CN104877315B - A kind of preparation method of high barrier poly lactic acid nano composite material - Google Patents
A kind of preparation method of high barrier poly lactic acid nano composite material Download PDFInfo
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- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 63
- 239000004626 polylactic acid Substances 0.000 title claims abstract description 63
- 230000004888 barrier function Effects 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 34
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 33
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 43
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000000178 monomer Substances 0.000 claims abstract description 24
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 23
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 229920001610 polycaprolactone Polymers 0.000 claims abstract description 18
- 239000004632 polycaprolactone Substances 0.000 claims abstract description 18
- 238000009830 intercalation Methods 0.000 claims abstract description 10
- 230000002687 intercalation Effects 0.000 claims abstract description 10
- 239000003999 initiator Substances 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001301 oxygen Substances 0.000 claims abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 7
- 238000005453 pelletization Methods 0.000 claims abstract description 7
- 229920002545 silicone oil Polymers 0.000 claims abstract description 7
- 241000446313 Lamella Species 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000007789 sealing Methods 0.000 claims abstract 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 3
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 235000011150 stannous chloride Nutrition 0.000 claims description 3
- 239000001119 stannous chloride Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- OQBLGYCUQGDOOR-UHFFFAOYSA-L 1,3,2$l^{2}-dioxastannolane-4,5-dione Chemical compound O=C1O[Sn]OC1=O OQBLGYCUQGDOOR-UHFFFAOYSA-L 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 2
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 claims description 2
- 150000004032 porphyrins Chemical class 0.000 claims description 2
- 230000004044 response Effects 0.000 claims description 2
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical group [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 2
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 claims description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 239000011159 matrix material Substances 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 238000006116 polymerization reaction Methods 0.000 abstract description 3
- 238000005406 washing Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000010410 layer Substances 0.000 description 9
- 239000006185 dispersion Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000002023 wood Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Biological Depolymerization Polymers (AREA)
Abstract
The present invention discloses the preparation method of a kind of high barrier poly lactic acid nano composite material, comprise the steps, (1) in the dry flask removing oxygen, add caprolactone monomer and montmorillonite, sealing and standing after ultrasonic vibration, make caprolactone monomer be adequately inserted in the lamella of montmorillonite, initiator is added in flask, heating carries out intercalation polymeric reaction, the product obtained is dissolved in toluene, centrifugation after supersonic vibration, it is dried through toluene washing, obtains Polycaprolactone modified montmorillonite；(2) make polylactic acid and silicone oil mixing, add Polycaprolactone modified montmorillonite mixed at high speed, then by extruder extruding pelletization, obtain intercepting master batch；(3) master batch and polylactic acid mix homogeneously will be intercepted, after melt blending, i.e. obtain high barrier poly lactic acid nano composite material.Use caprolactone in-situ intercalative polymerization modified montmorillonoid, make montmorillonite-based nano lamella be effectively peeled off, then make it be dispersed in polylactic acid matrix with masterbatch method, it is thus achieved that higher barrier property.
Description
Technical field
The present invention relates to the preparation method of a kind of high molecule nano material, particularly relate to a kind of high barrier polylactic acid nano
The preparation method of composite.
Background technology
Polylactic acid be at present research the most extensively, the Biodegradable material of most potentiality to be exploited, it has good biology
Degradability and environment friendly, but, the heat resistance of polylactic acid is very poor, constrains its application, meanwhile, its barrier properties for gases
Can also need to be improved further, to meet different application requirements.
Because the defect that the preparation of above-mentioned existing isolation-type polylactic acid exists, the present inventor sets based on being engaged in this series products
Meter manufactures practical experience abundant for many years and Professional knowledge, and coordinates the utilization of scientific principle, the most in addition research and innovation, to founding
The preparation method of a kind of novel high-barrier poly lactic acid nano composite material so that it is have more practicality.Through constantly studying,
Design, and after repeatedly studying sample and improving, finally create the present invention having practical value.
Summary of the invention
Present invention is primarily targeted at, overcome the defect that the preparation of existing isolation-type polylactic acid exists, and provide a kind of
The preparation method of novel high-barrier poly lactic acid nano composite material, improves the gas barrier property of polylactic acid, thus suitableeer
In practicality, and there is the value in industry.
