CN105330684A - Preparation method for potassium trimethylsilanolate - Google Patents
Preparation method for potassium trimethylsilanolate Download PDFInfo
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- CN105330684A CN105330684A CN201410389193.4A CN201410389193A CN105330684A CN 105330684 A CN105330684 A CN 105330684A CN 201410389193 A CN201410389193 A CN 201410389193A CN 105330684 A CN105330684 A CN 105330684A
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- preparation
- potassium hydroxide
- spray drying
- potassium
- trimethyl silicane
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Abstract
The invention discloses a preparation method for potassium trimethylsilanolate. The method comprises the following steps: adding hexamethyldichlorosilane into potassium hydroxide under stirring and carrying out reflux and water separation at 100 to 103 DEG C for 10 to 15 h; and subjecting a product of reflux and water separation to centrifugal spray drying at a rotating speed of 2500 to 3500 rpm and a temperature of 100 to 120 DEG C so as to obtain a potassium trimethylsilanolate crystal. The preparation method is simple and has low cost; and the prepared potassium trimethylsilanolate is a white crystal, has a purity of more than 99% and does not have methanol residual.
Description
Technical field
The invention belongs to chemical catalyst technical field, particularly a kind of method preparing trimethyl silicane potassium alcoholate.
Background technology
Trimethyl silicane potassium alcoholate, No. CAS is 10519-96-7, and molecular formula is C
3h
10kOSi, for preparing the custom catalysts of the polymerization catalyzed of polysiloxane and open loop catalysis, the polymerization catalyzed and open loop catalyzed reaction utilizing this catalyzer to carry out, without methyl alcohol in residue, without polychlorobiphenyl and polystream phenol, be therefore widely used in polymerization catalyzed and open loop catalysis.The trimethyl silicane potassium alcoholate produced in prior art is generally reacted in pyridine-methanol system by hexamethyldisilazane and potassium oxide, and its product is white powder, and purity is lower, also has methyl alcohol and remains, have impact on catalytic efficiency.
Summary of the invention
The object of the present invention is to provide a kind of method preparing trimethyl silicane potassium alcoholate, to solve the above-mentioned problems in the prior art.
For achieving the above object, technical scheme of the present invention is as follows:
Prepare a method for trimethyl silicane potassium alcoholate, comprise the steps:
Potassium hydroxide is added, reflux water-dividing 10 ~ 15h at 100 ~ 103 DEG C under being stirred by hexamethyl dichlorosilane;
By reflux water-dividing product at the rotating speed of 2500 ~ 3500rpm, carry out centrifugal spray drying at 100 ~ 120 DEG C, obtain trimethyl silicane potassium alcoholate crystal.
Preferably, the mol ratio of described hexamethyl dichlorosilane and potassium hydroxide is (1 ~ 10): 1.
Preferably, the mol ratio of described hexamethyl dichlorosilane and potassium hydroxide is (1 ~ 5): 1.
Preferably, the mol ratio of described hexamethyl dichlorosilane and potassium hydroxide is 4:1.
Present invention process is simple, and with low cost, the trimethyl silicane potassium alcoholate of preparation is white crystal, and purity, higher than 99%, remains without methyl alcohol.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but protection scope of the present invention is not only confined to embodiment.
Embodiment 1 one kinds prepares the method for trimethyl silicane potassium alcoholate, and the method comprises the steps:
109kg hexamethyl dichlorosilane is dropped in stirring tank, nitrogen 0.5h is passed into the flow velocity of 1L/min while stirring, continue stirring and add 56kg potassium hydroxide, at 100 DEG C after reflux water-dividing 10h blowing in centrifugal spray drying case, centrifugal spray drying 5h at 3000rpm rotating speed, the temperature of 100 DEG C, obtain white crystal product, purity is 99.99%.
Embodiment 2 one kinds prepares the method for trimethyl silicane potassium alcoholate, and the method comprises the steps:
436kg hexamethyl dichlorosilane is dropped in stirring tank, nitrogen 0.5h is passed into the flow velocity of 1L/min while stirring, continue stirring and add 56kg potassium hydroxide, at 103 DEG C after reflux water-dividing 10h blowing in centrifugal spray drying case, centrifugal spray drying 3h at 2500rpm rotating speed, the temperature of 120 DEG C, obtain white crystal product, purity is 99.98%.
Embodiment 3 one kinds prepares the method for trimethyl silicane potassium alcoholate, and the method comprises the steps:
545kg hexamethyl dichlorosilane is dropped in stirring tank, nitrogen 0.5h is passed into the flow velocity of 1L/min while stirring, continue stirring and add 56kg potassium hydroxide, at 103 DEG C after reflux water-dividing 12h blowing in centrifugal spray drying case, centrifugal spray drying 4h at 3500rpm rotating speed, the temperature of 110 DEG C, obtain white crystal product, purity is 99.97%.
