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Method for preparing plasticizer

A technology of plasticizer and end-capping agent, applied in the field of plasticizer preparation, can solve the problems of softening and sticking of polymer, loss of plasticizer effect, reduction of polymer performance, etc., and achieves good plasticizing and toughening effect, Improves extraction resistance and reduces volatilization

Active Publication Date: 2012-10-17
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the poor binding ability of small-molecule plasticizers to polymers and strong migration, small-molecule plasticizers tend to migrate to the surface of polymers as time goes by, making polymers soften and sticky or even brittle on the surface, losing The original role of the plasticizer; at the same time, the small molecule plasticizer will also be partially volatilized during the processing of the polymer, resulting in a decrease in the performance of the polymer

Method used

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preparation example Construction

[0023] The invention provides a method for preparing a plasticizer, comprising the following steps: A) heating nylon acid, diol and end-capping agent to 120°C to 200°C in a protective atmosphere to react to obtain an intermediate product. B) reacting the intermediate product at 180° C. to 260° C. and 5 Pa to 200 Pa to obtain a plasticizer.

[0024] Wherein, the step A is the esterification reaction of nylon acid and glycol, specifically: in a protective atmosphere, the temperature of nylon acid, glycol and end-capping agent is raised to 120°C~200°C, preferably 140°C~180°C , to obtain intermediate products. The protective atmosphere is a protective gas well known to those skilled in the art, preferably nitrogen, helium or argon, more preferably nitrogen. The reaction temperature of step A is relatively high and needs to be carried out in a protective atmosphere, otherwise side reactions such as oxidation and carbonization will occur, resulting in an increase in impurities in t...

Embodiment 1

[0041] 1.1 Add 2500g of nylon acid with an average molecular weight of 131g / mol, 1653g of 1,2-propanediol and 125g of activated carbon into the reactor. Under the protection of nitrogen, heat up to 100°C, stir for 12 hours, and filter while hot to obtain light-colored first intermediate product.

[0042] 1.2 Add 1523g of the first intermediate product obtained in 1.1, 68g of isooctyl alcohol and 5.3g of n-tetrabutyl titanate into the reaction kettle. Under the protection of nitrogen, raise the temperature to 140°C, stir and react for 4 hours, then raise the temperature to 200°C , Polycondensation reaction was carried out at 60pa, and nylon acid polyester plasticizer was obtained after 2h, which was a light yellow transparent viscous liquid.

[0043] The nylon acid polyester plasticizer obtained in 1.2 was analyzed by gel permeation chromatography, and its weight average molecular weight was 4100, and its molecular weight distribution index was 2.3.

[0044] The nylon acid pol...

Embodiment 2

[0054] 2.1 Add 2500g of nylon acid with an average molecular weight of 131g / mol, 2306g of diethylene glycol and 125g of activated carbon into the reactor. Under the protection of nitrogen, heat up to 120°C, stir for 12 hours, and filter while hot to obtain light-colored No. an intermediate product.

[0055] 2.2 Add 1762g of the first intermediate product obtained in 2.1, 68g of isooctyl alcohol, 3.1g of antimony trioxide and 3.1g of zinc acetate into the reaction kettle, and raise the temperature to 140°C under nitrogen protection, and stir for 4 hours. Raise the temperature to 200°C, carry out the polycondensation reaction at 60 Pa, and obtain the nylon acid polyester plasticizer in the form of light yellow viscous liquid after 6 hours.

[0056] The nylon acid polyester plasticizer obtained in 2.2 was analyzed by gel permeation chromatography, and its weight average molecular weight was 19800, and its molecular weight distribution index was 2.7.

[0057] The nylon acid polye...

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Abstract

The invention provides a method for preparing a plasticizer. The method comprises the following steps: raising the temperature of nylon acid, a dihydric alcohol and an end capping agent to 120-200 DEG C for a reaction to obtain an intermediate product in a protective atmosphere; and reacting the intermediate product at 180-260 DEG C at the pressure of 5-200Pa to obtain the plasticizer. Comparing with a small molecular plasticizer in the prior art, the method provided by the invention uses an industrial byproduct nylon acid as the main raw material and takes advantages of good solubility of nylon acid in the dihydric alcohol, the production process for preparing the polyurethane plasticizer with a low acid value at the low cost is shortened through two reactions including esterification and polycondensation. Firstly, the plasticizer has a good plastication; secondly, the plasticizer is a high molecular polyurethane plasticizer so that plasticizer volatilization is reduced in the processing process; moreover, interactions among polyurethane macromolecular chains and a polymer are greater than those among the small molecular plasticizers and a polymer, and the plasticizer provided by the invention has good migration resistance and extraction resistance.

Description

technical field [0001] The invention belongs to the technical field of additives, in particular to a preparation method of a plasticizer. Background technique [0002] Plasticizers have thermal stability and chemical reagent stability, and can be compatible with polymers within a certain range to increase the plasticity and flexibility of polymers. Plasticizers mainly increase the mobility of the polymer molecular chain and reduce the crystallinity by weakening the van der Waals force of the secondary bond between the polymer molecules, thereby increasing the plasticity of the polymer. Traditional plastic plasticizers are o-phthalic plasticizers, such as dioctyl phthalate (DOP) and diisodecyl phthalate (DIDP), but they belong to small molecule plasticizers and are weather-resistant Poorly resistant, it will migrate to the surface of plastic products after long-term use, resulting in a decrease in the performance of the product, and o-benzene plasticizers will cause harm to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/20C08G63/672C08L67/04C08L69/00C08L27/06C08L67/02
Inventor 张贵宝董丽松李悦生刘三荣张会良边俊甲
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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