CN1803622A - Method for preparing aluminium hydroxide micropowder - Google Patents

Method for preparing aluminium hydroxide micropowder Download PDF

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Publication number
CN1803622A
CN1803622A CN 200610042100 CN200610042100A CN1803622A CN 1803622 A CN1803622 A CN 1803622A CN 200610042100 CN200610042100 CN 200610042100 CN 200610042100 A CN200610042100 A CN 200610042100A CN 1803622 A CN1803622 A CN 1803622A
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aluminium hydroxide
preparation
hydroxide micropowder
product
crystal seed
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CN100411990C (en
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栾福森
张蕾
孙丽菊
颜廷厚
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Aluminum Corp of China Ltd
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SHANDONG ALUMINIUM INDUSTRY Co Ltd
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Abstract

The invention relates to a preparation method for micropowder aluminum hydroxide. Wherein, adding aluminum hydroxide as crystal seed into the material of sodium aluminate solution; liquid-solid separating the slurry, clearing and baking the solid; then using gas flow grinder for depolymerisation and stepped treatment to obtain the final product. Compared with prior art, this invention improves product quality and purity obviously, and reduces oil suction quantity and conductivity and sodium oxide content in product greatly.

Description

The preparation method of aluminium hydroxide micropowder
Technical field
The present invention relates to a kind of preparation method of improved aluminium hydroxide micropowder, belong to the production of aluminum hydroxide technical field.
Background technology
Aluminium hydroxide micropowder is done cable filler and is widely used, the character of aluminium hydroxide micropowder directly affects the characteristic of cable filler: (1) adopts suboxide sodium aluminium hydroxide micropowder to do cable filler, avoids common aluminium hydroxide micropowder because of sodium oxide (Na 2O:0.20~0.30%) the high and covering material of cable insulating property difference that causes of content and shortcoming such as easily aging; Adopt low sodium aluminium hydroxide micropowder to do cable filler, not only can improve the insulating property of goods, but also improve the decomposition temperature of goods when burning, flame retardant properties is further improved.(2) the aluminium hydroxide micropowder oil number is low, can increase the loading level of aluminium hydroxide micropowder, reduces the addition of other high price component, finally reduces the production cost of composite product; The aluminium hydroxide micropowder oil number is low, also can reduce the viscosity of product, and the product flowing property improves, thereby is easy to fill.(3) the aluminium hydroxide micropowder specific conductivity is low, and the anti-electric arc of anti-electric leakage, the ageing resistance of goods are obviously improved, and helps improving the flame retardant properties of product.
The main performance index of existing aluminium hydroxide micropowder product is respectively: purity is 99.5~99.7%, and is refining inadequately; Oil number is 44~50ml/100g, and is higher; The sodium oxide weight content is 0.20~0.30%, and is higher; Specific conductivity is 90~120 μ s.cm -1, higher; The meta particle diameter is 0.4~3 μ m, disperses; Or the like.Its performance awaits further improvement, raising.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of improved aluminium hydroxide micropowder, technical process is simple, operation control can obtain high-quality aluminium hydroxide micropowder product easily, has high purity, low oil absorption ferric, suboxide sodium content, low conductivity characteristics.
The preparation method of aluminium hydroxide micropowder of the present invention, with the sodium aluminate solution is raw material, add aluminium hydroxide crystal seed and carry out kind of a divisional processing, then slurries are carried out liquid-solid separation, separate solid is washed, dries aftertreatment get product, it is characterized in that handling through airflow milling depolymerization and air classification again after the separate solid drying is handled.
