CN101108785A - Method for extracting trimethylolpropane - Google Patents
Method for extracting trimethylolpropane Download PDFInfo
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- CN101108785A CN101108785A CNA2006100990632A CN200610099063A CN101108785A CN 101108785 A CN101108785 A CN 101108785A CN A2006100990632 A CNA2006100990632 A CN A2006100990632A CN 200610099063 A CN200610099063 A CN 200610099063A CN 101108785 A CN101108785 A CN 101108785A
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- trimethylolpropane
- ditrimethylolpropane
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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
The present invention relates to a kind of method of from the TriMethylolPropane(TMP) vinasse, extracting ditrimethylolpropane.
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, and the colored compound in the raffinate is extracted in the organic solvent, makes ditrimethylolpropane through technologies such as dissolving, crystallization, rectifying again.Yet, using a large amount of organic solvents, there is hidden danger simultaneously again in the energy that recycled consumption is a large amount of.In addition, organic solvent can't all remove the coloring matter in TriMethylolPropane(TMP) raffinate and the ditrimethylolpropane, 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.The vinasse that the TriMethylolPropane(TMP) production equipment produces, most of at home producers burn as low-grade fuel, cause the waste and the secondary pollution of resource.
Summary of the invention
The purpose of this invention is to provide and a kind ofly from the TriMethylolPropane(TMP) vinasse, obtain the method for ditrimethylolpropane, thereby solve problems such as organic solvent benzene series thing extracted products commonly used is still coloured, solvent recuperation power consumption height, contaminate environment with gac.
The objective of the invention is to be achieved by following technical scheme:
With TriMethylolPropane(TMP) vinasse deionized water dissolving, the consumption of deionized water is 2～10 times of raw material TriMethylolPropane(TMP) vinasse consumption weight, the dissolving back is under 45～75 ℃, adding shell class particle diameter is micron-sized gac, its consumption is 1～10% of a raw material TriMethylolPropane(TMP) vinasse consumption weight, stir and adsorbed in 30～120 minutes, filter with B then, the elimination gac, its filtrate cools to-5～1 ℃ of crystallizations, and keeps under this temperature 60～240 minutes; And then filter with xln and mother liquor separately with B, obtain flaxen xln ditrimethylolpropane crude product, collect mother liquor;
With the flaxen ditrimethylolpropane xln that obtains, with 1～10 times of its weight go dried up dissolving after, adding above-mentioned shell class particle diameter down at 30～90 ℃ is the micron order gac, and its consumption is 1～10% of a TriMethylolPropane(TMP) raffinate weight, stirs 30～120 minutes; Filter through B then, remove gac, its filtrate cools under-5～1 ℃ carries out crystallization, and after keeping 60～240 minutes under this temperature, filters with B xln is separated with mother liquor, reclaims mother liquor; Its xln obtains the ditrimethylolpropane product of white through dehydration, drying.
The specific surface area that described shell class particle diameter is the micron order gac is the 800-1200 meters squared per gram.
The particle diameter that described shell class particle diameter is the micron order gac is the 0.3-150 micron.
Described B filtering material eyelet≤0.3 μ m.
The weight ratio of total consumption of twice decolouring of described gac and raw material TriMethylolPropane(TMP) vinasse consumption is: 1～10: 100.
The present invention compared with prior art has significant technical progress and positive effect:
(1) the present invention with the TriMethylolPropane(TMP) vinasse with deionized water dissolving after, add the shell class, its particle diameter is that micron-sized gac is a sorbent material, through adsorption bleaching, filters post crystallization with B, then, successively xln is dissolved charcoal absorption decolouring, crystallization, filter, its resulting crystal drying or vacuum-drying can obtain white powdery or white plates ditrimethylolpropane purpose product.
(2) without benzene series things such as benzene, toluene and dimethylbenzene as extraction agent or solvent, thoroughly eradicated the pollution of benzene and homologue thereof; And save in a large number because of being used for the energy that organic extractant and Recovery of Organic Solvent consume, real realization non-harmful friendly process process in the production process.
(3) the finished product of the present invention, its weight hydroxy 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. 15.
(4) resulting mother liquor can circulate as raw material TriMethylolPropane(TMP) vinasse dissolved solvent after secondary crystal of the present invention filtered.
