Alpha,omega-(dihydroxyethyl) aminopropyl terminated polysiloxane, synthetic method and midbody thereof

A synthesis method and technology of polysiloxane, applied in the field of α, can solve the problems of unsaturated compounds being difficult to obtain, unsaturated compound reaction conditions are harsh, etc., and achieve the advantages of industrial application, easy availability of raw materials, high product yield and purity Effect

Inactive Publication Date: 2012-06-20
邬元娟
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the unsaturated compound containing two hydroxyl groups is not easy to o...

Method used

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  • Alpha,omega-(dihydroxyethyl) aminopropyl terminated polysiloxane, synthetic method and midbody thereof
  • Alpha,omega-(dihydroxyethyl) aminopropyl terminated polysiloxane, synthetic method and midbody thereof
  • Alpha,omega-(dihydroxyethyl) aminopropyl terminated polysiloxane, synthetic method and midbody thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Hydroxyl protection reaction (molar ratio diethanolamine: hexamethyldisilazane=1:1.5)

[0028] In a 250mL three-necked flask, add 52.50g of diethanolamine. At room temperature, slowly add 12110g of hexamethyldisilazane dropwise. reaction. The reaction solution was distilled under atmospheric pressure, and the fraction at 218-220° C. was collected to obtain 120.70 g of bis(trimethylsiloxy)ethylamine, with a yield of 97%. The compound corresponds to 1 H NMR (CDCl 3 , ppm) analysis data are as follows: 0.03 ~ 0.22 (m, 18H, Si-C H 3 ), 1.83(s, 1H, N H ), 2.73~2.75(t, 4H, N-C H 2 ), 3.69~3.71(t, 4H, O-C H 2 ).

[0029] Alkylation reaction (molar ratio: allyl bromide: bis(trimethylsilyloxy) ethylamine: triethylamine=1.2:1:1.5)

[0030]In a 250 mL three-necked flask, 99.60 g of bis(trimethylsiloxy)ethylamine, 60.60 g of triethylamine and 100 mL of dichloromethane were sequentially added. Place the three-neck flask in an ice-water bath, and slowly add 58.08 g of all...

Embodiment 2

[0042] Change the ratio of the amount of diethanolamine and hexamethyldisilazane in the hydroxyl protection reaction of Example 1 to 1:1.2, the reaction temperature is changed to 110°C, the reaction time is changed to 6h, and other reaction conditions are as in Example 1 As described, bis(trimethylsiloxy)ethylamine was obtained with a yield of 93%.

Embodiment 3

[0044] Allyl bromide is changed to allyl chloride in the alkylation reaction of embodiment 1, and the ratio of the amount of substances of allyl chloride, two (trimethylsilyloxy) ethylamine and triethylamine becomes 2 : 1: 3, other reaction conditions are as described in Example 1, N, N-bis(trimethylsilyloxy) ethylallylamine, the yield is 82%.

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Abstract

The invention discloses alpha,omega-(dihydroxyethyl) aminopropyl terminated polysiloxane, a synthetic method and a midbody thereof. The structure of the alpha,omega-(dihydroxyethyl) aminopropyl terminated polysiloxane is shown in the formula (I) described in the specification. A synthetic route is as follows: a target compound, namely the alpha,omega-(dihydroxyethyl) aminopropyl terminated polysiloxane, is obtained through hydroxyl protection, alkylation, hydrosilylation, alcoholysis and equilibrium polymerization by taking diethanol amine, hexamethyldisilazane, allyl bromide (or allyl chloride or allyl iodide), tetramethyldisiloxane and D4 as starting materials. Because two molecular ends of the alpha,omega-(dihydroxyethyl) aminopropyl terminated polysiloxane respectively have two hydroxyalkyl groups, the alpha,omega-(dihydroxyethyl) aminopropyl terminated polysiloxane can be reacted with other substances to obtain a polysiloxane modified material.

Description

technical field [0001] The invention relates to an α, ω-(bishydroxyethyl) aminopropyl-terminated polysiloxane, a synthesis method and an intermediate thereof. Background technique [0002] Due to the presence of chemically active hydroxyalkyl functional groups, more and more hydroxyalkyl polysiloxanes are used to react with isocyanate groups or carboxyl groups to modify certain synthetic resins (such as polyurethane and polyester). properties to improve various properties of materials. Compared with the hydroxyl group directly connected to the silicon atom, the introduction of the hydroxyl hydrocarbon group increases the stability of the polyurethane-siloxane and other copolymers against hydrolysis and alcoholysis. In addition, hydroxyhydrocarbyl siloxane also has the following advantages: first, the type and nature of the hydrocarbon group have a great influence on the properties of the oligomer, and there is a large room for formula design; second, the selection of an app...

Claims

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Application Information

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IPC IPC(8): C08G77/26C07F7/10
Inventor 邬元娟张萌郭栋梁丁蕊艳杜红霞李慧冬李瑞菊
Owner 邬元娟
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