CN104892882B - A kind of transparent polyurethane material and preparation method thereof - Google Patents
A kind of transparent polyurethane material and preparation method thereof Download PDFInfo
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- CN104892882B CN104892882B CN201410072186.1A CN201410072186A CN104892882B CN 104892882 B CN104892882 B CN 104892882B CN 201410072186 A CN201410072186 A CN 201410072186A CN 104892882 B CN104892882 B CN 104892882B
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- 239000004814 polyurethane Substances 0.000 title claims abstract description 48
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 47
- 239000000463 material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 claims abstract description 44
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 claims abstract description 23
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 11
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical class C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012948 isocyanate Substances 0.000 claims abstract description 11
- 239000004970 Chain extender Substances 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 238000005266 casting Methods 0.000 claims abstract description 6
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 6
- -1 aliphatic isocyanates Chemical class 0.000 claims abstract description 5
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 229920006264 polyurethane film Polymers 0.000 claims description 9
- 150000002513 isocyanates Chemical class 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 7
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 3
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 3
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 3
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 3
- 125000000969 xylosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)CO1)* 0.000 claims description 2
- 238000010345 tape casting Methods 0.000 claims 4
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- 239000003513 alkali Substances 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- 125000005442 diisocyanate group Chemical group 0.000 abstract description 2
- 239000005336 safety glass Substances 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 150000003742 xyloses Chemical class 0.000 abstract 1
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- 239000002994 raw material Substances 0.000 description 8
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 description 5
- 239000012528 membrane Substances 0.000 description 5
- 239000002362 mulch Substances 0.000 description 5
- 229920006255 plastic film Polymers 0.000 description 5
- 239000002985 plastic film Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- WBYWAXJHAXSJNI-VOTSOKGWSA-M .beta-Phenylacrylic acid Natural products [O-]C(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-M 0.000 description 3
- WBYWAXJHAXSJNI-SREVYHEPSA-N Cinnamic acid Chemical compound OC(=O)\C=C/C1=CC=CC=C1 WBYWAXJHAXSJNI-SREVYHEPSA-N 0.000 description 3
- 229930016911 cinnamic acid Natural products 0.000 description 3
- 235000013985 cinnamic acid Nutrition 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- WBYWAXJHAXSJNI-UHFFFAOYSA-N methyl p-hydroxycinnamate Natural products OC(=O)C=CC1=CC=CC=C1 WBYWAXJHAXSJNI-UHFFFAOYSA-N 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- LUZSPGQEISANPO-UHFFFAOYSA-N butyltin Chemical compound CCCC[Sn] LUZSPGQEISANPO-UHFFFAOYSA-N 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical group NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical class CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000003827 glycol group Chemical group 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical class OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- 229940051250 hexylene glycol Drugs 0.000 description 1
- SVTBMSDMJJWYQN-UHFFFAOYSA-N hexylene glycol Natural products CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000005474 octanoate group Chemical group 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920005906 polyester polyol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920003225 polyurethane elastomer Polymers 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
Landscapes
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention belongs to polyurethane high molecule Material Field, it is related to a kind of transparent polyurethane material and preparation method, transparent polyurethane material using acetone as solvent, ethylene glycol is chain extender, stannous octoate is catalyst, is prepared by xylose, aliphatic isocyanates polymerization.Preparation method：（In terms of mass parts）, using 900 ~ 1300 parts of tetrahydrofurans as reaction dissolvent, by 20 ~ 50 parts of xyloses（Moisture is less than 0.003%）With 80 ~ 150 parts of diisocyanate, reacted under catalyst and chain extender effect, can obtain polyurethane solutions, by the solution on polyfluortetraethylene plate casting film-forming, and solidify 6 10h at room temperature, you can obtain transparent polyurethane material.The polyurethane material of synthesis has acid resistance, alkali resistance, translucency, good oil resistivity and mechanical performance.Lampshade, safety glass before and after automobile, instrument and equipment and commodity external coating can be used as, plays the protection on the surfaces such as dust-proof, oil-stain-preventing, anti-corrosion.
Description
Technical field
The invention belongs to polyurethane-type high polymer material, and in particular to a kind of transparent polyurethane material and preparation method thereof.
Background technology
Polyurethane (PU) excellent performance, product species is more, is widely used in automobile, electrical equipment, building, machinery, light industry, doctor
The field such as treatment and Aero-Space, but the optical transparence of common polyurethane material is low, and heat resistance is poor, makes answering for some aspects
With the continuous expansion by a definite limitation, applied with automobile, transparent devices, space flight and aviation, medical equipment, security protection etc.
