CN103849306A - New method for comprehensive utilization of 1,4-butanediol distillation substrate - Google Patents

New method for comprehensive utilization of 1,4-butanediol distillation substrate Download PDF

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CN103849306A
CN103849306A CN201310297096.8A CN201310297096A CN103849306A CN 103849306 A CN103849306 A CN 103849306A CN 201310297096 A CN201310297096 A CN 201310297096A CN 103849306 A CN103849306 A CN 103849306A
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ultrafiltration
ether oligomer
alcohol ether
trapped fluid
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CN103849306B (en
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周桢
颜李秀
周小华
万玉萍
冯琳
陆文立
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Chongqing University
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/582Recycling of unreacted starting or intermediate materials

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Abstract

The invention provides a new method for comprehensively utilizing a 1,4-butanediol distillation substrate and in particular relates to a method for comprehensively utilizing 1,4-butanediol distillation substrate. The new method for comprehensively utilizing the 1,4-butanedio distillation substrate is that 1,4-butanedio distillation substrate is taken as a raw material and diluted firstly, so that a diluent is prepared, then grading ultrafiltration is carried out, and finally a cross linking reaction is carried out, so that alcohol ether oligomer spray drying powder and alcohol ether oligomer degradable paint are prepared. The new method for comprehensively utilizing a 1,4-butanedio distillation substrate has the characteristics of mild preparation conditions, simple operation steps, high product purity, high ratio of comprehensive utilization of resources, environment friendliness, no pollution and the like. The alcohol ether oligomer spray drying powder prepared by adopting the new method for comprehensively utilizing a 1,4-butanedio distillation substrate can be used as a plastic plasticizer, a raw material used for manufacturing resin and a raw material used for manufacturing an antifreezing agent, and the prepared alcohol ether oligomer paint can be used for painting the surfaces of buildings and metal materials, so that an anticorrosive effect is realized.

Description

A kind of novel method that fully utilizes BDO distillation substrate
One, technical field
The invention belongs to chemical byproduct comprehensive utilization technique field, be specifically related to fully utilize the method for BDO distillation substrate.
Two, background technology
BDO has another name called Isosorbide-5-Nitrae one dihydroxyl butane, butylidene glycol, tetramethylene glycol, and English name is Isosorbide-5-Nitrae-putylene glycol, is called for short BDO.BDO is oily liquids colourless, odorless more than 20C, flammable, can dissolve each other with water conservancy ethanol, dissolves in methyl alcohol, ethanol, acetone, is slightly soluble in ether, 235 ℃ of boiling points, 20.2 ℃ of fusing points.BDO is widely used in important Chemicals such as producing tetrahydrofuran (THF), gamma-butyrolactone, polybutylene terephthalate and urethane, also can be used as solvent, moistening agent, softening agent and urethane chain propagation agent and the linking agent etc. in synthetic.
The method of producing at present BDO has Reppe method, normal butane/cis-butenedioic anhydride method, butadiene process and propylene oxide method etc., wherein take improvement Reppe method as main.Produce the refining stage of BDO technique in improvement Reppe method, use scraped film evaporator to distill thick BDO, under the high temperature of scraped film evaporator, condition of high vacuum degree condition, there is autohemagglutination in part BDO, 1, the intermolecular dehydration of 4-butyleneglycol forms alcohol ether oligomer, and the difficult volatilization of this oligopolymer, forms 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 in " applied chemistry " the 2nd phase in 2012 " 1; analytical procedure of 4-butyleneglycol distillation substrate depolymerization solution composition ", the main component of pointing out this substrate is the water-soluble alcohol ether oligomer that the intermolecular dehydration of BDO forms, and viscosity-average molecular weight is 300~1500Da.As can be seen here, BDO distillation substrate is a kind of raw material that has DEVELOPMENT PROSPECT.At present, the major way of processing this substrate is for burning, and not only caused the wasting of resources but also contaminate environment, and therefore, research and development effectively utilize the novel method of distillation substrate, have important value.
About the exploitation of BDO distillation substrate, the paper " 1; recovery process of 4-butyleneglycol distillation substrate " of delivering in " University Of Chongqing's journal " the 3rd phase in 2012 along people such as peaces current rarely seen Wei, this article proposes: proposed under pressurized conditions, take dilute sulphuric acid as catalyzer, this substrate is hydrolyzed and processes the technological process that reclaims BDO and reduce waste discharge.Optimum process condition 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 ℃, and the reaction times is 7h, and the rate of recovery of BDO can reach 39.1%.The main drawback of this technique is: efficiency is low, and working concentration is hydrolyzed 6 hours up to 15% dilute sulphuric acid at 150 ℃, only obtains 39.1% BOD; Produce new source of pollution dilute sulphuric acid waste liquid, need carry out purifying treatment.