Wherein, the airflow milling depolymerization is the depolymerization of comminution by gas stream mill, and the product oil number after the depolymerization reduces greatly, and the comminution by gas stream mill can directly be bought for sophisticated existing installation, and it is respond well to be used to pulverize the former powder of aluminium hydroxide, directly requires to use according to routine to get final product.
The airflow milling principle of work:
Pressurized gas (air or other gas) is by reinforced injector, and the powder raw material that self-feeder is got off is generally below 60 orders; evenly enter pulverizer continuously; simultaneously, pressurized gas produces high velocity air by the pulverizing nozzle of crushiing chamber periphery; spray into crushiing chamber; gas particles is run foul of each other, friction and reach pulverizing purpose, the ultrafine particle after the pulverizing; major part is collected in the cyclonic separation bottom, and gas then sees through filter bag and discharges.General airflow milling main control parameters: air consumption: 18~28m 3/ min pulverizes pressure: 0.6~1.0MPa.
Air classification be mainly used to remove minute quantity in the product macroparticle, scab etc., impel granularity to concentrate uniform distribution.
Crystal seed adopts kind of a branch aluminium hydroxide crystal seed, plants the crystal seed sodium oxide content low (≤0.10%) that divides the aluminium hydroxide product to grind, at present the aluminium hydroxide product sodium oxide content height (0.30% ±) that uses; The meta particle diameter of crystal seed requires less than 1.0 μ m ,+325 purpose particle weight content≤0.02%; The aluminium hydroxide crystal seed even particle size distribution, thus coarsening rate and the degree of agglomeration of each crystal seed in sodium aluminate solution is consistent relatively, makes the even particle size distribution of aluminium hydroxide micropowder product.
In the used sodium aluminate solution of the present invention, alumina content is 95~110g/l, and solution caustic ratio α k is controlled to be 1.4~1.6.
In kind of divisional processing, suitable process control parameter is respectively:
The seed coefficient is controlled to be 6~12%, plants the branch temperature and is controlled to be 50~65 ℃, plants and divides the time to be controlled to be 6~8 hours, and rate of decomposition is controlled at 50~55%.
Confirm through test of many times, the basic mechanical design feature index of the aluminium hydroxide micropowder product that preparation method of the present invention obtains is: purity is greater than 99.8%, the meta particle diameter is 0.7~2.0 μ m, even particle size distribution, the sodium oxide weight content is not more than 0.1%, oil number is not more than 37ml/100g, and specific conductivity is not more than 60 μ s/cm.
Compare with existing aluminium hydroxide micropowder product, preparation method of the present invention has obviously improved quality product, improved the purity of aluminium hydroxide micropowder product, greatly reduce oil number, specific conductivity and the sodium oxide content of product, increase the interpolation umber of aluminium hydroxide micropowder product in electric wire, improved the insulating property of electric wire.
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
The preparation method of aluminium hydroxide micropowder of the present invention, with soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 100g/l, and α k1.44 adds kind of a branch aluminium hydroxide crystal seed down at 54 ℃, the seed coefficient is 8%, resolving time is 7 hours, and rate of decomposition 54% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, the oven dry material evenly enters into crushiing chamber continuously through self-feeder and carries out depolymerization, air consumption: 24m 3/ min pulverizes pressure: 0.8MPa, and the material after the depolymerization is conveyed in the filling tube to be drawn into by blower fan by feeder and carries out classification, rotor speed: 2100r/min, air capacity: 50m in the grading room 3/ min, fine powder is product after packing.The aluminium hydroxide micropowder product purity is 99.83% weight, and the meta particle diameter is 1.0 μ m, and the sodium oxide weight content is 0.1%, and specific conductivity is 47 μ s/cm, and oil number is 36ml/100g, and its chemical ingredients sees Table 1.
Embodiment 2
