CN109485847A - A kind of non-isocyanate polyurea elastomer - Google Patents
A kind of non-isocyanate polyurea elastomer Download PDFInfo
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- CN109485847A CN109485847A CN201811102763.1A CN201811102763A CN109485847A CN 109485847 A CN109485847 A CN 109485847A CN 201811102763 A CN201811102763 A CN 201811102763A CN 109485847 A CN109485847 A CN 109485847A
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- polyurea elastomer
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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
- C08G71/00—Macromolecular compounds obtained by reactions forming a ureide or urethane link, otherwise, than from isocyanate radicals in the main chain of the macromolecule
- C08G71/02—Polyureas
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Abstract
The present invention provides a kind of non-isocyanate polyurea elastomer synthesized by simple, green, environmentally friendly route, and formula composition includes: diamine compounds, dialkyl carbonate, amine terminated polyether；Mol ratio 1:10 ~ 10:1 of the dialkyl carbonate and diamine compounds.Passage capacity test, obtained polyurea elastomer number-average molecular weight is 25000 or more, tensile strength is 10-30MPa, elongation at break is 550% or more, and carry out antiseptic property test to it: salt spray resistance reaches 4500h or more, surveys that its stretching strength retentivity is 90% or more, elongation at break is 450% or more after the aqueous solution of resistance to 0.1%NaOH 168h；Survey that its stretching strength retentivity is 90% or more, elongation at break is 500% or more after resistance to 2% aqueous sulfuric acid 168h；Measuring softening point by softening point instrument is 200 DEG C or more.
Description
Technical field
Technical field of the invention belongs to functional polymer material field, can apply using with plastics, rubber and coating etc.
In field.
Background technique
Carbamide resin is a kind of material with high performance, and mechanical property can be by elasticity to rigid body in extensive range
Interior variation, the comprehensive performances such as wearability, skid resistance and intensity are one of optimal selections in existing polymer material.Polyureas at present
Mainly there are the performed polymer of isocyanates and amine substance to react to obtain, since isocyanate-monomer needs to use when synthesis
To phosgene, phosgene is harmful to environment and human body to extremely toxic substance, and isocyanates itself is also extremely toxic substance, if instead
It not exclusively can should also injure the health of people.Therefore, in order to solve this problem, people are striving to find a kind of method substitution
Isocyanates avoids isocyanates and its raw material from causing damages human health.Then there is the method with non-isocyanate
Come synthesis of polyurethane and polyureas.The non-isocyanate method synthesis of polyurethane such as journey original, specially with epoxy resin in pressurization
Under the conditions of be passed through carbon dioxide synthesizing cyclic carbonate ester, then synthesize the polyurethane of non-isocyanate type with diamine reactant again, this
Method needs to carry out under high pressure, and the requirement to equipment is high, and technique is also more complicated.Zhao Jingbo etc. using cyclic carbonate ester monomer with
Then diamine reactant elder generation synthesis of carbamates oligomer is carrying out melt polycondensation, although being improved in this technique, no
With using high-tension apparatus, but such method yield is relatively low, and properties of product are defective.
In order to solve problem above, the synthetic route that the present invention finds a kind of completely new green is gathered to synthesize non-isocyanate
Urea elastomers, this programme are raw material without using high pressure gas, and synthesis technology is more easy, green.
Summary of the invention
It is an object of the invention to overcome the deficiencies of existing technologies, provide a kind of by simple, green, environmentally friendly road
The non-isocyanate polyurea elastomer of line synthesis, to solve the problems, such as that isocyanates toxicity is big, and obtains its comprehensive performance
To raising.
To achieve the above object, the technical scheme adopted by the invention is that: a kind of non-isocyanate polyurea elastomer is provided,
It is characterized by: formula composition includes: diamine compounds, dialkyl carbonate, amine terminated polyether；The dialkyl carbonate
With mol ratio 1:10 ~ 10:1 of diamine compounds.
