CN114031909A - Starch-based degradable desorption tube material and preparation method thereof - Google Patents
Starch-based degradable desorption tube material and preparation method thereof Download PDFInfo
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- 229920002472 Starch Polymers 0.000 title claims abstract description 75
- 239000008107 starch Substances 0.000 title claims abstract description 75
- 235000019698 starch Nutrition 0.000 title claims abstract description 75
- 239000000463 material Substances 0.000 title claims abstract description 49
- 238000003795 desorption Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 21
- 239000010902 straw Substances 0.000 claims abstract description 38
- 239000002667 nucleating agent Substances 0.000 claims abstract description 29
- 229920001896 polybutyrate Polymers 0.000 claims abstract description 27
- UAUDZVJPLUQNMU-UHFFFAOYSA-N Erucasaeureamid Natural products CCCCCCCCC=CCCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-UHFFFAOYSA-N 0.000 claims abstract description 21
- UAUDZVJPLUQNMU-KTKRTIGZSA-N erucamide Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-KTKRTIGZSA-N 0.000 claims abstract description 21
- 239000004014 plasticizer Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims description 66
- 239000000203 mixture Substances 0.000 claims description 66
- 239000000843 powder Substances 0.000 claims description 44
- 239000002245 particle Substances 0.000 claims description 24
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 22
- 239000000155 melt Substances 0.000 claims description 17
- 229920000858 Cyclodextrin Polymers 0.000 claims description 16
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims description 16
- 238000001125 extrusion Methods 0.000 claims description 13
- 235000013773 glyceryl triacetate Nutrition 0.000 claims description 12
- 229960002622 triacetin Drugs 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 229920002261 Corn starch Polymers 0.000 claims description 10
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims description 10
- 239000012752 auxiliary agent Substances 0.000 claims description 10
- 239000008120 corn starch Substances 0.000 claims description 10
- 239000011812 mixed powder Substances 0.000 claims description 10
- 208000034530 PLAA-associated neurodevelopmental disease Diseases 0.000 claims description 9
- 239000004570 mortar (masonry) Substances 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 240000003183 Manihot esculenta Species 0.000 claims description 4
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 claims description 4
- SWKVSFPUHCMFJY-UHFFFAOYSA-N 6-methyl-2-oxo-5-pyridin-4-yl-1h-pyridine-3-carboxamide Chemical compound N1C(=O)C(C(N)=O)=CC(C=2C=CN=CC=2)=C1C SWKVSFPUHCMFJY-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- JKMHVFFHLPXIFV-UHFFFAOYSA-L zinc;phenyl phosphate Chemical compound [Zn+2].[O-]P([O-])(=O)OC1=CC=CC=C1 JKMHVFFHLPXIFV-UHFFFAOYSA-L 0.000 claims description 2
- 229940116351 sebacate Drugs 0.000 claims 2
- CXMXRPHRNRROMY-UHFFFAOYSA-L sebacate(2-) Chemical compound [O-]C(=O)CCCCCCCCC([O-])=O CXMXRPHRNRROMY-UHFFFAOYSA-L 0.000 claims 2
- 229920000747 poly(lactic acid) Polymers 0.000 abstract description 47
- 239000011347 resin Substances 0.000 abstract description 3
- 229920005989 resin Polymers 0.000 abstract description 3
- 239000002861 polymer material Substances 0.000 abstract description 2
- 239000004626 polylactic acid Substances 0.000 description 47
- PFQAIMSYOXGWGG-UHFFFAOYSA-N N'-benzoylbenzohydrazide decanedioic acid Chemical compound C(C1=CC=CC=C1)(=O)NNC(C1=CC=CC=C1)=O.C(=O)(O)CCCCCCCCC(=O)O PFQAIMSYOXGWGG-UHFFFAOYSA-N 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- 239000008187 granular material Substances 0.000 description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 7
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 4
- 239000000806 elastomer Substances 0.000 description 4
- 238000001746 injection moulding Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000011258 core-shell material Substances 0.000 description 3
- 238000011031 large-scale manufacturing process Methods 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 description 2
- 239000005062 Polybutadiene Substances 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 229920000704 biodegradable plastic Polymers 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920002857 polybutadiene Polymers 0.000 description 2
- 229920001195 polyisoprene Polymers 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 229930182843 D-Lactic acid Natural products 0.000 description 1
- JVTAAEKCZFNVCJ-UWTATZPHSA-N D-lactic acid Chemical compound C[C@@H](O)C(O)=O JVTAAEKCZFNVCJ-UWTATZPHSA-N 0.000 description 1
- 229920002988 biodegradable polymer Polymers 0.000 description 1
- 239000004621 biodegradable polymer Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 235000020965 cold beverage Nutrition 0.000 description 1
- 239000002361 compost Substances 0.000 description 1
- 238000009264 composting Methods 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 229940022769 d- lactic acid Drugs 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- OEBRCSBPOCUVMW-UHFFFAOYSA-N dibenzoyl decanedioate Chemical compound C=1C=CC=CC=1C(=O)OC(=O)CCCCCCCCC(=O)OC(=O)C1=CC=CC=C1 OEBRCSBPOCUVMW-UHFFFAOYSA-N 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D23/00—Producing tubular articles
- B29D23/001—Pipes; Pipe joints
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Biological Depolymerization Polymers (AREA)
Abstract
