CN106750244B - A method of polyether polyol is prepared using micro passage reaction - Google Patents
A method of polyether polyol is prepared using micro passage reaction Download PDFInfo
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- CN106750244B CN106750244B CN201611186754.6A CN201611186754A CN106750244B CN 106750244 B CN106750244 B CN 106750244B CN 201611186754 A CN201611186754 A CN 201611186754A CN 106750244 B CN106750244 B CN 106750244B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2642—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds characterised by the catalyst used
- C08G65/2645—Metals or compounds thereof, e.g. salts
- C08G65/2663—Metal cyanide catalysts, i.e. DMC's
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/30—Post-polymerisation treatment, e.g. recovery, purification, drying
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Abstract
The invention discloses a kind of methods using micro passage reaction preparation polyether polyol, using active hydride as initiator, oxyalkylene is raw material, using double metal cyanide as catalyst, the process for the polyether polyols alcohol synthesis reaction that number-average molecular weight is 700-1000 is completed in micro passage reaction, relatively narrow using Contents In Polyether Polyol molecular weight distribution made of this method, product degree of unsaturation is low, and no tailing peak generates.
Description
Technical field
The invention belongs to the preparation method fields of polyethers, and in particular to a kind of to prepare polyether polyols using micro passage reaction
The method of alcohol.
Background technique
Polyether polyol is the important source material in polyurethane production, generally by initiator and epoxy second containing polyhydroxy-alcohol
The epoxides such as alkane, propylene oxide, epoxy butane are made in the presence of basic catalyst through sudden reaction.Basic catalyst is general
Potassium hydroxide, sodium hydroxide etc. are selected, such catalyst is mainly catalyzed the open loop of epoxy olefins anion, the disadvantage is that preparing number
Unsaturated bond is easily formed during polyether polyol of the average molecular weight greater than 1000, the presence of these unsaturated bonds keeps polyethers more
The degree of functionality of first alcohol reduces, and hardness and mechanical performance to polyurethane material can have an adverse effect.
To reduce the degree of unsaturation in polyethers of the number-average molecular weight greater than 1000, the catalyst that industry is known to use is double gold
When belonging to cyanide (DMC), but preparing polyether polyol using DMC, reaction temperature is generally greater than 130 DEG C, in polyethers synthesis process
In a certain amount of polyether polyol tailing peak easily generated, cause molecular weight distribution to broaden, the viscosity of product is higher, affects product
Use field.
Patent CN1210549A describes a kind of method using dmc catalyst preparation polyether polyol, in a kettle
Hydroxy-containing compounds react in the presence of DMC with propylene oxide, are reduced in polyethers by way of being continuously added to initiator
The generation of tailing peak, but also have a small amount of tailing peak and exist.Patent CN1225652A is described continuously to be made using dmc catalyst
The method of standby polyether polyol, material is piston flow in pipe, and mixed effect is bad, and the molecular weight distribution index of product is higher,
Breadth coefficient D >=1.1.Patent CN1556829A describes the reaction unit that a set of reaction kettle and tubular reactor combine, reaction
It is to carry out in a kettle, material is post-processed in tubular reactor, purpose is mainly the epoxides reduced in material
Content.Patent DE19840587A1, patent US6362126, patent CN1400982A describe poly- for dmc catalyst preparation
Particular reactor in the continuation method of ethoxylated polyhydric alcohol, using DMC supported catalyst, and this kind of loaded catalyst is urged
Change activity is lower, and the universal service life of catalyst is shorter.
Currently, micro passage reaction obtained in reactions such as digestion reaction, hydrogenation reactions with certain risk it is good
Good utilization, improves the safety of reaction.But in the polymerization, micro- due to the uncertainty of response situation, complexity
The use of channel reactor also needs further research.
Summary of the invention
The problem to be solved in the present invention is, a certain amount of polyether polyol tailing peak easily generated in polyethers synthesis process,
Molecular weight distribution is caused to broaden, the viscosity of product is higher, and affect product uses field；Catalyst activity is lower, the service life compared with
It is short.
