CN113912865A - Preparation method of fiber composite material - Google Patents
Preparation method of fiber composite material Download PDFInfo
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- CN113912865A CN113912865A CN202111314120.5A CN202111314120A CN113912865A CN 113912865 A CN113912865 A CN 113912865A CN 202111314120 A CN202111314120 A CN 202111314120A CN 113912865 A CN113912865 A CN 113912865A
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- 239000002131 composite material Substances 0.000 title claims abstract description 89
- 239000000835 fiber Substances 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 108090000790 Enzymes Proteins 0.000 claims abstract description 68
- 102000004190 Enzymes Human genes 0.000 claims abstract description 68
- 239000003513 alkali Substances 0.000 claims abstract description 52
- 239000002994 raw material Substances 0.000 claims abstract description 51
- 239000002023 wood Substances 0.000 claims abstract description 51
- 238000002156 mixing Methods 0.000 claims abstract description 49
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- 239000000243 solution Substances 0.000 claims abstract description 45
- 238000001035 drying Methods 0.000 claims abstract description 40
- 239000000126 substance Substances 0.000 claims abstract description 38
- 238000002791 soaking Methods 0.000 claims abstract description 26
- 238000005303 weighing Methods 0.000 claims abstract description 24
- 239000002585 base Substances 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000010025 steaming Methods 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000001746 injection moulding Methods 0.000 claims abstract description 14
- 238000010790 dilution Methods 0.000 claims abstract description 13
- 239000012895 dilution Substances 0.000 claims abstract description 13
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 8
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 8
- 239000000314 lubricant Substances 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 5
- 238000001125 extrusion Methods 0.000 claims description 110
- 229920002545 silicone oil Polymers 0.000 claims description 23
- QQBLOZGVRHAYGT-UHFFFAOYSA-N tris-decyl phosphite Chemical group CCCCCCCCCCOP(OCCCCCCCCCC)OCCCCCCCCCC QQBLOZGVRHAYGT-UHFFFAOYSA-N 0.000 claims description 23
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 19
- 239000004626 polylactic acid Substances 0.000 claims description 19
- 101710121765 Endo-1,4-beta-xylanase Proteins 0.000 claims description 13
- 108010029182 Pectin lyase Proteins 0.000 claims description 13
- 238000010298 pulverizing process Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 240000000797 Hibiscus cannabinus Species 0.000 claims description 6
- 235000014676 Phragmites communis Nutrition 0.000 claims description 6
- 239000004743 Polypropylene Substances 0.000 claims description 6
- 229920001903 high density polyethylene Polymers 0.000 claims description 6
- 239000004700 high-density polyethylene Substances 0.000 claims description 6
- -1 polypropylene Polymers 0.000 claims description 6
- 229920001155 polypropylene Polymers 0.000 claims description 6
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims 8
- 240000004246 Agave americana Species 0.000 claims 1
- 244000193174 agave Species 0.000 description 20
- 241001391944 Commicarpus scandens Species 0.000 description 8
- 239000012535 impurity Substances 0.000 description 8
- 238000000354 decomposition reaction Methods 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 6
- 241000196324 Embryophyta Species 0.000 description 5
- 229920001277 pectin Polymers 0.000 description 5
- 235000010987 pectin Nutrition 0.000 description 5
- 239000001814 pectin Substances 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000005022 packaging material Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229920006238 degradable plastic Polymers 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H8/00—Macromolecular compounds derived from lignocellulosic materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/18—Homopolymers or copolymers of nitriles
- C08L33/20—Homopolymers or copolymers of acrylonitrile
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
Abstract
The invention provides a preparation method of a fiber composite material, and relates to the field of composite materials. A preparation method of a fiber composite material comprises the following steps: crushing the wood raw material, steaming at 85-100 ℃ for 150min, taking out the steamed raw material, and pretreating the steamed raw material by a mixed enzyme solution to obtain an enzyme treatment product; adding the enzyme treatment product into a sodium hydroxide solution, soaking for 20-28h, rinsing to be neutral, and drying to obtain an alkali treatment product; adding a silane coupling agent into absolute ethyl alcohol for dilution, adding an alkali treatment product, mixing, and drying to obtain a first treatment product; weighing the first treated substance, the base material, the antioxidant and the lubricant in proportion, adding into a double-screw extruder, and carrying out high-temperature mixing at the temperature of 170 ℃ and 220 ℃ and at the speed of 60-80r/min to obtain a blend; and crushing the blend, then performing injection molding, cooling and demolding to obtain the fiber composite material. The invention has the advantages of good biodegradability and difficult fracture.
Description
Technical Field
The invention relates to the technical field of composite materials, and particularly relates to a preparation method of a fiber composite material.
