CN102121199B - Ultrahigh starch filled polyolefin elastomer artificial leather - Google Patents
Ultrahigh starch filled polyolefin elastomer artificial leather Download PDFInfo
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- CN102121199B CN102121199B CN 201110060359 CN201110060359A CN102121199B CN 102121199 B CN102121199 B CN 102121199B CN 201110060359 CN201110060359 CN 201110060359 CN 201110060359 A CN201110060359 A CN 201110060359A CN 102121199 B CN102121199 B CN 102121199B
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- 229920002472 Starch Polymers 0.000 title claims abstract description 43
- 239000008107 starch Substances 0.000 title claims abstract description 43
- 235000019698 starch Nutrition 0.000 title claims abstract description 43
- 239000002649 leather substitute Substances 0.000 title claims abstract description 41
- 229920006124 polyolefin elastomer Polymers 0.000 title claims abstract description 16
- 239000004744 fabric Substances 0.000 claims abstract description 50
- 239000000463 material Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 14
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 20
- 238000012545 processing Methods 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000004067 bulking agent Substances 0.000 claims description 9
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 8
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical group C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 6
- 230000032050 esterification Effects 0.000 claims description 4
- 238000005886 esterification reaction Methods 0.000 claims description 4
- 238000005470 impregnation Methods 0.000 claims description 4
- 150000002605 large molecules Chemical class 0.000 claims description 4
- 229920002521 macromolecule Polymers 0.000 claims description 4
- 239000001254 oxidized starch Substances 0.000 claims description 4
- 235000013808 oxidized starch Nutrition 0.000 claims description 4
- 239000002759 woven fabric Substances 0.000 claims description 4
- 229920000742 Cotton Polymers 0.000 claims description 3
- 229920000881 Modified starch Polymers 0.000 claims description 3
- 238000001467 acupuncture Methods 0.000 claims description 3
- 238000003490 calendering Methods 0.000 claims description 2
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- 239000011265 semifinished product Substances 0.000 description 4
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- 229920002725 thermoplastic elastomer Polymers 0.000 description 4
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- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides a method for preparing ultrahigh starch filled polyolefin elastomer artificial leather. The method comprises the following steps of: preparing a base fabric of the artificial leather by adopting a scraping method, performing melting extrusion on polyolefin elastomer (POE), starch and macromolecular compatibilizer in a double-screw extruder, obtaining a flaky fabric through a calender, finally conveying the base fabric and the fabric to a joint wheel together, and pressing the base fabric and the fabric into the artificial leather at normal temperature. The artificial leather product produced by the method has softness, air permeability and biodegradability; the starch substance component which can be directly used for a microbe accounts for over 50 percent of the total amount; and the artificial leather is a novel high-performance artificial leather environmentally-friendly material.
Description
Technical field
The present invention relates to technical field of polymer materials, relate in particular to a kind of preparation method of ultrahigh starch filled polyolefin elastomer artificial leather.
Background technology
At present, because oil price rises steadily, the profit margin of Polymer Industry is dwindled just day by day, this wherein the artificial leather industry seem especially particularly outstanding.In China, artificial leather all is the very low low grade leather of added value basically, all be simple repetition technically between each factory, product duplicates and is absorbed in harmful competition on market, therefore set up and a kind ofly have good gas permeability and production technology is simple, cost is low, high resilience and compliance, and the manufacture method of biodegradable modified artificial leather material, prepare the elastomer artificial leather of novel excellent performance, this will further widen the application of present artificial leather.Polyolefin elastomer ethylene-octene copolymer (POE) is a kind of thermoplastic elastomer (TPE) of being produced by the in-situ polymerization technology of ethene, octene by Dupont DOW company, compared many advantages with traditional elastomeric material, high such as weld bond intensity brilliance, good dispersion, transparency, subduing property is good.Because these good comprehensive physical chemical properties, the thermoplastic elastomer (TPE) product is widely used in various fields such as automobile, electric wire, sports goods, building materials, electronic device, leather, seal, electric tool, IT industry, toys in recent years.Yet the biological degradable composite material about POE really has no report.
