Method for the isolation of trimethylolpropane and sodium formate from a reaction mixture

A technology for trimethylolpropane and reaction mixture, which is applied in the field of separating trimethylolpropane and sodium formate, can solve the problems of reduced product yield, loss of trimethylolpropane, etc., and achieves improved yield, reduced three-waste pollution, The effect of reducing dosage

Inactive Publication Date: 2007-09-19
天津天大天海化工新技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Due to the presence of sodium formate in the mixed liquid during heating and distillation, the trimethylolpropane is decomposed, and there is a loss of trimethylolpropane in these three methods, thereby reducing the product yield.

Method used

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  • Method for the isolation of trimethylolpropane and sodium formate from a reaction mixture
  • Method for the isolation of trimethylolpropane and sodium formate from a reaction mixture

Examples

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Embodiment 1

[0031] Using a 5-stage combined extraction tank, the reaction mixture obtained in the above synthesis process is continuously fed into the combined extraction tank, the flow rate is 1800g / h, and the extraction agent n-butyraldehyde is continuously fed into each of the 5-stage tanks at the same time, and each stage is passed through The flow rate that enters n-butyraldehyde is all 250g / h, and the ratio of the total mass flow rate of organic solvent and the mass flow rate of reaction mixture is organic solvent: reaction mixture=0.69: 1 now. The extracted organic phase contained 33% (W / W) of trimethylolpropane, and the raffinate aqueous phase contained 14% (W / W) of sodium formate. The organic phase was rectified to obtain trimethylolpropane, and the aqueous raffinate was concentrated by evaporation to obtain sodium formate.

Embodiment 2

[0033] Using a 5-stage combined extraction tank, the reaction mixture obtained in the above synthesis process is continuously passed into the combined extraction tank, the flow rate is 1800g / h, and the extraction agent isobutanol is continuously fed into each stage of the 5-stage tank at the same time, and each stage is passed through The flow rate that enters isobutanol is all 500g / h, and the ratio of the total mass flow rate of organic solvent and the mass flow rate of reaction mixture is organic solvent: reaction mixture=1.39: 1 now. The extracted organic phase contained 17% (W / W) of trimethylolpropane, and the raffinate aqueous phase contained 14% (W / W) of sodium formate. The organic phase was rectified to obtain trimethylolpropane, and the aqueous raffinate was concentrated by evaporation to obtain sodium formate.

Embodiment 3

[0035] Using a 5-stage combined extraction tank, the reaction mixture obtained in the above synthesis process is continuously passed into the combined extraction tank, the flow rate is 1800g / h, and the extraction agent n-octanol is continuously fed into each stage of the 5-stage tank at the same time, and each stage is passed through The flow rate of entering n-octanol is 200g / h, and the ratio of the total mass flow rate of the organic solvent and the mass flow rate of the reaction mixture is organic solvent: reaction mixture=0.56:1. The extracted organic phase contained 41% (W / W) of trimethylolpropane, and the raffinate aqueous phase contained 14% (W / W) of sodium formate. The organic phase was rectified to obtain trimethylolpropane, and the aqueous raffinate was concentrated by evaporation to obtain sodium formate.

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Abstract

The related method to separate trimethylolpropane and sodium formate from the mixture comprises: preparing trimethylolpropane with formaldehyde and butyladehyde; selecting a combined extraction groove with reacted liquor as aqueous phase and water-insoluble organic solvent with total mass flow rate to the mixed liquor as 0.5~3.0:1 as organic phase for countercurrent extraction; treating the organic phase to obtain the trimethylolpropane and sodium formate from residual water. This invention has no decomposition loss.

Description

technical field [0001] The invention relates to a method for separating trimethylolpropane and sodium formate from a reaction mixture in which trimethylolpropane is produced by reacting formaldehyde and n-butyraldehyde. Background technique [0002] The most economical process for producing trimethylolpropane is to carry out aldol condensation and Connizzaro reaction of formaldehyde and n-butyraldehyde in the presence of a basic catalyst. The basic reaction equation is as follows: [0003] In the first step, formaldehyde and n-butyraldehyde are condensed in the presence of a basic catalyst to generate 2,2-dimethylol butyraldehyde: [0004] C 3 h 7 CHO+2CH 2 O-→C 2 h 5 C(CH 2 Oh) 2 CHO [0005] The second step to generate products: [0006] C 2 h 5 C(CH 2 Oh) 2 CHO+CH 2 O+NaOH-→C 2 h 5 C(CH 2 Oh) 2 CH 2 OH+CHOONa [0007] There are trimethylolpropane and sodium formate in the reacted compound, since sodium formate will cause thermal decom...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/86C07C51/41C07C31/22C07C53/06
Inventor 张曾刘锋李崇李雪王芳张大治宗麟博张宝源
Owner 天津天大天海化工新技术有限公司
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