WO2012100555A1 - A method for the preparation of lower aluminum alkoxide by gas-solid phase reaction - Google Patents
A method for the preparation of lower aluminum alkoxide by gas-solid phase reaction Download PDFInfo
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- WO2012100555A1 WO2012100555A1 PCT/CN2011/080380 CN2011080380W WO2012100555A1 WO 2012100555 A1 WO2012100555 A1 WO 2012100555A1 CN 2011080380 W CN2011080380 W CN 2011080380W WO 2012100555 A1 WO2012100555 A1 WO 2012100555A1
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- Prior art keywords
- aluminum
- lower alkyl
- alkyl alcohol
- process according
- aluminum alkoxide
- Prior art date
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 105
- -1 aluminum alkoxide Chemical class 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000003746 solid phase reaction Methods 0.000 title claims abstract description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 61
- 125000005233 alkylalcohol group Chemical group 0.000 claims abstract description 32
- 229910052751 metal Inorganic materials 0.000 claims abstract description 28
- 239000002184 metal Substances 0.000 claims abstract description 28
- 239000003054 catalyst Substances 0.000 claims abstract description 25
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 claims description 25
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 7
- 229960003280 cupric chloride Drugs 0.000 claims description 6
- 238000007514 turning Methods 0.000 claims description 6
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 5
- 239000004677 Nylon Substances 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 229920001778 nylon Polymers 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- MYWQGROTKMBNKN-UHFFFAOYSA-N tributoxyalumane Chemical compound [Al+3].CCCC[O-].CCCC[O-].CCCC[O-] MYWQGROTKMBNKN-UHFFFAOYSA-N 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 description 19
- 239000002994 raw material Substances 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 238000009835 boiling Methods 0.000 description 7
- 239000012467 final product Substances 0.000 description 7
- 238000004821 distillation Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 4
- JPUHCPXFQIXLMW-UHFFFAOYSA-N aluminium triethoxide Chemical compound CCO[Al](OCC)OCC JPUHCPXFQIXLMW-UHFFFAOYSA-N 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005292 vacuum distillation Methods 0.000 description 3
- 238000011549 displacement method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- ACIAHEMYLLBZOI-ZZXKWVIFSA-N Unsaturated alcohol Chemical compound CC\C(CO)=C/C ACIAHEMYLLBZOI-ZZXKWVIFSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012450 pharmaceutical intermediate Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/68—Preparation of metal alcoholates
- C07C29/70—Preparation of metal alcoholates by converting hydroxy groups to O-metal groups
Definitions
- the invention relates to a novel process for the preparation of lower aluminum alkoxide by gas-solid phase reaction.
- Lower aluminum alkoxide can be widely used in fields such as organic raw materials, pharmaceutical intermediates, catalysts, dehydrators, etc., and is also an important precursor for the preparation of advanced ceramic materials. With the development of chemical industry and pharmaceutical industry, the need for lower aluminum alkoxide is also increasing.
- the disadvantage of this technology is that, since the reactants, raw materials and the catalysts are reacted together, the lower aluminum alkoxide has to be separated from the excessive alcohol by distillation after the reaction. Moreover, the distillation operation necessarily causes a small amount of alcohol to be mixed into the final product lower aluminum alkoxide, which lowers its purity. To increase the efficiency of separation, the manufacturer often employs vacuum distillation, which not only increases the investment on equipments, but also reduces the safety factor of the production. It is also disclosed in the patent document (publication No. CN 160 076 5 A) that acetates were additionally added into the reaction as solvents, and the separation thereof required distilling for a longer period, thus further increasing the energy consumption and the production cost of the manufacturer.
- Another method for the preparation of the lower aluminum alkoxide is the alcohol displacement method.
- the lower aluminum alkoxide was prepared with the alcohol displacement method wherein aluminum ethoxide and n-butanol were employed as the raw materials which were heated to reflux in a liquid state for several hours, displacing ethanol in aluminum ethoxide with n-butanol to prepare aluminum n-butoxide. Subsequently vacuum distillation procedure was employed, wherein the reaction was terminated at the second boiling point to yield aluminum n-butoxide.
- the disadvantages of this method are: the cost is too high for using aluminum ethoxide as a raw material, and the energy consumption is very high when the alcohol and lower aluminum alkoxide are individually separated by distillation. Moreover, the catalysts of choice in conventional aluminum alkoxide preparation are mostly chlorides of mercury or iodine, which are severe pollutant to the environment.
