Polysiloxane-ester polyols, and preparation method and application thereof

A technology of ester polyol and polysiloxane, which is applied in the field of polymer material preparation, can solve the problems of large molecular weight, poor stability and small intermolecular force of polyether segments, and achieves excellent comprehensive performance, stable reactivity, Highly reactive effect

Active Publication Date: 2019-10-22
MIRACLL CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Commonly used silicone reactive intermediates include hydroxyl silicone oil and polyether modified silicone oil, both of which can have active hydroxyl groups and can react with active groups such as diisocyanate, but the hydroxyl group of hydroxyl silicone oil is directly connected to siloxane, which has poor stability , Poor hydrolysis resistance, the performance of the polyurethane material prepared by it is poor, it is difficult to apply and promote; although the reactivity of polyether modified silicone oil is better than that of hydroxyl silicone oil, the stability is still poor, and the molecular weight of the general polyether segment is relatively large , the intermolecular force is small, and it cannot solve the incompatibility problem between the urethane group or urea group and polysiloxane, resulting in poor interfacial bonding force between the soft and hard segment of the polyurethane material, resulting in poor mechanical properties of the material

Method used

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  • Polysiloxane-ester polyols, and preparation method and application thereof
  • Polysiloxane-ester polyols, and preparation method and application thereof
  • Polysiloxane-ester polyols, and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0023] A polysiloxane-ester polyol, the components of which include in parts by weight: 2000g of hydroxyl silicone oil (molecular weight: 758g / mol), 2749.34g of ε-caprolactone monomer and 0.095g of stannous octoate.

[0024] The preparation method of above-mentioned polysiloxane-ester polyol, step is as follows:

[0025] (1) Dehydrate 2000g of hydroxy silicone oil at 100°C under reduced pressure, and the moisture content is determined to be 120ppm;

[0026] (2) Continue to add 2749.34 g of ε-caprolactone monomer that has been dewatered and dried by 4A molecular sieve, and after stirring and dispersing evenly, add 0.095 g of stannous octoate;

[0027] (3) Raise the temperature of the mixed components in step (2) to 140° C., react for 16 hours, react under reduced pressure for 4 hours, and lower the temperature to obtain polysiloxane-ester polyol.

[0028] According to the DIN 53240 standard, the acid value titration analysis test of the obtained polysiloxane-ester polyol has a...

Embodiment 2

[0030] A polysiloxane-ester polyol, its components include by weight parts: polyether modified silicone oil 1500g (molecular weight is 1100g / mol), ε-caprolactone monomer 1227.3g and bismuth carboxylate 0.082g ;

[0031] Wherein, the molecular weight of the polyether segment in the polyether-modified silicone oil is 102 g / mol.

[0032] The preparation method of above-mentioned polysiloxane-ester polyol, step is as follows:

[0033] (1) 1500g of polyether modified silicone oil was dehydrated under reduced pressure at 110°C, and the moisture content was confirmed to be 128ppm;

[0034] (2) Continue to add 1227.3 g of ε-caprolactone monomer dried by 4A molecular sieve, after stirring and dispersing evenly, add 0.082 g of bismuth carboxylate;

[0035] (3) Raise the temperature of the mixed components in step (2) to 150° C., react for 20 hours, react under reduced pressure for 3 hours, and lower the temperature to obtain polysiloxane-ester polyol.

[0036] According to the DIN 53...

Embodiment 3

[0038] A polysiloxane-ester polyol, its components include by weight parts: polyether modified silicone oil 2000g (molecular weight is 1600g / mol), ε-caprolactone monomer 1125g and tetraisopropyl titanate 0.11g;

[0039] Wherein, the molecular weight of the polyether segment in the polyether-modified silicone oil is 214 g / mol.

[0040] The preparation method of above-mentioned polysiloxane-ester polyol, step is as follows:

[0041] (1) 2000g of polyether modified silicone oil was dehydrated under reduced pressure at 110°C, and the moisture content was confirmed to be 132ppm;

[0042] (2) Continue to add 1125 g of ε-caprolactone monomer that has been dewatered and dried by 4A molecular sieve, and after stirring and dispersing evenly, add 0.11 g of tetraisopropyl titanate;

[0043] (3) Raise the temperature of the mixed components in step (2) to 150° C., react for 22 hours, react under reduced pressure for 4 hours, and lower the temperature to obtain polysiloxane-ester polyol. ...

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Abstract

The invention belongs to the technical field of high polymer material preparation, and particularly relates to polysiloxane-ester polyols, and a preparation method and application thereof. The polysiloxane-ester polyols provided by the invention participate in the preparation of a polyurethane material, so that the content of polysiloxane chain segments is retained; the reaction activity and the stability of polysiloxane polyols, diisocyanate and the like are improved through the introduction of the polysiloxane chain segments; intermolecular hydrogen bond interaction between the polysiloxanechain segments and ester groups as well as urethane groups or carbamido is much higher than the action force between the polysiloxane and the polyether as well as the urethane groups, so that high cohesion strength is achieved; the action force between a soft segment and a rigid segment is remarkably higher than that of the product based on hydroxyl silicone oil or polyether-modified silicone oil;the interface bonding force is high; the compatibility of an organic silicon chain segment and a rigid polyurethane segment is further improved; the obtained polyurethane material is excellent in comprehensive performance, and is particularly suitable for preparing low-rigidity (55 to 80 A) TPU, and can be applied to wearable materials, such as a watchband.

Description

technical field [0001] The invention belongs to the technical field of polymer material preparation, and in particular relates to a polysiloxane-ester polyol, its preparation method and application. Background technique [0002] Polysiloxane is a main chain formed by alternating silicon-oxygen bonds, and side chains are organic groups connected to silicon atoms. It has good thermal stability and good air permeability. It is widely used in construction, automobile, aerospace and other fields. It has a wide range of applications, but the low glass transition temperature and poor mechanical properties of polysiloxane limit its further application. Silicone materials such as polysiloxane are used more and more in the field of polyurethane. Polyurethane materials benefit from the introduction of silicone components to improve their surface properties and touch, high and low temperature resistance, and bacteria resistance. body for applied research in the field of polyurethane. ...

Claims

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Application Information

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IPC IPC(8): C08G63/695C08G63/08C08G63/85C08G64/18C08G64/30C08G18/46
CPCC08G63/695C08G63/08C08G63/823C08G64/186C08G64/30C08G18/4692
Inventor宋红玮刘德富傅恺凡战振生李庆钊
OwnerMIRACLL CHEM