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A kind of preparation method of reactive sealant resin

A sealant, reactive technology, applied in the field of sealants, can solve the problems affecting the performance of sealants, difficult to remove by-product salts, wide molecular weight distribution, etc., and achieve the effects of easy recovery, excellent mechanical properties, and narrow molecular distribution.

Active Publication Date: 2022-08-05
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]Into the 1L kettle, 32g (1mol) of methanol was added as the starting agent, 0.7g of catalyst sodium hydroxide was added, and nitrogen was replaced.

[0069] Add 6.68g allyl glycidyl ether, heat up to 100°C, pressurize to 0.05MPa and react for 1h; then add 460.92g propylene oxide, react until the pressure no longer changes, add 200.4g ethylene oxide, the total reaction time is 1h , until the reaction pressure no longer changes, the crude polyether product is obtained after curing for 1h, and the neutralizer phosphoric acid, 1% water, 0.1% adsorbent magnesium silicate and 0.01% of the total mass of the crude polyether are added. The filter aid diatomaceous earth is further filtered to obtain the purified second polyether polyol.

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

Embodiment 2

[0088] 2.3 g (0.05 mol) of ethanol and 4.6 g (0.05 mol) of triglyceride were added to the 1 L kettle as starting agents, and 10 g of catalyst potassium hydroxide was added, and nitrogen was replaced.

[0089] 14 g of methallyl glycidyl ether and 13.7 g of acrylic acid glycidyl ether were added, the temperature was raised to 150° C., and the pressure was increased to 0.5 MPa to react for 10 h. After the reaction pressure no longer changes, the crude polyether product is obtained after aging for 5 hours, adding 1% neutralizer phosphoric acid, 10% water, 8% adsorbent magnesium silicate and 1% filter aid accounting for the total mass of the crude polyether agent diatomaceous earth, and then filtered to obtain the purified second polyether polyol.

[0090] After measurement, the water content and acid value of the product are qualified; the hydroxyl value of the above product is 11.2mgKOH / g (theoretical hydroxyl value 11.22mgKOH / g), which proves that the molecular weight has reache...

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 to the 10L kettle - 3.04 g of propylene glycol, 1.04 g of neopentyl glycol and 1.64 g of sorbitan as starting agents, 2.5 g of catalyst sodium methoxide was added, and nitrogen was replaced.

[0107] 250 g of methallyl glycidyl ether and 750 g of acrylic acid glycidyl ether were added, the temperature was raised to 125° C., and the pressure was increased to 0.3 MPa to react for 5 h. Then add 80g propylene oxide, react until the pressure no longer changes, the total reaction time is 5h, and after curing for 2.5h, a crude polyether product is obtained, and 0.5% of the total mass of the crude polyether is added with neutralizing agent phosphoric acid, 5% water, 4% of the adsorbent magnesium silicate and 0.5% of the filter aid diatomaceous earth, and then filtered to obtain the second re...

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Abstract

The invention discloses a preparation method of a reactive sealant resin. The method comprises: (1) a hydroxyl-containing initiator is polymerized with an epoxy compound under the action of an alkali catalyst to obtain a polyether polyol; (2) In the polyether polyol obtained in step (1), an alkoxide reagent and a halogenated end-capping agent containing double bonds are added to react to obtain a double-bond-terminated polyether crude product, and the obtained crude product is refined to obtain Modified polyether product; (3) Under the action of hydrosilylation catalyst, the modified polyether and hydrogen-containing silane are subjected to silane end capping reaction to obtain the target product reactive sealant resin. The resin has excellent properties, good adhesion and paintability.

Description

technical field [0001] The invention relates to the field of sealants, in particular to a preparation method of a reactive sealant resin, which is mainly used for preparing elastic sealants. Background technique [0002] Since the 1980s, with the development of urban building modernization and the improvement of building function requirements, the variety and quantity of high-performance sealants for joint sealing of building structures in my country have increased. Acrylic, silicone and polyurethane sealants have been developed one after another, and the development is very rapid. Among them, silicone-based sealants have developed the fastest, with the advantages of fast curing speed, excellent high temperature resistance and weather resistance, but there are disadvantages such as low strength and unpaintable surface. Polyurethane sealants have high strength, oil and solvent resistance, and good wear resistance, but they have disadvantages such as easy foaming during curing...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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