(5) the once filtering mother liquor of the present invention can reclaim weight percentage in the TriMethylolPropane(TMP) vinasse and be 80～90% TriMethylolPropane(TMP), can obtain technical grade product through rectifying.
The used shell class particle diameter of the present invention is that 0.3～150 micron acticarbon is bought from the market.
Embodiment
Embodiment 1
(1) gets 100g TriMethylolPropane(TMP) vinasse (wherein ditrimethylolpropane content is about 40wt%), add the 300g deionized water, stirring and dissolving is after 90 minutes under 60 ± 10 ℃ of conditions, adding 2.5g shell class particle diameter is the micron order gac of 0.3-150 micron, stir 30 minutes adsorption bleachings, under said temperature, filter (filtering material eyelet≤0.3 μ m then with B, as follows), the described gac of elimination, its filtrate is carried out decrease temperature crystalline, being cooled to 0 ± 5 ℃ keeps after 280 minutes down, with the B filtration crystallization and filtrate are separated, obtain the flaxen thick ditrimethylolpropane xln that 72.5g contains certain moisture, reclaim its filtrate;
(2) dissolve adding the 145g deionized water in the above-mentioned 72.5g xln that makes, 60 ± 5 ℃ of condition stirring and dissolving 85 minutes, add the above-mentioned gac of 3.2g then, restir 65 minutes, under said temperature, remove by filter the coloring matter of described gac and absorption with B, filtrate is cooled to 0 ± 5 ℃ of following crystallization, and under this temperature, kept 200 minutes, obtain solid crystal and liquid mixture, filter with B again and obtain the white crystals body, put into baking oven, oven dry is 6 hours under 85 ℃ of conditions of temperature, obtains the powder-like product ditrimethylolpropane 38g of white, chromatograph purity 〉=96% (wt%).Measure moisture≤0.2% (wt%) with the karl Fischer method, measuring fusing point with capillary tube technique is 107～110 ℃, use the chemical titration hydroxyl value, and its weight percentage is 26.7%, number is No. 15 with Pt-Co method mensuration look.
Embodiment 2
Technological process and processing condition by the foregoing description 1 are operated, wherein, the consumption of described shell class micron order gac is on the basis of original consumption, step (1) and step (2) respectively increase 1g respectively, and (step 1 activated carbon dosage is 3.5g, step 2 activated carbon dosage is 4.2g), the ditrimethylolpropane that obtains, its look number drops to No. 10, other index is constant (as seen, when described activated carbon dosage increases, help decolouring, the product look number is No. 10).
Embodiment 3
(1) take by weighing 100g TriMethylolPropane(TMP) vinasse, add the 280g deionized water, dissolving is 90 minutes under 60 ± 10 ℃ of stirrings.Adding the described particle diameter of 2.8g then is the gac of 0.3-150 micron, stir decolouring 30 minutes, under said temperature, described gac is removed with described B filtration, resulting filtrate drops to 0 ± 5 ℃ and carries out crystallization, and keeps 240 minutes under this temperature, uses then, B is filtered, xln and solution separating obtain the flaxen ditrimethylolpropane xln that 71.2g contains certain moisture, reclaim its mother liquor;
(2) with in the resulting 71.2g xln, adding the 148g deionized water dissolves, 60 ± 5 ℃ of stirring and dissolving 85 minutes, add the described gac of 3.2g then, restir carried out adsorption bleaching in 65 minutes, under said temperature, remove the coloring matter of described gac and absorption thereof with millipore filtration, filtrate is cooled to 0 ± 5 ℃ of following crystallization, under this temperature, kept 180 minutes, obtain solid crystal and liquid mixture, filter its separation with B again, obtain the white crystals body, put into baking oven, baking is 6 hours under 85 ℃ of conditions of temperature, obtains the Powdered ditrimethylolpropane product of 41.3g white, chromatograph purity 〉=96% (wt%).Measure moisture≤0.25% (wt%) with the karl Fischer method, measuring fusing point with capillary tube technique is 107-110.5 ℃, is 26.75% (wt%) with the chemical titration hydroxyl value, number is No. 10 with Pt-Co method mensuration look.