In order to solve the above technical problems, the present invention provides a kind of side using micro passage reaction preparation polyether polyol
Method, specifically includes the following steps:
A) using active hydride as initiator, double metal cyanide is catalyst, by initiator and catalyst by stirring,
Heat up and vacuumize and to obtain mixed material；
B) said mixture material is continuously inputted in micro passage reaction respectively with oxyalkylene and is reacted, mixed material
It is 1 ﹕, 1~1 ﹕ 25 with oxyalkylene molar ratio；
C) above-mentioned to obtain crude polyoxyalkylene polyol after reaction；Crude polyoxyalkylene polyol removes small molecule after entering stripper, obtains
To Contents In Polyether Polyol；
After above-mentioned material continuously enters micro passage reaction, mixed at high speed simultaneously reacts, wherein in micro passage reaction
Temperature is 90~115 DEG C, and pressure is 0~0.3MPa, and residence time of material is 30s~600s.
In above-mentioned technical proposal, initiator is that there is the polyalcohol of 2-8 degree of functionality to be selected from ethylene glycol, diethylene glycol (DEG), 1,2- third
Glycol, 1,3- propylene glycol, 1,2- butanediol, 1,4- butanediol, 1,6-HD, triethylene glycol, dipropylene glycol, tripropylene glycol, third
Triol, trimethylolpropane, pentaerythrite, two polyglycereol, three polyglycereol, four polyglycereol, five polyglycereol, six polyglycereol, sorb
The reaction product of the mixture and oxyalkylene of one of alcohol, sucrose or any of the above combination arbitrary proportion, hydroxyl equivalent
It is 150~300.In the preparation of these products, the addition reaction catalyst of oxyalkylene be selected from potassium hydroxide, sodium hydroxide,
The mixture of one or more of potassium, sodium, potassium methoxide, sodium methoxide；Basic catalyst passes through crystallization or absorption point in post synthesis
From.
In above-mentioned technical proposal, catalyst double metal cyanide has following general formula:
Za[X(CN)b(A)c]d·fZgYn·h(H2O)·eW
In formula, Z is selected from: Mg2+、Zn2+、Fe2+、Cu2+、Co2+、Co3+、Ni2+、Mn2+、Sn2+、Pb2+、Mo4+、Al3+、V2+、V4 +、V5+、W4+、W6+、Cr2+、Cr3+、Cd2+、Pd2+Or Pt2+；
X is selected from: Fe2+、Fe3+、Mn2+、Mn3+、Co2+、Co3+、V4+、V5+、Cr2+、Cr3+、Ru2+、Rh3+Or Ir3+；
A is selected from: carboxylate radical, oxalate, cyanate radical, thiocyanate radical, cyanide, isocyano, nitrate anion or hydroxyl；
Y is selected from: carboxylate radical, oxalate, cyanate radical, thiocyanate radical, cyanide, isocyano, nitrate anion or hydroxyl；
W be ligand miscible with water, be selected from: alkyl compound, aldehyde, ketone, amide, lactams, ether, polyethers, ester, lactone,
Urea, nitrile or sulfide；
A, b, c, d, g and n respectively indicate Z, CN, A, X (CN)b(A)c, Z and Y number；E is the ligancy of ligand；F, h points
It is not greater than the integer equal to 0.
Wherein should be preferably with the multi-metal cyanide of crystal structure, the partial size of multi-metal cyanide is preferably in 0.1~50 μ
Within the scope of m.
In above-mentioned technical proposal, in the reaction system of step b), the mass percentage concentration of catalyst double metal cyanide is 5
~20ppm.
Further, raw material oxyalkylene preferably is selected from least one of ethylene oxide, propylene oxide or epoxy butane.
In a kind of method using micro passage reaction preparation polyether polyol provided by the invention, used microchannel
The microchannel internal diameter of reactor is preferably 0.10~1.5mm, and micro-tunnel length is preferably 1.5~20m, the material of micro passage reaction
Matter is selected from stainless steel, alloy, ceramics or carbon silica glass.Polyether polyol is prepared using the micro passage reaction, reaction mass transfer passes
The thermal efficiency increases substantially, and intermolecular contact-impact is greatly speeded up, and the efficiency of reaction and the quality of product have and significantly mention
It is high.