Background
The plant fiber is a renewable natural resource, widely exists in nature, and has the advantages of easy acquisition, recyclability and the like. The plant fiber polypropylene composite material has low cost, good performance and resource saving, and has wide application prospect in automobile parts. The improvement of various properties of the plant fiber composite material is researched for a long time, and the utilization rate of the plant fiber composite material is improved.
The application of plastics in real life is ubiquitous at present, and the harm to the environment caused by the difficulty of degradation of the plastics is obvious. With the increasing public awareness of environmental protection, degradable plastics are beginning to be used to protect the human living environment. In the field of food packaging, most of the packaging materials for medical disposable instruments are common plastic films, and a large amount of fresh-keeping materials are required to be used after packaging, so that great material waste (a large amount of disposable packaging materials are used) and environmental pollution are caused.
The common plastic is prepared from petroleum-based fibers, and the composite material has the defect of difficult degradation, so that the composite material with good biodegradability is urgently needed. In addition, the existing plastic material is brittle and easy to break.
Disclosure of Invention
The invention aims to provide a preparation method of a fiber composite material, and the fiber composite material with the advantages of good biodegradability and difficult fracture is obtained.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The embodiment of the application provides a preparation method of a fiber composite material, which comprises the following steps:
pulverizing the wood raw material, steaming at 85-100 deg.C for 150min,
taking out the steamed wood raw material, and pretreating the wood raw material by using a mixed enzyme solution to obtain an enzyme treatment product;
adding the enzyme treatment product into a sodium hydroxide solution, soaking for 20-28h, rinsing to be neutral, and drying to obtain an alkali treatment product;
adding a silane coupling agent into absolute ethyl alcohol for dilution, adding an alkali treatment product, mixing, and drying to obtain a first treatment product;
weighing the first treated substance, the base material, the antioxidant and the lubricant in proportion, adding into a double-screw extruder, and carrying out high-temperature mixing at the temperature of 170 ℃ and 220 ℃ and at the speed of 60-80r/min to obtain a blend;
and crushing the blend, then performing injection molding, cooling and demolding to obtain the fiber composite material.
Compared with the prior art, the embodiment of the invention has at least the following advantages or beneficial effects:
because the wood raw material is rich in natural fibers, and the composite material prepared by the inventor can utilize the self performance of the natural fibers when being applied to the composite material, the prepared composite material has better mechanical property and is not easy to break; the cross section performance of the wood raw material can be changed by steaming the wood raw material, so that the contact angle of the surface of the wood raw material is reduced, the wettability of the wood raw material is improved, the combination effect of the wood raw material and a base material is good, and the tensile strength and the toughness of the composite material are improved; the wood raw material contains impurities such as pectin and wax besides natural fibers, and the impurities can be dissolved and fiber parts are left by treating the wood raw material through mixed enzyme, so that the purity of the whole wood raw material is improved, and the prepared composite material has good toughness; then, the enzyme treatment product is subjected to alkali treatment, so that the alkali treatment product is not easy to bend, and the prepared composite material is not easy to break; then silane coupling agent is mixed with alkali treatment substance, which can react with hydroxyl on the surface of the fiber and has a group capable of reacting with the matrix, therefore, the connection between the fiber and the matrix can be enhanced, and the combination is firm. Because the wood raw material is selected to prepare the composite material, and the wood raw material has the advantages of low specific price, easy decomposition and wide source, the cost of the composite material can be reduced, and the composite material has the advantages of low price, easy decomposition and environmental protection.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a graph showing tensile property analysis of fiber composites prepared in examples 1 to 3 of the present application;
FIG. 2 is a graph showing tensile properties of fiber composites prepared in examples 2 and 4 to 10 of the present application;
FIG. 3 is a graph showing the bending properties of the fiber composite materials prepared in examples 1 to 3 of the present application;
FIG. 4 is a graph showing the bending properties of the fiber composite materials prepared in examples 2 and 4 to 10 of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to specific examples.
The invention provides a preparation method of a fiber composite material, which comprises the following steps: crushing the wood raw material, steaming at 85-100 ℃ for 150min, taking out the steamed wood raw material, and pretreating the steamed wood raw material by using a mixed enzyme solution to obtain an enzyme treatment product; adding the enzyme treatment product into a sodium hydroxide solution, soaking for 20-28h, rinsing to be neutral, and drying to obtain an alkali treatment product; adding a silane coupling agent into absolute ethyl alcohol for dilution, adding an alkali treatment product, mixing, and drying to obtain a first treatment product; weighing the first treated substance, the base material, the antioxidant and the lubricant in proportion, adding into a double-screw extruder, and carrying out high-temperature mixing at the temperature of 170 ℃ and 220 ℃ and at the speed of 60-80r/min to obtain a blend; and crushing the blend, then performing injection molding, cooling and demolding to obtain the fiber composite material.
