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Long-chain siloxy ethenyl siloxane, modified (methyl) acrylic ester polymer emulsion thereof, and preparation method

A technology of chain siloxyvinyl siloxane and polymer emulsion, which is applied in the field of long chain siloxyvinyl siloxane and its modified (meth)acrylate polymer emulsion and preparation, and can solve the problem of placement Poor stability, high activity of hydrolyzed groups, short molecular chains, etc., achieve good stability, good elongation at break and tensile strength, and improve water resistance

Active Publication Date: 2015-04-22
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of silane coupling agents alone has some disadvantages. For example, its molecular chain is usually short, and it is easily covered and embedded by acrylate chains during the reaction. The modification effect of silicone is not obvious; and its hydrolyzed groups are more active. , easy to react with each other and cross-linked entanglement, poor placement stability

Method used

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  • Long-chain siloxy ethenyl siloxane, modified (methyl) acrylic ester polymer emulsion thereof, and preparation method
  • Long-chain siloxy ethenyl siloxane, modified (methyl) acrylic ester polymer emulsion thereof, and preparation method
  • Long-chain siloxy ethenyl siloxane, modified (methyl) acrylic ester polymer emulsion thereof, and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 110g of deionized water, 4g of dodecylbenzenesulfonic acid (DBSA), 2g of alkylphenol polyoxyethylene ether (NP-9) into a reaction vessel equipped with a stirrer, a thermometer, a condenser tube and a nitrogen gas inlet tube , 37.5g octamethylcyclotetrasiloxane (D4), feed nitrogen, react at 70°C for 9h, then add 2.5g γ-methacryloxypropyl trimethoxysilane (KH-570), at 70 After reacting at ℃ for 9 hours, air-cool and discharge the material to obtain a long-chain siloxyvinyl siloxane emulsion, drop the obtained long-chain siloxyvinyl siloxane emulsion into ethanol twice its volume, and then oscillate with ultrasonic waves for 4 hours , let stand for 10h, pour off the supernatant to obtain long-chain siloxyvinyl siloxane, the structure of which is shown below.

[0028]

[0029] where R 5 , R 6 is methoxy, hydroxyl,

[0030] n4 and n5 are natural numbers divisible by 4 within 4 to 2000.

[0031] The infrared spectrum data of this long-chain siloxyvinyl siloxane i...

Embodiment 2

[0034] Add 80g of deionized water, 3g of dodecylbenzenesulfonic acid (DBSA), 2g of alkylphenol polyoxyethylene ether (NP-9) into a reaction vessel equipped with a stirrer, thermometer, condenser tube and nitrogen gas inlet tube , 10g octamethylcyclotetrasiloxane (D4), feed nitrogen, react at 70°C for 9h, then add 2.5g γ-methacryloxypropyltrimethoxysilane (KH-570), react at 70°C 9h, to obtain long-chain siloxyvinyl siloxane emulsion, then add 5.3g isooctyl methacrylate and 2.5g isobutyl methacrylate, 0.5g ammonium persulfate (dissolved in 10g deionized water), in After reacting at 70°C for 9 hours, the material was cooled in air to obtain a long-chain siloxyvinylsiloxane-modified (meth)acrylate polymer emulsion. Emulsion properties: emulsion solid content: 17.6%, emulsion particle size: 338nm, emulsion storage stability: 6 months; emulsion film-forming properties: elongation at break: 240%, tensile strength: 5.24MPa, water absorption: 26% .

Embodiment 3

[0036] Add 110g of deionized water, 4g of hexadecylbenzenesulfonic acid, 2g of alkylphenol polyoxyethylene ether (NP-9), 15g of eight Methylcyclotetrasiloxane (D4), feed nitrogen, react at 75°C for 7h, then add 4.0g vinyltrimethoxysilane, react at 75°C for 7h, and obtain long-chain siloxyvinylsiloxane emulsion , then add 13.5g butyl acrylate and 4.5g methyl methacrylate, 1.2g ammonium persulfate (dissolved in 10g deionized water), react at 75°C for 7h and discharge in air cooling to obtain long-chain siloxy vinyl siloxane Alkane-modified (meth)acrylate polymer emulsion. Emulsion properties: emulsion solid content: 22.7%, emulsion particle size: 362nm, emulsion storage stability: 6 months; emulsion film-forming properties: elongation at break: 265%, tensile strength: 6.47MPa, water absorption: 21% .

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Abstract

The invention discloses long-chain siloxy ethenyl siloxane, modified (methyl) acrylic ester polymer emulsion thereof, and a preparation method. The method comprises the steps that 80 to 150 parts of water, 3 to 6 parts of anionic emulsifier, 2 to 4 parts of non-ionic emulsifier and 8 to 37.5 parts of octamethyl cyclotetrasiloxane are reacted for 3 to 9h at 70 to 90 DEG C under nitrogen protection; then 2.5 to 7.5 parts of siloxane containing unsaturated double bond is added to be reacted with the mixture for 3 to 9h at 75 to 90 DEG C, so as to obtain long-chain siloxy ethenyl siloxane emulsion; the emulsion is conducted to demulsification through ethanol, so as to obtain long-chain siloxy ethenyl siloxane; and 97.5 to 167.5 parts of the siloxane emulsion, 7.8 to 50 parts of (methyl) acrylic ester monomer and 0.5 to 3 parts of initiator are reacted for 3 to9h at 70 to 90 DEG C, so as to obtain (methyl) acrylic ester polymer emulsion modified by the long-chain siloxy ethenyl siloxane. The emulsion has good water resistance, and the elongation at break and the tensile strength of a coating film of the emulsion are enhanced.

Description

technical field [0001] The invention relates to a long-chain siloxy vinyl siloxane and its modified (meth)acrylate polymer emulsion and a preparation method. Background technique [0002] Coatings with (meth)acrylic acid and its ester copolymers as the main film-forming substances are collectively referred to as acrylic coatings. Acrylic paint has light color, plump film and good mechanical strength, and has become an important type of paint. However, it also has disadvantages such as poor water resistance, brittleness at low temperature, and insufficient weather resistance, which affect its practical effect. Polysiloxane just has good water resistance, weather resistance, and good flexibility. For this reason, researchers have proposed acrylic-organic silicon coatings, which combine the strengths of acrylic coatings and silicone coatings. By introducing a certain amount of organic silicon functional groups into the main chain and side chain of acrylic resin macromolecules,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/20C07F7/18C07F7/08C08J3/09C08F283/12C08F230/08C09D151/08C09D143/04
Inventor 刘伟区苏奎
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI