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Method for extracting trimethylolpropane

A ditrimethylolpropane and trimethylolpropane technology, which is applied in the field of ditrimethylolpropane extraction, can solve the problems of environmental pollution, coloring, and high energy consumption of solvent recovery, and achieve the effect of eradicating pollution and saving energy

Active Publication Date: 2008-01-23
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of this invention is to provide a kind of method that obtains ditrimethylolpropane from trimethylolpropane distillation raffinate with activated carbon, thus solves the problem that the commonly used organic solvent benzene series extraction product is still colored, solvent recovery energy consumption is high, environmental pollution issues

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Take 100g of trimethylolpropane distillation raffinate (the content of ditrimethylolpropane is about 40wt%), add 300g of deionized water, stir and dissolve at 60±10°C for 90 minutes, then add 2.5g The particle size of fruit shells is micron activated carbon of 0.3-150 microns, stirred for 30 minutes to absorb and decolorize, then filter with a Buchner funnel at the above temperature (filter material pores≤0.3 μm, the same below), and filter out the activated carbon, The filtrate was cooled and crystallized, cooled to 0±5°C and kept for 280 minutes, then filtered with a Buchner funnel to separate the crystals from the filtrate to obtain 72.5 g of light yellow crude ditrimethylolpropane crystals containing a certain amount of water, and recover them filtrate;

[0020] (2) Add 145g of deionized water to the 72.5g crystals prepared above to dissolve, stir and dissolve at 60±5°C for 85 minutes, then add 3.2g of the above-mentioned activated carbon, and stir for another 6...

Embodiment 2

[0022] Operate according to the technological process and technological conditions of above-mentioned embodiment 1, wherein, the consumption of described fruit shell class micron activated carbon, on the basis of original consumption, step (1) and step (2) each increase 1g respectively (step 1 gac consumption is 3.5g, step 2 gac consumption is 4.2g), the ditrimethylol propane that obtains, its color number drops to No. 10, other index is constant (visible, when described gac consumption increases, is conducive to Decolorization, the product color number is No. 10).

Embodiment 3

[0024] (1) Weigh 100g of trimethylolpropane distilled raffinate, add 280g of deionized water, and dissolve under stirring at 60±10°C for 90 minutes. Then add 2.8g of activated carbon with a particle size of 0.3-150 microns, stir and decolorize for 30 minutes, filter with the Buchner funnel at the above temperature to remove the activated carbon, and the resulting filtrate drops to 0 ± 5 Carry out crystallization at this temperature for 240 minutes, then use a Buchner funnel to filter the crystals from the solution to obtain 71.2 g of light yellow ditrimethylolpropane crystals containing a certain amount of water, and reclaim its mother liquor;

[0025] (2) Add 148g of deionized water to the obtained 71.2g of crystals for dissolving, stir and dissolve at 60±5°C for 85 minutes, then add 3.2g of the above-mentioned activated carbon, and stir for another 65 minutes for adsorption and decolorization. , use microporous filtration to remove the activated carbon and its adsorbed color...

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Abstract

The invention relates to a method extracting the double trimethylolpropane from the trimethylolpropane distillation residual. The trimethylolpropane distillation residual is dissolved by the deionized water and is added with the active carbon with micron-sized fruit shell size to absorb, and is filtered through a Buchner funnel to filter the active carbon; the temperature of the filter liquor is reduced to minus 5 DEG C. to 1 DEG C. crystallization, and is filtered through the Buchner funnel to gain the crude product of the double trimethylolpropane and collect the mother liquid. The crude product crystals of the double trimethylolpropane are dissolved through the deionized water and is added with the active carbon with micron-sized fruit shell size to absorb, and is filtered through the Buchner funnel to filter the active carbon; the temperature of the filter liquor is reduced to minus 5 DEG C. to 1 DEG C. crystallization, and the filter liquor is filtered through the Buchner funnel to separate the crystals with the mother liquid which is recycled. The crystals gain the double trimethylolpropane products after dehydration and drying. The weight per centage of the hydroxyl is not less than 96 per cent; the weight per centage of the water is not more than 0.2 per cent; the melting point is 107 DEG C. to 110.5 DEG C.; the weight per centage of the hydroxyl value is 26 per cent to 26.7 per cent; the color number of the product is number 10 to number 15 and 80 per cent to 90 per cent of the trimethylolpropane can be recycled.

Description

technical field [0001] The invention relates to a method for extracting ditrimethylolpropane from trimethylolpropane distillation raffinate. Background technique [0002] Ditrimethylolpropane is a polyol compound. The hydroxyl group in its molecular structure has good reactivity, and it can react with many kinds of carboxylic acid compounds to generate a series of resins and polyurethane compounds. Therefore, it is widely used in various fields such as high-grade paints, coatings, and synthetic high-grade lubricants. There are usually two preparation methods for ditrimethylolpropane: one method is to use trimethylolpropane as a raw material to condense two molecules to obtain ditrimethylolpropane; the other method is to obtain ditrimethylolpropane from trimethylolpropane Distillation raffinate (contains about 40wt% ditrimethylolpropane) for extraction. The commonly used extraction method is to use organic solvent extraction, so that the colored compounds in the raffinate a...

Claims

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Application Information

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IPC IPC(8): C07C29/78C07C31/22
Inventor 常凤忱张险波张万玉王影李长红李连波文海峰潘艳秋
Owner BC P INC CHINA NAT PETROLEUM CORP
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