CN103849306B - A kind of method fully utilizing BDO distillation substrate - Google Patents
A kind of method fully utilizing BDO distillation substrate Download PDFInfo
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- CN103849306B CN103849306B CN201310297096.8A CN201310297096A CN103849306B CN 103849306 B CN103849306 B CN 103849306B CN 201310297096 A CN201310297096 A CN 201310297096A CN 103849306 B CN103849306 B CN 103849306B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
Abstract
Fully utilize a method for BDO distillation substrate, be specifically related to the method fully utilizing BDO distillation substrate.The present invention distills substrate for raw material, first by 1 with BDO, 4-butyleneglycol distillation substrate dilutes, and prepares diluent, then carries out classification ultrafiltration, finally carry out crosslinking reaction, prepare the degradable coating of alcohol ether oligomer spray-dried powders and alcohol ether oligomer.The features such as the present invention has preparation condition gentleness, operation steps is simple, product purity is high, comprehensive resource utilization rate is high, environment friendly and pollution-free.The alcohol ether oligomer spray-dried powders that the present invention can prepare can be used as plastic plasticizer, manufactures the raw material of resin and manufacture frostproofer etc., and the alcohol ether oligomer coating prepared can be used for brushing buildings, metal material surface, plays etch-proof effect.
Description
One, technical field
The invention belongs to chemical byproduct technical field of comprehensive utilization, be specifically related to the method fully utilizing BDO distillation substrate.
Two, background technology
BDO has another name called Isosorbide-5-Nitrae-dihydroxyl butane, butylen glycol, tetramethylene glycol, and English name is Isosorbide-5-Nitrae-putyleneglycol, is called for short BDO.BDO is oily liquids that is colourless, odorless more than 20 DEG C, flammable, can dissolve each other, dissolve in methyl alcohol, ethanol, acetone, be slightly soluble in ether, boiling point 235 DEG C, fusing point 20.2 DEG C with water and ethanol.BDO is widely used in and produces the important Chemicals such as tetrahydrofuran (THF), gamma-butyrolactone, polybutylene terephthalate and urethane, also can be used as chain propagation agent in the synthesis of solvent, moistening agent, softening agent and urethane and linking agent etc.
The method of current production BDO has Reppe method, normal butane/cis-butenedioic anhydride method, butadiene process and propylene oxide method etc., wherein to improve Reppe method.The refining stage of BDO technique is produced in improvement Reppe method, scraped film evaporator is used to distill thick BDO, under the high temperature, condition of high vacuum degree condition of scraped film evaporator, there is autohemagglutination in part BDO, namely 1, the intermolecular dehydration of 4-butyleneglycol forms alcohol ether oligomer, and this oligopolymer difficulty volatilization, is formed and scrape membrane distillation substrate.Produce the BDO production line of 60,000 tons per year for one according to statistics, distillation substrate reaches 400 kgs/hour.Wang Yujia etc. publish thesis " 1; the analytical procedure of 4-butyleneglycol distillation substrate depolymerization solution composition " in " applied chemistry " the 2nd phase in 2012, point out that the main component of this substrate is the water-soluble alcohol ether oligomer that the intermolecular dehydration of BDO is formed, viscosity-average molecular weight is 300 ~ 1500Da.As can be seen here, BDO distills substrate is a kind of raw material having DEVELOPMENT PROSPECT.At present, the major way processing this substrate is for burning, and not only caused the wasting of resources but also contaminate environment, therefore, research and development effectively utilize the method for distillation substrate, have important value.
The exploitation of substrate are distilled about BDO, the paper " 1; recovery process of 4-butyleneglycol distillation substrate " delivered in " University Of Chongqing's journal " the 3rd phase in 2012 along people such as peaces current rarely seen Wei, this article proposes: propose under an increased pressure, take dilute sulphuric acid as catalyzer, be hydrolyzed to process to this substrate and reclaim BDO and the technological process reducing waste discharge.Optimal technique process is: sulfuric acid massfraction is 15%, and dilute sulphuric acid and substrate mass ratio are 1.3: 1.0, and temperature of reaction is 150 DEG C, and the reaction times is that the rate of recovery of 7h, BDO can reach 39.1%.The main drawback of this technique is: efficiency is low, and working concentration is hydrolyzed 6 hours up to the dilute sulphuric acid of 15% at 150 DEG C, only obtains the BOD of 39.1%; Produce new source of pollution dilute sulphuric acid waste liquid, need purifying treatment be carried out.