The molecular formula of the non-isocyanate polyurea elastomer is as follows:
In formula:
R2 represents C1 ~ C18 fatty group or alicyclic group or aromatic series base；
R3 is polyether structure or alkylen structures.
The dialkyl carbonate, preferably dimethyl carbonate, diethyl carbonate and dipropyl carbonate it is one or more.
The diamine compounds, preferably ethylenediamine, 1,2- propane diamine, 1,3- propane diamine, Putriscine, 1,6- oneself two
Amine, 4, one of 4 diaminodiphenyl-methanes or a variety of.
The Amino End Group polymer, preferably one of D230, D400, D2000, D3000, T403 or a variety of.
The catalyst A is the oxide or simple substance or hydride or alcoholates or organic of alkali or alkaline earth metal
One of alkali, preferably potassium, potassium oxide, potassium methoxide, sodium, sodium oxide molybdena, sodium methoxide, TBD are a variety of.
The catalyst B is tin catalyst, titanium class catalyst, and tin catalyst is preferred: Dibutyltin oxide, octanoic acid
Stannous, dibutyl tin dilaurate it is one or more, titanium class catalyst is preferred: tetraethyl titanate, tetraisopropyl titanate, metatitanic acid
One of four butyl esters are a variety of.
The catalyst C is the preferred K2CO3, KCl of salt compounds of alkali or alkaline earth metal, Na2CO3, Na
Any one or more in Cl.
The non-isocyanate polyurea elastomer, prepares with the following method:
(1) diamine compounds, dialkyl carbonate are weighed by mass fraction, in temperature be 60 ~ 130 DEG C under catalyst A effect,
1 ~ 10h is reacted, rectifying goes out to react the alkylol generated, then increases temperature to 95 DEG C, and rectifying column tip temperature is 60 ~ 80 DEG C,
Rectifying object reaches theoretical amount after 2h, deviates from remaining dialkyl carbonate in the case where vacuum degree is -0.07MPa at this time, finally obtains
White needles powder；
Temperature described in the synthesis of alkyl diamino-methyl formate are as follows: 60 ~ 130 DEG C, the reaction time is 1 ~ 10 hour；
(2) white needles powder, the amine terminated polyether that (1) obtains are weighed by mass fraction, under catalyst B effect, normal pressure will
The fusing of white needles powder, is then added amine terminated polyether, in 80 ~ 200 DEG C of 1 ~ 10h of reaction, then in rough vacuum-
Deviate from alkylol under 0.07MPa, improves vacuum degree again to -0.097MPa after vacuumizing 2h, temperature is increased to 180 DEG C, continues to take out
Vacuum stops reaction, obtains flaxen non-isocyanate polyurea elastomer after viscosity does not change；The reaction temperature
Degree are as follows: 80 ~ 200 DEG C, the reaction time is 1 ~ 10 hour.
The synthesis of alkyl diamino-methyl formate in the step (1): dialkyl carbonate is at catalyst A certain
At a temperature of with diamine compounds occur ammonia esterification, deviate from alkylol, react a period of time after obtain the alkyl of small molecule
Diamino-methyl formate, reaction equation are as follows:
(1)
The R of above-mentioned formula (1)1Represent the fatty group or alicyclic group or aromatic series base of C1 ~ C8；
R2Represent C1 ~ C18 fatty group or alicyclic group or aromatic series base.
The polycondensation of non-isocyanate polyurea elastomer in the step (2) synthesizes: at a certain temperature, alkyl diamino
Under catalyst B effect polycondensation reaction occurs for methyl formate and Amino End Group polymer, deviates from alkylol, obtains after reacting a period of time
To a kind of required non-isocyanate polyurea elastomer, reaction equation is as follows:
(2)
The non-isocyanate polyurea elastomer can also be prepared using method two, be specifically comprised the following steps:
(1) diamine compounds, dialkyl carbonate, amine terminated polyether are weighed by mass fraction, under catalyst A effect, normal
Pressure reaction；
(2) temperature is then increased, rectifying, which goes out, reacts the alkylol generated, and rectifying column tip temperature is 60 ~ 80 DEG C, and rectifying goes out after 2h
Alkylol reach theoretical amount；
(3) another catalyst C is added at this time, is stepped up to 180 DEG C 120 DEG C of temperature, in the case where vacuum degree is -0.07MPa
Deviate from dialkyl carbonate；
(4) after there is no dialkyl carbonate to steam, temperature is gradually raised to 200 DEG C, and vacuum degree is mentioned-
0.097MPa, until viscosity stops reaction after not changing.
The step of the method two (1) is the synthesis of oligomer diamino-methyl formate, by diamine compounds and end ammonia
Based polyalcohol and dialkyl carbonate under catalyst A effect at a certain temperature with ammonia esterification occurs, deviate from alkylol,
The alkyl diamino-methyl formate of oligomer is obtained after reaction a period of time, reaction equation is as follows:
(3)
The temperature are as follows: 60 ~ 130 DEG C, the reaction time is 1 ~ 10 hour；
The step of the method two (2) is the melting of non-isocyanate polyurea elastomer from polycondensation: the alkyl diamino of oligomer
Melting occurs at a certain temperature at catalyst C for methyl formate from polycondensation, deviates from dialkyl carbonate, after reacting a period of time
A kind of non-isocyanate polyurea elastomer required for obtaining, reaction equation are as follows:
(4)
Traditional polyurea elastomer is easy to remain the complete isocyanate group of unreacted in product using isocyanates as raw material
Group, harmful to human body health, the non-isocyanate polyurea elastomer that this technique is synthesized is raw material without using isocyanates,
Prevent residual isocyanate groups in product.Dimethyl carbonate used in this application is that a kind of environmentally protective chemical industry is former
Material, phosgene, methylchloroformate, dimethyl suflfate of alternative severe toxicity etc. are used as methylating agent or carbonyl agent, improve life
The safety of operation is produced, environmental pollution is reduced.Entire synthesis process " zero-emission ", does not use organic solvent, synthesis process
In, dimethyl carbonate reacts methanol removal with amino-compound, after Methanol Recovery, can be used as the original for preparing dimethyl carbonate
Material, recycles, and is a kind of environmental-friendly technical process.
Passage capacity test, obtained polyurea elastomer number-average molecular weight are 25000 or more, tensile strength 10-
30MPa, elongation at break is 550% or more, and carries out antiseptic property test to it: salt spray resistance reaches 4500h or more, and resistance to 0.1%
Survey that its stretching strength retentivity is 90% or more, elongation at break is 450% or more after NaOH aqueous solution 168h；Resistance to 2% sulfuric acid is water-soluble
Survey that its stretching strength retentivity is 90% or more, elongation at break is 500% or more after liquid 168h；It is measured and is softened by softening point instrument
Point is 200 DEG C or more.
The beneficial effects of the present invention are: the non-isocyanate polyurea elastomer that this technique is synthesized is without using isocyanates
For raw material, raw material are environmentally protective；Reaction condition is mild, technical process gradual change, without filtering and purification, it is easy to accomplish industry
Change；Each step reaction used catalyst system simple and stable, and be commercial product, it is cheap and easy to get, it need not be separated after.
Specific embodiment
Below by specific embodiment narration product of the present invention and preparation method thereof.Embodiment is interpreted as illustrating
Property, the range being not intended to limit the present invention.For a person skilled in the art, without departing substantially from spirit and scope of the present invention
Under the premise of, protection scope of the present invention is belonged to the various changes of material component and dosage progress in these embodiments.
