CN100411983C - Method for preparing superfine alumina silicate - Google Patents
Method for preparing superfine alumina silicate Download PDFInfo
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- CN100411983C CN100411983C CNB2006100685358A CN200610068535A CN100411983C CN 100411983 C CN100411983 C CN 100411983C CN B2006100685358 A CNB2006100685358 A CN B2006100685358A CN 200610068535 A CN200610068535 A CN 200610068535A CN 100411983 C CN100411983 C CN 100411983C
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- powder
- alumina silicate
- superfine alumina
- preparation
- bauxite
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 14
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims description 37
- 239000000843 powder Substances 0.000 claims abstract description 61
- 229910001570 bauxite Inorganic materials 0.000 claims abstract description 34
- 230000032683 aging Effects 0.000 claims abstract description 26
- 239000012065 filter cake Substances 0.000 claims abstract description 26
- 238000005406 washing Methods 0.000 claims abstract description 25
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 24
- 239000006004 Quartz sand Substances 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000047 product Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 15
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 15
- 235000019738 Limestone Nutrition 0.000 claims abstract description 14
- 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 abstract description 14
- 239000006028 limestone Substances 0.000 claims abstract description 14
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 230000002194 synthesizing effect Effects 0.000 claims abstract 2
- 239000002245 particle Substances 0.000 claims description 39
- 239000007788 liquid Substances 0.000 claims description 35
- 238000002360 preparation method Methods 0.000 claims description 22
- 239000011734 sodium Substances 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 230000015572 biosynthetic process Effects 0.000 claims description 11
- 235000017550 sodium carbonate Nutrition 0.000 claims description 11
- KMWBBMXGHHLDKL-UHFFFAOYSA-N [AlH3].[Si] Chemical compound [AlH3].[Si] KMWBBMXGHHLDKL-UHFFFAOYSA-N 0.000 claims description 10
- 239000004411 aluminium Substances 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000003786 synthesis reaction Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 8
- 239000012295 chemical reaction liquid Substances 0.000 claims description 7
- 230000029087 digestion Effects 0.000 claims description 7
- 238000002386 leaching Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 229910021417 amorphous silicon Inorganic materials 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000000243 solution Substances 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 abstract 3
- 239000012045 crude solution Substances 0.000 abstract 2
- 229910000503 Na-aluminosilicate Inorganic materials 0.000 abstract 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 1
- 238000001354 calcination Methods 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 239000000429 sodium aluminium silicate Substances 0.000 abstract 1
- 235000012217 sodium aluminium silicate Nutrition 0.000 abstract 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 10
- 239000003973 paint Substances 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000004090 dissolution Methods 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 235000010215 titanium dioxide Nutrition 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 239000002671 adjuvant Substances 0.000 description 2
- PZZYQPZGQPZBDN-UHFFFAOYSA-N aluminium silicate Chemical class O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 208000032400 Retinal pigmentation Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 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 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000005018 casein Substances 0.000 description 1
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 description 1
- 235000021240 caseins Nutrition 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000013462 industrial intermediate Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000037452 priming Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000012747 synergistic agent Substances 0.000 description 1
Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
This invention relates to a method for preparing ultrafine aluminum silicate. The method comprises: (1) mixing bauxite powder and sodium carbonate at Na2O/Al2O3 ratio of 1.2-1.6, adding limestone powder (1-10 wt.% of bauxite) and quartz sand powder (2-15 wt.% of bauxite), and calcining to obtain a clinker; (2) dissolving the clinker to obtain a crude solution; (3) adding one of calcined kaolin powder, amorphorus sodium aluminosilicate and ultrafine aluminum silicate (0.5-2 wt.% of the crude solution), synthesizing and aging; (4) filtering the aged reaction solution to obtain a filter cake; (5) washing the filter cake, drying, and pulverizing by air flow to obtain ultrafine aluminum silicate product. The method has such advantages as high adaptability of raw materials, high product quality and purity, good product dispersibility, no wastewater discharge and no pollution.
Description
Technical field
The present invention relates to a kind of preparation method of superfine alumina silicate, belong to the synthetic technology of aluminium silicate compounds.
Background technology
Superfine alumina silicate is a kind of silicoaluminate of synthetic, and particle diameter belongs to good pigment synergistic agent smaller or equal to 2 μ m, and superfine alumina silicate has the good optical buffer action.In alkyd paint, acrylic acid or the like exterior coating, powder coating, white one priming paint, highway marking paint whitewash, can use by the instead of titanium white powder.Expect can replace in printing paste, the paper coating 15～25% titanium dioxides or other pigment the unglazed satin emulsion in indoor and outdoor, leather casein finiss, Xu especially, the appearance characteristics of the coating that is improved also can reduce to make and paint this.Mix superfine alumina silicate in the coating, its effect: save 15～25% titanium dioxides, especially rutile type or other pigment, reduce the production cost of making paint industry significantly.Physicalies such as opacifying power, glossiness and weathering resistance can not descend, and the whiteness of paint film also increases to some extent.The particle diameter of ultra-fine high-purity pure aluminium silicate is little, dispersiveness is high, can make emulsion paint thickening slightly, thus can prevent the generation of pigment precipitation caking and skin lamination phenomenon effectively, and improve opaqueness; Good resistance to settling.The ultra micro characteristic of superfine alumina silicate and high dispersive performance make coating thickening slightly, and prevent pigment sink to the bottom the caking and surperficial water-separation; The good jar effect of opening is arranged.
At present, the production technique of superfine alumina silicate mainly is to be raw material with Tai-Ace S 150 and water glass, be mixed with certain density solution, with two kinds of solution each with certain flow, add and have stirring, and realize that adding has in the retort of water and additive, use the steam indirect heating, keep homo(io)thermism, flow by stock liquid, system held is reacted under certain pH value, filter rear filtrate after aging then and discharge, filter cake washs, oven dry, comminution by gas stream obtain qualified superfine alumina silicate product.There are shortcomings such as quality product is inferior, bad dispersibility, ingredient requirement height, bad adaptability in this method, and a large amount of discharging of waste liquid are arranged simultaneously, causes environmental pollution.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of superfine alumina silicate, adaptability to raw material is good, the quality product height, and the purity height, good dispersity, no discharging of waste liquid pollutes, the protection environment.
The preparation method of superfine alumina silicate of the present invention, carry out according to the following step successively:
(1) bauxite powder and yellow soda ash are according to Na
2O/Al
2O
3Behind=1.2～1.6 mixes, add again after limestone powder (being called sintering aid) and quartz sand powder (being called silicon source auxiliary agent) carry out second batch, make grog through burning till reaction, 1100～1200 ℃ of temperature, 1～3 hour time, wherein, the Wingdale add-on is 1～10% of a bauxite weight, the quartz sand add-on be in the bauxite aluminium content weight 2～15%, preferred 5～10%;
(2) thick liquid will be got after the grog stripping;
(3) add in thick liquid that a kind of in calcined kaolin powder, amorphous silicon aluminium acid sodium or the superfine alumina silicate (all being called silicon source auxiliary agent) synthesizes, aging reaction, add-on is 0.5～2% of a thick liquid weight, preferred 1～1.5%; Wherein preferred calcined kaolin powder, arbitrarily kaolin can, preferably control particle diameter smaller or equal to 1.2 μ m, whiteness is greater than 98%;
(4) aging reaction liquid is filtered filter cake;
(5) after the filter cake washing, carry out drying, make the superfine alumina silicate product through comminution by gas stream then.
Control condition is as follows preferably among the present invention:
The aluminium silicon mol ratio of bauxite powder is 3.5～8, belongs to middle-low bauxite.
Yellow soda ash can directly use industrial sodium carbonate, or uses industrial intermediate product, and as using the evaporation carbon mother liquid in the sintering process production aluminum oxide flow process, consumption can be converted according to the content of yellow soda ash and get final product.
The particle diameter of bauxite powder, limestone powder and quartz sand powder is smaller or equal to 200 μ m, preferably smaller or equal to 100 μ m, preferably smaller or equal to 50 μ m.
The grog leaching condition is controlled to be: 70～110 ℃ of temperature, preferred 80～90 ℃, 0.8～1.2 hour time, liquid-solid ratio 6～12, preferred 7～10.
40～80 ℃ of synthesis temperatures, preferred 50～60 ℃, generated time 0.5～1.0 hour, preferred 0.8～1.0 hour; 60～70 ℃ of aging temperatures, digestion time 1.5～2.5 hours.
Filter cake adopts redistilled water to wash, the agitator treating mode, and 65～75 ℃ of temperature of washing water, temperature of washing water preferably are controlled at 70 ℃.Liquid-solid ratio is controlled to be 10～12, through repeatedly washing, Na in the last filtrate
2O content is less than 0.3g/L.