Three, summary of the invention
The object of the invention is the weak point for existing BDO distillation substrate recoverying and utilizing method, a kind of novel method that fully utilizes BDO distillation substrate is provided.The present invention can prepare degradable coating profit based on alcohol ether oligomer and can be used as plastic plasticizer, manufactures the raw material of resin and manufacture the alcohol ether oligomer spray-dried powders of frostproofer etc., and there is preparation condition gentleness, the feature such as operation steps is simple, product purity is high, comprehensive utilization of resources rate is high, environment friendly and pollution-free.
Mechanism of the present invention is: BDO distillation substrate mainly contains water-soluble alcohol ether oligomer, and alcohol ether oligomer is the etherate that between BDO molecule, dehydration forms.Due to the difference of the polymerization degree, cause its molecular weight difference, and the molecular diameter of different molecular weight compound there are differences, therefore, in the time seeing through the ultra-filtration membrane of determining aperture, the material that molecular diameter is greater than this ultra-filtration membrane bore dia is trapped, and the material that molecular diameter is less than this ultra-filtration membrane bore dia sees through, so just realized the fractional separation between the water-soluble alcohol ether oligomer of certain molecular weight difference.
Ehter bond claims again glycosidic link in biological chemistry, can be hydrolyzed by Glycosylase, and alcohol ether oligomer connects by ehter bond, therefore, belongs to biodegradable chemical bond; Epoxy silane linking agent contains epoxy group(ing) and alkoxysilane groups, can with water-soluble alcohol ether oligomer in hydroxyl reaction, 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 novel method of 4-butyleneglycol distillation substrate, with 1,4-butyleneglycol distillation substrate is raw material, first BDO is distilled to substrate and dilutes, prepare diluent, carry out again classification ultrafiltration, finally carry out crosslinking reaction, prepare the degradable coating based on alcohol ether oligomer.The concrete steps of described method are as follows:
(1) prepare alcohol ether oligomer diluent
According to 1,4-butyleneglycol distillation substrate: the volume ratio of distilled water is the ratio of 1L: 5~10L, first to 1, in 4-butyleneglycol distillation substrate, add distilled water, under agitation make BDO distillation substrate 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) prepare ultrafiltration fractional separation liquid
After (1) step completes, the rare stalk liquid pump of alcohol ether oligomer prepared by (1) step enters in ultra-fine filter, control ultrafiltration pressure is 0.05~0.2MPa, the ultra-filtration membrane that is 2000~5000Da with molecular weight cut-off carries out ultrafiltration fractional separation for the first time, until ultrafiltration trapped fluid volume is stopping for 1/5~1/9 o'clock of carbinol ether oligomer diluent volume.Collect respectively ultrafiltration filtered solution and ultrafiltration trapped fluid for the first time, for the filtered solution of ultrafiltration for the first time of collecting, for further ion-exchange, to reclaim catalyzer; For the trapped fluid of ultrafiltration for the first time of collecting, add distilled water, make volume return to carbinol ether oligomer diluent volume, after stirring, carry out again ultrafiltration fractional separation for the second time, the ultra-filtration membrane molecular weight cut-off that fractional separation is used is for the second time 10000~50000Da, and ultrafiltration pressure is 0.05~0.2MPa.When ultrafiltration trapped fluid volume be reduced to the alcohol ether oligomer diluted liquid that pumps into long-pending 1/5~1/9 time, stop ultrafiltration, collect respectively ultrafiltration filtered solution and ultrafiltration trapped fluid for the second time.Ultrafiltration filtered solution is ultrafiltration classification filtered solution for the second time, prepares alcohol ether oligomer spray-dried powders for next step; Ultrafiltration trapped fluid is ultrafiltration classification trapped fluid for the second time, prepares alcohol ether oligomer coating for next step.
