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Preparation method of reactive sealant resin

A kind of sealant, reactive technology, applied in the field of sealant, can solve the problems of affecting the performance of sealant, weather resistance deviation, wide molecular weight distribution, etc.

Active Publication Date: 2020-07-07
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 2. Synthesize a high molecular weight polyether with a double bond at one end and a hydroxyl group at one end, and then multiply it with a coupling agent (such as diisocyanate, etc.) to a modified polyether with a higher molecular weight, and then make a terminal siloxane through the end-capping process Based polyether, the molecular weight of the polyether used is relatively high, and the urethane group contained in the molecular chain is small, and a coupling reaction can be carried out by the coupling agent, which has little effect on the viscosity of the polymer, and there is no by-product of the coupling reaction , the process operation is relatively simple, but there are coupling agent residues in the product, and the weather resistance deviation
[0007] 3. Use the Williamson ether synthesis method to react the hydroxyl-terminated polyether with lower molecular weight with alkali metal or alkali metal hydroxide, couple with dichloromethane to double its molecular weight, and then react with allyl chloride to form a double-bonded polyether , through silicon-oxygen addition reaction to produce terminal siloxane-based polyether, but the molecular weight distribution of the chain extension product with dichloromethane is relatively wide, which directly affects the performance of sealants, and can only be used to prepare bifunctional resins
[0008] 4. Using bimetallic catalysts to synthesize high-molecular-weight hydroxyl-terminated polyethers, and then modify the polyethers to make siloxane-terminated polyethers through hydrosilicon addition, but the removal of by-product salts in the process is a difficult point. There is no reasonable solution yet

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Add 32 g (1 mol) of methanol into a 1 L kettle as a starter, add 0.7 g of catalyst sodium hydroxide, and replace with nitrogen.

[0069] Add 6.68g of allyl glycidyl ether, raise the temperature to 100°C, pressurize to 0.05MPa and react for 1h; then add 460.92g of propylene oxide, react until the pressure does not change, then add 200.4g of ethylene oxide, and the total reaction time is 1h , to obtain the crude polyether product after maturing for 1 h after the reaction pressure no longer changes, and add 0.1% neutralizing agent phosphoric acid, 1% water, 0.1% adsorbent magnesium silicate and 0.01% The filter aid diatomite is further filtered to obtain the refined second polyether polyol.

[0070] After determination, the water content and acid value of the product are qualified (moisture <0.05%, acid value <0.1mgKOH / g, the same below); the hydroxyl value is 80.1mgKOH / g (theoretical hydroxyl value is 80.14mgKOH / g), which proves that the molecular weight has reached the c...

Embodiment 2

[0088] Adding ethanol 2.3g (0.05mol) and triglycerol 4.6g (0.05mol) in a 1L kettle are starters, add catalyst potassium hydroxide 10g, and replace with nitrogen.

[0089] Add 14g of methallyl glycidyl ether and 13.7g of glycidyl acrylate ether, raise the temperature to 150°C, pressurize to 0.5MPa and react for 10h. After aging for 5 hours until the reaction pressure no longer changes to obtain the crude polyether product, add 1% neutralizing agent phosphoric acid, 10% water, 8% adsorbent magnesium silicate and 1% filter aid agent diatomaceous earth, and then filtered to obtain the refined second polyether polyol.

[0090] After measurement, the water content and acid value of the product are qualified; the above-mentioned product has a hydroxyl value of 11.2mgKOH / g (theoretical hydroxyl value 11.22mgKOH / g), which proves that the molecular weight has reached the calculated molecular weight of 10000, and the measured degree of unsaturation is 0.022mmol / g ( The theoretical degre...

Embodiment 3

[0106] Add 0.38g of ethylene glycol monomethyl ether, 0.45g of 1,2-propylene glycol monomethyl ether, 2.4g of diethylene glycol monomethyl ether, 0.62g of ethylene glycol, 1,2-propylene glycol / 1,3 -Propylene glycol 3.04g, neopentyl glycol 1.04g and sorbitan 1.64g are starters, catalyst sodium methoxide 2.5g is added, nitrogen replacement.

[0107] Add 250g of methallyl glycidyl ether and 750g of acrylate glycidyl ether, raise the temperature to 125°C, pressurize to 0.3MPa and react for 5h. Then add 80g of propylene oxide, react until the pressure does not change, the total reaction time is 5h, after aging for 2.5h, the crude polyether product is obtained, and add 0.5% neutralizing agent phosphoric acid, 5% water, 4% magnesium silicate as an adsorbent and 0.5% diatomite as a filter aid, and then filtered to obtain the refined second polyether polyol.

[0108] After measurement, the water content and acid value of the product are qualified; the hydroxyl value is 21.4mgKOH / g (th...

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Abstract

The invention discloses a preparation method of reactive sealant resin, which comprises the following steps: (1) polymerizing a hydroxyl-containing initiator with an epoxy compound under the action ofan alkali catalyst to obtain polyether polyol; (2) adding an alkoxide reagent and a halogenated end-capping reagent containing double bonds into the polyether polyol obtained in the step (1) to reactso as to obtain a double-bond end-capped polyether crude product, and refining the obtained crude product so as to obtain a modified polyether product; and (3) carrying out silane end-capping reaction on the modified polyether and hydrogen-containing silane under the action of a hydrosilylation catalyst to obtain the target product reactive sealant resin. The resin is excellent in property, and has good adhesion and finishing property.

Description

technical field [0001] The invention relates to the field of sealants, in particular to a method for preparing a reactive sealant resin, which is mainly used for preparing elastic sealants. Background technique [0002] Since the 1980s, with the modernization of urban buildings and the improvement of building function requirements, there are more and more varieties and quantities of high-performance sealants used for sealing joints in building structures in my country. The earliest used in buildings is the polysulfide type. Acrylic, silicone and polyurethane sealants have been developed successively, and the development is very rapid. Among them, the silicone type sealant has the fastest development, which has the advantages of fast curing speed, high temperature resistance and weather resistance, but has the disadvantages of low strength and unpaintable surface. Polyurethane sealants have high strength, good oil and solvent resistance, and good abrasion resistance, but they...

Claims

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Application Information

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IPC IPC(8): C08G65/26C08G65/336C08G65/337
CPCC08G65/2609C08G65/2648C08G65/337C08G65/336C08G2650/04
Inventor 鞠昌讯刘斌王明永叶天石正阳黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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