The material cake adopts tray drier to carry out drying, carries out superfine grinding by micronizer mill then, screens, and the control maximum particle diameter is no more than 2 microns, gets product.
Preparation method of the present invention has following technical characterstic:
(1) raw materials for production are bauxite, quartz sand etc., have reduced production link, have reduced production cost.
(2) secondary has added silicon source auxiliary agent in the building-up reactions, does the effect of seed, can obtain high-quality superfine alumina silicate product.
(3) mode of employing coproduction superfine alumina silicate on the alumina producing flow process, no waste is got rid of, and makes that Production Flow Chart has realized cleaning.
(4) when producing superfine alumina silicate, realized the first class purification of thick liquid in the sintering process production aluminum oxide flow process, finished the pre-desiliconization of thick liquid, reduced alumina production cost, promote the alumina producing ability.
(5) adopted full liquid phase synthetic technology, primary particle size control is even, D
50Maximum 1.5 μ m, dispersed fabulous, the product purity height, the product whiteness height can reach 98%, good product quality.
(6) but the serialization operation is convenient to carry out large industrialized production.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
The preparation method of superfine alumina silicate of the present invention, carry out according to following steps successively:
(1) the 500g particle diameter is smaller or equal to 70 μ m bauxite powders, Al
2O
3Weight content 62%, its aluminium silicon mol ratio is 5, with carbonate content be that the evaporation carbon mother liquid of 50g/l is according to Na
2O/Al
2O
3After=1.3 the ratio batching, add the 5g particle diameter simultaneously and carry out second batch smaller or equal to the adjuvant for combustion limestone powder of 50 μ m and 10g particle diameter smaller or equal to the quartz sand powder of 80 μ m, go into stove and burn till reaction, 1150 ℃ of temperature, make grog at 2 hours time.
(2) leaching condition that burns till grog control is: 80 ℃ of temperature, 1.2 hours time, liquid-solid ratio control 10 obtains thick liquid after stripping.
(3) adding particle diameter in above-mentioned thick liquid is 1.1 μ m, and whiteness is 98.5% 25g calcined kaolin powder, 50 ℃ of synthesis temperature controls, and generated time is controlled to be 0.8 hour; 60 ℃ of aging temperature controls, 2 hours time.
(4) after reaction finishes, filter and obtain filter cake, filtrate is delivered to the big flow process of alumina producing and is carried out the secondary-cleaned processing.
(5) adopt redistilled water that filter cake is washed, the agitator treating mode is adopted in 70 ℃ of temperature of washing water controls, and liquid-solid ratio control 10 is adopted repeatedly washing, last filtrate Na
2O content is less than 0.3g/L.
(6) adopt tray drier to filtration cakes torrefaction, carry out superfine grinding by micronizer mill then, screen, obtain salable product, it is heavy broken that coarse particles carries out returning charge.
Embodiment 2:
The preparation method of superfine alumina silicate of the present invention, carry out according to following steps successively:
(1) the 500g particle diameter is smaller or equal to the bauxite powder of 100 μ m, and its aluminium silicon mol ratio is 8, with the evaporation carbon mother liquid according to Na
2O/Al
2O
3After=1.3 the ratio batching, add the 50g particle diameter simultaneously and carry out second batch smaller or equal to the quartz sand powder of 60 μ m, go into stove and burn till reaction, make grog smaller or equal to the adjuvant for combustion limestone powder of 30 μ m and 50g particle diameter.
(2) with embodiment 1, different is that leaching condition is: 90 ℃ of temperature, 0.8 hour time, liquid-solid ratio control 7 obtains thick liquid after stripping.
(3) with embodiment 1, different is to add 80g calcined kaolin powder, 60 ℃ of synthesis temperature controls, and generated time is controlled to be 1.0 hours; 70 ℃ of aging temperature controls.
(4) with embodiment 1.
(5) with embodiment 1, different is liquid-solid ratio control 12.