The invention discloses a starch-based degradable straw material and a preparation method thereof, belonging to the technical field of high polymer materials, wherein the starch-based degradable straw material comprises the following components in parts by weight: 60-80 parts of PLA, 3-7 parts of PBAT, 5-30 parts of starch, 3-10 parts of plasticizer, 0.5-1 part of nucleating agent, 0.5-1 part of erucamide and 0.5-2 parts of hyperbranched assistant; the preparation method of the starch-based degradable desorption tube material comprises the following steps: PLA, PBAT, starch, a plasticizer, a nucleating agent, erucamide and hyperbranched resin are melted and blended uniformly at a high speed and then are extruded to obtain a starch-based degradable straw material; the starch-based degradable desorption tube material has high heat resistance, high toughness and biodegradability.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a starch-based degradable desorption tube material and a preparation method thereof.
Background
Biodegradable plastics, also called biodegradable plastics, are those which are degraded by the action of microorganisms present in nature under conditions of nature such as soil and/or sandy soil, and/or under specific conditions such as composting conditions or anaerobic digestion conditions or in aqueous culture solutions, and finally completely degraded to carbon dioxide (CO)2) Or/and methane (CH)4) Water (H)2O) and mineralized inorganic salts of the elements contained therein, and new plastics of biomass. Polylactic acid (PLA) is a completely biodegradable polymer, has mechanical properties similar to that of PET, can replace PET in a plurality of application fields, such as making cups, lunch boxes, lids and the like, and knife, fork, spoons, straws and the like used in the market at present are mostly made of PP materials, and the PP materials belong to petrochemical-based materials, are not degradable, and can cause environmental pollution when being discarded in the environment after being used. PLA belongs to a completely degradable material, can be completely degraded into carbon dioxide and water in the environment with the temperature of 50 ℃ and the humidity of 50 percent within 3 to 6 months, enters the environment, and has no pollution to the environment. Thus, polylactic acid is considered to be suitable for use in place of PP for extrusion of straws. The suction pipe and the knife and fork spoon which are suitable for being made of polylactic acid can only be used in the field of cold drinks at 30-50 ℃ and cannot be used at 80-100 ℃, in addition, the price of the polylactic acid is 3 ten thousand per ton, and the material cost is high, so that the application range of the polylactic acid as the suction pipe and other tableware is limited, and the polylactic acid as the tableware has the defect of poor heat resistance, and has the characteristic of being relatively brittle and has the problems of brittleness, breakage and cracking in the use process. With the vigorous promotion of national plastic prohibited orders, the tableware will be fully used in the futureThe polylactic acid composite material is made of degradable materials, so that the development of the polylactic acid composite material with high temperature resistance and high toughness is imminent.
In the prior art, the heat resistance and toughening modification of polylactic acid are carried out, and the high-purity polylactic acid is prepared by controlling the polymerization process and the purity of monomers such as multiple separation and purification in the aspect of polymerization. For example, the patent "CN 100567246C" is a process for preparing high-purity L-lactic acid, which adopts the idea. In another method, a nucleating agent is added in the polymerization process of polylactic acid to improve the heat resistance of the polylactic acid by increasing the crystallization rate, for example, patent "CN 101475736B" discloses an injection molding method of polylactic acid, which comprises mixing the nucleating agent into a solvent, mixing the polylactic acid into the solvent, drying the polylactic acid by a drying device to perform low-degree crystallization, and improving the heat resistance of the polylactic acid by matching with an injection molding process. The method has complex process, is not environment-friendly and is not beneficial to large-scale production. Patent "CN 106589872B" discloses a high-strength heat-resistant polylactic acid composition, which mainly adopts inorganic filler and glass fiber to improve heat resistance, and elastomer with core-shell structure to improve toughness. But the inorganic substance and the glass fiber are added, so that the flowability of the polylactic acid can be greatly reduced, a mold is difficult to fill with a melt in the injection molding process, and the stable injection molding cannot be realized, and the problems of uneven mixing, material mixing and powder leakage in the processing process are caused by the addition of the inorganic filler. On the other hand, the core is added with an elastomer with a core-shell structure, and the core layer is polybutadiene or polyisoprene; the shell layer is composed of styrene and poly D-lactic acid, polybutadiene or polyisoprene is a non-degradable material, degradation of the polylactic acid is influenced by introduction, the elastomer with the core-shell structure is expensive, the toughening effect is difficult to achieve after 5% of the elastomer is added, the degradable national standard GBT 20197-.
