CN108410145B - Method for preparing straw fiber/PBAT composite material based on radiation modification - Google Patents
Method for preparing straw fiber/PBAT composite material based on radiation modification Download PDFInfo
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- 239000010902 straw Substances 0.000 title claims abstract description 101
- 239000000835 fiber Substances 0.000 title claims abstract description 97
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 238000012986 modification Methods 0.000 title claims abstract description 20
- 230000004048 modification Effects 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 13
- 230000005855 radiation Effects 0.000 title claims abstract description 11
- 229920001896 polybutyrate Polymers 0.000 title claims abstract 15
- 238000011282 treatment Methods 0.000 claims abstract description 21
- 239000007822 coupling agent Substances 0.000 claims abstract description 13
- 238000001746 injection moulding Methods 0.000 claims description 23
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- 238000001291 vacuum drying Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 13
- 238000001125 extrusion Methods 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- 239000008187 granular material Substances 0.000 claims description 10
- 238000005469 granulation Methods 0.000 claims description 10
- 230000003179 granulation Effects 0.000 claims description 10
- 239000003963 antioxidant agent Substances 0.000 claims description 7
- 230000003078 antioxidant effect Effects 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- 238000005507 spraying Methods 0.000 claims description 7
- 239000004698 Polyethylene Substances 0.000 claims description 6
- -1 polyethylene Polymers 0.000 claims description 6
- 229920000573 polyethylene Polymers 0.000 claims description 6
- 238000009461 vacuum packaging Methods 0.000 claims description 6
- 239000000314 lubricant Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 240000007594 Oryza sativa Species 0.000 claims description 3
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 241000209140 Triticum Species 0.000 claims description 3
- 235000021307 Triticum Nutrition 0.000 claims description 3
- 240000008042 Zea mays Species 0.000 claims description 3
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 3
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 3
- 235000005822 corn Nutrition 0.000 claims description 3
- 238000010894 electron beam technology Methods 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 150000004645 aluminates Chemical class 0.000 claims description 2
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 2
- 239000008116 calcium stearate Substances 0.000 claims description 2
- 235000013539 calcium stearate Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 5
- 239000011347 resin Substances 0.000 abstract description 4
- 229920005989 resin Polymers 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 description 8
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- 229920000704 biodegradable plastic Polymers 0.000 description 3
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- 238000002156 mixing Methods 0.000 description 3
- AXKZIDYFAMKWSA-UHFFFAOYSA-N 1,6-dioxacyclododecane-7,12-dione Chemical compound O=C1CCCCC(=O)OCCCCO1 AXKZIDYFAMKWSA-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
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- 238000011160 research Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- WSQZNZLOZXSBHA-UHFFFAOYSA-N 3,8-dioxabicyclo[8.2.2]tetradeca-1(12),10,13-triene-2,9-dione Chemical compound O=C1OCCCCOC(=O)C2=CC=C1C=C2 WSQZNZLOZXSBHA-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 239000011174 green composite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- 238000005297 material degradation process Methods 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 238000005025 nuclear technology Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
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- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/001—Treatment with visible light, infrared or ultraviolet, X-rays
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/008—Treatment with radioactive elements or with neutrons, alpha, beta or gamma rays
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
Abstract
The invention discloses a method for preparing a straw fiber/PBAT composite material based on radiation modification, wherein the straw fiber is sprayed with a coupling agent and then subjected to radiation modification treatment; the straw fiber after radiation modification treatment reduces the smoothness of the surface of the fiber straw and improves the surface activity of the straw fiber, and when the straw fiber is added into PBAT resin, the interface compatibility of the straw fiber and the PBAT can be effectively improved.
Description
Technical Field
The invention belongs to the field of biological material degradation, relates to a straw fiber/PBAT composite material, in particular to a straw fiber/PBAT composite material prepared after the surface of straw fiber is improved by radiation and a preparation process thereof, and also belongs to the field of nuclear technology application.
