CN101182021A - Method for preparing beta-type aluminum hydroxide - Google Patents

Method for preparing beta-type aluminum hydroxide Download PDF

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Publication number
CN101182021A
CN101182021A CNA2007101161621A CN200710116162A CN101182021A CN 101182021 A CN101182021 A CN 101182021A CN A2007101161621 A CNA2007101161621 A CN A2007101161621A CN 200710116162 A CN200710116162 A CN 200710116162A CN 101182021 A CN101182021 A CN 101182021A
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aluminum hydroxide
beta
type aluminum
solution
carbon dioxide
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张蕾
王世全
苏爱玲
栾福森
王智锦
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Aluminum Corp of China Ltd
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Aluminum Corp of China Ltd
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Abstract

The invention relates to a preparation method of Beta-type aluminum hydroxide, which is used for preparing the Beta-type aluminum hydroxide. Sodium aluminate solution is used as raw material, neutralized by feeding carbon dioxide and then is treated with filtering washing and drying to obtain the Beta-type aluminum hydroxide product. The preparation method is characterized in that Beta-type aluminum hydroxide seeds are added before the carbon dioxide is fed so as to produce the Beta-type aluminum hydroxide product with high purity and large specific surface area; in addition, the method has simple production technology, easy control of particle size and easy manipulation of the operation process.

