CN100378000C - Method for producing micropowder aluminium hydroxide by neutralization method - Google Patents

Method for producing micropowder aluminium hydroxide by neutralization method Download PDF

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Publication number
CN100378000C
CN100378000C CNB2006100685767A CN200610068576A CN100378000C CN 100378000 C CN100378000 C CN 100378000C CN B2006100685767 A CNB2006100685767 A CN B2006100685767A CN 200610068576 A CN200610068576 A CN 200610068576A CN 100378000 C CN100378000 C CN 100378000C
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aluminium hydroxide
sodium aluminate
seed
aluminate solution
hydroxide micropowder
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CN1911807A (en
Inventor
栾福森
刘春利
鹿中科
邢国
张蕾
袁崇良
文钦果
毕效革
孙丽菊
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Aluminum Corp of China Ltd
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Aluminum Corp of China Ltd
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Abstract

The present invention relates to neutralizing process of producing fine aluminum hydroxide powder. The production process includes the neutralization reaction between sodium aluminate solution and acid solution to obtain neutral seed liquid of pH 6-8; adding the seed liquid into sodium aluminate solution in the seed coefficient of 0.5-2.0 % for seed separation of 4-8 at decomposition rate of 50-55 %; solid-liquid separation of the decomposed slurry, washing and drying the solid, and airflow depolymerization to obtain fine aluminum hydroxide powder. The production process is simple, easy to control and suitable for industrial production, and the obtained fine aluminum hydroxide powder has high purity, high sphericity, concentrated grain size distribution, low oil absorbing rate, low conductivity and high quality.

Description

Neutralisation is produced the method for aluminium hydroxide micropowder
Technical field
The present invention relates to a kind of neutralisation and produce the method for aluminium hydroxide micropowder, belong to the synthetic technology of aluminium hydroxide micropowder.
Background technology
The existing aluminium hydroxide micropowder method of producing mainly prepares crystal seed by machinery dry grinding method and mechanical process, adopts the seed addition decomposition method then.One, mechanical dry grinding method flow process is extremely simple, but has unfavorable factors such as granular size is irregular, particle surface is extremely coarse, foreign matter content height, now is eliminated gradually; Second method has just partly been eliminated the unfavorable factor of mechanical dry grinding method.Chinese patent, application number 200410049908.8, proposed " a kind of method of producing the low conductivity aluminium hydroxide micropowder ", the refined sodium aluminate solution desiliconization has been purified, made siliceous modulus more than 600, seston is less than 0.02%, add the crystal seed coefficient and be 3~12% crystal seed, under 50~73 ℃ of conditions, decomposed 3~8 hours, after filtration, washing, oven dry finally obtain the aluminium hydroxide micropowder product of low conductivity, its specific conductivity≤140 μ s/cm, meta particle diameter are 0.4~3 μ m.Because used crystal seed adopts the sand-blast preparation, thereby there are problems such as particle surface is coarse, size-grade distribution is wide, product foreign matter content height in the aluminium hydroxide micropowder product that causes preparing.
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.
Description of drawings
Fig. 1, process flow diagram of the present invention.
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
Figure C20061006857600061

Claims (5)

1. a neutralisation is produced the method for aluminium hydroxide micropowder, it is characterized in that carrying out neutralization reaction by sodium aluminate solution and acidic solution, acquisition pH value is 6~8 near neutral seed liquor, with the seed coefficient is 0.5~2.0%, in seed liquor, slowly add sodium aluminate solution, 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, solid is through washing and oven dry, pass through the air-flow depolymerization again, obtain aluminium hydroxide micropowder, wherein acidic solution is acetic acid solution or alum liquor.
2. neutralisation according to claim 1 is produced the method for aluminium hydroxide micropowder, and the temperature of reaction that it is characterized in that sodium aluminate solution and acidic solution is 20~90 ℃.
3. neutralisation according to claim 1 is produced the method for aluminium hydroxide micropowder, it is characterized in that sodium aluminate solution caustic ratio α k=1.4~1.6, and alumina content is 95~110g/L.
4. neutralisation according to claim 1 is produced the method for aluminium hydroxide micropowder, and the weight concentration that it is characterized in that acetic acid solution is 10~20%.
5. neutralisation according to claim 1 is produced the method for aluminium hydroxide micropowder, and the weight content that it is characterized in that aluminum oxide in the alum liquor is 7.5~8.3%.
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Publication number Priority date Publication date Assignee Title
CN102730728A (en) * 2012-06-18 2012-10-17 河南神火新材料有限公司 Preparation method for aluminum hydroxide used for filling material
CN104045102A (en) * 2014-06-27 2014-09-17 中国铝业股份有限公司 Production method for aluminum hydroxide
CN104045100A (en) * 2014-06-27 2014-09-17 中国铝业股份有限公司 Preparation method of aluminum hydroxide
CN110372021A (en) * 2019-06-13 2019-10-25 山东泰星新材料股份有限公司 A kind of preparation method and application of electronic circuit board or electrician's fire retardant aluminium hydroxide

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06316647A (en) * 1993-03-09 1994-11-15 Sumitomo Chem Co Ltd Aluminum hydroxide for packing resin and its production
JPH08325011A (en) * 1995-05-26 1996-12-10 Showa Denko Kk Aluminum hydroxide and its production
CN1287973A (en) * 2000-11-01 2001-03-21 中国长城铝业中州铝厂 Method for preparing super fine aluminium hydroxide
CN1433964A (en) * 2003-03-12 2003-08-06 湖南化工研究院 Process for preparing superfine aluminium hydroxide
CN1803622A (en) * 2006-01-23 2006-07-19 山东铝业股份有限公司 Method for preparing aluminium hydroxide micropowder

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06316647A (en) * 1993-03-09 1994-11-15 Sumitomo Chem Co Ltd Aluminum hydroxide for packing resin and its production
JPH08325011A (en) * 1995-05-26 1996-12-10 Showa Denko Kk Aluminum hydroxide and its production
CN1287973A (en) * 2000-11-01 2001-03-21 中国长城铝业中州铝厂 Method for preparing super fine aluminium hydroxide
CN1433964A (en) * 2003-03-12 2003-08-06 湖南化工研究院 Process for preparing superfine aluminium hydroxide
CN1803622A (en) * 2006-01-23 2006-07-19 山东铝业股份有限公司 Method for preparing aluminium hydroxide micropowder

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碳分晶种对铝酸钠溶液分解的影响. 吴玉胜,毕诗文,李文成,佟志芳,杨毅宏.轻金属,第9期. 2005 *
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