the making beating of 0.5g Sodium Polyacrylate simultaneously; Adding deionized water, to be diluted to solid content be 100g/L, and slurry is heated to 80 ℃, is that 10% aqueous hydrochloric acid solution adds in the slurry with the waterglass of 20g and weight concentration, and the control pH value of slurry is 9, until dripping.Keep the temperature-resistant of slurry, with 30g aluminum sulfate (Al
2(SO
4)
318H
2O) and 15% NaOH add in the slurry, until dripping.With slurries filtration, filter cake descended dry 3 hours at 120 ℃, obtained powder 98g;
Pull an oar coating first 98g powder and the 150g deionized water of protecting coating, add the 0.2g calgon simultaneously, add deionized water and be diluted to solid content 70g/L, slurry is heated to 85 ℃, is that 200g/L titanyl sulfate and weight concentration are that 15% the NaOH aqueous solution adds in the slurry with the 50ml solid content, and the control pH value of slurry is 11, with slurries filtration, filter cake 105 ℃ dry 3 hours down, then in muffle furnace in 870 ℃ of calcinings 3 hours, obtain powder 101g;
The 101g powder and the making beating of 120g deionized water of titanium dioxide will have been coated, add the 0.3g triethanolamine simultaneously, add deionized water and be diluted to solid content 150g/L, slurry is heated to 82 ℃, with the waterglass of 15g and weight concentration is that 10% aqueous hydrochloric acid solution adds in the slurry, the control pH value of slurry is 11, keeps the temperature-resistant of slurry, with 25g alchlor (AlCl
36H
2O) and weight concentration be that 15% the NaOH aqueous solution adds in the slurry, is the control pH value of slurry? keep the temperature-resistant of slurry, with control pH value of slurry in the NaOH adding slurry of 15g zirconium oxychloride and 15% is 2, with slurries filtration, filter cake descended dry 5 hours at 125 ℃, obtained powder 103g.
Record powder whiteness 95.1, reducing power 72.
Embodiment 2
In the 100g kaolin of average grain diameter 0.8 μ m, add the 120g deionized water, add the making beating of 0.4g Sodium Polyacrylate simultaneously, add deionized water and be diluted to solid content 100g/L, slurry is heated to 80 ℃, with the waterglass of 25g and weight concentration is that 10% aqueous sulfuric acid adds in the slurry, the control pH value of slurry is 8.5, until dripping.Keep the temperature-resistant of slurry, with 25g aluminum sulfate (Al
2(SO
4)
318H
2O) and weight concentration be that the aqueous solution of 15% KOH adds in the slurry, the control pH value of slurry is 9, with slurries filtration, filter cake 150 ℃ dry 2 hours down, obtain powder 96g.
The 96g powder and the making beating of 150g deionized water of separation layer will have been coated, add the 0.5g triethanolamine simultaneously, add deionized water and be diluted to solid content 90g/L, slurry is heated to 80 ℃, is that 150g/L titanium sulfate and weight concentration are that 15% the NaOH aqueous solution adds in the slurry with the 50ml solid content, and the control pH value of slurry is 6, with slurries filtration, filter cake 105 ℃ dry 3 hours down, prevent then in the muffle furnace obtaining powder 98g in 900 ℃ of calcinings 1.5 hours.
The 98g powder and the making beating of 120g deionized water of titanium dioxide will have been coated, add the 0.3g sodium pyrophosphate simultaneously, add deionized water and be diluted to solid content 120g/L, slurry is heated to 85 ℃, with the waterglass of 20g and weight concentration is that 10% aqueous sulfuric acid adds in the slurry, the control pH value of slurry is 10, keep the temperature-resistant of slurry, with 20g alchlor and weight concentration is that 15% the NaOH aqueous solution adds in the slurry, the control pH value of slurry is 4, keeping the temperature-resistant of slurry, is that 15% the NaOH aqueous solution adds in the slurry with 30g zirconium sulfate and weight concentration, and the control pH value of slurry is 8.With slurries filtration, filter cake descended dry 3 hours at 140 ℃, obtained powder 102g.Record powder whiteness 95.1, reducing power 76.
Embodiment 3
In the 100g powdered whiting of average grain diameter 2.0 μ m, adding the 100g deionized water, add the making beating of 0.5g sodium polyphosphate simultaneously, add deionized water and be diluted to solid content 120g/L, slurry is heated to 95 ℃, with 35g sodium metasilicate and weight concentration is that 10% aqueous hydrochloric acid solution adds in the slurry, the control pH value of slurry is 7.5, until dripping.Keeping the temperature-resistant of slurry, is that 10% aqueous hydrochloric acid solution adds in the slurry with 20g sodium aluminate and weight concentration, and the control pH value of slurry is 11, with slurries filtration, filter cake 150 ℃ dry 1 hour down, obtain powder 97g.
