CN105219044A - A kind of complete biodegradable heat-proof polylactic acid foam material and preparation method thereof - Google Patents
A kind of complete biodegradable heat-proof polylactic acid foam material and preparation method thereof Download PDFInfo
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- CN105219044A CN105219044A CN201510728879.6A CN201510728879A CN105219044A CN 105219044 A CN105219044 A CN 105219044A CN 201510728879 A CN201510728879 A CN 201510728879A CN 105219044 A CN105219044 A CN 105219044A
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Abstract
The invention discloses a kind of complete biodegradable heat-proof polylactic acid foam material and preparation method thereof, be made up of weight percent poly(lactic acid) 90 ~ 95%, PBAT resin 1 ~ 5%, chainextender 0.1 ~ 3%, nucleator 0.1 ~ 5%, blowing promotor 0.1 ~ 3%.Utilize this foam material can realize continuous foamed technology, the foamed products of preparation has the advantage that abscess-size is even, rate of closed hole is high, and maintain the biodegradable advantage of poly(lactic acid), meet the sustainable expanding economy demand of green low-carbon completely, wide application market can be had at disposable lunch-box, mess-tin and hamburger box, instant noodle bowl and packaging field.Preparation method of the present invention: first by poly(lactic acid) drying treatment, adds other components and mixes after cooling; Be added to tie rod, air-cooled, pelletizing after melt blending in twin screw extruder again, obtain final product.This preparation method is simple, is easy to control and implement, workable, is easy to industrialization and produces.
Description
Technical field
The present invention relates to heat-proof polylactic acid material and preparing technical field thereof, be specifically related to a kind of complete biodegradable heat-proof polylactic acid foam material and preparation method thereof.
Background technology
Along with global economy is fast-developing, plastics have penetrated into the every field of national economy.But used most plastics all derive from oil, greatly exacerbate " petroleum resources shortage " problem.In addition, because petroleum-based plastics has non-biodegradable, particularly disposable petroleum base foaming snack box, has the large and bulky feature of turnout, causes serious " white pollution ".The process means of unrenewable petroleum-based plastics are mainly burning, and this can aggravate Greenhouse effect and haze weather greatly.Along with petroleum resources shortage, white pollution, Greenhouse effect and haze weather are severe gradually, bio-based degradable high polymer material progressively receives the concern of people.Therefore, the environment-friendly and bio based high molecular material meeting low-carbon environment-friendly green economy growth requirement has wide development space, will certainly will progressively substitute non-degradable petroleum base macromolecular material.Poly(lactic acid) (PLA) is thought the environment-friendly polymers of most industrialization prospect by business circles.
This mainly derives from the biomass resources such as corn thus possesses recyclability due to poly(lactic acid), and has excellent biodegradability and the mechanical property of similar polystyrene.But poor heat resistance and price height are the key factors of the extensive commercial application of restriction poly(lactic acid).Expanded polylactic acid product can effectively reduce its density, thus can effectively reduce its single product weight, and then captures the high defect of its price.Heat-proof polylactic acid foam material has wide application market at disposable lunch-box, mess-tin and hamburger box, instant noodle bowl and packaging field.Therefore, the suitability for industrialized production of heat-proof polylactic acid foamed products, has great importance to the extensive PS base foaming snack box that replaces of realization.
But poly(lactic acid) is semicrystalline polymer, itself have that crystallization velocity is slow, poor heat resistance (being only about 55 DEG C), melt strength is low, process window is a narrow defect, cause existing foaming technique and technique and be not suitable for expanded polylactic acid.To foam a difficult problem for above-mentioned PLA, existing solution mainly comprises and adds nanoparticle and improve its foam performance, adopt chainextender increase molecular weight and change processing condition etc.These technical schemes can improve PLA foam performance to a certain extent, but substantially still at the experimental stage.Patent CN101362833B, CN102321269B and CN104140659A etc. disclose the intermittent type foaming techniques such as poly(lactic acid) moulded from foam or reactor, and complex forming technology, shaping cycle is long, is unfavorable for suitability for industrialized production.CN103819885A discloses a kind of polylactic acid foam material and preparation method thereof, but by the petroleum-based plastics such as composite polyethylene or polypropylene, sacrifice the biogenetic derivation of poly(lactic acid) and the advantage of biological degradability greatly, still thoroughly can not solve its petrol dependency and white pollution harm.US Patent No. 20080262118 and US20110263732 etc. utilize compound D-form PLA to prepare polylactic acid foam material, but foam size is comparatively large, and percentage of open area is high, and foam process precision is high, and cost is high, is difficult to realize suitability for industrialized production.
