TW202332565A - Preparation method of cellulose bio-based material and high-barrier full-biodegradable packaging bottle containing cellulose bio-based material - Google Patents
Preparation method of cellulose bio-based material and high-barrier full-biodegradable packaging bottle containing cellulose bio-based material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 49
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 38
- 229920002678 cellulose Polymers 0.000 title claims abstract description 30
- 239000001913 cellulose Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229920001046 Nanocellulose Polymers 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229920001661 Chitosan Polymers 0.000 claims abstract description 12
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 12
- 239000012760 heat stabilizer Substances 0.000 claims abstract description 12
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 229920000609 methyl cellulose Polymers 0.000 claims abstract description 11
- 239000001923 methylcellulose Substances 0.000 claims abstract description 11
- 239000004014 plasticizer Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims description 33
- 239000002023 wood Substances 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 19
- 239000003429 antifungal agent Substances 0.000 claims description 13
- 229940121375 antifungal agent Drugs 0.000 claims description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 claims description 10
- 239000002518 antifoaming agent Substances 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 10
- 235000011187 glycerol Nutrition 0.000 claims description 10
- -1 amide percarbonate Chemical class 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 8
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 8
- 241001330002 Bambuseae Species 0.000 claims description 8
- 229920000742 Cotton Polymers 0.000 claims description 8
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 8
- 240000008042 Zea mays Species 0.000 claims description 8
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 8
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 8
- 239000011425 bamboo Substances 0.000 claims description 8
- 235000005822 corn Nutrition 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical group C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 5
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 5
- 235000012424 soybean oil Nutrition 0.000 claims description 5
- 239000003549 soybean oil Substances 0.000 claims description 5
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- 241000723346 Cinnamomum camphora Species 0.000 claims description 3
- 229960000846 camphor Drugs 0.000 claims description 3
- 229930008380 camphor Natural products 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- 238000001746 injection moulding Methods 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000000341 volatile oil Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 2
- 239000002028 Biomass Substances 0.000 claims 1
- 239000000835 fiber Substances 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 2
- 239000004088 foaming agent Substances 0.000 abstract 1
- 235000010981 methylcellulose Nutrition 0.000 abstract 1
- 230000003449 preventive effect Effects 0.000 abstract 1
- 230000035699 permeability Effects 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 229920000704 biodegradable plastic Polymers 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 244000005700 microbiome Species 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L97/00—Compositions of lignin-containing materials
- C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/04—Pulping cellulose-containing materials with acids, acid salts or acid anhydrides
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/14—Gas barrier composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/10—Applications used for bottles
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- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Wood Science & Technology (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Biological Depolymerization Polymers (AREA)
- Containers Having Bodies Formed In One Piece (AREA)
- Wrappers (AREA)
Abstract
Description
本發明屬於可降解包裝瓶加工技術領域,具體涉及一種纖維素類生物基材料的製備方法及含該材料的高阻隔全生物降解包裝瓶。 The invention belongs to the technical field of degradable packaging bottle processing, and specifically relates to a preparation method of cellulose bio-based material and a high-barrier fully biodegradable packaging bottle containing the material.
目前的包裝瓶大都採用聚乙烯、聚酯為原料,這些包裝瓶,存在對氣體的透氣性阻隔性能、對濕度的阻隔性能的差異,且對於透氣量、透氧量的阻隔都需要進一步的提升;但是人們在研究如何降低透氣量、透氧量時,使用了大量的不可降解生物材料,如果人們隨意亂扔,就會造成環境污染,影響城市景觀。隨意丟棄和難以降解是造成白色污染的主要原因。白色污染不僅僅是視覺上的,更多的是對環境的壓力和對其處理的高成本,不利於可持續發展。 Most of the current packaging bottles use polyethylene and polyester as raw materials. These packaging bottles have differences in gas permeability barrier properties and humidity barrier properties, and the barrier properties of air permeability and oxygen permeability need to be further improved. ; However, when people are studying how to reduce air permeability and oxygen permeability, they use a large amount of non-degradable biological materials. If people throw them away randomly, it will cause environmental pollution and affect the urban landscape. Random disposal and difficulty in degradation are the main causes of white pollution. White pollution is not only visual, but also puts pressure on the environment and the high cost of its treatment, which is not conducive to sustainable development.
