CN1785946A - Manufacturing method of aluminium alkoxide - Google Patents
Manufacturing method of aluminium alkoxide Download PDFInfo
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- CN1785946A CN1785946A CN 200410089412 CN200410089412A CN1785946A CN 1785946 A CN1785946 A CN 1785946A CN 200410089412 CN200410089412 CN 200410089412 CN 200410089412 A CN200410089412 A CN 200410089412A CN 1785946 A CN1785946 A CN 1785946A
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- aluminium
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- acetate
- aluminium alcoholates
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Abstract
The present invention discloses a method for preparing aluminium alcoholate. Said method uses metal aluminium and alcohol as raw material, and adopts the following steps: in the acetate solution adding metal aluminium, alcohol and initiating agent, heating and refluxing to make reaction to obtain acetate solution of aluminium alcoholate, separating and evaporating so as to obtain aluminium alcoholate. The described acetate can be ethyl acetate, propyl acetate, isopropyl acetate and sec-butyl acetate, and the described alcohol can be ethyl alcohol, propyl alcohol, isopropyl alcohol and sec-butyl alcohol, the weight ratio of the described acetate and alcohol is 2-3:1.
Description
Technical field
The present invention relates to a kind of metal-organic manufacture method, especially a kind of manufacture method of aluminium alcoholates.
Background technology
Aluminium alcoholates is a kind of important underlying metal Organic Chemicals, be widely used in organic synthesis industry such as organic synthesis intermediate and medicine, agricultural chemicals, particularly fine chemistry industry industry develops rapidly, increasing day by day of organic chemistry kind, demand to aluminium alcoholates is increasing, and the market requirement of aluminum isopropylate is particularly evident.
Pure and mild aluminium can be produced aluminium alcoholates under the effect of catalyzer, its reaction is as follows:
The traditional mode of production aluminium alcoholates is to react by metallic aluminium and excessive alcohol heating for dissolving under the effect of catalyzer, fractionate out superfluous alcohol back redistillation then and go out the aluminium alcoholates product, as disclosed patent documentation (publication number: CN1062135A) in Patent Office of the People's Republic of China's on June 24th, 1992.The deficiency that this kind method exists is: the pure and mild distillation aluminium alcoholates product of fractionation surplus all need carry out under low-pressure state, particularly still-process generally need be below 10 mmhg, the manufacturing cost of aluminium alcoholates is increased, make production process have unsafe factor on the other hand; Distillation simultaneously need make the sex change of aluminium alcoholates mixture the aluminium alcoholates mixture heating up to higher temperature, influences the yield of product.
Preparation method's (publication No.: JP4-244037) of Japanese Patent disclosed aluminum isopropylate on September 1st, 1992, introduced a kind of preparation method of aluminum isopropylate, after it is the black mixture cooling that will obtain after metallic aluminium and the alcohol reaction, by adding flocculating aids, filtration obtains aluminum isopropylate, though this method is to carry out filter operation under normal pressure, avoided the deficiency of traditional technology security aspect, but owing to add flocculating aids, understand the effective constituent of absorption portion product, thereby cause the decline of product yield.
Summary of the invention
The manufacture method that the problem that quasi-solution of the present invention is determined provides a kind of yield height, separates the aluminium alcoholates simple, that purity is high to improve the security of production technique, reduces the manufacturing cost of aluminium alcoholates.
For addressing the above problem, the present invention is by the following technical solutions: a kind of manufacture method of aluminium alcoholates, it is to be raw material with metallic aluminium and alcohol, it is characterized in that in the acetates solvent, add metallic aluminium, pure and mild initiator, reflux, reaction obtains the acetic ester solution of aluminium alcoholates, obtains aluminium alcoholates through separating, evaporating.
In the such scheme, acetates is ethyl acetate, propyl acetate, isopropyl acetate, sec-butyl acetate, and described alcohol is respectively ethanol, propyl alcohol, Virahol, sec-butyl alcohol, and the weight ratio of described acetic ester and alcohol is 2-3: 1.Described metallic aluminium is aluminum shot or aluminium bits or aluminium powder, and its purity is more than 99%.Sedimentation is at normal temperatures and pressures adopted in described separation, and the settled time is 15-30 hour.The temperature of the acetic ester solution evaporation of described aluminium alcoholates after separating is to be evaporated to more than the boiling temperature of described acetic ester.Described initiator is an aluminum trichloride (anhydrous), and its add-on is the 0.1-2 ‰ of reaction solution total amount.
