CN101851429A - Lignin composite material and preparation method thereof - Google Patents
Lignin composite material and preparation method thereof Download PDFInfo
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- CN101851429A CN101851429A CN 201010199605 CN201010199605A CN101851429A CN 101851429 A CN101851429 A CN 101851429A CN 201010199605 CN201010199605 CN 201010199605 CN 201010199605 A CN201010199605 A CN 201010199605A CN 101851429 A CN101851429 A CN 101851429A
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- 239000002131 composite material Substances 0.000 title claims abstract description 66
- 229920005610 lignin Polymers 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000835 fiber Substances 0.000 claims abstract description 48
- 239000003063 flame retardant Substances 0.000 claims abstract description 46
- 239000000463 material Substances 0.000 claims abstract description 27
- 229920002101 Chitin Polymers 0.000 claims abstract description 22
- 239000000126 substance Substances 0.000 claims abstract description 18
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- -1 polyethylene Polymers 0.000 claims description 54
- 229920002521 macromolecule Polymers 0.000 claims description 25
- 239000011159 matrix material Substances 0.000 claims description 23
- 239000004902 Softening Agent Substances 0.000 claims description 22
- 239000003112 inhibitor Substances 0.000 claims description 22
- 230000003647 oxidation Effects 0.000 claims description 22
- 238000007254 oxidation reaction Methods 0.000 claims description 22
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 14
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims description 12
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 12
- 238000001125 extrusion Methods 0.000 claims description 12
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- 235000017491 Bambusa tulda Nutrition 0.000 claims description 7
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- 239000011425 bamboo Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
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- 238000003754 machining Methods 0.000 claims description 6
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 6
- YEVQZPWSVWZAOB-UHFFFAOYSA-N 2-(bromomethyl)-1-iodo-4-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=C(I)C(CBr)=C1 YEVQZPWSVWZAOB-UHFFFAOYSA-N 0.000 claims description 5
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- 239000003513 alkali Substances 0.000 claims description 5
- 239000004917 carbon fiber Substances 0.000 claims description 5
- MAMMVUWCKMOLSG-UHFFFAOYSA-N Cyclohexyl propionate Chemical compound CCC(=O)OC1CCCCC1 MAMMVUWCKMOLSG-UHFFFAOYSA-N 0.000 claims description 4
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 4
- 229920000578 graft copolymer Polymers 0.000 claims description 4
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 4
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 4
- 239000005014 poly(hydroxyalkanoate) Substances 0.000 claims description 4
- 229920000903 polyhydroxyalkanoate Polymers 0.000 claims description 4
- 229910000077 silane Inorganic materials 0.000 claims description 4
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 4
- 239000004743 Polypropylene Substances 0.000 claims description 3
- OBNCKNCVKJNDBV-UHFFFAOYSA-N ethyl butyrate Chemical compound CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical group Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 claims description 3
- 239000005050 vinyl trichlorosilane Substances 0.000 claims description 3
- WHBMMWSBFZVSSR-UHFFFAOYSA-N 3-hydroxybutyric acid Chemical compound CC(O)CC(O)=O WHBMMWSBFZVSSR-UHFFFAOYSA-N 0.000 claims description 2
- 244000198134 Agave sisalana Species 0.000 claims description 2
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 2
- 244000025254 Cannabis sativa Species 0.000 claims description 2
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims description 2
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 claims description 2
- 240000006240 Linum usitatissimum Species 0.000 claims description 2
- 235000004431 Linum usitatissimum Nutrition 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 240000000961 Setaria parviflora Species 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- DOOTYTYQINUNNV-UHFFFAOYSA-N Triethyl citrate Chemical compound CCOC(=O)CC(O)(C(=O)OCC)CC(=O)OCC DOOTYTYQINUNNV-UHFFFAOYSA-N 0.000 claims description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 2
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 2
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 2
- 235000009120 camo Nutrition 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 235000005607 chanvre indien Nutrition 0.000 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 claims description 2
- 239000011487 hemp Substances 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
- 239000000347 magnesium hydroxide Substances 0.000 claims description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims description 2
- YTXCAJNHPVBVDJ-UHFFFAOYSA-N octadecyl propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CC YTXCAJNHPVBVDJ-UHFFFAOYSA-N 0.000 claims description 2
- 150000003016 phosphoric acids Chemical class 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 2
- 239000001069 triethyl citrate Substances 0.000 claims description 2
- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 claims description 2
- 235000013769 triethyl citrate Nutrition 0.000 claims description 2
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 2
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims description 2
- 229940070710 valerate Drugs 0.000 claims description 2
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 244000082204 Phyllostachys viridis Species 0.000 claims 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 15
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- 229920000642 polymer Polymers 0.000 abstract description 3
- 230000004927 fusion Effects 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003963 antioxidant agent Substances 0.000 abstract 2
- 230000003078 antioxidant effect Effects 0.000 abstract 2
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
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- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
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- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention provides a lignin composite material and a preparation method thereof. The lignin composite material is formed by mixing lignin, a high molecular compound, a fiber substance, chitin, a plasticizer, a compatibilizer, an antioxidant and a flame retardant, wherein the lignin composite material comprises the following components in percentage by weight: 2.5 to 56.4 percent of lignin, 10 to 70.5 percent of high molecular compound, 2.5 to 16.92 percent of flame retardant, 0.5 to 7.52 percent of plasticizer, 0.5 to 9.4 percent of compatibilizer, 0.05 to 1.88 percent of antioxidant, 1 to 10 percent of chitin and 5 to 4 percent of fiber. The composite material is formed by compounding the lignin serving as a base material with at least one high molecular compound and gathering by fusion through a polymer, so the composite material has the advantages of low water absorption, high mechanical performance and degradability.
Description
Technical field
The invention belongs to technical field of polymer composite materials, specially refer to a kind of lignin composite material and preparation method thereof.
Background technology
Along with rapid economy development, the usage quantity of plastics is increasing, almost is penetrated into each link of people's life.But because the plastics major part of using utilizes petroleum resources synthetic at present, be nondegradable, thereby when consuming the bulk petroleum resource, return environment and brought severe contamination.The natural high moleculer eompound aboundresources has reproducibility, can degrade fully, is the ideal substitute of plastics, therefore is subjected to human consumer's the welcome and the attention of national governments.
Yet, natural high moleculer eompound generally all has very strong water-absorbent, therefore the matrix material page or leaf that utilizes natural high moleculer eompound to make at present all has very strong water-absorbent, and water-absorbent can further increase along with the adding of softening agent, and the mechanical property of matrix material can decline to a great extent after meeting water; Because natural high moleculer eompound at high temperature easily decomposes, cause its course of processing complexity simultaneously, and processing requirement is harsh relatively.
Summary of the invention
The objective of the invention is to propose that a kind of water-absorbent is little, good mechanical performance, degradable lignin composite material and preparation method thereof.
Lignin composite material of the present invention is by xylogen, macromolecular compound, fiber substance, chitin, softening agent, expanding material, oxidation inhibitor, fire retardant mixes, wherein the shared weight percent of each composition is as follows: the content of xylogen is 2.5%～56.4%, the content of macromolecular compound is 10%～70.5%, the content of fire retardant is 2.5%～16.92%, the content of softening agent is 0.5%～7.52%, the content of expanding material is 0.5%～9.4%, the content of oxidation inhibitor is 0.05%～1.88%, the content of chitin is 1%～10%, and the content of fiber is 5%～40%.
Described xylogen is the high pure alkali xylogen.
Described macromolecular compound is artificial synthetic macromolecular compound and/or natural high moleculer eompound, wherein the synthetic macromolecular compound is one or more in polyethylene, polypropylene, poly(lactic acid), the poly butylene succinate, and natural high moleculer eompound is one or more in starch, polycaprolactone, poly-beta-hydroxy-butyrate, poly-butyric ester, the poly-valerate.
Described fiber substance is one or more the combination in glass fibre, carbon fiber, bamboo fibers, hemp fibre, jute fibre, sisal fibers, flax fiber, the monkey grass, and the length-to-diameter ratio of above-mentioned fiber substance is 5～30.
Described fire retardant is one or more combination wherein such as triphenyl phosphite, ammonium polyphosphate, melamine, triphenylphosphate, phosphoric acid salt, melamine cyanurate, magnesium hydroxide, aluminium hydroxide, antimonous oxide, trioctyl phosphate, tributyl phosphate, zinc borate, tetramethylolmethane or polynite.Above-mentioned fire retardant all adopts halogen-free flame retardants, can not produce toxic substance, non-environmental-pollution in use and the combustion processes.