Exhibition, the both at home and abroad research to transparent polyurethane material are increasingly taken seriously, and transparent polyurethane develops as polyurethane in recent years
A recent studies on direction, United States Patent (USP) US693993982, US0017268A1, US7216976B2, US0000656Al,
US0281965AI, US2008017119 and Chinese patent 201210374773.7,201210072896.5,
201210336914.6 and Xue Feng etc.（The synthesis of transparent casting polyurethane resin material and performance study [J] the Central China University of Science and Technology are learned
Report (natural science edition), 2004,32 (7):98-101）, Chao Youming（The preparation of the transparent membrane material of one pack system quick-drying type polyurethane
Institutes Of Technology Of Taiyuan's journal, 2007,38 (4):324-327）, Wang Hua（The preparation of transparent polyurethane material and research (D), Xi'an
University of Science and Technology .2007.04.20）, Zhang Xiaohua etc.（Study on the synthesis [J] the plastics industries of high-performance polyurethane elastomer
2002,30(6):8-11）, Xue Shue etc.（The development polyurethane industrials .2007,22 (3) of high-hard, transparent polyurethane material:
37-40）, Chen Yuhong（The shaping of transparent polyurethane film and application study [J] engineering plastics application .2002,30 (3):35-
37）, prepared by transparent polyurethane and has been studied, but these transparent polyurethanes are with PPG or polyester polyols
Alcohol and isocyanates react and prepared, the application material that the transparent polyurethane material of preparation can be not high as transparency requirement
Material, the substitute of common optical glass, applied to window, front and rear lampshade before and after being made in automobile, aircraft, it can also be used to make glasses
The optics such as piece, safety glass, protective glasses.
The present invention seeks to reacted using xylose as raw material with aliphatic isocyanates and alicyclic isocyanate to make
Standby transparent polyurethane, xylose are to extract to prepare from the stalk, core, shell of natural plants, and raw material sources are extensive, are renewable money
Source, the utilization rate of resource can not only be improved by preparing polyurethane as raw material using xylose, and be provided inexpensively for polyurethane industrial
Raw material sources, the dependence to oil product is reduced, reduces cost, there is highly important reality to anticipate development polyurethane industrial
Justice.
The content of the invention
There is preferably transparent, excellent acidproof, alkali resistance, good mechanical property the purpose of the present invention is to propose to a kind of
Can polyurethane material and preparation method, transparent polyurethane be to be copolymerized polymerizeing of being formed with hard section diisocyanate by soft segment xylose
Thing.
The transparent polyurethane material of the present invention by xylose, isocyanates, solvent, chain extender, polymerize under catalyst action
It is prepared.The isocyanates is IPDI, hexamethylene diisocyanate, 4,4- dicyclohexyl first
Alkane diisocyanate, XDI, the solvent are tetrahydrofuran, acetone, ethyl acetate, N-N dimethyl
Formamide, the chain extender are ethylene glycol, BDO, 1,2-PD, 1,6- hexylene glycols, and the catalyst is two bays
Sour dibutyl tin, stannous octoate.
The transparent polyurethane material preparation method is：900 ~ 1300mL of tetrahydrofuran is first added to reactor by proportioning
In, reactor is vacuumized, xylose 30g, 80 ~ 150g of isocyanates is added under nitrogen protection, 30- is stirred at room temperature
0.03 ~ 0.05g of dibutyl tin laurate is added after 60min, reactor is warming up to 30 ~ 80 DEG C, continues 1 ~ 3h of stirring, with two just
NCO content in butylamine hair detection solution, when NCO content is 15 ~ 18,15 ~ 30g of ethylene glycol is added into reactor, continues to stir
15 ~ 60nim of reaction is mixed, removal of solvent under reduced pressure, obtains transparent viscous solution, with stream method is prolonged by clear solution plastic film mulch, in room temperature
Under the conditions of dry 6 ~ 10h, that is, can obtain transparent polyurethane film.The polyurethane film of preparation have translucency, acid resistance, alkali resistance,
Good mechanical performance.
The beneficial effects of the invention are as follows：React by raw material and isocyanates of xylose and prepare transparent polyurethane, xylose
It is to extract to prepare from the stalk, core, shell of natural plants, raw material sources are extensive, are renewable resources, prepared by raw material of xylose
Polyurethane can not only improve the utilization rate of resource, and cheap raw material sources are provided for polyurethane industrial, reduce to oil
The dependence of product, reduces cost, and development polyurethane industrial is of great practical significance.
Brief description of the drawings
Fig. 1 is the infrared spectrogram of transparent polyurethane film and xylose.
Embodiment
Below by embodiment, the present invention is described further, but the scope of protection of present invention is not limited to
The scope of embodiment expression.
