CN1032336A - The method for preparing soluble metal alkoxides by the reactant of low solubility - Google Patents
The method for preparing soluble metal alkoxides by the reactant of low solubility Download PDFInfo
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- CN1032336A CN1032336A CN 87106601 CN87106601A CN1032336A CN 1032336 A CN1032336 A CN 1032336A CN 87106601 CN87106601 CN 87106601 CN 87106601 A CN87106601 A CN 87106601A CN 1032336 A CN1032336 A CN 1032336A
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- magnesium
- magnesium alkoxide
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Abstract
Coagulate the aluminium-magnesium alkoxide of metal by aluminium alcoholates and the insoluble magnesium alkoxide prepared in reaction of organic solvent organic solvent soluble.
Description
The present invention narrates a kind of method for preparing the organic solvent soluble metal alkoxide mixt.
Magnesium alkoxide normally is not dissolved in the agent solvent, and the character of this low solubility makes them be difficult to handle, and particularly is difficult to plan to form synthetic mineral matter by the hydrolysis by alkoxide solution.
Aluminium alcoholates dissolves in organic solvent usually, and alkoxide improves the formation that dissolving has been used for promoting mixed metal alkoxide.For example No. 3946102 (authorizing IMThomas) existing introductions of United States Patent (USP).Mixed metal alkoxide in the Thomas patent is by MAGNESIUM METAL and metallic aluminium and alkoxyl group alcohols reaction generation.Emitting of hydrogen followed in this reaction.This inflammable hydrogen must be removed, and the product that obtains usually needs to handle impurity contained in the metal reactant.
It is desirable to develop the formation method of mixed metal alkoxide, wherein available is not the raw material of metal element.
The present invention uses (1) aluminium alcoholates, (2) magnesium alkoxide as the principal reaction thing, prepares the method for organic solvent soluble mixed metal alkoxide.
The inventive method is the soluble mixed metal alkoxide of preparation.Used in the present invention term " organic solvent is solvable " is defined as at 20 ℃, is being selected from toluene, and at least a solvent, the solvent degree reaches 15%(weight at least in hexane or the propyl carbinol).
The principal reaction thing of the inventive method is: (1) aluminium alcoholates; (2) magnesium alkoxide.Suitable aluminium alcoholates is represented with following chemical formula:
R wherein
1, R
2Be alkyl identical or different, that be selected from 1 to 20 carbon atom.R
1, R
2And R
3The alkyl that preferably contains 1 to 6 carbon atom.The typical aluminium alcoholates of the actual use of the present invention is as follows.
Aluminium secondary butylate, aluminum isopropylate, Pentyl alcohol aluminium.
The magnesium alkoxide component can be expressed from the next:
R wherein
4And R
5Be identical or with, the alkyl that is selected from 1 to 20 carbon atom.R
4And R
5The alkyl that preferably contains 1 to 6 carbon atom.The typical magnesium alkoxide of the actual use of the present invention is as follows:
Magnesium ethylate, isobutyl magnesium alkoxide, Pentyl alcohol magnesium.
The characteristics of magnesium alkoxide reactant are that organic solvent is insoluble, used in the present invention term " organic solvent is insoluble " be defined as 20 ℃, be selected from that solubleness is lower than 5%(weight at least a solvent in toluene, hexane, the propyl carbinol).
The preferred mixed alcoholate product of the present invention is the liquid of viscosity under room temperature (about 25 ℃).
The inventive method is by in having the reaction zone of stirring, principal reaction thing magnesium alkoxide is mixed with aluminium alcoholates, implements to guarantee that reactant contacts effectively.
Preferably in liquid phase reaction medium, react reactionlessness.The typical liquid phase hydro carbons that should be used as medium comprises:
Toluene, dimethylbenzene, benzene, hexanaphthene, heptane, hexane and their mixture.
On the other hand, alcohol can component part or complete reaction mixture.Yet, but as the hydro carbons part substituted metal alkoxide reactant of the alcohol of reaction medium and the R base in the mixed metal alkoxide of the present invention.
What recommend is that pure al composition can be dissolved in the reaction medium.The insoluble magnesium alkoxide reactant of organic solvent generally is to be suspended in the reaction medium.
The mixed metal alkoxide product is expressed from the next:
Mg
mAI
n（OR
6）
（2m+3n）
Each R wherein
5Can be identical or different, be selected from by previously defined R
1, R
2, R
2, R
4And R
5, m and n are 1 to 6.
The reacting by heating thing when insoluble relatively magnesium alkoxide becomes solution, thinks that then this reaction finishes.The dissolving of magnesium alkoxide can be regarded the terminal point of reaction as.
Aluminium alcoholates approximately is Mg with the optimal relative mol ratio of magnesium alkoxide: AI ≈ 1: 2.In general, the magnesium in the input reaction zone and the mol ratio of aluminium can change to about 1: 6 from about 1: 1, and the mol ratio of magnesium and aluminium is preferably from about 1: 1.5 to 1: 2.5.
Temperature of reaction is not strict, carries out under the reflux temperature of reaction medium usually.The reflux temperature of typically saying medium is from about 80 to about 150 ℃.
Reaction product can be by filtering and stripping be purified, and being higher than 50 ℃, vacuum tightness in temperature typically is to carry out stripping under 5mmHg or the higher condition.The productive rate of the inventive method generally is higher than 80%.
Following each embodiment has illustrated the inventive method
Embodiment 1
Present embodiment illustrates enforcement of the present invention.