Further, the feed opening of multiple oxyalkylenes, oxyalkylene and starting are equipped on the micro passage reaction
Agent can be added simultaneously, can also be segmented oxyalkylene and be added.When starter molecules amount is smaller, oxyalkylene can be catalyzed with being mixed with
The initiator of agent is added simultaneously, when starter molecules amount is larger, while the abundant progress for being unfavorable for reaction is added, segmentation is added
It is more advantageous to the chain growth of polyether polyol.
Further, step a) is that initiator and catalyst are added in the closed container of stirring in above-mentioned technical proposal,
Stirring is opened, 100~165 DEG C is warming up to, vacuum 0.5~1.5 hour, obtains mixed material, mixed material is stored in closed batch can
In.Due to oxyalkylene such as propylene oxide, initiator is heated up in advance with catalyst and is mixed, makes it by low boiling point highly volatile
It comes into full contact with,
The present invention prepares polyether polyol using micro passage reaction, and in micro flow channel, the specific surface area of material is significantly
Increase, interface transmitting is rapider, strengthens the transmitting of molecule contacts and heat, prepares Contents In Polyether Polyol using this method
Number-average molecular weight be 700~10000.Compared with traditional technology, have the advantages that
(1) reduce catalyst amount, catalyst amount is less than 25ppm；Reaction temperature is reduced, reaction temperature is lower than
120℃。
(2) the Contents In Polyether Polyol molecular weight distribution generated is relatively narrow, molecular weight distribution index D≤1.02；Product insatiable hunger
With lower, the degree of unsaturation≤0.002mmol/g of degree；No tailing peak generates.
(3) reactor is continuous flow reactor, and the reaction time foreshortened within 10 minutes, substantially increases the life of product
Efficiency is produced, production capacity is improved.
Specific embodiment
For a better understanding of the present invention, the present invention is further illustrated below with reference to embodiment.
Embodiment 1
The synthesis of initiator A-1:
304g propylene glycol, potassium hydroxide 4.8g are added into 2L reactor, nitrogen is replaced 2 times, is warming up to 60~70 DEG C, is taken out
Vacuum extremely -0.093MPa, keeps 0.5h, stops vacuumizing, be warming up to 110~120 DEG C, be continuously added to 1300.0g propylene oxide,
It controls reaction pressure and is no more than 0.30MPa, after propylene oxide has led to, after 120 DEG C of heat preservations are constant to pressure drop, be evacuated to-
0.093MPa keeps 0.5h, leads to nitrogen to normal pressure；Deionized water 50g is added to 60~80 DEG C in temperature drop, stirs 1h, adds phosphorus
Acid (50% concentration) 16.4g stirs 1h, is eventually adding magnesium silicate 4.9g, after stirring 1h, is warming up to 100~120 DEG C, vacuum is de-
The moisture in material is removed, is filtered under diminished pressure, the polyether polyol A-1 of 1570.0g number-average molecular weight 400 is obtained.
Index: appearance: colourless transparent liquid, hydroxyl value: 280.05mgKOH/g
Initiator A-1, catalyst double metal cyanide Zn is added in a closed container with stirring3[Co(CN)6]2·
ZnNO3·2H2O·C3H8O212ppm opens stirring, is warming up to 120 DEG C, vacuumizes 1.5 hours, obtain mixed material B-1, material
B-1 is stored in closed batch can；Material B-1 and propylene oxide are squeezed into micro passage reaction, material with metering pump respectively simultaneously
The molar ratio of B-2 and propylene oxide is 1 ﹕ 10.35,100 DEG C of temperature, pressure 0.01MPa in micro passage reaction, material stop
155s, material are flowed continually out from reactor outlet to receiving tank, obtain crude polyoxyalkylene polyol E-1, and crude polyoxyalkylene polyol enters stripping
Small molecule is removed after tower, obtains Contents In Polyether Polyol F-1.