Three, summary of the invention
The object of the invention is, for the weak point of existing BDO distillation substrate recoverying and utilizing method, to provide a kind of method fully utilizing BDO distillation substrate.The present invention can prepare based on alcohol ether oligomer degradable coating and can be used as plastic plasticizer, manufacture the raw material of resin and manufacture the alcohol ether oligomer spray-dried powders of frostproofer etc., and there is preparation condition gentleness, operation steps is simple, product purity is high, comprehensive resource utilization rate is high, the feature such as environment friendly and pollution-free.
Mechanism of the present invention is: BDO distillation substrate is mainly containing water-soluble alcohol ether oligomer, and alcohol ether oligomer is the etherate formed that to dewater between BDO molecule.Due to the difference of the polymerization degree, cause its molecular weight different, and the molecular diameter of different molecular weight compound there are differences, therefore, through when determining the ultra-filtration membrane in aperture, the material that molecular diameter is greater than this ultra-filtration membrane bore dia is trapped, the material that molecular diameter is less than this ultra-filtration membrane bore dia then through, so the fractional separation between the water-soluble alcohol ether oligomer just achieving certain molecular weight difference.
Ehter bond is also known as glycosidic link in biological chemistry, and by Glycosylase hydrolysis, alcohol ether oligomer is connected by ehter bond, therefore, belongs to biodegradable chemical bond; Epoxy silane crosslinker contains epoxy group(ing) and alkoxysilane groups, and with the hydroxyl reaction in water-soluble alcohol ether oligomer, can form netted etherate, this etherate can effectively be attached on base material, so just prepare the degradable coating for the protection of base material.
Realizing technical scheme of the present invention is: a kind of comprehensive utilization 1, the method of 4-butyleneglycol distillation substrate, with 1,4-butyleneglycol distillation substrate is raw material, first BDO is distilled substrate and dilutes, prepare diluent, carry out classification ultrafiltration again, finally carry out crosslinking reaction, prepare the degradable coating based on alcohol ether oligomer.The concrete steps of described method are as follows:
(1) alcohol ether oligomer diluent is prepared
According to 1,4-butyleneglycol distillation substrate: the volume ratio of distilled water is the ratio of 1L: 5 ~ 10L, first to 1, add distilled water in 4-butyleneglycol distillation substrate, under agitation make BDO distill substrate and dissolve completely, then filter, collect filtrate and abandon filter residue, filtrate is alcohol ether oligomer diluent, prepares ultrafiltration fractional separation liquid for next step.
(2) ultrafiltration fractional separation liquid is prepared
After (1) step completes, the alcohol ether oligomer diluting pump (1) step prepared enters in ultra-fine filter, control ultrafiltration pressure is 0.05 ~ 0.2MPa, first time ultrafiltration fractional separation is carried out, until when ultra-filter retentate volume is 1/5 ~ 1/9 of carbinol ether oligomer diluent volume only with the ultra-filtration membrane that molecular weight cut-off is 2000 ~ 5000Da.Collect ultrafiltration filtered solution and ultra-filter retentate for the first time respectively, for the first time ultrafiltration filtered solution collected, for further ion-exchange, to reclaim catalyzer; For the first time ultra-filter retentate collected, add distilled water, volume is made to return to carbinol ether oligomer diluent volume, second time ultrafiltration fractional separation is carried out again after stirring, the ultra-filtration membrane molecular weight cut-off that second time fractional separation uses is 10000 ~ 50000Da, and ultrafiltration pressure is 0.05 ~ 0.2MPa.When ultra-filter retentate volume be reduced to the alcohol ether oligomer diluted liquid that pumps into long-pending 1/5 ~ 1/9 time, stop ultrafiltration, collect second time ultrafiltration filtered solution and ultra-filter retentate respectively.Second time ultrafiltration filtered solution is ultrafiltration classification filtered solution, prepares alcohol ether oligomer spray-dried powders for next step; Second time ultra-filter retentate is ultrafiltration classification trapped fluid, prepares alcohol ether oligomer coating for next step.
