Summary of the invention
The object of the present invention is to provide a kind of neutralisation to produce the method for aluminium hydroxide micropowder, the technological process of production is simple, and operating process is easy to control, and the aluminium hydroxide micropowder purity height of acquisition, sphericity height, size-grade distribution are concentrated, oil number is low, specific conductivity is low.
Neutralisation of the present invention is produced the method for aluminium hydroxide micropowder, carry out neutralization reaction by sodium aluminate solution and acidic solution, acquisition pH value is 6~8 near neutral seed liquor, is 0.5~2.0% with the seed coefficient, slowly adds sodium aluminate solution in seed liquor, planting the branch time is 4~8 hours, rate of decomposition is controlled at 50~55%, gained is decomposed slurries carry out liquid-solid separation, and solid is through washing and oven dry, pass through the air-flow depolymerization again, obtain aluminium hydroxide micropowder.
The present invention obtains seed liquor by neutralization reaction, compares with solid-state seed, need not to grind, and does not also have development impurity and brings into, has improved the purity of aluminium hydroxide micropowder, the sphericity height, and size-grade distribution is concentrated, and oil number is low, and specific conductivity is low.And slowly add sodium aluminate solution, can add speed by motorized valve and under meter control sodium aluminate solution, sustainable 3~5 hours of joining day, thus crystalline growth velocity is suitable, reduces agglomeration, good sphericity.
Among the present invention, control condition is as follows preferably:
The temperature of reaction of sodium aluminate solution and acidic solution is controlled to be 20~90 ℃;
Sodium aluminate solution caustic ratio α k=1.4~1.6, alumina content is 95~110g/L;
Acidic solution is acetic acid solution or alum liquor, and the weight concentration of acetic acid solution is controlled to be 10~20%, and the weight content of aluminum oxide is controlled to be 7.5~8.3% in the alum liquor.
The air-flow depolymerization is by reinforced injector by pressurized gas (air or other gas), the powder raw material that self-feeder is got off, be generally below 60 orders, evenly enter depolymerizer continuously, pressurized gas is by the outdoor nozzle that encloses of depolymerization simultaneously, produce high velocity air, spray into the depolymerization chamber, make the mutual collision friction of gas particles and reach the depolymerization purpose, the ultrafine particle after the depolymerization, major part is collected in the cyclonic separation bottom, and gas then sees through filter bag and discharges.It is the depolymerization of comminution by gas stream mill that the air-flow depolymerization can be used the airflow milling depolymerization, and the comminution by gas stream mill can directly be bought for sophisticated existing installation,
The aluminium hydroxide micropowder product purity that is made by preparation method of the present invention is greater than 99.7%, meta particle diameter 0.1~2.0 μ m, and size-grade distribution is concentrated, particle sphericity height, oil number is not more than 40mL/100g, and specific conductivity is not more than 70 μ s/cm.
Neutralisation of the present invention is produced the method for aluminium hydroxide micropowder, the technological process of production is simple, and operating process is easy to control, is convenient to industrializing implementation, and the aluminium hydroxide micropowder purity height that obtains, sphericity height, size-grade distribution are concentrated, oil number is low, specific conductivity is low, the quality product height.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 100g/L, α k=1.44, under 25 ℃, carry out with weight concentration be that 15% acetic acid solution carries out neutralization reaction, acquisition pH value is 7 seed liquor, with the seed coefficient is 0.5%, slowly adds sodium aluminate solution and decomposes, and the resolving time is 7 hours, rate of decomposition 54%, decompose slurries and carry out liquid-solid separation, washing and oven dry, air-flow depolymerization pressure 0.6Mpa, obtaining aluminium hydroxide micropowder purity is 99.71%, 1.13 microns of meta particle diameters, specific conductivity 47 μ s/cm, oil number 35mL/100g, its chemical ingredients sees Table 1.
Embodiment 2
Soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 104g/L, α k=1.46, under 30 ℃, carry out with weight concentration be that 12% acetic acid solution carries out neutralization reaction, acquisition pH value is 6.6 seed liquor, with the seed coefficient is 0.5%, slowly adds sodium aluminate solution and decomposes, and the resolving time is 8 hours, rate of decomposition 55%, decompose slurries and carry out liquid-solid separation, washing and oven dry, air-flow depolymerization pressure 0.6Mpa, obtaining aluminium hydroxide micropowder purity is 99.73%, 1.10 microns of meta particle diameters, specific conductivity 55 μ s/cm, oil number 35ml/100g, its chemical ingredients sees Table 1.