Background
With the development of society and the continuous progress of scientific technology, more and more petroleum-based plastic materials are consumed in the fields of industry, agriculture, buildings and the like, the problem of global environmental pollution caused by the preparation and consumption of the materials is increasingly serious, and the environment protection bureau rapidly develops green environment-friendly materials as one of the main research directions in the 21 st century at present. According to related statistical data of the european bioplastic association in 2014, the yield of the global biodegradable plastics reaches 670 ten thousand tons by 2018, which is 3 times more than 2013. Therefore, research and development of renewable, low-carbon and environment-friendly biodegradable plastics have become the main development trend of the polymer material industry.
The poly (butylene adipate/terephthalate) (PBAT) is a copolymer of butylene adipate and butylene terephthalate, not only has flexibility of a long methylene chain and toughness of an aromatic ring, but also has better ductility and elongation at break, better heat resistance, impact performance and the like, and is a biodegradable material. In addition, PBAT and LDPE have similar mechanical properties and are expected to be widely used for environment-friendly mulching film films and the like. Although the PBAT has good elongation at break which can reach 650% at room temperature, the tensile strength of the PBAT is poor and is less than 17MPa, and the development and the wide application of the PBAT are seriously restricted. In addition, the production cost of PBAT is high, and a certain influence is also generated on the wide application of PBAT.
The crops in the middle and north areas of China are mainly wheat and corn, and the crops in the south area are mainly used for planting rice and the like, so that the straw resources are rich. At present, the straws of the crops are mainly treated by the traditional modes of direct returning to the field, processing coarse fodder and the like, and the straws are discarded in disorder, subjected to uncontrolled incineration and the like in local areas, so that resources are wasted, and the environment is polluted. On the whole, the straw material in China has the defects of low utilization rate, low conversion rate, low economic benefit and serious environmental pollution. The plant straws contain rich straw fibers, and the straw fibers have excellent mechanical properties, particularly higher tensile strength. The treated straw fiber is used as a reinforcing material to prepare the biodegradable straw fiber/PBAT composite material, which not only combines the advantages of PBAT and straw fiber, but also has very important significance for solving the problem of resource waste and protecting the environment. But the straw fiber has smooth surface and high inertia and poor bonding strength of the resin matrix, so that the mechanical property of the straw fiber reinforced PBAT composite material is not obvious. Therefore, how to improve the surface activity of the straw fiber and improve the compatibility of the straw fiber and PBAT is one of the key problems to be solved for preparing the straw fiber/PBAT composite material with excellent performance.
In order to improve the interfacial compatibility between different polar components in the composite material, a lot of research work is done by domestic and foreign scholars. The currently common straw modification treatment methods include a physical method and a chemical method. The physical method mainly comprises heat treatment, microwave, corona discharge, steam explosion, stretching, rolling, etc. The chemical method mainly comprises alkali treatment, acid treatment, oxidation treatment, grafting modification, infiltration treatment and the like. The physical modification is mainly used for the pretreatment of raw materials, and the effect is not obvious; the chemical modification has the problems of serious environmental pollution, high energy consumption, low efficiency and the like. The high-energy physical method is a green and environment-friendly technology and is increasingly paid more attention by people. The high-energy physical method mainly refers to plasma treatment, ultrasonic treatment, gamma ray treatment and the like, wherein proper surface treatment by utilizing gamma rays can realize improvement of the polarity of the surface of the straw fiber, improvement of the compatibility with PBAT and expansion of the application range of the straw fiber/PBAT composite material.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a green composite material which is prepared by improving the surface activity of straw fibers after radiation modification treatment and increasing the bonding strength with PBAT resin, and adding a coupling agent to improve the compatibility of the straw fibers and PBAT, and has excellent performance and environmental friendliness, so as to meet the requirements of sustainable development of human society.
