Phosphorous acid containing organic ester anti-oxidant and synthetic method

Abstract

The invention provides a novel phosphorus-containing anti-oxidant-3-distearate pentaerythritol diphosphite. The product is mainly used as an auxiliary anti-oxidant for polyethylene, polypropylene, polyvinyl chloride, ABS resin, polyester and other various synthetic resins. The product has protruding effects for preventing oxidation, improving color and the like; the product has higher heat stability, weather resistance, hydrolysis resistance stability, and good processing stability. The product has a pentaerythritol structure and a high molecular weight characteristic, has functions for lubrication, plasticizing and stabilization, and the product is widely applied to polymeric materials which require high temperature processing. The structure of the product does not have alkylphenol, the product is safe and nontoxic, and the product accords with newest market regulations and development trend. The product can be applied to packaging materials for foodstuff (TITLE 21 CFR.178.2010). Theproduct is mainly suitable for production and processing of auxiliary agents for compounding ABS, PS, HIPS, NBR, SBS, PP, PE, LLDPE, PVC, PC, PA, PET, UP, amide fiber, polyester fiber, an adhesive, paint, and printing ink; and compounding a calcium zinc stabilizing agent.

Description

technical field

[0001] The invention belongs to the technical field of fine chemical industry, and specifically refers to a kind of antioxidant-tri-disstearic acid pentaerythritol diphosphite containing phosphorous acid organic ester and a synthesis method thereof. Background technique

[0002] Phosphite antioxidants are a fast-growing category of antioxidant products. The annual growth rate of global antioxidants is 5%, while the annual growth rate of phosphite antioxidants has reached more than 7%. Speed ​​has a leading position in the whole antioxidant. 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 antio...

Examples

example 1

[0027] In a reaction flask equipped with electric stirring, electric heating, reflux condenser, and temperature measuring system, 67 grams of pentaerythritol, 279 grams of stearic acid, and 1 gram of catalyst stannous chloride were added to the reaction flask respectively, and protected under vacuum conditions. The esterification reaction was carried out at 150-220°C, and the reaction time was 150 minutes. After the reaction was completed, it was cooled to below 100°C, 54 grams of triethyl phosphite was added, and 2 grams of catalyst phosphoric acid was added, and the second reaction was carried out under the protection of nitrogen. Step-by-step reaction, control the reaction temperature at 140-200°C, and the reaction time is 150 minutes. After the reaction is completed, cool to below 100°C. The product is filtered through a constant temperature oven at about 80°C to obtain the product of organic phosphite antioxidant—tri-distearin Acid pentaerythritol diphosphite.

example 2

[0029] In a reaction flask equipped with electric stirring, electric heating, reflux condenser, and temperature measuring system, 50 grams of pentaerythritol, 209 grams of stearic acid, and 1.3 grams of catalyst phosphoric acid were added to the reaction flask respectively, and esterification was carried out under nitrogen protection. Reaction, control the reaction temperature at 130-220°C, and the reaction time is 180 minutes. After the reaction is completed, cool to below 100°C, then add 41 grams of triethyl phosphite, add 0.5 grams of catalyst phosphoric acid, and carry out the second step reaction under the protection of nitrogen. Control the reaction temperature at 140-200°C, and the reaction time is 150 minutes. After the reaction is completed, cool to below 100°C. The product is then filtered in a constant temperature oven at about 80°C to obtain the organic phosphite antioxidant product—pentaerythritol di-tri-distearate Phosphite.

example 3

[0031] In a reaction flask equipped with electric stirring, electric heating, reflux condenser, and temperature measuring system, 136 grams of pentaerythritol and 270 grams of palmitic acid were added to the reaction flask, and 3.4 grams of catalyst isopropyl titanate were carried out under nitrogen protection. For esterification reaction, control the reaction temperature at 170-220°C, and the reaction time is 180 minutes. After the reaction is completed, cool to below 100°C, add 58 grams of triethyl phosphite, and add 1 gram of catalyst isopropyl titanate, under the protection of nitrogen Carry out the second step of reaction, control the reaction temperature at 150-210°C, and the reaction time is 180 minutes. After the reaction is completed, cool down to below 100°C. The product is filtered through a constant temperature oven at about 80°C to obtain the product of organic phosphite antioxidant—three- Pentaerythritol Diphosphite Dipalmitate.

technical field

[0001] The invention belongs to the technical field of fine chemical industry, and specifically refers to a kind of antioxidant-tri-disstearic acid pentaerythritol diphosphite containing phosphorous acid organic ester and a synthesis method thereof. Background technique

[0002] Phosphite antioxidants are a fast-growing category of antioxidant products. The annual growth rate of global antioxidants is 5%, while the annual growth rate of phosphite antioxidants has reached more than 7%. Speed ​​has a leading position in the whole antioxidant. 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 antio...

Examples

example 1

[0027] In a reaction flask equipped with electric stirring, electric heating, reflux condenser, and temperature measuring system, 67 grams of pentaerythritol, 279 grams of stearic acid, and 1 gram of catalyst stannous chloride were added to the reaction flask respectively, and protected under vacuum conditions. The esterification reaction was carried out at 150-220°C, and the reaction time was 150 minutes. After the reaction was completed, it was cooled to below 100°C, 54 grams of triethyl phosphite was added, and 2 grams of catalyst phosphoric acid was added, and the second reaction was carried out under the protection of nitrogen. Step-by-step reaction, control the reaction temperature at 140-200°C, and the reaction time is 150 minutes. After the reaction is completed, cool to below 100°C. The product is filtered through a constant temperature oven at about 80°C to obtain the product of organic phosphite antioxidant—tri-distearin Acid pentaerythritol diphosphite.

example 2

[0029] In a reaction flask equipped with electric stirring, electric heating, reflux condenser, and temperature measuring system, 50 grams of pentaerythritol, 209 grams of stearic acid, and 1.3 grams of catalyst phosphoric acid were added to the reaction flask respectively, and esterification was carried out under nitrogen protection. Reaction, control the reaction temperature at 130-220°C, and the reaction time is 180 minutes. After the reaction is completed, cool to below 100°C, then add 41 grams of triethyl phosphite, add 0.5 grams of catalyst phosphoric acid, and carry out the second step reaction under the protection of nitrogen. Control the reaction temperature at 140-200°C, and the reaction time is 150 minutes. After the reaction is completed, cool to below 100°C. The product is then filtered in a constant temperature oven at about 80°C to obtain the organic phosphite antioxidant product—pentaerythritol di-tri-distearate Phosphite.

example 3

[0031] In a reaction flask equipped with electric stirring, electric heating, reflux condenser, and temperature measuring system, 136 grams of pentaerythritol and 270 grams of palmitic acid were added to the reaction flask, and 3.4 grams of catalyst isopropyl titanate were carried out under nitrogen protection. For esterification reaction, control the reaction temperature at 170-220°C, and the reaction time is 180 minutes. After the reaction is completed, cool to below 100°C, add 58 grams of triethyl phosphite, and add 1 gram of catalyst isopropyl titanate, under the protection of nitrogen Carry out the second step of reaction, control the reaction temperature at 150-210°C, and the reaction time is 180 minutes. After the reaction is completed, cool down to below 100°C. The product is filtered through a constant temperature oven at about 80°C to obtain the product of organic phosphite antioxidant—three- Pentaerythritol Diphosphite Dipalmitate.

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