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Siloxane-containing polyacrylate capable of being moisture-cured at room temperature, and preparation method thereof

A siloxane polyacrylate and polyacrylate technology, which is applied in the field of room temperature moisture-curable siloxane-containing polyacrylate and its preparation, can solve the problem of long surface drying time, harsh synthesis reaction conditions, and unfavorable large-scale industrial Production and other issues, to achieve the effect of rapid curing

Inactive Publication Date: 2020-05-08
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these two methods can introduce active siloxane groups into the polyacrylate molecular chain and realize the moisture curing of acrylate, they also have some shortcomings: such as the polymer prepared by the direct synthesis method of KH570 Slow curing speed, long surface dry time
Silicone-based polyacrylate synthesized by living radical polymerization, the synthesis reaction conditions are relatively harsh; the process is complicated, which is not conducive to large-scale industrial production

Method used

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  • Siloxane-containing polyacrylate capable of being moisture-cured at room temperature, and preparation method thereof
  • Siloxane-containing polyacrylate capable of being moisture-cured at room temperature, and preparation method thereof
  • Siloxane-containing polyacrylate capable of being moisture-cured at room temperature, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Preparation of double bond-containing siloxane coupling agent

[0031] Add 4 g (0.034 mol) of hydroxyethyl acrylate, 7.052 g (0.034 mol) of 3-isocyanatopropyltrimethoxysilane, 0.02 g of stannous octoate, and mechanically stir in a four-necked flask equipped with a thermometer and a stirring paddle. The bath was warmed to 70°C for reaction. The reaction was monitored by a Fourier transform infrared spectrometer until the -NCO infrared absorption peak disappeared to obtain a double bond-containing siloxane coupling agent with a yield of 100%. The NMR characterization is shown in the attached figure.

[0032] (2) Preparation of siloxane-containing polyacrylate

[0033] Weigh 75g of methyl acrylate, 0.8g of dodecyl mercaptan, 0.71g of azobisisobutyronitrile, and 11.052g of double bond-containing siloxane coupling agent, mix them together, and place them in a beaker for subsequent use; Add 20g of solvent ethanol to the reflux condenser and mechanically stirred four-ne...

Embodiment 2

[0037] (1) Preparation of double bond-containing siloxane coupling agent

[0038] Add 4.92g (0.034mol) of hydroxypropyl methacrylate, 8.39g (0.034mol) of 3-isocyanatopropyltriethoxysilane, and 0.02g of butyltin dilaurate into a four-necked flask equipped with a thermometer and a stirring paddle , mechanically stirred, and the oil bath was heated to 50°C for reaction. The reaction is monitored by a Fourier transform infrared spectrometer until the -NCO infrared absorption peak disappears to obtain a double bond-containing siloxane coupling agent with a yield of 100%.

[0039] (2) Preparation of siloxane-containing polyacrylate

[0040] Weigh 60g of ethyl acrylate, 15g of methyl methacrylate, 1.6g of octyl mercaptan, 0.71g of benzoyl peroxide, and 12.81g of double bond-containing siloxane coupling agent, mix them together, and place them in a beaker for later use; Add 20 g of solvent methanol to a four-necked flask equipped with a reflux condenser and mechanical stirring, add ...

Embodiment 3

[0044] (1) Preparation of double bond-containing siloxane coupling agent

[0045] Add hydroxyethyl acrylate 4g (0.034mol), 3-isocyanate group propyl methyl dimethoxysilane 6.426g (0.034mol) in the four-necked flask that thermometer, stirring paddle are housed, catalyzer stannous octoate 0.02g, Stir mechanically, and heat the oil bath to 70°C for reaction. The reaction is monitored by a Fourier transform infrared spectrometer until the infrared stretching vibration peak of -NCO disappears to obtain a siloxane coupling agent containing a double bond with a yield of 100%.

[0046] (2) Preparation of siloxane-containing polyacrylate

[0047] Weigh 40g of methyl acrylate, 35g of ethyl acrylate, 2.4g of dodecyl mercaptan, 0.71g of azobisisobutyronitrile, and 11.052g of double bond-containing siloxane coupling agent, mix them together, and place them in a beaker Standby; add 20g of solvent ethanol to a four-necked flask equipped with a reflux condenser and mechanical stirring, add ...

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Abstract

The invention belongs to the field of chemical materials, and particularly relates to a siloxane-containing polyacrylate capable of being moisture-cured at room temperature, and a preparation method thereof. The preparation method comprises the following steps: synthesizing a siloxane coupling agent containing double bonds, and carrying out free radical copolymerization on the siloxane coupling agent containing double bonds and an alkene monomer to prepare the siloxane-containing polyacrylate capable of being moisture-cured at room temperature. The invention provides a preparation method of the double bond-containing siloxane coupling agent, and the invention also provides the preparation method of the siloxane-containing polyacrylate capable of being moisture-cured at room temperature. The method for synthesizing the siloxane-containing acrylate polymer capable of being moisture-cured at normal temperature has the advantages of mild reaction conditions and simple process; and the obtained polymer has the advantages of high mechanical strength and adjustable surface drying time.

Description

technical field [0001] The invention belongs to the field of chemical materials, and in particular relates to a room-temperature moisture-curable silicone-containing polyacrylate and a preparation method thereof. Background technique [0002] Silicone-containing polymers can be moisture-cured using moisture in the air. Compared with isocyanate moisture-curing, silicone moisture-curing process does not release gas, does not bubble, and the Si-O-Si bond in the cured structure The polymer has good heat resistance and weather resistance, so it is widely used in coatings, adhesives, elastomers and other fields. At present, there are many studies on the synthesis of silicone moisture-curing polymers, such as silicone-terminated polyether (MS) and silicone-terminated polyurethane (SPU), which have been commercialized. However, SPU and MS have some disadvantages. For example, the main chain of SPU molecule is urethane, and the polymer has high viscosity, which affects its construct...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/14C08F220/18C08F212/08C08F230/08
CPCC08F220/14C08F220/18C08F230/08
Inventor 李坚池全超任强汪称意
Owner CHANGZHOU UNIV