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Preparation method of environment-friendly plasticizer

An environmentally friendly plasticizer and catalyst technology, applied in the production of bulk chemicals, etc., can solve the problems of high cost of polyester plasticizer, general plasticizing effect, thermal degradation of decarboxylation, etc., and achieves low equipment requirements, easy to promote, increase Compatibility effect

Active Publication Date: 2019-06-21
QINGDAO UNIV OF SCI & TECH
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Problems solved by technology

[0005] At present, there are some vegetable oil-based ester plasticizers synthesized by grafting esters and vegetable oils. The plasticizing effect is average, and there are some problems in the synthesis: the production of vegetable oil-based plasticizers at home and abroad is generally divided into two steps. , first synthesize the ester plasticizer, and then graft the ester plasticizer to epoxy vegetable oil through epoxy ring-opening
The temperature of polyester synthesized by direct esterification method and transesterification method often exceeds 200°C in the later stage of the reaction, and side reactions such as decarboxylation and thermal degradation will occur, which will affect the reaction and generate by-products
Moreover, polyester plasticizers are relatively expensive and rarely used alone, and their plasticizing effects need to be improved

Method used

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preparation example Construction

[0032] As introduced in the background technology, the current vegetable oil-based ester plasticizers have general plasticizing effects, complex synthesis methods, and many side reactions. Therefore, the present invention proposes a kind of environment-friendly plasticizer and preparation method thereof, and its synthetic route is as follows figure 1 As shown, the specific steps are as follows:

[0033](1) Take 10g of airgel and place it in a flask, then measure 10g of ethanol to fully dissolve 5g of stannous chloride, soak the airgel for 6 hours under ultrasonic vibration conditions, and heat to 100°C to obtain airgel-supported chloride Sn catalyst;

[0034] (2) Add epoxidized soybean oil, succinic acid, hexanediol, and 3-chloro-1,2-propanediol to the reactor in a molar ratio of 1:10:7.9:2.6, and then add 70 parts of N-hexyl Pyridine hexafluorophosphate was used as solvent, and 3 parts of stannous chloride catalysts adsorbed by airgel were added, and stirred and mixed;

[...

Embodiment 1

[0041] Under the condition of nitrogen protection, epoxidized soybean oil, succinic acid, hexanediol, and 3-chloro-1,2-propanediol were added to the reactor according to the molar ratio of 1:10:7.9:2.6, and then 70 parts The ionic liquid was used as a solvent, 3 parts of stannous chloride catalyst adsorbed by airgel were added, the temperature was controlled at 160° C., and the airgel catalyst was filtered out after 4 hours. Control the temperature at 180° C. and react for another 3 hours to obtain epoxy soybean oil-based polyhexamethylene succinate 3 chloride 1,2 propylene glycol plasticizer (I). Add 40 parts of this plasticizer and 3 parts of calcium zinc heat stabilizer to 100 parts of PVC to make PVC splines.

Embodiment 2

[0043] Under the conditions of Example 1, 3-chloro 1,2 propanediol was replaced by 1,2 propanediol. The epoxy soybean oil-based polyhexamethylene succinate 1,2-propylene glycol plasticizer was obtained. Add 40 parts of this plasticizer and 3 parts of calcium zinc heat stabilizer to 100 parts of PVC to make PVC splines.

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Abstract

The invention relates to a preparation method of an environment-friendly plasticizer. The method comprises the following steps: epoxidized soybean oil, succinic acid, hexanediol and 3-chloro-1,2-propanediol are dissolved in an ionic liquid system having solvent and catalyst functions, a reaction is performed in presence of an aerogel catalyst, after the reaction, the aerogel catalyst is removed byfiltering, a solvent is removed, and a product, namely, the environment-friendly plasticizer is collected, wherein the aerogel catalyst adopts aerogel particles containing a stannous chloride catalyst. According to the synthesis method of the epoxidized soybean oil based polyester plasticizer, the epoxidized soybean oil and a polyester plasticizer are combined by the reaction of epoxy groups andcarboxyl groups, synthesis cost of the plasticizer is reduced, compatibility of the plasticizer with PVC is improved, plastification efficiency is increased, and the plasticizer has excellent durability.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis, in particular to a method for synthesizing epoxy soybean oil-based polyester with high plasticizing efficiency. Background technique [0002] Polyvinyl chloride (PVC) is one of the most widely used resin materials at present. It is cheap and widely used in various aspects such as life and transportation. Plasticizer, as a large amount of additives in PVC, plays an important role in improving the application performance of PVC. At present, there are more than 1,000 kinds of plasticizers that have been commercialized at home and abroad, and the main varieties are phthalate plasticizers, especially the production and consumption of dioctyl phthalate (DOP). Although this type of monomeric plasticizer has high plasticizing efficiency, its relative molecular weight is small, and its compatibility with materials is poor. It is easy to be extracted by organic solvents during application, and it...

Claims

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Application Information

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IPC IPC(8): C08G63/682C08G63/16C08L27/06C08L67/02
CPCY02P20/54
Inventor 高传慧王汇淄刘月涛张迪陈颖王传兴武玉民
Owner QINGDAO UNIV OF SCI & TECH