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Siloxane-terminated polymer homopolymerization reaction preparation method and moisture-curable composition

A polymerization reaction and polymer technology, applied in the field of materials, can solve problems affecting the storage stability of siloxane-terminated polymers, the degradation of isocyanate-based siloxane of the blocking agent, and the high viscosity of siloxane-terminated polymers. , to achieve excellent storage stability, reduction of capping side reaction products, and high hydrolytic crosslinking activity

Active Publication Date: 2021-10-01
娄从江
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the poor compatibility between the strongly polar and highly crystalline urea bonds and the polyether main chain, the resulting siloxane-terminated polymer has a very high viscosity, which brings inconvenience to the subsequent use process
In addition, if the basic aminosiloxane remains, it will greatly affect the storage stability of the obtained siloxane-terminated polymer
[0013] When capping with isocyanatosiloxanes, other side reactions may occur in addition to the carbamate forming reactions expected in polymer preparation. Lead to degradation and loss of blocking agent - isocyanate siloxane

Method used

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  • Siloxane-terminated polymer homopolymerization reaction preparation method and moisture-curable composition
  • Siloxane-terminated polymer homopolymerization reaction preparation method and moisture-curable composition
  • Siloxane-terminated polymer homopolymerization reaction preparation method and moisture-curable composition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0103] Embodiment 1: Preparation of siloxane-terminated polymer (P) by homopolymerization method

[0104] Dehydrate 3500g of pre-dehydrated DL-12000D polyether polyol (120°C with vacuum stirring for 2 hours, and cool to room temperature with N 2 protection), add in a 5L four-necked flask (respectively with anchor stirrer port, thermometer port, vacuum / nitrogen port, feeding port), and then add 2.0g metal-containing titanium catalyst ( TPT) and 1.5g metal-containing bismuth (III) catalyst ( C716), stirring and vacuum degassing, using N 2 Puncture the vacuum and replace with N 2 protection, add 130.0gIPDI, at N 2 After stirring evenly under protection, heat in a water bath until the temperature of the material is 80 to 85°C, and continue to pass N 2 Protect and maintain the reaction for 2 hours.

[0105] Sampling shall be carried out by titration method to detect the isocyanate content of the prepolymer. Stop heating until the isocyanate content reaches 0.67%. Continue co...

Embodiment 2

[0111] Embodiment 2: Preparation of siloxane-terminated polymer (P) by homopolymerization method

[0112] Dehydrate 3500g of pre-dehydrated DL-8000D polyether polyol (120°C with vacuum stirring for 2 hours, and cool to room temperature with N 2 protection), add 5L double planetary vacuum stirring tank (XGFJ-8L type planetary high-speed mixer, equipment manufacturer: Chengdu Silicon Special Automation Equipment Co., Ltd.), and then add 1.1g catalyst solution containing metal iron (acetylacetonate iron (III ), 50wt% pre-dissolved in toluene) and 0.9g metal-containing zinc catalyst (zinc dimethacrylate (II)), stirring and vacuum degassing, using N 2 Puncture the vacuum and replace with N 2 protection, adding 147.7gHDI, in N 2 After stirring evenly under protection, heat in a water bath until the temperature of the material is 80 to 85°C, and continue to pass N 2 Protect and maintain the reaction for 2 hours.

[0113] Sampling shall be carried out by titration to detect the is...

Embodiment 3

[0119] Embodiment 3: Preparation of siloxane-terminated polymer (P) by homopolymerization method

[0120] Dehydrate 40kg of pre-dehydrated DL-8000D polyether polyol (heated at 120°C with vacuum stirring for 2 hours, and cool to room temperature with N 2 protection), add 50L double planetary vacuum stirring tank (XGFJ-8L type planetary high-speed mixer, equipment manufacturer: Chengdu Silicon Special Automation Equipment Co., Ltd.), and then add 40.0g catalyst solution containing metal zirconium (zirconium acetylacetonate (IV ), 50wt% dissolved in acetone) and 20.0g metal-containing titanium catalyst (titanium tetraisopropoxide (IV), TPT), stirring and vacuum degassing, using N 2 Puncture the vacuum and replace with N 2 For protection, add 1.97kg Vestanat H 12 MDI, in N 2 After stirring evenly under protection, heat in a water bath until the temperature of the material is 80 to 85°C, and continue to pass N 2 Protect and maintain the reaction for 2 hours.

[0121] Sampling...

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Abstract

The invention discloses a homopolymerization method for preparing a siloxane-terminated polymer (P) with high end-capping rate and high reaction activity, and a moisture-curable composition (C) containing the polymer. According to the preparation method, the preparation process of the siloxane-terminated polymer (P) does not contain a tin catalyst, so that the product is endowed with the excellent characteristics of high termination rate, insensitivity to moisture in air and the like, and the polymer (P) has good storage stability. The moisture-curable composition (C) should further contain, based on 100 parts by mass of the polymer (P), 0.1 to 35 parts of a combination of a catalyst (C1) selected from the group consisting of a metal-containing catalyst, guanidine and imidazole, a promoter (C2) comprising a unit of formula (II), which moisture-curable composition (C) has very high moisture-curing activity, is quickly surface-dried, and is capable of completely eliminating viscosity, and the composition (C) is particularly suitable for applications such as adhesives, sealants, coatings and the like.

Description

technical field [0001] The invention relates to a method for preparing a siloxane-terminated polymer and a moisture-curing composition, in particular to a method for preparing a siloxane-terminated polymer by homopolymerization; and a moisture-curing composition containing the siloxane-terminated polymer The preparation and application of the curing composition belong to the technical field of materials. Background technique [0002] Changing the function of oligomers and polymers through homopolymer reactions is an important synthetic method in the chemical industry, which can adjust and change the properties of polymers, such as polymer reactivity, cross-linking properties, adhesion, Solubility, form and thermal stability, etc. The reaction conditions of several steps of homopolymer reaction are the same or similar, and continuous production can be realized through the design of the production line, which is beneficial to the stability and uniformity of the product, and c...

Claims

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Application Information

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IPC IPC(8): C08G18/75C08G18/73C08G18/71C08G18/66C08G18/48C08G18/32C09D175/08C09D7/61C09D7/63C08L75/08C08K13/02C08K3/26C08K3/36C08K5/12
CPCC08G18/718C08G18/755C08G18/73C08G18/758C08G18/6674C08G18/4825C09D175/08C09D7/61C09D7/63C08K13/02C08K3/26C08K3/36C08K5/12C08K2003/2227C08K3/22C08K3/34C08K5/5419C08L75/08
Inventor 娄从江
Owner 娄从江
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