CN111576048A - Preparation method of composite material for military protective clothing - Google Patents
Preparation method of composite material for military protective clothing Download PDFInfo
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- CN111576048A CN111576048A CN202010274450.5A CN202010274450A CN111576048A CN 111576048 A CN111576048 A CN 111576048A CN 202010274450 A CN202010274450 A CN 202010274450A CN 111576048 A CN111576048 A CN 111576048A
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- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/55—Epoxy resins
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/06—Thermally protective, e.g. insulating
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/10—Impermeable to liquids, e.g. waterproof; Liquid-repellent
- A41D31/102—Waterproof and breathable
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/4007—Curing agents not provided for by the groups C08G59/42 - C08G59/66
- C08G59/4014—Nitrogen containing compounds
- C08G59/4021—Ureas; Thioureas; Guanidines; Dicyandiamides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5033—Amines aromatic
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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
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D2600/00—Uses of garments specially adapted for specific purposes
- A41D2600/20—Uses of garments specially adapted for specific purposes for working activities
-
- 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
- D06M2101/06—Vegetal fibres cellulosic
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- 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
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
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- 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
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
- D06M2101/36—Aromatic polyamides
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Textile Engineering (AREA)
- Materials Engineering (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a preparation method of a composite material for military protective clothing, which relates to the technical field of clothing fabrics.
Description
The technical field is as follows:
the invention relates to the technical field of garment materials, in particular to a preparation method of a composite material for military protective clothing.
Background art:
military protective clothing, which helps soldiers effectively resist, prevent and resist severe weather conditions and conventional, nuclear, biological and chemical warfare to the utmost extent. The main performance requirements are as follows: (1) mechanical and physical properties, can be exposed to severe weather environment for a long time and bear severe abrasion, and has high tensile strength and tearing strength; (2) in terms of environment, water resistance, wind resistance, snow resistance and insect prevention are required; (3) in the physiological aspect, the requirements are light weight, convenient wearing, small thermal stress, air permeability, moisture permeability, sweat dissipation and comfort; (4) the protective performance requires bulletproof property, flame retardance, chemical agent resistance and biological agent resistance, nuclear weapon remote thermal effect resistance, good camouflage property and small sound. In addition to the above requirements, military protective clothing for special purposes should also have strong acid, liquid oxygen, liquid nitrogen, liquid ammonia resistance, and the like. The invention develops a novel composite material for military protective clothing, which has a plurality of good service performances, particularly waterproof moisture permeability and heat insulation.
The invention content is as follows:
the technical problem to be solved by the invention is to provide a preparation method of a composite material for military protective clothing, the preparation method is simple and convenient to operate and good in repeatability, and the prepared composite material has good waterproof moisture permeability and heat insulation.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
the preparation method of the composite material for military protective clothing comprises the following preparation steps:
(1) preparing modified bamboo fibers: dispersing bamboo fibers in ethanol, adding N-cyclopropyl-2-hydroxy-benzamide and a catalyst, heating to a reflux state, carrying out heat preservation reaction, standing after the reaction is finished, filtering, washing with ethanol, washing with water, and drying to obtain modified bamboo fibers;
(2) preparing the composite fiber fabric: the aramid fiber, the polypropylene fiber, the modified bamboo fiber and the ramie fiber are blended, twisted and woven to prepare the composite fiber fabric;
(3) preparing glue solution: adding epoxy resin and a curing agent into a solvent, and uniformly mixing to obtain a glue solution;
(4) preparing a composite material: and (3) soaking the prepared composite fiber fabric in the prepared glue solution, taking out, drying and curing to obtain the composite material.
In the step (1), the mass ratio of the bamboo fiber, the N-cyclopropyl-2-hydroxy-benzamide to the catalyst is (30-50): (5-15): 0.1-5).
The catalyst in the step (1) is an alkaline catalyst.
In the step (2), the mass ratio of the aramid fiber, the polypropylene fiber, the modified bamboo fiber and the ramie fiber is (5-20): (1-10): 0.5-5.
The mass ratio of the epoxy resin to the curing agent in the step (3) is (80-90) to (10-20).
The solid content of the glue solution in the step (3) is 40-60%.
And (3) the solvent in the step (3) is ethanol or ethanol water solution.
The curing agent in the step (3) is dicyandiamide.
In the step (4), the dipping temperature is 30-50 ℃, and the dipping time is 10-30 min.