The 97g powder and the making beating of 150g deionized water of separation layer will have been coated, add the 0.2g calgon simultaneously, add deionized water and be diluted to solid content 110g/L, slurry is heated to 83 ℃, is that 200g/L titanium tetrachloride and weight concentration are that 15% the NaOH aqueous solution adds in the slurry with the 50ml solid content, and the control pH value of slurry is 11, with slurries filtration, filter cake 110 ℃ dry 3 hours down, prevent then in the muffle furnace obtaining powder 102g in 850 ℃ of calcinings 3 hours.
The 102g powder and the making beating of 120g deionized water of titanium dioxide will have been coated, add the 0.3g Sodium Polyacrylate simultaneously, add deionized water and be diluted to solid content 110g/L, slurry is heated to 90 ℃, with 25g sodium aluminate and weight concentration is that 10% aqueous hydrochloric acid solution adds in the slurry, the control pH value of slurry is 5, keep the temperature-resistant of slurry, with 25g zirconium sulfate and weight concentration is that 15% the NaOH aqueous solution adds in the slurry, the control pH value of slurry is 8, with slurries filtration, filter cake descended dry 4 hours at 130 ℃, obtained powder 96g.Record powder whiteness 94.8, reducing power 78.
Embodiment 4
In the 100g mica of average grain diameter 1.2 μ m, adding the 120g deionized water, adding the making beating of 0.5g triethanolamine simultaneously, adding deionized water and be diluted to solid content 100g/L, slurry is being heated to 80 ℃, 25g aluminum sulfate (Al
2(SO
4)
318H
2O) and weight concentration be that 15% the NaOH aqueous solution adds in the slurry, the control pH value of slurry is 8.0, until dripping.Keeping the temperature-resistant of slurry, is that 15% the NaOH aqueous solution adds in the slurry with 15g zirconium oxychloride and weight concentration, and the control pH value of slurry is 7, with slurries filtration, filter cake 120 ℃ dry 3 hours down, obtain powder 99g.
The 99g powder and the making beating of 150g deionized water of separation layer will have been coated, add the 0.4g calgon simultaneously, add deionized water and be diluted to solid content 75g/L, slurry is heated to 85 ℃, is that 200g/L titanyl sulfate and weight concentration are that 15% the NaOH aqueous solution adds in the slurry with the 50ml solid content, and the control pH value of slurry is 9, with slurries filtration, filter cake 105 ℃ dry 3 hours down, then in muffle furnace in 850 ℃ of calcinings 3 hours, obtain powder 102g.
The 102g powder and the making beating of 120g deionized water of titanium dioxide will have been coated, add the 0.3g calgon simultaneously, add deionized water and be diluted to solid content 150g/L, slurry is heated to 82 ℃, with the waterglass of 18g and weight concentration is that 10% aqueous hydrochloric acid solution adds in the slurry, the control pH value of slurry is 5, keeps the temperature-resistant of slurry, with 28g alchlor (Alcl
36H
2O) and weight concentration be that 15% the NaOH aqueous solution adds in the slurry, the control pH value of slurry is 10, with slurries filtration, filter cake 90 ℃ dry 5 hours down, obtain powder 101g.Record powder whiteness 94.3, reducing power 73.
Embodiment 5
In the white carbon black of the 100g of average grain diameter 0.4 μ m, adding the 150g deionized water, add the making beating of 0.8g diethanol amine simultaneously, add deionized water and be diluted to solid content 100g/L, slurry is heated to 80 ℃, with 15g zirconium oxychloride and weight concentration is that 15% the NaOH aqueous solution adds in the slurry, the control pH value of slurry is 10.0, until dripping.With slurries filtration, filter cake descended dry 3 hours at 120 ℃, obtained powder 95g.
The 95g powder and the making beating of 150g deionized water of separation layer will have been coated, add the 0.5g calgon simultaneously, add deionized water and be diluted to solid content 60g/L, slurry is heated to 85 ℃, is that 200g/L titanium sulfate and weight concentration are that 10% ammonia spirit adds in the slurry with the 50ml solid content, and the control pH value of slurry is 8, with slurries filtration, filter cake 105 ℃ dry 3 hours down, then in muffle furnace in 850 ℃ of calcinings 3 hours, obtain powder 97g.