Because the wood raw material is rich in natural fibers, and the composite material prepared by the inventor can utilize the self performance of the natural fibers when being applied to the composite material, the prepared composite material has better mechanical property and is not easy to break; the cross section performance of the wood raw material can be changed by steaming the wood raw material, so that the contact angle of the surface of the wood raw material is reduced, the wettability of the wood raw material is improved, the combination effect of the wood raw material and a base material is good, and the tensile strength and the toughness of the composite material are improved; the wood raw material contains impurities such as pectin and wax besides natural fibers, and the impurities can be dissolved and fiber parts are left by treating the wood raw material through mixed enzyme, so that the purity of the whole wood raw material is improved, and the prepared composite material has good toughness; then, the enzyme treatment product is subjected to alkali treatment, so that the alkali treatment product is not easy to bend, and the prepared composite material is not easy to break; then silane coupling agent is mixed with alkali treatment substance, which can react with hydroxyl on the surface of the fiber and has a group capable of reacting with the matrix, therefore, the connection between the fiber and the matrix can be enhanced, and the combination is firm. Because the wood raw material is selected to prepare the composite material, and the wood raw material has the advantages of low specific price, easy decomposition and wide source, the cost of the composite material can be reduced, and the composite material has the advantages of low price, easy decomposition and environmental protection.
In some embodiments of the invention, the wood-based feedstock comprises agave, reed, palm and kenaf, and the crushed wood-based feedstock has a particle size of 40-65 μm. Agave, reed, palm and kenaf are all inexpensive and readily available, and in addition they all contain a large amount of fiber. The crushing of the powder to the particle size of 40-65 μm can make the powder react better and accelerate the preparation speed.
In some embodiments of the present invention, the mixed enzyme comprises (0.1-0.4) by mass: (1.5-1.8) pectin lyase and xylanase, wherein the concentration of the mixed enzyme is 30-40%. The pectin lyase can catalyze the elimination and cracking of pectin molecular chains, accelerate the decomposition of pectin and reduce the impurities of enzyme-treated substances; xylanases are capable of degrading heterogeneous polysaccharides in plant cell walls, thus leaving less impurities of the enzyme-treated material.
In some embodiments of the present invention, the mixed enzyme solution treatment comprises the following steps: mixing the steamed wood raw material with a mixed enzyme solution according to the weight ratio of 1: (2-3), soaking for 5-8h at 45-55 ℃, washing, and drying at 35-45 ℃ to obtain an enzyme treatment product.
In some embodiments of the invention, the sodium hydroxide solution is 5-10% concentrated and the alkaline treated product is dried at 35-45 ℃.
In some embodiments of the present invention, the mass ratio of the above silane coupling agent to the alkali-treated product is (0.3 to 0.8): 1, the mass ratio of the silane coupling agent to the absolute ethyl alcohol is 1: (8-10).
In some embodiments of the present invention, the silane coupling agent is diluted and then added with the alkali treatment product to be mixed at a speed of 900-.
In some embodiments of the present invention, the mass ratio of the first treatment substance, the base material, the antioxidant and the lubricant is (3-7): (93-97): (0.05-0.15): (0.05-0.15). The extrusion is carried out in the proportion, so that the composite material has better mechanical property, is not easy to break and is easy to degrade.
In some embodiments of the present invention, the substrate is one of polylactic acid, high density polyethylene, polyacrylonitrile, and polypropylene; the silane coupling agent is KH550 or KH 560; the lubricant is silicone oil; the antioxidant is tridecyl phosphite. The silicone oil has better lubricating property, and can enable various raw materials to be better mixed together. The tridecyl phosphite can ensure that the prepared fiber composite material is not easy to oxidize and can ensure that the fiber composite material has longer service life.