The drying temperature in the step (4) is 80-100 ℃.
According to the invention, carbonyl in lignin molecules contained in the bamboo fibers and hydroxyl in N-cyclopropyl-2-hydroxy-benzamide molecules are subjected to aldol condensation reaction to generate ether bonds, and cyclopropyl, ether groups and amide groups are introduced into the bamboo fiber structure, so that the application performance of the bamboo fibers is improved.
Dicyandiamide belongs to epoxy resin curing agents commonly used in the field, but the problem of high curing temperature exists, and the dicyandiamide is chemically modified aiming at reducing the input cost of curing energy consumption.
The curing agent is modified dicyandiamide.
The modified dicyandiamide is prepared by reacting dicyandiamide with 1-naphthylethylamine, and the structural formula is as follows:
compared with the existing dicyandiamide curing agent, the curing agent not only can obviously reduce the curing temperature, but also can optimize the application performance of the finally prepared composite material, and the technical effect is that the existing dicyandiamide curing agent cannot obtain.
The invention has the beneficial effects that: the military protective clothing composite material is prepared through the preparation of the modified bamboo fibers, the preparation of the composite fibers, the preparation of the glue solution and the preparation of the composite material, the adopted preparation method is simple and convenient to operate and has good repeatability, and the prepared composite material has good waterproof moisture permeability and heat insulation performance and meets the requirements of the military protective clothing on waterproof, heat insulation and moisture permeability under the outdoor environment.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
In the following examples and comparative examples, the epoxy resin is purchased from E-44 of Jinan Yisheng resins Co., Ltd, the epoxy equivalent is 210-250g/eq, and the softening point is 12-20 ℃; aramid fiber was purchased from dupont aramid kevlar fiber K29400D (440 Dtex); polypropylene fibers were purchased from polypropylene monofilament fibers of new materials science and technology ltd, liltdon, usa; bamboo fiber was purchased from Shandong Xintaiyuan New materials science and technology Co., Ltd; ramie fibers were purchased from Nanjing Xinhe textile Co., Ltd.
Example 1
Preparing a composite material:
(1) preparing modified bamboo fibers: dispersing 21.8g of bamboo fiber in 200g of ethanol, adding a saturated aqueous solution prepared from 4.1g N-cyclopropyl-2-hydroxy-benzamide and 0.6g of anhydrous potassium carbonate, heating to a reflux state, keeping the temperature, reacting for 5 hours, standing after the reaction is finished, filtering, washing with ethanol, washing with water, and drying at 80 ℃ to obtain modified bamboo fiber;
(2) preparing the composite fiber fabric: aramid fiber, polypropylene fiber, modified bamboo fiber and ramie fiber in a mass ratio of 10:6:1.5:0.8 are blended to prepare blended single yarns with the linear density of 91.4dtex, then the two blended single yarns are combined and twisted to obtain blended yarn plied yarns with the linear density of 980 twists/meter and 182.8dtex, then the blended yarn plied yarns are used as warp and weft yarns, the warp density is 620 pieces/10 cm, and the weft density is 350 pieces/10 cm, so that the composite fiber fabric is prepared;
(3) preparing glue solution: adding 85g of epoxy resin and 15g of dicyandiamide curing agent into 70% ethanol solution, and uniformly mixing to obtain glue solution with solid content of 52%;
(4) preparing a composite material: and (3) soaking the prepared composite fiber fabric in the glue solution prepared at the temperature of 45 ℃ for 30min, taking out, drying at the temperature of 80 ℃, and curing at the temperature of 195 ℃ for 5h to obtain the composite material.
Example 2
Example 2 differs from example 1 only in that the mass ratio of aramid fibers, polypropylene fibers, modified bamboo fibers and ramie fibers was replaced with 9.5:6:2: 0.8.
