CN1587053A - Purifying method for trace silicon in removing alumino-alkoxide - Google Patents
Purifying method for trace silicon in removing alumino-alkoxide Download PDFInfo
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- CN1587053A CN1587053A CN 200410050332 CN200410050332A CN1587053A CN 1587053 A CN1587053 A CN 1587053A CN 200410050332 CN200410050332 CN 200410050332 CN 200410050332 A CN200410050332 A CN 200410050332A CN 1587053 A CN1587053 A CN 1587053A
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- Prior art keywords
- aluminium
- alcohol salt
- alkoxide
- transforming agent
- silicon
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention provides a purification method of removing trace silicon from alumino-alkoxide, and relates to the deep desilication technology of alumino-alkoxide as the precursor of high purity superfine alumina. The present invention features that industrial aluminum ingot as material is reacted with alcohol to produce alumino-alkoxide. During synthesizing alkoxide, trace converting agent is added to convert the produced low boiling point silicon-containing organic matter into high boiling point one; and alumino-alkoxide with low boiling point is first distilled out in decompression distillation of alkoxide while the high boiling point silicon-containing organic matter is distilled out lastly. Thus, collecting the first 90-95 wt% fraction may reach the aim of eliminating impurity silicon. The present invention can reduce the silicon content from 50-200 ppm to below 8 ppm.
Description
Technical field
The invention belongs to inorganic materials purification technique field, specially refer to the deep desilication technology of high-purity ultra-fine alumina precursor-aluminium-alcohol salt.
Background technology
High-purity ultra-fine alumina demonstrates special role and superiority in fields such as luminescent material, electronic substrates, window material, far-infrared material and biological ceramicss as important inorganic materials/starting material.Aluminium-alcohol salt is the important precursor of this aluminum oxide of preparation, has the product purity height, granularity is ultra-fine, particle shape is easy to control and does not cause characteristics such as environmental pollution, has therefore realized suitability for industrialized production both at home and abroad.But, generally (press Al at 50～200ppm by its sila matter content of aluminum oxide that aluminium-alcohol salt is prepared
2O
3Meter) in the scope, can not satisfy raw material index or product performance requirement for some specific function materials.For this reason, the invention provides a kind of technology of aluminium-alcohol salt deep desilication.
Summary of the invention
The purpose of this invention is to provide a kind of simple industrialization technology, trace silicon in the aluminium-alcohol salt is removed, purify the back product purity at 99.99% (Al
2O
3Meter) more than, wherein silicone content is at 8ppm (Al
2O
3Meter) below.
Technical scheme of the present invention is, with industrial aluminium ingot is raw material, it is added the alkoxide that carries out back flow reaction generation aluminium in the alcohol, in reflux course, add a kind of trace chemistry transforming agent simultaneously, make itself and the lower boiling silicon-containing compound that generates carry out conversion reaction, form the high boiling point silicon-containing compound, utilize the lower boiling character of aluminium-alcohol salt to carry out underpressure distillation then, the siliceous impurity of high boiling point is left in the still kettle, thereby reaches the purpose of purifying.Here, transforming agent kind and consumption are the important factors that influences the silica removal effect.
Effect of the present invention and benefit be, the desiliconization technology of utilizing the present invention to propose can make in the aluminium-alcohol salt silicone content by 50～200ppm (Al of common underpressure distillation
2O
3Meter) reduces to below the 8ppm.The high-purity ultra-fine alumina purity that obtains after the aluminium-alcohol salt hydrolysis is more than 99.99%, and prior application prospect will will be used widely and have in this low silicon or alumina powder jointed electronic material or the field such as window material in special purpose of not having silicon.
Embodiment
Below be described in detail the specific embodiment of the present invention.
Trace silicon removal methods in the aluminium-alcohol salt of the present invention is characterized in that transforming agent kind selected in the aluminium-alcohol salt synthetic reaction process and formula rate (weight ratio) thereof are as follows:
Transforming agent is chosen in containing the compound of rare earth element in the prescription, and transforming agent can contain the rare earth element more than 2 kinds simultaneously.
The weight ratio of transforming agent and metallic aluminium is 1: 20～1: 1000 in the prescription.Do suitable adjustment according to silicone content in the aluminium.The technical process of whole purification technique is as follows:
Step 1: synthetic aluminium-alcohol salt and lower boiling contain the conversion of silicide: with the Industrial Metal aluminium ingot is raw material, be cut into behind the fragment under normal pressure to return and heat up in a steamer reaction and make aluminium generate aluminium-alcohol salt with anhydrous organic alcohol, the transforming agent that adds specified rate when adding aluminium flake makes itself and the lower boiling sila matter that generates carry out conversion reaction, so that form high boiling silicon-containing compound.Add little amount of catalyst (HgCl when synthesizing aluminium-alcohol salt for the first time
2Deng), be that activator gets final product with the distillation recrement later on.