生物降解塑料是指利用環境中的溫度、濕度、礦物質和微生物(如細菌、真菌、藻類等)將聚合物材料水解或酶解為低分子物質,再由微生物吞噬完全分解,所分解的產物和殘留對環境沒有任何危害,從而引起了人們的高度關注,世界各國競相發展生物降解塑料。目前發現的生物降解塑料有很多,但均因其自身或多或少的缺陷而極大限制了其作為材料單獨使用的大規模應用。對生物降解材料進行共混改性,選取性能合適的生物降解材料組份,調節生物降解材料組份之間的配比,改善生物降解材料之間的相容性和採取適宜的材料加工手段,可以在各個生物降解材料之間 取長補短,開發出高性能的包裝瓶,這是目前包裝瓶領域的熱點研究問題。 Biodegradable plastic refers to the use of temperature, humidity, minerals and microorganisms (such as bacteria, fungi, algae, etc.) in the environment to hydrolyze or enzymatically decompose polymer materials into low molecular substances, which are then completely decomposed by microorganisms. and residues do no harm to the environment, which has attracted great attention. Countries around the world are competing to develop biodegradable plastics. There are many biodegradable plastics discovered so far, but all of them have more or less defects that greatly limit their large-scale application as single materials. Blending and modifying biodegradable materials, selecting biodegradable material components with suitable properties, adjusting the ratio of biodegradable material components, improving the compatibility between biodegradable materials and adopting appropriate material processing methods, between various biodegradable materials Learning from each other's strengths and compensating for weaknesses to develop high-performance packaging bottles is currently a hot research issue in the field of packaging bottles.
本發明的目的在於提供一種纖維素類生物基材料的製備方法及含有該材料的高阻隔全生物降解包裝瓶,該纖維素類生物基材料的主要組分均可以全生物降解,製備的包裝瓶,具有防黴、抗菌、耐熱、高阻隔、基本全生物降解的優點。 The object of the present invention is to provide a method for preparing a cellulose-based bio-based material and a high-barrier fully biodegradable packaging bottle containing the material. The main components of the cellulose-based bio-based material can all be fully biodegraded. The prepared packaging bottle , has the advantages of being mildew-proof, antibacterial, heat-resistant, high-barrier, and basically fully biodegradable.
為了實現上述目的,本發明提供了一種纖維素類生物基材料的製備方法,該纖維素類生物基材料原料組成成分按重量份數由以下比例組成:氮化木質纖維素50~100份,納米纖維素60~90份,聚乙烯醇20~30份,殼聚糖5~10份,甲基纖維素3~5份,消泡劑0.5~1.0份,增塑劑2~3份,甘油10~15份,熱穩定劑0.1~0.2份,防黴劑0.1~1份,水0~30份。上述纖維素類生物基材料的製備方法,包括以下步驟: In order to achieve the above purpose, the present invention provides a method for preparing a cellulose-based bio-based material. The raw material components of the cellulose-based bio-based material are composed of the following proportions in parts by weight: 50 to 100 parts of nitrogenated lignocellulose, 60~90 parts of cellulose, 20~30 parts of polyvinyl alcohol, 5~10 parts of chitosan, 3~5 parts of methylcellulose, 0.5~1.0 parts of defoaming agent, 2~3 parts of plasticizer, 10 parts of glycerin ~15 parts, heat stabilizer 0.1~0.2 parts, antifungal agent 0.1~1 part, water 0~30 parts. The preparation method of the above-mentioned cellulose bio-based material includes the following steps:
(1)將上述重量份的氮化木質纖維素,納米纖維素,聚乙烯醇和殼聚糖,依次加入高速混合機中攪拌1~3h,混合均勻; (1) Add the above weight portions of nitrogenated lignocellulose, nanocellulose, polyvinyl alcohol and chitosan to a high-speed mixer in sequence and stir for 1 to 3 hours until evenly mixed;
(2)將上述重量份的甲基纖維素,消泡劑,增塑劑,甘油,熱穩定劑,防黴劑和水,依次加入高速混合機中攪拌1~3h,混合均勻; (2) Add the above weight portions of methylcellulose, defoaming agent, plasticizer, glycerin, heat stabilizer, antifungal agent and water to a high-speed mixer in turn and stir for 1 to 3 hours until evenly mixed;
(3)將步驟(1)和步驟(2)得到的混合物,脫色、真空除水後,依次加入高速混合機中攪拌1~2h,混合均勻後,用80~130℃平面板熱壓2~6h後,得到纖維素類生物基材料。 (3) After decolorizing and vacuum dehydrating the mixture obtained in steps (1) and (2), add it to a high-speed mixer and stir for 1 to 2 hours. After mixing evenly, heat press it with a flat plate at 80 to 130°C for 2 to After 6 hours, cellulosic bio-based materials were obtained.