- the invention provides a novel process for the preparation of lower aluminum alkoxide by gas-solid phase reaction which is green, safe, highly efficient and having low energy consumption. It solves the problems that, for example, the manufacture of lower aluminum alkoxide causes high costs, has complicated process, relatively low safety factor and relatively low reaction rate. Moreover, the lower aluminum alkoxide product yielded by the invention also has a high purity. BRIEF DESCRIPTION OF THE DRAWINGS
- Figure 1 the infrared spectrum of the product aluminum n-butoxide obtained in Example 1 .
- the invention provides a process for the preparation of lower aluminum alkoxide by gas-solid phase reaction, comprising reacting gaseous lower alkyl alcohol with metal aluminum.
- a process for the preparation of lower aluminum alkoxide comprising the steps of: adding the lower alkyl alcohol into a container and heating it to reflux to generate a gaseous lower alkyl alcohol;
- the lower alkyl alcohol can be a C2-C4 saturated or unsaturated alcohol, preferably a C2-C4 saturated alcohol, including ethanol, propanol, butanol, in particular butanol, preferably n-butanol.
- the lower alkyl alcohol which is in a gaseous state, is contacted with the metal aluminum and reacted.
- the metal aluminum used in this process can be in any form including aluminum ingot, aluminum flake, aluminum block, aluminum turning and aluminum slag.
- the purity of the aluminum is 99% or above.
- aluminum is excessive in stoichiometry.
- lower alkyl alcohol : aluminum is ⁇ 1 : 1 (molar ratio), preferably lower alkyl alcohol : aluminum is 1 : 3 (molar ratio), and generally between 1 : 3 and 1 : 1.
- the metal aluminum is not contacted with the liquid lower alkyl alcohol prior to the reaction.
- the metal aluminum raw material is placed above the lower alkyl alcohol and separated therefrom.
- the porous material can be any material that is inert under the reaction conditions, for example including, but not limited to various materials such as glass mesh, steel mesh, nylon mesh, etc.
- the catalyst includes any catalyst commonly used in the production of lower aluminum alkoxide, preferably a catalyst in a solid form, such as anhydrous aluminum trichloride, cupric chloride or stannic tetrachloride catalyst.
- the catalyst can be added into the lower aluminum alkoxide, or placed on the porous material together with the metal aluminum raw material.
- the catalyst is a solid and is placed in the upper part of the container together with the aluminum raw material.
- a process for the preparation of lower aluminum alkoxide of high purity by a gas-solid phase reaction with aluminum and n-butanol used as the raw materials wherein the aluminum can be aluminum flake, aluminum block, aluminum turning or aluminum slag with a purity of 99% or more, and the aluminum has to be excessive, i.e., aluminum : n-butanol > 1 : 3 (molar ratio), generally between 1 /3 and 1 , and the process is green, safe, highly efficient and has low energy consumption.
- the n-butanol involved in the reaction is in a gaseous state rather a liquid state.
- Anhydrous aluminum trichloride, cupric chloride or stannic tetrachloride is used as the catalyst, and 0.5 to 3 g of the catalyst per liter of n- butanol is needed.
- the specific process for the preparation of lower aluminum alkoxide of high purity by gas-solid phase reaction is as follows: firstly, n-butanol is added into the reactor, and then a porous mesh containing a mixture of aluminum and catalyst is placed above the liquid which is then heated to reflux. When the boiling point of n-butanol (for example, 1 17.73 ° C under atmospheric pressure) is reached, the evaporated gaseous n-butanol will react with the metal aluminum in the presence of the catalyst as it passes through the porous mesh, and the lower aluminum alkoxide generated will drop back into the reactor through the porous mesh. With the increase of the amount of the lower aluminum alkoxide in the reactor, the azeotropic temperature also increases.
- the aluminum involved in the reaction is excessive, and the lower alkyl alcohol is involved in the reaction in a gaseous state rather than the conventional liquid state, which contributes to the increase of reaction rate. Omission of distillation simplifies the process, reduces the energy consumption, reduces the equipment investment by the enterprise, and increases the safety of the production.
- Using anhydrous aluminum trichloride, cupric chloride or stannic tetrachloride as the catalyst is both economical and friendly to the environment.
