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Diisodecyl phthalate preparation method

A technology of diisodecyl phthalate and phthalic anhydride, which is applied in the field of plasticizer preparation, can solve complex process, low product yield, volatility, extraction resistance and migration resistance, heat aging resistance Insufficient resistance, volume resistivity, water resistance and oil resistance, etc., to achieve the effect of simplifying the process, high volume resistivity, and excellent aging resistance

Inactive Publication Date: 2006-02-15
CNPC JILIN CHEM GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the commonly used plasticizers are phthalate plasticizers, and the main product sold on the market is dioctyl phthalate, but the product is volatile, resistant to extraction and migration, heat resistance Aging resistance, volume resistivity, water resistance and oil resistance are not good enough, and the process adopted in the industrial production of dioctyl phthalate is relatively complicated, and the product needs to be decolorized to meet the requirements of user applications, and the product yield is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Esterification reaction

[0029] ①Monoesterification reaction: Add 143.5g of phthalic anhydride and 383g of isodecyl alcohol into a reaction kettle equipped with a stirrer, thermometer, water separator, condenser pipe and nitrogen gas inlet pipe, and at the same time, nitrogen gas is introduced, and the stirring is turned on The device starts to heat up, and when the reaction temperature reaches 140-150° C., it is kept for 10 minutes to end the monoesterification reaction.

[0030] ②Diesterification reaction: After phthalic anhydride is completely converted into monodecyl phthalate acid, continue to stir and heat up to 180°C, add 100 μL catalyst isopropyl titanate, and continue to stir and heat up to 210°C. Carry out constant temperature double esterification reaction 4 hours, after double esterification reaction finishes, product is cooled to room temperature, takes a sample and measures product acid value with acid-base titration (following analysis method is the ...

Embodiment 2

[0037] (1) Esterification reaction

[0038] ①Monoesterification reaction: Add 71.70g of phthalic anhydride and 197.4g of isodecyl alcohol into a reaction kettle equipped with a stirrer, thermometer, water separator, condenser tube and nitrogen inlet tube, and at the same time, nitrogen gas is introduced, and the Stirrer, start to heat up, when the reaction temperature reaches 140 ~ 150 ℃, keep for 10 minutes to end the monoesterification reaction.

[0039] ②Diesterification reaction: After the monoesterification reaction, raise the temperature to 180°C, add 50 μL catalyst isopropyl titanate, continue to raise the temperature to 220°C, carry out the double esterification reaction at constant temperature for 3 hours, and then end the diesterification reaction. Sampling analysis.

[0040] (2) post-processing

[0041] The process of dealcoholization under reduced pressure, alkali washing, water washing, steam stripping, cooling, and filtration, the operation process and conditio...

Embodiment 3

[0044] (1) Esterification reaction

[0045] ①Monoesterification reaction: Weigh 71.70g of phthalic anhydride and 191.5g of isodecyl alcohol into a reaction kettle equipped with a stirrer, thermometer, water separator, condenser pipe and nitrogen inlet pipe, and feed nitrogen at the same time. Turn on the stirrer and start to heat up. When the reaction temperature reaches 140-150°C, keep it for 10 minutes to end the monoesterification reaction

[0046] ② Diesterification reaction: After the monoesterification reaction, continue to heat up to 180°C, add 50 μL of catalyst isopropyl titanate, then continue to heat up to 190°C, carry out constant temperature double esterification reaction for 4.5 hours, and then end the monoester reaction. Sampling analysis.

[0047] (2) post-processing

[0048] The process of dealcoholization under reduced pressure, alkali washing, water washing, steam stripping, cooling, and filtration, the operation process and conditions are the same as in Ex...

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Abstract

The invention relates to a process for preparing diisodecyl phthalate, which comprises using phthalic anhydride and isodecanol as raw material, at the presence of nitrogen, first carrying out esterification reaction, then carrying out diesterification reaction by using ipropyl titanate as catalyst, obtaining crude product of diisodecyl phthalate, finally carrying out dealcoholizing, alkaline cleaning, water scrubbing and steam extraction to obtain the end product.

Description

technical field [0001] The invention relates to a method for preparing a plasticizer, in particular to a method for producing diisodecyl phthalate. Background technique [0002] At present, the commonly used plasticizers are phthalate plasticizers, and the main product sold on the market is dioctyl phthalate, but the product is volatile, resistant to extraction and migration, heat resistance Aging resistance, volume resistivity, water resistance and oil resistance are not good enough, and the process adopted in the industrial production of dioctyl phthalate is relatively complicated. The product needs to be decolorized to meet the requirements of user applications, and the product yield is low. Contents of the invention [0003] The purpose of the present invention is to overcome the deficiencies in the prior art and provide a method for producing diisodecyl phthalate with phthalic anhydride and isodecyl alcohol as raw materi...

Claims

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Application Information

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IPC IPC(8): C07C69/80C07C67/08
Inventor 刘乃青王勋章王硕侯淑兰
Owner CNPC JILIN CHEM GROUP CORP
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