進一步地,上述氮化木質纖維素的製備方法,包括以下步驟: Further, the preparation method of the above-mentioned nitrogenated lignocellulose includes the following steps:
(1)選取棉花或玉米莖切割,除雜,粉碎,過篩,得到 210~280目的木粉; (1) Select cotton or corn stalks, cut them, remove impurities, crush them, and sift to obtain 210~280 mesh wood powder;
(2)將210~280目的木粉加入到水和乙醇質量比為100比5的混合溶液中,保持溫度在25℃~40℃之間,然後進行攪拌研磨,時間為1h-5h,即得到木質纖維素分散液; (2) Add 210~280 mesh wood powder into a mixed solution of water and ethanol with a mass ratio of 100:5, keep the temperature between 25℃~40℃, and then stir and grind for 1h-5h to obtain Lignocellulose dispersions;
(3)在木質纖維素分散液中添加尿素,加熱至65-74℃,攪拌均勻後,再添加過氧乙酸或者過碳酸醯胺,繼續攪拌反應2小時,然後進行過濾,洗滌,乾燥至恆重,得到氮化木質纖維素。 (3) Add urea to the lignocellulose dispersion, heat to 65-74°C, stir evenly, then add peracetic acid or amide percarbonate, continue stirring for 2 hours, then filter, wash, and dry to constant temperature. Heavy to obtain nitrogenated lignocellulose.
進一步地,上述防黴劑為檸檬酸、香樟精油和孟宗竹提取物中的至少一種。 Further, the above-mentioned antifungal agent is at least one of citric acid, camphor essential oil and Mengzong bamboo extract.
進一步地,上述防黴劑為孟宗竹提取物。 Further, the above-mentioned antifungal agent is an extract of Mengzong bamboo.
進一步地,上述納米纖維素的製備方法,包括以下步驟: Further, the preparation method of the above-mentioned nanocellulose includes the following steps:
(1)選取棉花或玉米莖切割,除雜,粉碎,過篩,得到210~280目的木粉; (1) Select cotton or corn stems to cut, remove impurities, crush and sieve to obtain 210~280 mesh wood powder;
(2)將木粉與質量百分含量為62~65%的硫酸混合,攪拌均勻,得到木粉硫酸混合液; (2) Mix wood powder with sulfuric acid with a mass percentage of 62~65%, stir evenly, and obtain a wood powder sulfuric acid mixture;
(3)將步驟(2)得到的混合液在光波反應器中預處理,反應溫度60℃,處理時間30min; (3) Pretreat the mixed solution obtained in step (2) in a light wave reactor at a reaction temperature of 60°C and a treatment time of 30 minutes;
(4)將經過光波預處理的反應混合液體在65~70℃下,添加5%的氯化鈣溶液,水解2個小時; (4) Add 5% calcium chloride solution to the reaction mixed liquid pretreated by light waves at 65~70°C, and hydrolyze it for 2 hours;
(5)將水解後的混合液體,離心、過濾、洗滌; (5) Centrifuge, filter and wash the hydrolyzed mixed liquid;
(6)將洗滌後固體真空乾燥後,用超聲波粉碎,篩分,得到納米纖維素。 (6) After vacuum drying the washed solid, use ultrasonic pulverization and sieving to obtain nanocellulose.
進一步地,上述消泡劑為聚二甲基矽氧烷,增塑劑為環氧大豆油,熱穩定劑為磷酸三苯酯。 Further, the above-mentioned defoaming agent is polydimethylsiloxane, the plasticizer is epoxidized soybean oil, and the heat stabilizer is triphenyl phosphate.
