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Environment-friendly production method of diisopentyl oxalate without adding water-carrying agent

A technology of diisoamyl oxalate and diisoamyl oxalate, which is applied in the field of green production of diisoamyl oxalate, can solve the problems of energy saving, environmental protection effect and poor economy, and lower product yield , increase the evaporation of liquid phase, etc., to achieve the effect of green production, simplifying production links, and reducing production costs

Active Publication Date: 2016-06-15
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, it is often necessary to distill and separate the reaction liquid during the post-treatment process of the product. During the distillation process, the water-carrying agent used as the front fraction will bring out a small amount of the target product ester and reduce the product yield.
[0004] Since isoamyl alcohol and water can form an azeotrope (water 49.6%wt in isoamyl alcohol-water azeotropic composition, azeotropic point 95.15 ℃), and use cyclohexane water-carrying agent (cyclohexane-water azeotropic composition in Water accounts for 8.4%wt, and the azeotropic point is 68.95 ℃), compared with adding cyclohexane with water agent, it will increase the liquid phase evaporation, and will reduce the temperature of the reaction system, increase the post-treatment cost, and increase the pollutants in the system, so the energy saving effect , environmental protection effect and poor economy
In addition, when using low-boiling point organic solvents with water, attention should be paid to safety issues such as fire prevention and volatile toxicity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add oxalic acid and isoamyl alcohol into the reaction kettle in a certain proportion, use zinc sulfate as a catalyst, install a water separator and a reflux condenser, heat to reflux, collect fractions through rectification and separate the generated water. After the temperature of the reaction kettle rises to 145-150°C, keep the reaction for 30 minutes, then collect the isoamyl alcohol fraction by rectification and cut off the tail, and use vacuum distillation to collect the high-purity product. The final product is diisoamyl oxalate ester. The esterification rate is >95% in the whole production process. After the water generated in the reaction process is collected, it is separated by reverse osmosis membrane separation equipment, and the fresh water passed through the membrane is discharged up to the standard, and the concentrated water and oil phase are used to recover isoamyl alcohol. The isoamyl alcohol obtained by rectification and tail cutting and the recovered...

Embodiment 2

[0019] Add oxalic acid and isoamyl alcohol into the reaction kettle in a certain proportion, use p-toluenesulfonic acid as a catalyst, install a water separator and a reflux condenser, heat to reflux, collect fractions through rectification and separate the generated water. When the temperature of the reaction kettle reaches 130-140°C, keep the reaction for 40 minutes, then collect the isoamyl alcohol fraction through rectification and cut off the tail, and finally the kettle liquid is decolorized by activated carbon and filtered to obtain the product diisoamyl oxalate. The esterification rate of the whole reaction preparation process is >96%. After the water produced in the reaction process is collected, it is separated by reverse osmosis organic membrane separation equipment, and the fresh water passed through the membrane is discharged up to the standard, and the concentrated water and oil phase are used to recover isoamyl alcohol. The isoamyl alcohol obtained by rectificat...

Embodiment 3

[0022] Add oxalic acid and isoamyl alcohol into the reaction kettle in a certain proportion, use alumina-loaded solid acid as the catalyst, and cyclohexane as the water-carrying agent, install a water separator and a reflux condenser, heat to reflux, and pass through the fine Distillation collects fractions and separates the resulting water. When the temperature of the reaction kettle reaches 120-130°C, react for 50 minutes, then collect the isoamyl alcohol fraction through rectification and cut off the tail, and finally obtain the product diisoamyl oxalate after the kettle liquid is filtered. The esterification rate of the whole reaction process is >97%. After the water produced in the reaction process is collected, it is separated by reverse osmosis organic membrane separation equipment, and the fresh water passed through the membrane is discharged up to the standard, and the concentrated water and oil phase are used to recover isoamyl alcohol. The isoamyl alcohol obtained ...

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Abstract

The invention relates to an environment-friendly production method of diisopentyl oxalate without adding a water-carrying agent.Oxalic acid and isoamyl alcohol serve as raw materials, an esterification reaction is performed under the action of a catalyst, reactant isoamyl alcohol and water form azeotrope, the azeotrope is condensed and subjected to water diversion, the isoamyl alcohol subjected to water diversion is recycled, isoamyl alcohol and diisopentyl oxalate are separated after a reaction ends, and the diisopentyl oxalate product is obtained.The environment-friendly production method of diisopentyl oxalate has the advantages that by means of the azeotropic characteristic of isoamyl alcohol and water, no water-carrying agent needs to be additionally added, pollution of newly-added substances is avoided, production links are simplified, production cost is reduced, an esterification reaction is easy, and separation and purification of the product are easy; meanwhile, water in the product is separated through a membrane separation method, the process is environmentally friendly, and environment-friendly production of the whole technological process of diisopentyl oxalate is achieved.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a green production method of diisoamyl oxalate without adding a water-carrying agent. Background technique [0002] Diisoamyl oxalate is a new type of cetane number (CetaneNumber, CN) improver, adding a certain proportion of diisoamyl oxalate can increase CN by 2-20 units, and it can be compared with diesel oil Good mutual solubility, so it is expected to replace nitrate esters and become the most promising class of ester improvers. [0003] Using oxalic acid and isoamyl alcohol as raw materials, carry out esterification reaction under catalyst conditions to produce diisoamyl oxalate, and the water carrier has an important influence on the reaction. The water-carrying agent can take the water generated by the esterification reaction out of the reaction system, which is beneficial to the reaction. However, common water-carrying agents such as benzene, toluene, xylene, cyclohexane a...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/48C07C67/52C07C67/54C07C69/36
CPCC07C67/08C07C67/48C07C67/52C07C67/54C07C69/36
Inventor 王岚潘繁荣赵宇培王龙耀陈群
Owner CHANGZHOU UNIV
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