In order to improve the heat resistance of polylactic acid, increase the toughness of the polylactic acid, reduce the material cost, overcome the defects of low heat resistance, large material brittleness, high cost and the like, a starch-based degradable straw material with heat resistance, toughness and low cost and a preparation method thereof are developed, the straw material can be degraded into carbon dioxide and water in 3-6 months under the condition of compost, and the relative biological decomposition rate is more than 90 percent.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to solve the technical problem of providing a starch-based degradable desorption tube material and a preparation method thereof.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the starch-based degradable desorption tube material comprises the following components in parts by weight:
60-80 parts of PLA, 3-7 parts of PBAT, 5-30 parts of starch, 3-10 parts of plasticizer, 0.5-1 part of nucleating agent, 0.5-1 part of erucamide and 0.5-2 parts of hyperbranched assistant;
wherein the optical purity of the PLA is 95-100%, and the melt index (190 ℃, 2.16kg) of the PLA is 2-8g/10 min.
As a further scheme of the invention: the paint comprises the following components in parts by weight:
65-70 parts of PLA, 3-7 parts of PBAT, 5-30 parts of starch, 3-10 parts of plasticizer, 0.5-1 part of nucleating agent, 0.5-1 part of erucamide and 0.5-2 parts of hyperbranched assistant;
wherein the optical purity of the PLA is more than or equal to 99.9 percent, and the melt index (190 ℃, 2.16kg) of the PLA is 3-7g/10 min.
As a further scheme of the invention: the melt index of the PBAT is 3 to 6g/10min (190 ℃, 2.16 kg).
As a further scheme of the invention: the starch is one or a mixture of two of corn starch and cassava starch, the mesh number of the starch is more than or equal to 100 meshes, and the whiteness is more than or equal to 90%.
As a further scheme of the invention: the plasticizer is one or a mixture of glycerol triacetate and tributyl citrate.
As a further scheme of the invention: the nucleating agent is one or a mixture of more of potassium benzene sulfonate, zinc phenyl phosphate, dibenzoyl sebacate, organic phosphate and cyclodextrin.
As a further scheme of the invention: the nucleating agent is a blend of sebacic acid dibenzoyl hydrazine and cyclodextrin, the erucamide is selected from one of PMC model of ArmoslipE, British Poa (Croda) and Korean pathwel, the hyperbranched auxiliary agent is solid powder, and the melting range is 145-155 ℃.
The preparation method of the starch-based degradable desorption tube material comprises the following steps:
grinding the nucleating agent particles in a mortar to obtain uniformly dispersed nucleating agent powder A;
mixing the powder A, the starch, the erucamide and the hyperbranched auxiliary agent in a cold mixer to obtain uniformly mixed powder B;
adding PLA and PBAT into a high-speed mixer, blending for 20min, uniformly adding a plasticizer while stirring in the process of blending the mixture, and blending for 10min to obtain a mixture C;
adding the powder B and the powder C into a high-speed mixer, and mixing for 10min to obtain a blend D;
adding the blend D into a double-screw extruder for melt extrusion granulation to obtain starch-based degradable straw material particles E;
and adding the degradable particles E into a single-screw straw, extruding and pulling the straw to obtain the starch-based degradable straw.
As a further scheme of the invention: the temperature of the granulation and tube drawing is 160-205 ℃.
As a further scheme of the invention: the conditions for granulating and extruding the drawn tube comprise: the temperature of the first zone is 170 +/-5 ℃, the temperature of the second zone is 180 +/-5 ℃, the temperature of the third zone is 190 +/-5 ℃, the temperature of the fourth zone is 195 +/-5 ℃ and the temperature of the fifth zone is 200 +/-5 ℃.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a starch-based degradable desorption tube material and a preparation method thereof, wherein sebacic acid dibenzoylhydrazine and cyclodextrin in a nucleating agent are compounded with PLA, the compatibility with PLA is good, and the crystallization rate of PLA is accelerated in a lower addition range, so that the heat resistance is improved; the glycerol triacetate and the tributyl citrate in the plasticizer are blended with the PBAT for use and compounded with the PLA, so that the brittleness of the PLA can be reduced, and the toughness of the PLA can be improved; the invention adopts starch as filling material to be compounded with PLA, thereby greatly reducing the material cost while ensuring the biodegradability; the invention adopts a blending granulation mode, and the nucleating agent is ground into powder for use, thereby being beneficial to improving the dispersity and crystallization efficiency of the nucleating agent in the composite material; the preparation method is characterized in that the sebacic acid dibenzoyl hydrazine, the cyclodextrin, the glycerol triacetate, the PBAT, the erucamide and the PLA are blended and granulated, the process is simple, the operation condition is mild, and the preparation method is suitable for industrial large-scale production.