One 1 liter three-necked flask is equipped with a condenser, thermometer and agitator.Aluminium secondary butylate and 300 with 209 grams 95%
Toluene joins in the flask, adds 48.4 gram magnesium ethylates under nitrogen protection in this mixture.This magnesium compound does not dissolve under stirring at room.The reacting by heating mixture is to reflux temperature, and after five hours, almost all magnesium compound becomes solution.Filtering reacting liquid uses flash distillation to be stripped to constant weight to remove unreacted matters then.Stripping operation is to be to carry out under the 20mmHg at 60 to 70 ℃, vacuum tightness.The output of product is 227 grams, suitable 92% productive rate.
Embodiment 2
Present embodiment illustrates method of the present invention.
In this experiment, use method and the instrument of embodiment 1.
In 200 milliliters of Pentyl alcohols, 53.3 gram normal-butyl magnesium mix with Pentyl alcohol solution with 222.4 grams, three amylalcohol al dissolutions.Adding fashionablely, in reaction medium, having the amylalcohol magnesium precipitate to produce immediately.Reflux and remove precipitation, and make all reactants become solution thereafter.The output of product is 262 grams, is equivalent to 95% productive rate.
Embodiment 3
Present embodiment illustrates method of the present invention.
In this experiment, use method and the instrument of embodiment 2.
Except aluminium secondary butylate and normal-butyl reactive magnesium in a sec-butyl alcohol reaction medium, used all is the reactant of embodiment 2.Being deposited in when refluxing of generating in reaction zone disappears.The productive rate of product almost is quantitative.
Claims (11)
1, the method for preparation a kind of organic solvent soluble hybrid metal aluminium/magnesium alkoxide, it comprises reactive chemical combination:
(a) a kind of pure al reactant and (b) the insoluble magnesium alkoxide reactant of a kind of organic solvent.
2, the method for a kind of organic solvent soluble hybrid metal magnesium/aluminium-alcohol salt of preparation, it comprises reactive chemical combination:
(a) a kind of with chemical formula
The aluminium alcoholates of expression, R in the formula
1, R
2And R
3It is alkyl identical or different, that be selected from 1 to 20 carbon atom.
(b) a kind of with chemical formula
The insoluble magnesium alkoxide of organic solvent of expression, R in the formula
4And R
5It is alkyl identical or different, that be selected from 1 to 20 carbon atom.
3, the method for claim 2, wherein the mol ratio of magnesium alkoxide reactant and pure al reactant is from 1: 1 to 1: 6.
4, the method for claim 3, wherein the mol ratio of magnesium alkoxide reactant and pure al reactant is from 1: 1.5 to 1: 2.5.
5, the method for claim 2, wherein pure al reactant is selected from aluminium secondary butylate, aluminum isopropylate, Pentyl alcohol aluminium and their mixture.
6, the process of claim 1 wherein that the magnesium alkoxide reactant is selected from magnesium alkoxide, sec-butyl alcohol magnesium, Pentyl alcohol magnesium and their mixture.
7, the method for claim 2 is to carry out in liquid phase reaction medium, and this reaction medium is a kind of solvent to pure al reactant, and is a kind of non-solvent to the magnesium alkoxide reactant.
8, the method for claim 2, wherein temperature of reaction is with about 30 to 200 ℃.
9, the method for claim 7, wherein the reaction of magnesium alkoxide and aluminium alcoholates is to carry out under the reflux temperature of liquid phase reaction medium.
10, the method for claim 7, wherein liquid phase reaction medium is selected from toluene, benzene, dimethylbenzene, sec-butyl alcohol, Pentyl alcohol, Virahol or their mixture.
11, the method for claim 2, wherein reactant is wanted the chemical combination time enough, so that remove organic solvent soluble magnesium alkoxide reactant basically.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87106601 CN1032336A (en) | 1986-06-09 | 1987-09-28 | The method for preparing soluble metal alkoxides by the reactant of low solubility |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US06/872,329 US4731461A (en) | 1986-06-09 | 1986-06-09 | Process for preparing tin alkoxides |
| CN 87106601 CN1032336A (en) | 1986-06-09 | 1987-09-28 | The method for preparing soluble metal alkoxides by the reactant of low solubility |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1032336A true CN1032336A (en) | 1989-04-12 |
Family
ID=25742363
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 87106601 Pending CN1032336A (en) | 1986-06-09 | 1987-09-28 | The method for preparing soluble metal alkoxides by the reactant of low solubility |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1032336A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109071354A (en) * | 2016-02-16 | 2018-12-21 | 新罗纳米技术有限公司 | The formation and modification of ceramic nano line and its use in functional material |
| CN111511751A (en) * | 2017-09-14 | 2020-08-07 | 戴森技术有限公司 | Magnesium salt |
-
1987
- 1987-09-28 CN CN 87106601 patent/CN1032336A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109071354A (en) * | 2016-02-16 | 2018-12-21 | 新罗纳米技术有限公司 | The formation and modification of ceramic nano line and its use in functional material |
| CN109071354B (en) * | 2016-02-16 | 2021-09-14 | 新罗纳米技术有限公司 | Formation and modification of ceramic nanowires and their use in functional materials |
| US11328832B2 (en) | 2016-02-16 | 2022-05-10 | Sila Nanotechnologies Inc. | Formation and modifications of ceramic nanowires and their use in functional materials |
| CN111511751A (en) * | 2017-09-14 | 2020-08-07 | 戴森技术有限公司 | Magnesium salt |
| CN111511751B (en) * | 2017-09-14 | 2023-05-02 | 戴森技术有限公司 | Magnesium salt |
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| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |