Silicon-containing low-chlorine epoxy resin and preparation method thereof

A technology of chlorine epoxy resin and epichlorohydrin, which is applied in the direction of silicon organic compounds, can solve the problem of insignificant chlorine removal effect, achieve clear reaction mechanism, increase strength, and simple preparation method

Pending Publication Date: 2022-04-05
智仑超纯环氧树脂(西安)有限公司
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  • Description
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  • Application Information

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Problems solved by technology

[0004] This application provides a silicon-containing low-chlorine epoxy resin and its preparation method to solve the problem of insignificant chlorine removal effect existing in existing removal rate methods

Method used

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  • Silicon-containing low-chlorine epoxy resin and preparation method thereof
  • Silicon-containing low-chlorine epoxy resin and preparation method thereof
  • Silicon-containing low-chlorine epoxy resin and preparation method thereof

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preparation example Construction

[0041] The preparation principle of the silicon-containing low-chlorine epoxy resin in the embodiment of the present application is as follows: when preparing the silicon-containing low-chlorine epoxy resin, firstly, the raw materials bisphenol A and epichlorohydrin undergo polycondensation reaction under the catalysis of NaOH to obtain epoxy resin. high polymer. Subsequently, the epoxy polymer reacts with butyl orthosilicate, and the butyl orthosilicate acts as a nucleophile to attack the epoxy group of the polymer to obtain a modified silicon-containing epoxy resin. On the basis of the traditional low-chlorine epoxy resin, a flexible silicon-containing segment is introduced, which improves the strength, temperature resistance, and moisture resistance of the epoxy resin after curing, improves its hydrophobicity, and reduces its water absorption. Therefore, The possibility of its hydrolysis can be reduced to a certain extent. On the basis of the traditional low-chlorine epoxy...

Embodiment 1

[0053] Add 1 mol of bisphenol A and 2.75 mol of epichlorohydrin into a three-necked flask equipped with a magnet, then raise the temperature to 65°C, and keep it warm for 30 minutes. After the reaction raw materials are completely dissolved, lower the temperature to 50°C, and add A 30% sodium hydroxide solution with a sodium hydroxide content of 1 mol was reacted for 4 hours to obtain the first intermediate product.

[0054] After the reaction is completed, the temperature is raised to 80° C., and the unreacted epichlorohydrin is recovered under reduced pressure under the condition of a vacuum degree >600 mmHg for 2 hours.

[0055] After recovery, the temperature was lowered to 75° C., and 0.5 mol of butyl orthosilicate was added into the three-necked flask, and the reaction was kept for 1 hour to obtain the second intermediate product. Add 60wt% benzene solvent to the second intermediate product, keep the temperature at 70° C. for 30 minutes to dissolve, and ensure that the s...

Embodiment 2

[0058] Add 1 mol of bisphenol A and 2.8 mol of epichlorohydrin into a three-necked flask equipped with a magnet, then raise the temperature to 70°C, and keep it warm for 40 minutes. After the reaction raw materials are completely dissolved, lower the temperature to 55°C, and add A 30% sodium hydroxide solution with a sodium hydroxide content of 1.5 mol was reacted for 5 hours.

[0059] After the reaction was completed, the temperature was raised to 75° C., and the unreacted epichlorohydrin was recovered under reduced pressure under the condition of vacuum degree >600 mmHg for 3 hours. After recovery, raise the temperature to 80°C, add 0.55mol of butyl orthosilicate to the three-necked flask, add 70wt% benzene solvent after 1.5h of heat preservation reaction, keep the temperature at 75°C for 40min to ensure that the contents of the three-necked flask are fully Soluble in benzene.

[0060] Cool down to 70°C, continue to slowly add dropwise a 30% sodium hydroxide solution with a...

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Abstract

The invention provides silicon-containing low-chlorine epoxy resin and a preparation method thereof. The preparation method comprises the following steps: obtaining a first mixed solution of bisphenol A and epoxy chloropropane; adding a sodium hydroxide solution into the first mixed solution, and carrying out a first contact reaction to obtain a first intermediate product; recovering unreacted epichlorohydrin in the first intermediate product under reduced pressure; adding tetrabutyl orthosilicate, and carrying out a second contact reaction to obtain a second intermediate product; adding an organic solvent into the second intermediate product, and fully dissolving the second intermediate product to obtain a second mixed solution; dropwise adding a sodium hydroxide solution into the second mixed solution, and carrying out a third contact reaction to obtain a third intermediate product; and separating an organic phase from the third intermediate product, and carrying out rotary evaporation on the organic phase to remove the organic solvent in the organic phase to obtain the silicon-containing low-chlorine epoxy resin. The silicon-containing low-chlorine epoxy resin can generate n-butyl alcohol through hydrolysis reaction in the synthesis stage, so that the dehydrochlorination efficiency is improved, and the chlorine content of the silicon-containing low-chlorine epoxy resin is reduced.

Description

technical field [0001] The present application relates to the technical field of epoxy resins, in particular to a silicon-containing low-chlorine epoxy resin and a preparation method thereof. Background technique [0002] With the rapid development of science and technology and the continuous innovation of chip technology, the application rate of epoxy resin in semiconductor encapsulant or as integrated circuit chip adhesive is getting higher and higher. However, when epoxy resin is used as a semiconductor encapsulant, the hydrolyzable chlorine in its structure will be hydrolyzed to release hydrochloric acid during the pressure cooker test under high temperature and high pressure, which will cause corrosion of electronic circuits; epoxy resin is used in integrated circuit chip adhesives At the same time, the hydrolyzable chlorine in the epoxy resin structure also causes corrosion to the metal chip, so semiconductor encapsulants and integrated circuit chip adhesives especiall...

Claims

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Application Information

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IPC IPC(8): C07F7/04
Inventor 杜彪
Owner 智仑超纯环氧树脂(西安)有限公司
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