通過採用上述原材料優選,本發明的纖維素類生物基材料主要組分為基本可以全生物降解的氮化木質纖維素,納米纖維素,聚乙烯醇和殼聚糖等的特定比例配合,配以本發明獨特的製備工藝,誘導纖維素分子鏈的重排,使得各成分的結合更加緊密,促進纖維素網格結構之間形成緻密的納米纖維,阻隔空氣和水分的透入;且本發明製備的纖維素類生物基材料基本可以全生物降解,綠色環保性能顯著提高,通過添加熱穩定劑,本發明的包裝瓶的耐熱溫度可以提高到120℃以上;通過添加防黴劑,本發明的包裝瓶防黴抗菌性能顯著提高,防黴等級均為0或者1級。 By using the above-mentioned raw material optimization, the main components of the cellulose bio-based material of the present invention are a specific proportion of nitrogenated lignocellulose, nanocellulose, polyvinyl alcohol and chitosan, which are basically fully biodegradable. The unique preparation process is invented to induce the rearrangement of cellulose molecular chains, making the combination of each component closer, promoting the formation of dense nanofibers between the cellulose grid structures, and blocking the penetration of air and moisture; and the products prepared by the invention Cellulosic bio-based materials can basically be completely biodegraded, and their green and environmental protection properties are significantly improved. By adding heat stabilizers, the heat-resistant temperature of the packaging bottles of the present invention can be increased to above 120°C; by adding antifungal agents, the heat-resistant temperature of the packaging bottles of the present invention can be improved. The anti-mildew and anti-bacterial performance is significantly improved, and the anti-mildew levels are all 0 or 1.
本發明還提供一種利用上述纖維素類生物基材料製備的高阻隔全生物降解包裝瓶,其製備方法包括以下步驟: The invention also provides a high-barrier fully biodegradable packaging bottle prepared by using the above-mentioned cellulose bio-based material, and its preparation method includes the following steps:
(1)將上述纖維素類生物基材料在儲料倉內減壓處理1-2小時脫氣,然後用擠出設備擠出加工得到母粒; (1) The above-mentioned cellulosic bio-based materials are decompressed and degassed in a storage silo for 1-2 hours, and then extruded using extrusion equipment to obtain masterbatch;
(2)將步驟(1)得到的母粒,經擠出或注塑成型後,得到管狀型坯,趁熱或加熱到軟化狀態,吹塑置於合模中; (2) After extruding or injection molding the masterbatch obtained in step (1), a tubular parison is obtained, which is heated or heated to a softened state, and then blow molded and placed in a closed mold;
(3)模具合模冷卻定型,開模後成品進入副模,在副模內切口去邊,製得包裝瓶。 (3) The mold is closed and cooled to shape. After the mold is opened, the finished product enters the auxiliary mold, and the edges are cut in the auxiliary mold to produce a packaging bottle.
本發明製得的包裝瓶,由於原材料的優異性能和先進的製備工藝,使得本發明製備的安全瓶,具有防黴、抗菌、耐熱、高阻隔的性能,使用後的包裝瓶能夠幾乎全部降解形成小分子,並在光、氧氣以及微生物的共同作用下分解形成二氧化碳和水,對環境的污染性大大降低,有利於 提高與生物相容性。 Due to the excellent properties of the raw materials and the advanced preparation process, the packaging bottles prepared by the present invention have the properties of mildew-proof, antibacterial, heat-resistant and high barrier properties, and the packaging bottles after use can be almost completely degraded to form Small molecules, and decompose to form carbon dioxide and water under the combined action of light, oxygen and microorganisms, which greatly reduces the pollution to the environment and is beneficial to Improve biocompatibility.
本發明的包裝瓶可以廣泛應用於化工、化妝品、食品、醫藥等領域。 The packaging bottle of the present invention can be widely used in chemical industry, cosmetics, food, medicine and other fields.
下面對本發明實施例中的技術方案進行清楚、完整的描述,顯然,所描述的實施例僅僅是本發明的一部分實施例,而不是全部的實施例。基於本發明中的實施例,本領域普通技術人員在沒有做出創造性勞動前提下所獲得的所有其他實施例,都屬於本發明保護的範圍。應當理解,此處所描述的具體實施例僅僅用以解釋本發明,並不用於限定本發明。 The technical solutions in the embodiments of the present invention are clearly and completely described below. Obviously, the described embodiments are only some of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the scope of protection of the present invention. It should be understood that the specific embodiments described here are only used to explain the present invention and are not intended to limit the present invention.