Another object of the present invention is to provide a method for preparing the composite material. According to the method, the straw fibers are uniformly dispersed in the PBS matrix through melt blending of the double-screw extruder, and the structure of the straw fibers is improved through an efficient, environment-friendly and simple and feasible method of radiation modification treatment, so that the interface compatibility of the straw fibers and the PBS is improved.
The invention is realized by the following technical scheme:
a straw fiber reinforced PBAT composite material is characterized by comprising the following components in parts by weight:
wherein the content of the first and second substances,
the straw fiber is modified by irradiation, and the fineness of the straw powder is 80-100 meshes.
Preferably, the straw fiber is modified by irradiation according to the following process: firstly, drying the straw fiber in a vacuum drying oven at 80 ℃ for 12 hours; and secondly, dissolving the coupling agent in an acetone solution, uniformly spraying the acetone solution on the dried straw fibers, airing and drying at room temperature, carrying out vacuum packaging by using a polyethylene bag, and carrying out irradiation treatment at room temperature by adopting rays with the dose of 6-15 kGy to obtain the straw fibers subjected to surface irradiation modification treatment.
Preferably, the stalk fiber is wheat stalk, rice stalk or corn stalk.
Preferably, the coupling agent is at least one of silane coupling agent (KH-550), aluminate coupling agent (DL-411) and titanate coupling agent (DN-201).
Preferably, the lubricant is at least one of stearic acid, zinc stearate and calcium stearate.
Preferably, the antioxidant is at least one of 1010, 168, B215 and B225.
According to another aspect of the present invention, the present invention also provides a method for preparing the above straw fiber reinforced PBAT composite material, comprising the steps of:
SS1 feed pretreatment
(1) Carrying out irradiation modification treatment on straw fibers: firstly, drying the straw fiber in a vacuum drying oven at 80 ℃ for 12 hours; secondly, dissolving a coupling agent in an acetone solution, uniformly spraying the acetone solution on the dried straw fibers, airing and drying at room temperature, carrying out vacuum packaging by using a polyethylene bag, and carrying out irradiation treatment at room temperature by adopting rays with the dose of 6-15 kGy to obtain the straw fibers with the modified surfaces;
(2) respectively placing the PBAT and the straw fiber subjected to irradiation modification treatment in a vacuum drying oven to dry for 20-40 h at the temperature of 60-90 ℃;
(3) and stirring the dried PBAT, the straw fiber, the lubricant and the antioxidant in a predetermined ratio in a high-speed mixer at normal temperature for 4-5 min.
SS2. twin-screw extrusion granulation
(1) Putting the mixture prepared in the step SS1 into a double-screw extruder for melt extrusion granulation, wherein the temperature of the first section of the extruder is 115-125 ℃, the temperature of the second section is 118-128 ℃, the temperature of the third section is 119-129 ℃, the temperature of the fourth section is 119-129 ℃, the temperature of the fifth section is 120-130 ℃, the temperature of the sixth section is 120-130 ℃, and the temperature of a machine head is 115-125 ℃; the rotating speed of the screw main machine is 3.0-4.5 Hz, and the rotating speed of the feeding machine is 2.0-3.5 Hz.
SS3. forming of articles
(1) Drying the granules prepared in the step SS2 in a vacuum drying oven at 80-90 ℃ for 20-40 h;
(2) processing the dried granules on an injection molding machine to form injection molded products, wherein the injection molding temperature (5 sections from a feed inlet of the injection molding machine) is as follows: the temperature of the first section is 115-125 ℃, the temperature of the second section is 118-128 ℃, the temperature of the third section is 115-125 ℃, the temperature of the fourth section is 113-123 ℃, and the temperature of the fifth section is 110-120 ℃; the injection molding pressure is as follows: 15-25 MPa; the injection molding speed is as follows: 25-40 Hz; the molding cycle is as follows: 40-60 s.
Preferably, in step SS1, the irradiation radiation may be any one of gamma rays generated by 60Co, electron beams generated by an electron accelerator, or X-rays.