In some embodiments of the present invention, the first stage extrusion temperature of the twin-screw extruder is 170 ℃, the second stage extrusion temperature is 190 ℃, the third stage extrusion temperature is 190 ℃, the fourth stage extrusion temperature is 210 ℃, and the fifth stage base temperature is 220 ℃. The fiber composite material is extruded in different sections at different temperatures, so that the prepared fiber composite material is uniformly mixed, and the material has stable performance and better toughness.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
A preparation method of a fiber composite material comprises the following steps:
pulverizing folium agaves Variegatae to 40 μm, steaming at 85 deg.C for 130min,
according to the weight ratio of 0.1: 1.5, mixing pectin lyase and xylanase according to the mass ratio of 1: 2, soaking for 5 hours at 45 ℃, washing, and drying at 35 ℃ to obtain an enzyme treatment product;
adding a sodium hydroxide solution with the concentration of 5% into the enzyme treatment product, soaking for 20h, rinsing to be neutral, and drying at 35 ℃ to obtain an alkali treatment product;
according to KH550 with base treatment product 0.3: weighing KH550 and an alkali treatment product according to the mass ratio of 1, adding a silane coupling agent into absolute ethyl alcohol with the mass being 8 times that of the silane coupling agent, diluting, adding the alkali treatment product, mixing for 20min at the speed of 900r/min, and drying at 70 ℃ for 100min to obtain a first treatment product;
according to the following steps of 3: 93: 0.05: weighing a first treatment substance, polylactic acid, tridecyl phosphite and silicone oil according to a mass ratio of 0.05, adding the first treatment substance, the polylactic acid, the tridecyl phosphite and the silicone oil into a double-screw extruder, and carrying out high-temperature mixing, wherein the extrusion temperature of a first section is 170 ℃, the extrusion speed is 60r/min, the extrusion temperature of a second section is 180 ℃, the extrusion speed is 60r/min, the extrusion temperature of a third section is 190 ℃, the extrusion speed is 60r/min, the extrusion temperature of a fourth section is 190 ℃, the extrusion speed is 60r/min, the extrusion temperature of a fifth section is 200 ℃, and the extrusion speed is 60 r/min;
and crushing the blend, then performing injection molding, cooling and demolding to obtain the fiber composite material.
Example 2
A preparation method of a fiber composite material comprises the following steps:
pulverizing folium agaves Variegatae to 50 μm, steaming at 90 deg.C for 140min,
according to the weight ratio of 0.3: 1.7 mixing pectin lyase and xylanase according to the mass ratio to prepare a mixed enzyme solution with the concentration of 35%, mixing the steamed agave with the mixed enzyme solution according to the ratio of 1: 2.5, soaking at 50 ℃ for 7 hours, washing, and drying at 40 ℃ to obtain an enzyme treatment product;
adding 8% sodium hydroxide solution into the enzyme treated product, soaking for 24h, rinsing to neutrality, and drying at 40 deg.C to obtain alkali treated product;
according to KH550 with base treatment product 0.6: weighing KH550 and an alkali treatment product according to the mass ratio of 1, adding the KH550 into 9 times of anhydrous ethanol by mass for dilution, adding the alkali treatment product, mixing at the speed of 1100r/min for 23min, and drying at 75 ℃ for 120min to obtain a first treatment substance;
according to the following steps: 95: 0.1: weighing a first treatment substance, polylactic acid, tridecyl phosphite and silicone oil according to a mass ratio of 0.1, adding the first treatment substance, the polylactic acid, the tridecyl phosphite and the silicone oil into a double-screw extruder, and carrying out high-temperature mixing, wherein the extrusion temperature of a first section is 170 ℃, the extrusion speed is 70r/min, the extrusion temperature of a second section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a third section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fourth section is 210 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fifth section is 220 ℃, and the extrusion speed is 70 r/min;
and crushing the blend, then performing injection molding, cooling and demolding to obtain the fiber composite material.
Example 3
A preparation method of a fiber composite material comprises the following steps:
pulverizing folium agaves Variegatae to 65 μm, steaming at 100 deg.C for 150min,
according to the weight ratio of 0.4: 1.8 mixing pectin lyase and xylanase according to the mass ratio to prepare a mixed enzyme solution with the concentration of 30-40%, mixing the steamed agave with the mixed enzyme solution according to the ratio of 1: 3, soaking at 55 ℃ for 8 hours, washing, and drying at 45 ℃ to obtain an enzyme treatment product;
adding 10% sodium hydroxide solution into the enzyme treated product, soaking for 28h, rinsing to neutrality, and drying at 45 deg.C to obtain alkali treated product;
according to KH550 with base treatment product 0.8: weighing KH550 and an alkali treatment product according to the mass ratio of 1, adding the KH550 into 10 mass times of absolute ethanol for dilution, adding the alkali treatment product, mixing at the speed of 1200r/min for 25min, and drying at 80 ℃ for 140min to obtain a first treatment product;
according to the following steps: 97: 0.15: weighing a first treatment substance, polylactic acid, tridecyl phosphite and silicone oil according to a mass ratio of 0.15, adding the first treatment substance, the polylactic acid, the tridecyl phosphite and the silicone oil into a double-screw extruder, and carrying out high-temperature mixing, wherein the extrusion temperature of a first section is 180 ℃, the extrusion speed is 80r/min, the extrusion temperature of a second section is 190 ℃, the extrusion speed is 80r/min, the extrusion temperature of a third section is 200 ℃, the extrusion speed is 80r/min, the extrusion temperature of a fourth section is 210 ℃, the extrusion speed is 80r/min, the extrusion temperature of a fifth section is 220 ℃, and the extrusion speed is 80 r/min;
and crushing the blend, then performing injection molding, cooling and demolding to obtain the fiber composite material.