- the process according to the invention wherein the lower aluminum alkoxide is prepared by reacting gaseous lower alkyl alcohol with solid metal aluminum, provides the following advantages: the raw materials is easy to obtain; the process itself is safe and convenient with a simple post processing, and requires low energy consumption, reduces the intervention of other substances during the reaction, and is able to produce lower aluminum alkoxide of high purity in a way that saves energy and is economically advantageous.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The invention provides a novel process for the preparation of lower aluminum alkoxide of high purity by gas-solid phase reaction, wherein the lower aluminum alkoxide is prepared by reacting gaseous lower alkyl alcohol with solid metal aluminum. By using the process of the invention, the process for the production of lower aluminum alkoxide is simplified, investment on equipments and energy consumption is reduced, and it is friendly to the environment. This process solves the following problems that, for example, the production of aluminum n-butoxide has complicate processes, excessively high cost, relatively low safety factor, catalyst pollution, etc..
Description
A METHOD FOR THE PREPARATION OF LOWER ALUMINUM ALKOXIDE BY
GAS-SOLID PHASE REACTION TECHNICAL FIELD
The invention relates to a novel process for the preparation of lower aluminum alkoxide by gas-solid phase reaction.
BACKGROUND
Lower aluminum alkoxide can be widely used in fields such as organic raw materials, pharmaceutical intermediates, catalysts, dehydrators, etc., and is also an important precursor for the preparation of advanced ceramic materials. With the development of chemical industry and pharmaceutical industry, the need for lower aluminum alkoxide is also increasing.
Conventional methods for the preparation of lower aluminum alkoxide mostly employ direct reactions, usually carried out in a solvent or in a state of solution, comprising generating lower aluminum alkoxide by using metal aluminum and lower alkyl alcohol as the raw materials and heating them for several hours in the present of a catalyst, wherein the alcohol needs to be excessive. Subsequently, the final product lower aluminum alkoxide are obtained by subjecting the lower aluminum alkoxide to an atmospheric distillation or a vacuum distillation. For example, this method was employed in patent documents with publication Nos. CN 120 103 5 A and CN 160 076 5 A. The disadvantage of this technology is that, since the reactants, raw materials and the catalysts are reacted together, the lower aluminum alkoxide has to be separated from the excessive alcohol by distillation after the reaction. Moreover, the distillation operation necessarily causes a small amount of alcohol to be mixed into the final product lower aluminum alkoxide, which lowers its purity. To increase the efficiency of separation, the manufacturer often employs vacuum distillation, which not only increases the investment on equipments, but also
reduces the safety factor of the production. It is also disclosed in the patent document (publication No. CN 160 076 5 A) that acetates were additionally added into the reaction as solvents, and the separation thereof required distilling for a longer period, thus further increasing the energy consumption and the production cost of the manufacturer.
Another method for the preparation of the lower aluminum alkoxide is the alcohol displacement method. As described in Chou Xiujian et al. Yunnan Chemical Industry 2004 31 (2): 1 -3, the lower aluminum alkoxide was prepared with the alcohol displacement method wherein aluminum ethoxide and n-butanol were employed as the raw materials which were heated to reflux in a liquid state for several hours, displacing ethanol in aluminum ethoxide with n-butanol to prepare aluminum n-butoxide. Subsequently vacuum distillation procedure was employed, wherein the reaction was terminated at the second boiling point to yield aluminum n-butoxide. The disadvantages of this method are: the cost is too high for using aluminum ethoxide as a raw material, and the energy consumption is very high when the alcohol and lower aluminum alkoxide are individually separated by distillation. Moreover, the catalysts of choice in conventional aluminum alkoxide preparation are mostly chlorides of mercury or iodine, which are severe pollutant to the environment.
In the field of lower aluminum alkoxide, there is still a need for a process capable of having an easy reaction procedure and a simple post processing, saving energy and yielding products of high purity.
SUMMARY
The invention provides a novel process for the preparation of lower aluminum alkoxide by gas-solid phase reaction which is green, safe, highly efficient and having low energy consumption. It solves the problems that, for example, the manufacture of lower aluminum alkoxide causes high costs, has complicated process, relatively low safety factor and relatively low reaction rate. Moreover, the lower aluminum alkoxide product yielded by the invention also has a high purity.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings, which are included to provide a further understanding of the, illustrate embodiments of the invention together with the description which serves to explain the principle of the invention. Therefore, the invention is not limited to the embodiments. In the drawings:
Figure 1 : the infrared spectrum of the product aluminum n-butoxide obtained in Example 1 . DETAILED DESCRIPTION
An embodiment of the present invention will now be described in detail in conjunction with the drawings. In the following description, some detailed descriptions of known functions and configurations may be omitted for clarity and conciseness.