Step 2: the distillation purifying of aluminium-alcohol salt: after reaction is carried out fully in step 1, steam unreacted organic alcohol earlier under normal pressure, carry out underpressure distillation then, distillation pressure generally is controlled at below the 12mmHg, and corresponding temperature is no more than 160 ℃.When distillation fraction reaches the about 95%wt of aluminium-alcohol salt total amount, switch the product receptor, remainder is received in another container.The silicone content of its front-end volatiles aluminium-alcohol salt (Al below 8ppm
2O
3Meter), the iron of after cut aluminium-alcohol salt and other foreign matter content are higher, as substandard products or other purposes product treatment.
Below provide most preferred embodiment of the present invention.
With 100 kilograms of Al
2O
3Be example, get 55 kilograms of metal aluminium flakes, 400 kilograms of anhydrous isopropyl alcohols, transforming agent (in the compound that contains lanthanum, europium or dysprosium, choosing) 0.5 gram and join to return in the reactor that has a heating jacket and heat up in a steamer the preparation aluminum isopropylate, will generate about 400 kilograms of aluminum isopropylates.In this reactor or with reaction solution, pour in another reactor after reaction finishes and distill.Earlier under normal pressure, distill out unnecessary Virahol, carry out underpressure distillation then.In the speed stabilizing still-process, collect about about 370 kilograms of front-end volatiles.This cut is the rafifinal alkoxide, and its hydrolysis, drying and calcining are obtained silicone content less than the 8ppm high purity alumina powder.
Claims (3)
1. purification process that removes trace silicon in the aluminium-alcohol salt is characterized in that transforming agent kind selected in the aluminium-alcohol salt synthetic reaction process and formula rate (weight ratio) thereof are as follows:
Transforming agent is chosen in containing the compound of rare earth element in the prescription, can contain rare earth element more than 2 kinds simultaneously in the transforming agent;
The weight ratio of transforming agent and metallic aluminium is 1: 20～1: 1000 in the prescription; The technical process of purification process is as follows:
(1) synthetic aluminium-alcohol salt and lower boiling contain the conversion of silicide: with the Industrial Metal aluminium ingot is raw material, be cut into behind the fragment under normal pressure to return and heat up in a steamer reaction and make aluminium generate aluminium-alcohol salt with anhydrous organic alcohol, when adding aluminium flake, add the specified rate transforming agent and make itself and the lower boiling sila matter that generates carry out conversion reaction, so that form high boiling siliceous organism;
(2) distillation purifying of aluminium-alcohol salt: after the alkoxide building-up reactions is carried out fully, steam unreacted organic alcohol earlier under normal pressure, carry out underpressure distillation then, distillation pressure generally is controlled at below the 12mmHg, and corresponding temperature is no more than 160 ℃; When distillation fraction reaches 90%～95%wt of aluminium-alcohol salt total amount, switch the product receptor, remainder is received in another container; The silicone content of its front-end volatiles aluminium-alcohol salt (Al below 8ppm
2O
3Meter).
2. a kind of purification process that removes trace silicon in the aluminium-alcohol salt according to claim 1, the weight ratio of transforming agent and metallic aluminium is 1: 20～1: 1000 in it is characterized in that filling a prescription, and does suitable adjustment according to silicone content in the aluminium.
3. a kind of purification process that removes trace silicon in the aluminium-alcohol salt according to claim 1 is characterized in that can containing rare earth more than 2 kinds simultaneously in the described transforming agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410050332 CN1290769C (en) | 2004-08-26 | 2004-08-26 | Purifying method for trace silicon in removing alumino-alkoxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410050332 CN1290769C (en) | 2004-08-26 | 2004-08-26 | Purifying method for trace silicon in removing alumino-alkoxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1587053A true CN1587053A (en) | 2005-03-02 |
| CN1290769C CN1290769C (en) | 2006-12-20 |
Family
ID=34602225
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410050332 Expired - Fee Related CN1290769C (en) | 2004-08-26 | 2004-08-26 | Purifying method for trace silicon in removing alumino-alkoxide |
Country Status (1)
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|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948090A (en) * | 2016-06-14 | 2016-09-21 | 袁伟昊 | Ultra-pure nano-alumina green synthesis method and industrialization device |
| CN111187147A (en) * | 2020-01-13 | 2020-05-22 | 大连理工大学 | Process for continuously synthesizing aluminum alkoxide |
-
2004
- 2004-08-26 CN CN 200410050332 patent/CN1290769C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948090A (en) * | 2016-06-14 | 2016-09-21 | 袁伟昊 | Ultra-pure nano-alumina green synthesis method and industrialization device |
| CN111187147A (en) * | 2020-01-13 | 2020-05-22 | 大连理工大学 | Process for continuously synthesizing aluminum alkoxide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1290769C (en) | 2006-12-20 |
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Granted publication date: 20061220 Termination date: 20090928 |