Preparing a composite material:
(1) preparing modified bamboo fibers: dispersing 21.8g of bamboo fiber in 200g of ethanol, adding a saturated aqueous solution prepared from 4.1g N-cyclopropyl-2-hydroxy-benzamide and 0.6g of anhydrous potassium carbonate, heating to a reflux state, keeping the temperature, reacting for 5 hours, standing after the reaction is finished, filtering, washing with ethanol, washing with water, and drying at 80 ℃ to obtain modified bamboo fiber;
(2) preparing the composite fiber fabric: aramid fiber, polypropylene fiber, modified bamboo fiber and ramie fiber in a mass ratio of 9.5:6:2:0.8 are blended to prepare blended single yarns with the linear density of 91.4dtex, then the two blended single yarns are combined and twisted to obtain blended yarn plied yarns with the linear density of 980 twists/meter and 182.8dtex, then the blended yarn plied yarns are used as warp and weft yarns, the warp density is 620 pieces/10 cm, and the weft density is 350 pieces/10 cm, so that the composite fiber fabric is prepared;
(3) preparing glue solution: adding 85g of epoxy resin and 15g of dicyandiamide curing agent into 70% ethanol solution, and uniformly mixing to obtain glue solution with solid content of 52%;
(4) preparing a composite material: and (3) soaking the prepared composite fiber fabric in the glue solution prepared at the temperature of 45 ℃ for 30min, taking out, drying at the temperature of 80 ℃, and curing at the temperature of 195 ℃ for 5h to obtain the composite material.
Example 3
Example 3 differs from example 1 only in that the dicyandiamide curing agent is replaced with a modified dicyandiamide curing agent.
Preparation of modified dicyandiamide curing agent: mixing 17.1g of 1-naphthylethylamine, 9.0g of dicyandiamide and 200g of 70% ethanol solution, adding 38% concentrated hydrochloric acid to adjust the pH value to 5-6, heating to boiling, carrying out reflux heat preservation reaction for 5 hours, distilling to recover ethanol, transferring to an environment at 5 ℃ for cooling and crystallizing for 12 hours, filtering, washing with water, and drying at 80 ℃ to obtain the modified dicyandiamide curing agent. Elemental analysis: theoretical value C, 57.63; h, 6.22; cl, 12.15; and N, 24.00. Found C, 57.64; h, 6.23; cl, 12.12; n, 24.01.
Preparing a composite material:
(1) preparing modified bamboo fibers: dispersing 21.8g of bamboo fiber in 200g of ethanol, adding a saturated aqueous solution prepared from 4.1g N-cyclopropyl-2-hydroxy-benzamide and 0.6g of anhydrous potassium carbonate, heating to a reflux state, keeping the temperature, reacting for 5 hours, standing after the reaction is finished, filtering, washing with ethanol, washing with water, and drying at 80 ℃ to obtain modified bamboo fiber;
(2) preparing the composite fiber fabric: aramid fiber, polypropylene fiber, modified bamboo fiber and ramie fiber in a mass ratio of 10:6:1.5:0.8 are blended to prepare blended single yarns with the linear density of 91.4dtex, then the two blended single yarns are combined and twisted to obtain blended yarn plied yarns with the linear density of 980 twists/meter and 182.8dtex, then the blended yarn plied yarns are used as warp and weft yarns, the warp density is 620 pieces/10 cm, and the weft density is 350 pieces/10 cm, so that the composite fiber fabric is prepared;
(3) preparing glue solution: adding 85g of epoxy resin and 15g of dicyandiamide curing agent into 70% ethanol solution, and uniformly mixing to obtain glue solution with solid content of 52%;
(4) preparing a composite material: and (3) soaking the prepared composite fiber fabric in the glue solution prepared at the temperature of 45 ℃ for 30min, taking out, drying at the temperature of 80 ℃, and curing at the temperature of 135 ℃ for 5h to obtain the composite material.
Comparative example
The comparative example is different from example 1 only in that the bamboo fiber is not modified.
Preparing a composite material:
(1) preparing the composite fiber fabric: aramid fiber, polypropylene fiber, bamboo fiber and ramie fiber in a mass ratio of 10:6:1.5:0.8 are blended to prepare blended single yarns with the linear density of 91.4dtex, then the two blended single yarns are combined and twisted to obtain blended yarn plied yarns with the linear density of 980 twists/meter and 182.8dtex, and then the blended yarn plied yarns are used as warp and weft yarns, the warp density of 620 pieces/10 cm and the weft density of 350 pieces/10 cm to prepare the composite fiber fabric;
(2) preparing glue solution: adding 85g of epoxy resin and 15g of dicyandiamide curing agent into 70% ethanol solution, and uniformly mixing to obtain glue solution with solid content of 52%;
(3) preparing a composite material: and (3) soaking the prepared composite fiber fabric in the glue solution prepared at the temperature of 45 ℃ for 30min, taking out, drying at the temperature of 80 ℃, and curing at the temperature of 195 ℃ for 5h to obtain the composite material.
