Synthesis method of three-terminal epoxy-modified silicone oil

A synthetic method and technology of modifying silicon, which is applied in the chemical field to achieve the effect of wide application range, high temperature resistance, and suitable for large-scale production

Inactive Publication Date: 2014-11-19
CHANGCHUN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The modified silicone oil containing epoxy groups at the three ends has not yet appeared,

Method used

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  • Synthesis method of three-terminal epoxy-modified silicone oil
  • Synthesis method of three-terminal epoxy-modified silicone oil
  • Synthesis method of three-terminal epoxy-modified silicone oil

Examples

Experimental program
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preparation example Construction

[0032] Step 3, the preparation of three-terminal epoxy-modified silicone oil, the capping agent prepared in step 2 and octamethylcyclotetrasiloxane (D4), 3-glycidyl propyl (dimethoxy) methyl silane Add it to a three-necked flask, and add 0.05% to 0.1% of tetramethylammonium hydroxide as a catalyst, and react for 4 hours at a temperature of 70°C to 75°C; add glacial acetic acid to the three-necked flask to adjust the pH of the product to 6.8-7.2 , vacuum rotary evaporation to remove low boilers, and collect the three-terminal epoxy-modified silicone oil product.

[0033] The three-necked flask used in the step two and step three is equipped with a thermometer, a reflux condenser and a dropping funnel.

[0034] The catalyst used in the step 3 is tetramethylammonium hydroxide catalyst or potassium hydroxide catalyst.

[0035] The catalyst used in the third step is a basic catalyst.

[0036] Such as figure 1 The infrared spectrum of AGE and capping agent shown, in the figure (a...

Embodiment 1

[0043] Embodiment 1, get 5mLAGE and 70ppm catalyst, place in the there-necked flask that is equipped with thermometer, reflux condenser and dropping funnel, under N2 condition, activate 1.5h at 55 ℃, drop 2mLHMM with constant pressure dropping funnel, After the dropwise addition, the reaction was carried out at 58° C. for 4 h. After the reaction, the unreacted monomer was removed by vacuum rotary evaporation to obtain a light yellow liquid. D4: The molar ratio of coupling agent: end-capping agent is 1:1:1, and the amount of catalyst is 0.05% of the total amount of monomers. A three-terminal epoxy-modified silicone oil with a molecular weight of 1013 was obtained.

Embodiment 2

[0044] Example 2, take 5mLAGE and 70ppm catalyst, place in a three-necked flask equipped with a thermometer, a reflux condenser and a dropping funnel, activate it at 55°C for 1.5h under N2 conditions, add 2mLHMM dropwise with a constant pressure dropping funnel, After the dropwise addition, the reaction was carried out at 58° C. for 4 h. After the reaction, the unreacted monomer was removed by vacuum rotary evaporation to obtain a light yellow liquid. D4: The molar ratio of coupling agent: end-capping agent is 2:3:1, and the amount of catalyst is 0.05% of the total amount of monomers. A three-terminal epoxy-modified silicone oil with a molecular weight of 1751 was obtained.

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Abstract

The invention relates to a synthesis method of three-terminal epoxy-modified silicone oil, and relates to the field of chemistry. The three-terminal epoxy-modified silicone oil is synthesized through two steps. Tetramethyl disiloxane and allyl glycidyl ether are adopted as raw materials; chloroplatinic acid-isopropanol is adopted as a catalyst; and 1,3-diglycidoxypropyl-1,1,3,3-tetramethyl disiloxane with epoxy groups on two terminals is synthesized through a hydrosilylation reaction. The 1,3-diglycidoxypropyl-1,1,3,3-tetramethyl disiloxane is adopted as a capping agent; octamethyl cyclotetrasiloxane and 3-glycidylpropyl(dimethoxy)methylsilane are adopted as raw materials; tetramethyl ammonium hydroxide is adopted as a catalyst; and epoxy-modified silicone oil with epoxy groups on three terminals is synthesized through a bulk polymerization method. Through controlling a reaction material ratio, products with different molecular weights can be prepared. According to the invention, modified silicon oil with epoxy groups on three terminals is synthesized for a first time. Reaction activity is enhanced, and high-temperature resistance is improved.

Description

technical field [0001] The invention belongs to the field of chemistry, in particular to a method for synthesizing modified silicone oil. Background technique [0002] In recent years, modified silicone oil has received extensive attention and research due to its excellent physical and chemical properties. Epoxy-modified silicone oil is the main one among many modified silicone oils, and has been widely used due to its own reactivity and high adsorption. [0003] Epoxy-modified silicone oil, that is, silicone oil modified by epoxy groups. Epoxy-modified silicone oil has the dual properties of epoxy group and polydimethylsiloxane at the same time. It not only has the characteristics of soft chain segment and heat resistance, but also can make polydimethylsiloxane by using the reactivity of epoxy group. The oxane is bonded with the organic polymer to achieve the expected purpose. Due to the high reactivity of epoxy silicone oil, it is often used as a fiber fabric finishing ...

Claims

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Application Information

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IPC IPC(8): C08G77/18C08G77/08
Inventor 张宝昌赵莹宋晓峰崔晴晴李同国
Owner CHANGCHUN UNIV OF TECH
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