Table 1, superfine alumina silicate product index table
| Index | Moisture content % | Bulk density Kg/L | Oil number g/100g | Whiteness % | Crystal formation | D 50(μm) | PH value (5% aqueous solution) | Outward appearance |
| Embodiment 1 | 6-10 | 0.25-0.35 | 30 | ＞98 | Unformed | ＜1.5 | 9.5-10.6 | White powder |
| Embodiment 2 | 2-4 | 0.27-0.37 | 100-130 | ＞97 | Unformed | ＜1.5 | 7.3-8.5 | White powder |
Embodiment 3:
As described in embodiment 1, different is:
(1) add 500g, particle diameter is smaller or equal to the bauxite powder of 90 μ m, and its aluminium silicon mol ratio is 7, add the limestone powder of 25g particle diameter smaller or equal to 60 μ m, carry out second batch with the 25g particle diameter smaller or equal to the quartz sand powder of 40 μ m, go into stove and burn till reaction, make grog.
(2) with embodiment 1, different is that leaching condition is: 85 ℃ of temperature, 0.9 hour time, liquid-solid ratio control 9 obtains thick liquid after stripping.
(3) with embodiment 1, different is to add 50g calcined kaolin powder, 55 ℃ of synthesis temperature controls, and generated time is controlled to be 0.9 hour, 65 ℃ of aging temperature controls.
(4) with embodiment 1.
(5) with embodiment 1, different is liquid-solid ratio control 11.
Other is with embodiment 1.
Embodiment 4:
The preparation method of superfine alumina silicate of the present invention, carry out according to the following step successively:
(1) particle diameter is smaller or equal to bauxite powder 500 gram of 100 μ m, and the aluminium silicon mol ratio is 5, with yellow soda ash according to Na
2O/Al
2O
3Behind=1.2 mixes, add again after particle diameter carries out second batch smaller or equal to the limestone powder of 100 μ m and particle diameter smaller or equal to the quartz sand powder of 50 μ m, make grog through burning till reaction, 1160 ℃ of temperature, 1.8 hours time, wherein, the Wingdale add-on is 6% of a bauxite weight, the quartz sand add-on be in the bauxite aluminium content weight 10%.
(2) thick liquid, 90 ℃ of stripping temperature, dissolution time 1.1 hours, liquid-solid ratio 8 will be got after the grog stripping.
(3) add in thick liquid that the calcined kaolin powder synthesizes, aging reaction, add-on is 1% of a thick liquid weight, and wherein calcined kaolin powder footpath is smaller or equal to 1.2 μ m, and whiteness is greater than 98%; 55 ℃ of synthesis temperatures, generated time 1 hour; 63 ℃ of aging temperatures, digestion time 2.2 hours.
(4) aging reaction liquid is filtered filter cake, filter cake adopts redistilled water to wash, the agitator treating mode, 72 ℃ of temperature of washing water, liquid-solid ratio is controlled to be 11, through repeatedly washing, Na in the last filtrate
2O content is less than 0.3g/L.
(5) after the filter cake washing, adopt tray drier to carry out drying, carry out superfine grinding by micronizer mill then, screen, the control maximum particle diameter is no more than 2 microns, gets product.
Embodiment 5:
The preparation method of superfine alumina silicate of the present invention, carry out according to the following step successively:
(1) particle diameter is smaller or equal to bauxite powder 500 gram of 100 μ m, and the aluminium silicon mol ratio is 6.5, with yellow soda ash according to Na
2O/Al
2O
3Behind=1.4 mixes, add again after particle diameter carries out second batch smaller or equal to the limestone powder of 70 μ m and particle diameter smaller or equal to the quartz sand powder of 70 μ m, make grog through burning till reaction, 1180 ℃ of temperature, 1.4 hours time, wherein, the Wingdale add-on is 4% of a bauxite weight, the quartz sand add-on be in the bauxite aluminium content weight 5%.
(2) thick liquid, 80 ℃ of stripping temperature, dissolution time 0.9 hour, liquid-solid ratio 9 will be got after the grog stripping.
(3) add in thick liquid that the calcined kaolin powder synthesizes, aging reaction, add-on is 1.5% of a thick liquid weight, and particle diameter is smaller or equal to 1.2 μ m, and whiteness is greater than 98%; 70 ℃ of synthesis temperatures, generated time 1.0 hours, 66 ℃ of aging temperatures, digestion time 2 hours.
(4) aging reaction liquid is filtered filter cake, filter cake adopts redistilled water to wash, the agitator treating mode, 68 ℃ of temperature of washing water, liquid-solid ratio is controlled to be 10, through repeatedly washing, Na in the last filtrate
2O content is less than 0.3g/L.
(5) after the filter cake washing, adopt tray drier to carry out drying, carry out superfine grinding by micronizer mill then, screen, the control maximum particle diameter is no more than 2 microns, gets product.
