CN102491391A - Preparation method for high-purity alumina - Google Patents
Preparation method for high-purity alumina Download PDFInfo
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- CN102491391A CN102491391A CN2011104160612A CN201110416061A CN102491391A CN 102491391 A CN102491391 A CN 102491391A CN 2011104160612 A CN2011104160612 A CN 2011104160612A CN 201110416061 A CN201110416061 A CN 201110416061A CN 102491391 A CN102491391 A CN 102491391A
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Abstract
A preparation method for high-purity alumina powder includes: preparing aluminum alkoxide in liquid state at the room temperature by means of reaction of metallic aluminum with sec-butyl alcohol, using the reduced pressure distillation method for purifying, and preparing the high-purity alumina powder by means of hydrolyzing, reduced pressure distillation and calcinations. Using the method to prepare high-purity alumina powder has the advantages of simple preparation process, no pollution, low energy consumption, fine operating conditions, zero emission and the like. The alumina powder prepared by the method is applicable to the field of catalysts and can also be applied to the fields of laser crystals, sapphires, transparent alumina ceramics, sodium lamps, metal halides, high-grade abrasives and the like.
Description
Technical field
The present invention relates to a kind of preparation method of high-purity alpha-alumina, belong to catalyst preparation technical field.
Background technology
A kind of high purity alumina powder technology of preparing, the metal alkoxide that adopts methodology of organic synthesis to utilize metallic aluminium and the synthetic room temperature of organic alcohol to be in a liquid state prepares high purity alumina powder through purification, hydrolysis, hydrothermal treatment consists, drying under reduced pressure and calcining process.It is pollution-free that the present invention has technological process, and the synthetic alkoxide is easy to transport, and hydrolytic process good uniformity, alcohol reclaim convenient controlled, characteristics such as the good dispersivity of product powder, granularity and controllable size distribution.
Along with the develop rapidly of high-tech industry, the demand of high purity alumina powder is increased day by day, market outlook are very wide.At present, China's high-pressure sodium fluorescent tube output is up to 100,000,000, and aluminum oxide IC substrate annual requirement is above 1,000,000 square metres.Products such as sapphire IC substrate, Metal-halogen lamp, automobile fluorescent tube and digital form also put goods on the market successively; According to preresearch estimates, only China market can be up to more than 10,000 tons to the annual requirement of high purity alumina powder; The amount of money is up to 8,000,000,000 yuans, and the world market scale is then more considerable.
The method that China prepares high purity aluminium oxide at present mainly contains two kinds of methods; A kind of is aluminium carbonate amine thermolysis process, and the alumina powder jointed purity of this method preparation does not reach the 5N level, and another kind of method is to adopt aluminum isopropylate preparing alumina by hydrolysis powder; Though this method can obtain the very high powder of purity; But in the preparation process, exist the aluminum isopropylate room temperature to solidify, easy blocking pipeline in operating process, hard transportation; Need hydrolysis under the temperature more than 80 ℃ during hydrolysis, shortcoming such as hydrolytic process is restive.To the problem that exists in the existing high purity aluminium oxide technology of preparing, research is adopted under a kind of room temperature and is in a liquid state, and has good fluidity, and the aluminium-alcohol salt that is easy to again purify simultaneously prepares high purity aluminium oxide, is very necessary to overcoming the problem that exists in the prior art.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of high-purity alpha-alumina; In the preparation process; Prepare the aluminium-alcohol salt that is in a liquid state under the room temperature, prepare purity up to 99.99～99.999% high purity alumina powder through purification, hydrolysis, decompression and calcining process.The present invention has simple, pollution-free, the characteristics such as energy consumption is low, good operation conditions, zero release of preparation technology.