The present invention makes the method for aluminium alcoholates, and being reflected in the acetic ester solvent of pure and mild aluminium carried out, because its solvation, raw alcohol, the active raising of aluminium, effectively improve the transformation efficiency of reaction, and reduced the add-on of initiator, reduced the foreign matter content in the reaction system.Simultaneously,, can remove this class impurity, directly obtain the higher aluminium alcoholates acetic ester solution of purity, remove the acetic ester solvent, can obtain the aluminium alcoholates finished product by evaporation by settlement separate because metallic impurity are insoluble in the acetic ester.Because sepn process is all carried out under normal pressure, improved the security of producing, also improve product yield greatly, reduced manufacturing cost.Experiment showed, that the aluminium alcoholates purity that adopts the inventive method to produce is higher, wherein metal and metal oxide impurities content are below 0.01%.
Embodiment
Reactional equation of the present invention is as follows:
Embodiment 1
Take back in the there-necked flask that flows prolong at 3 liters, put into 0.15kg (excessive) purity and be 99% aluminum shot, 0.15g aluminum trichloride (anhydrous), 1kg ethyl acetate solvent, add 0.33kg ethanol then, stir, heating, the control solution temperature is to carry out back flow reaction about 77 ℃, after 2 hours, obtain black and contain al alcoholate mixt solution, the suction discharging, through sedimentation in 15 hours, sucking-off upper strata colourless transparent solution, contain aluminum ethylate 30% in this solution, be heated to 77 ℃ and begin distillation, along with the ethyl acetate evaporation, distillation temperature progressively improves, during to 110 ℃, stop heating, obtain the aluminum ethylate finished product after the cooling, wherein metal and metal oxide impurities content are below 0.01%.The ethyl acetate that evaporates can be recycled.
In the foregoing description, do not change other condition, only change the alcoholic acid add-on and be 0.5 or 0.4kg, can finish reaction equally, obtain the aluminum ethylate finished product.
In addition, the add-on that can also only change aluminum trichloride (anhydrous) is 3g or 0.8g, can finish reaction equally.
Simultaneously, the settling time extends to 20 hours or 30 hours, can finish reaction equally.
Embodiment 2
Take back in the there-necked flask that flows prolong at 3 liters, put into 0.15kg (excessive) purity and be 99% aluminum shot, 0.15g aluminum trichloride (anhydrous), 1kg propyl acetate solvent, add the 0.33kg propyl alcohol then, stir, heating, the control solution temperature is to carry out back flow reaction about 100 ℃, after 2 hours, obtain black and contain the Tripropoxyaluminum mixture solution, the suction discharging, through sedimentation in 15 hours, sucking-off upper strata colourless transparent solution, contain Tripropoxyaluminum 30% in this solution, be heated to 100 ℃ and begin distillation, along with the propyl acetate evaporation, distillation temperature progressively improves, during to 120 ℃, stop heating, obtain the Tripropoxyaluminum finished product after the cooling, wherein metal and metal oxide impurities content are below 0.01%.The propyl acetate that evaporates can be recycled.
In the foregoing description, do not change other condition, the add-on that only changes propyl alcohol is 0.5 or 0.4kg, can finish reaction equally.
In addition, the add-on that can also only change aluminum trichloride (anhydrous) is 3g or 0.8g, can finish reaction equally, obtains the Tripropoxyaluminum finished product.
Simultaneously, the settling time extends to 20 hours or 30 hours, can finish reaction equally.
Embodiment 3
Take back in the there-necked flask that flows prolong at 3 liters, put into 0.15kg (excessive) purity and be 99% aluminum shot, 0.15g aluminum trichloride (anhydrous), 1kg isopropyl acetate solvent, add the 0.33kg Virahol then, stir, heating, the control solution temperature is to carry out back flow reaction about 85 ℃, after 2 hours, obtain black and contain the aluminum isopropylate mixture solution, the suction discharging, through sedimentation in 15 hours, sucking-off upper strata colourless transparent solution, contain aluminum isopropylate 30% in this solution, be heated to 90 ℃ and begin distillation, along with the isopropyl acetate evaporation, distillation temperature progressively improves, during to 120 ℃, stop heating, obtain the aluminum isopropylate finished product after the cooling, wherein metal and metal oxide impurities content are below 0.01%.The isopropyl acetate that evaporates can be recycled.
In the foregoing description, do not change other condition, the add-on that only changes Virahol is 0.5 or 0.4kg, can finish reaction equally, obtains the aluminum isopropylate finished product.
In addition, the add-on that can also only change aluminum trichloride (anhydrous) is 3g or 0.8g, can finish reaction equally.
Simultaneously, the settling time extends to 20 hours or 30 hours, can finish reaction equally.