Detailed Description
Example 1
The preparation method of the starch-based degradable desorption tube material comprises the following steps:
(1) grinding 0.15 part of sebacic acid dibenzoylhydrazine and 0.25 part of cyclodextrin particles in a mortar for 15min to obtain uniformly dispersed nucleating agent powder A;
(2) 0.4 part of powder A, 28.3 parts of 100-mesh corn starch, 0.6 part of erucamide and 0.4 part of hyperbranched auxiliary agent are mixed for 5min at low speed in a cold mixer to obtain uniformly mixed powder B;
(3) adding 64 parts of PLA and 0.35 part of PBAT into high-speed mixing, carrying out high-speed blending for 20min, uniformly adding 7.5 parts of tributyl citrate while stirring in the process of blending the mixture, and carrying out high-speed blending for 10min to obtain a mixture C;
(4) adding the powder B and the mixture C into a high-speed mixer, and mixing at a high speed for 10min to obtain a blend D;
(5) melting, extruding and granulating the blend D to obtain the starch-based degradable granular material E; the melt extrusion conditions include: the temperature of the first zone is 170 ℃, the temperature of the second zone is 180 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 195 ℃ and the temperature of the fifth zone is 200 ℃; the rotating speed of the screw is 200-350 rpm/min;
(6) adding the degradable particles E into a single-screw straw extruder to extrude and draw a pipe to obtain a starch-based degradable straw, wherein the conditions of extruding and drawing the pipe comprise: the temperature in the first zone is 170 ℃, the temperature in the second zone is 180 ℃, the temperature in the third zone is 190 ℃, the temperature in the fourth zone is 195 ℃ and the temperature in the fifth zone is 200 ℃.
Example 2
The preparation method of the starch-based degradable desorption tube material comprises the following steps:
(1) grinding 0.15 part of sebacic acid dibenzoylhydrazine and 0.25 part of cyclodextrin particles in a mortar for 15min to obtain uniformly dispersed nucleating agent powder A;
(2) 0.4 part of powder A, 28.3 parts of 100-mesh corn starch, 0.6 part of erucamide and 0.4 part of hyperbranched auxiliary agent are mixed for 5min at low speed in a cold mixer to obtain uniformly mixed powder B;
(3) adding 64 parts of PLA into the high-speed mixing, carrying out high-speed blending for 5min, uniformly adding 7.85 parts of PBAT while stirring in the process of blending the mixture, and carrying out high-speed blending for 10min to obtain a mixture C;
(4) adding the powder B and the mixture C into a high-speed mixer, and mixing at a high speed for 10min to obtain a blend D;
(5) melting, extruding and granulating the blend D to obtain the starch-based degradable granular material E; the melt extrusion conditions include: the temperature of the first zone is 170 ℃, the temperature of the second zone is 180 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 195 ℃ and the temperature of the fifth zone is 200 ℃; the rotating speed of the screw is 200-350 rpm/min;
(6) adding the degradable particles E into a single-screw straw extruder to extrude and draw a pipe to obtain a starch-based degradable straw, wherein the conditions of extruding and drawing the pipe comprise: the temperature in the first zone is 170 ℃, the temperature in the second zone is 180 ℃, the temperature in the third zone is 190 ℃, the temperature in the fourth zone is 195 ℃ and the temperature in the fifth zone is 200 ℃.
Example 3
The preparation method of the starch-based degradable desorption tube material comprises the following steps:
(1) grinding 0.15 part of sebacic acid dibenzoylhydrazine and 0.25 part of cyclodextrin particles in a mortar for 15min to obtain uniformly dispersed nucleating agent powder A;
(2) 0.4 part of powder A, 28.3 parts of cassava starch with 100 meshes, 0.6 part of erucamide and 0.5 part of hyperbranched auxiliary agent are mixed for 5min at low speed in a cold mixer to obtain uniformly mixed powder B;
(3) adding 64 parts of PLA and 0.35 part of PBAT into high-speed mixing, blending at a high speed for 20min, uniformly adding 7.5 parts of glycerol triacetate while stirring in the process of blending the mixture, and blending at a high speed for 10min to obtain a mixture C;
(4) adding the powder B and the mixture C into a high-speed mixer, and mixing at a high speed for 10min to obtain a blend D;
(5) melting, extruding and granulating the blend D to obtain the starch-based degradable granular material E; the melt extrusion conditions include: the temperature of the first zone is 170 ℃, the temperature of the second zone is 180 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 195 ℃ and the temperature of the fifth zone is 200 ℃; the rotating speed of the screw is 200-350 rpm/min;
(6) adding the degradable particles E into a single-screw straw extruder to extrude and draw a pipe to obtain a starch-based degradable straw, wherein the conditions of extruding and drawing the pipe comprise: the temperature in the first zone is 170 ℃, the temperature in the second zone is 180 ℃, the temperature in the third zone is 190 ℃, the temperature in the fourth zone is 195 ℃ and the temperature in the fifth zone is 200 ℃.