Embodiment 1
According to the preparation method of the polyurethane of the present embodiment, it comprises the following steps：Ethyl acetate 900mL is added to instead
Answer in kettle, to reaction system vacuumize process, add xylose 30g and IPDI under nitrogen protection
90.06g, stir at room temperature and react 30min, catalyst dibutyltin cinnamic acid two is then added into the reaction system for continuing stirring
Butyl tin 0.032g, oil bath are warming up to 50 DEG C, react 3.0h, the content of-NCO in solution are detected with di-n-butylamine method, as-NCO
Content when reaching 15 ~ 18%, chain extender BDO 20.12g is added into reactor, continues to react 30min, decompression removes
Ethyl acetate solvent is removed, obtains transparent viscous solution, by prolonging stream method by transparent viscous solution plastic film mulch, in the condition of room temperature
Lower solidification 7h, obtains transparent polyurethane membrane material.
Embodiment 2
According to the preparation method of the polyurethane of the present embodiment, it comprises the following steps：Tetrahydrofuran 1280mL is added to
In reactor, to reaction system vacuumize process, xylose 30g and hexamethylene diisocyanate are added under nitrogen protection
148.6g, stir at room temperature and react 60min, octoate catalyst stannous is then added into the reaction system for continuing stirring
0.048g, oil bath are warming up to 70 DEG C, react 2.5h, the content of-NCO in solution are detected with di-n-butylamine method, when-NCO content
When reaching 15 ~ 18%, chain extender 1 is added into reactor, 6- hexylene glycol 29.12g, continues to react 15min, tetrahydrochysene is removed under reduced pressure
THF solvent, transparent viscous solution is obtained, by prolonging stream method by transparent viscous solution plastic film mulch, solidified under conditions of room temperature
10h, obtain transparent polyurethane membrane material.
Embodiment 3
According to the preparation method of the polyurethane of the present embodiment, it comprises the following steps：Acetone 990mL is added to reactor
In, to reaction system vacuumize process, xylose 30g and 4,4- dicyclohexyl methyl hydride diisocyanate are added under nitrogen protection
110.35g, stir at room temperature and react 40min, catalyst dibutyltin cinnamic acid is then added into the reaction system for continuing stirring
Dibutyl tin 0.035g, oil bath are warming up to 80 DEG C, react 1h, the content of-NCO in solution are detected with di-n-butylamine method, as-NCO
Content when reaching 15 ~ 18%, chain extender 1,2-PD 15.10g is added into reactor, continues to react 45min, decompression removes
Acetone solvent is removed, obtains transparent viscous solution, it is solid under conditions of room temperature by prolonging stream method by transparent viscous solution plastic film mulch
Change 6h, obtain transparent polyurethane membrane material.
Embodiment 4
According to the preparation method of the polyurethane of the present embodiment, it comprises the following steps：By N-N dimethylformamides 1110mL
It is added in reactor, to reaction system vacuumize process, adds xylose 30g and the isocyanide of phenylenedimethylidyne two under nitrogen protection
Acid esters 125.16g, 50min is stirred at room temperature, catalyst dibutyltin cinnamic acid two is then added into the reaction system for continuing stirring
Butyl tin 0.041g, oil bath are warming up to 35 DEG C, react 2h, the content of-NCO in solution are detected with di-n-butylamine method, when-NCO's
When content reaches 15 ~ 18%, glycol chain extender 25.05g is added into reactor, continues to react 60min, N-N bis- is removed under reduced pressure
NMF solvent, transparent viscous solution is obtained, by prolonging stream method by transparent viscous solution plastic film mulch, in the condition of room temperature
Lower solidification 9h, obtains transparent polyurethane membrane material.
Tensile strength is carried out by GB/T 2568-1995 to gained polyurethane film in embodiment 1-4 and elongation at break is surveyed
Amount, the optical transparence test light transmittance of UV-7500 types ultraviolet-visible spectrophotometer measurement sample, sample thickness 10
Mm, acidproof and alkali resistance is carried out to transparent polyurethane film and tested, test result is shown in Table 1.
The polyurethane film performance of table 1
Refering to Fig. 1, b is xylose infrared absorpting light spectra in figure, in 3521.6cm-1And 3128cm-1The relatively strong absorption occurred
Peak, it is the stretching vibration absworption peak of hydroxyl.A is transparent polyurethane infrared absorpting light spectra in figure, the infared spectrum phase with xylose
Than in 3384.5cm-1Absworption peak substantially weaken, illustrate that the hydroxyl on xylose take part in reaction, in 1731.8cm in figure-1
There is stronger absworption peak in place, is-C=O in the carbamate groups that system generates（Urethane carbonyl）Stretching vibration absworption peak,
Illustrate that-the OH in-NCO and xylose in isocyanates is reacted, i.e., xylose has participated in reaction and has been introduced in polyurethane point
In the main chain of son, in 3384.5cm-1The stretching vibration absworption peak of place's hydroxyl substantially weakens, and the hydroxyl on further explanation xylose is
Reaction is take part in, xylose has been connected to form polymer with isocyanates.