Embodiment 4
Take back in the there-necked flask that flows prolong at 3 liters, put into 0.15kg (excessive) purity and be 99% aluminum shot, 0.15g aluminum trichloride (anhydrous), 1kg sec-butyl acetate solvent, add the 0.33kg sec-butyl alcohol then, stir, heating, the control solution temperature is to carry out back flow reaction about 100 ℃, after 2 hours, obtain black and contain different aluminium secondary butylate mixture solution, the suction discharging, through sedimentation in 15 hours, sucking-off upper strata colourless transparent solution, contain aluminium secondary butylate 30% in this solution, be heated to 110 ℃ and begin distillation, along with the sec-butyl acetate evaporation, distillation temperature progressively improves, during to 125 ℃, stop heating, obtain the aluminium secondary butylate finished product after the cooling, wherein metal and metal oxide impurities content are below 0.01%.The sec-butyl acetate that evaporates can be recycled.
In the foregoing description, do not change other condition, the add-on that only changes sec-butyl alcohol is 0.5 or 0.4kg, can finish reaction equally, obtains the aluminium secondary butylate finished product.
In addition, the add-on that can also only change aluminum trichloride (anhydrous) is 3g or 0.8g, can finish reaction equally.
Simultaneously, the settling time extends to 20 hours or 30 hours, can finish reaction equally.
Certainly, the also available purity of the aluminum shot of the foregoing description 1-4 is 99% above aluminium bits or aluminium powder.
Claims (10)
1. the manufacture method of an aluminium alcoholates, it is to be raw material with metallic aluminium and alcohol, it is characterized in that in the acetates solvent, adds metallic aluminium, pure and mild initiator, reflux, reaction obtains the acetic ester solution of aluminium alcoholates, through separate, evaporation obtains aluminium alcoholates.
2. the manufacture method of aluminium alcoholates according to claim 1 is characterized in that described acetates is an ethyl acetate, and described alcohol is ethanol, and described ethyl acetate and alcoholic acid weight ratio are 2-3: 1
3. the manufacture method of aluminium alcoholates according to claim 1 is characterized in that described acetates is a propyl acetate, and described alcohol is propyl alcohol, and the weight ratio of described propyl acetate and propyl alcohol is 2-3: 1.
4. the manufacture method of aluminium alcoholates according to claim 1 is characterized in that described acetates is an isopropyl acetate, and described alcohol is Virahol, and the weight ratio of described isopropyl acetate and Virahol is 2-3: 1.
5. the manufacture method of aluminium alcoholates according to claim 1 is characterized in that described acetates is a sec-butyl acetate, and described alcohol is sec-butyl alcohol, and the weight ratio of described sec-butyl acetate and sec-butyl alcohol is 2-3: 1.
6. according to the manufacture method of any described aluminium alcoholates of claim 1-5, it is characterized in that described metallic aluminium is aluminum shot or aluminium bits or aluminium powder, its purity is more than 99%.
7. according to the manufacture method of any described aluminium alcoholates of claim 1-5, it is characterized in that described separation is the sedimentation of adopting at normal temperatures and pressures.
8. the manufacture method of aluminium alcoholates according to claim 7 is characterized in that the described settled time is 15-30 hour.
9. according to the manufacture method of any described aluminium alcoholates of claim 1-5, it is characterized in that the temperature of the acetic ester solution evaporation of described aluminium alcoholates after separating is to be evaporated to more than the boiling temperature of described acetic ester.
10. according to the manufacture method of any described aluminium alcoholates of claim 1-5, it is characterized in that described initiator is an aluminum trichloride (anhydrous), its add-on is the 0.1-2 ‰ of reaction solution total amount.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410089412 CN1785946A (en) | 2004-12-08 | 2004-12-08 | Manufacturing method of aluminium alkoxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410089412 CN1785946A (en) | 2004-12-08 | 2004-12-08 | Manufacturing method of aluminium alkoxide |
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| CN1785946A true CN1785946A (en) | 2006-06-14 |
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| CN 200410089412 Pending CN1785946A (en) | 2004-12-08 | 2004-12-08 | Manufacturing method of aluminium alkoxide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1318363C (en) * | 2003-09-27 | 2007-05-30 | 章浩龙 | Method for fabricating aluminum alkoxide |
| CN103781750A (en) * | 2011-09-13 | 2014-05-07 | 住友化学株式会社 | Method for producing aluminum alkoxide |
| CN106673038A (en) * | 2015-11-11 | 2017-05-17 | 中国石油化工股份有限公司 | Aluminum alkoxide preparation method |
-
2004
- 2004-12-08 CN CN 200410089412 patent/CN1785946A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1318363C (en) * | 2003-09-27 | 2007-05-30 | 章浩龙 | Method for fabricating aluminum alkoxide |
| CN103781750A (en) * | 2011-09-13 | 2014-05-07 | 住友化学株式会社 | Method for producing aluminum alkoxide |
| CN106673038A (en) * | 2015-11-11 | 2017-05-17 | 中国石油化工股份有限公司 | Aluminum alkoxide preparation method |
| CN106673038B (en) * | 2015-11-11 | 2018-04-10 | 中国石油化工股份有限公司 | A kind of preparation method of aluminium-alcohol salt |
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