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Method for accelerating two-phase separation in synthesis of silicone resin

A phase separation, silicone resin technology, applied in the field of silicone polymer preparation, can solve the problems of not very obvious difference in the density of silicone polymers, unclear two-phase separation interface, long separation time, etc. volume, saving production time and cost, and the effect of fast separation

Inactive Publication Date: 2017-06-20
惠州市佳的利实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Since the organosilicon polymer structure contains a large number of Si-O-Si units, the unit has a certain degree of hydrophilicity, and the difference between the density of the organosilicon polymer and the density of water is not obvious, so organic silicon polymers need to be carried out during the synthesis process. Often difficult and time-consuming to separate phases from aqueous phases
When performing liquid-solid separation, if the solid particles are small (such as activated carbon) and the density is not very different from that of polyorganosiloxane, there is also the problem that it is difficult to separate layers and takes a long time.
Therefore, the method of natural separation between two phases has problems such as unclear two-phase separation interface, long separation time, poor separation effect and low production efficiency.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1. Mix 1000g of water, 15g of 0.1N hydrochloric acid and 300g of isopropanol, then add 4600g of tetraethyl orthosilicate, 300g of vinyl monocap, 500g of hexamethyldisiloxane and 10kg of cyclohexane, and stir quickly The temperature was raised to 77° C., and the reaction was stopped after maintaining reflux for 6 hours to generate a reaction solution.

[0020] 2. Pour the above reaction solution into a 50L high-speed centrifuge, and set the speed of the centrifuge to 3000 rpm. After running for 3 minutes, two upper and lower liquid layers with a clear interface are formed, the impurity water phase of the lower layer is separated, and the organic silicon polymer phase of the upper layer is retained.

[0021] 3. Add 10kg of deionized water into the silicone polymer phase, stir mechanically for 5 minutes, and repeat the above step 2.

[0022] 4. Repeat step 3 more than five times to obtain a clear and transparent organosilicon polymer phase without water-soluble impurities...

Embodiment 2

[0024] 1. Mix the original 5000g yellowish 5000cps vinyl silicone oil, 200g activated carbon and 2000g cyclohexane, stir for 0.5 hours to remove impurities and decolorize.

[0025] 2. Pour the above mixture into a 50L high-speed centrifuge, and set the speed of the centrifuge to 3000 rpm. After running for 3 minutes, the activated carbon in the lower layer was removed to obtain a clear and transparent organic phase.

[0026] 3. Optionally, if activated carbon remains in the process of removing activated carbon in the above step 2, this step can be performed. The mixture after step 2 is filtered through slow filter paper under negative pressure, so as to completely remove residual activated carbon.

Embodiment 3

[0028] 1. Mix 10000g of 1000cps vinyl silicone oil containing a small amount of tetramethylammonium hydroxide catalyst, then add 3000g of ethanol and stir for 0.5 hours.

[0029] 2. Pour the above mixed liquid into a 50L high-speed centrifuge, and set the speed of the centrifuge to 3000 rpm. After running for 3 minutes, two upper and lower liquid layers with a clear interface were formed, the upper ethanol phase was separated, and the lower organic silicon polymer phase was retained.

[0030] 3. Repeat the above steps for more than 5 times.

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PUM

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Abstract

The present invention discloses a method for accelerating two-phase separation in the synthesis of silicone resin. According to the method, a two-phase mixture is subjected to centrifugal separation at high speed by using a centrifuge, so the separation speed is high and the production time cost is saved. The two-phase interface is clear after layering, so it is easy to separate the two phases and the loss of useful materials owing to the misjudgment of an operator is reduced. Because the interface after two-phase layering is clear, the two-phase separation is complete, the method can reduce the number of water washing and water consumption compared with a traditional natural layering process, achieves the purpose of thorough washing, avoids the decline of the quality of silicone polymers due to the presence of trace halogen or other impurities, and ensures the purity of the target product.

Description

technical field [0001] The application belongs to the technical field of organosilicon polymer preparation, and in particular relates to a method for accelerating two-phase separation in the synthesis of silicone resin. Background technique [0002] In the scientific research or manufacturing industry in the field of chemistry and chemical engineering, the process of two-phase separation is usually involved. The purpose of separation is to remove unnecessary impurities and leave a pure target, specifically including the separation of liquid from liquid, or liquid Separation from solids. In order to achieve a better separation and purification effect, it is usually necessary to take advantage of the characteristic differences between the target substance and the impurity, and use a reasonable method for purification. [0003] Since the organosilicon polymer structure contains a large number of Si-O-Si units, the unit has a certain degree of hydrophilicity, and the difference...

Claims

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Application Information

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IPC IPC(8): C08G77/34
CPCC08G77/34
Inventor 刘兴宏
Owner 惠州市佳的利实业有限公司