Embodiment 6:
The preparation method of superfine alumina silicate of the present invention, carry out according to the following step successively:
(1) particle diameter is smaller or equal to bauxite powder 500 gram of 200 μ m, and the aluminium silicon mol ratio is 4, with yellow soda ash according to Na
2O/Al
2O
3Behind=1.22 mixes, add again after particle diameter carries out second batch smaller or equal to the limestone powder of 100 μ m and particle diameter smaller or equal to the quartz sand powder of 60 μ m, make grog through burning till reaction, 1160 ℃ of temperature, 2.2 hours time, wherein, the Wingdale add-on is 4.5% of a bauxite weight, the quartz sand add-on be in the bauxite aluminium content weight 7%.
(2) thick liquid, 100 ℃ of stripping temperature, dissolution time 0.9 hour, preferred 11 will be got after the grog stripping.
(3) add in thick liquid that the calcined kaolin powder synthesizes, aging reaction, add-on is 0.8% of a thick liquid weight, and calcined kaolin powder footpath is smaller or equal to 1.2 μ m, and whiteness is greater than 98%; 70 ℃ of synthesis temperatures, generated time 0.8 hour; 60～70 ℃ of aging temperatures, digestion time 2 hours.
(4) aging reaction liquid is filtered filter cake, filter cake adopts redistilled water to wash agitator treating mode, 70 ℃ of temperature of washing water.Liquid-solid ratio is controlled to be 10.5, through repeatedly washing, Na in the last filtrate
2O content is less than 0.3g/L.
(5) after the filter cake washing, adopt tray drier to carry out drying, carry out superfine grinding by micronizer mill then, screen, the control maximum particle diameter is no more than 2 microns, gets product.
Embodiment 7:
The preparation method of superfine alumina silicate of the present invention, carry out according to the following step successively:
(1) particle diameter is smaller or equal to bauxite powder 500 gram of 150 μ m, and the aluminium silicon mol ratio is 5, with yellow soda ash according to Na
2O/Al
2O
3Behind=1.5 mixes, add again after particle diameter carries out second batch smaller or equal to the limestone powder of 80 μ m and particle diameter smaller or equal to the quartz sand powder of 80 μ m, make grog through burning till reaction, 1150 ℃ of temperature, 2 hours time, wherein, the Wingdale add-on is 5% of a bauxite weight, the quartz sand add-on be in the bauxite aluminium content weight 6%.
(2) thick liquid, 85 ℃ of stripping temperature, dissolution time 1 hour, liquid-solid ratio 7 will be got after the grog stripping.
(3) add in thick liquid that amorphous silicon aluminium acid sodium synthesizes, aging reaction, add-on is 1% of a thick liquid weight; 56 ℃ of synthesis temperatures, generated time 0.9 hour, preferred 0.9 hour; 70 ℃ of aging temperatures, digestion time 2 hours.
(4) aging reaction liquid is filtered filter cake, filter cake adopts redistilled water to wash agitator treating mode, 68 ℃ of temperature of washing water.Liquid-solid ratio is controlled to be 11.5, through repeatedly washing, Na in the last filtrate
2O content is less than 0.3g/L.
(5) after the filter cake washing, adopt tray drier to carry out drying, carry out superfine grinding by micronizer mill then, screen, the control maximum particle diameter is no more than 2 microns, gets product.
Embodiment 8:
The preparation method of superfine alumina silicate of the present invention, carry out according to the following step successively:
(1) particle diameter is smaller or equal to bauxite powder 500 gram of 90 μ m, and the aluminium silicon mol ratio is 7, with yellow soda ash according to Na
2O/Al
2O
3Behind=1.4 mixes, add again after particle diameter carries out second batch smaller or equal to the limestone powder of 70 μ m and particle diameter smaller or equal to the quartz sand powder of 80 μ m, make grog through burning till reaction, 1160 ℃ of temperature, 2.3 hours time, wherein, the Wingdale add-on is 4% of a bauxite weight, the quartz sand add-on be in the bauxite aluminium content weight 3%.
(2) thick liquid, 75 ℃ of stripping temperature, dissolution time 0.9 hour, liquid-solid ratio 8 will be got after the grog stripping.
(3) add in thick liquid that superfine alumina silicate synthesizes, aging reaction, add-on is 1.5% of a thick liquid weight, 52 ℃ of synthesis temperatures, generated time 0.6 hour, 62 ℃ of aging temperatures, digestion time 2.2 hours.
