Preparation method for aminoalkyl ended polysiloxane

A technology of polyorganosiloxane and aminoalkyl sealing is applied in the field of preparation of polyorganosiloxane, which can solve problems such as low molecular weight and achieve the effects of improving flexibility, high and low temperature resistance, and improving adhesion

Inactive Publication Date: 2012-10-31
广州市爱弘迪新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] There are few independent reports on the preparation of polyorganosiloxane whose main chain is terminated by aminoalkyl groups. US5235082 mentions the use of hydrogen-containing silicone oil with a low degree of polymerization and N, N-di Methallylamine reaction to synthesize aminopropylpolysiloxane, but only a low molecular weight transitional intermediate

Method used

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  • Preparation method for aminoalkyl ended polysiloxane
  • Preparation method for aminoalkyl ended polysiloxane
  • Preparation method for aminoalkyl ended polysiloxane

Examples

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Embodiment 1

[0038] Synthesis of N-trimethylsilylallylamine (Step 1)

[0039] In a 1L three-necked flask equipped with magnetic stirring, a reflux condenser, and a dropping funnel, after purging with nitrogen, add 195.5 g (1.8 mol) of trimethylchlorosilane, 363 g of triethylamine, and 100 ml of n-hexane in sequence, and heat under stirring. To 50°C, 85.8g (1.5mol) of allylamine was added dropwise within 1 hour, and after the addition, the temperature was raised to 70°C for 1 hour to react. The triethylamine hydrochloride produced by the reaction is removed by filtration, and the excess trimethylchlorosilane and solvent are distilled off from the filtrate, and then rectified with a 60cm fractionating column to collect a fraction at 108-110°C to obtain the product N-trimethylsilylene Propylamine 178.4g., yield 92%.

Embodiment 2

[0041]This embodiment is basically the same as Embodiment 1. The difference is that the feeding method of trimethylchlorosilane and allylamine is reversed, that is, allylamine is added to the flask, trimethylchlorosilane is added dropwise in 1 hour, and then reacted at 60°C for 2 hours, and the product N- Trimethylsilyl allylamine 157.1g, yield 81%.

Embodiment 3

[0043] This embodiment is basically the same as Embodiment 1. The difference is that the reaction does not add solvent n-hexane, but the HCl absorbent triethylamine is increased to 405g, and the reaction is carried out at 80°C for 1 hour, and the product N-trimethylsilylallylamine is 184.3g, and the yield is 95%. .

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Abstract

The invention discloses a preparation method for aminoalkyl ended polysiloxane. The preparation method comprises the following steps: (1) allyl amine and trimethylchlorosilane react to produce N-trimethylsililyl allylamine with protective groups; (2) HSi key ended hydrosilicone oil and N-trimethylsililyl allylamine are subjected to hydrosilylation reaction to produce N-trimethyl silicane aminopropyl ended polysiloxane; and (3) the N-trimethyl silicane aminopropyl ended polysiloxane is subject to alcoholysis to remove the protective groups to obtain aminopropyl ended polysiloxane. Both the flexibility and the high-and-low temperature resistance of an LED epoxy resin packaging material adopting the product prepared by the method are improved, and the adhesion of LED addition pouring silicone rubber adopting the product can also be improved.

Description

Technical field: [0001] The invention relates to a preparation method of polyorganosiloxane, in particular to a preparation method of polyorganosiloxane whose main chain is terminated by aminoalkyl groups. Background technique: [0002] At present, aminoalkyl polyorganosiloxanes have been widely reported as fabric finishing agents, leather and paper softeners and slip agents, and as cosmetic additives. In these reports, the methods for preparing aminoalkyl polyorganosiloxane mainly include bulk polymerization and emulsion polymerization, and the synthesis principles of the two methods are basically the same. Generally, amino-containing silane or its hydrolyzed prepolymer and linear or cyclic silicone oligomer are used for hydrolysis condensation, ring opening, and equilibrium under alkali catalysis, and then the catalyst is neutralized to obtain the product. Some representative preparation methods can be found in the following publications: CN101805996A, CN101463134A, CN101...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/388
Inventor 冯文利何启祥
Owner 广州市爱弘迪新材料科技有限公司
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