Example 4
This example differs from example 2 in that: the agave was replaced with palm.
A preparation method of a fiber composite material comprises the following steps:
pulverizing palm to 50 μm, steaming at 90 deg.C for 140min,
according to the weight ratio of 0.3: 1.7 mixing pectin lyase and xylanase according to the mass ratio to prepare a mixed enzyme solution with the concentration of 35%, mixing the steamed palm and the mixed enzyme solution according to the ratio of 1: 2.5, soaking at 50 ℃ for 7 hours, washing, and drying at 40 ℃ to obtain an enzyme treatment product;
adding 8% sodium hydroxide solution into the enzyme treated product, soaking for 24h, rinsing to neutrality, and drying at 40 deg.C to obtain alkali treated product;
according to KH550 with base treatment product 0.6: weighing KH550 and an alkali treatment product according to the mass ratio of 1, adding the KH550 into 9 times of anhydrous ethanol by mass for dilution, adding the alkali treatment product, mixing at the speed of 1100r/min for 23min, and drying at 75 ℃ for 120min to obtain a first treatment substance;
according to the following steps: 95: 0.1: weighing a first treatment substance, polylactic acid, tridecyl phosphite and silicone oil according to a mass ratio of 0.1, adding the first treatment substance, the polylactic acid, the tridecyl phosphite and the silicone oil into a double-screw extruder, and carrying out high-temperature mixing, wherein the extrusion temperature of a first section is 170 ℃, the extrusion speed is 70r/min, the extrusion temperature of a second section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a third section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fourth section is 210 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fifth section is 220 ℃, and the extrusion speed is 70 r/min;
and crushing the blend, then performing injection molding, cooling and demolding to obtain the fiber composite material.
Example 5
This example differs from example 2 in that: the agave is replaced by reed.
A preparation method of a fiber composite material comprises the following steps:
pulverizing rhizoma Phragmitis to 50 μm, steaming at 90 deg.C for 140min,
according to the weight ratio of 0.3: 1.7 mixing pectin lyase and xylanase according to the mass ratio to prepare a mixed enzyme solution with the concentration of 35%, mixing the steamed reed and the mixed enzyme solution according to the ratio of 1: 2.5, soaking at 50 ℃ for 7 hours, washing, and drying at 40 ℃ to obtain an enzyme treatment product;
adding 8% sodium hydroxide solution into the enzyme treated product, soaking for 24h, rinsing to neutrality, and drying at 40 deg.C to obtain alkali treated product;
according to KH550 with base treatment product 0.6: weighing KH550 and an alkali treatment product according to the mass ratio of 1, adding the KH550 into 9 times of anhydrous ethanol by mass for dilution, adding the alkali treatment product, mixing at the speed of 1100r/min for 23min, and drying at 75 ℃ for 120min to obtain a first treatment substance;
according to the following steps: 95: 0.1: weighing a first treatment substance, polylactic acid, tridecyl phosphite and silicone oil according to a mass ratio of 0.1, adding the first treatment substance, the polylactic acid, the tridecyl phosphite and the silicone oil into a double-screw extruder, and carrying out high-temperature mixing, wherein the extrusion temperature of a first section is 170 ℃, the extrusion speed is 70r/min, the extrusion temperature of a second section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a third section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fourth section is 210 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fifth section is 220 ℃, and the extrusion speed is 70 r/min;
and crushing the blend, then performing injection molding, cooling and demolding to obtain the fiber composite material.
Example 6
This example differs from example 2 in that: the agave is replaced by kenaf.
