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A kind of synthetic method of polysiloxane terminated by tertiary hydroxyl group

A technology of hydrogen-terminated polysiloxane and polysiloxane, which is applied in the field of synthesis of polysiloxane, can solve problems that are not suitable for the preparation of linear polymers such as block copolymers and hydroxyl-terminated polysiloxane. Applicable to problems such as long-term storage, to save the steps of hydroxyl protection and deprotection, easy to control the reaction, and reduce production costs

Active Publication Date: 2016-03-30
HANGZHOU ZHIJIANG NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the hydroxyl-terminated polysiloxane prepared by the method mentioned in the patent, the hydroxyl groups at both ends are directly connected to Si to form a Si-O-H structure, which is unstable and not suitable for long-term storage
In 2012, Shi Zhendong included the preparation method of hydroxyl-terminated polysiloxane in his patent CN102649844A and patent CN102206347A. This method also prepared polysiloxane with Si-O-H structure at both ends. The hydroxyl-terminated polysiloxane prepared by this method Alkanes are also unstable
However, the polysiloxane prepared by this method has two hydroxyl groups at both ends, which is not suitable for the preparation of linear polymers such as block copolymers or graft copolymers.

Method used

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  • A kind of synthetic method of polysiloxane terminated by tertiary hydroxyl group
  • A kind of synthetic method of polysiloxane terminated by tertiary hydroxyl group
  • A kind of synthetic method of polysiloxane terminated by tertiary hydroxyl group

Examples

Experimental program
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Effect test

Embodiment 1

[0052] 1) Using tetramethyldisiloxane as an end-capping agent, under the catalysis of acid clay and octamethylcyclotetrasiloxane D 4 Ring-opening polymerization to prepare hydrogen-terminated polysiloxane, in which tetramethyldisiloxane and octamethylcyclotetrasiloxane D 4 The molar ratio of is 1:n / 4, and n is 65;

[0053] In a flask equipped with a stirrer, thermometer and reflux condenser, add octamethylcyclotetrasiloxane D 4 The quality of 100.00g, tetramethyldisiloxane 2.78g and acid clay 0.72g, tetramethyldisiloxane and octamethylcyclotetrasiloxane D 4 The molar ratio is 1:16.25, in N 2 Under normal pressure, the temperature was raised to 80°C under protection, and the reaction was carried out under reflux conditions for 18 hours; then the temperature was kept at 100°C and the pressure was reduced to below 3kPa, the unreacted raw materials were distilled off, and the acid clay was removed by filtration to obtain hydrogen-terminated polysiloxane;

[0054] 2) Combine the...

Embodiment 2

[0058] The dihydromyrcenyl alcohol that adopts in the embodiment 1 is changed into 2-methyl-3-buten-2-alcohol, and implementation steps are as follows:

[0059] 1) Using tetramethyldisiloxane as an end-capping agent, under the catalysis of acid clay and octamethylcyclotetrasiloxane D 4 Ring-opening polymerization to prepare hydrogen-terminated polysiloxane, in which tetramethyldisiloxane and octamethylcyclotetrasiloxane D 4 The molar ratio of is 1:n / 4, and n is 25;

[0060] In a flask equipped with a stirrer, thermometer and reflux condenser, add octamethylcyclotetrasiloxane D 4 The quality of 100.00g, tetramethyldisiloxane 7.23g and acid clay 1.50g, tetramethyldisiloxane and octamethylcyclotetrasiloxane D 4 The molar ratio is 1:6.25, in N 2 Under normal pressure, the temperature was raised to 80°C under protection, and the reaction was carried out under reflux conditions for 18 hours; then the temperature was kept at 100°C and the pressure was reduced to below 3kPa, the un...

Embodiment 3

[0065] 1) Using tetramethyldisiloxane as an end-capping agent, under the catalysis of acid clay and octamethylcyclotetrasiloxane D 4 Ring-opening polymerization to prepare hydrogen-terminated polysiloxane, in which tetramethyldisiloxane and octamethylcyclotetrasiloxane D 4 The molar ratio of is 1:n / 4, and n is 30;

[0066] In a flask equipped with a stirrer, thermometer and reflux condenser, add octamethylcyclotetrasiloxane D 4 The quality of 100.00g, tetramethyldisiloxane 6.23g and acid clay 5.35g, tetramethyldisiloxane and octamethylcyclotetrasiloxane D 4 The molar ratio is 1:7.25, in N 2 Under protection, the temperature was raised to 30°C under normal pressure and reacted under reflux conditions for 48 hours; then the temperature was raised to 100°C and the pressure was reduced to below 3kPa, the unreacted raw materials were distilled off, and the acid clay was removed by filtration to obtain hydrogen-terminated polysiloxane;

[0067] 2) Combine the hydrogen-terminated po...

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Abstract

The invention discloses a method for synthesizing tertiary hydroxyl terminated polysiloxane. According to the method, tetramethyldisiloxane is used as an end-capping reagent, and subjected to ring opening polymerization with octamethylcyclotetrasiloxane under an acid catalyst, so as to prepare hydrogen-terminated polysiloxane, and then carrying out hydrosilylation with unsaturated enol containing tertiary hydroxyl, so as to obtain the tertiary hydroxyl terminated polysiloxane. The tertiary hydroxyl terminated polysiloxane synthesized by the method disclosed by the invention is very stable, and can be stored for a long period of time. Hydroxyl protection is not needed at the hydrosilylation stage, and the operation process is simple and easy to grasp. Just one hydroxyl is contained at two ends of the prepared polysiloxane, and the method has a great influence on preparation of a linear block polymer, and is used for modifying high polymer materials such as polyurethane, polyamide and polyester.

Description

technical field [0001] The invention relates to a method for synthesizing polysiloxane, in particular to a method for synthesizing tertiary hydroxyl-terminated polysiloxane. Background technique [0002] Linear polysiloxane is different from ordinary organics with -C-C- as the main chain, it is based on -Si-O-Si- as the main chain. The particularity of structure determines the particularity of its chemical properties, such as high and low temperature resistance, ultraviolet resistance, radiation resistance, weather resistance, electrical insulation, chemical resistance, high gas permeability and physiological inertia. Therefore, it is widely used in aviation, aerospace, electrical and electronic, chemical instrumentation, automobile, machinery, construction, industry, medical and health, daily life and other fields. [0003] On the one hand, polysiloxane can be used alone as a material to prepare silicone rubber and silicone resin. However, when polysiloxane is used as a s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/38C08G77/12C08G77/08
Inventor 范宏李伯耿张延延
Owner HANGZHOU ZHIJIANG NEW MATERIAL CO LTD
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