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Purification method of 1,2-cyclohexane diisononyl phthalate

A technology of diisononyl cyclohexanedicarboxylate and ethyl difluoroacetate is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of low adsorption efficiency, complicated process and the like, To achieve the effect of increasing the adsorption capacity

Inactive Publication Date: 2016-09-21
张玲
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purification processes used in existing patents and literature technologies all use distillation or evaporation processes, or adsorbents such as silica gel. The process is complex and the adsorption efficiency is low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Step 1. Carboxylation reaction

[0018] In a 1000L stirred tank, add 100Kg of phenyl high-resolution agarose microspheres, 3Kg of ethyl difluoroacetate, 3Kg of furandicarboxylic acid, 0.05Kg of 1-carboxymethyl-3-butylimidazole nitrate, 300Kg of water, and heat up to 60 ℃, heat preservation for 45h, to obtain the adsorption resin.

[0019] Step 2, purification of diisononyl 1,2-cyclohexanedicarboxylate

[0020] Add 100Kg of the adsorption resin product obtained in step 1 to the exchange column, add industrial grade 1,2-cyclohexanedicarboxylic acid diisononyl from above the exchange column, the flow rate is 100L / h, and the effluent is the purified 1, 2-Diisononyl cyclohexanedicarboxylate. The product purity is shown in Table 1.

Embodiment 2

[0022] Step 1. Carboxylation reaction

[0023] In a 1000L stirred tank, add 100Kg of phenyl high-resolution agarose microspheres, 1Kg of ethyl difluoroacetate, 1Kg of furandicarboxylic acid, 0.01Kg of 1-carboxymethyl-3-butylimidazole nitrate, 100Kg of water, and heat up to 50 ℃, heat preservation 30h, get the adsorption resin.

[0024] Step 2, purification of diisononyl 1,2-cyclohexanedicarboxylate

[0025] Add 100Kg of the adsorption resin product obtained in step 1 to the exchange column, and add industrial grade 1,2-cyclohexanedicarboxylate diisononyl from above the exchange column at a flow rate of 50L / h, and the effluent is the purified 1, 2-Diisononyl cyclohexanedicarboxylate. The product purity is shown in Table 1.

Embodiment 3

[0027] Step 1. Carboxylation reaction

[0028] In a 1000L stirred tank, add 100Kg of phenyl high-resolution agarose microspheres, 5Kg of ethyl difluoroacetate, 5Kg of furandicarboxylic acid, 0.1Kg of 1-carboxymethyl-3-butylimidazole nitrate, 400Kg of water, and heat up to 80 ℃, heat preservation 60h, get the adsorption resin.

[0029] Step 2, purification of diisononyl 1,2-cyclohexanedicarboxylate

[0030] Add 100Kg of the adsorption resin product obtained in step 1 to the exchange column, and add industrial grade 1,2-cyclohexanedicarboxylate diisononyl from above the exchange column at a flow rate of 150L / h, and the effluent is the purified 1, 2-Diisononyl cyclohexanedicarboxylate. The product purity is shown in Table 1.

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PUM

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Abstract

The invention discloses a purification method of 1,2-cyclohexane diisononyl phthalate. The method comprises the following steps: adding phenyl high-resolution agarose microspheres, ethyl difluoroacetate, furandicarboxylic acid, 1-carboxymethyl-3-butyl imidazole nitrate and water into a stirring reactor, increasing the temperature to optimal temperature, then keeping the temperature to obtain adsorption resin; adding the adsorption resin obtained in the step 1 into an exchange column, refining crude 1,2-cyclohexane diisononyl phthalate via the adsorption resin to obtain purified 1,2-cyclohexane diisononyl phthalate.

Description

technical field [0001] The invention relates to a method for purifying a product, in particular to a method for purifying diisononyl 1,2-cyclohexanedicarboxylate. Background technique [0002] Plasticizers are widely used plastic additives, which can enhance the flexibility of plastics, facilitate processing, and meet various purposes. Plasticizers are the plastic additives with the largest production and consumption, and phthalate plasticizers play a dominant role in plasticizers. Phthalates are mainly used in polyvinyl chloride materials to change polyvinyl chloride from hard plastic to elastic plastic and act as a plasticizer. It is widely used in hundreds of kinds of toys, food packaging materials, medical blood bags and hoses, vinyl floors and wallpapers, cleaners, lubricants, personal care products such as nail polish, hair spray, soap and shampoo products, but have serious harm to human health. [0003] CN105254501A discloses the preparation method of diisononyl cy...

Claims

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Application Information

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IPC IPC(8): C07C69/75C07C67/56B01J20/26B01J20/30
Inventor 王琪宇
Owner 张玲