實施例1 Example 1
一種纖維素類生物基材料的製備方法,該纖維素類生物基材料原料組成成分按重量份數由以下比例組成:氮化木質纖維素50份,納米纖維素60份,聚乙烯醇20份,殼聚糖5份,甲基纖維素3份,聚二甲基矽氧烷0.5份,環氧大豆油2份,甘油10份,磷酸三苯酯0.1份,檸檬酸0.1份。 A method for preparing cellulose-based bio-based materials. The raw material components of the cellulose-based bio-based materials are composed of the following proportions in parts by weight: 50 parts of nitrogenated lignocellulose, 60 parts of nanocellulose, and 20 parts of polyvinyl alcohol. 5 parts of chitosan, 3 parts of methylcellulose, 0.5 parts of polydimethylsiloxane, 2 parts of epoxidized soybean oil, 10 parts of glycerin, 0.1 part of triphenyl phosphate, and 0.1 part of citric acid.
上述纖維素類生物基材料的製備方法,包括以下步驟: The preparation method of the above-mentioned cellulose bio-based material includes the following steps:
(1)將上述重量份的氮化木質纖維素,納米纖維素,聚乙烯醇和殼聚糖,依次加入高速混合機中攪拌1h,混合均勻; (1) Add the above weight portions of nitrogenated lignocellulose, nanocellulose, polyvinyl alcohol and chitosan to a high-speed mixer in sequence and stir for 1 hour until evenly mixed;
(2)將上述重量份的甲基纖維素,消泡劑,增塑劑,甘油,熱穩定劑和防黴劑,依次加入高速混合機中攪拌1h,混合均勻; (2) Add the above weight parts of methylcellulose, defoaming agent, plasticizer, glycerin, heat stabilizer and antifungal agent to a high-speed mixer in sequence and stir for 1 hour until evenly mixed;
(3)將步驟(1)和步驟(2)得到的混合物,脫色、真空除水後,依次加入高速混合機中攪拌1~2h,混合均勻後,用80~130℃平面板熱壓2~6h後,得到纖維素類生物基材料。 (3) After decolorizing and vacuum dehydrating the mixture obtained in steps (1) and (2), add it to a high-speed mixer and stir for 1 to 2 hours. After mixing evenly, heat press it with a flat plate at 80 to 130°C for 2 to After 6 hours, cellulosic bio-based materials were obtained.
上述氮化木質纖維素的製備方法,包括以下步驟: The preparation method of the above-mentioned nitrogenated lignocellulose includes the following steps:
(1)選取棉花或玉米莖切割,除雜,粉碎,過篩,得到210~280目的木粉; (1) Select cotton or corn stems to cut, remove impurities, crush and sieve to obtain 210~280 mesh wood powder;
(2)將210~280目的木粉加入到水和乙醇質量比為100比5的混合溶液中,保持溫度在25~30℃之間,然後進行攪拌研磨,時間為1h,即得到木質纖維素分散液; (2) Add 210~280 mesh wood powder to a mixed solution of water and ethanol with a mass ratio of 100:5, keep the temperature between 25~30°C, and then stir and grind for 1 hour to obtain lignocellulose Dispersions;
(3)在木質纖維素分散液中添加尿素,加熱至65-70℃,攪拌均勻後,再添加過氧乙酸,繼續攪拌反應2小時,然後進行過濾,洗滌,乾燥至恆重,得到氮化木質纖維素。 (3) Add urea to the lignocellulose dispersion, heat to 65-70°C, stir evenly, then add peracetic acid, continue stirring for 2 hours, then filter, wash, and dry to constant weight to obtain nitrided Lignocellulose.