Embodiment 1
7.4 parts of 1,3 propane diamine, 54 parts of dimethyl carbonate, 0.1 part of sodium methoxide and 10 parts of methanol are weighed by mass fraction, in normal pressure
4h is reacted at 70 DEG C, then increases the temperature to 88 DEG C, and rectifying, which goes out, reacts the methanol generated, and rectifying column tip temperature is 63 DEG C, 2h
Rectifying object reaches theoretical amount afterwards, deviates from remaining dimethyl carbonate in the case where vacuum degree is -0.07MPa at this time, finally obtains white
Needle powder, yield 65%.
15.2 parts of the white needles powder that embodiment 1 obtains, 65 parts of amine terminated polyether D800 are weighed by mass fraction, and
0.1 part of dibutyl tin dilaurate.Under normal pressure, white needles powder is melted, amine terminated polyether is then added, at 120 DEG C
0.5h is reacted, then deviates from methanol at rough vacuum -0.07MPa, vacuumizes and improves vacuum degree after 2h again to -0.097MPa,
Temperature is increased to 180 DEG C, continues to vacuumize, and after viscosity does not change, stops reaction, it is poly- to obtain flaxen non-isocyanate
Urea elastomers.Measuring softening point by softening point instrument is 260 DEG C.Passage capacity test, the obtained equal molecule of polyurea elastomer number
Amount is 41300, tensile strength 17MPa, elongation at break 660%, and carries out antiseptic property test to it: salt spray resistance reaches
Surveyed after 5800h, the aqueous solution of resistance to 0.1%NaOH 168h its stretching strength retentivity be 95%, elongation at break 560%；Resistance to 2% sulfuric acid
Surveyed after aqueous solution 168h its stretching strength retentivity be 97%, elongation at break 600%.
Embodiment 2
13.2 parts of Isosorbide-5-Nitrae butanediamine, 54 parts of dimethyl carbonate, 0.7 part of potassium and 20 parts of methanol are weighed by mass fraction, at 70 DEG C of normal pressure
Then lower reaction 4h increases the temperature to 88 DEG C, rectifying, which goes out, reacts the methanol generated, and rectifying column tip temperature is 63 DEG C, smart after 2h
It evaporates object and reaches theoretical amount, deviate from remaining dimethyl carbonate in the case where vacuum degree is -0.07MPa at this time, finally obtain white needles
Powder, yield 70%.
24.48 parts of the white needles powder that embodiment 2 obtains, 50.4 parts of amine terminated polyether D400 are weighed by mass fraction
With 0.3 part of butyl titanate.Under normal pressure, white needles powder is melted, amine terminated polyether is then added, reacted at 120 DEG C
Then 0.5h deviates from methanol at rough vacuum -0.07MPa, improve vacuum degree again to -0.097MPa, temperature after vacuumizing 2h
180 DEG C are increased to, continues to vacuumize, after viscosity does not change, stops reaction, obtains flaxen non-isocyanate polyureas bullet
Property body.Measuring softening point by softening point instrument is 230 DEG C.Passage capacity test, obtained polyurea elastomer number-average molecular weight are
33800, tensile strength 24MPa, elongation at break 530%, and antiseptic property test is carried out to it: salt spray resistance reaches
Surveyed after 5000h, the aqueous solution of resistance to 0.1%NaOH 168h its stretching strength retentivity be 92%, elongation at break 450%；Resistance to 2% sulfuric acid
Surveyed after aqueous solution 168h its stretching strength retentivity be 95%, elongation at break 480%.
Embodiment 3
10 parts of 1,6 hexamethylene diamine, 46.5 parts of dimethyl carbonate, 0.05 part of potassium methoxide and 15 parts of methanol are weighed by mass fraction, normal
4h to be reacted at 70 DEG C of pressure, then increases the temperature to 88 DEG C, rectifying, which goes out, reacts the methanol generated, and rectifying column tip temperature is 63 DEG C,
Rectifying object reaches theoretical amount after 2h, deviates from remaining dimethyl carbonate in the case where vacuum degree is -0.07MPa at this time, finally obtains white
Color needle powder, yield 52%.
