CN101475444B - Partial dehydration and purification process for crude glycerine - Google Patents

Partial dehydration and purification process for crude glycerine Download PDF

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Publication number
CN101475444B
CN101475444B CN2009100369462A CN200910036946A CN101475444B CN 101475444 B CN101475444 B CN 101475444B CN 2009100369462 A CN2009100369462 A CN 2009100369462A CN 200910036946 A CN200910036946 A CN 200910036946A CN 101475444 B CN101475444 B CN 101475444B
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China
Prior art keywords
glycerol
glycerine
percent
purity
purification process
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Expired - Fee Related
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CN2009100369462A
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Chinese (zh)
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CN101475444A (en
Inventor
余建
孙宁
贾长生
姜少华
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JIANGMEN HONGJIE FINE CHEMICAL INDUSTRY Co Ltd
Wuyi University
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JIANGMEN HONGJIE FINE CHEMICAL INDUSTRY Co Ltd
Wuyi University
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Abstract

The invention relates to a method for purifying crude glycerol, in particular to a method for purifying crude glycerol derived from biodiesel production. The method mainly comprises the steps of removing moisture in glycerol and raising the purity of the glycerol. The method is characterized in that the crude glycerol is filtered to remove solid impurities and then is evaporated to remove 50 to 100 percent of moisture and 80 to 100 percent of methanol; the glycerol enters an ion exchange column for exchange; water accounting for 5 to 20 percent of the mass of the glycerol is added for adjusting viscosity; effluent liquid is collected at the same time; and the effluent liquid is subjected to thin-film distillation, so the glycerol with the purity of more than 95 percent is obtained. The method first removes partial water so as to lower the material flow in a dehydration follow-up process, reduce equipment size and save equipment investment, simultaneously removes most of salts and inorganic water-soluble substances, reduces the pressure of follow-up ion exchange, and is favorable for obtaining high-purity glycerol.

Description

Partial dehydration and purification process for crude glycerine
One, technical field
The present invention relates to a kind of purification process of raw glycerine, be specifically related to be derived from the purification process of the raw glycerine of production of biodiesel, mainly is the moisture in the deglycerizin, improves the purity of glycerine.
Two, background technology
Biofuel lower floor by-product glycerin content is about 45%, and methanol content is about 28%, and fatty acid soaps content also contains a small amount of grease, free alkali etc. in addition about 22%.Because the used oil lipid species is different, biofuel lower floor by product shade differs, and various component concentrations also have difference.The difficulty of recovery, refining glycerine is bigger from biofuel lower floor by product.On the other hand, high purity glycerine is a kind of very important industrial raw material, in industry such as food, medicine, makeup and tobacco, is widely used.Usually, operations such as the raw glycerine purge process will be passed through filtration, concentrated, chemicaladditives, distillation if be used in fields such as food, makeup, medicine, also need further to handle.China's glycerine is in the situation that supply falls short of demand always, and especially highly purified glycerine (glycerol content is more than 99.5%) such as food grade, medical grade, cosmetics-stage almost all rely on import.
The traditional glycerol purification process mainly contains two kinds of underpressure distillation and IXs.The distillation under vacuum main drawback is that vacuum tightness is high, and energy consumption is big, and simultaneous temperature is still too high, and the easy polymerization of still liquid glycerine produces side reaction, influences purity, color and luster and the yield of glycerine; And in vacuum distillation process along with the continuous gasification of glycerine; Remaining organic impurity constantly concentrates, coking; Finally cause glycerine to be wrapped in interior can't the gasification; Tightly cohere with distillation wall and heating coil after the remaining organic impurity coking, not only reduced distillation yield, and the residue after the coking is removed comparatively difficulty.Ion exchange method has important utilization in glycerine production, major part is edible, medical glycerine all is to obtain through ion exchange resin is refining at last.
Three, summary of the invention
A kind of partial dehydration and purification process for crude glycerine that the objective of the invention is to be directed against the deficiency of prior art and provide, it is simple to operate, and equipment requirements is low, saves facility investment greatly, and product purity is high.
The concrete technical scheme that realizes the object of the invention is:
A kind of partial dehydration and purification process for crude glycerine; It is characterized in that: with the quantity of methyl alcohol of evaporating, remove part moisture in it and 80%~100% behind the raw glycerine solids removed by filtration impurity earlier; Again glycerine is got in the ion exchange column and exchange, carry out the adjustment dilution of amount of water, collect effluent simultaneously according to the viscosity of glycerine; Again to the effluent thin film distillation, promptly get purity greater than 95% glycerine.
Described partial dehydration and purification process for crude glycerine is characterized in that the described moisture that evaporates earlier, removes in it is 50%~100%.
Described partial dehydration and purification process for crude glycerine is characterized in that described is 5%~20% of qualities of glycerin through adding the adding water yield that water carries out the viscosity adjustment of glycerine.
The invention has the beneficial effects as follows, at first portion water is removed in the raw glycerine purifying process that make that the mass flow in the dehydration subsequent technique reduces, the size of equipment reduces, and saves facility investment; Remove most of salinities and inorganic water-soluble substances simultaneously, reduce the pressure of follow-up IX, help obtaining highly purified glycerine.
Four, embodiment
Embodiment one:
Partial dehydration and purification process for crude glycerine of the present invention; It is characterized in that: with the quantity of methyl alcohol of evaporating, remove its interior 50% moisture and 80%~100% behind the raw glycerine solids removed by filtration impurity earlier; Again glycerine is got in the ion exchange column and exchange; Carry out the adjustment dilution of amount of water according to the viscosity of glycerine, adding the water yield is 5% of qualities of glycerin.Collect effluent simultaneously,, promptly get purity greater than 95% glycerine again to the effluent thin film distillation.
Embodiment two:
Partial dehydration and purification process for crude glycerine of the present invention; It is characterized in that: with the quantity of methyl alcohol of evaporating, remove its interior 70% moisture and 80%~100% behind the raw glycerine solids removed by filtration impurity earlier; Again glycerine is got in the ion exchange column and exchange; Carry out the adjustment dilution of amount of water according to the viscosity of glycerine, adding the water yield is 10% of qualities of glycerin.Collect effluent simultaneously,, promptly get purity greater than 95% glycerine again to the effluent thin film distillation.
Embodiment three:
Partial dehydration and purification process for crude glycerine of the present invention; It is characterized in that: with the quantity of methyl alcohol of evaporating, remove its interior 90% moisture and 80%~100% behind the raw glycerine solids removed by filtration impurity earlier; Again glycerine is got in the ion exchange column and exchange; Carry out the adjustment dilution of amount of water according to the viscosity of glycerine, adding the water yield is 15% of qualities of glycerin.Collect effluent simultaneously,, promptly get purity greater than 95% glycerine again to the effluent thin film distillation.