Example 4
The preparation method of the starch-based degradable desorption tube material comprises the following steps:
(1) grinding 0.15 part of sebacic acid dibenzoylhydrazine and 0.25 part of cyclodextrin particles in a mortar for 15min to obtain uniformly dispersed nucleating agent powder A;
(2) 0.4 part of powder A, 28.3 parts of 100-mesh corn starch, 0.6 part of erucamide and 0.5 part of hyperbranched auxiliary agent are mixed for 5min at low speed in a cold mixer to obtain uniformly mixed powder B;
(3) adding 64 parts of PLA into high-speed mixing, carrying out high-speed blending for 5min, uniformly adding 5.35 parts of PBAT and 2 parts of glycerol triacetate while stirring in the process of blending the mixture, and carrying out high-speed blending for 10min to obtain a mixture C;
(4) adding the powder B and the mixture C into a high-speed mixer, and mixing at a high speed for 10min to obtain a blend D;
(5) melting, extruding and granulating the blend D to obtain the starch-based degradable granular material E; the melt extrusion conditions include: the temperature of the first zone is 170 ℃, the temperature of the second zone is 180 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 195 ℃ and the temperature of the fifth zone is 200 ℃; the rotating speed of the screw is 200-350 rpm/min;
(6) adding the degradable particles E into a single-screw straw extruder to extrude and draw a pipe to obtain a starch-based degradable straw, wherein the conditions of extruding and drawing the pipe comprise: the temperature in the first zone is 170 ℃, the temperature in the second zone is 180 ℃, the temperature in the third zone is 190 ℃, the temperature in the fourth zone is 195 ℃ and the temperature in the fifth zone is 200 ℃.
Example 5
The preparation method of the starch-based degradable desorption tube material comprises the following steps:
(1) grinding 0.15 part of sebacic acid dibenzoylhydrazine and 0.25 part of cyclodextrin particles in a mortar for 15min to obtain uniformly dispersed nucleating agent powder A;
(2) 0.4 part of powder A, 28.3 parts of 100-mesh corn starch, 0.6 part of erucamide and 0.5 part of hyperbranched auxiliary agent are mixed for 5min at low speed in a cold mixer to obtain uniformly mixed powder B;
(3) adding 64 parts of PLA into high-speed mixing, carrying out high-speed blending for 5min, uniformly adding 4.35 parts of PBAT and 3 parts of glycerol triacetate while stirring in the process of blending the mixture, and carrying out high-speed blending for 10min to obtain a mixture C;
(4) adding the powder B and the mixture C into a high-speed mixer, and mixing at a high speed for 10min to obtain a blend D;
(5) melt-extruding and granulating the blend D to obtain the starch-based degradable granular material E; the melt extrusion conditions include: the temperature of the first zone is 170 ℃, the temperature of the second zone is 180 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 195 ℃ and the temperature of the fifth zone is 200 ℃; the rotating speed of the screw is 200-350 rpm/min;
(6) adding the degradable particles E into a single-screw straw extruder to extrude and draw a pipe to obtain a starch-based degradable straw, wherein the conditions of extruding and drawing the pipe comprise: the temperature in the first zone is 170 ℃, the temperature in the second zone is 180 ℃, the temperature in the third zone is 190 ℃, the temperature in the fourth zone is 195 ℃ and the temperature in the fifth zone is 200 ℃.