上述納米纖維素的製備方法,包括以下步驟: The preparation method of the above-mentioned nanocellulose includes the following steps:
(1)選取棉花或玉米莖切割,除雜,粉碎,過篩,得到210~280目的木粉; (1) Select cotton or corn stems to cut, remove impurities, crush and sieve to obtain 210~280 mesh wood powder;
(2)將木粉與質量百分含量為62~65%的硫酸混合,攪拌均勻,得到木粉硫酸混合液; (2) Mix wood powder with sulfuric acid with a mass percentage of 62~65%, stir evenly, and obtain a wood powder sulfuric acid mixture;
(3)將步驟(2)得到的混合液在光波反應器中預處理,反應溫度60℃,處理時間30min; (3) Pretreat the mixed solution obtained in step (2) in a light wave reactor at a reaction temperature of 60°C and a treatment time of 30 minutes;
(4)將經過光波預處理的反應混合液體在65~70℃下,添加5%的氯化鈣溶液,水解2個小時; (4) Add 5% calcium chloride solution to the reaction mixed liquid pretreated by light waves at 65~70°C, and hydrolyze it for 2 hours;
(5)將水解後的混合液體,離心、過濾、洗滌; (5) Centrifuge, filter and wash the hydrolyzed mixed liquid;
(6)將洗滌後固體真空乾燥後,用超聲波粉碎,篩分,得到納米纖維素。 (6) After vacuum drying the washed solid, use ultrasonic pulverization and sieving to obtain nanocellulose.
利用上述纖維素類生物基材料製備的包裝瓶,其製備方法包 括以下步驟: Packaging bottles prepared using the above-mentioned cellulosic bio-based materials, the preparation method includes Includes the following steps:
(1)將上述纖維素類生物基材料在儲料倉內減壓處理1-2小時脫氣,然後用擠出設備擠出加工得到母粒; (1) The above-mentioned cellulosic bio-based materials are decompressed and degassed in a storage silo for 1-2 hours, and then extruded using extrusion equipment to obtain masterbatch;
(2)將步驟(1)得到的母粒,經擠出或注塑成型後,得到管狀型坯,趁熱或加熱到軟化狀態,吹塑置於合模中; (2) After extruding or injection molding the masterbatch obtained in step (1), a tubular parison is obtained, which is heated or heated to a softened state, and then blow molded and placed in a closed mold;
(3)模具合模冷卻定型,開模後成品進入副模,在副模內切口去邊,製得包裝瓶。 (3) The mold is closed and cooled to shape. After the mold is opened, the finished product enters the auxiliary mold, and the edges are cut in the auxiliary mold to produce a packaging bottle.
實施例2 Example 2
一種纖維素類生物基材料的製備方法,該纖維素類生物基材料原料組成成分按重量份數由以下比例組成:氮化木質纖維素90份,納米纖維素90份,聚乙烯醇30份,殼聚糖10份,甲基纖維素4份,聚二甲基矽氧烷1份,環氧大豆油3份,甘油15份,磷酸三苯酯0.2份,香樟精油和孟宗竹提取物的混合物1份,水25份。 A method for preparing cellulose-based bio-based materials. The raw materials of the cellulose-based bio-based materials are composed of the following proportions in parts by weight: 90 parts of nitrogenated lignocellulose, 90 parts of nanocellulose, and 30 parts of polyvinyl alcohol. 10 parts of chitosan, 4 parts of methylcellulose, 1 part of polydimethylsiloxane, 3 parts of epoxidized soybean oil, 15 parts of glycerin, 0.2 parts of triphenyl phosphate, a mixture of camphor essential oil and Mengzong bamboo extract 1 part, 25 parts water.
上述纖維素類生物基材料的製備方法,包括以下步驟: The preparation method of the above-mentioned cellulose bio-based material includes the following steps:
(1)將上述重量份的氮化木質纖維素,納米纖維素,聚乙烯醇和殼聚糖,依次加入高速混合機中攪拌3h,混合均勻; (1) Add the above weight portions of nitrogenated lignocellulose, nanocellulose, polyvinyl alcohol and chitosan to a high-speed mixer in turn and stir for 3 hours until evenly mixed;
(2)將上述重量份的甲基纖維素,消泡劑,增塑劑,甘油,熱穩定劑,防黴劑和水,依次加入高速混合機中攪拌3h,混合均勻; (2) Add the above weight parts of methylcellulose, defoaming agent, plasticizer, glycerin, heat stabilizer, antifungal agent and water to a high-speed mixer in sequence and stir for 3 hours until evenly mixed;
(3)將步驟(1)和步驟(2)得到的混合物,脫色、真空除水後,依次加入高速混合機中攪拌1~2h,混合均勻後,用80~130℃平面板熱壓2~6h後,得到纖維素類生物基材料。 (3) After decolorizing and vacuum dehydrating the mixture obtained in steps (1) and (2), add it to a high-speed mixer and stir for 1 to 2 hours. After mixing evenly, heat press it with a flat plate at 80 to 130°C for 2 to After 6 hours, cellulosic bio-based materials were obtained.