Preparation high-purity hydrogen method of alumina of the present invention is characterized in that comprising the steps:
1. with raw materials mix, react 3～8h down at 80～100 ℃; Wherein, described mixing raw material is formed by following part by weight:
Metallic aluminium 10～25
Sec-butyl alcohol 75～90
HgCl
2 0.001～0.003；
Wherein, the purity of metallic aluminium is more than 99.99%;
2. aluminium-alcohol salt filters, and underpressure distillation gets the liquid aluminium alkoxide;
3. normal temperature under the agitation condition, adds aqueous sec-butyl alcohol in the liquid aluminium alkoxide, is hydrolyzed;
4. mixing liquid is 3. carried out underpressure distillation, get aluminium hydroxide powder;
5. aluminium hydroxide powder is calcined.
In the above-mentioned reaction process, carry out underpressure distillation, effectively improve the purity of aluminium-alcohol salt, the condition of providing convenience for the processing in later stage through the synthetic aluminium-alcohol salt that obtains.The underpressure distillation condition that the inventor selected for use is 190～210 ℃, carries out under 1mmHg～10mmHg.
Further hydrolysis adds aqueous sec-butyl alcohol and controls the aluminium-alcohol salt hydrolysis rate, can make the even hydrolysis of aluminium-alcohol salt, and the water cut of preferred sec-butyl alcohol is 15wt%; The mol ratio of aluminium-alcohol salt and water is 1: 2～6; Preferred hydrolysis time is 1～3h.
In the above-mentioned reaction process of the present invention, through underpressure distillation separation of hydrogen aluminum oxide and sec-butyl alcohol, underpressure distillation is under 80～99 ℃, to carry out; And isolated sec-butyl alcohol after the underpressure distillation; Can be used for the raw material of step in 1., reach the raw material reusable edible, realized reducing the preparation cost of product.
In the above-mentioned reaction process of the present invention, under 1200 ℃, obtain the alumina powder jointed calcining of high-purity hydrogen 3h alumina powder jointed.
It is thus clear that the present invention has the following advantages:
Prepare a kind of aluminium-alcohol salt; This alkoxide not only at room temperature is in a liquid state; Can also pass through simultaneously vacuum distillation method and purify, so this aluminium-alcohol salt can also guarantee the particularity of product hydrolysis control and the high purity of product under assurance flowability and transport property condition.Alcohol that is adopted and water have certain solubleness, thereby both can guarantee the even hydrolysis of aluminium-alcohol salt, simultaneously the also accurate add-on of water in the control hydrolysis process.Through the control hydrolysis process, fully carry out obtaining absolute alcohol simultaneously under the prerequisite in the assurance hydrolysis, help the recycle of alcohol, thereby reduce the preparation cost of product greatly.Adopt the high purity alumina powder of method preparation of the present invention, realized outstanding characteristics such as preparation technology is simple, pollution-free, energy consumption is low, good operation conditions, zero release in the preparation process.
Description of drawings
Accompanying drawing 2 width of cloth of the present invention,
Fig. 1 is the sem photograph of embodiment 1;
Fig. 2 is the X ray diffracting spectrum of embodiment, and wherein, a is the X ray diffracting spectrum of embodiment 1; B is the X ray diffracting spectrum of embodiment 2; C is the X ray diffracting spectrum of embodiment 3.
Embodiment
Following non-limiting example can make those of ordinary skill in the art more fully understand the present invention, but does not limit the present invention in any way.As there is not specified otherwise, employed synthesis reactor among the present invention (DN800/900, the great pressurized vessel in sky, Yangzhou ltd).
Embodiment 1
Get purity and be 99.996% metallic aluminium 0.5kg, sec-butyl alcohol 4kg, HgCl
2For 0.1g joins in the synthesis reactor, under refluxad, be heated to 90 ℃, reaction 6h, reaction finishes.The mixed solution that obtains is drawn into capable underpressure distillation through filtration, and under 190 ℃, underpressure distillation under the 10mmHg vacuum obtains the aluminium-alcohol salt that room temperature is in a liquid state.Room temperature is that the 6.67kg sec-butyl alcohol of 15wt% slowly joins in the aluminium-alcohol salt with water cut under the agitation condition, and the mol ratio of aluminium-alcohol salt and water remained on 1: 3, fully behind the hydrolysis 1h, under 80 ℃, carried out underpressure distillation, steamed unnecessary alcohol, obtained aluminium hydroxide powder.1200 ℃ down calcining 3h obtain purity be 99.999% alumina powder jointed.Shown in Fig. 2 a, each diffraction peak is the characteristic diffraction peak of aluminum oxide.It is alumina powder jointed to adopt the atomic spectrum quantitative analysis tech to analyze, and test result is as shown in table 1, can find out the alumina impurity content prepared through this method seldom, and finds out that through SEM (as shown in Figure 1) size distribution of aluminum oxide is more even.