The preparation method of aluminium hydroxide micropowder of the present invention, with soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 104g/l, and α k1.46 adds kind of a branch aluminium hydroxide crystal seed down at 60 ℃, the seed coefficient is 8%, resolving time is 7 hours, and rate of decomposition 51% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, the oven dry material evenly enters into crushiing chamber continuously through self-feeder and carries out depolymerization, air consumption: 24m 3/ min pulverizes pressure: 0.8MPa, and the material after the depolymerization is conveyed in the filling tube to be drawn into by blower fan by feeder and carries out classification, rotor speed: 2100r/min, air capacity: 50m in the grading room 3/ min, fine powder is product after packing.The aluminium hydroxide micropowder product purity is 99.85% weight, and the meta particle diameter is 1.4 μ m, and the sodium oxide weight content is 0.08%, and specific conductivity is 36 μ s/cm, and oil number is 34ml/100g, and its chemical ingredients sees Table 1.
Embodiment 3
The preparation method of aluminium hydroxide micropowder of the present invention, with soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 98g/l, and α k1.52 adds kind of a branch aluminium hydroxide crystal seed down at 55 ℃, the seed coefficient is 10%, resolving time is 7 hours, and rate of decomposition 55% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, the oven dry material evenly enters into crushiing chamber continuously through self-feeder and carries out depolymerization, air consumption: 24m 3/ min pulverizes pressure: 0.8MPa, and the material after the depolymerization is conveyed in the filling tube to be drawn into by blower fan by feeder and carries out classification, rotor speed: 2100r/min, air capacity: 50m in the grading room 3/ min, fine powder is product after packing.The aluminium hydroxide micropowder product purity is 99.82% weight, and the meta particle diameter is 0.7 μ m, and the sodium oxide weight content is 0.09%, and specific conductivity is 55 μ s/cm, and oil number is 37ml/100g, and its chemical ingredients sees Table 1.
Embodiment 4
The preparation method of aluminium hydroxide micropowder of the present invention, with soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 100g/l, and α k1.48 adds kind of a branch aluminium hydroxide crystal seed down at 62 ℃, the seed coefficient is 10%, resolving time is 7 hours, and rate of decomposition 52% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, the oven dry material evenly enters into crushiing chamber continuously through self-feeder and carries out depolymerization, air consumption: 24m 3/ min pulverizes pressure: 0.8MPa, and the material after the depolymerization is conveyed in the filling tube to be drawn into by blower fan by feeder and carries out classification, rotor speed: 2100r/min, air capacity: 50m in the grading room 3/ min, fine powder is product after packing.The aluminium hydroxide micropowder product purity is 99.85% weight, and the meta particle diameter is 1.2 μ m, and the sodium oxide weight content is 0.07%, and specific conductivity is 28 μ s/cm, and oil number is 35ml/100g, and its chemical ingredients sees Table 1.
Embodiment 5
The preparation method of aluminium hydroxide micropowder of the present invention, with soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 105g/l, and α k1.53 adds kind of a branch aluminium hydroxide crystal seed down at 60 ℃, the seed coefficient is 6%, resolving time is 8 hours, and rate of decomposition 50% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, the oven dry material evenly enters into crushiing chamber continuously through self-feeder and carries out depolymerization, air consumption: 24m 3/ min pulverizes pressure: 0.8MPa, and the material after the depolymerization is conveyed in the filling tube to be drawn into by blower fan by feeder and carries out classification, rotor speed: 2100r/min, air capacity: 50m in the grading room 3/ min, fine powder is product after packing.The aluminium hydroxide micropowder product purity is 99.84% weight, and the meta particle diameter is 1.6 μ m, and the sodium oxide weight content is 0.1%, and specific conductivity is 38 μ s/cm, and oil number is 34ml/100g, and its chemical ingredients sees Table 1.
Embodiment 6