(3) prepare alcohol ether oligomer spray-dried powders
After (2) step completes, ultrafiltration classification filtered solution prepared by (2) step 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 respectively reverse osmosis filtered solution and reverse osmosis concentrated liquid, for the reverse osmosis filtered solution of collecting, for the preparation of lower batch of alcohol ether oligomer diluent; For the reverse osmosis concentrated liquid of collecting, pump in spray-drier, be spray and be dried under 150~180 ℃, the rotating speed condition that is 5000~10000r/min in temperature, just prepare 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) prepare alcohol ether oligomer coating
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, according to linking agent XR-500, or silane resin acceptor kh-550, or silane coupling A-151 and ultrafiltration trapped fluid volume ratio are that the ratio of 1L: 50~80L adds linking agent XR-500, or silane resin acceptor kh-550, or silane coupling A-151, under agitation process 15~60 minutes, then just prepare alcohol ether oligomer coating, can be used for brushing buildings, metal material surface, play etch-proof effect.
The present invention adopts after technique scheme, mainly contains following effect:
(1) the present invention in process of production, adopt ultrafiltration process to carry out fractional separation to alcohol ether oligomer, obtain respectively the filtered solution of ultrafiltration for the first time that can be used for reclaiming catalyzer, the raw material of preparing and can be used as plastic plasticizer, manufacturing resin and manufacture the filtered solution of ultrafiltration for the second time of the alcohol ether oligomer spray-dried powders of frostproofer etc., and for the preparation of the trapped fluid of ultrafiltration for the second time of alcohol ether oligomer coating.Whole recyclings of alcohol ether oligomer are realized.Thereby improved production efficiency, reduced product cost, save energy, is conducive to Sustainable development.
(2) the present invention in process of production, mainly uses ultrafiltration, reverse osmosis, the spraying equipment bought of being easy to such as dry, and production unit is general, working specification and be easy to control, and therefore production safety reduces production costs again.
(3) the present invention in process of production, does not use poisonous and harmful reagent and has realized whole recyclings of alcohol ether oligomer, without " three wastes " discharge, also makes full use of resource.
(4) excellent property of the product that the present invention obtains, the raw materials such as alternative ethylene glycol or energy priming paint etc.
Four, embodiment
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment 1
(1) prepare alcohol ether oligomer diluent
According to 1,4-butyleneglycol distillation substrate: the volume ratio of distilled water is the ratio of 1L: 7L, first to 1, in 4-butyleneglycol distillation substrate, add distilled water, under agitation make BDO distillation substrate 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) prepare ultrafiltration fractional separation liquid
After (1) step completes, alcohol ether oligomer diluting pump prepared by (1) step enters in ultra-fine filter, control ultrafiltration pressure is 0.1MPa, the ultra-filtration membrane that is 3000Da with molecular weight cut-off carries out ultrafiltration fractional separation for the first time, until ultrafiltration trapped fluid volume is stopping for 1/7 o'clock of carbinol ether oligomer diluent volume.Collect respectively ultrafiltration filtered solution and ultrafiltration trapped fluid for the first time, for the filtered solution of ultrafiltration for the first time of collecting, for further ion-exchange, to reclaim catalyzer; For the trapped fluid of ultrafiltration for the first time of collecting, add distilled water, make volume return to the rare stalk liquid of carbinol ether oligomer long-pending, after stirring, carry out again ultrafiltration fractional separation for the second time, the ultra-filtration membrane molecular weight cut-off that fractional separation is used is for the second time 30000Da, and ultrafiltration pressure is 0.1MPa.When ultrafiltration trapped fluid volume be reduced to the alcohol ether oligomer diluted liquid that pumps into long-pending 1/7 time, stop ultrafiltration, collect respectively ultrafiltration filtered solution and ultrafiltration trapped fluid for the second time.Ultrafiltration filtered solution is ultrafiltration classification filtered solution for the second time, prepares alcohol ether oligomer spray-dried powders for next step; Ultrafiltration trapped fluid is ultrafiltration classification trapped fluid for the second time, prepares alcohol ether oligomer coating for next step.
