CN100411983C - Method for preparing superfine alumina silicate - Google Patents

Method for preparing superfine alumina silicate Download PDF

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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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alumina silicate
superfine alumina
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CN1915813A (en
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高建阳
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Aluminum Corp of China Ltd
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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

The preparation method of superfine alumina silicate
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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Publication number Priority date Publication date Assignee Title
CN101148258B (en) * 2007-08-31 2010-09-15 安徽工业大学 Method for preparing hydrated aluminum silicate

Citations (3)

* Cited by examiner, † Cited by third party
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
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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