By mass fraction weigh 18 parts of the white needles powder that embodiment 3 obtains, 82.87 parts of amine terminated polyether D2000 and
0.5 part of stannous octoate.Under normal pressure, white needles powder is melted, amine terminated polyether is then added, in 120 DEG C of reaction 0.5h,
Then deviate from methanol at rough vacuum -0.07MPa, improve vacuum degree again to -0.097MPa after vacuumizing 2h, temperature is increased to
180 DEG C, continue to vacuumize, after viscosity does not change, stops reaction, obtain flaxen non-isocyanate polyurea elastomer.
Measuring softening point by softening point instrument is 200 DEG C.Passage capacity test, obtained polyurea elastomer number-average molecular weight are 48600,
Tensile strength is 13MPa, elongation at break 750%, and antiseptic property test is carried out to it: salt spray resistance reaches 5000h, resistance to
Surveyed after 0.1%NaOH aqueous solution 168h its stretching strength retentivity be 94%, elongation at break 670%；Resistance to 2% aqueous sulfuric acid
Surveyed after 168h its stretching strength retentivity be 96%, elongation at break 720%.
Embodiment 4
By mass fraction weigh 1.76 parts of 1,3 propane diamine, 90 parts of dimethyl carbonate, 285.7 parts of amine terminated polyether D2000,
CH32 parts of ONa and CH310 parts of OH, 6h is reacted at 70 DEG C of normal pressure, then increases the temperature to 92 DEG C, rectifying goes out to react generation
CH3OH, rectifying column tip temperature are 63 DEG C, the CH that rectifying goes out after 2h3OH reaches theoretical amount.Another catalyst is added at this time
K2CO32 parts, temperature is stepped up to 130 DEG C, first rough vacuum is to deviate from dimethyl carbonate under -0.07MPa, when not having carbon
After dimethyl phthalate steams, temperature is gradually raised to 200 DEG C, and vacuum degree is mentioned -0.97MPa, until viscosity does not change
Stop reaction afterwards.Measuring softening point by softening point instrument is 180 DEG C.Passage capacity test, obtained polyurea elastomer number are divided equally
Son amount is 25200, tensile strength 11MPa, elongation at break 870%, and carries out antiseptic property test: salt spray resistance to it
Up to 4500h, surveyed after the aqueous solution of resistance to 0.1%NaOH 168h its stretching strength retentivity be 90%, elongation at break 740%；Resistance to 2% sulphur
Surveyed after aqueous acid 168h its stretching strength retentivity be 92%, elongation at break 800%.
Embodiment 5
2.75 parts of 1,4 butanediamine, 135 parts of dimethyl carbonate, 175 parts of amine terminated polyether D800, CH are weighed by mass fraction3ONa
1.8 parts and CH310 parts of OH, 6h is reacted at 70 DEG C of normal pressure, then increases the temperature to 92 DEG C, rectifying goes out to react the CH generated3OH,
Rectifying column tip temperature is 63 DEG C, the CH that rectifying goes out after 2h3OH reaches theoretical amount.Another catalyst KOH 1.5 is added at this time
Part, temperature is stepped up to 130 DEG C, first rough vacuum is to deviate from dimethyl carbonate under -0.07MPa, when not having carbonic acid diformazan
After ester steams, temperature is gradually raised to 200 DEG C, and vacuum degree is mentioned -0.97MPa, until viscosity stops after not changing
Reaction.Measuring softening point by softening point instrument is 220 DEG C.Passage capacity test, obtained polyurea elastomer number-average molecular weight are
31800, tensile strength 17MPa, elongation at break 710%, and antiseptic property test is carried out to it: salt spray resistance reaches
Surveyed after 6000h, the aqueous solution of resistance to 0.1%NaOH 168h its stretching strength retentivity be 96%, elongation at break 680%；Resistance to 2% sulfuric acid
Surveyed after aqueous solution 168h its stretching strength retentivity be 98%, elongation at break 690%.