A preparation method of a fiber composite material comprises the following steps:
pulverizing kenaf to 50 μm, steaming at 90 deg.C for 140min,
according to the weight ratio of 0.3: 1.7 mixing pectin lyase and xylanase according to the mass ratio to prepare a mixed enzyme solution with the concentration of 35%, mixing the steamed kenaf and the mixed enzyme solution according to the ratio of 1: 2.5, soaking at 50 ℃ for 7 hours, washing, and drying at 40 ℃ to obtain an enzyme treatment product;
adding 8% sodium hydroxide solution into the enzyme treated product, soaking for 24h, rinsing to neutrality, and drying at 40 deg.C to obtain alkali treated product;
according to KH550 with base treatment product 0.6: weighing KH550 and an alkali treatment product according to the mass ratio of 1, adding the KH550 into 9 times of anhydrous ethanol by mass for dilution, adding the alkali treatment product, mixing at the speed of 1100r/min for 23min, and drying at 75 ℃ for 120min to obtain a first treatment substance;
according to the following steps: 95: 0.1: weighing a first treatment substance, polylactic acid, tridecyl phosphite and silicone oil according to a mass ratio of 0.1, adding the first treatment substance, the polylactic acid, the tridecyl phosphite and the silicone oil into a double-screw extruder, and carrying out high-temperature mixing, wherein the extrusion temperature of a first section is 170 ℃, the extrusion speed is 70r/min, the extrusion temperature of a second section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a third section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fourth section is 210 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fifth section is 220 ℃, and the extrusion speed is 70 r/min;
and crushing the blend, then performing injection molding, cooling and demolding to obtain the fiber composite material.
Example 7
This example differs from example 2 in that: KH550 is replaced with KH 560.
A preparation method of a fiber composite material comprises the following steps:
pulverizing folium agaves Variegatae to 50 μm, steaming at 90 deg.C for 140min,
according to the weight ratio of 0.3: 1.7 mixing pectin lyase and xylanase according to the mass ratio to prepare a mixed enzyme solution with the concentration of 35%, mixing the steamed agave with the mixed enzyme solution according to the ratio of 1: 2.5, soaking at 50 ℃ for 7 hours, washing, and drying at 40 ℃ to obtain an enzyme treatment product;
adding 8% sodium hydroxide solution into the enzyme treated product, soaking for 24h, rinsing to neutrality, and drying at 40 deg.C to obtain alkali treated product;
the reaction was carried out according to KH560 with base treatment product 0.6: weighing KH560 and an alkali treatment product according to the mass ratio of 1, adding KH560 into 9 times of absolute ethanol by mass for dilution, adding the alkali treatment product, mixing at the speed of 1100r/min for 23min, and drying at 75 ℃ for 120min to obtain a first treatment substance;
according to the following steps: 95: 0.1: weighing a first treatment substance, polylactic acid, tridecyl phosphite and silicone oil according to a mass ratio of 0.1, adding the first treatment substance, the polylactic acid, the tridecyl phosphite and the silicone oil into a double-screw extruder, and carrying out high-temperature mixing, wherein the extrusion temperature of a first section is 170 ℃, the extrusion speed is 70r/min, the extrusion temperature of a second section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a third section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fourth section is 210 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fifth section is 220 ℃, and the extrusion speed is 70 r/min;
and crushing the blend, then performing injection molding, cooling and demolding to obtain the fiber composite material.
Example 8
This example differs from example 2 in that: polylactic acid is replaced by high density polyethylene.
A preparation method of a fiber composite material comprises the following steps:
pulverizing folium agaves Variegatae to 50 μm, steaming at 90 deg.C for 140min,
according to the weight ratio of 0.3: 1.7 mixing pectin lyase and xylanase according to the mass ratio to prepare a mixed enzyme solution with the concentration of 35%, mixing the steamed agave with the mixed enzyme solution according to the ratio of 1: 2.5, soaking at 50 ℃ for 7 hours, washing, and drying at 40 ℃ to obtain an enzyme treatment product;
adding 8% sodium hydroxide solution into the enzyme treated product, soaking for 24h, rinsing to neutrality, and drying at 40 deg.C to obtain alkali treated product;
according to KH550 with base treatment product 0.6: weighing KH550 and an alkali treatment product according to the mass ratio of 1, adding the KH550 into 9 times of anhydrous ethanol by mass for dilution, adding the alkali treatment product, mixing at the speed of 1100r/min for 23min, and drying at 75 ℃ for 120min to obtain a first treatment substance;
according to the following steps: 95: 0.1: weighing a first treatment substance, high-density polyethylene, tridecyl phosphite and silicone oil according to a mass ratio of 0.1, adding the first treatment substance, the high-density polyethylene, the tridecyl phosphite and the silicone oil into a double-screw extruder, and carrying out high-temperature mixing, wherein the extrusion temperature of a first section is 170 ℃, the extrusion speed is 70r/min, the extrusion temperature of a second section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a third section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fourth section is 210 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fifth section is 220 ℃, and the extrusion speed is 70 r/min;
and crushing the blend, then performing injection molding, cooling and demolding to obtain the fiber composite material.
Example 9
This example differs from example 2 in that: polylactic acid is replaced by polyacrylonitrile.