Summary of the invention
For capturing the continuous foamed difficult problem of heat-proof polylactic acid, the invention provides a kind of complete biodegradable heat-proof polylactic acid foam material and preparation method thereof, expansion ratio is high, and abscess-size is even, and percentage of open area is low, process warm and, preparation is simple,
A kind of complete biodegradable heat-proof polylactic acid foam material, be made up of the raw material of following weight percent:
Described poly(lactic acid) is the commercially available general trade mark, comprises 4032D and 2002D etc. of U.S. Natureworks.
Described poly-hexanodioic acid/butylene terephthalate (PBAT resin) can adopt the commercially available general trade mark, as BASF Ecoflex series and prosperous rich medicine company Biocosafe series etc.
The chainextender ADR4368C that described chainextender can adopt BASF AG to produce and the chainextender ADR4370 etc. that BASF AG produces.
Described nucleator is one or more (comprising two kinds) in ethylene two-12-hydroxystearic (EBH), nano organic montmorillonite, talcum powder etc.Further preferably, described nucleator is the mixture of the two-12-hydroxystearic (EBH) of ethylene and nano organic montmorillonite or ethylene pair-12-hydroxystearic (EBH) and talcous mixture.Described talcous particle diameter is 4000 ~ 6000 orders.The mass ratio of the two-12-hydroxystearic (EBH) of described ethylene and nano organic montmorillonite is 1:1.5 ~ 2.5, and the two-12-hydroxystearic (EBH) of described ethylene and talcous mass ratio are 1:1.5 ~ 2.5.Composite nucleator can play synergy, has better foaming nucleation effect.
Described blowing promotor is one or more in polyoxyethylene sorbitan fatty acid ester, Sorbitan fatty acid ester, castor oil polyoxyethylene ether, lauric monoglyceride etc.
As preferably, described complete biodegradable heat-proof polylactic acid foam material, be made up of the raw material of following weight percent:
Most preferably, described complete biodegradable heat-proof polylactic acid foam material, be made up of the raw material of following weight percent:
Described nucleator is the two-12-hydroxystearic (EBH) of ethylene and talcous mixture, described talcous particle diameter is 5000 orders, the weight percentage of the two-12-hydroxystearic of ethylene is 1%, and talcous weight percentage is 2%;
Described blowing promotor is polyoxyethylene sorbitan fatty acid ester.
As can be seen from embodiment 4,5, the component of above-mentioned weight percentage has more excellent foam performance, be in particular in abscess-size evenly, rate of closed hole is higher.
Present invention also offers a kind of preparation method of complete biodegradable heat-proof polylactic acid foam material, process be simple, be easy to control, workable, can continuous seepage, be easy to industrializing implementation.
A preparation method for complete biodegradable heat-proof polylactic acid foam material, comprises the following steps:
Utilize high-speed mixer under 100 DEG C ~ 110 DEG C (preferably 105 DEG C) by poly(lactic acid) drying treatment 20 ~ 40min (preferred 30min), add other components after cooling, and mix, obtain mixed material; Again mixed material is added to tie rod, air-cooled, pelletizing after melt blending in twin screw extruder, obtains complete biodegradable heat-proof polylactic acid foam material.
The screw slenderness ratio of described twin screw extruder is 35:1 ~ 45:1; The temperature of described melt blending is 170 DEG C ~ 180 DEG C.