The preparation method of aluminium hydroxide micropowder of the present invention, with soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 100g/l, and α k1.49 adds kind of a branch aluminium hydroxide crystal seed down at 55 ℃, the seed coefficient is 10%, resolving time is 6 hours, and rate of decomposition 53% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, the oven dry material evenly enters into crushiing chamber continuously through self-feeder and carries out depolymerization, air consumption: 24m 3/ min pulverizes pressure: 0.8MPa, and the material after the depolymerization is conveyed in the filling tube to be drawn into by blower fan by feeder and carries out classification, rotor speed: 2100r/min, air capacity: 50m in the grading room 3/ min, fine powder is product after packing.The aluminium hydroxide micropowder product purity is 99.83% weight, and the meta particle diameter is 1.0 μ m, and the sodium oxide weight content is 0.1%, and specific conductivity is 42 μ s/cm, and oil number is 36ml/100g, and its chemical ingredients sees Table 1.
Embodiment 7
The preparation method of aluminium hydroxide micropowder of the present invention, with soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 100g/l, and α k1.44 adds kind of a branch aluminium hydroxide crystal seed down at 65 ℃, the seed coefficient is 12%, resolving time is 8 hours, and rate of decomposition is 50%, decomposes slurries and carries out liquid-solid separation, washing and oven dry, the oven dry material evenly enters into crushiing chamber continuously through self-feeder and carries out depolymerization, air consumption: 24m 3/ min pulverizes pressure: 0.8MPa, and the material after the depolymerization is conveyed in the filling tube to be drawn into by blower fan by feeder and carries out classification, rotor speed: 2100r/min, air capacity: 50m in the grading room 3/ min, fine powder is product after packing.The aluminium hydroxide micropowder product purity is 99.86%, and the meta particle diameter is 1.5 μ m, and the sodium oxide weight content is 0.08%, and specific conductivity is 35 μ s/cm, and oil number is 33ml/100g, and its chemical ingredients sees Table 1.
Embodiment 8
The preparation method of aluminium hydroxide micropowder of the present invention, with soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 100g/l, and α k1.44 adds kind of a branch aluminium hydroxide crystal seed down at 55 ℃, the seed coefficient is 6%, resolving time is 8 hours, and rate of decomposition 51% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, the oven dry material evenly enters into crushiing chamber continuously through self-feeder and carries out depolymerization, air consumption: 24m 3/ min pulverizes pressure: 0.8MPa, and the material after the depolymerization is conveyed in the filling tube to be drawn into by blower fan by feeder and carries out classification, rotor speed: 2100r/min, air capacity: 50m in the grading room 3/ min, fine powder is product after packing.The aluminium hydroxide micropowder product purity is 99.85% weight, and the meta particle diameter is 1.3 μ m, and the sodium oxide weight content is 0.1%, and specific conductivity is 46 μ s/cm, and oil number is 36ml/100g, and its chemical ingredients sees Table 1.
Embodiment 9
The preparation method of aluminium hydroxide micropowder of the present invention, with soda-lime sintering process gained refined sodium aluminate solution, its composition is alumina content 105g/l, and α k1.54 adds kind of a branch aluminium hydroxide crystal seed down at 60 ℃, the seed coefficient is 12%, resolving time is 6 hours, and rate of decomposition 50% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, the oven dry material evenly enters into crushiing chamber continuously through self-feeder and carries out depolymerization, air consumption: 24m 3/ min pulverizes pressure: 0.8MPa, and the material after the depolymerization is conveyed in the filling tube to be drawn into by blower fan by feeder and carries out classification, rotor speed: 2100r/min, air capacity: 50m in the grading room 3/ min, fine powder is product after packing.The aluminium hydroxide micropowder product purity is 99.84% weight, and the meta particle diameter is 1.2 μ m, and the sodium oxide weight content is 0.09%, and specific conductivity is 40 μ s/cm, and oil number is 35ml/100g, and its chemical ingredients sees Table 1.
(continued on next page)
Table 1, product analysis be table as a result
Figure A20061004210000081