A preparation method of a fiber composite material comprises the following steps:
pulverizing folium agaves Variegatae to 50 μm, steaming at 90 deg.C for 140min,
according to the weight ratio of 0.3: 1.7 mixing pectin lyase and xylanase according to the mass ratio to prepare a mixed enzyme solution with the concentration of 35%, mixing the steamed agave with the mixed enzyme solution according to the ratio of 1: 2.5, soaking at 50 ℃ for 7 hours, washing, and drying at 40 ℃ to obtain an enzyme treatment product;
adding 8% sodium hydroxide solution into the enzyme treated product, soaking for 24h, rinsing to neutrality, and drying at 40 deg.C to obtain alkali treated product;
according to KH550 with base treatment product 0.6: weighing KH550 and an alkali treatment product according to the mass ratio of 1, adding the KH550 into 9 times of anhydrous ethanol by mass for dilution, adding the alkali treatment product, mixing at the speed of 1100r/min for 23min, and drying at 75 ℃ for 120min to obtain a first treatment substance;
according to the following steps: 95: 0.1: weighing a first treatment substance, polyacrylonitrile, tridecyl phosphite and silicone oil according to a mass ratio of 0.1, adding the first treatment substance, the polyacrylonitrile, the tridecyl phosphite and the silicone oil into a double-screw extruder, and carrying out high-temperature mixing, wherein the extrusion temperature of a first section is 170 ℃, the extrusion speed is 70r/min, the extrusion temperature of a second section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a third section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fourth section is 210 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fifth section is 220 ℃, and the extrusion speed is 70 r/min;
and crushing the blend, then performing injection molding, cooling and demolding to obtain the fiber composite material.
Example 10
This example differs from example 2 in that: polylactic acid is replaced by polypropylene.
A preparation method of a fiber composite material comprises the following steps:
pulverizing folium agaves Variegatae to 50 μm, steaming at 90 deg.C for 140min,
according to the weight ratio of 0.3: 1.7 mixing pectin lyase and xylanase according to the mass ratio to prepare a mixed enzyme solution with the concentration of 35%, mixing the steamed agave with the mixed enzyme solution according to the ratio of 1: 2.5, soaking at 50 ℃ for 7 hours, washing, and drying at 40 ℃ to obtain an enzyme treatment product;
adding 8% sodium hydroxide solution into the enzyme treated product, soaking for 24h, rinsing to neutrality, and drying at 40 deg.C to obtain alkali treated product;
according to KH550 with base treatment product 0.6: weighing KH550 and an alkali treatment product according to the mass ratio of 1, adding the KH550 into 9 times of anhydrous ethanol by mass for dilution, adding the alkali treatment product, mixing at the speed of 1100r/min for 23min, and drying at 75 ℃ for 120min to obtain a first treatment substance;
according to the following steps: 95: 0.1: weighing a first treatment substance, polypropylene, tridecyl phosphite and silicone oil according to a mass ratio of 0.1, adding the first treatment substance, the polypropylene, the tridecyl phosphite and the silicone oil into a double-screw extruder, and carrying out high-temperature mixing, wherein the extrusion temperature of a first section is 170 ℃, the extrusion speed is 70r/min, the extrusion temperature of a second section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a third section is 190 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fourth section is 210 ℃, the extrusion speed is 70r/min, the extrusion temperature of a fifth section is 220 ℃, and the extrusion speed is 70 r/min;
and crushing the blend, then performing injection molding, cooling and demolding to obtain the fiber composite material.
Examples of the experiments
Firstly, the tensile property of the fiber composite materials prepared in examples 1 to 10 is measured according to the determination of plastic tensile property GB/T1040.1 to 2018, an instrument is an XWW-20A electronic universal tester, and the loading speed is 2 mm/min. For the experiments, 5 samples were taken from each example and the average was taken. The results are shown in FIGS. 1 and 2.
From fig. 1, it can be seen that the tensile strength is best in example 2 between examples 1-3, 64.51MPa, which indicates that the tensile strength of the fiber composite obtained is best under this condition.
From fig. 2, it can be seen that the tensile strength is the best in example 8 between examples 2 and 4-10, 65.58MPa, which indicates that the tensile strength of the obtained fiber composite is the best under this condition. Among the various wood raw materials, the most suitable raw material of agave is agave; the high-density polyethylene is selected as the base material, so that the combination effect with the wood raw material is optimal; the silane coupling agent is preferably selected from KH 550.
Secondly, the bending properties of the fiber composite materials prepared in examples 1-10 were measured according to GB/9341-2008, the apparatus is an XWW-20A electronic universal tester, and the loading speed is 2 mm/min. For the experiments, 5 samples were taken from each example and the average was taken. The results are shown in FIGS. 3 and 4.
From FIG. 3, it can be seen that, among examples 1 to 3, the flexural modulus is preferably 2195MPa in example 2; this indicates that under these conditions, the flexural modulus of the resulting fiber composite is optimal.