Described complete biodegradable heat-proof polylactic acid foam material, has the advantages such as crystallization rate is fast, good heat resistance, process window are wide, and maintains the complete biodegradable advantage of itself.In addition, utilize twin screw to extrude continuously, adopt blown with carbon dioxide technology, the heat-proof polylactic acid foam sheet of preparation has the advantage that abscess-size is even, rate of closed hole is high.
Compared with prior art, tool of the present invention has the following advantages:
The present invention is by adding chainextender, improve molecular weight and the molecular chain length of poly(lactic acid) greatly, thus improve the melt strength of poly(lactic acid) and widen the process window of poly(lactic acid), thoroughly break through the low restriction to poly-lactic acid material foaming narrow with process window of melt strength.
There is the defect that frothing percentage is low, abscess-size is uneven and percentage of open area is high in polylactic acid foam material prepared by prior art, if this is not because poly(lactic acid) abscess is grown up out of control causing.By the screening of a large amount of blowing promotor, a kind of auxiliary agent expanded polylactic acid to stabilization of final acquisition, thus realize the controllability of poly(lactic acid) abscess growth, the final polylactic acid foam material that obtains has the advantage that abscess-size is even, rate of closed hole is high.This mainly due to, this type of blowing promotor effectively can improve the affinity at poly(lactic acid) and supercritical co interface, realizes the stabilized growth of poly(lactic acid) abscess, thus overcomes the high difficult problem of the uneven and percentage of open area of poly(lactic acid) abscess-size.
Heat-proof polylactic acid foam material prepared by the present invention, utilizes supercritical carbon dioxide foaming technology, can realize twin screw continuous foamed, the plastic uptake product heat resisting temperature of preparation reach 110 DEG C and more than, foam materials such as realizing extensive substituting PS is had great importance.Heat-proof polylactic acid foam material disclosed by the invention has wide application market at disposable lunch-box, mess-tin and hamburger box, instant noodle bowl and packaging field, has great importance to the extensive petroleum-based plastics foamed products such as PS that replace of realization.
Heat-proof polylactic acid foam material of the present invention maintains the advantage of the complete biodegradable of poly(lactic acid), meets U.S. ASTMD6400 and European Union EN13432 degraded Valuation Standard completely, and have passed the authoritative department certifications such as BPI, FDA, SGS.
Embodiment
Following examples and comparative example further describe the present invention, but the present invention is not limited to these embodiments.
Embodiment 1
Take the raw material of following weight:
Poly(lactic acid) (4032D of U.S. Natureworks) 92.5Kg, PBAT resin (Biocosafe2003, hundred million Fan Xinfu medicine company limited-liability company) 3Kg, chainextender (ADR4370, BASF stock company) 1Kg, nucleator (EBH, Suzhou Liansheng Chemicals Co., Ltd., 1kg; Talcum powder, 5000 orders, be bestowed by heaven fire retardant material Science and Technology Ltd. in Dandong, 2kg), blowing promotor (polyoxyethylene sorbitan fatty acid ester T-80, the prosperous Industrial Co., Ltd. of upper marial rocks) 0.5kg.
The preparation method of heat-proof polylactic acid foam material:
First, poly(lactic acid) is added high-speed mixing drying machine, at 105 DEG C of dry 30min, add other auxiliary agents after cooling and mix; Then mixed material is added to melt blending in twin screw extruder (extruder temperature is 170 DEG C-180 DEG C) tie rod, air-cooled, pelletizing afterwards, obtains complete biodegradable heat-proof polylactic acid foam material.The screw slenderness ratio of the twin screw extruder selected is 36:1.