The modified bamboo fiber prepared in example 1 was analyzed by infrared ray to show 1680cm-1Absorption of the amide group showed that N-cyclopropyl-2-hydroxy-benzamide was successfully grafted onto the bamboo fiber.
The use properties of the composite materials prepared in examples 1 to 3 and comparative example were measured, and the results are shown in Table 1.
The hydrostatic pressure is determined according to the standard FZ/T01004-.
According to standard GB/T12704.1-2009 part 1 of textile fabric moisture permeability test method: moisture absorption method, the higher the value of the moisture permeability, the better the moisture permeability.
The Crohn value is determined according to the standard GB/T11048 and 2018' determination of thermal resistance and wet resistance of textile under the steady-state condition of physiological comfort, and the larger the Crohn value is, the better the heat retention is.
TABLE 1
Item | Example 1 | Example 2 | Example 3 | Comparative example |
Hydrostatic pressure kPa | 54.1 | 54.5 | 55.2 | 52.5 |
Moisture permeability g/m2.d | 5832 | 6014 | 6357 | 4296 |
CLO value CLO | 5.45 | 5.53 | 5.74 | 5.02 |
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The preparation method of the composite material for military protective clothing is characterized by comprising the following preparation steps:
(1) preparing modified bamboo fibers: dispersing bamboo fibers in ethanol, adding N-cyclopropyl-2-hydroxy-benzamide and a catalyst, heating to a reflux state, carrying out heat preservation reaction, standing after the reaction is finished, filtering, washing with ethanol, washing with water, and drying to obtain modified bamboo fibers;
(2) preparing the composite fiber fabric: the aramid fiber, the polypropylene fiber, the modified bamboo fiber and the ramie fiber are blended, twisted and woven to prepare the composite fiber fabric;
(3) preparing glue solution: adding epoxy resin and a curing agent into a solvent, and uniformly mixing to obtain a glue solution;
(4) preparing a composite material: and (3) soaking the prepared composite fiber fabric in the prepared glue solution, taking out, drying and curing to obtain the composite material.
2. The method of making a composite material for military protective apparel of claim 1, wherein the method comprises the steps of: in the step (1), the mass ratio of the bamboo fiber, the N-cyclopropyl-2-hydroxy-benzamide to the catalyst is (30-50): (5-15): 0.1-5).
3. The method of making a composite material for military protective apparel of claim 1, wherein the method comprises the steps of: the catalyst in the step (1) is an alkaline catalyst.
4. The method of making a composite material for military protective apparel of claim 1, wherein the method comprises the steps of: in the step (2), the mass ratio of the aramid fiber, the polypropylene fiber, the modified bamboo fiber and the ramie fiber is (5-20): (1-10): 0.5-5.
5. The method of making a composite material for military protective apparel of claim 1, wherein the method comprises the steps of: the mass ratio of the epoxy resin to the curing agent in the step (3) is (80-90) to (10-20).
6. The method of making a composite material for military protective apparel of claim 1, wherein the method comprises the steps of: the solid content of the glue solution in the step (3) is 40-60%.
7. The method of making a composite material for military protective apparel of claim 1, wherein the method comprises the steps of: and (3) the solvent in the step (3) is ethanol or ethanol water solution.
8. The method of making a composite material for military protective apparel of claim 1, wherein the method comprises the steps of: the curing agent in the step (3) is dicyandiamide.
9. The method of making a composite material for military protective apparel of claim 1, wherein the method comprises the steps of: in the step (4), the dipping temperature is 30-50 ℃, and the dipping time is 10-30 min.
10. The method of making a composite material for military protective apparel of claim 1, wherein the method comprises the steps of: the drying temperature in the step (4) is 80-100 ℃.
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2020
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US20150044924A1 (en) * | 2012-03-02 | 2015-02-12 | Avic Composite Corporation Ltd. | Composite having plant fiber textile and fabricating method thereof |
CN104356416A (en) * | 2014-11-14 | 2015-02-18 | 西安超码复合材料有限公司 | Method for preparing special shielding material |
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Title |
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王春红等: "表面改性对竹纤维与聚丙烯纤维混杂毡平铺复合材料湿热老化影响", 塑料, vol. 45, no. 04, pages 50 - 54 * |
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