Claims (1)

1. partial dehydration and purification process for crude glycerine; It is characterized in that: with the quantity of methyl alcohol of evaporating, remove its interior 50%~100% moisture and 80%~100% behind the raw glycerine solids removed by filtration impurity earlier; Again glycerine is got in the ion exchange column and exchange; Carry out the adjustment dilution of amount of water according to the viscosity of glycerine, adding the water yield is 5%~20% of qualities of glycerin; Collect effluent simultaneously,, promptly get purity greater than 95% glycerine again to the effluent thin film distillation.
CN2009100369462A 2009-01-22 2009-01-22 Partial dehydration and purification process for crude glycerine Expired - Fee Related CN101475444B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2009100369462A CN101475444B (en) 2009-01-22 2009-01-22 Partial dehydration and purification process for crude glycerine

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Application Number Priority Date Filing Date Title
CN2009100369462A CN101475444B (en) 2009-01-22 2009-01-22 Partial dehydration and purification process for crude glycerine

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CN101475444A CN101475444A (en) 2009-07-08
CN101475444B true CN101475444B (en) 2012-05-30

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Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102229521B (en) * 2011-05-14 2013-11-06 江门市鸿捷精细化工有限公司 Process for refining crude glycerin and recovering byproducts
FR3002936B1 (en) 2013-03-06 2015-03-06 Arkema France USE OF SULFONIC ACID FOR THE RECOVERY OF GLYCEROL RESULTING FROM TRIGLYCERIDE TRANS-ESTERIFICATION REACTION
CN103965019B (en) * 2014-04-04 2016-07-13 天长市康宁塑胶科技有限公司 A kind of purifying production process of glycerol
CN104447201B (en) * 2014-11-11 2017-05-10 上海中华药业南通有限公司 Glycerol production device and glycerol production process

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101265160A (en) * 2008-04-30 2008-09-17 上海三瑞高分子材料有限公司 Method for purifying biological diesel oil byproduct glycerin

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101265160A (en) * 2008-04-30 2008-09-17 上海三瑞高分子材料有限公司 Method for purifying biological diesel oil byproduct glycerin

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈铭.发酵甘油的制备、提取与纯化.《日用化学工业》.1999,(第6期), *

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