Embodiment 2
Take the raw material of following weight:
Poly(lactic acid) (4032D of U.S. Natureworks) 90.5Kg, PBAT resin (Biocosafe2003, hundred million Fan Xinfu medicine company limited-liability company) 5Kg, chainextender (ADR4370, BASF stock company) 1.5Kg, nucleator (EBH, Suzhou Liansheng Chemicals Co., Ltd., 1kg; Talcum powder, 5000 orders, be bestowed by heaven fire retardant material Science and Technology Ltd. in Dandong, 1kg), blowing promotor (polyoxyethylene sorbitan fatty acid ester T-80, the prosperous Industrial Co., Ltd. of upper marial rocks) 1kg.
Preparation method as described in Example 1.
Embodiment 3
Take the raw material of following weight:
Poly(lactic acid) (4032D of U.S. Natureworks) 91Kg, PBAT resin (Biocosafe2003, hundred million Fan Xinfu medicine company limited-liability company) 4Kg, chainextender (ADR4370, BASF stock company) 0.5Kg, nucleator (EBH, Suzhou Liansheng Chemicals Co., Ltd., 0.5kg; Talcum powder, 5000 orders, be bestowed by heaven fire retardant material Science and Technology Ltd. in Dandong, 1kg), blowing promotor (polyoxyethylene sorbitan fatty acid ester T-80, the prosperous Industrial Co., Ltd. of upper marial rocks) 3kg.
Preparation method as described in Example 1.
Embodiment 4
Take the raw material of following weight:
Poly(lactic acid) (4032D of U.S. Natureworks) 93Kg, PBAT resin (Biocosafe2003, hundred million Fan Xinfu medicine company limited-liability company) 4Kg, chainextender (ADR4370, BASF stock company) 0.5Kg, nucleator (EBH, Suzhou Liansheng Chemicals Co., Ltd., 0.5kg; Talcum powder, 5000 orders, be bestowed by heaven fire retardant material Science and Technology Ltd. in Dandong, 1kg), blowing promotor (polyoxyethylene sorbitan fatty acid ester T-80, the prosperous Industrial Co., Ltd. of upper marial rocks) 1kg.
Preparation method as described in Example 1.
Embodiment 5
Take the raw material of following weight:
Poly(lactic acid) (4032D of U.S. Natureworks) 92Kg, PBAT resin (Biocosafe2003, hundred million Fan Xinfu medicine company limited-liability company) 3Kg, chainextender (ADR4370, BASF stock company) 1Kg, nucleator (EBH, Suzhou Liansheng Chemicals Co., Ltd., 1kg; Talcum powder, 5000 orders, be bestowed by heaven fire retardant material Science and Technology Ltd. in Dandong, 2kg), blowing promotor (polyoxyethylene sorbitan fatty acid ester T-80, the prosperous Industrial Co., Ltd. of upper marial rocks) 1kg.
Preparation method as described in Example 1.
Embodiment 6
Take the raw material of following weight:
Poly(lactic acid) (4032D of U.S. Natureworks) 91Kg, PBAT resin (Biocosafe2003, hundred million Fan Xinfu medicine company limited-liability company) 3Kg, chainextender (ADR4370, BASF stock company) 1Kg, nucleator (EBH, Suzhou Liansheng Chemicals Co., Ltd., 1kg; Talcum powder, 5000 orders, be bestowed by heaven fire retardant material Science and Technology Ltd. in Dandong, 2kg), blowing promotor (polyoxyethylene sorbitan fatty acid ester T-80, the prosperous Industrial Co., Ltd. of upper marial rocks) 2kg.
Preparation method as described in Example 1.
Comparative example 1
Take the raw material of following weight:
Poly(lactic acid) (4032D of U.S. Natureworks) 91Kg, PBAT resin (Biocosafe2003, hundred million Fan Xinfu medicine company limited-liability company) 3Kg, chainextender (ADR4370, BASF stock company) 1Kg, nucleator (EBH, Suzhou Liansheng Chemicals Co., Ltd., 1kg; Talcum powder, 5000 orders, be bestowed by heaven fire retardant material Science and Technology Ltd. in Dandong, 2kg).
Preparation method as described in Example 1.