The 97g powder and the making beating of 120g deionized water of titanium dioxide will have been coated, add the 0.3g triethanolamine simultaneously, add deionized water and be diluted to solid content 150g/L, slurry is heated to 82 ℃, with 15g zirconium oxychloride and weight concentration is that 15% the NaOH aqueous solution adds in the slurry, and the control pH value of slurry is 6, with slurries filtration, filter cake descended dry 5 hours at 125 ℃, obtained powder 98g.Record powder whiteness 93.8, reducing power 78.
Embodiment 6
In the 100g bentonite of average grain diameter 0.8 μ m, adding the 150g deionized water, add the making beating of 0.3g Sodium Polyacrylate simultaneously, add deionized water and be diluted to solid content 80g/L, slurry is heated to 80 ℃, with the waterglass of 10g and weight concentration is that 10% aqueous sulfuric acid adds in the slurry, the control pH value of slurry is 8.5, until dripping.Keep the temperature-resistant of slurry, with 25g alchlor (Alcl
36H
2O) and weight concentration be that 15% the NaOH aqueous solution adds in the slurry, the control pH value of slurry is 5, with slurries filtration, filter cake 120 ℃ dry 3 hours down, obtain powder 97g.
The 97g powder and the making beating of 150g deionized water of separation layer will have been coated, add the 0.3g calgon simultaneously, add deionized water and be diluted to solid content 90g/L, slurry is heated to 85 ℃, is that 200g/L titanium tetrachloride and weight concentration are that 10% ammonia spirit adds in the slurry with the 50ml solid content, and the control pH value of slurry is 8, with slurries filtration, filter cake 105 ℃ dry 3 hours down, then in muffle furnace in 860 ℃ of calcinings 3 hours, obtain powder 100g.Record powder whiteness 94.2, reducing power 74.
Embodiment 7
In the 100g attapulgite of average grain diameter 0.7 μ m, adding the 150g deionized water, add the making beating of 0.5g Sodium Polyacrylate simultaneously, add deionized water and be diluted to solid content 100g/L, slurry is heated to 80 ℃, with the waterglass of 20g and weight concentration is that 10% aqueous hydrochloric acid solution adds in the slurry, the control pH value of slurry is 8.0, until dripping.Keep the temperature-resistant of slurry, with 30g aluminum sulfate (Al
2(SO
4)
318H
2O) and weight concentration be that 15% the NaOH aqueous solution adds in the slurry, the control pH value of slurry is 9, with slurries filtration, filter cake 120 ℃ dry 3 hours down, obtain powder 99g.
The 99g powder and the making beating of 150g deionized water of separation layer will have been coated, add the 0.4g calgon simultaneously, add deionized water and be diluted to solid content 70g/L, slurry is heated to 85 ℃, is that 200g/L titanyl sulfate and weight concentration are that 15% the NaOH aqueous solution adds in the slurry with the 50ml solid content, and the control pH value of slurry is 7, with slurries filtration, filter cake 105 ℃ dry 3 hours down, then in muffle furnace in 870 ℃ of calcinings 3 hours, obtain powder 105g.Record powder whiteness 92.8, reducing power 82.
Embodiment 8
The needle slurry: broad-leaved slurry=65: 35, take from sun paper industry
Paper pulp mixes the back: beating degree 30oSR, weight in wet base 5-8g
Composite titania material addition: 10% (to the oven dry stock meter)
Composite titania material is embodiment 1,2,3,4,5,6,7 resulting samples
Retention agent is a cationic polyacrylamide, and consumption is 1000ppm (to the oven dry stock meter)
Design is copied paper with slurry amount (the quantitative 40g/m that immobilizes
2), after load weighted paper pulp stirred 1 minute, add composite titania material scattered in advance and through filtering, stir after 1 minute, add retention agent, stir and took off in 1 minute, the square handshcet former (is copied sheet on 400 * 400mm) in the laboratory, (500 * 450mm) go up drying, and pattern presses down optical processing once at the pressure of 0.3MPa, and equilibrium water conten is 24 hours under the normal temperature at the heating polisher then.Paper of whiteness adopts standard GB/T7974-2002 to measure; The opacity of paper is measured according to standard GB 1543-1988.The result is as follows:
| Whiteness | Opacity | |
| Embodiment 1 | ?84.3 | ?84.7 |
| Embodiment 2 | ?83.7 | ?84.5 |
| Embodiment 3 | ?84.3 | ?84.9 |
| Embodiment 4 | ?83.9 | ?85.4 |
| Embodiment 5 | ?83.8 | ?85.1 |
| Embodiment 6 | ?84.1 | ?84.7 |
| Embodiment 7 | ?84.4 | ?85.6 |
Claims (10)
1. a composite titania material is characterized in that, comprises graininess core as carrier, is coated on first clad of carrier outside and is coated on the second outer clad of first clad;
Said carrier is selected from one or more the mixture in talcum powder, kaolin, precipitated calcium carbonate, powdered whiting, mica, white carbon black, bentonite or the attapulgite;
The material of said first clad comprises one or more the mixture in silica, aluminium oxide or the zirconia;
The material of said second clad comprises one or both the mixture in titanium dioxide or the hydrated titanium dioxide.
