CN101108786A - Method of decolorizing and refining double trimethylolpropane - Google Patents
Method of decolorizing and refining double trimethylolpropane Download PDFInfo
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- CN101108786A CN101108786A CNA2006100990628A CN200610099062A CN101108786A CN 101108786 A CN101108786 A CN 101108786A CN A2006100990628 A CNA2006100990628 A CN A2006100990628A CN 200610099062 A CN200610099062 A CN 200610099062A CN 101108786 A CN101108786 A CN 101108786A
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- ditrimethylolpropane
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- double trimethylolpropane
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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 is added 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. to zero 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 number 20 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 consumed energy 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
The present invention relates to a kind of method of decolorizing and refining of the coloured ditrimethylolpropane that from the TriMethylolPropane(TMP) vinasse, extracts with solvent extration.
Background technology
Ditrimethylolpropane is a kind of polyol compound, and the hydroxyl in its molecular structure has good reaction activity, can with a variety of carboxylic acid compound generation esterification reactions, and then generate a series of resenes and polyurethanes compound.Therefore be widely used in high-grade paint, coating, every field such as synthetic top-grade lubricating oil.
Ditrimethylolpropane has two kinds of preparation methods usually: a kind of method is to be raw material with the TriMethylolPropane(TMP), carries out two molecule condensations and then obtains ditrimethylolpropane; Another kind method is to extract from TriMethylolPropane(TMP) vinasse (containing the ditrimethylolpropane about 40wt%).Extracting method commonly used is to use organic solvent extraction, when extraction obtains ditrimethylolpropane, colored compound in the raffinate is extracted in the organic solvent, organic solvent can't all remove the coloring matter in TriMethylolPropane(TMP) raffinate and the ditrimethylolpropane crude product, prepares lower ditrimethylolpropane product outstanding number.The ditrimethylolpropane product that particularly utilizes benzene class organic solvent extraction to make, outward appearance has pale pink, and repeated multiple times is used organic solvent extraction and washing to no effect, still is pale pink, can't satisfy user's service requirements.
Summary of the invention
The purpose of this invention is to provide a kind of color of utilizing the ditrimethylolpropane that the gac effective elimination extracts with organic solvent from the TriMethylolPropane(TMP) vinasse, obtain the method for the ditrimethylolpropane of white crystal.
The present invention is achieved by following technical scheme:
Take the ditrimethylolpropane that has color of organic solvent extractionprocess preparation, add the 2-10 deionized water doubly of ditrimethylolpropane weight, controlled temperature is 60～65 ℃, stirring and dissolving, and its mixing speed is 90～120 rev/mins; The gac that the dissolving back adds the 1-10% of ditrimethylolpropane weight carries out adsorption bleaching, continues to stir after 50～60 minutes, is cooled to 50～55 ℃ of filtrations, removes solid activated carbon, and the filtrate that obtains cools to-1～0 ℃ of crystallization, and is incubated 180 minutes; Again with xln and mother liquor filtering separation, the xln that obtains white is put into vacuum drying oven in 80～85 ℃ of following oven dry 4～5 hours, obtain the ditrimethylolpropane powder-product of white, sampling analysis, purity 96.4%, moisture 0.25%, 107～110.48 ℃ of fusing points, hydroxyl 26.7%, No. 20, look number (platinum-cobalt method).
Above-mentioned decoloring method, the particle diameter of its described micron order gac are 0.3～150 μ m.
Above-mentioned decoloring method, its described filtering material aperture is≤0.3 μ m.
Under the present invention compared with prior art, have significant technical progress and tangible positively effect:
(1) after faint yellow, peach ditrimethylolpropane carries out decolorizing and refining with technical scheme provided by the invention, becomes white crystals body ditrimethylolpropane.Its product weight percentage composition 〉=96%, moisture weight percentage≤0.2%, fusing point are 107～110.5 ℃, the hydroxyl value weight percentage is 26～26.7%, product look numbers 10～No. 20.
(2) without benzene series things such as benzene, toluene and dimethylbenzene as solvent, eradicated the pollution of benzene and homologue thereof; And save in a large number because of being used for the energy that Recovery of Organic Solvent consumes, real realization non-harmful friendly process process in the production process.
Embodiment
Embodiment 1:
Take by weighing the ditrimethylolpropane 100g that has pale pink that makes with organic solvent extractionprocess, add the 250g deionized water, be warmed up to 65 ℃ at the glass there-necked flask, start agitator, controlling its rotating speed is under 120 rev/mins, stir after 90 minutes, add 2.5 gram particles and directly be the micron order charcoal absorption decolouring of 0.3～150 μ m, continue to stir after 60 minutes, cool to 50 ℃ and filter with cloth formula funnel, the filtering material aperture is≤0.3 μ m, the elimination gac is added to filtrate in the Glass Containers and stirs cooling, keeps 3 hours after dropping to 0 ℃, with cloth formula funnel xln is filtered, obtain the white crystals body and send in the vacuum drying oven, dried by the fire 4 hours down, obtain white powdery ditrimethylolpropane 95g at 80 ℃, sampling analysis, purity 96.4%, moisture 0.25%, 107～110.48 ℃ of fusing points, hydroxyl 26.7%, No. 20, look number (platinum-cobalt method).