Embodiment 4
(1) takes by weighing 100g TriMethylolPropane(TMP) vinasse, add the 400g deionized water and dissolve, 60 ± 10 ℃ of stirring and dissolving 90 minutes.Add the described gac of 3.0g then, adsorption bleaching is 30 minutes under stirring, then under said temperature, remove by filter described gac with B, resulting filtrate is cooled to 0 ± 5 ℃ of crystallization, and under this temperature, kept 240 minutes, filter with B then and obtain the flaxen ditrimethylolpropane xln that 72.8g contains certain moisture.
(2) adding the 150g deionized water in the 72.8g xln that obtains dissolves, stirred 85 minutes 60 ± 5 ℃ of conditions, add the described gac of 3.2g then and carry out adsorption bleaching, restir 65 minutes, under said temperature, remove by filter the coloring matter of described gac and absorption through B, filtrate is cooled to 0 ± 5 ℃ of crystallization, and under this temperature, kept 200 minutes, obtain solid crystal and liquid mixture, obtain the white crystals body with the B filtration, put into baking oven, baking is 8 hours under 85 ℃ of conditions of temperature, obtain the Powdered ditrimethylolpropane product of white, chromatograph purity 〉=96% (wt%).Measure moisture≤0.15% (wt%) with the karl Fischer method, measuring fusing point with capillary tube technique is 107～110 ℃, be 26.7% (wt%) with Pt-Co method mensuration look with the chemical titration hydroxyl value number is No. 15.Its secondary filtrate is returned the solvent of step (1) as described raw material.
Embodiment 5-9 (seeing following table for details)
| Sequence number | Activated carbon dosage | Solvent load | Working method | Operational condition | Quality product |
| Example 5 | 2g | 600g | With embodiment 1 | With embodiment 1 | Look numbers No. 25, other are with embodiment 1 |
| Example 6 | 8g | 1000g | With embodiment 1 | With embodiment 1 | Numbers No. 5 other are with embodiment 1 for look |
| Example 7 | 10g | 500g | With embodiment 1 | With embodiment 1 | Look numbers No. 5, other are with embodiment 1 |
| Embodiment 8 | 6g | 900g | With embodiment 1 | With embodiment 1 | Numbers No. 10 other are with embodiment 1 for look |
| Example 9 | 5g | 450g | With embodiment 1 | With embodiment 1 | Numbers No. 15 other are with embodiment 1 for look |
Comparative Examples 1: the preparation of ditrimethylolpropane
Get 100g TriMethylolPropane(TMP) vinasse and add the 300g deionized water, stirring and dissolving is 90 minutes under 50 ± 5 ℃ of temperature, add 350g toluene, in the glass there-necked flask, stir extraction 40 minutes, said mixture was joined in the glass separating funnel of 500ml static layering 60 minutes, sharp interface and cotton-shaped filtering layer appear, upper organic phase is a light brown, lower floor's water is yellow, open shunting funnel bottom valve, water is put into the dimethylbenzene washing that glass beaker adds equal proportion, static layering, water intaking phase decrease temperature crystalline, undertaken by the embodiment of the invention 1 processing condition: the mixture that obtains yellow crystal body and mother liquor, after filtering, B obtains 70.2g yellow crystal body, above-mentioned xln is added the 150g deionized water to be dissolved, add with the isopyknic dimethylbenzene of lysate again and carry out reextraction, washing, the xln that obtains having pale pink is filtered in crystallization, put into vacuum drying oven dry 360 minutes, obtain having the powder of lightpink 41g, measure look with the Pt-Co method numbers No. 200, other index is identical with resulting index among the embodiment 1.
Comparative Examples 2:
Repeat the operation of Comparative Examples 1, with the powder that has pale pink that obtains, after the dimethylbenzene washed twice with 2 times of weights of described pale pink powder weight, its powder still is faint yellow, measure look with the Pt-Co method, other index is identical with resulting index among the embodiment 1 numbers No. 200.
Comparative Examples 3:
To having in the flaxen powder that Comparative Examples 2 obtains, the deionized water that adds its 3 times of weight, dissolved 30 minutes, add 3% above-mentioned gac 58 ℃ of conditions, adsorption bleaching is 30 minutes under stirring, and filters with B and removes gac, with the filtrate crystallization, press the conditional operation of embodiment 1, obtain white powder 36.5g, every index has reached the level of embodiment 1.