Embodiment 2
Get purity and be 99.996% metallic aluminium 0.75kg, sec-butyl alcohol 4.5kg, HgCl
2For 0.3g joins in the synthesis reactor, under refluxad, be heated to 90 ℃, reaction 6h, reaction finishes.The mixed solution that obtains is drawn into capable underpressure distillation through filtration, and under 190 ℃, underpressure distillation under the 10mmHg vacuum obtains the aluminium-alcohol salt that room temperature is in a liquid state.Room temperature is that the 13.33kg sec-butyl alcohol of 15wt% slowly joins in the aluminium-alcohol salt with water cut under the agitation condition, and the mol ratio of aluminium-alcohol salt and water remained on 1: 4, fully behind the hydrolysis 2h, under 80 ℃, carried out underpressure distillation, steamed unnecessary alcohol, obtained aluminium hydroxide powder.1200 ℃ down calcining 3h obtain purity be 99.999% alumina powder jointed.Shown in Fig. 2 b, each diffraction peak is the characteristic diffraction peak of aluminum oxide.
Embodiment 3
Get purity and be 99.996% metallic aluminium 1.25kg, sec-butyl alcohol 3.75kg, HgCl
2For 0.2g joins in the synthesis reactor, under refluxad, be heated to 90 ℃, reaction 6h, reaction finishes.The mixed solution that obtains is drawn into capable underpressure distillation through filtration, and at 190 ℃, underpressure distillation under the 10mmHg vacuum obtains the aluminium-alcohol salt that room temperature is in a liquid state.Room temperature is that the 33.33kg sec-butyl alcohol of 15wt% slowly joins in the aluminium-alcohol salt with water cut under the agitation condition, and the mol ratio of aluminium-alcohol salt and water remained on 1: 6, fully behind the hydrolysis 3h, under 80 ℃, carried out underpressure distillation, steamed unnecessary alcohol, obtained aluminium hydroxide powder.1200 ℃ down calcining 3h obtain purity be 99.999% alumina powder jointed.Shown in Fig. 2 c, each diffraction peak is the characteristic diffraction peak of aluminum oxide.
Table 1
Claims (8)
1. the preparation method of a high-purity alpha-alumina is characterized in that comprising the steps:
1. with raw materials mix, react 3～8h down at 80～100 ℃; Wherein, described raw material is made up of following component by weight:
Metallic aluminium 10～25
Sec-butyl alcohol 75～90
HgCl
2 0.001～0.003；
Wherein, the purity of metallic aluminium is more than 99.99%;
2. filter, underpressure distillation gets the liquid aluminium alkoxide;
3. normal temperature under the agitation condition, joins aqueous sec-butyl alcohol in the liquid aluminium alkoxide, is hydrolyzed;
4. mixing liquid is 3. carried out underpressure distillation, get aluminium hydroxide powder;
5. aluminium hydroxide powder is calcined.
2. the preparation method of the described high-purity alpha-alumina of claim 1, it is characterized in that described step 3. the water cut of sec-butyl alcohol be 15wt%.
3. the preparation method of the described high-purity alpha-alumina of claim 2, it is characterized in that described step 3. the mol ratio of aluminium-alcohol salt and water be 1: 2～6.
4. the preparation method of the arbitrary described high-purity alpha-alumina of claim 1～3, it is characterized in that described step 2. underpressure distillation carry out under 1mmHg～10mmHg at 190～210 ℃.
5. the preparation method of the arbitrary described high-purity alpha-alumina of claim 1～3, it is characterized in that described step 3. hydrolysis time be 1～3h.