The invention has the advantages that:
(1) the straw fiber is prepared by spraying the coupling agent and then performing irradiation modification treatment, and the radiation modification method has the advantages of simple process, environmental protection, reaction at normal temperature and the like.
(2) The treated straw fiber reduces the smoothness of the surface of the fiber straw and improves the surface activity of the straw fiber, and when the treated straw fiber is added into PBAT resin, the interface compatibility of the straw fiber and the PBAT can be effectively improved.
(3) The straw fiber reinforced PBAT composite material prepared by the invention improves the mechanical property and the like of the composite material and expands the application range of the composite material.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the content of the present invention, but the content of the present invention is not limited to the following examples.
Example 1: preparation of irradiation modified straw fiber
Dissolving 30g of silane coupling agent (KH-550) in 200ml of acetone solvent, uniformly spraying the solution on 1.0kg of straw fibers dried for 10 hours at 80 ℃ in a vacuum drying oven, naturally airing the straw fibers, vacuum-packaging the dried straw fibers by using polyethylene, and irradiating the straw fibers at normal temperature by using gamma rays with the dose of 10kGy to obtain the straw fibers with the modified surfaces.
Example 2: preparation of irradiation modified straw fiber
Dissolving 20g of silane coupling agent (KH-550) in 150ml of acetone solvent, uniformly spraying the solution on 1.0kg of straw fibers dried for 12 hours at 70 ℃ in a vacuum drying oven, naturally airing the straw fibers, vacuum-packaging the dried straw fibers by using polyethylene, and irradiating the straw fibers at normal temperature by using gamma rays with the dosage of 8kGy to obtain the straw fibers with the modified surfaces.
Example 3: preparation of straw fiber/PBAT composite material
(1) Pretreatment of raw materials: drying PBAT and the irradiation modified straw fiber prepared in the embodiment 1 for 20 hours at the temperature of 80 ℃ in a vacuum drying oven; ② mixing PBAT and the irradiation modified straw fiber prepared in the embodiment 1 according to the proportion in the table 1, 25g of stearic acid and 15g of antioxidant in a high-speed mixer at normal temperature for 5 min.
TABLE 1 straw fiber/PBAT composite materials of different compositions
(2) Double screw extrusion granulation
Putting the mixed raw materials into a double-screw extruder for extrusion granulation, wherein the extrusion conditions are that the first-stage temperature is 115 ℃, the second-stage temperature is 120 ℃, the third-stage temperature is 122 ℃, the fourth-stage temperature is 124 ℃, the fifth-stage temperature is 120 ℃, the sixth-stage temperature is 120 ℃ and the head temperature is 115 ℃; the rotating speed of the screw main machine is 4.0Hz, and the rotating speed of the feeding machine is 3.0 Hz.
(3) Sample preparation
Putting the granules into a vacuum drying oven to be dried for 30 hours at the temperature of 80 ℃;
and secondly, performing injection molding on the dried granules in an injection molding machine to obtain a test sample strip of the straw fiber/PBAT composite material with the serial number of 1-5. The injection temperature (5 sections from the feed inlet of the injection molding machine) is as follows: the first-stage temperature is 115 ℃, the second-stage temperature is 118 ℃, the third-stage temperature is 115 ℃, the fourth-stage temperature is 114 ℃, and the fifth-stage temperature is 112 ℃; the injection molding pressure is as follows: 20 MPa; the injection molding speed is as follows: 30 Hz; the molding cycle is as follows: 45 s.
(4) Mechanical Property test
The mechanical properties of test specimens No. 1 to 5 were measured under conditions of relative humidity of 50% and temperature of 25 ℃ in accordance with the regulations in the national standards. The test results are shown in table 2.