Embodiment 4 one kinds prepares the method for trimethyl silicane potassium alcoholate, and the method comprises the steps:
654kg hexamethyl dichlorosilane is dropped in stirring tank, nitrogen 0.5h is passed into the flow velocity of 1L/min while stirring, continue stirring and add 56kg potassium hydroxide, at 100 DEG C after reflux water-dividing 15h blowing in centrifugal spray drying case, centrifugal spray drying 4h at 3500rpm rotating speed, the temperature of 110 DEG C, obtain white crystal product, purity is 99.98%.
Embodiment 5 one kinds prepares the method for trimethyl silicane potassium alcoholate, and the method comprises the steps:
1090kg hexamethyl dichlorosilane is dropped in stirring tank, nitrogen 0.5h is passed into the flow velocity of 1L/min while stirring, continue stirring and add 56kg potassium hydroxide, at 100 DEG C after reflux water-dividing 15h blowing in centrifugal spray drying case, centrifugal spray drying 8h at 3500rpm rotating speed, the temperature of 110 DEG C, obtain white crystal product, purity is 99.98%.
Embodiment 6 one kinds prepares the method for trimethyl silicane potassium alcoholate, and the method comprises the steps:
872kg hexamethyl dichlorosilane is dropped in stirring tank, nitrogen 0.5h is passed into the flow velocity of 1L/min while stirring, continue stirring and add 56kg potassium hydroxide, at 100 DEG C after reflux water-dividing 13h blowing in centrifugal spray drying case, centrifugal spray drying 4h at 3500rpm rotating speed, the temperature of 110 DEG C, obtain white crystal product, purity is 99.99%.
Present invention process is simple, and with low cost, the trimethyl silicane potassium alcoholate of preparation is white crystal, and purity, higher than 99%, remains without methyl alcohol.
Last it is noted that above embodiment only in order to illustrate the present invention and and unrestricted technical scheme described in the invention; Therefore, although this specification sheets with reference to each above-mentioned embodiment to present invention has been detailed description, those of ordinary skill in the art should be appreciated that and still can modify to the present invention or equivalent to replace; And all do not depart from technical scheme and the improvement thereof of the spirit and scope of the present invention, it all should be encompassed in right of the present invention.
Claims (4)
1. prepare a method for trimethyl silicane potassium alcoholate, it is characterized in that, comprise the steps:
Potassium hydroxide is added, reflux water-dividing 10 ~ 15h at 100 ~ 103 DEG C under being stirred by hexamethyl dichlorosilane;
By reflux water-dividing product at the rotating speed of 2500 ~ 3500rpm, carry out centrifugal spray drying at 100 ~ 120 DEG C, obtain trimethyl silicane potassium alcoholate crystal.
2. preparation method according to claim 1, is characterized in that: the mol ratio of described hexamethyl dichlorosilane and potassium hydroxide is (1 ~ 10): 1.
3. preparation method according to claim 1, is characterized in that: the mol ratio of described hexamethyl dichlorosilane and potassium hydroxide is (1 ~ 5): 1.
4. the preparation method according to Claims 2 or 3, is characterized in that: the mol ratio of described hexamethyl dichlorosilane and potassium hydroxide is 4:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410389193.4A CN105330684A (en) | 2014-08-08 | 2014-08-08 | Preparation method for potassium trimethylsilanolate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410389193.4A CN105330684A (en) | 2014-08-08 | 2014-08-08 | Preparation method for potassium trimethylsilanolate |
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| Publication Number | Publication Date |
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| CN105330684A true CN105330684A (en) | 2016-02-17 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410389193.4A Pending CN105330684A (en) | 2014-08-08 | 2014-08-08 | Preparation method for potassium trimethylsilanolate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114214027A (en) * | 2021-12-27 | 2022-03-22 | 东莞市正安有机硅科技有限公司 | Non-gel hardening type alkali glue and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491993A (en) * | 2011-11-24 | 2012-06-13 | 山东大学 | Preparation method of lithium trimethylsilanolate |
-
2014
- 2014-08-08 CN CN201410389193.4A patent/CN105330684A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491993A (en) * | 2011-11-24 | 2012-06-13 | 山东大学 | Preparation method of lithium trimethylsilanolate |
Non-Patent Citations (1)
| Title |
|---|
| MARIJA LOVRIC等: ""Scope and Limitations of Sodium and Potassium Trimethylsilanolate as Reagents for Conversion of Esters to Carboxylic Acids"", 《CROATICA CHEMICA ACTA》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114214027A (en) * | 2021-12-27 | 2022-03-22 | 东莞市正安有机硅科技有限公司 | Non-gel hardening type alkali glue and preparation method thereof |
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Application publication date: 20160217 |
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| RJ01 | Rejection of invention patent application after publication |