Index: appearance: colourless transparent liquid, hydroxyl value: 112.2mgKOH/g, degree of unsaturation 0.001mmol/g, molecular weight point
Cloth coefficient 1.02, no tailing peak.
Embodiment 2
Initiator A-1, catalyst double metal cyanide Zn in embodiment 1 are added in a closed container with stirring3
[Co(CN)6]2·ZnNO3·2H2O·C3H8O220ppm opens stirring, is warming up to 125 DEG C, vacuumizes 1.5 hours, must mix
Material B-2, material B-2 are stored in closed batch can；Material B-2 and propylene oxide are squeezed into microchannel with metering pump respectively simultaneously
The molar ratio of reactor, material B-2 and propylene oxide is 1 ﹕ 20.7,100 DEG C of temperature in micro passage reaction, pressure
0.015MPa, material stop 195s, material are flowed continually out from reactor outlet to receiving tank, obtain crude polyoxyalkylene polyol E-2, thick poly-
Ethoxylated polyhydric alcohol removes small molecule after entering stripper, obtains Contents In Polyether Polyol F-2.
Index: appearance: colourless transparent liquid, hydroxyl value: 56.1mgKOH/g, degree of unsaturation 0.0005mmol/g, molecular weight point
Cloth coefficient 1.01, no tailing peak.
Embodiment 3
Initiator A-1, catalyst double metal cyanide Zn in embodiment 1 are added in a closed container with stirring3
[Co(CN)6]2·ZnNO3·2H2O·C3H8O215ppm opens stirring, is warming up to 130 DEG C, vacuumizes 1.5 hours, obtain material
B-3, material B-3 are stored in closed batch can；Material B-3 and butylene oxide are squeezed into microchannel plate simultaneously with metering pump respectively to answer
The molar ratio of device, material B-3 and butylene oxide is 1 ﹕ 8.57,115 DEG C of temperature, pressure 0.02MPa in micro passage reaction, material
405s is stopped, material is flowed continually out from reactor outlet to receiving tank, obtains crude polyoxyalkylene polyol E-3, and crude polyoxyalkylene polyol enters
Small molecule is removed after stripper, obtains Contents In Polyether Polyol F-3.
Index: appearance: colourless transparent liquid, hydroxyl value: 112.1mgKOH/g, degree of unsaturation 0.0013mmol/g, molecular weight
Breadth coefficient 1.02, no tailing peak.
Embodiment 4
The synthetic method of initiator A-4:
276g glycerine, potassium hydroxide 3.0g are added into 2L reactor, nitrogen is replaced 2 times, is warming up to~100 DEG C, is taken out
Vacuum extremely -0.093MPa, keeps 1.0h, stops vacuumizing, be warming up to 110~120 DEG C, be continuously added to 1226.0g propylene oxide,
It controls reaction pressure and is no more than 0.30MPa, after propylene oxide has led to, after 120 DEG C of heat preservations are constant to pressure drop, be evacuated to-
0.093MPa keeps 1.5h, leads to nitrogen to normal pressure；Deionized water 75g is added to 60~80 DEG C in temperature drop, stirs 1h, adds phosphorus
Acid (50% concentration) 10.2g stirs 1h, is eventually adding magnesium silicate 4.4g, after stirring 1h, is warming up to 100~120 DEG C, vacuum is de-
The moisture in material is removed, is filtered under diminished pressure, the polyether polyol A-4 of 1498.1g number-average molecular weight 500 is obtained.