Embodiment 6
By mass fraction weigh 2.49 parts of 1,6 hexamethylene diamine, 81 parts of dimethyl carbonate, 42.86 parts of amine terminated polyether D400,
CH30.5 part of ONa and CH35 parts of OH, 6h is reacted at 70 DEG C of normal pressure, then increases the temperature to 92 DEG C, rectifying goes out to react generation
CH3OH, rectifying column tip temperature are 63 DEG C, the CH that rectifying goes out after 2h3OH reaches theoretical amount.Another catalyst is added at this time
Na2CO31 part, temperature is stepped up to 130 DEG C, first rough vacuum is to deviate from dimethyl carbonate under -0.07MPa, when not having carbon
After dimethyl phthalate steams, temperature is gradually raised to 200 DEG C, and vacuum degree is mentioned -0.97MPa, until viscosity does not change
Stop reaction afterwards.Measuring softening point by softening point instrument is 270 DEG C.Passage capacity test, obtained polyurea elastomer number are divided equally
Son amount is 35500, tensile strength 25MPa, elongation at break 600%, and carries out antiseptic property test: salt spray resistance to it
Up to 6500h, surveyed after the aqueous solution of resistance to 0.1%NaOH 168h its stretching strength retentivity be 97%, elongation at break 580%；Resistance to 2% sulphur
Surveyed after aqueous acid 168h its stretching strength retentivity be 99%, elongation at break 590%.
Claims (9)
1. a kind of non-isocyanate polyurea elastomer, it is characterised in that: formula composition includes: diamine compounds, dialkyl carbonate
Base ester, amine terminated polyether；Mol ratio 1:10 ~ 10:1 of the dialkyl carbonate and diamine compounds；The non-isocyanide
The molecular formula of acid esters polyurea elastomer is as follows:
In formula: R2Represent C1 ~ C18 fatty group or alicyclic group or aromatic series base；
R3For polyether structure or alkylen structures.
2. a kind of non-isocyanate polyurea elastomer according to claim 1, it is characterised in that: the dialkyl carbonate
Ester, preferably dimethyl carbonate, diethyl carbonate and dipropyl carbonate it is one or more.
3. a kind of non-isocyanate polyurea elastomer according to claim 1, it is characterised in that: the Diamines chemical combination
Object, preferably ethylenediamine, 1,2- propane diamine, 1,3- propane diamine, Putriscine, 1,6- hexamethylene diamine, 4,4 diaminodiphenyl-methanes
It is one or more.
4. a kind of non-isocyanate polyurea elastomer according to claim 1, it is characterised in that: the Amino End Group polymerization
Object, preferably D230, D400, D2000, D3000, T403's is one or more.
5. a kind of non-isocyanate polyurea elastomer according to claim 1, it is characterised in that: the catalyst A is alkali metal
Or the oxide or simple substance or hydride or alcoholates or organic base of alkaline-earth metal, preferably potassium, potassium oxide, potassium methoxide, sodium, oxygen
Change sodium, sodium methoxide, TBD it is one or more.
6. a kind of non-isocyanate polyurea elastomer according to claim 1, it is characterised in that: the catalyst B is that tin class is urged
Agent, titanium class catalyst；Tin catalyst is preferred: Dibutyltin oxide, stannous octoate, dibutyl tin dilaurate one kind or
A variety of, titanium class catalyst is preferred: tetraethyl titanate, tetraisopropyl titanate, butyl titanate it is one or more.
7. a kind of non-isocyanate polyurea elastomer according to claim 1, it is characterised in that: the catalyst C is alkali metal
Or the salt compounds of alkaline-earth metal, preferably K2CO3、KCl、Na2CO3、, any one or more in Na Cl.