Embodiment 2
Take by weighing the flaxen ditrimethylolpropane 100g that has, add the 280g deionized water with the organic solvent extractionprocess preparation, heating for dissolving under in the glass there-necked flask, stirring, 90 rev/mins of stirring velocitys, its temperature are 60 ℃; Adding the 3.0g particle diameter then is the micron order gac of 0.3～150 μ m, continue to stir 50 minutes, with cloth formula funnel gac is carried out millipore filtration to remove gac then, the filtering material aperture is≤0.3 μ m, filtrate joined stir decrease temperature crystalline in the Glass Containers, under this temperature, kept 3.5 hours when dropping to-1 ℃, and under this temperature, crystallisate is filtered, obtain the white crystals body, put into vacuum drying oven and under 85 ℃ of conditions, dried 4.5 hours, obtain the ditrimethylolpropane 93.5g of white, sampling analysis purity 96.8%, No. 15, look number (platinum-cobalt method), moisture≤0.2%, hydroxyl value 26.8%, 107.3～110 ℃ of fusing points.
Embodiment 3-6 (seeing following table for details)
| Sequence number | Activated carbon dosage | The deionized water consumption | Working method | Operational condition | Product index |
| Example 3 | 4g | 400g | With embodiment 1 | With embodiment 1 | Look numbers No. 15, other and embodiment 1 |
| Example 4 | 6g | 600g | With embodiment 1 | With embodiment 1 | Look numbers No. 10, other and embodiment 1 |
| Example 5 | 8g | 650g | With embodiment 1 | With embodiment 1 | Look numbers No. 5, other and embodiment 1 |
| Example 6 | 10g | 4500g | With embodiment 1 | With embodiment 1 | Look numbers No. 10 other and embodiment 1 |
Comparative Examples 1
Take by weighing embodiment 1 used ditrimethylolpropane 100g, add 250g toluene agitator treating in Glass Containers, washing material is filtered with cloth formula funnel, adding 250g toluene again carries out putting into 85 ℃ of oven dry of vacuum drying oven 4.5 hours behind secondary washing, the secondary filtration, still had pale pink glossy powder, sampling analysis look number 120 (platinum-cobalt method), other data are identical with embodiment 1.
Comparative Examples 2
Get the example 2 used flaxen ditrimethylolpropane 100g that have and add 200g dimethylbenzene washed twice in Glass Containers, obtain 98g by the method filtration drying of Comparative Examples 1 and have faint yellow glossy powder, sampling analysis purity: 96.80%, look number: No. 140, (platinum-cobalt method), fusing point: 107.2-110.5 ℃.Moisture 0.25%, hydroxyl value: 26.7%.
Claims (3)
1. the method for decolorizing and refining of a ditrimethylolpropane is characterized in that:
Take the ditrimethylolpropane that has color of organic solvent extractionprocess preparation, add ditrimethylolpropane weight 2-10 deionized water doubly, controlled temperature is 60～65 ℃, stirring and dissolving, and its mixing speed is 90～120 rev/mins; The gac that the dissolving back adds the 1-10% of ditrimethylolpropane weight carries out adsorption bleaching, continues to stir after 50～60 minutes, is cooled to 50～55 ℃ of filtrations, removes solid activated carbon, and the filtrate that obtains cools to-1～0 ℃ of crystallization, is incubated 180 minutes; With xln and mother liquor filtering separation, the xln that obtains white is put into vacuum drying oven in 80～85 ℃ of following oven dry 4～5 hours, obtains the ditrimethylolpropane powder of white again.
2. the method for decolorizing and refining of a kind of ditrimethylolpropane according to claim 1, it is characterized in that: the particle diameter of described micron order gac is 0.3～150 μ m.
3. the method for decolorizing and refining of a kind of ditrimethylolpropane according to claim 1 is characterized in that: used its aperture of filtering material of described filtration is≤0.3 μ m.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2006100990628A CN101108786B (en) | 2006-07-18 | 2006-07-18 | Method of decolorizing and refining double trimethylolpropane |
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| CN2006100990628A CN101108786B (en) | 2006-07-18 | 2006-07-18 | Method of decolorizing and refining double trimethylolpropane |
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| CN101108786A true CN101108786A (en) | 2008-01-23 |
| CN101108786B CN101108786B (en) | 2010-06-30 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550070B (en) * | 2008-12-30 | 2013-07-17 | 湖北三江化工有限责任公司 | Production process of ditrimethylolpropane |
| CN105732335A (en) * | 2016-04-18 | 2016-07-06 | 百川化工(如皋)有限公司 | Crystallization process of ditrimethylolpropane |
| CN109503325A (en) * | 2018-12-10 | 2019-03-22 | 安徽金禾实业股份有限公司 | A kind of method that pentaerythrite reduces coloration |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE468714B (en) * | 1990-09-24 | 1993-03-08 | Perstorp Ab | PROCEDURES FOR THE PREPARATION OF DITRIMETHYLOLPROPAN |
| JP3807514B2 (en) * | 1996-04-03 | 2006-08-09 | 三菱瓦斯化学株式会社 | Method for producing ditrimethylolpropane |
| EP1491521A1 (en) * | 2003-06-13 | 2004-12-29 | Mitsubishi Gas Chemical Company, Inc. | Method for producing ditrimethylolpropane |
-
2006
- 2006-07-18 CN CN2006100990628A patent/CN101108786B/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550070B (en) * | 2008-12-30 | 2013-07-17 | 湖北三江化工有限责任公司 | Production process of ditrimethylolpropane |
| CN105732335A (en) * | 2016-04-18 | 2016-07-06 | 百川化工(如皋)有限公司 | Crystallization process of ditrimethylolpropane |
| CN109503325A (en) * | 2018-12-10 | 2019-03-22 | 安徽金禾实业股份有限公司 | A kind of method that pentaerythrite reduces coloration |
| CN109503325B (en) * | 2018-12-10 | 2021-12-21 | 安徽金禾实业股份有限公司 | Method for reducing chroma of pentaerythritol |
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| CN101108786B (en) | 2010-06-30 |
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