The invention provides a process for the preparation of lower aluminum alkoxide by gas-solid phase reaction, comprising reacting gaseous lower alkyl alcohol with metal aluminum.
According to an embodiment of the invention, it is provided a process for the preparation of lower aluminum alkoxide, comprising the steps of:
adding a lower alkyl alcohol into a container;
introducing metal aluminum into the container in a way that the metal aluminum is placed separately from the lower alkyl alcohol; and
refluxing the lower alkyl alcohol to generate a gas which contacts and reacts with metal aluminum.
According to another embodiment of the invention, it is provided a process for the preparation of lower aluminum alkoxide, comprising the steps of:
adding the lower alkyl alcohol into a container and heating it to reflux to generate a gaseous lower alkyl alcohol; and
reacting the gaseous lower alkyl alcohol under reflux with the metal aluminum, wherein the liquid lower aluminum alkoxide in the container is not contacted with the metal aluminum.
In this process, the lower alkyl alcohol can be a C2-C4 saturated or unsaturated alcohol, preferably a C2-C4 saturated alcohol, including ethanol, propanol, butanol, in particular butanol, preferably n-butanol. During the reaction, the lower alkyl alcohol, which is in a gaseous state, is contacted with the metal aluminum and reacted.
The metal aluminum used in this process can be in any form including aluminum ingot, aluminum flake, aluminum block, aluminum turning and aluminum slag. Preferably, the purity of the aluminum is 99% or above. During the reaction, it is preferable that aluminum is excessive in stoichiometry. Usually lower alkyl alcohol : aluminum is ≥ 1 : 1 (molar ratio), preferably lower alkyl alcohol : aluminum is 1 : 3 (molar ratio), and generally between 1 : 3 and 1 : 1.
During the gas-solid phase preparation of lower aluminum alkoxide, the metal aluminum is not contacted with the liquid lower alkyl alcohol prior to the reaction. To maintain the separation between the metal aluminum and the liquid lower alkyl alcohol, it is preferable to place the raw material metal aluminum on a porous material, thus to be separated from the liquid lower alkyl alcohol. In particular, the metal aluminum raw material is placed above the lower alkyl alcohol and separated therefrom. There is no limit to the separation distance between the metal aluminum and the liquid lower alkyl alcohol as long as the surface of the liquid lower alkyl alcohol under reflux does not directly contact with the metal aluminum. The porous material can be any material that is inert under the reaction conditions, for example including, but not limited to various materials such as glass mesh, steel mesh, nylon mesh, etc.
To facilitate the reaction, it is preferable to add a catalyst. The catalyst includes any catalyst commonly used in the production of lower aluminum alkoxide, preferably a catalyst in a solid form, such as anhydrous aluminum trichloride, cupric chloride or stannic tetrachloride catalyst. During the reaction, the catalyst can be added into the lower aluminum alkoxide, or placed on the porous material together with the metal aluminum raw material. To facilitate the reaction, it is preferable that the catalyst is a solid and is placed in the upper part of the container together with the aluminum raw material.
According to one aspect of the invention, it is provided a process for the preparation of lower aluminum alkoxide of high purity by a gas-solid phase reaction with aluminum and n-butanol used as the raw materials, wherein the aluminum can be aluminum flake, aluminum block, aluminum turning or aluminum slag with a purity of 99% or more, and the aluminum has to be excessive, i.e., aluminum : n-butanol > 1 : 3 (molar ratio), generally between 1 /3 and 1 , and the process is green, safe, highly efficient and has low energy consumption. The n-butanol involved in the reaction is in a gaseous state rather a liquid state. Anhydrous aluminum trichloride, cupric chloride or stannic tetrachloride is used as the catalyst, and 0.5 to 3 g of the catalyst per liter of n- butanol is needed.