With regard to current plastics pollution, adopt the Biodegradable starch resin, can realize the requirement of innoxious, minimizing and resource.Find through the retrieval to existing document, U.S. Patent No. 5,461,094 discloses and has a kind ofly prepared biodegradable film by starch and Polyethylene Chain chemical bonding.In addition, U.S. Patent No. 2005/0171249 discloses and has added granular starch in the polymer with the cost that reduces polymer derivant so that this derivative biodegradable more.It is worth mentioning that, present degradative plastics take starch as raw material, content of starch is lower, and is synthesized resin-coating, and biology is difficult to contact starch, biodegradation, so be not the Ideal Substitute of Phthalates; These degradative plastics goods, no matter light degradation or light-Sheng degraded, it is few that its degradation property really reaches the product of similar starch degradation course; Just has this performance more than 25% because only reach content of starch.Undoubtedly, content of starch is higher, and its degradation property is better, but along with the increase of content of starch, its intensity and elongation at break reduce greatly, the security that impact is used.Therefore, carry out ultrahigh starch filled polyolefin elastomer environmental friendliness artificial leather developmental research will have important real industrial application value.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of ultrahigh starch filled polyolefin elastomer environmental friendliness artificial leather is provided.
The present invention is achieved by the following technical solutions:
A kind of preparation method of ultrahigh starch filled polyolefin elastomer artificial leather, it is characterized in that may further comprise the steps: it is for subsequent use to prepare the artificial leather base fabric, again polyolefin elastomer POE, starch and large molecule bulking agent POE-g-MAH mixture are melt extruded, and obtain the sheet fabric by calendering, at last base fabric and fabric are pressed into artificial leather at normal temperature condition.
Content of starch is amount of the mixture 50-60 wt% in the mixture, and POE-g-MAH content is the 5-10 wt% of amount of the mixture, and the content of polyolefin elastomer POE is the 35-40 wt% of amount of the mixture.
The artificial leather base fabric is impregnation cloth, Woven Fabrics, knitted cloth, spins inner skin or have an acupuncture treatment cotton.
The artificial leather base fabric is that to scrape legal system standby and get with being coated with; Mixture is to melt extrude at double screw extruder.
Large molecule bulking agent POE-g-MAH be by POE,
Maleic anhydride, initator melt extrudes in double screw extruder and obtains.
Initator is cumyl peroxide, and its consumption is 0.08～0.1 wt% of POE; Described
Maleic anhydrideConsumption is the 1-3 wt% of POE.
1～6 section temperature of double screw extruder is: 90-120 ℃, 120-150 ℃, 150-180 ℃, 180-200 ℃, 180-200 ℃, 160-190 ℃, and head temperature is 160-190 ℃; Screw speed is 50-80 r/min, and the feeding rotating speed is that rotating speed is 250-350 r/min.
Starch is pre-gelatinized starch, crosslinked starch, oxidized starch or esterification starch.
The processing temperature of double screw extruder is followed successively by 90-120 ℃, 120-150 ℃, 150-180 ℃, 180-200 ℃, 180-200 ℃, 160-190 ℃ from the charge door to the outlet, head temperature is 160-190 ℃; Screw speed is 50-80 r/min, and the feeding rotating speed is that rotating speed is 250-350 r/min; The time that material stops in barrel is 5-10min.
Sheet fabric method for making is rolling process, and processing temperature is 115～145
oC.
Preferred version of the present invention is:
(1) use is coated with the method for scraping with being coated with the cutter frictioning and it being coated on the base fabric, and wherein, glue normal operation polyurethane glue is then 120 ℃ of bakings 1 minute, so that base fabric and sizing material paste the jail.Described base fabric is selected impregnation cloth, Woven Fabrics, knitted cloth, is spun inner skin, in the acupuncture treatment cotton any one.
(2) with POE,
Maleic anhydride(MAH), initator evenly mixes, and melt extrudes in double screw extruder, obtains the colourless or lurid bulking agent POE-g-MAH of good fluidity.Described initator is cumyl peroxide (DCP), and its consumption is 0.1 wt% of POE, and the MAH consumption is 2 wt% of POE.Each section of double screw extruder temperature (1～6/ ℃): 100,140,170,190,190,180,180 ℃ of heads, screw speed 60 r/min, feeding 300 r/min.