TABLE 2 mechanical Properties of straw fiber/PBAT composite
Example 4: preparation of straw fiber/PBAT composite material
(1) Pretreatment of raw materials:
drying PBAT and the irradiation modified straw fiber prepared in the embodiment 1 for 20 hours at the temperature of 80 ℃ in a vacuum drying oven; ② mixing PBAT and the irradiation modified straw fiber prepared in the embodiment 2 according to the proportion in the table 3, 20g stearic acid and 12g antioxidant in a high-speed mixer for 5min at normal temperature.
TABLE 3 straw fiber/PBAT composite materials of different compositions
(2) Double screw extrusion granulation
Putting the mixed raw materials into a double-screw extruder for extrusion granulation, wherein the extrusion conditions are that the first-stage temperature is 120 ℃, the second-stage temperature is 123 ℃, the third-stage temperature is 124 ℃, the fourth-stage temperature is 124 ℃, the fifth-stage temperature is 125 ℃, the sixth-stage temperature is 125 ℃ and the head temperature is 120 ℃; the rotating speed of the screw main machine is 3.0Hz, and the rotating speed of the feeding machine is 2.4 Hz.
(3) Sample preparation
Putting the granules into a vacuum drying oven to be dried for 20 hours at the temperature of 90 ℃;
and secondly, performing injection molding on the dried granules in an injection molding machine to obtain a test sample strip of the straw fiber/PBAT composite material with the serial number of 6-10. The injection temperature (5 sections from the feed inlet of the injection molding machine) is as follows: the first-stage temperature is 120 ℃, the second-stage temperature is 123 ℃, the third-stage temperature is 120 ℃, the fourth-stage temperature is 118 ℃, and the fifth-stage temperature is 116 ℃; the injection molding pressure is as follows: 20 MPa; the injection molding speed is as follows: 38 Hz; the molding cycle is as follows: for 50 s.
(4) Mechanical Property test
The mechanical properties of test specimens No. 6 to 10 were measured under conditions of a relative humidity of 50% and a temperature of 25 ℃ in accordance with the regulations in the national standards. The test results are shown in table 4.
TABLE 4 mechanical Properties of straw fiber/PBAT composite
The above-mentioned embodiments further explain the objects, technical solutions and advantages of the present invention in detail. It should be understood that the above-mentioned embodiments are only exemplary of the present invention, and are not intended to limit the present invention, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A straw fiber reinforced PBAT composite material is characterized by comprising the following components in parts by weight:
wherein the content of the first and second substances,
the straw fibers are modified by irradiation, and the fineness of the straw fibers is 80-100 meshes;
the straw fiber reinforced PBAT composite material is prepared by the following steps:
SS1 feed pretreatment
(1) Irradiation modification of straw fiber:
firstly, drying the straw fiber in a vacuum drying oven at 80 ℃ for 12 hours;
secondly, dissolving the coupling agent in an acetone solution, uniformly spraying the acetone solution on the dried straw fibers, airing and drying the straw fibers at room temperature, and then carrying out vacuum packaging by using a polyethylene bag by adopting rays with the dosage of 6-15 kGyPerforming irradiation treatment at normal temperature by using rays60Any one of gamma rays generated by Co and electron beams or X rays generated by an electron accelerator to obtain the straw fiber subjected to surface irradiation modification treatment;
(2) respectively placing the PBAT and the straw fiber subjected to irradiation modification treatment in a vacuum drying oven to dry for 20-40 h at the temperature of 60-90 ℃;
(3) stirring the dried PBAT, the straw fiber, the lubricant and the antioxidant in a predetermined ratio in a high-speed mixer at normal temperature for 4-5 min;
SS2. twin-screw extrusion granulation
(1) Putting the mixture prepared in the step SS1 into a double-screw extruder for melt extrusion granulation, wherein the temperature of the first section of the extruder is 115-125 ℃, the temperature of the second section is 118-128 ℃, the temperature of the third section is 119-129 ℃, the temperature of the fourth section is 119-129 ℃, the temperature of the fifth section is 120-130 ℃, the temperature of the sixth section is 120-130 ℃, and the temperature of a machine head is 115-125 ℃; the rotating speed of the screw main machine is 3.0-4.5 Hz, and the rotating speed of the feeding machine is 2.0-3.5 Hz;
SS3. forming of articles
(1) Drying the granules prepared in the step SS2 in a vacuum drying oven at 80-90 ℃ for 20-40 h;
(2) processing the dried granules on an injection molding machine to form injection molded products, wherein the injection molding temperature of 5 sections in total from a feed inlet of the injection molding machine is as follows in sequence: the temperature of the first section is 115-125 ℃, the temperature of the second section is 118-128 ℃, the temperature of the third section is 115-125 ℃, the temperature of the fourth section is 113-123 ℃, and the temperature of the fifth section is 110-120 ℃; the injection pressure is 15-25 MPa; the injection molding speed is 25-40 Hz, and the molding cycle is 40-60 s.
