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Method for preparing siloxane potassium alcoholate

A technology of potassium siloxanolate and polysiloxane, applied in the field of preparing potassium siloxanolate, can solve problems such as long reaction time, unfavorable application of potassium siloxanolate, etc., and achieve the effect of avoiding environmental pollution and the danger of operation

Active Publication Date: 2014-04-02
SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The method for preparing potassium silanolate proposed in U.S. Patent US 5969173 also uses the organic solvent toluene. Although the reaction temperature is low, the reaction time is long, and organic matter (should be mainly solvent) and water are observed in the thermogravimetric analysis data of the reaction product. This is detrimental to the subsequent application of potassium silicate

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  • Method for preparing siloxane potassium alcoholate
  • Method for preparing siloxane potassium alcoholate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The method for preparing potassium siloxanate, the steps are as follows:

[0034]Rinse the surface of the sheet-shaped potassium hydroxide quickly under the protection of nitrogen with twice-distilled water that has been boiled to remove carbon dioxide, then quickly weigh 40g of potassium hydroxide and dissolve it in 40g of secondary water that has removed carbon dioxide, and transfer it to 500ml four-port under the protection of nitrogen. Then add 360g of dimethylsiloxane mixed rings into the flask. The four-necked flask is equipped with a water separator, and the temperature is raised to 120°C under the condition of constant stirring and nitrogen, and then the vacuum is turned on to maintain dehydration at -0.04Mpa. When it is observed that the speed at which the water droplets are collected becomes slow, the vacuum degree can be gradually increased to -0.09MPa until it is found that no water droplets are collected within 10 minutes, and the reaction ends. Then it was...

Embodiment 2

[0039] The method for preparing potassium siloxanate, the steps are as follows:

[0040] Rinse the surface of the sheet-shaped potassium hydroxide quickly under the protection of nitrogen with twice-distilled water that has been boiled to remove carbon dioxide, then quickly weigh 20g of potassium hydroxide and dissolve it in 10g of secondary water that has removed carbon dioxide, and transfer it to 500ml four-port under nitrogen protection. In the flask, then add a mixture of 380g cyclic polysiloxane and hydroxyl-terminated linear polysiloxane, wherein the mass ratio of the two siloxanes is 3:7, and the viscosity is 28mpas. The four-neck flask was equipped with a water separator, and the temperature was raised to 120°C under the condition of constant stirring and nitrogen, and then the vacuum was opened to maintain dehydration at -0.05Mpa. When it is observed that the speed at which the water droplets are collected becomes slow, the vacuum degree can be gradually increased to ...

Embodiment 3

[0042] The method for preparing potassium siloxanate, the steps are as follows:

[0043] Dissolve 40g of potassium hydroxide in 15g of double-distilled water from which carbon dioxide has been removed, then add 10g of strong basic macroporous anion exchange resin, exchange and adsorb for 2 hours, quickly filter and transfer to a 500ml four-necked flask equipped with it, and then add 360 g 70 mpas of hydroxyl terminated linear polysiloxane. The four-neck flask was equipped with a water separator, and the temperature was raised to 120°C under the condition of constant stirring and nitrogen, and then the vacuum was opened to maintain dehydration at -0.05Mpa. When it is observed that the speed at which the water droplets are collected becomes slow, the vacuum degree can be gradually increased to -0.09MPa until it is found that no water droplets are collected within 10 minutes, and the reaction ends. Then it was naturally cooled to 60°C under the protection of nitrogen, transferre...

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Abstract

The invention relates to a method for preparing siloxane potassium alcoholate, which belongs to the field of organic polymerization. The method is characterized by comprising the following steps: preparing a water solution from potassium hydroxide after purification in a reaction bottle, then adding polysiloxane which is well metered, increasing the temperature under the conditions of continuously introducing dry nitrogen and stirring, then opening vacuum, maintaining negative-pressure dehydration, and finishing reaction when observing that no water beads are collected any more to obtain the glutinous siloxane potassium alcoholate. An organic solvent is not used, environmental pollution and operation risk are avoided, and the time required for removing the solvent by increasing the temperature after the end of the reaction can be simultaneously saved.

Description

technical field [0001] The invention relates to a method for preparing potassium siloxane alkoxide, which belongs to the field of organic polymerization. Background technique [0002] Alkali metal silicon alkoxide such as sodium siloxane, potassium siloxane, cesium siloxane, etc. can be used as a basic catalyst for the ring-opening polymerization of cyclosiloxane for the preparation of high molecular weight siloxane polymerization things. In general, potassium silanolate can be applied to the ring-opening polymerization of cyclotrisiloxane, cyclotetrasiloxane, cyclopentasiloxane, and the like. Lithium silanolate can be used for the ring-opening polymerization of cyclotrisiloxane and cyclotetrasiloxane, whereby siloxane polymers with narrow molecular weight distribution can be prepared. [0003] Alkali metal silicon alkoxides can also form silicon-oxygen bonds through polycondensation reactions. The reaction process is as follows: ≡Si-X+MO-Si≡→≡Si-O-Si≡+MX [0004] Wherei...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/16C08G77/06
Inventor 桑圣凯胡生祥伊港付佃亮宋超张停
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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