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Antioxidant containing phosphite organic ester and its synthesis method

A synthetic method, the technology of pentylenetetyl triphosphite ethyl ester, which is applied in the fields of organic chemistry, chemical instruments and methods, adhesive additives, etc., can solve the problems that affect the promotion and use of products, cannot meet the demand, and the pungent phosphorous acid smell, etc. Achieve outstanding anti-oxidation effect, high-efficiency anti-oxidation effect, and color improvement

Active Publication Date: 2019-12-06
浙江锦润生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Domestic phosphite antioxidants have received more and more attention, but most of the existing phosphite antioxidants are hindered phenols, bisphenols and phosphite antioxidants containing benzene. Although it has good anti-oxidation performance, it is strictly a toxic product due to the ingredients containing phenol and benzene
However, non-toxic and environmentally friendly phosphites are still rare, which cannot meet the growing demand for non-toxic antioxidants in the development of the rubber and plastics industry.
In addition, most of these products are liquid products, with a pungent phosphorous acid smell, and the molecular weight is not large, and the defects of extraction and migration will occur during use, thus affecting the popularization and use of the product

Method used

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  • Antioxidant containing phosphite organic ester and its synthesis method
  • Antioxidant containing phosphite organic ester and its synthesis method
  • Antioxidant containing phosphite organic ester and its synthesis method

Examples

Experimental program
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Effect test

example 1

[0029] Add 84 grams of dipentaerythritol, 163 grams of triethyl phosphite, and 1 gram of catalyst phosphoric acid to the reaction flask equipped with electric stirring, electric heating, reflux condenser, temperature measuring system, and nitrogen device. , feed nitrogen to carry out the esterification reaction, control the reaction temperature at 100-180°C, and the reaction time is 180 minutes, and cool to below 100°C after the reaction is completed. Then add 253 grams of stearyl alcohol (i.e. stearyl alcohol), add 3.6 grams of catalyst tetrabutyl titanate, pass through nitrogen to carry out the second step of esterification reaction, the reaction temperature is 150-210 ° C, the reaction time is 180 minutes, after the reaction Cool to below 100°C, heat-preserve and filter through a constant temperature oven at about 80-100°C to obtain a solid organic phosphite antioxidant product - dipentaerythritol triphosphite stearyl alcohol ester.

example 2

[0031] In the reaction flask equipped with electric stirring, electric heating, reflux condenser, temperature measuring system, and nitrogen device, put 90 grams of dipentaerythritol, 272 grams of triethyl phosphite into the reaction flask, and 1.8 grams of catalyst phosphoric acid. Nitrogen is used for esterification reaction, the reaction temperature is 100-180°C, and the reaction time is about 180 minutes. After the reaction is completed, it is cooled to below 100°C. Then add 138 grams of octanol, add 0.7 grams of catalyst stannous chloride, feed nitrogen to carry out the second step of esterification reaction, the reaction temperature is 140-200 ° C, and the reflux reaction time is 180 minutes. After the reaction is completed, it is cooled to below 100 ° C. Filtrate in a constant temperature oven at about 80°C to obtain a liquid organic phosphite antioxidant product - dipentaerythritol triphosphite octanol ester.

example 3

[0033] In the reaction flask equipped with electric stirring, electric heating, reflux condenser, temperature measuring system, and nitrogen device, 81 grams of dipentaerythritol, 159 grams of triethyl phosphite, and 3 grams of catalyst phosphoric acid are put into the reaction flask and passed Enter nitrogen to carry out the esterification reaction, the reaction temperature is 100-180°C, and the reaction time is about 180 minutes. After the reaction is completed, cool to below 100°C. Then add 260 grams of dodecyl hydroxystearyl alcohol, pass through nitrogen to carry out the second step of esterification reaction, control the reaction temperature 150-200 ° C, the reaction time is 150 minutes, then pull vacuum at 200 ° C for 30 minutes, and cool to 100 °C after the reaction is completed. Below 100°C, heat-preserve and filter in a constant temperature oven at about 100°C to obtain a solid organic phosphite antioxidant product-dipentaerythritol triphosphite dodecyl hydroxystearyl...

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Abstract

The invention discloses a novel high-performance phosphorus-containing antioxidant-bipentaerythritol triphosphatidyl ester which is mainly used as an antioxidant of various synthetic resins, such as polyethylene, polypropylene, polyvinyl chloride, ABS resin, polyester and the like. The antioxidant has prominent effects on preventing oxidation, improving color and luster and the like; the antioxidant has high thermal stability, weathering resistance and hydrolysis resistance stability, so the processing stability is good. Due to the dipentaerythritol structure and the characteristic of high molecular weight, the product is quite suitable for application of polymeric materials requiring high temperature processing; due to containing of a triphosphite structure, the content of alkyl trivalentphosphorus is high, and thus the antioxidant effect is more prominent and highly efficient. The product does not contain alkyl phenol in structure and is safe and non-toxic. The product is mainly suitable for production processing of ABS, PS, HIPS, NBR, SBS, PP, PE, LLDPE, PVC, PC, PA, PET, UP, amide fibers, polyester fibers, adhesives, paints, inks and compound auxiliary agents and compounding of calcium and zinc stabilizers.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and specifically refers to an antioxidant containing organic phosphite-dipentaerythritol triphosphite fatty alcohol ester and a synthesis method thereof. Background technique [0002] Phosphite antioxidants are a fast-growing category of antioxidants. The annual growth rate of global antioxidants is about 5%, while the annual growth rate of phosphite antioxidants has reached more than 7%. The development speed is in the leading position among the whole antioxidant species. Due to the rapid growth of plastic production capacity and output, the growth of production and consumption of antioxidants has been stimulated and stimulated, and the growth rate of domestic antioxidants is currently maintained at a growth rate of 10%. Domestic phosphite antioxidants have received more and more attention, but most of the existing phosphite antioxidants are hindered phenols, bisphenols and phosphite ant...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/141C07F9/142C08K5/524D01F1/10D01F6/92C09J11/06C09D7/40C09D11/03
CPCC07F9/1411C07F9/142C08K5/524C09D11/03C09J11/06D01F1/10D01F6/92
Inventor 李熊伟李建成
Owner 浙江锦润生物科技有限公司