8. a kind of non-isocyanate polyurea elastomer according to claim 1, it is characterised in that: the non-isocyanate is poly-
Urea elastomers are prepared with the following method:
(1) diamine compounds, dialkyl carbonate are weighed by mass fraction, is 60 ~ 130 in temperature under catalyst A effect
DEG C, 1 ~ 10h is reacted, rectifying goes out to react the alkylol generated, then increases temperature to 95 DEG C, rectifying column tip temperature is 60 ~ 80
DEG C, rectifying object reaches theoretical amount after 2h, deviates from remaining dialkyl carbonate in the case where vacuum degree is -0.07MPa at this time, final to obtain
To white needles powder；
Temperature described in the synthesis of alkyl diamino-methyl formate are as follows: 60 ~ 130 DEG C, the reaction time is 1 ~ 10 hour；
(2) white needles powder, the amine terminated polyether that (1) obtains are weighed by mass fraction, under catalyst B effect, normal pressure will
The fusing of white needles powder, is then added amine terminated polyether, in 80 ~ 200 DEG C of 1 ~ 10h of reaction, then in rough vacuum-
Deviate from alkylol under 0.07MPa, improves vacuum degree again to -0.097MPa after vacuumizing 2h, temperature is increased to 180 DEG C, continues to take out
Vacuum stops reaction, obtains flaxen non-isocyanate polyurea elastomer after viscosity does not change；The reaction temperature
Degree are as follows: 80 ~ 200 DEG C, the reaction time is 1 ~ 10 hour.
9. a kind of non-isocyanate polyurea elastomer according to claim 1, it is characterised in that: the non-isocyanate is poly-
Urea elastomers are prepared with the following method:
(1) diamine compounds, dialkyl carbonate, amine terminated polyether are weighed by mass fraction, under catalyst A effect, often
Pressure reaction；
(2) temperature is then increased, rectifying, which goes out, reacts the alkylol generated, and rectifying column tip temperature is 60 ~ 80 DEG C, and rectifying goes out after 2h
Alkylol reach theoretical amount；
(3) another catalyst C is added at this time, temperature is stepped up to 180 DEG C from 120 DEG C, is -0.07MPa in vacuum degree
Lower abjection dialkyl carbonate；
(4) after there is no dialkyl carbonate to steam, temperature is gradually raised to 200 DEG C, and vacuum degree is mentioned -0.97MPa,
Until viscosity stops reaction after not changing.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112011049A (en) * | 2019-05-30 | 2020-12-01 | 中国科学院化学研究所 | Thermoplastic polyurea elastomer and preparation method thereof |
| CN116253876A (en) * | 2022-12-19 | 2023-06-13 | 北京东方雨虹防水技术股份有限公司 | Non-isocyanate polyurea material and preparation method and application thereof |
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| CN107400233A (en) * | 2016-05-18 | 2017-11-28 | 北京化工大学 | The method that one kettle way prepares non-isocyanate thermoplasticity polyureas |
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| JPH0873411A (en) * | 1994-09-02 | 1996-03-19 | Mitsubishi Chem Corp | Production of dialkyl carbonate |
| CN1796439A (en) * | 2004-12-23 | 2006-07-05 | 华东理工大学 | Environment friendly method for synthesizing polyurethane |
| CN104513393A (en) * | 2013-09-28 | 2015-04-15 | 北京化工大学 | Method for preparing biodegradable thermoplastic poly(ether-urethane) by employing a non-isocyanate process |
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| CN112011049A (en) * | 2019-05-30 | 2020-12-01 | 中国科学院化学研究所 | Thermoplastic polyurea elastomer and preparation method thereof |
| CN116253876A (en) * | 2022-12-19 | 2023-06-13 | 北京东方雨虹防水技术股份有限公司 | Non-isocyanate polyurea material and preparation method and application thereof |
| CN116253876B (en) * | 2022-12-19 | 2024-04-26 | 北京东方雨虹防水技术股份有限公司 | Non-isocyanate polyurea material and preparation method and application thereof |
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