上述氮化木質纖維素的製備方法,包括以下步驟: The preparation method of the above-mentioned nitrogenated lignocellulose includes the following steps:
(1)選取棉花或玉米莖切割,除雜,粉碎,過篩,得到210~280目的木粉; (1) Select cotton or corn stems to cut, remove impurities, crush and sieve to obtain 210~280 mesh wood powder;
(2)將210~280目的木粉加入到水和乙醇質量比為100比5的混合溶液中,保持溫度在35~40℃之間,然後進行攪拌研磨,時間為5h,即得到木質纖維素分散液; (2) Add 210~280 mesh wood powder to a mixed solution of water and ethanol with a mass ratio of 100:5, keep the temperature between 35~40°C, and then stir and grind for 5 hours to obtain lignocellulose Dispersions;
(3)在木質纖維素分散液中添加尿素,加熱至69-74℃,攪拌均勻後,再添加過氧乙酸,繼續攪拌反應2小時,然後進行過濾,洗滌,乾燥至恆重,得到氮化木質纖維素。 (3) Add urea to the lignocellulose dispersion, heat to 69-74°C, stir evenly, then add peracetic acid, continue stirring for 2 hours, then filter, wash, and dry to constant weight to obtain nitrided Lignocellulose.
其中,納米纖維素和包裝瓶的製備方法同實施例1。 Among them, the preparation methods of nanocellulose and packaging bottles are the same as in Example 1.
實施例3 Example 3
一種纖維素類生物基材料的製備方法,該纖維素類生物基材料原料組成成分按重量份數由以下比例組成:氮化木質纖維素80份,納米纖維素70份,聚乙烯醇25份,殼聚糖8份,甲基纖維素4份,聚二甲基矽氧烷1份,環氧大豆油3份,甘油15份,磷酸三苯酯0.3份,孟宗竹提取物0.5份,水10份。 A method for preparing cellulose-based bio-based materials. The raw material components of the cellulose-based bio-based materials are composed of the following proportions by weight: 80 parts of nitrogenated lignocellulose, 70 parts of nanocellulose, and 25 parts of polyvinyl alcohol. 8 parts of chitosan, 4 parts of methylcellulose, 1 part of polydimethylsiloxane, 3 parts of epoxidized soybean oil, 15 parts of glycerin, 0.3 parts of triphenyl phosphate, 0.5 parts of Mengzong bamboo extract, 10 parts of water .
上述纖維素類生物基材料的製備方法,包括以下步驟: The preparation method of the above-mentioned cellulose bio-based material includes the following steps:
(1)將上述重量份的氮化木質纖維素,納米纖維素,聚乙烯醇和殼聚糖,依次加入高速混合機中攪拌2h,混合均勻; (1) Add the above weight portions of nitrogenated lignocellulose, nanocellulose, polyvinyl alcohol and chitosan to a high-speed mixer in sequence and stir for 2 hours until evenly mixed;
(2)將上述重量份的甲基纖維素,消泡劑,增塑劑,甘油,熱穩定劑,防黴劑和水,依次加入高速混合機中攪拌2h,混合均勻; (2) Add the above weight parts of methylcellulose, defoaming agent, plasticizer, glycerin, heat stabilizer, antifungal agent and water to a high-speed mixer in sequence and stir for 2 hours until evenly mixed;
(3)將步驟(1)和步驟(2)得到的混合物,脫色、真空除水後,依次加入高速混合機中攪拌1~2h,混合均勻後,用80~130℃平面板熱壓2~6h後,得到纖維素類生物基材料。 (3) After decolorizing and vacuum dehydrating the mixture obtained in steps (1) and (2), add it to a high-speed mixer and stir for 1 to 2 hours. After mixing evenly, heat press it with a flat plate at 80 to 130°C for 2 to After 6 hours, cellulosic bio-based materials were obtained.