(4) aging reaction liquid is filtered filter cake, filter cake adopts redistilled water to wash agitator treating mode, 67 ℃ of temperature of washing water.Liquid-solid ratio is controlled to be 12, through repeatedly washing, Na in the last filtrate
2O content is less than 0.3g/L.
(5) after the filter cake washing, adopt tray drier to carry out drying, carry out superfine grinding by micronizer mill then, screen, the control maximum particle diameter is no more than 2 microns, gets product.
Claims (10)
1. the preparation method of a superfine alumina silicate is characterized in that carrying out according to the following step successively:
(1) bauxite powder and yellow soda ash are according to Na
2O/Al
2O
3Behind=1.2～1.6 mixes, add again after limestone powder and quartz sand powder carry out second batch, making grog through burning till reaction, wherein, the Wingdale add-on is 1～10% of a bauxite weight, the quartz sand add-on be in the bauxite aluminium content weight 2～15%;
(2) thick liquid will be got after the grog stripping;
(3) add in thick liquid that a kind of in calcined kaolin powder, amorphous silicon aluminium acid sodium or the superfine alumina silicate synthesizes, aging reaction, add-on is 0.5～2% of a thick liquid weight;
(4) aging reaction liquid is filtered filter cake;
(5) after the filter cake washing, carry out drying, make the superfine alumina silicate product through comminution by gas stream then.
2. the preparation method of superfine alumina silicate according to claim 1, the aluminium silicon mol ratio that it is characterized in that bauxite powder is 3.5～8.
3. the preparation method of superfine alumina silicate according to claim 1 is characterized in that yellow soda ash is that sintering process is produced the evaporation carbon mother liquid in the aluminum oxide flow process.
4. the preparation method of superfine alumina silicate according to claim 1, the particle diameter that it is characterized in that bauxite powder, limestone powder and quartz sand powder is smaller or equal to 200 μ m.
5. the preparation method of superfine alumina silicate according to claim 4, the particle diameter that it is characterized in that bauxite powder, limestone powder and quartz sand powder is smaller or equal to 100 μ m.
6. the preparation method of superfine alumina silicate according to claim 1 is characterized in that adding the calcined kaolin powder in thick liquid, and its particle diameter is smaller or equal to 1.2 μ m, and whiteness is greater than 98%.
7. the preparation method of superfine alumina silicate according to claim 1 is characterized in that the grog leaching condition is controlled to be: 70～110 ℃ of temperature, 0.8～1.2 hour time, liquid-solid ratio 6～12.
8. the preparation method of superfine alumina silicate according to claim 1 is characterized in that synthesizing, the aged condition is: 40～80 ℃ of synthesis temperatures, generated time 0.5～1.0 hour; 60～70 ℃ of aging temperatures, digestion time 1.5～2.5 hours.
9. the preparation method of superfine alumina silicate according to claim 1 is characterized in that filter cake adopts redistilled water to wash, the agitator treating mode, and 65～75 ℃ of temperature of washing water, liquid-solid ratio is controlled to be 10～12, through repeatedly washing, Na in the last filtrate
2O content is less than 0.3g/L.
10. the preparation method of superfine alumina silicate according to claim 1 is characterized in that expecting that cake adopts tray drier to carry out drying, carries out superfine grinding by micronizer mill then, screens, and gets product.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0000870A1 (en) * | 1977-08-24 | 1979-03-07 | Kali-Chemie Aktiengesellschaft | Process for improving the properties of sodium aluminosilicate doughs and powders |
| JPS63166714A (en) * | 1986-12-27 | 1988-07-09 | Kyoritsu Yogyo Genryo Kk | Production of aluminum silicate fine powder |
| CN1400164A (en) * | 2002-09-13 | 2003-03-05 | 冯乃谦 | Production method of aluminium silicate mineral superfine powder |
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2006
- 2006-08-23 CN CNB2006100685358A patent/CN100411983C/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0000870A1 (en) * | 1977-08-24 | 1979-03-07 | Kali-Chemie Aktiengesellschaft | Process for improving the properties of sodium aluminosilicate doughs and powders |
| JPS63166714A (en) * | 1986-12-27 | 1988-07-09 | Kyoritsu Yogyo Genryo Kk | Production of aluminum silicate fine powder |
| CN1400164A (en) * | 2002-09-13 | 2003-03-05 | 冯乃谦 | Production method of aluminium silicate mineral superfine powder |
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