According to one aspect of the invention, the specific process for the preparation of lower aluminum alkoxide of high purity by gas-solid phase reaction is as follows: firstly, n-butanol is added into the reactor, and then a porous mesh containing a mixture of aluminum and catalyst is placed above the liquid which is then heated to reflux. When the boiling point of n-butanol (for example, 1 17.73 °C under atmospheric pressure) is reached, the evaporated gaseous n-butanol will react with the metal aluminum in the presence of the catalyst as it passes through the porous mesh, and the lower aluminum alkoxide generated will drop back into the reactor through the porous mesh. With the increase of the amount of the lower aluminum alkoxide in the reactor, the azeotropic temperature also increases. When the temperature of the liquid in
the reactor reaches the boiling point of the lower aluminum alkoxide (242 °C under atmospheric pressure), all n-butanol has been exhausted by the reaction. Heating is continued for e.g. half an hour, generally 0.5-5 hours before being stopped. During the reaction, a small amount of aluminum turnings will drop. After removal of the porous mesh, the solution yielded is filtered to remove the aluminum turnings to yield the final product lower aluminum alkoxide with an impurity content of less than 0.01 %.
In the invention, the aluminum involved in the reaction is excessive, and the lower alkyl alcohol is involved in the reaction in a gaseous state rather than the conventional liquid state, which contributes to the increase of reaction rate. Omission of distillation simplifies the process, reduces the energy consumption, reduces the equipment investment by the enterprise, and increases the safety of the production. Using anhydrous aluminum trichloride, cupric chloride or stannic tetrachloride as the catalyst is both economical and friendly to the environment.
The process according to the invention, wherein the lower aluminum alkoxide is prepared by reacting gaseous lower alkyl alcohol with solid metal aluminum, provides the following advantages: the raw materials is easy to obtain; the process itself is safe and convenient with a simple post processing, and requires low energy consumption, reduces the intervention of other substances during the reaction, and is able to produce lower aluminum alkoxide of high purity in a way that saves energy and is economically advantageous.
Examples
Example 1 :
300 ml n-butanol was initially added into a reactor, and then a porous mesh containing a mixture of aluminum and anhydrous aluminum trichloride was suspended above the liquid, wherein the aluminum turning was 27 g and the catalyst was 0.3 g. The reaction was heated to reflux until the liquid temperature reached the boiling point of the lower aluminum alkoxide, and then the heating was continued for another half an hour before being stopped. After removal of
the porous mesh, the solution yielded was filtered to yield the final product aluminum n-butoxide with an impurity content of less than 0.01 %.
Example 2:
300 ml n-butanol was initially added into a reactor, and then a porous mesh containing a mixture of aluminum and cupric chloride was suspended above the liquid, wherein the aluminum flake was 35 g and the catalyst was 0.5 g. The reaction was heated to reflux until the liquid temperature reached the boiling point of the lower aluminum alkoxide, and then the heating was continued for another half an hour before being stopped. After removal of the porous mesh, the solution yielded was filtered to yield the final product aluminum n-butoxide with an impurity content of less than 0.01 %.
Example 3:
500 ml n-butanol was initially added into a reactor, and then a porous mesh containing a mixture of aluminum and the catalyst stannic tetrachloride was suspended above the liquid, wherein the aluminum ingot was 45 g and the catalyst was 0.5 g. The reaction was heated to reflux until the liquid temperature reached the boiling point of the lower aluminum alkoxide, and then the heating was continued for another half an hour before being stopped After removal of the porous mesh, the solution yielded was filtered to yield the final product lower aluminum alkoxide with an impurity content of less than 0.01 %.
Example 4:
1000 ml n-butanol was initially added into a reactor, and then a porous mesh containing a mixture of aluminum and catalysts anhydrous aluminum trichloride and cupric chloride was suspended above the liquid, wherein the aluminum particle was 100 g and the catalyst was 1.5 g. The reaction was heated to reflux until the liquid temperature reached the boiling point of the lower
aluminum alkoxide, and then the heating was continued for another half an hour before being stopped. After removal of the porous mesh, the solution yielded was filtered to yield the final product aluminum n-butoxide with an impurity content of less than 0.01 %.
A number of implementations have been described. Nevertheless, it will be understood that various modifications may be made. For example, elements of different implementations may be combined, supplemented, modified, or removed to produce other implementations. Additionally, one of ordinary skill will understand that other structures and processes may be substituted for those disclosed and the resulting implementations will perform at least substantially the same function(s), in at least substantially the same way(s), to achieve at least substantially the same result(s) as the implementations disclosed. Accordingly, these and other implementations shall fall in the scope of the invention.
Claims
1. A process for the preparation of lower aluminum alkoxide by gas-solid phase reaction, comprising the step of reacting a gaseous lower alkyl alcohol with metal aluminum.