Described softening agent is a kind of in glycerine, methane amide, dioctyl phthalate (DOP), polyoxyethylene glycol, diethyl phthalate, tributyl citrate, acetylize triethyl citrate, the methane amide acetylize tributyl citrate.
Described expanding material is a kind of in polyethylene vinyl acetate, maleic anhydride graft copolymer, polycaprolactone, polyhydroxyalkanoate, the Resins, epoxy.
Described oxidation inhibitor is four (β-(3,5 di-tert-butyl-hydroxy phenyls) propionic acid) pentaerythritol ester, (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid octadecyl ester, β-(3, the 5-di-tert-butyl-hydroxy phenyl) cyclohexyl propionate, a kind of in the Tyox B.
As shown in Figure 1, the preparation method of lignin composite material of the present invention comprises the steps:
A: with xylogen, macromolecular compound, fire retardant drying treatment, the drying treatment temperature is 50～80 ℃, and be 3～12 hours time of drying;
B: dried xylogen, macromolecular compound, fire retardant in softening agent, expanding material, oxidation inhibitor and the steps A are stirred in the exsiccant homogenizer according to certain weight proportion, it is mixed, putting into twin screw extruder then reacts, screw speed is 15rpm～180rpm, extrusion temperature is 150 ℃～200 ℃, with the product cooling and dicing of extruding, oven dry obtains the matrix material master batch; Wherein the shared weight percent of each composition is as follows: the content of xylogen is 5%～60%, the content of macromolecular compound is 20%～75%, the content of fire retardant is 5%～18%, the content of softening agent is 1%～8%, the content of expanding material is 1%～10%, and the content of oxidation inhibitor is 0.1%～2%;
C: with fiber substance concentration is that 0.1%～2% silane coupler solution is soaked, and obtains modified fibre;
D: the modified fibre that matrix material master batch that step B is obtained and chitin and step C obtain successively adds and carries out Compound Machining in the twin screw extruder, screw speed is 35rpm～200rpm, extrusion temperature is 160 ℃～220 ℃, finally obtains lignin composite material; Wherein the shared weight percent of each composition is as follows: the content of matrix material master batch is 50%～94%, and the content of chitin is 1%～10%, and the content of fiber is 5%～40%.
Silane coupling agent described in the step C is vinyl trichloro silane, vinyl three (beta-methoxy-oxyethyl group) silane, vinyltriethoxysilane, γ-metacryloxy Trimethoxy silane, β-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane, γ-glycidoxypropyltrimewasxysilane, a kind of in N-(beta-aminoethyl)-γ TSL 8330, γ-An Bingjisanyiyangjiguiwan, N-phenyl-gamma-amino propyl trimethoxy silicane, γ-methyl mercapto propyl trimethoxy silicane and the γ-r-chloropropyl trimethoxyl silane.
Xylogen is after Mierocrystalline cellulose, second renewable, the degradable natural polymer child resource that enriches on the earth, and good mechanical performance such as intensity, rigidity, shock-resistant, ultraviolet resistance is good, and water-absorbent is little, simultaneously heat insulation, sound-absorbing.Present xylogen mainly obtains from papermaking wastewater, aboundresources, and cost is low, has both rationally utilized resource, has reduced environmental pollution again.
The present invention is base material with the xylogen, at least compound a kind of macromolecular compound, and the fusion by polymkeric substance assembles and forms matrix material, this matrix material not only has the character as the timber, simultaneously can make different shape easily by injection moulding again, easy to process.The present invention has complementary advantages by composite modified making between the different polymer materialss, and control performance of composites by the content of regulating each composition, make it have good anti-uv-ray, high strength, high rigidity, high shock resistance and fire-retardant, degradable performance etc. can be widely used in a plurality of fields such as automobile, aviation, building and electronic apparatus.
Description of drawings
Fig. 1 is preparation method's schema of the lignin composite material of each embodiment among the present invention;
Fig. 2 is the test form of mechanical property, flame retardant properties, degradation property and the water-intake rate of the lignin composite material of each embodiment among the present invention.
