A kind of thiourea copolymer heat stabilizer and preparation method thereof

A heat stabilizer and copolymer technology, applied in the field of thiourea copolymer heat stabilizers and their preparation, can solve the problems of poor thermal stability, affecting the thermal stability of heat stabilizers, affecting the thermal stability of heat stabilizers, etc. , to achieve the effects of improving thermal stability, inhibiting autocatalysis, and reducing the formation of conjugated systems

Active Publication Date: 2019-06-18
SOUTHEAST UNIV
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Problems solved by technology

Chinese patent CN105949667A discloses a β-diketone organic barium / zinc polyvinyl chloride heat stabilizer and a preparation method thereof, although the β-diketone organic barium / zinc polyvinyl chloride heat stabilizer prepared by the method combines barium / The advantages of zinc stabilizer and β-diketone compound auxiliary heat stabilizer, but there is a phenomenon of "zinc burning" during the use of the heat stabilizer, which affects the thermal stability of the heat stabilizer
Chinese patent CN105936679A discloses a monovinyl alcohol maleate barium salt heat stabilizer and a preparation method thereof. The heat stabilizer prepared by the method has poor thermal stability when acting on polyvinyl chloride alone, and cannot be used alone. Only when used in combination with zinc soap can it show certain thermal stability
Chinese patent CN105885087A discloses a novel polyvinyl chloride heat stabilizer bis(pyridin-4-ylmethyl)zinc adipate, although the heat stabilizer can absorb free hydrogen chloride, there will also be "zinc burning" Phenomenon, affecting the thermal stabilization effect of the thermal stabilizer

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  • A kind of thiourea copolymer heat stabilizer and preparation method thereof
  • A kind of thiourea copolymer heat stabilizer and preparation method thereof
  • A kind of thiourea copolymer heat stabilizer and preparation method thereof

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preparation example Construction

[0036] The preparation method of above-mentioned this thiourea copolymer thermal stabilizer is:

[0037]a. At room temperature, add the ammonium thiocyanate acetone solution with a concentration of 100~150g / L into the reaction kettle. Acyl chloride is added into the reaction kettle, after reaction at room temperature, centrifuged to obtain a mixture of benzoyl isothiocyanate and acetone. Add it to the above-mentioned benzoyl isothiocyanate-acetone mixture, heat up, and react. According to the mass ratio of acryloyl chloride to benzoyl chloride is 0.5:1-0.9:1, add acryloyl chloride to the above-mentioned reaction liquid, heat up, After the reaction, it was cooled to room temperature and centrifuged to obtain 4-(3-benzoylthioureido)phenylacrylate, washed with absolute ethanol 4 to 6 times the quality of benzoyl chloride, and dried in vacuo to obtain 4- (3-benzoylthioureido)phenyl acrylate monomer;

[0038] b. At room temperature, add acrylamide-acetone solution with a concentr...

Embodiment 1

[0042] a. At 25°C, add 1.2L of 100g / L ammonium thiocyanate in acetone solution into the reactor, add 120g of benzoyl chloride into the reactor within 0.5h, react at 25°C for 1h, and centrifuge to obtain benzoyl Acyl isothiocyanate acetone mixture, add 96g of p-aminophenol to the above benzoyl isothiocyanate acetone mixture, heat up to 40°C, react for 3h, then add 78g of acryloyl chloride to the above reaction solution, Raise the temperature to 70°C, react for 6 hours, cool down to room temperature, and centrifuge to obtain 4-(3-benzoylthioureido)phenylacrylate, wash 3 times with 400g of absolute ethanol, and dry in vacuum at 60°C for 10h to obtain 4-(3-benzoylthioureido)phenyl acrylate monomer;

[0043] b. At 25°C, add 1.2L of 150g / L acrylamide-acetone solution into the reaction kettle, add 330g of N-piperazinecarboxylic acid into the reaction kettle, raise the temperature to 60°C, react for 7 hours, cool down to room temperature, and centrifuge. To obtain N-acryloyl piperazi...

Embodiment 2

[0047] a. At 25°C, add 1.2L of 100g / L ammonium thiocyanate in acetone solution into the reactor, add 60g of benzoyl chloride into the reactor within 1 hour, react at 25°C for 2 hours, and centrifuge to obtain benzoyl Isothiocyanate-acetone mixed solution, add 51g of p-aminophenol to the above-mentioned benzoyl isothiocyanate-acetone mixed solution, raise the temperature to 60°C, react for 6h, add 45g of acryloyl chloride to the above-mentioned reaction solution, heat up After reacting for 8 hours at 85°C, cool down to room temperature, and centrifuge to obtain 4-(3-benzoylthioureido)phenylacrylate, wash with 200g of absolute ethanol three times, and dry in vacuum at 60°C for 10h to obtain 4 -(3-benzoylthioureido)phenyl acrylate monomer;

[0048] b. At 25°C, add 1.2L of 200g / L acrylamide-acetone solution into the reaction kettle, add 440g of N-piperazinecarboxylic acid into the reaction kettle, raise the temperature to 80°C, react for 9 hours, cool down to room temperature, and...

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Abstract

The invention relates to a thiourea copolymer heat stabilizer and a preparation method thereof, the heat stabilizer is composed of 4-(3-benzoylthiourea group) phenyl acrylate monomer and acrylamide N heterocyclic derivative The monomer is prepared by free radical copolymerization, and its general structural formula is: one of, the degree of polymerization X is 300-500, and the degree of polymerization Y is 600-1000. The thiourea copolymer heat stabilizer is a high-molecular copolymer, which is environmentally friendly. Its unique disubstituted thiourea structure can easily replace the unstable chlorine atoms on the polyvinyl chloride chain during processing, forming a stable structure and reducing conjugation. The formation of the system, the imine group and the basic N heterocyclic group contained in the molecular side chain can quickly absorb the generated hydrogen chloride, inhibit the autocatalysis of hydrogen chloride, improve the thermal stability of polyvinyl chloride, and the ester in the molecular structure The base has a lubricating effect.

Description

technical field [0001] The invention relates to the field of heat stabilizers for polyvinyl chloride processing additives, in particular to a thiourea copolymer heat stabilizer and a preparation method thereof. Background technique [0002] Polyvinyl chloride has the advantages of high strength, plasticization, corrosion resistance, flame retardant, good insulation and high transparency. It is used in building materials, industrial products, daily necessities, floor leather, floor tiles, artificial leather, pipes, wires and cables, packaging films , bottles, foaming materials, sealing materials, fibers, etc. are widely used. However, in the actual polymerization process of polyvinyl chloride, many side reactions will occur, so that there are many defective structures in the molecular structure of polyvinyl chloride. Therefore, polyvinyl chloride is prone to dehydrochlorination reaction under the action of temperature and pressure during processing. The degradation performan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/60C08F220/38C08L27/06C08L33/24
CPCC08L27/06C08L2201/08C08F220/603C08L33/24C08F220/387
Inventor 周钰明黄双何曼任慧丁彬彬申华黄裕中
Owner SOUTHEAST UNIV
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