2. The stalk fiber reinforced PBAT composite of claim 1 wherein the stalk fibers are wheat, rice or corn stalks.
3. The straw fiber reinforced PBAT composite material according to claim 1, wherein the coupling agent is at least any one of a silane coupling agent (KH-550), an aluminate coupling agent (DL-411) and a titanate coupling agent (DN-201).
4. The straw fiber reinforced PBAT composite of claim 1, wherein the lubricant is at least any one of stearic acid, zinc stearate, calcium stearate.
5. The straw fiber reinforced PBAT composite material of claim 1, wherein the antioxidant is at least any one of 1010, 168, B215, B225.
6. A method of making a straw fibre reinforced PBAT composite material according to any of the preceding claims 1 to 5, comprising the steps of:
SS1 feed pretreatment
(1) Carrying out irradiation modification treatment on straw fibers:
firstly, drying the straw fiber in a vacuum drying oven at 80 ℃ for 12 hours;
secondly, dissolving a coupling agent in an acetone solution, uniformly spraying the acetone solution on the dried straw fibers, airing and drying at room temperature, carrying out vacuum packaging by using a polyethylene bag, and carrying out irradiation treatment at room temperature by adopting rays with the dose of 6-15 kGy to obtain the straw fibers with the modified surfaces;
(2) respectively placing the PBAT and the straw fiber subjected to irradiation modification treatment in a vacuum drying oven to dry for 20-40 h at the temperature of 60-90 ℃;
(3) stirring the dried PBAT, the straw fiber, the lubricant and the antioxidant in a predetermined ratio in a high-speed mixer at normal temperature for 4-5 min;
SS2. twin-screw extrusion granulation
Putting the mixture prepared in the step SS1 into a double-screw extruder for melt extrusion granulation, wherein the temperature of the first section of the extruder is 115-125 ℃, the temperature of the second section is 118-128 ℃, the temperature of the third section is 119-129 ℃, the temperature of the fourth section is 119-129 ℃, the temperature of the fifth section is 120-130 ℃, the temperature of the sixth section is 120-130 ℃, and the temperature of a machine head is 115-125 ℃; the rotating speed of the screw main machine is 3.0-4.5 Hz, and the rotating speed of the feeding machine is 2.0-3.5 Hz;
SS3. forming of articles
(1) Drying the granules prepared in the step SS2 in a vacuum drying oven at 80-90 ℃ for 20-40 h;
(2) processing the dried granules on an injection molding machine to form injection molded products, wherein the injection molding temperature of 5 sections in total from a feed inlet of the injection molding machine is as follows in sequence: the temperature of the first section is 115-125 ℃, the temperature of the second section is 118-128 ℃, the temperature of the third section is 115-125 ℃, the temperature of the fourth section is 113-123 ℃, and the temperature of the fifth section is 110-120 ℃; the injection pressure is 15-25 MPa; the injection molding speed is 25-40 Hz; the molding cycle is 40-60 s.
7. The method of claim 6, wherein in step SS1, the radiation used for irradiation is60Gamma rays generated by Co, electron beams generated by an electron accelerator, or X-rays.