Claims (4)
1. a kind of preparation method of transparent polyurethane material, it is characterised in that step and condition are as follows：
By proportioning, first solvent is added in three-necked flask, to being vacuumized in three-necked flask, added under nitrogen protection sugared and different
Cyanate, 10 ~ 45min is stirred at room temperature, adds catalyst, heat up and 0.5 ~ 2h of reaction is carried out at 50 ~ 80 DEG C, wherein, it is sugared and more
OH/NCO mol ratios in first isocyanates are 0.5 ~ 0.9:1, when-NCO content reaches 10 ~ 18%, added into three-necked flask
Chain extender, continue 15 ~ 30min of reaction, stop reaction, removal of solvent under reduced pressure, obtain transparent viscous solution, will by the tape casting
Solution casting film-forming on polyfluortetraethylene plate, and solidify 6 ~ 12h at room temperature, you can obtain polyurethane transparent film；It is described
Sugar is xylose.
A kind of 2. preparation method of transparent polyurethane material according to claim 1, it is characterised in that：Synthesis step and bar
Part is as follows：
First tetrahydrofuran 1150mL is added in three-necked flask, to being vacuumized in three-necked flask, adds sugar under nitrogen protection
40g and IPDI 146.65g, 15min is stirred at room temperature, add dibutyl tin laurate 0.03g, heating
To 50 DEG C of reaction 2h, with the content of-NCO in di-n-butylamine method measure solution, when-NCO content reaches 10 ~ 13%, Xiang Sankou
BDO 12.65g is added in flask, continues to react 20min, stops reaction, removal of solvent under reduced pressure, obtains transparent sticky
Solution, by the tape casting by the solution casting film-forming on polyfluortetraethylene plate, and solidify 6h at room temperature, you can obtain transparent
Polyurethane film.
A kind of 3. preparation method of transparent polyurethane material according to claim 1, it is characterised in that：Synthesis step and bar
Part is as follows：
First N, dinethylformamide 950mL are added in three-necked flask, to being vacuumized in three-necked flask, under nitrogen protection
Sugared 40g and hexamethylene diisocyanate 95.65g is added, stirs 30min at room temperature, stannous octoate 0.04g is added, is warming up to
70 DEG C of reaction 1h, the content of-NCO in solution is determined with di-n-butylamine method, when-NCO content reaches 12 ~ 15%, is burnt to three mouthfuls
Ethylene glycol 16.38g is added in bottle, continues to react 15min, stops reaction, removal of solvent under reduced pressure, obtain transparent viscous solution,
By the tape casting by the solution casting film-forming on polyfluortetraethylene plate, and solidify 8h at room temperature, you can obtain transparent poly- ammonia
Ester film.
A kind of 4. preparation method of transparent polyurethane material according to claim 1, it is characterised in that：Synthesis step and bar
Part is as follows：
First acetone 1250mL is added in three-necked flask, to being vacuumized in three-necked flask, add under nitrogen protection sugared 40g and
4,4 '-dicyclohexyl methyl hydride diisocyanate 116.35g, 45min is stirred at room temperature, add dibutyl tin laurate
0.05g, be warming up to 80 DEG C of reaction 1.5h, the content of-NCO in solution determined with di-n-butylamine method, when-NCO content reaches 16 ~
When 18%, 1,2-PD 18.15g is added into three-necked flask, continues to react 30min, stops reaction, removal of solvent under reduced pressure, obtain
To transparent viscous solution, by the tape casting by the solution casting film-forming on polyfluortetraethylene plate, and solidify at room temperature
10h, you can obtain transparent polyurethane film.
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| CN105254837A (en) * | 2015-11-12 | 2016-01-20 | 淄博德信联邦化学工业有限公司 | Polyurethane transparent skin material and preparing method thereof |
| CN108699385A (en) * | 2016-02-29 | 2018-10-23 | 科思创聚合物（中国）有限公司 | surface protection composition |
| CN106681049A (en) * | 2017-03-23 | 2017-05-17 | 合肥鑫晟光电科技有限公司 | Manufacturing method of display substrate, manufacturing method of display panel and display panel |
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| Title |
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| 木糖醇芳香型聚氨酯的制备及性能研究;龚伟;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20131215(第S2（2013）期);第2.2.3和2.3.7节 * |
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| CN104892882A (en) | 2015-09-09 |
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