Comparative example 2
Take the raw material of following weight:
Poly(lactic acid) (4032D of U.S. Natureworks) 92Kg, PBAT resin (Biocosafe2003, hundred million Fan Xinfu medicine company limited-liability company) 3Kg, nucleator (EBH, Suzhou Liansheng Chemicals Co., Ltd., 1kg; Talcum powder, 5000 orders, be bestowed by heaven fire retardant material Science and Technology Ltd. in Dandong, 2kg), blowing promotor (polyoxyethylene sorbitan fatty acid ester T-80, the prosperous Industrial Co., Ltd. of upper marial rocks) 2kg.
Preparation method as described in Example 1.
Adopt supercritical carbon dioxide foaming technology, utilize twin screw extruder to be undertaken continuous foamed by the heat-proof polylactic acid foam material that embodiment 1 ~ 6 and comparative example 1 ~ 2 obtain, and test foam sheet, its test result is as shown in table 1.
Table 1
As shown in Table 1, by embodiment 1 ~ 6 compared with comparative example 1 ~ 2, embodiment 1-6 has excellent foam performance, is in particular in that abscess-size is even, rate of closed hole is high.In addition, this heat-proof polylactic acid foam material maintains the biodegradable advantage of poly(lactic acid), meets U.S. ASTMD6400 and European Union EN13432 degraded Valuation Standard completely, has great importance to the shortage of alleviation petroleum resources and solution white pollution.Therefore, this matrix material meets green low-carbon expanding economy demand completely, has wide application space.
Claims (10)
1. a complete biodegradable heat-proof polylactic acid foam material, is characterized in that, is made up of the raw material of following weight percent:
2. complete biodegradable heat-proof polylactic acid foam material according to claim 1, is characterized in that, be made up of the raw material of following weight percent:
3. complete biodegradable heat-proof polylactic acid foam material according to claim 1 and 2, is characterized in that, described nucleator is one or more in the two-12-hydroxystearic of ethylene, nano organic montmorillonite, talcum powder.
4. complete biodegradable heat-proof polylactic acid foam material according to claim 3, it is characterized in that, described nucleator is the mixture of the two-12-hydroxystearic of ethylene and nano organic montmorillonite or the two-12-hydroxystearic of ethylene and talcous mixture.
5. complete biodegradable heat-proof polylactic acid foam material according to claim 4, is characterized in that, described talcous particle diameter is 4000 ~ 6000 orders.
6. complete biodegradable heat-proof polylactic acid foam material according to claim 4, the mass ratio of the two-12-hydroxystearic of described ethylene and nano organic montmorillonite is 1:1.5 ~ 2.5, and the two-12-hydroxystearic of described ethylene and talcous mass ratio are 1:1.5 ~ 2.5.
7. complete biodegradable heat-proof polylactic acid foam material according to claim 1 and 2, it is characterized in that, described blowing promotor is one or more in polyoxyethylene sorbitan fatty acid ester, Sorbitan fatty acid ester, castor oil polyoxyethylene ether, lauric monoglyceride.
8. complete biodegradable heat-proof polylactic acid foam material according to claim 1, is characterized in that, be made up of the raw material of following weight percent:
Described nucleator is the two-12-hydroxystearic of ethylene and talcous mixture, and described talcous particle diameter is 5000 orders, and the weight percentage of the two-12-hydroxystearic of ethylene is 1%, and talcous weight percentage is 2%;
Described blowing promotor is polyoxyethylene sorbitan fatty acid ester.
9. the preparation method of the complete biodegradable heat-proof polylactic acid foam material according to any one of claim 1 ~ 8, is characterized in that, comprise the following steps:
Utilize high-speed mixer at 100 DEG C ~ 110 DEG C by poly(lactic acid) drying treatment 20 ~ 40min, add other components after cooling, and mix, obtain mixed material; Again mixed material is added to tie rod, air-cooled, pelletizing after melt blending in twin screw extruder, obtains complete biodegradable heat-proof polylactic acid foam material.