6. the preparation method of the arbitrary described high-purity alpha-alumina of claim 1～3, it is characterized in that described step 4. underpressure distillation under 80～99 ℃, carry out.
7. the preparation method of the arbitrary described high-purity alpha-alumina of claim 1～3, it is characterized in that described step 5. calcination condition be 1200 ℃ of calcining 3h down.
8. the preparation method of the arbitrary described high-purity alpha-alumina of claim 1～3, it is characterized in that described step 4. the sec-butyl alcohol that obtains of underpressure distillation as step raw material 1..
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2528979C1 (en) * | 2013-05-13 | 2014-09-20 | Общество с ограниченной ответственностью "ПРИМА" | Method of producing alpha-phase of aluminium oxide |
| RU2538606C1 (en) * | 2013-12-30 | 2015-01-10 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" | Method of producing highly pure aluminium oxide by electrolysis |
| CN106365188A (en) * | 2016-08-26 | 2017-02-01 | 孟玲 | Preparation device of micron-sized aluminum oxide powder |
| CN110386614A (en) * | 2019-06-20 | 2019-10-29 | 广西玉林市思达粉体技术有限公司 | Preparation method that is a kind of while obtaining large, medium and small aperture boehmite |
| CN112209415A (en) * | 2020-09-18 | 2021-01-12 | 新疆众和股份有限公司 | Process for recovering alcohol water in production of high-purity superfine alumina powder |
| CN112939045A (en) * | 2021-02-03 | 2021-06-11 | 浙江爱科新材料有限公司 | Preparation method of superfine high-purity gamma-alumina |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4615875A (en) * | 1986-02-03 | 1986-10-07 | Allied Corporation | Process for preparing high purity alpha-alumina |
| CN1195646A (en) * | 1997-04-09 | 1998-10-14 | 大连铁道学院精细陶瓷工程研究中心 | Technology for preparing ultra-high purity superfine aluminium oxide powder |
| CN1316382A (en) * | 2000-04-04 | 2001-10-10 | 韩嵬 | Process for preparing high-purity superfine alumina powder by aluminium alkoxide hydrolysis |
-
2011
- 2011-12-13 CN CN2011104160612A patent/CN102491391A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4615875A (en) * | 1986-02-03 | 1986-10-07 | Allied Corporation | Process for preparing high purity alpha-alumina |
| CN1195646A (en) * | 1997-04-09 | 1998-10-14 | 大连铁道学院精细陶瓷工程研究中心 | Technology for preparing ultra-high purity superfine aluminium oxide powder |
| CN1316382A (en) * | 2000-04-04 | 2001-10-10 | 韩嵬 | Process for preparing high-purity superfine alumina powder by aluminium alkoxide hydrolysis |
Non-Patent Citations (1)
| Title |
|---|
| 刘建良 等: "高纯超细氧化铝粉制备方法最新研究进展", 《昆明理工大学学报（理工版）》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2528979C1 (en) * | 2013-05-13 | 2014-09-20 | Общество с ограниченной ответственностью "ПРИМА" | Method of producing alpha-phase of aluminium oxide |
| RU2538606C1 (en) * | 2013-12-30 | 2015-01-10 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" | Method of producing highly pure aluminium oxide by electrolysis |
| CN106365188A (en) * | 2016-08-26 | 2017-02-01 | 孟玲 | Preparation device of micron-sized aluminum oxide powder |
| CN110386614A (en) * | 2019-06-20 | 2019-10-29 | 广西玉林市思达粉体技术有限公司 | Preparation method that is a kind of while obtaining large, medium and small aperture boehmite |
| CN112209415A (en) * | 2020-09-18 | 2021-01-12 | 新疆众和股份有限公司 | Process for recovering alcohol water in production of high-purity superfine alumina powder |
| CN112939045A (en) * | 2021-02-03 | 2021-06-11 | 浙江爱科新材料有限公司 | Preparation method of superfine high-purity gamma-alumina |
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Application publication date: 20120613 |