(3) with the bulking agent POE-g-MAH of step (2) gained and POE 40 ℃ of lower vacuumizes at least 3 hours, starch is 105 ℃ of lower dryings at least 3 hours, to guarantee to remove moisture.POE and the starch of drying are mixed according to a certain ratio, and adding POE-g-MAH(content is total amount 5 wt%).Described starch is any one in pre-gelatinized starch (GS), crosslinked starch (CS), oxidized starch (OS), the esterification starch (ES).Described content of starch is 55 wt%
(4) blend that step (3) is obtained plastifies mixing in double screw extruder.The screw diameter of described double screw extruder is 60mm, draw ratio is 48:1, has plural natural steam vent, for the steady propelling that guarantees material is extruded, the screw thread original paper that its mixing original paper employing specification is 36 helical pitches carries out assembled arrangement, thereby the time that the control material stops in barrel is at 6 min.Processing temperature is followed successively by 120 ℃ from the charge door to the outlet, and 140 ℃, 140 ℃, 120 ℃, times 8 min, rotating speed 50 r/min.
(5) blend that step (4) is synthesized is put into 4 roll calendars and is rolled processing temperature 125
oC is pressed into the sheet fabric with sizing material.
(6) fabric that the base fabric that step (1) is obtained and step (5) obtain is delivered to laminating wheel in the lump, is pressed into artificial leather at normal temperature condition, and thickness is 2 mm, then these artificial leather semi-finished product is cooled off through cooling wheel, is taken out by crimping wheel at last.
A kind of ultrahigh starch filled polyolefin elastomer environmental friendliness artificial leather provided by the invention compared with prior art, has following advantage:
(1) the artificial leather product of method production of the present invention has flexibility, gas permeability and biodegradability, and the starch material composition that wherein directly can be used as the microorganism utilization accounts for more than 50% of total content, and all the other components are degraded to 10 in the degradation time of regulation
-2The particulate of mm level is novel high-performance artificial leather environment-friendly materials.
(2) the present invention directly makes raw material with industrial starch, has saved required huge equipment, the long-time dry energy consumption of dry starch, has saved a large amount of man power and materials, has shortened simultaneously processing link, and process is simple.
(3) softening temperature of starch polymer is more than 200 ℃, can not soften under traditional elastomer temperature or melting and effectively blend or be dispersed in the elastomer matrix.This project adopts big L/D ratio, high rotating speed, high moment of torsion, powerful double screw extruder, solved the problem of traditional handicraft because of the high starch charing that causes of temperature, can be under low heating-up temperature, by screw element mechanical energy is converted into the internal energy of molecular of each component, thereby has promoted the even mixing of each component materials.
Description of drawings
Fig. 1.The electron microscope result of the brittle failure face of artificial leather fabric among the embodiment 1.
Fig. 2.(a) photo of artificial leather after laboratory environment 1 year and (b) soil buries 180 days.
Specific implementation method:
Embodiment 1
Polyurethane glue is coated on the impregnation cloth base fabric with being coated with cutter with being coated with the method for scraping, then at 120 ℃ of baking 1 min, so that base fabric and sizing material paste the jail.With 500 g POE, 10 g
Maleic anhydride, the 0.5g cumyl peroxide evenly mixes, and melt extrudes in double screw extruder, obtains the colourless or lurid bulking agent POE-g-MAH of good fluidity.Each section of double screw extruder temperature (1～6): 100 ℃, 140 ℃, 170 ℃, 190 ℃, 190 ℃, 180 ℃, 180 ℃ of heads, screw speed 60 r/min, feeding 300 r/min.The POE-g-MAH of 500 g POE and 500 g esterified crosslinked starch, 80g is evenly mixed, and in double screw extruder plasticizing forming.The screw diameter of double screw extruder is 60mm, and draw ratio is 48:1, and the screw thread original paper that its mixing original paper employing specification is the 36-44 helical pitch carries out assembled arrangement, thereby the time that the control material stops in barrel is at 5-10min.Processing temperature is followed successively by 120 ℃ from the charge door to the outlet, and 140 ℃, 140 ℃, 120 ℃, times 8 min, rotating speed 50 r/min.The blend that obtains is put into 4 roll calendars roll, processing temperature 125
oC is pressed into the sheet fabric with sizing material.At last base fabric and fabric are delivered to laminating wheel in the lump, be pressed into artificial leather at normal temperature condition, thickness is 2 mm, then these artificial leather semi-finished product is cooled off through cooling wheel, is taken out by crimping wheel at last.