The object of the invention to solve the technical problems realizes by the following technical solutions.Propose according to the present invention
The preparation method of high barrier poly lactic acid nano composite material, comprise the steps:
(1) preparation of Polycaprolactone modified montmorillonite: be passed through nitrogen 30min in dry flask to remove oxygen, so
Adding caprolactone monomer and montmorillonite in backward flask, by dispersion liquid supersonic vibration 1h, room temperature lower seal places 24h, in making oneself
Ester monomer is adequately inserted in montmorillonite layer；In flask, add initiator, carry out intercalation polymeric reaction after heating, by obtain
Product is dissolved in toluene, centrifugation after supersonic vibration, and centrifugal product is drying to obtain polycaprolactone after toluene repeatedly washs and is centrifuged
Modified montmorillonoid.
(2) intercept the preparation of master batch: by high mixer, make polylactic acid and the mixing of a small amount of silicone oil, add polycaprolactone
Modified montmorillonoid mixed at high speed 4min, then by double screw extruder extruding pelletization, extrusion temperature 180 DEG C.
(3) preparation of high barrier poly lactic acid nano composite material: master batch and polylactic acid mix homogeneously, torque flow will be intercepted
Become melt blending 8min on instrument, mixing temperature 190 DEG C, obtain high barrier poly lactic acid nano composite material.
Further, the preparation method of aforesaid high barrier poly lactic acid nano composite material, montmorillonite in described (1)
Consumption is the 5%～10% of caprolactone monomer quality.
Further, the preparation method of aforesaid high barrier poly lactic acid nano composite material, initiator in described (1)
Consumption is the 0.2%～0.8% of caprolactone monomer consumption.
Further, the preparation method of aforesaid high barrier poly lactic acid nano composite material, described initiator is pungent
Acid stannous, stannous chloride, acetylacetone,2,4-pentanedione stannum, stannous oxalate, aluminum isopropylate., triethyl aluminum, porphyrin aluminum, butyl titanate, metatitanic acid
One in orthocarbonate or isobutyl group trisphenol titanium.
Further, the preparation method of aforesaid high barrier poly lactic acid nano composite material, polylactic acid in described (2)
It is 100:20～30 with the mass ratio of Polycaprolactone modified montmorillonite.
Further, the preparation method of aforesaid high barrier poly lactic acid nano composite material, described (3) described poly-breast
Acid is 100:1～5 with the mass ratio of obstruct master batch.
Further, the preparation method of aforesaid high barrier poly lactic acid nano composite material, in described (1), intercalation gathers
The reaction temperature closed is 140～180 DEG C, and the response time is 8～12h.
By technique scheme, under the preparation method of high barrier poly lactic acid nano composite material of the present invention at least has
Row advantage:
Montmorillonite is the silicate mineral of the layer structure of a quasi-representative, its lamella by two silicon-oxy tetrahedron wafers it
Between clip alumina octahedral wafer and constitute, in " sandwich " structure.And general organic monomer or polymer are oleophylic hates
Water type, therefore effectively facilitate montmorillonite disperse in monomer or matrix polymer, intercalation or stripping, improve organic and inorganic boundary
The bonding force in face, forms intercal type or exfoliated structure, and the montmorillonite layer being dispersed in polylactic acid matrix increases gas diffusion
Path, be the effective measures of gas barrier property improving polylactic acid.
The extent of exfoliation of montmorillonite layer and dispersion size are the key factors affecting composite barrier property, melted slotting
Layer is due to the dimensional effect of macromole, and the steric hindrance inserting interlayer is relatively big, and therefore the present invention uses caprolactone in-situ intercalative polymerization
Modified montmorillonoid, it is thus achieved that type modified montmorillonoid is completely exfoliated, uses masterbatch method to improve the deployment conditions of montmorillonite, then by melted
The poly lactic acid nano composite material that prepare high barrier is blended, it is thus achieved that higher barrier property.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of description, after describing in detail such as with presently preferred embodiments of the present invention below.
Detailed description of the invention
By further illustrating the technological means and effect that the present invention taked by reaching predetermined goal of the invention, to according to this
Its detailed description of the invention of preparation method, feature and the effect thereof of the high barrier poly lactic acid nano composite material that invention proposes, in detail
Describe in detail bright as after.
Embodiment 1
(1) preparation of Polycaprolactone modified montmorillonite: be passed through nitrogen 30min in dry flask to remove oxygen, so
Backward flask adds caprolactone monomer and montmorillonite that mass ratio is 100:5, by dispersion liquid supersonic vibration 1h, room temperature lower seal
Place 24h, make caprolactone monomer be adequately inserted in montmorillonite layer, add drawing of caprolactone monomer quality 0.2% in flask
Send out agent butyl titanate, intercalation polymeric carries out 8h at 180 DEG C of lower seals, the product obtained is dissolved in toluene, after supersonic vibration from
The heart separates, and centrifugal product is drying to obtain Polycaprolactone modified montmorillonite after toluene repeatedly washs and is centrifuged.