Index: appearance: colourless transparent liquid, hydroxyl value: 336.1mgKOH/g
Amount to one with addition initiator A-4 in the closed container stirred, catalyst double metal cyanide Zn3[Co
(CN)6]2·ZnNO3·2H2O·C3H8O218ppm opens stirring, is warming up to 120 DEG C, vacuumizes 1.5 hours, obtain mixed material
B-4, material B-4 are stored in closed batch can；Material B-4 and propylene oxide are squeezed into microchannel plate simultaneously with metering pump respectively to answer
The molar ratio of device, material B-4 and propylene oxide is 1 ﹕ 8.62,110 DEG C of temperature, pressure 0.05MPa in micro passage reaction, material
165s is stopped, material is flowed continually out from reactor outlet to receiving tank, obtains crude polyoxyalkylene polyol E-4, and crude polyoxyalkylene polyol enters
Small molecule is removed after stripper, obtains Contents In Polyether Polyol F-4.
Index: appearance: colourless transparent liquid, hydroxyl value: 168.2mgKOH/g, degree of unsaturation 0.0008mmol/g, molecular weight
Breadth coefficient 1.0, no tailing peak.
Embodiment 5
Amount to one with the initiator A-4 being added in the closed container stirred in embodiment 4, catalyst double metal cyanide
Zn3[Co(CN)6]2·ZnNO3·2H2O·C3H8O216ppm opens stirring, is warming up to 120 DEG C, vacuumizes 1.5 hours, obtain mixed
Material B-5 is closed, material B-5 is stored in closed batch can；Material B-5 and propylene oxide are squeezed into metering pump simultaneously respectively micro- logical
The molar ratio of road reactor, material B-5 and propylene oxide is 1 ﹕ 43.1,115 DEG C of temperature in micro passage reaction, pressure
0.1MPa, material stop 605s, material are flowed continually out from reactor outlet to receiving tank, obtain crude polyoxyalkylene polyol E-5, thick polyethers
Polyalcohol removes small molecule after entering stripper, obtains Contents In Polyether Polyol F-5.
Index: appearance: colourless transparent liquid, hydroxyl value: 56.1.mgKOH/g, degree of unsaturation 0.001mmol/g, molecular weight point
Cloth coefficient 1.01, no tailing peak.
Above-described embodiment is only preferred embodiment, is not limited the embodiments.For the common of fields
For technical staff, other different forms of changes or modifications may be made based on the above description.It is all according to the present invention
Equivalent changes and modifications made by the content of claim all should be used as technology scope of the invention.
Claims (3)
1. a kind of method using micro passage reaction preparation polyether polyol, it is characterised in that the following steps are included:
A) using active hydride as initiator, double metal cyanide is catalyst, and initiator and catalyst are passed through stirring, heating
With vacuumize to obtain mixed material；
B) said mixture material is continuously inputted in micro passage reaction respectively with oxyalkylene and is reacted, mixed material and oxygen
Change olefin molar ratio is 1 ﹕, 1~1 ﹕ 25；
C) above-mentioned to obtain crude polyoxyalkylene polyol after reaction, crude polyoxyalkylene polyol removes small molecule after entering stripper, is gathered
Ethoxylated polyhydric alcohol product；
After above-mentioned material continuously enters micro passage reaction, the raw reaction of hybrid concurrency, wherein temperature is 90 in micro passage reaction
~115 DEG C, pressure is 0~0.3MPa, and residence time of material is 30s~600s；
The microchannel internal diameter of micro passage reaction is 0.10~1.5mm, and micro-tunnel length is 1.5~20m, micro passage reaction
Material is selected from stainless steel, alloy, ceramics or carbon silica glass；
Step a) is that initiator and catalyst are added in the closed container of stirring, opens stirring, is warming up to 100~165 DEG C, very
It is 0.5~1.5 hour empty, mixed material is obtained, mixed material is stored in closed batch can；
In step b), the mass percentage concentration of the double metal cyanide is 5~20ppm；
The initiator be have 2-8 degree of functionality polyalcohol be selected from ethylene glycol, diethylene glycol (DEG), 1,2- propylene glycol, 1,3- propylene glycol,
1,2- butanediol, 1,4- butanediol, 1,6-HD, triethylene glycol, dipropylene glycol, tripropylene glycol, glycerine, trihydroxy methyl third
One of alkane, pentaerythrite, two polyglycereol, three polyglycereol, four polyglycereol, five polyglycereol, six polyglycereol, sorbierite, sucrose
Or any of the above combines the mixture of arbitrary proportion and the reaction product of oxyalkylene, hydroxyl equivalent is 150~300；
The oxyalkylene is selected from least one of propylene oxide or epoxy butane.