(3) alcohol ether oligomer spray-dried powders is prepared
After (2) step completes, the ultrafiltration classification filtered solution (2) step prepared is pumped in counter-osmosis device, control pressure is 0.1 ~ 0.5MPa, carries out reverse osmosis concentration, until reverse osmosis trapped fluid volume is 1/8 ~ 1/10 of former ultrafiltration classification filtered solution volume.Collect reverse osmosis filtered solution and reverse osmosis concentrated liquid respectively, for the reverse osmosis filtered solution collected, for the preparation of lower batch of alcohol ether oligomer diluent; For the reverse osmosis concentrated liquid collected, pump in spray-drier, temperature be 150 ~ 180 DEG C, rotating speed carries out spraying dry under being the condition of 5000 ~ 10000r/min, just prepares alcohol ether oligomer spray-dried powders.This powder can be used as plastic plasticizer, manufactures the raw material of resin and manufacture frostproofer etc.
(4) alcohol ether oligomer coating is prepared
After (2) step completes, according to dehydrated alcohol: the volume ratio of ultrafiltration classification trapped fluid is the ratio of 1L: 4 ~ 7L, under agitation dehydrated alcohol is joined in compounding kettle, after stirring, the ratio being 1L: 50 ~ 80L according to linking agent XR-500 or silane resin acceptor kh-550 or silane coupling A-151 and ultra-filter retentate volume ratio adds linking agent XR-500 or silane resin acceptor kh-550 or silane coupling A-151, under agitation carry out process 15 ~ 60 minutes, then just prepare alcohol ether oligomer coating; Can be used for brushing buildings, metal material surface, play etch-proof effect.
After the present invention adopts technique scheme, mainly contain following effect:
(1) the present invention in process of production, ultrafiltration process is adopted to carry out fractional separation to alcohol ether oligomer, obtain the first time ultrafiltration filtered solution that can be used for reclaiming catalyzer respectively, the raw material prepare and can be used as plastic plasticizer, manufacturing resin and manufacture the second time ultrafiltration filtered solution of alcohol ether oligomer spray-dried powders of frostproofer etc., and for the preparation of the second time ultra-filter retentate of alcohol ether oligomer coating.Achieve whole recyclings of alcohol ether oligomer.Thus improve production efficiency, reduce product cost, save energy, is conducive to Sustainable development.
(2) the present invention is in process of production, mainly use ultrafiltration, reverse osmosis, spraying dry etc. be easy to buy equipment, production unit is general, working specification and be easy to control, therefore production safety reduces production cost again.
(3) the present invention in process of production, do not use poisonous and harmful reagent and achieve whole recyclings of alcohol ether oligomer, without " three wastes " discharge, also makes full use of resource.
(4) excellent property of product that obtains of the present invention, raw materials such as alternative ethylene glycol or can priming paint etc.
Four, embodiment
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment 1
(1) alcohol ether oligomer diluent is prepared
According to 1,4-butyleneglycol distillation substrate: the volume ratio of distilled water is the ratio of 1L: 7L, first to 1, add distilled water in 4-butyleneglycol distillation substrate, under agitation make BDO distill substrate and dissolve completely, then filter, collect filtrate and abandon filter residue, filtrate is alcohol ether oligomer diluent, prepares ultrafiltration fractional separation liquid for next step.
(2) ultrafiltration fractional separation liquid is prepared
After (1) step completes, the alcohol ether oligomer diluting pump (1) step prepared enters in ultra-fine filter, control ultrafiltration pressure is 0.1MPa, first time ultrafiltration fractional separation is carried out, until when ultra-filter retentate volume is 1/7 of carbinol ether oligomer diluent volume only with the ultra-filtration membrane that molecular weight cut-off is 3000Da.Collect ultrafiltration filtered solution and ultra-filter retentate for the first time respectively, for the first time ultrafiltration filtered solution collected, for further ion-exchange, to reclaim catalyzer; For the first time ultra-filter retentate collected, add distilled water, make volume return to carbinol ether oligomer diluent volume, after stirring, carry out second time ultrafiltration fractional separation again, the ultra-filtration membrane molecular weight cut-off that second time fractional separation uses is 30000Da, and ultrafiltration pressure is 0.1MPa.When ultra-filter retentate volume be reduced to the alcohol ether oligomer diluted liquid that pumps into long-pending 1/7 time, stop ultrafiltration, collect second time ultrafiltration filtered solution and ultra-filter retentate respectively.Second time ultrafiltration filtered solution is ultrafiltration classification filtered solution, prepares alcohol ether oligomer spray-dried powders for next step; Second time ultra-filter retentate is ultrafiltration classification trapped fluid, prepares alcohol ether oligomer coating for next step.