10. the preparation method of complete biodegradable heat-proof polylactic acid foam material according to claim 9, is characterized in that, the screw slenderness ratio of described twin screw extruder is 35:1 ~ 45:1; The temperature of described melt blending is 170 DEG C ~ 180 DEG C.
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| CN106751611A (en) * | 2016-12-08 | 2017-05-31 | 吉林中粮生化有限公司 | A kind of high fondant-strength expanded polylactic acid is resin dedicated and preparation method thereof |
| CN106967280A (en) * | 2017-04-21 | 2017-07-21 | 桑德（天津）再生资源投资控股有限公司 | A kind of preparation method of the fully biodegradable foamed material of high magnification |
| CN107337912A (en) * | 2017-06-21 | 2017-11-10 | 佛山市高明科力机械有限公司 | A kind of biodegradable foamed cutlery box production technology of PLA PLAs |
| CN109762314A (en) * | 2019-01-14 | 2019-05-17 | 温州信环生物材料科技有限公司 | A kind of biodegradable foamed material and the method for manufacturing heat-resisting foaming snack box using it |
| WO2019104946A1 (en) | 2017-12-01 | 2019-06-06 | 宁波家联科技股份有限公司 | Heat resistant polylactic acid continuous extrusion foaming material and preparation method therefor |
| CN110615976A (en) * | 2019-06-24 | 2019-12-27 | 天津市大林新材料科技股份有限公司 | Biodegradable PLA microcellular foam material |
| CN111253722A (en) * | 2019-03-11 | 2020-06-09 | 汕头市三马塑胶制品有限公司 | Foaming-grade modified polylactic acid and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106751611A (en) * | 2016-12-08 | 2017-05-31 | 吉林中粮生化有限公司 | A kind of high fondant-strength expanded polylactic acid is resin dedicated and preparation method thereof |
| CN106967280A (en) * | 2017-04-21 | 2017-07-21 | 桑德（天津）再生资源投资控股有限公司 | A kind of preparation method of the fully biodegradable foamed material of high magnification |
| CN107337912A (en) * | 2017-06-21 | 2017-11-10 | 佛山市高明科力机械有限公司 | A kind of biodegradable foamed cutlery box production technology of PLA PLAs |
| WO2019104946A1 (en) | 2017-12-01 | 2019-06-06 | 宁波家联科技股份有限公司 | Heat resistant polylactic acid continuous extrusion foaming material and preparation method therefor |
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| CN109762314A (en) * | 2019-01-14 | 2019-05-17 | 温州信环生物材料科技有限公司 | A kind of biodegradable foamed material and the method for manufacturing heat-resisting foaming snack box using it |
| CN111253722A (en) * | 2019-03-11 | 2020-06-09 | 汕头市三马塑胶制品有限公司 | Foaming-grade modified polylactic acid and preparation method thereof |
| CN111253722B (en) * | 2019-03-11 | 2022-10-04 | 汕头市三马塑胶制品有限公司 | Foaming-grade modified polylactic acid and preparation method thereof |
| CN110615976A (en) * | 2019-06-24 | 2019-12-27 | 天津市大林新材料科技股份有限公司 | Biodegradable PLA microcellular foam material |
| CN112409648A (en) * | 2020-10-16 | 2021-02-26 | 安徽省怀宁县希望纸塑有限责任公司 | Starch polymer for preparing tableware and preparation method thereof |
| CN113480837A (en) * | 2021-07-29 | 2021-10-08 | 南京旭智材料科技有限公司 | Biodegradable mesh cover foaming material for fruits and vegetables and preparation method thereof |
| CN114656764A (en) * | 2022-02-23 | 2022-06-24 | 安徽丰原生物新材料有限公司 | Polylactic acid heat-resistant lunch box capable of being formed at high speed and preparation method thereof |
| CN115181320A (en) * | 2022-08-15 | 2022-10-14 | 中国科学院宁波材料技术与工程研究所 | Extrusion foaming bead capable of degrading PLA/PBAT and preparation method thereof |
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Application publication date: 20160106 |