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Preparation method of novel environment-friendly phosphite ester antioxidant

A technology of phosphite and liquid phosphite, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of rising prices of nonylphenol and antioxidant TNPP High performance, high purity and other issues such as the coloring environment of downstream products and human hazards

Inactive Publication Date: 2012-10-10
NANXIONG ZHIYI FINE CHEM
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  • Claims
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Problems solved by technology

The antioxidant tris(nonylphenol) phosphite (TNPP) is one of the most widely used, but the price of the antioxidant TNPP remains high due to the continuous increase in the price of the raw material nonylphenol. In addition, other The remaining nonylphenol and chloride ions in the system will cause coloring of downstream products and harm the environment and human body. Therefore, it is urgent to develop a cheap and environmentally friendly liquid phosphite antioxidant that can replace the antioxidant TNPP

Method used

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  • Preparation method of novel environment-friendly phosphite ester antioxidant
  • Preparation method of novel environment-friendly phosphite ester antioxidant
  • Preparation method of novel environment-friendly phosphite ester antioxidant

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preparation example Construction

[0019] The preparation method of the above-mentioned novel environment-friendly phosphite antioxidant, its process step is: in the four-necked bottle that is equipped with reflux condenser, thermometer, dropping funnel and nitrogen conduit, press raw material cardanol or hydrogenated cardanol and trichloro Add cardanol or hydrogenated cardanol at the molar ratio of phosphorous chloride, pass N 2 or CO 2 Protected by inert gas, stir and heat up to 55-70°C, add phosphorus trichloride dropwise, dropwise for 1.5-2 hours, keep warm for 1-3 hours, slowly heat up to 120-130°C, and heat up for 0.5-1 hour , keep warm for 1-5 hours, heat up to 140-150°C, keep warm for 1-5 hours, distill under reduced pressure to remove low boiling point substances, cool down to 100-120°C, add amine high-efficiency adsorption resin, stir for 0.5-3 hours, remove Unreacted free phenol and Cl - , filter and recover the adsorption resin, regenerate it with alkaline water, and recycle it to obtain a new typ...

Embodiment 1

[0027] Add 566 grams of cardanol in the 1000 milliliter four-necked bottle, pass N 2 protection, stirred and heated to 55 ° C, slowly added dropwise 82 grams of PCl 3 , the dropping time is 1.5 to 2 hours, keep warm for 1 hour, slowly heat up to 120 °C, heat up for 1 hour, keep warm for 1 hour, continue to heat up to 140 °C, keep warm for 2 hours, remove low boiling point substances by distillation under reduced pressure, and obtain yellow 540 grams of liquid crude product, gas chromatography records its content greater than 94%, free phenol content is about 5%; ion chromatography records Cl - The content is 0.1%.

Embodiment 2

[0029] The crude product of embodiment 1 gained is in N 2 Protect and heat up to 110°C, add 25 grams of amine high-efficiency adsorption resin, stir for 1 hour, and obtain a low-phenol and low-chlorine light yellow product after filtration. The content of the product is greater than 99.5% by gas chromatography, and the content of free phenol is less than 0.05%; measured by ion chromatography Cl - The content is 0.0002%. ZHIYI-8 amine high-efficiency adsorption resin is washed with 30% sodium hydroxide aqueous solution to regenerate it and recover free phenol.

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Abstract

The invention relates to a novel environment-friendly phosphite ester antioxidant, wherein a preparation of the novel environment-friendly phosphite ester antioxidant comprises the following steps of: taking cashew nut shell oil extractive such as anacardol or hydrogenated cashew phenol and phosphorus trichloride as raw materials, and reacting according to the molar ratio of the anacardol or the hydrogenated cashew phenol to the phosphorus trichloride of (3.0:1.0)-(3.5:1.0) to prepare a liquid phosphite ester antioxidant product without a solvent and a catalyst. The preparation method is simple in technology, the raw materials are low in price and easy to obtain, the antioxidant tris-(nonyl phenol) phosphite ester (TNPP) can be replaced by the synthesized product to be taken as the antioxidant and the stabilizing agent in the fields such as nature rubber, synthetic rubber, emulsion, plastic and the like, so that the phosphite ester antioxidant not only is better in emulsification performance, hydrolysis resistance and thermal stability performance compared with the TNPP, but also has the characteristics of being low in price and environment-friendly, thereby according with the future development tendency of the antioxidant, and the antioxidant which is synthesized by taking the anacardol as the raw material is the reaction type antioxidant having double bonds.

Description

technical field [0001] The invention belongs to the technical field of phosphite antioxidants and preparation thereof, and relates to a preparation method of a novel environment-friendly phosphite antioxidant. Background technique [0002] Phosphite antioxidants, as hydroperoxide decomposers and free radical scavengers, are widely used in rubber industry, plastics industry and other fields. They can effectively inhibit the oxidation and discoloration of polymer materials, and can be used together with phenolic antioxidants. It produces excellent synergistic effect, and it is the most rapidly developed type of antioxidant in recent years. The antioxidant tris(nonylphenol) phosphite (TNPP) is one of the most widely used, but the price of the antioxidant TNPP remains high due to the continuous increase in the price of the raw material nonylphenol. In addition, other The residual nonylphenol and chloride ions in the system will cause coloring of downstream products and harm the...

Claims

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Application Information

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IPC IPC(8): C07F9/145C08K5/526
Inventor 刘少平解西京王峰
Owner NANXIONG ZHIYI FINE CHEM
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