2. the method according to claim 1 using micro passage reaction preparation polyether polyol, it is characterised in that described
Double metal cyanide has following general formula:
Za[X(CN)b(A)c]d·fZgYn·h(H2O)·eW
In formula, Z is selected from: Mg2+、Zn2+、Fe2+、Cu2+、Co2+、Co3+、Ni2+、Mn2+、Sn2+、Pb2+、Mo4+、Al3+、V2+、V4+、V5+、
W4+、W6+、Cr2+、Cr3+、Cd2+、Pd2+Or Pt2+；
X is selected from: Fe2+、Fe3+、Mn2+、Mn3+、Co2+、Co3+、V4+、V5+、Cr2+、Cr3+、Ru2+、Rh3+Or Ir3+；
A is selected from: carboxylate radical, oxalate, cyanate radical, thiocyanate radical, cyanide, isocyano, nitrate anion or hydroxyl；
Y is selected from: carboxylate radical, oxalate, cyanate radical, thiocyanate radical, cyanide, isocyano, nitrate anion or hydroxyl；
W is ligand miscible with water, is selected from: alkyl compound, aldehyde, ketone, amide, lactams, ether, polyethers, ester, lactone, urea, nitrile
Or sulfide；
A, b, c, d, g and n respectively indicate Z, CN, A, X (CN)b(A)c, Z and Y number；E is the ligancy of ligand；F, h is respectively
Integer more than or equal to 0.
3. a kind of method using micro passage reaction preparation polyether polyol according to claim 1, it is characterised in that
The micro passage reaction is equipped with the feed opening of multiple oxyalkylenes, and oxyalkylene segmentation is added.
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| CN109651609B (en) * | 2018-11-28 | 2021-04-06 | 山东蓝星东大有限公司 | Preparation method of polyether polyol with high EO content |
| CN110156982B (en) * | 2019-06-21 | 2022-02-08 | 常州中英新材料有限公司 | Liquid-liquid homogeneous phase method for synthesizing polyarylether by using continuous flow microchannel reactor |
| CN110317336B (en) * | 2019-06-21 | 2022-02-15 | 常州中英新材料有限公司 | Method for synthesizing thermosetting polyarylether by using continuous flow microchannel reactor |
| CN110156983B (en) * | 2019-06-21 | 2022-05-13 | 常州中英新材料有限公司 | Liquid-liquid heterogeneous method for synthesizing polyarylether by using continuous flow microchannel reactor |
| CN110483762B (en) * | 2019-08-07 | 2022-05-13 | 常州中英新材料有限公司 | Method for synthesizing thermosetting polyarylether resin by using continuous flow microchannel reactor |
| CN110835409B (en) * | 2019-12-03 | 2020-08-28 | 山东益丰生化环保股份有限公司 | Method for producing polythiol by using microchannel reactor through continuous reaction |
| CN111925514A (en) * | 2020-07-02 | 2020-11-13 | 西华大学 | A method for continuous production of high molecular weight polyether using microchannel reactor |
| CN113274956A (en) * | 2021-05-08 | 2021-08-20 | 袁相质 | Microchannel reaction system and method for preparing epoxy compound |
| CN114672012A (en) * | 2022-03-16 | 2022-06-28 | 中国石油化工股份有限公司 | Method for preparing polyether polyol based on micro mixer and micro-channel reactor |
| CN114621428A (en) * | 2022-03-16 | 2022-06-14 | 中国石油化工股份有限公司 | Preparation method of polyether polyol with higher molecular weight |
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| DE10156117A1 (en) * | 2001-11-15 | 2003-05-28 | Basf Ag | Process for the preparation of polyether alcohols |
| DE102004013551A1 (en) * | 2004-03-19 | 2005-10-06 | Goldschmidt Gmbh | Alkoxylations in microstructured capillary reactors |
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