From figure 4, it can be seen that the best flexural modulus between examples 2, 4-10 is example 5, which illustrates the best flexural modulus of the fibrous composite material made from reed.
In conclusion, the wood raw material is rich in natural fiber, and the composite material prepared by the invention can utilize the self performance of the natural fiber when being applied to the composite material, so that the prepared composite material has better mechanical property and is not easy to break; the cross section performance of the wood raw material can be changed by steaming the wood raw material, so that the contact angle of the surface of the wood raw material is reduced, the wettability of the wood raw material is improved, the combination effect of the wood raw material and a base material is good, and the tensile strength and the toughness of the composite material are improved; the wood raw material contains impurities such as pectin and wax besides natural fibers, and the impurities can be dissolved and fiber parts are left by treating the wood raw material through mixed enzyme, so that the purity of the whole wood raw material is improved, and the prepared composite material has good toughness; then, the enzyme treatment product is subjected to alkali treatment, so that the alkali treatment product is not easy to bend, and the prepared composite material is not easy to break; then silane coupling agent is mixed with alkali treatment substance, which can react with hydroxyl on the surface of the fiber and has a group capable of reacting with the matrix, therefore, the connection between the fiber and the matrix can be enhanced, and the combination is firm. Because the wood raw material is selected to prepare the composite material, and the wood raw material has the advantages of low specific price, easy decomposition and wide source, the cost of the composite material can be reduced, and the composite material has the advantages of low price, easy decomposition and environmental protection.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. A preparation method of a fiber composite material is characterized by comprising the following steps:
pulverizing the wood raw material, steaming at 85-100 deg.C for 150min,
taking out the steamed wood raw material, and pretreating the wood raw material by using a mixed enzyme solution to obtain an enzyme treatment product;
adding the enzyme treatment product into a sodium hydroxide solution, soaking for 20-28h, rinsing to be neutral, and drying to obtain an alkali treatment product;
adding a silane coupling agent into absolute ethyl alcohol for dilution, adding an alkali treatment product, mixing, and drying to obtain a first treatment product;
weighing the first treated substance, the base material, the antioxidant and the lubricant in proportion, adding into a double-screw extruder, and carrying out high-temperature mixing at the temperature of 170 ℃ and 220 ℃ and at the speed of 60-80r/min to obtain a blend;
and crushing the blend, then performing injection molding, cooling and demolding to obtain the fiber composite material.
2. The method of claim 1, wherein the wood-based material comprises agave, reed, palm and kenaf, and the crushed wood-based material has a particle size of 40-65 μm.
3. The method for preparing a fiber composite material according to claim 1, wherein the mixed enzyme comprises the following components in a mass ratio of (0.1-0.4): (1.5-1.8) pectin lyase and xylanase, wherein the concentration of the mixed enzyme is 30-40%.
4. The method for preparing a fiber composite material according to claim 1, wherein the mixed enzyme solution treatment comprises the following steps: mixing the steamed wood raw material with a mixed enzyme solution according to the weight ratio of 1: (2-3), soaking for 5-8h at 45-55 ℃, washing, and drying at 35-45 ℃ to obtain an enzyme treatment product.
5. The method of claim 1, wherein the sodium hydroxide solution has a concentration of 5 to 10%, and the alkali-treated product is dried at 35 to 45 ℃.
6. The method for preparing a fiber composite material according to claim 1, wherein the mass ratio of the silane coupling agent to the alkali-treated product is (0.3-0.8): 1, wherein the mass ratio of the silane coupling agent to the absolute ethyl alcohol is 1: (8-10).
7. The method as claimed in claim 1, wherein the silane coupling agent is diluted and then mixed with the alkali treatment product at a speed of 900-1200r/min for 20-25min, and the first treated material is dried at 70-80 ℃ for 100-140 min.
8. The preparation method of the fiber composite material, according to claim 1, characterized in that the mass ratio of the first treatment substance, the base material, the antioxidant and the lubricant is (3-7): (93-97): (0.05-0.15): (0.05-0.15).
9. The method for preparing the fiber composite material according to claim 1, wherein the base material is one of polylactic acid, high-density polyethylene, polyacrylonitrile and polypropylene; the silane coupling agent is KH550 or KH 560; the lubricant is silicone oil; the antioxidant is tridecyl phosphite.
10. The method for preparing a fiber composite material according to claim 1, wherein the first stage extrusion temperature of the twin-screw extruder is 170 ℃, the second stage extrusion temperature is 190 ℃, the third stage extrusion temperature is 190 ℃, the fourth stage extrusion temperature is 210 ℃, and the fifth stage extrusion temperature is 220 ℃.
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