(2) intercept the preparation of master batch: by high mixer, make polylactic acid and the mixing of a small amount of silicone oil, add 10% poly-own
Lactone-modified montmorillonite mixed at high speed 4min, then by double screw extruder extruding pelletization, extrusion temperature 180 DEG C.
(3) preparation of high barrier poly lactic acid nano composite material: obstruct master batch and polylactic acid are mixed with the proportioning of 1:100
Close uniformly, melt blending 8min on torque rheometer, mixing temperature 190 DEG C, obtain high barrier polylactic acid nano composite wood
Material.
Embodiment 2
(1) preparation of Polycaprolactone modified montmorillonite: be passed through nitrogen 30min in dry flask to remove oxygen, so
Backward flask adds caprolactone monomer and montmorillonite that mass ratio is 100:6, by dispersion liquid supersonic vibration 1h, room temperature lower seal
Place 24h, make caprolactone monomer be adequately inserted in montmorillonite layer, add drawing of caprolactone monomer quality 0.4% in flask
Sending out agent stannous octoate, intercalation polymeric carries out 9h at 170 DEG C of lower seals.The product obtained is dissolved in toluene, centrifugal after supersonic vibration
Separating, centrifugal product is drying to obtain Polycaprolactone modified montmorillonite after toluene repeatedly washs and is centrifuged.
(2) intercept the preparation of master batch: by high mixer, make polylactic acid and the mixing of a small amount of silicone oil, add 15% poly-own
Lactone-modified montmorillonite mixed at high speed 4min, then by double screw extruder extruding pelletization, extrusion temperature 180 DEG C.
(3) preparation of high barrier poly lactic acid nano composite material: obstruct master batch and polylactic acid are mixed with the proportioning of 2:100
Close uniformly, melt blending 8min on torque rheometer, mixing temperature 190 DEG C, obtain high barrier polylactic acid nano composite wood
Material.
Embodiment 3
(1) preparation of Polycaprolactone modified montmorillonite: be passed through nitrogen 30min in dry flask to remove oxygen, so
Backward flask adds caprolactone monomer and montmorillonite that mass ratio is 100:8, by dispersion liquid supersonic vibration 1h, room temperature lower seal
Place 24h, make caprolactone monomer be adequately inserted in montmorillonite layer, add drawing of caprolactone monomer quality 0.6% in flask
Send out agent metatitanic acid orthocarbonate, intercalation polymeric carries out 8h at 180 DEG C of lower seals, the product obtained is dissolved in toluene, after supersonic vibration from
The heart separates, and centrifugal product is drying to obtain Polycaprolactone modified montmorillonite after toluene repeatedly washs and is centrifuged.
(2) intercept the preparation of master batch: by high mixer, make polylactic acid and the mixing of a small amount of silicone oil, add 12% poly-own
Lactone-modified montmorillonite mixed at high speed 4min, then by double screw extruder extruding pelletization, extrusion temperature 180 DEG C.
(3) preparation of high barrier poly lactic acid nano composite material: obstruct master batch and polylactic acid are mixed with the proportioning of 5:100
Close uniformly, melt blending 8min on torque rheometer, mixing temperature 190 DEG C, obtain high barrier polylactic acid nano composite wood
Material.
Embodiment 4
(1) preparation of Polycaprolactone modified montmorillonite: be passed through nitrogen 30min in dry flask to remove oxygen, so
Backward flask adds caprolactone monomer and montmorillonite that mass ratio is 100:10, by dispersion liquid supersonic vibration 1h, close under room temperature
Envelope places 24h, makes caprolactone monomer be adequately inserted in montmorillonite layer, adds caprolactone monomer quality 0.8% in flask
Initiator stannous chloride, intercalation polymeric carries out 10h at 150 DEG C of lower seals, the product obtained is dissolved in toluene, after supersonic vibration from
The heart separates, and centrifugal product is drying to obtain Polycaprolactone modified montmorillonite after toluene repeatedly washs and is centrifuged.
(2) intercept the preparation of master batch: by high mixer, make polylactic acid and the mixing of a small amount of silicone oil, add 10% poly-own
Lactone-modified montmorillonite mixed at high speed 4min, then by double screw extruder extruding pelletization, extrusion temperature 180 DEG C.
(3) preparation of high barrier poly lactic acid nano composite material: obstruct master batch and polylactic acid are mixed with the proportioning of 5:100
Close uniformly, melt blending 8min on torque rheometer, mixing temperature 190 DEG C, obtain high barrier polylactic acid nano composite wood
Material.