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| CN110218424A (en) * | 2019-06-05 | 2019-09-10 | 辽宁东盛塑业有限公司 | Straw powder/PLA/PBAT biomass full degradable plastics and preparation method |
| CN110128800A (en) * | 2019-06-05 | 2019-08-16 | 辽宁东盛塑业有限公司 | The biomass-based Wholly-degradable material of powdered rice hulls/PBAT and preparation method |
| CN111073326B (en) * | 2019-12-04 | 2022-03-04 | 沈阳化工大学 | Preparation method of rice hull powder/PBAT composite material |
| CN113736220A (en) * | 2020-05-27 | 2021-12-03 | 李小文 | Plant fiber plasticizing material and preparation method thereof |
| CN113461983A (en) * | 2021-06-23 | 2021-10-01 | 沈阳化工大学 | Preparation method of full-degradable seed film added with straw powder |
| CN113462131A (en) * | 2021-06-23 | 2021-10-01 | 沈阳化工大学 | Preparation method of esterified straw powder PBAT full-degradable composite material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101434735A (en) * | 2007-11-13 | 2009-05-20 | 吉林师范大学 | Plant fibre reinforced biodegradable film material and preparation thereof |
| CN101725032A (en) * | 2009-12-22 | 2010-06-09 | 暨南大学 | Microwave modification method of plant fiber and application thereof |
| CN104479385A (en) * | 2014-11-18 | 2015-04-01 | 江苏大学 | Preparation method of reinforced straw fiber composite material |
| CN104987742A (en) * | 2015-07-24 | 2015-10-21 | 苏州荣昌复合材料有限公司 | Straw reinforced composite material and preparation method therefor |
| CN107418169A (en) * | 2017-07-05 | 2017-12-01 | 佛山杰致信息科技有限公司 | Degradable foaming packaging material and preparation method thereof |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101775167B (en) * | 2010-01-18 | 2011-08-10 | 河南省科学院同位素研究所有限责任公司 | Environment protective plastic-wood composite material and preparation method thereof |
| CN102643503B (en) * | 2012-03-19 | 2013-12-25 | 浙江大学 | Method for manufacturing polymerized wood by irradiation grafting |
| CN102627864A (en) * | 2012-03-19 | 2012-08-08 | 浙江大学 | Method for manufacturing polymerized wood by irradiation polymerization |
| CN103265716B (en) * | 2013-06-03 | 2014-08-20 | 河南省科学院同位素研究所有限责任公司 | Straw fiber/PBS(poly butylene succinate)/PBAT (propylene adipate and polybutylene terephthalate) composite and preparation method thereof |
| CN103289334B (en) * | 2013-07-02 | 2015-03-18 | 河南省科学院同位素研究所有限责任公司 | Straw fiber/PBS (Poly Butylene Succinate) composite material based on radiation modification and preparation method thereof |
| CN106751554B (en) * | 2016-11-10 | 2018-10-16 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of sisal hemp reinforced polyester master batch and preparation method thereof |
-
2018
- 2018-03-23 CN CN201810245006.3A patent/CN108410145B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101434735A (en) * | 2007-11-13 | 2009-05-20 | 吉林师范大学 | Plant fibre reinforced biodegradable film material and preparation thereof |
| CN101725032A (en) * | 2009-12-22 | 2010-06-09 | 暨南大学 | Microwave modification method of plant fiber and application thereof |
| CN104479385A (en) * | 2014-11-18 | 2015-04-01 | 江苏大学 | Preparation method of reinforced straw fiber composite material |
| CN104987742A (en) * | 2015-07-24 | 2015-10-21 | 苏州荣昌复合材料有限公司 | Straw reinforced composite material and preparation method therefor |
| CN107418169A (en) * | 2017-07-05 | 2017-12-01 | 佛山杰致信息科技有限公司 | Degradable foaming packaging material and preparation method thereof |
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