Embodiment 2
Polyurethane glue is coated on the Woven Fabrics base fabric with being coated with cutter with being coated with the method for scraping, then at 120 ℃ of baking 1 min, so that base fabric and sizing material paste the jail.With 500 g POE, 10 g
Maleic anhydride, the 0.5g cumyl peroxide evenly mixes, and melt extrudes in double screw extruder, obtains the colourless or lurid bulking agent POE-g-MAH of good fluidity.Each section of double screw extruder temperature (1～6): 100 ℃, 140 ℃, 170 ℃, 190 ℃, 190 ℃, 180 ℃, 180 ℃ of heads, screw speed 60 r/min, feeding 300 r/min.The POE-g-MAH of 450 g POE and the pre-gelatinization cornstarch of 550 g, 50g is evenly mixed, and in double screw extruder plasticizing forming.The screw diameter of double screw extruder is 60mm, and draw ratio is 48:1, and the screw thread original paper that its mixing original paper employing specification is the 36-44 helical pitch carries out assembled arrangement, thereby the time that the control material stops in barrel is at 5-10min.Processing temperature is followed successively by 120 ℃ from the charge door to the outlet, and 140 ℃, 140 ℃, 120 ℃, times 8 min, rotating speed 50 r/min.The blend that obtains is put into 4 roll calendars roll, processing temperature 120
oC is pressed into the sheet fabric with sizing material.At last base fabric and fabric are delivered to laminating wheel in the lump, be pressed into artificial leather at normal temperature condition, thickness is 3 mm, then these artificial leather semi-finished product is cooled off through cooling wheel, is taken out by crimping wheel at last.
Embodiment 3
Polyurethane glue is coated on the knitted cloth base fabric with being coated with cutter with being coated with the method for scraping, then at 120 ℃ of baking 1 min, so that base fabric and sizing material paste the jail.With 500 g POE, 10 g
Maleic anhydride, the 0.5g cumyl peroxide evenly mixes, and melt extrudes in double screw extruder, obtains the colourless or lurid bulking agent POE-g-MAH of good fluidity.Each section of double screw extruder temperature (1～6): 100 ℃, 140 ℃, 170 ℃, 190 ℃, 190 ℃, 180 ℃, 180 ℃ of heads, screw speed 60 r/min, feeding 300 r/min.The POE-g-MAH of 400 g POE and 600 g esterification cornstarchs, 100g is evenly mixed, and in double screw extruder plasticizing forming.The screw diameter of double screw extruder is 60mm, and draw ratio is 48:1, and the screw thread original paper that its mixing original paper employing specification is the 36-44 helical pitch carries out assembled arrangement, thereby the time that the control material stops in barrel is at 5-10min.Processing temperature is followed successively by 120 ℃ from the charge door to the outlet, and 140 ℃, 140 ℃, 120 ℃, times 8 min, rotating speed 50 r/min.The blend that obtains is put into 4 roll calendars roll, processing temperature 135
oC is pressed into the sheet fabric with sizing material.At last base fabric and fabric are delivered to laminating wheel in the lump, be pressed into artificial leather at normal temperature condition, thickness is 4 mm, then these artificial leather semi-finished product is cooled off through cooling wheel, is taken out by crimping wheel at last.
Experimental example 4
1. surface topography test
Adopt observer's fabricate-leather specimen surface pattern on the JSM-6330F field emission scanning electron microscope.The result as shown in Figure 1.
2. biodegradation experiment
Pour plate into after the basis dissolved without carbon source agar medium heating.In Biohazard Safety Equipment, respectively specimen surface is sprayed mycotic spore suspension equably with art spray gun, leave standstill about 1 min, then sample is positioned over above the agar that solidifies.Avoid between the print, contact between print and the plate.Culture dish sealed with adhesive tape be placed in the mold incubator, 28～30 ℃ of temperature, relative humidity is no less than 85%, cultivates 28 days.