2. The process according to claim 1 , said reaction is performed at a temperature of refluxing the lower aluminum alkoxide or above the temperature.
3. The process according to claim 1 , comprising the steps of:
adding the lower alkyl alcohol into a container;
heating the lower alkyl alcohol to reflux to obtain a gaseous lower alkyl alcohol; and
reacting the gaseous lower alkyl alcohol with metal aluminum.
4. The process according to claim 2, wherein the lower alkyl alcohol and the metal aluminum are placed separately.
5. The process according to any of claims 1 -4, wherein the lower alkyl alcohol is selected from C2-C4 alcohols.
6. The process according to claim 5, wherein the lower alkyl alcohol is propanol or butanol.
7. The process according to any of claims 1-6, wherein the metal aluminum is selected from the group consisting of aluminum turning, aluminum flake and aluminum particle.
8. The process according to any of claims 1 -7, wherein the metal aluminum has a purity of 99% or more.
9. The process according to any of claims 1 -8, wherein the ratio of the metal aluminum to the lower alkyl alcohol is such that the metal aluminum is excessive in stoichiometry, preferably 1 :1 to 3:1 (molar ratio).
10. The process according to any of claim 1 -9, wherein the gaseous lower alkyl alcohol and the metal aluminum are reacted in the presence of a catalyst.
1 1. The process according to claim 10, wherein said catalyst is selected from a group consisting of anhydrous aluminum trichloride, cupric chloride or stannic tetrachloride.
12. The process according to any of claims 1 -1 1 , wherein the metal aluminum is separated from the lower alkyl alcohol using a porous mesh.
13. The process according to claim 1 1 , wherein the porous mesh is selected from a group consisting of glass mesh, steel mesh and nylon mesh.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110028268.2 | 2011-01-26 | ||
| CN201110028268.2A CN102153448B (en) | 2011-01-26 | 2011-01-26 | Method for preparing low-level alkanol aluminum by gas-solid phase reaction |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2012100555A1 true WO2012100555A1 (en) | 2012-08-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/CN2011/080380 WO2012100555A1 (en) | 2011-01-26 | 2011-09-29 | A method for the preparation of lower aluminum alkoxide by gas-solid phase reaction |
Country Status (2)
| Country | Link |
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| CN (1) | CN102153448B (en) |
| WO (1) | WO2012100555A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153448B (en) * | 2011-01-26 | 2014-04-30 | 连云港连连化学有限公司 | Method for preparing low-level alkanol aluminum by gas-solid phase reaction |
| CN106673959B (en) * | 2015-11-11 | 2019-11-15 | 中国石油化工股份有限公司 | A kind of preparation method of raffinal alkoxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB654408A (en) * | 1948-01-27 | 1951-06-20 | British Aluminium Co Ltd | Improvements in the manufacture of aluminium alkoxides |
| US4052428A (en) * | 1975-12-15 | 1977-10-04 | Stauffer Chemical Company | Stable aluminum alkoxide solutions |
| CN1201035A (en) * | 1997-06-04 | 1998-12-09 | 中国石油化工总公司 | A kind of preparation method of low carbon alkoxide aluminum |
| CN102153448A (en) * | 2011-01-26 | 2011-08-17 | 连云港连连化学有限公司 | Method for preparing low-level alkanol aluminum by gas-solid phase reaction |
-
2011
- 2011-01-26 CN CN201110028268.2A patent/CN102153448B/en active Active
- 2011-09-29 WO PCT/CN2011/080380 patent/WO2012100555A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB654408A (en) * | 1948-01-27 | 1951-06-20 | British Aluminium Co Ltd | Improvements in the manufacture of aluminium alkoxides |
| US4052428A (en) * | 1975-12-15 | 1977-10-04 | Stauffer Chemical Company | Stable aluminum alkoxide solutions |
| CN1201035A (en) * | 1997-06-04 | 1998-12-09 | 中国石油化工总公司 | A kind of preparation method of low carbon alkoxide aluminum |
| CN102153448A (en) * | 2011-01-26 | 2011-08-17 | 连云港连连化学有限公司 | Method for preparing low-level alkanol aluminum by gas-solid phase reaction |
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| Publication number | Publication date |
|---|---|
| CN102153448B (en) | 2014-04-30 |
| CN102153448A (en) | 2011-08-17 |
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