Description

The preparation method of Beta-type aluminum hydroxide
Technical field
The present invention relates to a kind of preparation method of Beta-type aluminum hydroxide, be used to produce Beta-type aluminum hydroxide.
Background technology
The production method of Beta-type aluminum hydroxide has a variety of, and domestic relevant patent documentation has:
Application number is the preparation method of 90105317.1 Beta-type aluminum hydroxide, and the refined sodium aluminate solution alumina content is controlled to be 35~45g/l, feeds the carbon dioxides neutralization at 35~45 ℃, and gas feeding speed is 30~50m 3/ hour m 3Solution, aeration time are 60~70 minutes, degradation production under 70~100 ℃ of temperature aging 1~6 hour, and after filtration, washing and oven dry finally obtain the Beta-type aluminum hydroxide product, its purity reaches 70~80%, specific surface 200m 2About/g.The sodium aluminate solution alumina concentration is not high in this scheme, needs to wear out, and product purity is not enough, and specific surface is relatively low.
Application number is the preparation method of 00132219.2 Beta-type aluminum hydroxide, the refined sodium aluminate solution alumina content is controlled to be 85~100g/l, solution caustic ratio (α k) 1.4~1.6, at 40~70 ℃ of carbon dioxides that feed concentration 35~40% down, gas feeding amount is 100~150m 3/ hour m 3Solution, aeration time are 60~90 minutes, rate of decomposition 88~90%, and obtaining product Beta-type aluminum hydroxide content is more than 97%.Do not relate to specific surface in this scheme, through experimental verification, the specific surface of product is 150~250m 2/ g, carbon dioxide feeding amount is bigger.
Application number is the production method of 200510104601.8 Beta-type aluminum hydroxide, is raw material with the sodium aluminate solution, and its alumina content is 45~65g/l, and caustic ratio (α k) 1.4~1.6 under 15~35 ℃ of temperature, feeds concentration and be 30~40% CO 2Gas, in and after 15~25 minutes, stop to feed carbon dioxide gas, continue after 20~30 minutes to feed carbon dioxide gas, the whole aeration time of carbonic acid gas are 40~90 minutes, and rate of decomposition is controlled at 65~88%, resulting Beta-type aluminum hydroxide purity is 90~99%, specific surface 300~500m 2/ g.The sodium aluminate solution alumina concentration is not high in this scheme, and rate of decomposition is lower, decomposes the system relative complex, the granularity control difficulty of product.。
Summary of the invention
The object of the present invention is to provide a kind of preparation method of Beta-type aluminum hydroxide, can produce purity height, Beta-type aluminum hydroxide product that specific surface is big, the technological process of production is simple, and granularity is controlled easily, and operating process is easy to grasp.
The preparation method of Beta-type aluminum hydroxide of the present invention, with the sodium aluminate solution is raw material, feeds carbon dioxide and neutralizes, more after filtration, washing and oven dry, obtain the Beta-type aluminum hydroxide product, it is characterized in that before feeding carbon dioxide, adding the Beta-type aluminum hydroxide seed.
The Beta-type aluminum hydroxide seed can adopt wet pulverization to become d 50Be 0.5~10 μ m, also can adopt dry method can be ground into d 50Be 10~20 μ m.
The better processing condition of suitable control are among the present invention:
Alumina content is 45~75g/l in the sodium aluminate solution, and the solution caustic ratio is 1.4~1.6.
Under 15~35 ℃ of temperature, add the Beta-type aluminum hydroxide seed of 1~10g/l, the d of Beta-type aluminum hydroxide seed 50Be 0.5~20 μ m.
The mass concentration of carbon dioxide is 30~40%, in and the time be 40~90 minutes.
Rate of decomposition is controlled at 65~95%.
The present invention is owing to added the Beta-type aluminum hydroxide seed, when decomposing, play guiding function, the stability of quality product is greatly improved, and alumina content is improved in the sodium aluminate solution, has improved rate of decomposition and productive rate, improved the specific surface of Beta-type aluminum hydroxide, the quality of Beta-type aluminum hydroxide product is good, and the technological process of production is simple, and granularity is controlled easily, operating process is easy to grasp, and is beneficial to industrial implementation.
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 are alumina content 110g/l, and α k1.44 towards rare alumina content 50.3g/l that arrives, down adds 7kg/m at 20 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 2.5 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 40m 3/ hour m 3Solution decomposed 70 minutes, and rate of decomposition 90% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 99.0%, specific surface 445m 2/ g, d 50Be 25.6 μ m, its materialization the results are shown in Table 1.
Embodiment 2
Soda-lime sintering process gained refined sodium aluminate solution, its composition are alumina content 110g/l, and α k1.44 towards rare alumina content 50.3g/l that arrives, down adds 1kg/m at 15 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 0.5 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 30m 3/ hour m 3Solution decomposed 90 minutes, and rate of decomposition 93% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 94.4%, specific surface 485m 2/ g, d 50Be 31.8 μ m, its materialization the results are shown in Table 1.
Embodiment 3
Soda-lime sintering process gained refined sodium aluminate solution, its composition are alumina content 110g/l, and α k1.44 towards rare alumina content 50.3g/l that arrives, down adds 4kg/m at 25 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 10.6 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 40m 3/ hour m 3Solution decomposed 70 minutes, and rate of decomposition 90% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 92.2%, specific surface 386m 2/ g, d 50Be 38.6 μ m, its materialization the results are shown in Table 1.
Embodiment 4
Soda-lime sintering process gained refined sodium aluminate solution, its composition are alumina content 110g/l, and α k1.44 towards rare alumina content 50.3g/l that arrives, down adds 10kg/m at 35 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 18.9 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 3m 3/ hour m 3Solution decomposed 90 minutes, and rate of decomposition 98% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 93.0%, specific surface 357m 2/ g, d 50Be 36.3 μ m, its materialization the results are shown in Table 1.
Embodiment 5
Soda-lime sintering process gained refined sodium aluminate solution, its composition are alumina content 110g/l, and α k1.44 towards rare alumina content 35.7g/l that arrives, down adds 1kg/m at 20 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 10.6 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 30m 3/ hour m 3Solution decomposed 70 minutes, and rate of decomposition 96% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 94.3%, specific surface 405m 2/ g, d 50Be 48.7 μ m, its materialization the results are shown in Table 1.
Embodiment 6
Soda-lime sintering process gained refined sodium aluminate solution, its composition are alumina content 110g/l, and α k1.44 towards rare alumina content 35.7g/l that arrives, down adds 7kg/m at 15 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 18.9 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 40m 3/ hour m 3Solution decomposed 50 minutes, and rate of decomposition 96% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 91.6%, specific surface 427m 2/ g, d 50Be 29.6 μ m, its materialization the results are shown in Table 1.
Embodiment 7
Soda-lime sintering process gained refined sodium aluminate solution, its composition are alumina content 110g/l, and α k1.44 towards rare alumina content 35.7g/l that arrives, down adds 10kg/m at 25 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 2.5 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 40m 3/ hour m 3Solution decomposed 40 minutes, and rate of decomposition 75% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 96.0%, specific surface 427m 2/ g, d 50Be 18.3 μ m, its materialization the results are shown in Table 1.
Embodiment 8
Soda-lime sintering process gained refined sodium aluminate solution, its composition are alumina content 110g/l, and α k1.44 towards rare alumina content 35.7g/l that arrives, down adds 4kg/m at 35 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 0.5 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 40m 3/ hour m 3Solution decomposed 50 minutes, and rate of decomposition 90% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 92.7%, specific surface 475m 2/ g, d 50Be 24.3 μ m, its materialization the results are shown in Table 1.
Embodiment 9
Soda-lime sintering process gained refined sodium aluminate solution, its composition are alumina content 110g/l, and α k1.44 towards rare alumina content 65.9g/l that arrives, down adds 4kg/m at 20 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 18.9 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 40m 3/ hour m 3Solution decomposed 60 minutes, and rate of decomposition 65% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 96.0%, specific surface 386m 2/ g, d 50Be 35.8 μ m, its materialization the results are shown in Table 1.
Embodiment 10
Soda-lime sintering process gained refined sodium aluminate solution, its composition are alumina content 110g/l, and α k1.44 towards rare alumina content 65.9g/l that arrives, down adds 10kg/m at 15 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 10.6 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 40m 3/ hour m 3Solution decomposed 90 minutes, and rate of decomposition 94% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 91.0%, specific surface 414m 2/ g, d 50Be 24.9 μ m, its materialization the results are shown in Table 1.
Embodiment 11
Soda-lime sintering process gained refined sodium aluminate solution, its composition are alumina content 110g/l, and α k1.44 towards rare alumina content 65.9g/l that arrives, down adds 7kg/m at 25 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 0.5 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 40m 3/ hour m 3Solution decomposed 70 minutes, and rate of decomposition 85% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 99.0%, specific surface 438m 2/ g, d 50Be 19.6 μ m, its materialization the results are shown in Table 1.
Embodiment 12
Soda-lime sintering process gained refined sodium aluminate solution, its composition are alumina content 110g/l, and α k1.44 towards rare alumina content 65.9g/l that arrives, down adds 1kg/m at 35 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 2.5 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 40m 3/ hour m 3Solution decomposed 90 minutes, and rate of decomposition 95% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 95.4%, specific surface 375m 2/ g, d 50Be 38.6 μ m, its materialization the results are shown in Table 1.
Embodiment 13
Soda-lime sintering process gained refined sodium aluminate solution, its composition are alumina content 110g/l, and α k1.44 towards rare alumina content 74.8g/l that arrives, down adds 10kg/m at 20 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 0.5 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 40m 3/ hour m 3Solution decomposed 70 minutes, and rate of decomposition 65% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 93.0%, specific surface 398m 2/ g, d 50Be 18.6 μ m, its materialization the results are shown in Table 1.
Embodiment 14
Soda-lime sintering process gained refined sodium aluminate solution, its composition are alumina content 110g/l, and α k1.44 towards rare alumina content 74.8g/l that arrives, down adds 4kg/m at 15 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 2.5 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 40m 3/ hour m 3Solution decomposed 80 minutes, and rate of decomposition 99% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 96.7%, specific surface 445m 2/ g, d 50Be 35.1 μ m, its materialization the results are shown in Table 1.
Embodiment 15
Soda-lime sintering process gained refined sodium aluminate solution, its composition are alumina content 110g/l, and α k1.44 towards rare alumina content 74.8g/l that arrives, down adds 7kg/m at 35 ℃ with distilled water 3The Beta-type aluminum hydroxide seed of solution, the granularity d of Beta-type aluminum hydroxide seed 50Be 10.6 μ m, feed the carbon dioxide of concentration 36%, ventilation speed is 30m 3/ hour m 3Solution decomposed 90 minutes, and rate of decomposition 96% is decomposed slurries and carried out liquid-solid separation, washing and oven dry, and obtaining Beta-type aluminum hydroxide purity is 91.3%, specific surface 367m 2/ g, d 50Be 31.8 μ m, its materialization the results are shown in Table 1.
(table 1 vides infra)
Table 1, product analysis be table (weight percent) as a result
Figure S2007101161621D00061