(3) alcohol ether oligomer spray-dried powders is prepared
After (2) step completes, the ultrafiltration classification filtered solution (2) step prepared is pumped in counter-osmosis device, and control pressure is 0.3MPa, carries out reverse osmosis concentration, until reverse osmosis trapped fluid volume is 1/9 of former ultrafiltration classification filtered solution volume.Collect reverse osmosis filtered solution and reverse osmosis concentrated liquid respectively, for the reverse osmosis filtered solution collected, for the preparation of lower batch of alcohol ether oligomer diluent; For the reverse osmosis concentrated liquid collected, pump in spray-drier, temperature be 165 DEG C, rotating speed carries out spraying dry under being the condition of 8000r/min, just prepares alcohol ether oligomer spray-dried powders.This powder can be used as plastic plasticizer, manufactures the raw material of resin and manufacture frostproofer etc.
(4) alcohol ether oligomer coating is prepared
After (2) step completes, according to dehydrated alcohol: the volume ratio of ultrafiltration classification trapped fluid is the ratio of 1L: 6L, under agitation dehydrated alcohol is joined in compounding kettle, after stirring, the ratio being 1L: 65L according to linking agent XR-500 and ultra-filter retentate volume ratio adds linking agent XR-500, under agitation carries out process 40 minutes, then just prepares alcohol ether oligomer coating, can be used for brushing buildings, metal material surface, play etch-proof effect.
Embodiment 2
(1) alcohol ether oligomer diluent is prepared
According to 1,4-butyleneglycol distillation substrate: the volume ratio of distilled water is the ratio of 1L: 5L, first to 1, add distilled water in 4-butyleneglycol distillation substrate, under agitation make BDO distill substrate and dissolve completely, then filter, collect filtrate and abandon filter residue, filtrate is alcohol ether oligomer diluent, prepares ultrafiltration fractional separation liquid for next step.
(2) ultrafiltration fractional separation liquid is prepared
After (1) step completes, the alcohol ether oligomer diluting pump (1) step prepared enters in ultra-fine filter, control ultrafiltration pressure is 0.05MPa, first time ultrafiltration fractional separation is carried out, until when ultra-filter retentate volume is 1/5 of carbinol ether oligomer diluent volume only with the ultra-filtration membrane that molecular weight cut-off is 2000Da.Collect ultrafiltration filtered solution and ultra-filter retentate for the first time respectively, for the first time ultrafiltration filtered solution collected, for further ion-exchange, to reclaim catalyzer; For the first time ultra-filter retentate collected, add distilled water, make volume return to carbinol ether oligomer diluent volume, after stirring, carry out second time ultrafiltration fractional separation again, the ultra-filtration membrane molecular weight cut-off that second time fractional separation uses is 10000Da, and ultrafiltration pressure is 0.05MPa.When ultra-filter retentate volume be reduced to the alcohol ether oligomer diluted liquid that pumps into long-pending 1/5 time, stop ultrafiltration, collect second time ultrafiltration filtered solution and ultra-filter retentate respectively.Second time ultrafiltration filtered solution is ultrafiltration classification filtered solution, prepares alcohol ether oligomer spray-dried powders for next step; Second time ultra-filter retentate is ultrafiltration classification trapped fluid, prepares alcohol ether oligomer coating for next step.
(3) alcohol ether oligomer spray-dried powders is prepared
After (2) step completes, the ultrafiltration classification filtered solution (2) step prepared is pumped in counter-osmosis device, and control pressure is 0.1MPa, carries out reverse osmosis concentration, until reverse osmosis trapped fluid volume is 1/8 of former ultrafiltration classification filtered solution volume.Collect reverse osmosis filtered solution and reverse osmosis concentrated liquid respectively, for the reverse osmosis filtered solution collected, for the preparation of lower batch of alcohol ether oligomer diluent; For the reverse osmosis concentrated liquid collected, pump in spray-drier, temperature be 150 DEG C, rotating speed carries out spraying dry under being the condition of 5000r/min, just prepares alcohol ether oligomer spray-dried powders.This powder can be used as plastic plasticizer, manufactures the raw material of resin and manufacture frostproofer etc.
