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.