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Method for recovering ditrimethylolpropane from trimethylolpropane raffinate

A technology of ditrimethylolpropane and ditrimethylolpropane mother, which is applied in the field of ditrimethylolpropane recovery, can solve the problems of low recovery efficiency, uneconomical, air pollution, etc., and avoid the problems caused by incineration. Effect of waste gas, improvement of product competitiveness, and reduction of production cost

Active Publication Date: 2015-12-16
NANTONG BAICHUAN NEW MATERIAL CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are generally two ways to deal with the above-mentioned residual liquid in China. One is to transport the residual liquid to solid waste for incineration to produce steam. Because the gas production is very low, direct incineration is very uneconomical and pollutes the air.
The second is the adhesive used to make resin, but the price of making resin is relatively low, and it is not economical
Therefore, how to recover 50% of the ditrimethylolpropane in the raffinate is the research direction for enterprises to increase benefits. There have been studies in Japan that used solvents to extract the raffinate at low temperature to recover a certain amount of ditrimethylolpropane. , but the recycling efficiency is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Step S1: First, add a mixed solvent of acetone and ethanol at a mass ratio of 2:1 into the crystallization tank, and the addition amount is 5t; Trimethylolpropane content is 50%;

[0013] Step S2: After adding the trimethylolpropane raffinate, keep the crystallization kettle at -7°C for constant temperature crystallization for 5 hours;

[0014] Step S3: Transfer the material in the crystallization tank to the filter for filtration. At the beginning of the filtration, first connect the filter and the crystallization tank through a circulation pipeline to form a material circulation loop, and then circulate the material through the material circulation loop for 1 hour, after 1 hour , perform filtration to obtain a filter cake and filtrate, transport the filtrate to the recovery ditrimethylolpropane mother liquor tank, and use nitrogen to purge the filter for 40 minutes after the filtration is completed;

[0015] Step S4: Heat the filter cake obtained by filtering in step...

Embodiment 2

[0019] Step S1: First, add a mixed solvent of acetone and ethanol at a mass ratio of 2:1 into the crystallization tank, and the addition amount is 3t; Trimethylolpropane content is 50%;

[0020] Step S2: After adding the trimethylolpropane raffinate, keep the crystallization kettle at -10°C for constant temperature crystallization for 3 hours;

[0021] Step S3: Transfer the material in the crystallization tank to the filter for filtration. At the beginning of the filtration, first connect the filter and the crystallization tank through a circulation pipeline to form a material circulation loop, and then circulate the material through the material circulation loop for 1 hour, after 1 hour , perform filtration to obtain a filter cake and filtrate, transport the filtrate to the recovery ditrimethylolpropane mother liquor tank, and use nitrogen to purge the filter for 30 minutes after the filtration is completed;

[0022] Step S4: Heat the filter cake obtained by filtering in ste...

Embodiment 3

[0026] Step S1: First, add the mixed solvent of acetone and ethanol according to the mass ratio of 2:1 into the crystallization kettle, and the addition amount is 4t; and add 4t of trimethylolpropane raffinate in the crystallizer; Trimethylolpropane content is 50%;

[0027] Step S2: After adding the trimethylolpropane raffinate, keep the crystallization kettle at -5°C for constant temperature crystallization for 4 hours;

[0028] Step S3: Transfer the material in the crystallization tank to the filter for filtration. At the beginning of the filtration, first connect the filter and the crystallization tank through a circulation pipeline to form a material circulation loop, and then circulate the material through the material circulation loop for 1 hour, after 1 hour , perform filtration to obtain a filter cake and filtrate, transport the filtrate to the recovery ditrimethylolpropane mother liquor tank, and use nitrogen to purge the filter for 35 minutes after the filtration is ...

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Abstract

The invention relates to a method for recovering ditrimethylolpropane from trimethylolpropane raffinate. The method is characterized by comprising the steps: firstly adding a mixed solvent, which is prepared from acetone and ethanol according to the mass ratio of 2: 1, into a crystallization kettle; adding the trimethylolpropane raffinate, of which the mass is equal to that of the solvent, into the crystallization kettle, and carrying out constant-temperature crystallization for 3-5 hours at the temperature of -5 to -10 DEG C; and carrying out filtering, heating filter cakes to the temperature of 80-120 DEG C in a filter so as to melt the filter cakes, meanwhile, vacuumizing the filter, and completely removing the solvent from the filter cakes, thereby obtaining solvent-free ditrimethylolpropane. Over 40% of ditrimethylolpropane can be recovered from the raffinate by the method, so that resources are thoroughly utilized, the production cost is reduced, and the economic benefit and product competitiveness are improved.

Description

technical field [0001] The invention relates to a method for recovering ditrimethylolpropane from trimethylolpropane raffinate, which belongs to the separation and purification part in the technical field of fine chemical industry. Background technique [0002] In the production process of trimethylolpropane, a by-product commonly known as ditrimethylolpropane will be produced. Since the production of ditrimethylolpropane is very small, the price is relatively high. Generally, it is 2- trimethylolpropane 3 times. Therefore, improving the yield of ditrimethylolpropane as much as possible is the research direction for enterprises to increase benefits. The existing methods for recovering ditrimethylolpropane generally go through the steps of decolorization, filtration, crystallization, re-filtration, evaporation and slicing, wherein the mother liquor is extracted from the trimethylolpropane and ditrimethylolpropane through the extraction tower. Come out, then reclaim the solv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/13C07C41/40
CPCC07C41/40C07C43/13
Inventor 郑铁江赵红伟蒋国强马阳升曹圣平孙百亚吴晓明杜发举陶植姜伟伟
Owner NANTONG BAICHUAN NEW MATERIAL CO LTD
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