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Catalyst for synthesizing diisooctyl phthalate plasticizer and preparation method and application of catalyst

A technology of diisooctyl phthalate and catalyst is applied to the catalyst for synthesizing diisooctyl phthalate plasticizer and the field of preparation thereof, and can solve the problems of high separation difficulty, low esterification rate, cumbersomeness and the like , to reduce the reaction temperature, improve the esterification rate, and achieve the effect of light color

Active Publication Date: 2019-10-01
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Concentrated sulfuric acid (Chinese invention patent, application number: 201310109696.7), p-toluenesulfonic acid (Chinese invention patent, application number: 201310525488.5), tetraisopropyl titanate (Chinese invention patent, application number: 200610014747.8) and other liquid acids are used as catalysts However, there are disadvantages such as equipment corrosion and separation difficulty
Therefore, people have conducted a lot of research on the application of solid acid catalysts in this reaction: the Chinese invention patent (application number: 201810919768.7) uses magnetic iron oxide-coated cobalt oxide nanocomposites as catalysts, and the preparation conditions are harsh and cumbersome. A large amount of organic wastewater is produced, which is not conducive to large-scale industrial production; in the Chinese invention patent (application number: 201410460384.5), hydroxypropyl-β-cyclodextrin / aluminophosphotungstic acid is used as a catalyst, and the esterification rate (94.5%) is low. The reaction temperature (150°C) is high, which will easily lead to darkening of the product color and affect the appearance of the product

Method used

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  • Catalyst for synthesizing diisooctyl phthalate plasticizer and preparation method and application of catalyst
  • Catalyst for synthesizing diisooctyl phthalate plasticizer and preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dissolve 11.7g of cesium nitrate (0.06mol) and 6.0g of copper tungstic acid (0.01mol) in 50mL of deionized water, stir and mix evenly, pour into a hydrothermal reactor, react at 100°C for 12h, and then the reaction product Cool to room temperature, filter, and dry the obtained solid to obtain the copper cesium tungstate catalyst. The XRF characterization results are shown in Table 1. It is determined by XRF characterization that n=6 in the molecular formula, that is, the catalyst is Cs 6 wxya 2 o 10 .

[0026] Add 13.0g isooctyl alcohol and 7.4g phthalic anhydride (molar ratio 2:1) into a four-necked flask with a reflux condenser, then add 0.5g (2.5%) of Cs 6 wxya 2 o 10 Catalyst, flow rate is 5mL / min nitrogen protection, heating to 100 ° C, after stirring for 4h, stop heating and stirring, vacuum distillation to remove the remaining iso-octanol, filter to remove the catalyst, to obtain di-isooctyl phthalate, Through high-performance liquid chromatography analysis...

Embodiment 2

[0028] Dissolve 10.7g of cesium nitrate (0.055mol) and 6.0g of copper tungstic acid (0.01mol) in 60mL of deionized water, stir and mix evenly, pour into a hydrothermal reactor, react at 120°C for 24h, and then the reaction product Cool to room temperature, filter, and dry the obtained solid to obtain the copper cesium tungstate catalyst. The XRF characterization results are shown in Table 1. It is determined by XRF characterization that n=5.5 in the molecular formula, that is, the catalyst is H 0.5 Cs 5.5 wxya 2 o 10 .

[0029] Add 22.8g of isooctyl alcohol and 7.4g of phthalic anhydride (molar ratio 3.5:1) into a four-necked flask with a reflux condenser, then add 0.3g (1%) of H 0.5 Cs 5.5 wxya 2 o 10 The catalyst was protected by nitrogen with a flow rate of 10mL / min, heated to 130°C, stirred for 6 hours, then stopped heating and stirring, distilled under reduced pressure to remove the remaining isooctyl alcohol, and filtered to remove the catalyst to obtain diisoocty...

Embodiment 3

[0031] Dissolve 1.0g of cesium nitrate (0.005mol) and 6.0g of copper tungstic acid (0.01mol) in 70mL of deionized water, stir and mix evenly, pour into a hydrothermal reactor, react at 120°C for 24h, and then the reaction product Cool to room temperature, filter, and dry the obtained solid to obtain the copper cesium tungstate catalyst. The XRF characterization results are shown in Table 1. It is determined by XRF characterization that n=0.5 in the molecular formula, that is, the catalyst is H 5.5 Cs 0.5 wxya 2 o 10 .

[0032] Add 15.6g isooctyl alcohol and 7.4g phthalic anhydride (molar ratio 2.4:1) into a four-necked flask with a reflux condenser, then add 0.4g of H 5.5 Cs 0.5 wxya 2 o 10 The catalyst was protected by nitrogen gas with a flow rate of 8mL / min, heated to 130°C, and stirred for 4 hours, then the heating and stirring were stopped, the remaining isooctyl alcohol was removed by distillation under reduced pressure, and the catalyst was removed by filtration ...

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Abstract

The invention discloses a catalyst for synthesizing a diisooctyl phthalate plasticizer and a preparation method and application of the catalyst. The molecular general formula of the catalyst is H6-nCsnCuW2O10; the value of n is 0.5-6. Cerium salt and copper tungstate are dissolved in deionized water, stirring and uniform mixing are conducted, heating is conducted to 80-120 DEG C for a reaction of12-36 hours, a reaction product is cooled to room temperature, and the obtained solid is filtered and dried to obtain the catalyst. The prepared cesium copper tungstate serves as the catalyst and is used for synthesizing the diisooctyl phthalate plasticizer through an alcoholysis reaction of phthalic anhydride and isooctanol, the reaction temperature can be significantly lowered, the esterification rate of the phthalic anhydride and the yield of diisooctyl phthalate are increased, and the obtained plasticizer product is light in color and luster.

Description

technical field [0001] The invention relates to the field of catalyst synthesis, in particular to a catalyst used for the synthesis of di-isooctyl phthalate plasticizers, a preparation method and application thereof. Background technique [0002] Plasticizer is a polymer material additive widely used in industry. Adding this substance in plastic processing can make it more flexible and easy to process. There are many kinds of plasticizers, and the most widely used ones are phthalates. Among them, di-isooctyl phthalate is the product with the largest output and superior performance among plasticizers, and it has good compatibility. , high plasticizing efficiency, low volatility and other advantages. [0003] The industrial production of di-isooctyl phthalate is mainly obtained through the alcoholysis reaction of phthalic anhydride and iso-octanol, which needs to be carried out under the action of a catalyst. Concentrated sulfuric acid (Chinese invention patent, application ...

Claims

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Application Information

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IPC IPC(8): B01J23/888C07C67/08C07C69/80
CPCB01J23/888C07C67/08C07C69/80
Inventor 丁建飞秦娜娣刘心雨邵荣许伟关荣锋张义东颜秀花
Owner YANCHENG INST OF TECH
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