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Preparation method of rare earth heat stabilizer used for PVC

A rare earth thermal stabilizer and the technology of preparation steps, applied in the field of plastic additives, can solve the problems of poor thermal stability, poor compatibility, low dosage, etc., achieve long-term stability improvement, overcome high toxicity, low cost and environmental friendliness. Effect

Inactive Publication Date: 2017-07-25
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention: aiming at the disadvantages that inorganic rare earths have poor initial thermal stability to PVC, poor compatibility with PVC, and relatively serious coloring property, a kind of hydroxy acid and carboxyl group undergoes amination reaction, and then Oxidation of hydroxyl groups into carboxyl groups to obtain substances containing amino groups and carboxyl groups, and then reacting with rare earth salts to obtain organic rare earths, and then supplementing with thermal stability additives to prepare rare earth heat stabilizers for PVC. The present invention first uses 3-hydroxypropyl The acid is used as the raw material, and the hydroxyl group is protected by trimethylchlorosilane, and then reacted with thionyl chloride to form an acid chloride, and then reacted with glutamic acid to form an amine substance, and then oxidized to obtain a substance containing an amine group and a carboxyl group. After saponification, it reacts with inorganic rare earth salts to generate organic rare earths, and the amine groups can neutralize the generated HCl to prevent automatic oxidation. Finally, it is mixed and dried with thermal stability additives to obtain rare earth thermal stabilizers for PVC. Rare earth heat stabilizers for PVC can not only overcome the shortcomings of existing heat stabilizers such as high toxicity and slow initial thermal stability, but also improve the long-term stability and initial coloring of PVC, non-toxic and environmentally friendly, low energy consumption, Less consumption, low price, and broad industrial application prospects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0017] Weigh 25g of 3-hydroxypropionic acid and add it to a three-neck flask equipped with a thermometer and a reflux device, place the flask in an ice-water bath, control the temperature at 0°C, add 100mL of absolute ethanol and 3mL of triethylamine into the flask, stir and mix After 10 minutes, add 5g of trimethylchlorosilane to the flask, stir for 40 minutes, then raise the temperature to 60°C, add 15mL of thionyl chloride and 1mL of N,N-dimethylformamide into the flask, and continue to stir for 2h After the above reaction is finished, adding mass fraction in the flask is 5% sodium hydroxide to adjust the pH to be 7.2, then add 30g of glutamic acid in the flask, continue to stir and react for 1h, after the reaction ends, stop heating, and then add 3g of periodic acid, stirred and reacted for 40min to obtain the product, the product was placed in a rotary evaporator, and rotatably concentrated to 1 / 3 of the original volume of the product to obtain a concentrated solution for ...

example 2

[0020] Weigh 30g of 3-hydroxypropionic acid and add it into a three-necked flask with a thermometer and a reflux device, place the flask in an ice-water bath, control the temperature at 5°C, add 200mL of absolute ethanol and 5mL of triethylamine into the flask, stir and mix After 15 minutes, add 8g of trimethylchlorosilane to the flask, stir for 50 minutes, then raise the temperature to 70°C, add 20mL of thionyl chloride and 3mL of N,N-dimethylformamide into the flask, and continue to stir for 3h After the above reaction is finished, adding mass fraction in the flask is 5% sodium hydroxide to adjust the pH to be 7.5, then add 40g of glutamic acid in the flask, continue to stir and react for 2h, after the reaction ends, stop heating, and then add 5g of periodic acid, stirred and reacted for 50min to obtain the product, the product was placed in a rotary evaporator, and rotatably concentrated to 1 / 3 of the original volume of the product to obtain a concentrated solution for subse...

example 3

[0023] Weigh 28g of 3-hydroxypropionic acid into a three-necked flask with a thermometer and a reflux device, place the flask in an ice-water bath, control the temperature at 3°C, add 150mL of absolute ethanol and 4mL of triethylamine into the flask, stir and mix After 13 minutes, add 7 g of trimethylchlorosilane to the flask, stir and react for 45 minutes, then raise the temperature to 65°C, add 18 mL of thionyl chloride and 2 mL of N,N-dimethylformamide into the flask, and continue to stir for 2.5 minutes. h; when the above reaction is finished, add 5% sodium hydroxide to the flask to adjust the pH to 7.4, then add 35g of glutamic acid to the flask, continue to stir and react for 1.5h, after the reaction is over, stop heating, and then add Add 4g of periodic acid to the mixture, stir and react for 45 minutes to obtain the product, put the product in a rotary evaporator, and concentrate it to 1 / 3 of the original volume of the product to obtain a concentrated solution, which is...

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Abstract

The invention discloses a preparation method of a rare earth heat stabilizer used for PVC, and belongs to the technical field of plastic assistants. The preparation method comprises the following steps: protecting the hydroxyl group of 3-hydroxypropionic acid used as a raw material with trimethylchlorosilane, reacting the hydroxyl group protected 3-hydroxypropionic acid with thionyl chloride to generate acyl chloride, reacting the acyl chloride with glutamic acid to generate an amine substance, oxidizing the amine substsance to obtain a substance containing an amino group and a carboxyl group, saponifying the substance containing an amino group and a carboxyl group, reacting the saponified substance with an inorganic rare earth salt to generate organic rare earth with generated HCl neutralized by the amino group in order to prevent automatic oxidation, mixing the organic rare earth with a heat stabilization assistant, and drying the obtained mixture to obtain the rare earth heat stabilizer used for PVC. The rare earth heat stabilizer used for PVC overcomes the disadvantages of large toxicity, poor initial heat stability and slow speed of existing heat stabilizers, and has the advantages of improvement of the long-term stability and the initial coloring property of the PVC, non-toxicity, environmental protection, low energy consumption, low dosage, low price and broad industrial application prospect.

Description

technical field [0001] The invention discloses a preparation method of a rare earth heat stabilizer for PVC, belonging to the technical field of plastic additives. Background technique [0002] Polyvinyl chloride (PVC) is widely used in various fields because of its excellent mechanical properties and good processing properties, as well as corrosion resistance, aging resistance, low cost, rich raw materials, and mature manufacturing technology. One of the general resins. However, there is a fatal flaw in the processing of PVC, that is, its decomposition temperature is usually lower than its processing temperature. Under a certain temperature or light, PVC is easy to decompose and release hydrogen chloride, and its thermal stability is poor. Therefore, heat stabilizers must be used in PVC processing. [0003] At present, the heat stabilizers commonly used in PVC mainly include lead salts, organotins, metal soaps and rare earths. Lead salt heat stabilizers are the earliest ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L27/06C08K13/02C08K5/17C08K5/524C08K3/26C08K5/098
CPCC08K13/02C08K3/26C08K5/098C08K5/175C08K5/524C08L27/06C08L2201/08C08L91/06
Inventor 陈兴权王维李雪晴林晨
Owner CHANGZHOU UNIV
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