Comparative example 1
The preparation method of the starch-based degradable desorption tube material comprises the following steps:
(1) mixing 0.15 part of sebacic acid dibenzoylhydrazine and 0.25 part of cyclodextrin particles for 5min to obtain uniformly dispersed nucleating agent powder A;
(2) 0.4 part of powder A, 28.3 parts of 100-mesh corn starch, 0.6 part of erucamide and 0.5 part of hyperbranched auxiliary agent are mixed for 5min at low speed in a cold mixer to obtain uniformly mixed powder B;
(3) adding 64 parts of PLA and 0.35 part of PBAT into high-speed mixing, carrying out high-speed blending for 20min, uniformly adding 4 parts of PBAT and 3 parts of glycerol triacetate while stirring in the process of blending the mixture, and carrying out high-speed blending for 10min to obtain a mixture C;
(4) adding the powder B and the mixture C into a high-speed mixer, and mixing at a high speed for 10min to obtain a blend D;
(5) melt-extruding and granulating the blend D to obtain the starch-based degradable granular material E; the melt extrusion conditions include: the temperature of the first zone is 170 ℃, the temperature of the second zone is 180 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 195 ℃ and the temperature of the fifth zone is 200 ℃; the rotating speed of the screw is 200-350 rpm/min;
(6) adding the degradable particles E into a single-screw straw extruder to extrude and draw a pipe to obtain a starch-based degradable straw, wherein the conditions of extruding and drawing the pipe comprise: the temperature in the first zone is 170 ℃, the temperature in the second zone is 180 ℃, the temperature in the third zone is 190 ℃, the temperature in the fourth zone is 195 ℃ and the temperature in the fifth zone is 200 ℃.
Comparative example 2
The preparation method of the starch-based degradable desorption tube material comprises the following steps:
(1) grinding 0.15 part of sebacic acid dibenzoylhydrazine and 0.25 part of cyclodextrin particles in a mortar for 15min to obtain uniformly dispersed nucleating agent powder A;
(2) 0.4 part of powder A, 28.3 parts of cassava starch with 100 meshes, 0.6 part of erucamide and 0.5 part of hyperbranched resin are mixed for 5min at low speed in a cold mixer to obtain uniformly mixed powder B;
(3) adding 71 parts of PLA and 0.35 part of PBAT into high-speed mixing, and carrying out high-speed mixing for 20min to obtain a mixture C;
(4) adding the powder B and the mixture C into a high-speed mixer, and mixing at a high speed for 10min to obtain a blend D;
(5) melting, extruding and granulating the blend D to obtain the starch-based degradable granular material E; the melt extrusion conditions include: the temperature of the first zone is 170 ℃, the temperature of the second zone is 180 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 195 ℃ and the temperature of the fifth zone is 200 ℃; the rotating speed of the screw is 200-350 rpm/min;
(6) adding the degradable particles E into a single-screw straw extruder to extrude and draw a pipe to obtain a starch-based degradable straw, wherein the conditions of extruding and drawing the pipe comprise: the temperature in the first zone is 170 ℃, the temperature in the second zone is 180 ℃, the temperature in the third zone is 190 ℃, the temperature in the fourth zone is 195 ℃ and the temperature in the fifth zone is 200 ℃.
Comparative example 3
The preparation method of the starch-based degradable desorption tube material comprises the following steps:
(1) grinding 0.4 part of sebacic acid dibenzoylhydrazine for 15min to obtain uniformly dispersed nucleating agent powder A;
(2) 0.4 part of powder A, 28.3 parts of 100-mesh corn starch, 0.6 part of erucamide and 0.5 part of hyperbranched auxiliary agent are mixed for 5min at low speed in a cold mixer to obtain uniformly mixed powder B;
(3) adding 64 parts of PLA and 0.35 part of PBAT homopolymer into high-speed mixing, carrying out high-speed mixing for 20min, uniformly adding 4 parts of PBAT and 3 parts of glycerol triacetate while stirring in the process of mixing the mixture, and carrying out high-speed mixing for 10min to obtain a mixture C;
(4) adding the powder B and the mixture C into a high-speed mixer, and mixing at a high speed for 10min to obtain a blend D;
(5) melt-extruding and granulating the blend D to obtain the starch-based degradable granular material E; the melt extrusion conditions include: the temperature of the first zone is 170 ℃, the temperature of the second zone is 180 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 195 ℃ and the temperature of the fifth zone is 200 ℃; the rotating speed of the screw is 200-350 rpm/min;
(6) adding the degradable particles E into a single-screw straw extruder to extrude and draw a pipe to obtain a starch-based degradable straw, wherein the conditions of extruding and drawing the pipe comprise: the temperature in the first zone is 170 ℃, the temperature in the second zone is 180 ℃, the temperature in the third zone is 190 ℃, the temperature in the fourth zone is 195 ℃ and the temperature in the fifth zone is 200 ℃.
