CN1057052A - After-treatment of methyl glucoside - Google Patents
After-treatment of methyl glucoside Download PDFInfo
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- CN1057052A CN1057052A CN 90103843 CN90103843A CN1057052A CN 1057052 A CN1057052 A CN 1057052A CN 90103843 CN90103843 CN 90103843 CN 90103843 A CN90103843 A CN 90103843A CN 1057052 A CN1057052 A CN 1057052A
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Abstract
The aftertreatment technology of direct production methylglucoside in the presence of acid catalyst proposes three kinds of methods to starch and methyl alcohol, product yield is brought up to more than 90%, fusing point＞150 ℃, mother liquor obtains the application of various ways, improved plant factor, reduce the pollution of methyl alcohol, for applying of this product created favourable condition to environment.
Description
Methylglucoside (abbreviated as MEG) is that a kind of usefulness is coated with Organic Chemicals widely.Be mainly used in polyvalent alcohol, Synolac, tensio-active agent, tackiness agent and the thermosetting resin properties-correcting agent of producing polyurethane foaming body.
Methylglucoside is to produce in the presence of acid catalyst with glucose and methyl alcohol the earliest.Because the production cost height, the selling price height has limited applying of it.China Shanghai reagent two factories began production SILVER REAGENT methylglucoside in 1966, and enrolled the biochemical reagents handbook, were numbered 2663.
United States Patent (USP) 3,296 in 1967, and 246 reveal a kind of single stage method by starch direct production α-MEG, have caused the attention on chemical boundary.Arrived the seventies, U.S. Staley company, the existing production equipment of CPC Internalional Inc., product is also sold to Japan except that the U.S. uses.
China Shenyang petrochemical complex design and research institute, units such as Kuan Dianxian auxiliary reagent factory, Liaoning Province, Jiangsu Research Inst. of Chemical Industry and Liming chemical Inst of the Ministry of Chemical Industry have successively carried out the research work of alkyl glucose glucoside, and obtained very great achievement, but in producing, MEG also has some problems, The present invention be directed to these problems proposes, purpose is to improve product yield, fusing point and plant factor, solves problems such as mother liquor processing, methyl alcohol contaminate environment.According to foreign patent, not so difficult with starch and methyl alcohol this one of direct production MEG in the presence of an acidic catalyst, once through yield can reach about 40%, and problem is aftertreatment technology, and three kinds of aftertreatment technologys that the present invention proposes can address the above problem basically.These three kinds of aftertreatment technologys are:
(1) mother liquor after the primary first-order equation is carried out acid treatment under 60～160 ℃ of conditions, the gained material through filtration, concentrate, crystallization, separation, drying, obtain qualified product.Yield in kind with pure amylometer reaches more than 20%.
Because it is a more stable composition that the product that starch and methyl alcohol are produced in the presence of acid catalyst is formed.Wherein α-MEG accounts for about 60%, β-MEG accounts for about 30%, when after a part of α-the MEG Crystallization Separation is gone out, it is big that β-MEG accounts in the mother liquor ratio becomes, occur uneven, to this unbalanced mother liquor through as above acid treatment, can make a part of β-MEG change into α-MEG, and be separated, with primary first-order equation crystallization method ratio repeatedly, total recovery improves more than 20%.
A mother liquor new mother liquor can occur again after peracid treatment, be called secondary mother liquid.This secondary mother liquid through behind the activated carbon decolorizing, is recycled in the new batching, carries out recycle.This part cycle stock can effectively suppress the new generation of paying reaction, thereby makes the starch of adding mainly generate MEG.Secondary mother liquid can recycle more than five times, makes product yield more than 90%.
(2) mother liquor is neutralized with alkali, use the water vapor straight run distillation then, the methyl alcohol in the mother liquor is all steamed, generate the aqueous solution of MEG.This MEG aqueous solution is decoloured, filters, concentrates, be prepared into the solid component content and be 60% the aqueous solution, be used to produce phenolic aldehyde, urine aldehyde tackiness agent and polyether glycol.