Test one
Mechanics Performance Testing: the impact property of high barrier poly lactic acid nano composite material sample is in izodtest
Carrying out on machine, specimen size is straight 80mm × 10mm × 3mm.Use universal electrical stretching-machine test high barrier polylactic acid nano
The tensile property of composite, size of sample is 80mm × 10mm × 3mm., experimental data is as shown in the table:
| Polylactic acid/modified montmorillonoid | Hot strength (MPa) | Elongation at break (%) | Impact strength (KJ/m2) |
| 0 | 54.3 | 4.2 | 18.4 |
| 100/1 | 55.1 | 5.8 | 20.5 |
| 100/2 | 56.5 | 7.8 | 21.7 |
| 100/3 | 62.8 | 13.8 | 23.2 |
| 100/4 | 52.5 | 9.2 | 18.9 |
| 100/5 | 49.8 | 6.3 | 17.4 |
Test two
Barrier property is tested: use calorstat according to GB1037-1988 standard at 38 DEG C, measures thickness and be under 90% humidity
The barrier property WVTR value of 200 mum sample, experimental data is as shown in the table:
| Polylactic acid/modified montmorillonoid ratio | WVTR |
| 100/0 | 1.62×10-14 |
| 100/1 | 1.31×10-14 |
| 100/2 | 1.14×10-14 |
| 100/3 | 1.02×10-14 |
| 100/4 | 9.62×10-15 |
| 100/5 | 8.32×10-15 |
The present invention uses caprolactone in-situ intercalative polymerization modified montmorillonoid, makes montmorillonite-based nano lamella be effectively peeled off, then
It is made to be dispersed in polylactic acid matrix with masterbatch method, it is thus achieved that higher barrier property.
The above, be only presently preferred embodiments of the present invention, and the present invention not makees any pro forma restriction, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any technology people being familiar with this specialty
Member, in the range of without departing from technical solution of the present invention, when the technology contents of available the disclosure above makes a little change or modification
For the Equivalent embodiments of equivalent variations, as long as being the content without departing from technical solution of the present invention, the technical spirit of the foundation present invention
Any simple modification, equivalent variations and the modification being made above example, all still falls within the range of technical solution of the present invention.
Claims (4)
1. the preparation method of a high barrier poly lactic acid nano composite material, it is characterised in that: comprise the steps,
(1) preparation of Polycaprolactone modified montmorillonite: add caprolactone monomer and montmorillonite in the dry flask removing oxygen,
Sealing and standing after ultrasonic vibration, makes caprolactone monomer be adequately inserted in the lamella of montmorillonite, adds initiator, heating in flask
Carrying out intercalation polymeric reaction, the product obtained is dissolved in toluene, centrifugation after supersonic vibration, centrifugal product is repeatedly washed through toluene
Wash and be dried after being centrifuged, obtain Polycaprolactone modified montmorillonite；Montmorillonite consumption is the 5% ~ 10% of caprolactone monomer quality；
(2) preparation of master batch is intercepted: make polylactic acid and silicone oil mix by high mixer, add Polycaprolactone modified montmorillonite high
Speed mixing, then by extruder extruding pelletization, obtains intercepting master batch；Polylactic acid and the mass ratio of Polycaprolactone modified montmorillonite
For 100:20 ~ 30；
(3) preparation of high barrier poly lactic acid nano composite material: master batch and polylactic acid mix homogeneously will be intercepted, after melt blending
Obtain high barrier poly lactic acid nano composite material；Polylactic acid is 100:1 ~ 5 with the mass ratio of obstruct master batch.
The preparation method of high barrier poly lactic acid nano composite material the most according to claim 1, it is characterised in that: described
(1) in, initiator amount is the 0.2% ~ 0.8% of caprolactone monomer consumption.
The preparation method of high barrier poly lactic acid nano composite material the most according to claim 1 and 2, it is characterised in that:
Described initiator is stannous octoate, stannous chloride, acetylacetone,2,4-pentanedione stannum, stannous oxalate, aluminum isopropylate., triethyl aluminum, porphyrin aluminum, titanium
One in acid four butyl esters, metatitanic acid orthocarbonate or isobutyl group trisphenol titanium.
The preparation method of high barrier poly lactic acid nano composite material the most according to claim 1, it is characterised in that: described
(1) in, the reaction temperature of intercalation polymeric is 140 ~ 180 DEG C, and the response time is 8 ~ 12h.
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