(3) prepare alcohol ether oligomer spray-dried powders
After (2) step completes, ultrafiltration classification filtered solution prepared by (2) step 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 respectively reverse osmosis filtered solution and reverse osmosis concentrated liquid, for the reverse osmosis filtered solution of collecting, for the preparation of lower batch of alcohol ether oligomer diluent; For the reverse osmosis concentrated liquid of collecting, pump in spray-drier, be spray and be dried under 165 ℃, the rotating speed condition that is 8000r/min in temperature, just prepare 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) prepare alcohol ether oligomer coating
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 that is 1L: 65L according to linking agent XR-500 and ultrafiltration trapped fluid volume ratio adds linking agent XR-500, under agitation processes 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) prepare alcohol ether oligomer diluent
According to 1,4-butyleneglycol distillation substrate: the volume ratio of distilled water is the ratio of 1L: 5L, first to 1, in 4-butyleneglycol distillation substrate, add distilled water, under agitation make BDO distillation substrate 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) prepare ultrafiltration fractional separation liquid
After (1) step completes, alcohol ether oligomer diluting pump prepared by (1) step enters in ultra-fine filter, control ultrafiltration pressure is 0.05MPa, the ultra-filtration membrane that is 2000Da with molecular weight cut-off carries out ultrafiltration fractional separation for the first time, until ultrafiltration trapped fluid volume is stopping for 1/5 o'clock of carbinol ether oligomer diluent volume.Collect respectively ultrafiltration filtered solution and ultrafiltration trapped fluid for the first time, for the filtered solution of ultrafiltration for the first time of collecting, for further ion-exchange, to reclaim catalyzer; For the trapped fluid of ultrafiltration for the first time of collecting, add distilled water, make volume return to carbinol ether oligomer diluent volume, after stirring, carry out again ultrafiltration fractional separation for the second time, the ultra-filtration membrane molecular weight cut-off that fractional separation is used is for the second time 10000Da, and ultrafiltration pressure is 0.05MPa.When ultrafiltration trapped fluid volume be reduced to the alcohol ether oligomer diluted liquid that pumps into long-pending 1/5 time, stop ultrafiltration, collect respectively ultrafiltration filtered solution and ultrafiltration trapped fluid for the second time.Ultrafiltration filtered solution is ultrafiltration classification filtered solution for the second time, prepares alcohol ether oligomer spray-dried powders for next step; Ultrafiltration trapped fluid is ultrafiltration classification trapped fluid for the second time, prepares alcohol ether oligomer coating for next step.
(3) prepare alcohol ether oligomer spray-dried powders
After (2) step completes, ultrafiltration classification filtered solution prepared by (2) step 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 respectively reverse osmosis filtered solution and reverse osmosis concentrated liquid, for the reverse osmosis filtered solution of collecting, for the preparation of lower batch of alcohol ether oligomer diluent; For the reverse osmosis concentrated liquid of collecting, pump in spray-drier, be spray and be dried under 150 ℃, the rotating speed condition that is 5000r/min in temperature, just prepare 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) prepare alcohol ether oligomer coating
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 that is 1L: 50L according to silane resin acceptor kh-550 and ultrafiltration trapped fluid volume ratio adds silane resin acceptor kh-550, processes 15 minutes in stirring, then just prepares alcohol ether oligomer coating, can be used for brushing buildings, metal material surface, play etch-proof effect.
Embodiment 3
(1) prepare alcohol ether oligomer diluent
According to 1,4-butyleneglycol distillation substrate: the volume ratio of distilled water is the ratio of 1L: 10L, first to 1, in 4-butyleneglycol distillation substrate, add distilled water, under agitation make BDO distillation substrate 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) prepare ultrafiltration fractional separation liquid
After (1) step completes, alcohol ether oligomer diluting pump prepared by (1) step enters in ultra-fine filter, control ultrafiltration pressure is 0.2MPa, the ultra-filtration membrane that is 5000Da with molecular weight cut-off carries out ultrafiltration fractional separation for the first time, until ultrafiltration trapped fluid volume is carbinol ether oligomer, rare stalk liquid stops for long-pending 1/9 o'clock.Collect respectively ultrafiltration filtered solution and ultrafiltration trapped fluid for the first time, for the filtered solution of ultrafiltration for the first time of collecting, for further ion-exchange, to reclaim catalyzer; For the trapped fluid of ultrafiltration for the first time of collecting, add distilled water, make volume return to carbinol ether oligomer diluent volume, after stirring, carry out again ultrafiltration fractional separation for the second time, the ultra-filtration membrane molecular weight cut-off that fractional separation is used is for the second time 50000Da, and ultrafiltration pressure is 0.2MPa.When ultrafiltration trapped fluid volume be reduced to the alcohol ether oligomer diluted liquid that pumps into long-pending 1/9 time, stop ultrafiltration, collect respectively ultrafiltration filtered solution and ultrafiltration trapped fluid for the second time.Ultrafiltration filtered solution is ultrafiltration classification filtered solution for the second time, prepares alcohol ether oligomer spray-dried powders for next step; Ultrafiltration trapped fluid is ultrafiltration classification trapped fluid for the second time, prepares alcohol ether oligomer coating for next step.