Claims (5)

1. the preparation method of a Beta-type aluminum hydroxide, with the sodium aluminate solution is raw material, feeds carbon dioxide and neutralizes, more after filtration, washing and oven dry, obtain the Beta-type aluminum hydroxide product, it is characterized in that before feeding carbon dioxide, adding the Beta-type aluminum hydroxide seed.
2. the preparation method of Beta-type aluminum hydroxide according to claim 1 is characterized in that alumina content is 45~75g/l in the sodium aluminate solution, and the solution caustic ratio is 1.4~1.6.
3. the preparation method of Beta-type aluminum hydroxide according to claim 1 and 2 is characterized in that under 15~35 ℃ of temperature, adds the Beta-type aluminum hydroxide seed of 1~10g/l, the d of Beta-type aluminum hydroxide seed 50Be 0.5~20 μ m.
4. the preparation method of Beta-type aluminum hydroxide according to claim 3, the mass concentration that it is characterized in that carbon dioxide is 30~40%, in and the time be 40~90 minutes.
5. the preparation method of Beta-type aluminum hydroxide according to claim 4 is characterized in that rate of decomposition is controlled at 65~95%.
CNA2007101161621A 2007-12-11 2007-12-11 Method for preparing beta-type aluminum hydroxide Pending CN101182021A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101837999A (en) * 2010-06-10 2010-09-22 中国铝业股份有限公司 Preparation method of Beta-type aluminum hydroxide
CN115231596A (en) * 2022-08-05 2022-10-25 洛阳中超新材料股份有限公司 Industrial preparation method of bayer stone

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101837999A (en) * 2010-06-10 2010-09-22 中国铝业股份有限公司 Preparation method of Beta-type aluminum hydroxide
CN101837999B (en) * 2010-06-10 2012-08-01 中国铝业股份有限公司 Preparation method of Beta-type aluminum hydroxide
CN115231596A (en) * 2022-08-05 2022-10-25 洛阳中超新材料股份有限公司 Industrial preparation method of bayer stone

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