Claims (5)
1. method of extracting ditrimethylolpropane is characterized in that:
With TriMethylolPropane(TMP) vinasse deionized water dissolving, the consumption of deionized water is 2～10 times of raw material TriMethylolPropane(TMP) vinasse consumption weight, the dissolving back is under 45～75 ℃, adding shell class particle diameter is micron-sized gac, its consumption is 1～10% of a raw material TriMethylolPropane(TMP) vinasse consumption weight, stir and adsorbed in 30～120 minutes, filter with B then, the elimination gac, its filtrate cools to-5～1 ℃ of crystallizations, and keeps under this temperature 60～240 minutes; And then filter with xln and mother liquor separately with B, obtain flaxen xln ditrimethylolpropane crude product, collect mother liquor;
With the flaxen ditrimethylolpropane xln that obtains, with 1～10 times of its weight go dried up dissolving after, adding above-mentioned shell class particle diameter down at 30～90 ℃ is the micron order gac, and its consumption is 1～10% of a TriMethylolPropane(TMP) raffinate weight, stirs 30～120 minutes; Remove by filter gac through B then, its filtrate cools under-5～1 ℃ carries out crystallization, and after keeping 60～240 minutes under this temperature, filters with B xln is separated with mother liquor, reclaims mother liquor; Its xln obtains the ditrimethylolpropane product of white through dehydration, drying.
2. a kind of method of extracting ditrimethylolpropane according to claim 1 is characterized in that: the specific surface area of described shell class micron order gac is the 800-1200 meters squared per gram.
3. a kind of method of extracting ditrimethylolpropane according to claim 1 is characterized in that: the particle diameter of described shell class micron order gac is 0.3～150 micron.
4. a kind of method of extracting ditrimethylolpropane according to claim 1 is characterized in that: the weight ratio of total consumption of twice decolouring of described gac and raw material TriMethylolPropane(TMP) vinasse consumption is: 1～10: 100.
5. a kind of method of extracting ditrimethylolpropane according to claim 1 is characterized in that: filtering material eyelet≤0.3 μ m that cloth formula funnel is used.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100990632A CN100548953C (en) | 2006-07-18 | 2006-07-18 | A kind of method of extracting ditrimethylolpropane |
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| CNB2006100990632A CN100548953C (en) | 2006-07-18 | 2006-07-18 | A kind of method of extracting ditrimethylolpropane |
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| CN101108785A true CN101108785A (en) | 2008-01-23 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011530567A (en) * | 2008-08-16 | 2011-12-22 | ランクセス・ドイチュランド・ゲーエムベーハー | Method for isolating ditrimethylolpropane |
| CN101550070B (en) * | 2008-12-30 | 2013-07-17 | 湖北三江化工有限责任公司 | Production process of ditrimethylolpropane |
| CN108675919A (en) * | 2018-06-25 | 2018-10-19 | 南通百川新材料有限公司 | A kind of method that double trimethylolpropane is extracted in trimethylolpropane heavy constituent |
| CN109485554A (en) * | 2018-11-27 | 2019-03-19 | 濮阳市永安化工有限公司 | The method of double trimethylolpropane is isolated from trimethylolpropane heavy constituent |
-
2006
- 2006-07-18 CN CNB2006100990632A patent/CN100548953C/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011530567A (en) * | 2008-08-16 | 2011-12-22 | ランクセス・ドイチュランド・ゲーエムベーハー | Method for isolating ditrimethylolpropane |
| CN101550070B (en) * | 2008-12-30 | 2013-07-17 | 湖北三江化工有限责任公司 | Production process of ditrimethylolpropane |
| CN108675919A (en) * | 2018-06-25 | 2018-10-19 | 南通百川新材料有限公司 | A kind of method that double trimethylolpropane is extracted in trimethylolpropane heavy constituent |
| CN109485554A (en) * | 2018-11-27 | 2019-03-19 | 濮阳市永安化工有限公司 | The method of double trimethylolpropane is isolated from trimethylolpropane heavy constituent |
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| CN100548953C (en) | 2009-10-14 |
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