Embodiment 3
Soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 98g/L, α k=1.52, under 30 ℃, carry out with weight concentration be that 18% acetic acid solution carries out neutralization reaction, acquisition pH value is 7.5 seed liquor, with the seed coefficient is 0.5%, slowly adds sodium aluminate solution and decomposes, and the resolving time is 8 hours, rate of decomposition 55%, decompose slurries and carry out liquid-solid separation, washing and oven dry, air-flow depolymerization pressure 0.8Mpa, obtaining aluminium hydroxide micropowder purity is 99.74%, 1.05 microns of meta particle diameters, specific conductivity 35 μ s/cm, oil number 36mL/100g, its chemical ingredients sees Table 1.
Embodiment 4
Soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 100g/L, α k=1.48, under 30 ℃, carry out with weight concentration be that 16% acetic acid solution carries out neutralization reaction, acquisition pH value is 7.2 seed liquor, with the seed coefficient is 1.0%, slowly adds sodium aluminate solution and decomposes, and the resolving time is 8 hours, rate of decomposition 56%, decompose slurries and carry out liquid-solid separation, washing and oven dry, air-flow depolymerization pressure 0.6Mpa, obtaining aluminium hydroxide micropowder purity is 99.74%, 0.68 micron of meta particle diameter, specific conductivity 58 μ s/cm, oil number 40mL/100g, its chemical ingredients sees Table 1.
Embodiment 5
Soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 105g/L, α k=1.53, under 30 ℃, carry out with weight concentration be that 13% acetic acid solution carries out neutralization reaction, acquisition pH value is 6.8 seed liquor, with the seed coefficient is 1.0%, slowly adds sodium aluminate solution and decomposes, and the resolving time is 6 hours, rate of decomposition 55%, decompose slurries and carry out liquid-solid separation, washing and oven dry, air-flow depolymerization pressure 0.8Mpa, obtaining aluminium hydroxide micropowder purity is 99.75%, 0.65 micron of meta particle diameter, specific conductivity 51 μ s/cm, oil number 40mL/100g, its chemical ingredients sees Table 1.
Embodiment 6
Soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 100g/L, α k=1.49, under 35 ℃, carry out with weight concentration be that 14% acetic acid solution carries out neutralization reaction, acquisition pH value is 7.2 seed liquor, with the seed coefficient is 1.0%, slowly adds sodium aluminate solution and decomposes, and the resolving time is 7 hours, rate of decomposition 55%, decompose slurries and carry out liquid-solid separation, washing and oven dry, air-flow depolymerization pressure 0.8Mpa, obtaining aluminium hydroxide micropowder purity is 99.78%, 0.66 micron of meta particle diameter, specific conductivity 24 μ s/cm, oil number 40mL/100g, its chemical ingredients sees Table 1.
Embodiment 7
Soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 100g/L, α k=1.44, under 40 ℃, carry out weight content with aluminum oxide and be 8% alum liquor and carry out neutralization reaction, acquisition pH value is 7 seed liquor, with the seed coefficient is 2.0%, slowly add sodium aluminate solution and decompose, the resolving time is 5 hours, rate of decomposition 60%, decompose slurries and carry out liquid-solid separation, washing and oven dry, air-flow depolymerization pressure 0.8Mpa, obtaining aluminium hydroxide micropowder purity is 99.75%, 0.24 micron of meta particle diameter, specific conductivity 37 μ s/cm, its chemical ingredients sees Table 1.
Embodiment 8
Soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 100g/L, α k=1.44, under 30 ℃, carry out weight content with aluminum oxide and be 7.6% alum liquor and carry out neutralization reaction, acquisition pH value is 6.5 seed liquor, with the seed coefficient is 2.0%, slowly add sodium aluminate solution and decompose, the resolving time is 6 hours, rate of decomposition 62%, decompose slurries and carry out liquid-solid separation, washing and oven dry, air-flow depolymerization pressure 0.8Mpa, obtaining aluminium hydroxide micropowder purity is 99.75%, 0.15 micron of meta particle diameter, specific conductivity 17 μ s/cm, its chemical ingredients sees Table 1.
Embodiment 9
Soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 105g/L, α k1.54, under 30 ℃, carry out weight content with aluminum oxide and be 8.2% alum liquor and carry out neutralization reaction, acquisition pH value is 7.7 seed liquor, with the seed coefficient is 2.0%, slowly add sodium aluminate solution and decompose, the resolving time is 8 hours, rate of decomposition 65%, decompose slurries and carry out liquid-solid separation, washing and oven dry, air-flow depolymerization pressure 0.8Mpa, obtaining aluminium hydroxide micropowder purity is 99.75%, 0.13 micron of meta particle diameter, specific conductivity 8 μ s/cm, its chemical ingredients sees Table 1.
Table 1, product analysis be table as a result