Method for preparing alpha, omega-bis(aminopropyl)polydimethylsiloxane

A dimethylsiloxane and aminopropyl technology, applied in the alpha field, can solve the problems of low product yield and slow reaction rate, and achieve the effects of high amino end capping rate, eliminating interference and shortening the equilibrium reaction time.

Active Publication Date: 2012-11-14
GUANGZHOU TINCI MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In the patent CN101838395A, a method for preparing double-ended amino silicone oil is disclosed, but the double-ended amino silicone oil contains a branched chain structure, has a high molecular weight, and is directly catalyzed by an alkaline substance, resulting in slow reaction rate and low product yield. question

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  • Method for preparing alpha, omega-bis(aminopropyl)polydimethylsiloxane
  • Method for preparing alpha, omega-bis(aminopropyl)polydimethylsiloxane
  • Method for preparing alpha, omega-bis(aminopropyl)polydimethylsiloxane

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Embodiment 1

[0032] In this embodiment, the preparation method of α, ω-bis(aminopropyl)polydimethylsiloxane comprises the following steps:

[0033] (1) Preparation of silicon alkoxide catalyst: Add 80g NaOH and 800g dimethylsiloxane mixed ring (DMC) into a stirred reactor, raise the temperature to 90°C at 7KPa, dehydrate for 4 hours, and obtain a uniform and transparent Oily NaOH siliconate (siliconate catalyst);

[0034] (2) Add 960g of hexamethylcyclotrisiloxane (D 3 ), remove moisture at 70°C and 2KPa; then add 1.2g of the silicon alkoxide catalyst obtained in step (1) to start the catalytic reaction, the temperature of the catalytic reaction is 110°C, and add 87.0g of 1,3-bis( 3-aminopropyl)-1,1,3,3-tetramethyldisiloxane for equilibrium reaction for 5 hours;

[0035] (3) Add H to the mixture obtained after the reaction in step (2) 3 PO 4 Neutralize the catalyst, and then remove the low boilers at 150°C and 0.5kPa to obtain the α,ω-bis(aminopropyl)polymer with a colorless and transp...

Embodiment 2

[0044] In this embodiment, the preparation method of α, ω-bis(aminopropyl)polydimethylsiloxane comprises the following steps:

[0045] (1) Preparation of silicon alkoxide catalyst: Add 80g NaOH and 800g dimethylsiloxane mixed ring (DMC) into a stirred reactor, raise the temperature to 90°C at 7KPa, dehydrate for 4 hours, and obtain a uniform and transparent Oily NaOH silicon alkoxide (siliconate catalyst);

[0046] (2) Add 1100g of dimethylsiloxane mixed rings into a reactor equipped with a stirrer and a nitrogen pipe, and remove moisture at 90°C and 5KPa; then add the silicon alkoxide catalyst obtained in step (1) 1.5g, start the catalytic reaction, the temperature of the catalytic reaction is 150°C, add 2.5g of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane after the catalytic reaction for 30min Equilibrium reaction, reaction 6h;

[0047](3) Add H to the mixture obtained after the reaction in step (2) 3 PO 4 Neutralize the catalyst, and then remove the low boilers ...

Embodiment 3

[0053] In this embodiment, the preparation method of α, ω-bis(aminopropyl)polydimethylsiloxane comprises the following steps:

[0054] (1) Preparation of silicon alkoxide catalyst: Add 80g NaOH and 800g dimethylsiloxane mixed ring (DMC) into a stirred reactor, raise the temperature to 90°C at 7KPa, dehydrate for 4 hours, and obtain a uniform and transparent Oily NaOH siliconate (siliconate catalyst);

[0055] (2) Add 1200g decamethylcyclopentasiloxane (D 5 ), remove moisture at 90°C and 4KPa; then add 2.5g of the silicon alkoxide catalyst obtained in step (1) to start the catalytic reaction, the temperature of the catalytic reaction is 150°C, and add 3.0g of 1,3-bis( 3-aminopropyl)-1,1,3,3-tetramethyldisiloxane for equilibrium reaction, reacted for 7 hours;

[0056] (3) Add H to the mixture obtained after the reaction in step (2) 3 PO 4 Neutralize the catalyst, and then remove the low boilers at 170°C and 1.0kPa to obtain the α,ω-bis(aminopropyl)polymer with a colorless an...

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Abstract

The invention discloses a method for preparing alpha, omega-bis(aminopropyl)polydimethylsiloxane. A siliconate catalyst is prepared through alkali compound which is provided by the preparation method and then the catalyst has a good compatibility in the reaction solution, thus improving the catalytic reaction rate and obviously shortening the equilibrium reaction time. Raw materials are dehydrated before the reaction to eliminate the interference of end-capped hydroxy group and increase reaction efficiency. The final product synthesized has the characteristics of high amino termination yield, good stability and the like. The obtained product can be used as a basic raw material for siloxane-organic block copolymer and can also be used as an excellent conditioning agent in the hair care composition.

Description

technical field [0001] The invention belongs to the field of organosilicon synthesis, in particular to a preparation method of α,ω-bis(aminopropyl)polydimethylsiloxane. Background technique [0002] In the field of polymer synthesis chemistry, the research of multi-block copolymers with polyorganosiloxane as soft segment and organic polymer as hard segment is attracting more and more attention. α, ω-bis(aminopropyl)polydimethylsiloxane is one of the most common silicone comonomers due to the reactive aminohydrocarbon groups at both ends of the long chain of the polysiloxane molecule. [0003] A method for preparing polydimethylsiloxane-polyamide multi-block elastomers is disclosed in the patent CN101392063B. This patent describes the preparation of α,ω-bis(aminopropyl)polydimethylsiloxane as an intermediate, which is directly catalyzed by tetramethylammonium hydroxide. The disadvantage of this method is that the catalyst has poor compatibility and low catalytic efficiency,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/26C08G77/08C07F7/10
Inventor 罗啸秋张利萍吴海龙
Owner GUANGZHOU TINCI MATERIALS TECH
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