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Phosphorus acid organic ester-containing antioxidant and synthetic method thereof

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 popularization 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: 2018-07-20
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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  • Phosphorus acid organic ester-containing antioxidant and synthetic method thereof
  • Phosphorus acid organic ester-containing antioxidant and synthetic method thereof
  • Phosphorus acid organic ester-containing antioxidant and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0029] Add 84 grams of dipentaerythritol, 163 grams of triethyl phosphite, and 1 gram of catalyst phosphoric acid into the reaction flask equipped with electric stirring, electric heating, reflux condenser, temperature measurement system and nitrogen flow device. , Blow in nitrogen gas to carry out the esterification reaction, control the reaction temperature at 100-180°C, the reaction time is 180 minutes, and cool to below 100°C after the reaction. Then add 253 grams of stearyl alcohol (i.e. stearyl alcohol), add 3.6 grams of tetrabutyl titanate as the catalyst, and pass in nitrogen for the second step of esterification reaction. The reaction temperature is 150-210°C and the reaction time is 180 minutes. After the reaction is over It is cooled to below 100°C, and filtered through a constant temperature oven at about 80-100°C to obtain a solid organic phosphite antioxidant product-stearyl dipentaerythritol triphosphite.

example 2

[0031] In a reaction flask equipped with electric stirring, electric heating, reflux condenser, temperature measurement system, and nitrogen flow device, put 90 grams of dipentaerythritol and 272 grams of triethyl phosphite into the reaction flask, and pass 1.8 grams of catalyst phosphoric acid into the reaction flask. The esterification reaction is carried out under nitrogen, and the reaction temperature is 100-180°C, and the reaction time is about 180 minutes. After the reaction, it is cooled to below 100°C. Then add 138 grams of octanol, add 0.7 grams of stannous chloride as a catalyst, bubbling in nitrogen for the second step of esterification reaction, the reaction temperature is 140-200°C, the reflux reaction time is 180 minutes, and after the reaction is cooled to below 100°C, Heat preservation and filtration in a constant temperature oven at around 80°C to obtain a liquid organic phosphite antioxidant product-octanol dipentaerythritol triphosphite.

example 3

[0033] In a reaction flask equipped with electric stirring, electric heating, reflux condenser, temperature measurement system and nitrogen flow device, put 81 grams of dipentaerythritol, 159 grams of triethyl phosphite, and 3 grams of catalyst phosphoric acid into the reaction flask, Enter nitrogen gas for esterification reaction, the reaction temperature is 100-180°C, and the reaction time is about 180 minutes. After the reaction, it is cooled to below 100°C. Then add 260 grams of dodecyl hydroxystearyl alcohol, blow in nitrogen for the second step of esterification reaction, control the reaction temperature to 150-200°C, the reaction time is 150 minutes, and then pull the vacuum at 200°C for 30 minutes, and cool to 100 after the reaction is over Below ℃, heat preservation and filtration in a constant temperature oven at about 100 ℃ to obtain a solid organic phosphite antioxidant product-dipentaerythritol triphosphite dodecylhydroxystearyl ester.

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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 chemical industry, and specifically refers to a fatty alcohol ester containing dipentaerythritol triphosphite, an antioxidant containing organic phosphite, and a synthesis method thereof. Background technique [0002] Phosphite antioxidants are one of the fastest growing types of antioxidants. The annual growth rate of global antioxidants is about 5%, while the annual growth rate of phosphite antioxidants is more than 7%. The development speed has a leading position in the entire antioxidant species. Due to the rapid growth of plastic production capacity and output, which stimulated and stimulated the growth of the production and consumption of antioxidants, the growth of domestic antioxidants has maintained a growth rate of 10%. Domestic phosphite antioxidants have received more and more attention, but most of the current phosphite antioxidants are hindered phenols, bisphenols and benzene-containing pho...

Claims

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Application Information

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Patent Type & Authority Applications(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
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