2. composite titania material according to claim 1 is characterized in that, the weight of first clad is the 0.1-25% (wt) of vehicle weight.
3. composite titania material according to claim 1 is characterized in that, the weight of second clad is the 0.1-20% (wt) of vehicle weight.
4. according to claim 1,2 or 3 described composite titania materials, it is characterized in that, be coated with the 3rd clad at second clad, the 3rd layer material comprises one or more the mixture in silica, aluminium oxide or the zirconia.
5. composite titania material according to claim 4 is characterized in that, the weight of described the 3rd clad is the 0.1-20% (wt) of vehicle weight.
6. composite titania material according to claim 5 is characterized in that, the average grain diameter 0.3-2.0 μ m of said carrier.
7. prepare the method for the described composite titania material of claim 6, comprise the steps:
(1) mixture of carrier, water and dispersant is pulled an oar together, the weight concentration of carrier is 30-80% during making beating, and the addition of dispersant is the 0.1-10% of carrier dry weight, obtains the carrier slurry;
(2) thin up to solid content is 50g/L-250g/L then, be heated to 60～95 ℃, silicon source and/or aluminium source and/or zirconium source and acid or alkali are joined in the carrier slurry, the pH value of the hierarchy of control is 2-11, slurries filtration, filter cake is dry under 90～150 ℃, obtains to be coated with the carrier of first clad;
(3) carrier and the dispersant that will be coated with first clad pulled an oar with the mixture of water, the weight concentration that is coated with the carrier of first clad is 30-80%, the addition of dispersant is for coating the 0.1-5% of back carrier dry weight, be diluted with water to solid content 50g/L-200g/L, under 40～95 ℃ temperature, be 10-500g TiO with concentration
2The aqueous solution in the titanium source of/L and weight concentration are that the aqueous alkali of 5-50% joins in the slurry, the pH value of the hierarchy of control is 6-11, slurries filtration, filter cake is dry down at 90--150 ℃, dried material obtains to be coated with the carrier of second clad 500--1000 ℃ temperature lower calcination 0.5-10 hour.
8. method according to claim 7, it is characterized in that, the carrier of second layer clad will be coated with, the mixture of dispersant and water is pulled an oar together, the weight concentration that is coated with the carrier of the second layer clad during making beating is 30-80%, the addition of dispersant is the 0.1-8% of weight that is coated with the carrier of second layer clad, be diluted with water to solid content 50g/L-250g/L then, under 60--95 ℃ temperature, in adding silicon source or the aluminium source one or both, and acid or alkali, the pH value of the hierarchy of control is 2-11, filters, filter cake is dry under 90--150 ℃ temperature, obtains to be coated with the carrier of the 3rd clad.
9. method according to claim 7 is characterized in that, described dispersant is one or more the mixture in Sodium Polyacrylate, calgon, sodium pyrophosphate, sodium polyphosphate, triethanolamine or the diethanol amine;
Described silicon source is one or more the mixture in sodium metasilicate, Ludox or the ethyl orthosilicate;
Described aluminium source is one or more the mixture in aluminium chloride, aluminum sulfate, sodium aluminate or the aluminium isopropoxide;
Described zirconium source is one or more the mixture in zirconium oxychloride, zirconium sulfate or the zirconium oxysulfate;
Described titanium source is one or more the mixture in titanyl sulfate, titanium sulfate, titanium tetrachloride, tetrabutyl titanate or the isopropyl titanate;
Described acid is one or more the mixture in sulfuric acid, hydrochloric acid, nitric acid or the acetic acid;
Described alkali is one or more the mixture in NaOH, sodium carbonate, sodium bicarbonate, potassium hydroxide or the ammoniacal liquor.
10. according to the application of each described composite titania material of claim 1～6, it is characterized in that, be used for filler.
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| CN108570248B (en) * | 2018-04-16 | 2021-06-22 | 河南骏化发展股份有限公司 | Preparation method of core-shell titanium dioxide coated silicon dioxide |
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