Also mother liquor can be concentrated under 40～70 ℃ gradually, methyl alcohol is steamed, when overhead product seldom the time, carry out vacuum hydro-extraction, temperature rises gradually, when solid content is 75% when above, gets final product discharging to pallet, and naturally cooling is divided into 10 * 10 * 5 centimetres
3Fritter, packing is dispatched from the factory, and is used to do polyether glycol.This technology is fairly simple, has reduced the pollution of methyl alcohol to environment, and mother liquor is fully used, and the economic benefit height is applied easily.
(3) aqueous solution circulation crystallization process.With in the primary first-order equation liquid and after, with open steam distillation, methyl alcohol is all steamed, material becomes the MEG aqueous solution, again through decolouring, remove by filter impurity, and material is concentrated to 60～70%, then in crystallization below 15 ℃.The mother liquor of telling the crystallization product is recycled in the MEG aqueous solution that next still obtains with same manner, and the MEG concentration ratio in this solution is big for the first time, therefore, crystallization easily, it is many to obtain the crystallization product.Repeat the above-mentioned practice, the bigger aqueous solution of the MEG concentration of getting back, the separation of decrystallizing again can circulate more than ten times like this, and product yield is more than 90%, and good product quality does not have methyl alcohol to pollute.
In addition, the domestic production equipment that has, product yield has improved, but fusing point has descended again.The invention provides a kind of under higher yields, the technology that fusing point does not descend.The wet product that centrifugation soon obtains carries out the purified technology with low-carbon alcohol, makes product appearance very white on the one hand, and the product fusing point does not descend but then, all more than 150 ℃, can satisfy the needs of doing polyether glycol.
Claims (1)
- Three kinds of aftertreatment technologys of the present invention and wet product purification technology all can be used in industrial production, and patent right requires as follows:1, one of finishing process method of starch and methyl alcohol direct production MEG in the presence of acid catalyst carries out acid treatment with the mother liquor of primary first-order equation at 70 ℃～160 ℃, and product yield is increased more than 20%, then with the method for the mother liquid recycling of secondary reaction.2, a mother liquor is prepared into the MEG aqueous solution, is used to produce phenolic aldehyde, urine aldehyde tackiness agent, also a mother liquor can be prepared into the solid composition and be the block MEG more than 75%, be used to produce polyether glycol.3, MEG aqueous solution circulation crystallization process is prepared into the MEG aqueous solution with the primary first-order equation resultant, and crystallization then circulates.4, with the wet method of product purification of low-carbon alcohol, make product pure white, fusing point does not descend again, and yield is again than higher.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90103843 CN1057052A (en) | 1990-06-01 | 1990-06-01 | After-treatment of methyl glucoside |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90103843 CN1057052A (en) | 1990-06-01 | 1990-06-01 | After-treatment of methyl glucoside |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1057052A true CN1057052A (en) | 1991-12-18 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90103843 Pending CN1057052A (en) | 1990-06-01 | 1990-06-01 | After-treatment of methyl glucoside |
Country Status (1)
| Country | Link |
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| CN (1) | CN1057052A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104017033A (en) * | 2014-06-14 | 2014-09-03 | 济南卡博唐生物科技有限公司 | Method for preparing glucoside |
| CN104497063A (en) * | 2014-12-22 | 2015-04-08 | 中国林业科学研究院林产化学工业研究所 | Efficient catalytic and crystal habit control method for synthesis of methyl glucoside by woody fiber and starch |
| CN108690102A (en) * | 2018-03-23 | 2018-10-23 | 夏冶 | A kind of method of purification of methyl glucoside |
-
1990
- 1990-06-01 CN CN 90103843 patent/CN1057052A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104017033A (en) * | 2014-06-14 | 2014-09-03 | 济南卡博唐生物科技有限公司 | Method for preparing glucoside |
| CN104017033B (en) * | 2014-06-14 | 2016-08-17 | 济南尚博生物科技有限公司 | A kind of method preparing glucosides |
| CN104497063A (en) * | 2014-12-22 | 2015-04-08 | 中国林业科学研究院林产化学工业研究所 | Efficient catalytic and crystal habit control method for synthesis of methyl glucoside by woody fiber and starch |
| CN108690102A (en) * | 2018-03-23 | 2018-10-23 | 夏冶 | A kind of method of purification of methyl glucoside |
| CN108690102B (en) * | 2018-03-23 | 2020-08-25 | 浙江国盛源实业有限公司 | Method for purifying methyl glucoside |
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