Comparative example 4
The preparation method of the starch-based degradable desorption tube material comprises the following steps:
(1) grinding 0.4 part of cyclodextrin for 15min to obtain uniformly dispersed nucleating agent powder A;
(2) blending 0.4 part of powder A, 28.3 parts of 100-mesh corn starch, 0.6 part of erucamide and 0.5 part of hyperbranched resin in a cold mixer at low speed for 5min to obtain uniformly blended powder B;
(3) adding 64 parts of PLA and 0.35 part of PBAT into high-speed mixing, carrying out high-speed blending for 20min, uniformly adding 4 parts of PBAT and 3 parts of glycerol triacetate while stirring in the process of blending the mixture, and carrying out high-speed blending for 10min to obtain a mixture C;
(4) adding the powder B and the mixture C into a high-speed mixer, and mixing at a high speed for 10min to obtain a blend D;
(5) melt-extruding and granulating the blend D to obtain the starch-based degradable granular material E; the melt extrusion conditions include: the temperature of the first zone is 170 ℃, the temperature of the second zone is 180 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 195 ℃ and the temperature of the fifth zone is 200 ℃; the rotating speed of the screw is 200-350 rpm/min;
(6) adding the degradable particles E into a single-screw straw extruder to extrude and draw a pipe to obtain a starch-based degradable straw, wherein the conditions of extruding and drawing the pipe comprise: the temperature in the first zone is 170 ℃, the temperature in the second zone is 180 ℃, the temperature in the third zone is 190 ℃, the temperature in the fourth zone is 195 ℃ and the temperature in the fifth zone is 200 ℃.
Comparative example 5
The preparation method of the starch-based degradable desorption tube material comprises the following steps:
(1) grinding 0.15 part of sebacic acid dibenzoylhydrazine and 0.25 part of cyclodextrin particles in a mortar for 15min to obtain uniformly dispersed nucleating agent powder A;
(2) blending 0.4 part of powder A, 28.7 parts of 100-mesh corn starch and 0.6 part of erucamide in a cold mixer at low speed for 5min to obtain uniformly blended powder B;
(3) adding 64 parts of PLA and 0.35 part of PBAT into high-speed mixing, carrying out high-speed blending for 20min, uniformly adding 4 parts of PBAT and 3 parts of glycerol triacetate while stirring in the process of blending the mixture, and carrying out high-speed blending for 10min to obtain a mixture C;
(4) adding the powder B and the mixture C into a high-speed mixer, and mixing at a high speed for 10min to obtain a blend D;
(5) melt-extruding and granulating the blend D to obtain the starch-based degradable granular material E; the melt extrusion conditions include: the temperature of the first zone is 170 ℃, the temperature of the second zone is 180 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 195 ℃ and the temperature of the fifth zone is 200 ℃; the rotating speed of the screw is 200-350 rpm/min;
(6) adding the degradable particles E into a single-screw straw extruder to extrude and draw a pipe to obtain a starch-based degradable straw, wherein the conditions of extruding and drawing the pipe comprise: the temperature in the first zone is 170 ℃, the temperature in the second zone is 180 ℃, the temperature in the third zone is 190 ℃, the temperature in the fourth zone is 195 ℃ and the temperature in the fifth zone is 200 ℃.
Performance detection
The starch-based degradable desorption tube materials prepared in examples 1-5 and comparative examples 1-5 are subjected to performance detection; tensile properties were measured in accordance with GB/T1040-1992 standards, flexural properties were measured in accordance with GB/T9341-2000 standards, impact properties were measured in accordance with GB/T1043-1992 standards, melt index was measured in accordance with GB/T3682-2000 standards, Vicat softening temperature was measured in accordance with GB/T19466.2-2004 standards, and relative biodegradability was measured in accordance with ASTM D6400/EN13432 standards, with the results shown in Table 1.
TABLE 1
| Item | Tensile strength | Modulus of elasticity | Elongation at break | Impact strength | Melt index | Vicat softening temperature | Relative rate of biological decomposition |
| Example 1 | 46.82MPa | 3039MPa | 2.28％ | 2.69KJ/m2 | 5.9g/10min | 88.3℃ | ＞90％ |
| Example 2 | 46.93MPa | 3346MPa | 3.27％ | 3.34KJ/m2 | 5.7g/10min | 90.1℃ | ＞90％ |
| Example 3 | 48.68MPa | 3363MPa | 2.81％ | 2.88KJ/m2 | 6.4g/10min | 89.9℃ | ＞90％ |
| Example 4 | 55MPa | 3200MPa | 5％ | 7.5KJ/m2 | 4.7g/10min | 92℃ | ＞90％ |
| Example 5 | 54.21MPa | 3269MPa | 4.92％ | 7.58KJ/m2 | 5.6g/10min | 90.6℃ | ＞90％ |
| Comparative example 1 | 60.13MPa | 2777MPa | 2.98％ | 3.35KJ/m2 | 4.2g/10min | 87.8℃ | ＞90％ |
| Comparative example 2 | 46.57MPa | 3378MPa | 2.14％ | 2.32KJ/m2 | 3.7g/10min | 88℃ | ＞90％ |
| Comparative example 3 | 54MPa | 3199MPa | 4.8％ | 6.7KJ/m2 | 4.6g/10min | 85℃ | ＞90％ |
| Comparative example 4 | 53.9MPa | 3200MPa | 4.6％ | 6.5KJ/m2 | 3.5g/10min | 86℃ | ＞90％ |
| Comparative example 5 | 55MPa | 3200MPa | 5％ | 7.5KJ/m2 | 3.8g/10min | 92℃ | ＞90％ |
In summary, the following steps: through compounding sebacic acid dibenzoyl hydrazine, cyclodextrin and PLA, the PLA composite material has good compatibility with PLA, and the crystallization rate of the PLA is accelerated in a range of lower addition amount, so that the heat resistance is improved; the glycerol triacetate, the tributyl citrate and the PBAT are blended and compounded with the polylactic acid, so that the brittleness of the PLA can be reduced, and the toughness of the PLA can be improved; starch is adopted as filling for compounding with PLA, so that the material cost is greatly reduced while the biodegradability is ensured; the method has simple process and mild operation condition, and is suitable for industrial large-scale production.