(3) prepare alcohol ether oligomer spray-dried powders
After (2) step completes, ultrafiltration classification filtered solution prepared by (2) step 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 respectively reverse osmosis filtered solution and reverse osmosis concentrated liquid, for the reverse osmosis filtered solution of collecting, for the preparation of the lower batch of rare stalk liquid of alcohol ether oligomer; For the reverse osmosis concentrated liquid of collecting, pump in spray-drier, be spray and be dried under 180 ℃, the rotating speed condition that is 10000r/min in temperature, just prepare 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) prepare alcohol ether oligomer coating
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 that is 1L: 80L according to silane coupling A-151 and ultrafiltration trapped fluid volume ratio adds silicon a heatable brick bed coupling agent A-151, under agitation processes 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. a novel method that fully utilizes BDO distillation substrate, is characterized in that concrete steps are as follows:
(1) prepare alcohol ether oligomer diluent
Distill substrate according to BDO: the volume ratio of distilled water is the ratio of 1L: 5~10L, to 1, in 4-butyleneglycol distillation substrate, add distilled water, under agitation make BDO distillation substrate dissolve completely, then filter, collect filtrate and be alcohol ether oligomer diluent;
(2) prepare ultrafiltration fractional separation liquid
After (1) step completes, alcohol ether oligomer diluting pump prepared by (1) step enters in ultra-fine filter, control ultrafiltration pressure is 0.05~0.2MPa, the ultra-filtration membrane that is 2000~5000Da with molecular weight cut-off carries out ultrafiltration fractional separation for the first time, until ultrafiltration trapped fluid volume is stopping for 1/5~1/9 o'clock of carbinol ether oligomer diluent volume, collect respectively ultrafiltration filtered solution and ultrafiltration trapped fluid for the first time, for the filtered solution of ultrafiltration for the first time of collecting, further catalyzer is reclaimed in ion-exchange; For the trapped fluid of ultrafiltration for the first time of collecting, add distilled water, make volume return to carbinol ether oligomer diluent volume, after stirring, carry out again ultrafiltration fractional separation for the second time, the ultra-filtration membrane molecular weight cut-off that fractional separation is used is for the second time 10000~50000Da, ultrafiltration pressure is 0.05~0.2MPa, when ultrafiltration trapped fluid volume be reduced to the alcohol ether oligomer diluted liquid that pumps into long-pending 1/5~1/9 time, stop ultrafiltration, collect respectively the filtered solution of ultrafiltration classification for the second time and ultrafiltration classification trapped fluid;
(3) prepare alcohol ether oligomer spray-dried powders
After (2) step completes, ultrafiltration classification filtered solution prepared by (2) step 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 respectively reverse osmosis filtered solution and reverse osmosis concentrated liquid, for the reverse osmosis filtered solution of collecting, for the preparation of lower batch of alcohol ether oligomer diluent; For the reverse osmosis concentrated liquid of collecting, be spray and be dried under 150~180 ℃, the rotating speed condition that is 5000~10000r/min in temperature, prepare alcohol ether oligomer spray-dried powders;
(4) prepare alcohol ether oligomer coating
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 that is 1L: 50~80L according to linking agent XR-500 or silane resin acceptor kh-550 or silane coupling A-151 and ultrafiltration trapped fluid volume ratio adds linking agent XR-500 or silane resin acceptor kh-550 or silane coupling A-151, under agitation process 15~60 minutes, then just prepare alcohol ether oligomer coating.
CN201310297096.8A 2013-07-08 2013-07-08 A kind of method fully utilizing BDO distillation substrate Expired - Fee Related CN103849306B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104829030A (en) * 2015-05-12 2015-08-12 苏州苏净环保工程有限公司 Treatment and recovery method of wastewater containing sodium terephthalate and 1,4-butanediol
CN115141163A (en) * 2022-08-01 2022-10-04 万华化学集团股份有限公司 Method for efficiently recovering effective components in waste liquid of 1, 4-butanediol prepared by epoxypropane method

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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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104829030A (en) * 2015-05-12 2015-08-12 苏州苏净环保工程有限公司 Treatment and recovery method of wastewater containing sodium terephthalate and 1,4-butanediol
CN115141163A (en) * 2022-08-01 2022-10-04 万华化学集团股份有限公司 Method for efficiently recovering effective components in waste liquid of 1, 4-butanediol prepared by epoxypropane method
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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