Claims (4)

1, a kind of preparation method of aluminium hydroxide micropowder, with the sodium aluminate solution is raw material, add aluminium hydroxide crystal seed and carry out kind of a divisional processing, then slurries are carried out liquid-solid separation, separate solid is washed, dries aftertreatment obtain product, it is characterized in that handling through airflow milling depolymerization and air classification again after the separate solid drying is handled.
2, the preparation method of aluminium hydroxide micropowder according to claim 1 is characterized in that crystal seed adopts kind of a branch aluminium hydroxide crystal seed.
3, the preparation method of aluminium hydroxide micropowder according to claim 1 and 2 is characterized in that in the used sodium aluminate solution that alumina content is 95~110g/l, and solution caustic ratio α k is 1.4~1.6.
4, the preparation method of aluminium hydroxide micropowder according to claim 3 is characterized in that in kind of the divisional processing, the seed coefficient is controlled to be 6~12%, plants the branch temperature and is controlled to be 50~65 ℃, plants and divides the time to be controlled to be 6~8 hours, and rate of decomposition is controlled at 50~55%.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100378000C (en) * 2006-08-25 2008-04-02 中国铝业股份有限公司 Method for producing micropowder aluminium hydroxide by neutralization method
WO2010096974A1 (en) * 2009-02-24 2010-09-02 河南未来铝业(集团)有限公司 Method for preparing aluminum hydroxide and use of combination of methanol and inducer in process for preparing aluminum hydroxide
CN109626406A (en) * 2018-12-10 2019-04-16 贵州博汇联润铝业有限公司 A kind of ultra-fine ultrawhite aluminum hydroxide micro mist preparation method
CN110655095A (en) * 2019-10-16 2020-01-07 淄博鹏丰铝业有限公司 Preparation method of low-oil-absorption-value aluminum hydroxide micropowder flame retardant
CN114436302A (en) * 2022-01-10 2022-05-06 中铝山东新材料有限公司 Particulate aluminum hydroxide, preparation method, production system and application thereof

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KR100632720B1 (en) * 1997-11-28 2006-10-16 꽁빠니 제네랄 드 에따블리세망 미쉘린-미쉘린 에 씨 Reinforcing aluminous filler, a process for manufacturing said filler, a rubber composition comprising said filler, and a tyre and a tread for a tyre, reinforced with said filler
US6221233B1 (en) * 1999-03-08 2001-04-24 John S. Rendall Aluminum production utilizing positively charged alumina
CN1162513C (en) * 2002-12-03 2004-08-18 中国铝业股份有限公司 Process for preparing aluminium hydroxide fire retardant
CN1278938C (en) * 2004-06-18 2006-10-11 中国铝业股份有限公司 Preparation method low electric conductiving super fine aluminium hydroxide micro powder
CN1285510C (en) * 2004-10-27 2006-11-22 上海大学 Prepn process of nano aluminium hydroxide

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100378000C (en) * 2006-08-25 2008-04-02 中国铝业股份有限公司 Method for producing micropowder aluminium hydroxide by neutralization method
WO2010096974A1 (en) * 2009-02-24 2010-09-02 河南未来铝业(集团)有限公司 Method for preparing aluminum hydroxide and use of combination of methanol and inducer in process for preparing aluminum hydroxide
CN109626406A (en) * 2018-12-10 2019-04-16 贵州博汇联润铝业有限公司 A kind of ultra-fine ultrawhite aluminum hydroxide micro mist preparation method
CN109626406B (en) * 2018-12-10 2021-03-16 贵州博汇联润铝业有限公司 Preparation method of superfine ultra-white aluminum hydroxide micro powder
CN110655095A (en) * 2019-10-16 2020-01-07 淄博鹏丰铝业有限公司 Preparation method of low-oil-absorption-value aluminum hydroxide micropowder flame retardant
CN110655095B (en) * 2019-10-16 2021-11-30 淄博鹏丰新材料科技有限公司 Preparation method of low-oil-absorption-value aluminum hydroxide micropowder flame retardant
CN114436302A (en) * 2022-01-10 2022-05-06 中铝山东新材料有限公司 Particulate aluminum hydroxide, preparation method, production system and application thereof
CN114436302B (en) * 2022-01-10 2024-08-27 中铝山东新材料有限公司 Particulate aluminum hydroxide, preparation method, production system and application thereof

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