(4) alcohol ether oligomer coating is prepared
After (2) step completes, according to dehydrated alcohol: the volume ratio of ultrafiltration classification trapped fluid is the ratio of 1L: 4L, under agitation dehydrated alcohol is joined in compounding kettle, after stirring, the ratio being 1L: 50L according to silane resin acceptor kh-550 and ultra-filter retentate volume ratio adds silane resin acceptor kh-550, under agitation carries out process 15 minutes, then just prepares alcohol ether oligomer coating, can be used for brushing buildings, metal material surface, play etch-proof effect.
Embodiment 3
(1) alcohol ether oligomer diluent is prepared
According to 1,4-butyleneglycol distillation substrate: the volume ratio of distilled water is the ratio of 1L: 10L, first to 1, add distilled water in 4-butyleneglycol distillation substrate, under agitation make BDO distill substrate and dissolve completely, then filter, collect filtrate and abandon filter residue, filtrate is alcohol ether oligomer diluent, prepares ultrafiltration fractional separation liquid for next step.
(2) ultrafiltration fractional separation liquid is prepared
After (1) step completes, the alcohol ether oligomer diluting pump (1) step prepared enters in ultra-fine filter, control ultrafiltration pressure is 0.2MPa, first time ultrafiltration fractional separation is carried out, until when ultra-filter retentate volume is 1/9 of carbinol ether oligomer diluent volume only with the ultra-filtration membrane that molecular weight cut-off is 5000Da.Collect ultrafiltration filtered solution and ultra-filter retentate for the first time respectively, for the first time ultrafiltration filtered solution collected, for further ion-exchange, to reclaim catalyzer; For the first time ultra-filter retentate collected, add distilled water, make volume return to carbinol ether oligomer diluent volume, after stirring, carry out second time ultrafiltration fractional separation again, the ultra-filtration membrane molecular weight cut-off that second time fractional separation uses is 50000Da, and ultrafiltration pressure is 0.2MPa.When ultra-filter retentate volume be reduced to the alcohol ether oligomer diluted liquid that pumps into long-pending 1/9 time, stop ultrafiltration, collect second time ultrafiltration filtered solution and ultra-filter retentate respectively.Second time ultrafiltration filtered solution is ultrafiltration classification filtered solution, prepares alcohol ether oligomer spray-dried powders for next step; Second time ultra-filter retentate is ultrafiltration classification trapped fluid, prepares alcohol ether oligomer coating for next step.
(3) alcohol ether oligomer spray-dried powders is prepared
After (2) step completes, the ultrafiltration classification filtered solution (2) step prepared is pumped in counter-osmosis device, control pressure is 0.5MPa, carries out reverse osmosis concentration, until reverse osmosis trapped fluid volume is 1/10 of former ultrafiltration classification filtered solution volume.Collect reverse osmosis filtered solution and reverse osmosis concentrated liquid respectively, for the reverse osmosis filtered solution collected, for the preparation of lower batch of alcohol ether oligomer diluent; For the reverse osmosis concentrated liquid collected, pump in spray-drier, temperature be 180 DEG C, rotating speed carries out spraying dry under being the condition of 10000r/min, just prepares alcohol ether oligomer spray-dried powders.This powder can be used as plastic plasticizer, manufactures the raw material of resin and manufacture frostproofer etc.
(4) alcohol ether oligomer coating is prepared
After (2) step completes, according to dehydrated alcohol: the volume ratio of ultrafiltration classification trapped fluid is the ratio of 1L: 7L, under agitation dehydrated alcohol is joined in compounding kettle, after stirring, the ratio being 1L: 80L according to silane coupling A-151 and ultra-filter retentate volume ratio adds silane coupling A-151, under agitation carries out process 60 minutes, then just prepares alcohol ether oligomer coating, can be used for brushing buildings, metal material surface, play etch-proof effect.