上述氮化木質纖維素的製備方法,包括以下步驟: The preparation method of the above-mentioned nitrogenated lignocellulose includes the following steps:
(1)選取棉花或玉米莖切割,除雜,粉碎,過篩,得到210~280目的木粉; (1) Select cotton or corn stems to cut, remove impurities, crush and sieve to obtain 210~280 mesh wood powder;
(2)將210~280目的木粉加入到水和乙醇質量比為100比5的混合溶液中,保持溫度在35~40℃之間,然後進行攪拌研磨,時間為3h,即得到木質纖維素分散液; (2) Add 210~280 mesh wood powder to a mixed solution of water and ethanol with a mass ratio of 100:5, keep the temperature between 35~40°C, and then stir and grind for 3 hours to obtain lignocellulose Dispersions;
(3)在木質纖維素分散液中添加尿素,加熱至69-74℃,攪拌均勻後,再添加過氧乙酸,繼續攪拌反應2小時,然後進行過濾,洗滌,乾燥至恆重,得到氮化木質纖維素。 (3) Add urea to the lignocellulose dispersion, heat to 69-74°C, stir evenly, then add peracetic acid, continue stirring for 2 hours, then filter, wash, and dry to constant weight to obtain nitrided Lignocellulose.
其中,納米纖維素和包裝瓶的製備方法同實施例1。 Among them, the preparation methods of nanocellulose and packaging bottles are the same as in Example 1.
對比例1 Comparative example 1
一種包裝瓶的製備方法,該包裝瓶原材料組成成分按重量份數由以下比例組成:聚乙烯100份,消泡劑0.5~1.0份,增塑劑2~3份,包裝瓶的製備方法同實施例1。 A method for preparing a packaging bottle. The raw material components of the packaging bottle are composed of the following proportions in parts by weight: 100 parts of polyethylene, 0.5 to 1.0 parts of defoaming agent, and 2 to 3 parts of plasticizer. The preparation method of the packaging bottle is the same as in the implementation example 1.
性能測試 Performance testing
對以上實施例和對比例製得的包裝瓶進行性能測試,測試結果見表1。 Performance tests were performed on the packaging bottles prepared in the above examples and comparative examples. The test results are shown in Table 1.
表1 包裝瓶性能測試結果
以上資料表明,由於採用獨特的原材料和特殊的製備工藝過 程,使得本發明製備的包裝瓶的氧氣通過量,水蒸氣透過量,耐壓強度等指標均明顯優於對比例,本發明採用可降解的原材料,使得本發明製得的包裝瓶降解率為98%;採用熱穩定劑磷酸三苯酯後,本發明製得的包裝瓶熱穩定性顯著提高,耐熱溫度提高到120℃以上,但是添加量沒有隨著添加量的增加對包裝瓶的熱穩定性而增加,0.2份的添加量為最合適的量;添加防黴劑孟宗竹提取物後,本發明的安全瓶防黴等級均為0級,表明在本發明中孟宗竹提取物的防黴效果更好。 The above data shows that due to the use of unique raw materials and special preparation processes process, so that the oxygen throughput, water vapor permeability, pressure resistance strength and other indicators of the packaging bottle prepared by the present invention are significantly better than those of the comparative example. The present invention uses degradable raw materials, so that the degradation rate of the packaging bottle prepared by the present invention is 98%; after using the heat stabilizer triphenyl phosphate, the thermal stability of the packaging bottle prepared by the present invention is significantly improved, and the heat-resistant temperature is increased to above 120°C, but the added amount does not improve the thermal stability of the packaging bottle as the added amount increases. properties are increased, and the addition amount of 0.2 parts is the most appropriate amount; after adding the antifungal agent Mengzong bamboo extract, the anti-mold levels of the safety bottles of the present invention are all level 0, indicating that the anti-mold effect of the Mengzong bamboo extract in the present invention is better good.
以上所述僅為本發明的優選實施例,並非因此限制本發明的專利範圍,凡是在本發明的構思下,利用本發明說明書所作的等效結構變換,或直接/間接運用在其他相關的技術領域均包括在本發明的專利保護範圍內。 The above are only preferred embodiments of the present invention, and do not limit the patent scope of the present invention. Under the concept of the present invention, equivalent structural transformations made by using the description of the present invention, or directly/indirectly applied to other related technologies All fields are included in the patent protection scope of the present invention.
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CN202210127767.5A CN114163833B (en) | 2022-02-11 | 2022-02-11 | Preparation method of cellulose bio-based material and high-barrier full-biodegradable packaging bottle containing cellulose bio-based material |
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