3. soil buries experiment
Sample is cut into the dumbbell shaped batten, wraps in the soil that is embedded under the outdoor natural conditions with nylon gauze, it is dark to bury about 30 mm, and the place is Guangzhou, and the time is 2006.04～2006.11.The soil moisture and humidity and natural environment are consistent.Take out sample every month from soil, clean with deionized water, and 40 ℃ of dryings are at least 24 hours in vacuum drying chamber, then put into the drier constant weight.Weigh the weight before and after the record sample degradation.
It is as shown in table 1 that biodegradation experiment and soil bury experimental results.Artificial leather soil buries photo after 180 days and artificial leather at the photo in 1 year of laboratory environment as shown in Figure 2.
4. mechanical property
Test at the power test puller system, draw speed is 50 mm/min.
Table 1.Biodegradation experiment and soil bury the test result of experiment
Claims (7)
1. the preparation method of a ultrahigh starch filled polyolefin elastomer artificial leather, it is characterized in that may further comprise the steps: it is for subsequent use to prepare the artificial leather base fabric, again polyolefin elastomer POE, starch and large molecule bulking agent POE-g-MAH mixture are melt extruded, and obtain the sheet fabric by calendering, at last base fabric and fabric are pressed into artificial leather at normal temperature condition;
Content of starch is amount of the mixture 50-60 wt% in the described mixture, and POE-g-MAH content is the 5-10 wt% of amount of the mixture, and the content of polyolefin elastomer POE is the 35-40 wt% of amount of the mixture;
The processing temperature that described mixture melt extrudes the double screw extruder that adopts is followed successively by 90-120 ℃, 120-150 ℃, 150-180 ℃, 180-200 ℃, 180-200 ℃, 160-190 ℃ from the charge door to the outlet, head temperature is 160-190 ℃; Screw speed is 50-80 r/min, and the feeding rotating speed is that rotating speed is 250-350 r/min; The time that material stops in barrel is 5-10min;
Described sheet fabric method for making is rolling process, and processing temperature is 115～145
oC.
2. preparation method as claimed in claim 1 is characterized in that described artificial leather base fabric is impregnation cloth, Woven Fabrics, knitted cloth, spins inner skin or have an acupuncture treatment cotton.
3. preparation method as claimed in claim 2 is characterized in that described artificial leather base fabric is that to scrape legal system standby and get with being coated with; Mixture is to melt extrude at double screw extruder.
4. preparation method as claimed in claim 1 is characterized in that described large molecule bulking agent POE-g-MAH is melt extruded in double screw extruder by POE, maleic anhydride, initator to obtain.
5. preparation method as claimed in claim 4 is characterized in that described initator is cumyl peroxide, and its consumption is 0.08～0.1 wt% of POE; The 1-3 wt% that described maleic anhydride consumption is POE.
6. preparation method as claimed in claim 4 is characterized in that 1～6 section temperature of double screw extruder is: 90-120 ℃, 120-150 ℃, 150-180 ℃, 180-200 ℃, 180-200 ℃, 160-190 ℃, and head temperature is 160-190 ℃; Screw speed is 50-80 r/min, and the feeding rotating speed is that rotating speed is 250-350 r/min.
7. preparation method as claimed in claim 1 is characterized in that described starch is pre-gelatinized starch, crosslinked starch, oxidized starch or esterification starch.
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| CN103044719B (en) * | 2012-12-19 | 2015-09-16 | 华南理工大学 | A kind of have thermoplastic starch plastic of high hydrophobicity energy and preparation method thereof |
| CN114889296B (en) * | 2022-05-19 | 2023-01-17 | 东莞市科迪实业有限公司 | Crease-resistant environment-friendly synthetic leather and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6141375A (en) * | 1984-08-01 | 1986-02-27 | Toray Ind Inc | Production of artificial fur |
| JPS61215782A (en) * | 1985-03-15 | 1986-09-25 | Toray Ind Inc | Production of artificial leather sheet |
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| CN1135550A (en) * | 1996-01-16 | 1996-11-13 | 北京市海淀区太生新工程材料研究所 | Degraded leather-imitation and production method and application thereof |
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