Claims (10)
1. The starch-based degradable desorption tube material is characterized by comprising the following components in parts by weight:
60-80 parts of PLA, 3-7 parts of PBAT, 5-30 parts of starch, 3-10 parts of plasticizer, 0.5-1 part of nucleating agent, 0.5-1 part of erucamide and 0.5-2 parts of hyperbranched assistant;
wherein the optical purity of the PLA is 95-100%, and the melt index (190 ℃, 2.16kg) of the PLA is 2-8g/10 min.
2. The starch-based degradable desorption tube material as claimed in claim 1, which comprises the following components in parts by weight:
65-70 parts of PLA, 3-7 parts of PBAT, 5-30 parts of starch, 3-10 parts of plasticizer, 0.5-1 part of nucleating agent, 0.5-1 part of erucamide and 0.5-2 parts of hyperbranched assistant;
wherein the optical purity of the PLA is more than or equal to 99.9 percent, and the melt index (190 ℃, 2.16kg) of the PLA is 3-7g/10 min.
3. The starch-based degradable straw material of claim 1, wherein the PBAT has a melt index of 3-6g/10min (190 ℃, 2.16 kg).
4. The starch-based degradable desorption tube material as claimed in claim 1, wherein the starch is one or a blend of corn starch and cassava starch, the starch mesh number is larger than or equal to 100 meshes, and the whiteness is larger than or equal to 90%.
5. The starch-based degradable release tube material of claim 1, wherein the plasticizer is one or a blend of glycerol triacetate and tributyl citrate.
6. The starch-based degradable desorption tube material of claim 1, wherein the nucleating agent is one or a mixture of potassium benzene sulfonate, zinc phenyl phosphate, dibenzoylhydrazide sebacate, organic phosphate and cyclodextrin.
7. The starch-based degradable desorption tube material as claimed in claim 1, wherein the nucleating agent is a blend of dibenzoylhydrazide sebacate and cyclodextrin, the erucamide is selected from one of PMC model of ArmoslipE, Poa prata (Croda), Korean Pathwel, and the hyperbranched assistant is solid powder with melting range of 145-155 ℃.
8. A method for preparing a starch-based degradable desorption tube material according to any one of claims 1-7, which comprises the following steps:
grinding the nucleating agent particles in a mortar to obtain uniformly dispersed nucleating agent powder A;
mixing the powder A, the starch, the erucamide and the hyperbranched auxiliary agent in a cold mixer to obtain uniformly mixed powder B;
adding PLA and PBAT into a high-speed mixer, blending for 20min, uniformly adding a plasticizer while stirring in the process of blending the mixture, and blending for 10min to obtain a mixture C;
adding the powder B and the powder C into a high-speed mixer, and mixing for 10min to obtain a blend D;
adding the blend D into a double-screw extruder for melt extrusion granulation to obtain starch-based degradable straw material particles E;
and adding the degradable particles E into a single-screw straw, extruding and pulling the straw to obtain the starch-based degradable straw.
9. The method as claimed in claim 8, wherein the temperature of the granulating and tube-drawing is 160-205 ℃.
10. The method for preparing a starch-based degradable straw material according to claim 9, wherein the conditions for granulating and extruding the straw comprise: the temperature of the first zone is 170 +/-5 ℃, the temperature of the second zone is 180 +/-5 ℃, the temperature of the third zone is 190 +/-5 ℃, the temperature of the fourth zone is 195 +/-5 ℃ and the temperature of the fifth zone is 200 +/-5 ℃.
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