Claims (1)
1. fully utilize a method for BDO distillation substrate, it is characterized in that concrete steps are as follows:
(1) alcohol ether oligomer diluent is prepared
According to BDO distillation substrate: the volume ratio of distilled water is the ratio of 1L: 5 ~ 10L, to 1, add distilled water in 4-butyleneglycol distillation substrate, under agitation make BDO distill substrate and dissolve completely, then filter, collect filtrate and be alcohol ether oligomer diluent;
(2) ultrafiltration fractional separation liquid is prepared
After (1) step completes, the alcohol ether oligomer diluting pump (1) step prepared enters in ultra-fine filter, control ultrafiltration pressure is 0.05 ~ 0.2MPa, first time ultrafiltration fractional separation is carried out with the ultra-filtration membrane that molecular weight cut-off is 2000 ~ 5000Da, until when ultra-filter retentate volume is 1/5 ~ 1/9 of carbinol ether oligomer diluent volume only, collect ultrafiltration filtered solution and ultra-filter retentate for the first time respectively, for the first time ultrafiltration filtered solution collected, catalyzer is reclaimed in further ion-exchange; For the first time ultra-filter retentate collected, add distilled water, volume is made to return to carbinol ether oligomer diluent volume, second time ultrafiltration fractional separation is carried out again after stirring, the ultra-filtration membrane molecular weight cut-off that second time fractional separation uses is 10000 ~ 50000Da, ultrafiltration pressure is 0.05 ~ 0.2MPa, when ultra-filter retentate volume be reduced to the alcohol ether oligomer diluted liquid that pumps into long-pending 1/5 ~ 1/9 time, stop ultrafiltration, collect second time ultrafiltration classification filtered solution and ultrafiltration classification trapped fluid respectively;
(3) alcohol ether oligomer spray-dried powders is prepared
After (2) step completes, the ultrafiltration classification filtered solution (2) step prepared is pumped in counter-osmosis device, control pressure is 0.1 ~ 0.5MPa, carry out reverse osmosis concentration, until reverse osmosis trapped fluid volume is 1/8 ~ 1/10 of former ultrafiltration classification filtered solution volume, collect reverse osmosis filtered solution and reverse osmosis concentrated liquid respectively, for the reverse osmosis filtered solution collected, for the preparation of lower batch of alcohol ether oligomer diluent; For the reverse osmosis concentrated liquid collected, temperature be 150 ~ 180 DEG C, rotating speed carries out spraying dry under being the condition of 5000 ~ 10000r/min, prepares alcohol ether oligomer spray-dried powders;
(4) alcohol ether oligomer coating is prepared
After (2) step completes, according to dehydrated alcohol: the volume ratio of ultrafiltration classification trapped fluid is the ratio of 1L: 4 ~ 7L, under agitation dehydrated alcohol is joined in compounding kettle, after stirring, the ratio being 1L: 50 ~ 80L according to linking agent XR-500 or silane resin acceptor kh-550 or silane coupling A-151 and ultra-filter retentate volume ratio adds linking agent XR-500 or silane resin acceptor kh-550 or silane coupling A-151, under agitation carry out process 15 ~ 60 minutes, then just prepare alcohol ether oligomer coating.
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| CN115141163B (en) * | 2022-08-01 | 2023-12-19 | 万华化学集团股份有限公司 | Method for efficiently recycling effective components in waste liquid of 1, 4-butanediol prepared by epoxypropane method |
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| JPS4998898A (en) * | 1973-01-13 | 1974-09-18 | ||
| US4946939A (en) * | 1989-05-30 | 1990-08-07 | The Dow Chemical Company | High purity polyether polyols |
| CN1780680A (en) * | 2003-04-25 | 2006-05-31 | 纳幕尔杜邦公司 | Processes for recovering oligomers of glycols and polymerization catalyst from waste streams |
| CN102161615A (en) * | 2011-02-22 | 2011-08-24 | 重庆大学 | Process for recovering 1,4-butanediol |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4998898A (en) * | 1973-01-13 | 1974-09-18 | ||
| US4946939A (en) * | 1989-05-30 | 1990-08-07 | The Dow Chemical Company | High purity polyether polyols |
| CN1780680A (en) * | 2003-04-25 | 2006-05-31 | 纳幕尔杜邦公司 | Processes for recovering oligomers of glycols and polymerization catalyst from waste streams |
| CN102161615A (en) * | 2011-02-22 | 2011-08-24 | 重庆大学 | Process for recovering 1,4-butanediol |
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