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Production method of environment-friendly polyester plasticizer

The technology of a polyester plasticizer and a production method is applied in the field of synthesizing phthalic anhydride diol polyester with tetra-n-butyl titanate as a catalyst, and can solve the problems of pollution, complicated process flow, poor product quality and the like, Achieve the effect of low product pollution, high product purity and high quality

Inactive Publication Date: 2015-03-11
郑建东
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional production process of uniform plasticizer has the disadvantages of serious pollution, complicated process, poor product quality (color up to 200#), and most of them use acidic catalysts.

Method used

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  • Production method of environment-friendly polyester plasticizer
  • Production method of environment-friendly polyester plasticizer
  • Production method of environment-friendly polyester plasticizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Poly-1,2-propylene glycol phthalate production method comprises the steps:

[0023] Add 1 mol (148.1 g) of phthalic anhydride, 85 ml (87.5 g) of 1,2 propylene glycol, and 2- Ethylhexanol 102ml (85g), add 1.2g tetra-n-butyl titanate as an esterification catalyst, pass high-purity nitrogen gas, stir and heat, when the temperature reaches 180-230°C, the reaction temperature is controlled at about 220°C, the reaction The time is 6 to 8 hours. When the reaction acid value is less than 10 mg KOH / g, the esterification reaction ends and the dealcoholization refining process is carried out. Atmospheric pressure dealcoholization is carried out first, the temperature is controlled at 140-190°C, and then vacuum distillation is carried out, the vacuum degree is controlled above 0.098Mpa, and the dealcoholization time is 2-3 hours. Take a sample to measure the acid value. When the acid value is 2mgKOH / When it is less than g, the dealcoholization refining process is finished, and th...

Embodiment 2

[0026] A kind of poly-1,3-butylene phthalate production method, comprises the steps:

[0027] Add 1.2mol (177.8g) of phthalic anhydride and 124ml (124.4g) of 1,3-butanediol into a 500ml glass four-necked flask equipped with a stirrer, a water separator, a spherical condenser and a thermometer. Terminal agent 2-ethylhexanol 122ml (102g), add 1.5g tetra-n-butyl titanate as an esterification catalyst, pass high-purity nitrogen, stir and heat, when the temperature reaches 180-230°C, the reaction temperature is controlled at 230°C ℃, the reaction time is 7-8 hours, when the reaction acid value is less than 10mg KOH / g, the esterification reaction is over, and the dealcoholization refining process is carried out. Atmospheric pressure dealcoholization is carried out first, the temperature is controlled at 160-200°C, and then vacuum distillation is carried out, the vacuum degree is controlled above 0.098Mpa, and the dealcoholization time is 3 hours. Take a sample to measure the acid va...

Embodiment 3

[0030] A kind of poly-1,4-butylene phthalate production method, comprises the steps:

[0031] Add 1.5mol (222.2g) of phthalic anhydride and 153ml (155.5g) of 1,4-butanediol into a 500ml glass four-necked flask equipped with a stirrer, a water separator, a spherical condenser and a thermometer. Terminal agent 2-ethylhexanol 153ml (128g), add 1.8g tetra-n-butyl titanate as an esterification catalyst, pass high-purity nitrogen, stir and heat, when the temperature reaches 180-230°C, the reaction temperature is controlled at 230°C ℃, the reaction time is 7-8 hours, when the reaction acid value is less than 10mg KOH / g, the esterification reaction is over, and the dealcoholization refining process is carried out. Atmospheric pressure dealcoholization is carried out first, the temperature is controlled at 180-210°C, and then vacuum distillation is carried out, the vacuum degree is controlled above 0.098Mpa, and the dealcoholization time is 3 hours. Take a sample to measure the acid va...

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Abstract

The invention discloses a catalytic synthesis method of an environment-friendly polyester plasticizer. The method comprises the following specific steps: adding dihydric alcohol and phthalic anhydride to a reactor according to a molar ratio of 1.1:1 to 1.2:1, adding an end-capping reagent 2-ethyl hexanol with a molar ratio to phthalic anhydride of 0.5:1 to 0.9:1, then adding a catalyst tetra-n-butyl titanate which accounts for 0.5-1% of the mass of phthalic anhydride, feeding high purity nitrogen, stirring and gradually raising the temperature to 180-230 DEG C, carrying out a reaction for 6-8 hours in a heat preservation manner under the condition that the acid value of the reaction solution is lower than 10 mg KOH*g<-1>, ending the reaction, and cooling to obtain the phthalic acid polyester plasticizer. The method disclosed by the invention adopts a little of catalyst during the process to improve the conversion efficiency and reduce the energy consumption; the obtained product is basically pale yellow, and has the special advantages of low toxicity and solvent extraction resistance; the whole process is low in pollution; the product is good in quality and high in purity.

Description

technical field [0001] The invention relates to a production method of phthalic anhydride diol polyester, in particular to a production method in which tetra-n-butyl titanate is used as a catalyst to synthesize phthalic anhydride diol polyester. Background technique [0002] Plasticizer is an ester substance that is added to high polymers (such as rubber, plastics, coatings, etc.) to increase their plasticity and flow properties during processing and to make the finished product flexible. [0003] Phthalic anhydride diol polyester is an environmentally friendly special plasticizer with excellent performance. Due to the difference in molecular structure, it has high volume resistance, narrow relative molecular mass distribution, low volatility, and can be compatible with PVC wires. The sheath and the filler in the formula are completely wetted, have a high flash point, and are non-flammable. The low-temperature flexibility and high-temperature resistance of the plasticized po...

Claims

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Application Information

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IPC IPC(8): C08G63/181C08G63/85C07C67/08C07C69/80
Inventor 郑建东候金松李永红
Owner 郑建东
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