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Method of decolorizing and refining double trimethylolpropane

A technology of bis-trimethylolpropane and a refining method, which is applied in the preparation of hydroxyl compounds, separation/purification of hydroxyl compounds, chemical instruments and methods, etc. Effect

Active Publication Date: 2010-06-30
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

In particular, the ditrimethylolpropane product obtained by extraction with benzene organic solvents has a light pink appearance, repeated extraction and washing with organic solvents has no effect, and is still light pink, which cannot meet the user's requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Weigh 100 g of light pink ditrimethylolpropane obtained by organic solvent extraction, add 250 g of deionized water, heat up to 65 °C in a glass three-necked flask, start the stirrer, and control its speed to 120 rpm After stirring for 90 minutes, add 2.5 grams of micron-sized activated carbon with a particle size of 0.3 to 150 μm for adsorption and decolorization. After continuing to stir for 60 minutes, cool down to 50°C and filter with a Buchner funnel. The filter material has a pore size of ≤0.3 μm and removes the activated carbon. Add the filtrate to a glass container and stir to lower the temperature. After dropping to 0°C, keep it for 3 hours. Filter the crystals with a Buchner funnel to obtain white crystals, put them in a vacuum oven, and bake them at 80°C for 4 hours to obtain white powder bismuth Trimethylolpropane 95g, sampling analysis, purity 96.4%, moisture 0.25%, melting point 107-110.48°C, hydroxyl 26.7%, color number (platinum-cobalt method) No. 20.

Embodiment 2

[0015] Weigh 100g of ditrimethylolpropane with a light yellow color prepared by organic solvent extraction, add 280g of deionized water, heat and dissolve in a three-neck glass flask with stirring, the stirring speed is 90 rpm, and the temperature is 60°C ; then add 3.0 g of micron-sized activated carbon with a particle size of 0.3 to 150 μm, continue to stir for 50 minutes, and then use a Buchner funnel to filter the activated carbon with micropores to remove the activated carbon. The filter material has a pore size of ≤0.3 μm, and the filtrate is added to the glass container Stir in medium temperature to cool down and crystallize, keep at this temperature for 3.5 hours when it drops to -1 ° C, and filter the crystals at this temperature to obtain white crystals, put them in a vacuum oven and dry them at 85 ° C for 4.5 hours to get White ditrimethylolpropane 93.5g, sampling analysis purity 96.8%, color number (platinum-cobalt method) No. 15, moisture ≤ 0.2%, hydroxyl value 26....

Embodiment 3-6

[0016] Embodiment 3-6 (see the table below for details)

[0017] serial number

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Abstract

The invention relates to a decoloring and refining method of the colored double trimethylolpropane extracting from the trimethylolpropane distillation residual by the solvent extraction method. The colored double trimethylolpropane is added with the deionized water with weight 2 times to 10 times that of the colored double trimethylolpropane with temperature controlled at 60 DEG C. to 65 DEG C. and is stirred and dissolved with rotary speed of 90r / min to 120r / min. After dissolving, the micron-sized active carbon with weight 1 per cent to 10 per cent of that of the double trimethylolpropane isadded and stirred continuously for 50min to 60min, and then the temperature is lowered to 50 DEG C. to 55 DEG C. to filter; the temperature of the gained filter liquor is lowered to minus 1 DEG C. tozero DEG C. to crystallize is kept for 180min to filter; the gained white crystals are put into a vacuum drying oven to dry below 80 DEG C. to 85 DEG C. to gain the white powder double trimethylolpropane which is measured by weight per centage with purity of 96.4 per cent, water content of 0.25 per cent and hydroxyl of 26.7 per cent, the color number (platinum-cobalt method) of number 5 to number20 and the melting point of 107 DEG C. to 110.48 DEG C.. The invention does not use benzene series as the solvent, which eradicates the pollution of the benzene series, saves a great deal of consumedenergy because of being used for the recycling of the organic solvent and really realizes the green technology process without hazard during production.

Description

technical field [0001] The invention relates to a method for decolorizing and refining colored ditrimethylolpropane extracted from trimethylolpropane distillation raffinate by solvent extraction. 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. [0003] 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. A commonly used extraction method is extraction with an or...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/26C07C29/78C07C29/94
Inventor 常凤忱张险波张万玉王影李长红逄金国梁绍杰曲行东
Owner BC P INC CHINA NAT PETROLEUM CORP