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Preparation method of plasticizer triethylene glycol di-2-ethylhexoate

A technology of triethylene glycol and isooctanoate, which is applied in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problem of low content and yield of triethylene glycol diisooctanoate. and other problems, to achieve the effect of reducing product yield, improving ester content and yield, and simple operation

Active Publication Date: 2015-02-25
江苏明魁高分子材料技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the invention is to solve the problem of low ester content and yield of triethylene glycol diisocaprylate in the prior art, and provide a kind of preparation method of plasticizer triethylene glycol diisocaprylate

Method used

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  • Preparation method of plasticizer triethylene glycol di-2-ethylhexoate

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Experimental program
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Effect test

Embodiment 1

[0025] Weigh 100g triethylene glycol, 220g isooctanoic acid, 1.22g gac, 0.58gN,N-dimethylformamide, 0.32g zirconium hydrogen phosphate (crystalline zirconium hydrogen phosphate [α-Zr(HPO 4 ) 2 ·H 2 [0], the same below) and 0.32g of tetraisopropyl titanate were added to a three-neck flask (800ml) equipped with a thermometer, a water separator and a reflux condenser, stirred and heated to reflux, and heated to 205°C for esterification reaction for 10 hours Finally, no water belt was observed in the water separator, and the esterification reaction was completed, and unreacted excess isooctanoic acid was recovered by distillation. The reaction solution of the esterification reaction is filtered to obtain the crude triethylene glycol diisocaprylate liquid, and the crude triethylene glycol diisocaprylate liquid is neutralized and washed until the acid value of the crude product is lower than 0.1mgKOH g -1 . The crude triethylene glycol diisocaprylate washed with neutralization wa...

Embodiment 2

[0027] Weigh 100g of triethylene glycol, 240g of isooctanoic acid, 1.36g of activated carbon, 0.68g of N,N-dimethylformamide, 0.85g of zirconium hydrogen phosphate and 0.41g of tetraisopropyl titanate, add a thermometer and water separator In a three-necked flask (800ml) with a reflux condenser, stir and heat to reflux, and heat up to 215°C for esterification for 8 hours. After 8 hours of esterification, no water bands are observed in the water separator. bitter. The reaction solution of the esterification reaction is filtered to obtain the crude triethylene glycol diisocaprylate liquid, and the crude triethylene glycol diisocaprylate liquid is neutralized and washed until the acid value of the crude product is lower than 0.1mgKOH g -1 . The crude triethylene glycol diisocaprylate washed with neutralization water was dehydrated at a vacuum degree of 5 kPa and a temperature of 120° C. for 2 hours to obtain 221.69 g of a crude triethylene glycol diisocaprylate. Add 0.22g of ac...

Embodiment 3

[0029] Weigh 100g of triethylene glycol, 260g of isooctanoic acid, 1.62g of activated carbon, 0.82g of N,N-dimethylformamide, 1.44g of zirconium hydrogen phosphate and 0.57g of tetraisopropyl titanate, add a thermometer, water separator and In the three-necked flask (800ml) of the reflux condenser, stir and heat to reflux, and raise the temperature to 220°C for 5 hours of esterification reaction. bitter. The reaction solution of the esterification reaction is filtered to obtain the crude triethylene glycol diisocaprylate liquid, and the crude triethylene glycol diisocaprylate liquid is neutralized and washed until the acid value of the crude product is lower than 0.1mgKOH g -1 . The crude triethylene glycol diisocaprylate washed with neutralized water was dehydrated at a vacuum degree of 5 kPa and a temperature of 120° C. for 2 hours to obtain 233.32 g of a crude triethylene glycol diisocaprylate. Add 0.23g of activated carbon to the dehydrated crude triethylene glycol diiso...

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Abstract

The invention discloses a preparation method of plasticizer triethylene glycol di-2-ethylhexoate. The preparation method comprises the following steps of: blending, esterification reaction, filtration, neutralization washing, dehydration and decoloration and particularly comprises the following steps of: weighing triethylene glycol and ethylhexanoic acid as raw materials, adding active carbon, N,N-dimethyl formamide and a catalyst, heating to 200-230 DEG C, and carrying out the esterification reaction for 3-10 hours; filtering reaction liquid of the esterification reaction to obtain a crude triethylene glycol di-2-ethylhexoate liquid product, and carrying out the neutralization washing on the crude triethylene glycol di-2-ethylhexoate liquid product; carrying out vacuum decompression dehydration on the crude triethylene glycol di-2-ethylhexoate liquid product subjected to the neutralization washing; carrying out the decoloration on the crude triethylene glycol di-2-ethylhexoate liquid product subjected to dehydration treatment to obtain a finished triethylene glycol di-2-ethylhexoate product. The preparation method disclosed by the invention is simple to operate, can be used for increasing the ester content and yield of triethylene glycol di-2-ethylhexoate, can at least achieve the ester content by 98%, and can be used for increasing the yield more than 70% and reducing the cost by 20% through the increase of the product yield.

Description

technical field [0001] The invention relates to a preparation method of a resin plasticizer, in particular to a preparation method of the plasticizer triethylene glycol diisocaprylate. Background technique [0002] Triethylene glycol diisocaprylate (3GO) is a solvent-based cold-resistant plasticizer, which has excellent low temperature resistance, durability, oil resistance, ultraviolet radiation resistance and antistatic properties, and has low viscosity and certain lubricity. The polarity close to the resin makes it compatible with many natural resins and synthetic rubbers. It is widely used in PVB security films, synthetic rubbers, vinyl resins, PVC, industrial coatings, sealing materials and other fields. In recent years, due to the improvement of the quality requirements of plasticizers in the PVB safety film, synthetic rubber and other material markets, the demand for triethylene glycol diisocaprylate has gradually increased. In 2013, the domestic consumption of 3GO wa...

Claims

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Application Information

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IPC IPC(8): C07C69/28C07C67/08
CPCC07C67/08C07C67/56C07C67/60C07C69/28
Inventor 蒋继明徐奎
Owner 江苏明魁高分子材料技术有限公司
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