Embodiment
Describe the present invention in detail below in conjunction with specific embodiments and the drawings.
Embodiment 1:
The embodiment of the invention 1 has proposed a kind of lignin composite material, this lignin composite material is mixed by high pure alkali xylogen, macromolecular compound, fiber substance, chitin, softening agent, expanding material, oxidation inhibitor, fire retardant, wherein macromolecular compound adopts poly(lactic acid), poly butylene succinate, fiber substance adopts bamboo fibers, softening agent adopts glycerine, expanding material adopts polyhydroxyalkanoate, oxidation inhibitor to adopt four (β-(3,5 di-tert-butyl-hydroxy phenyls) pentaerythritol ester propionic acid), fire retardant adopts triphenyl phosphite.
Concrete, the lignin composite material preparation method that the invention process 1 proposes is as follows:
A: high pure alkali xylogen, poly(lactic acid), poly butylene succinate, fire retardant triphenyl phosphite were removed moisture down in dry 12 hours at 50 ℃ respectively;
B: with the high pure alkali xylogen after the A step drying treatment, poly(lactic acid), poly butylene succinate, fire retardant triphenyl phosphite and softening agent glycerine, expanding material polyhydroxyalkanoate, oxidation inhibitor four (β-(3,5 di-tert-butyl-hydroxy phenyls) propionic acid) pentaerythritol ester is even in the high speed blender and mixing according to weight percent 5%, 65%, 10%, 18%, 1%, 1%, 0.1% respectively, putting into twin screw extruder then reacts, product is through cooling, pelletizing, oven dry obtains the matrix material master batch; Wherein screw speed is 180rpm, 150 ℃ of extrusion temperatures;
C: with length-to-diameter ratio is that 5 bamboo fibers was immersed in the aqueous solution that concentration is 0.1% silane coupling agent (vinyl trichloro silane) after 5 hours, carries out drying treatment, obtains the consistency bamboo fibers of surface modification;
D: matrix material master batch that step B is obtained and the modification bamboo fibers that obtains of chitin and step C successively join and carry out Compound Machining in the twin screw extruder, and screw speed is 200rpm, and extrusion temperature is 160 ℃, finally obtains lignin composite material; Wherein the weight content of matrix material master batch, chitin and bamboo fibers is respectively 94%, 1% and 5%.
The lignin composite material that the present invention proposes has the following advantages: water-absorbent is little, good mechanical performance and degradable, and the lignin composite material preparation method that the present invention proposes is simple, easy to process, this lignin composite material can be widely used in a plurality of fields such as automobile, aviation, building and electronic apparatus.
As shown in Figure 2, the every good mechanical performance of the lignin composite material of present embodiment, degradability is good.
Utilize flame retardant resistance UL94V to test the flame retardant resistance of the lignin composite material of testing present embodiment: the above-mentioned lignin composite material of preparing is vertically placed, and wherein, the specification of lignin composite material is: long 127 millimeters * wide 12.7 millimeters * thick 1.6 millimeters.Lignin composite material test furnace down-firing 10 seconds, is measured the self-extinguishing time that lignin composite material catches fire; After fray-out of flame lignin composite material was lighted a fire for 10 seconds again, the test flame self-extinguishing time is investigated the kindling material that falls simultaneously and whether can be lighted absorbent cotton.By for the first time and secondary ignition time and absorbent cotton catch fire the evaluating material grade of burning.Wherein, burning grade V0 level represents that the grade of material combustion is the highest, and the burning grade is downwards V1 level and V2 level with this.
Through test, the flame retardant resistance of the lignin composite material of present embodiment is the V0 grade.
Embodiment 2
The embodiment of the invention 2 has proposed a kind of lignin composite material, this lignin composite material is mixed by xylogen, macromolecular compound, fiber substance, chitin, softening agent, expanding material, oxidation inhibitor, fire retardant, wherein macromolecular compound adopts polypropylene, poly-butyric ester, fiber substance adopts jute fibre, softening agent adopts glycerine, expanding material adopts polycaprolactone, oxidation inhibitor to adopt four (β-(3,5 di-tert-butyl-hydroxy phenyls) pentaerythritol ester propionic acid), fire retardant adopts antimonous oxide.
Concrete, the lignin composite material preparation method that the invention process 2 proposes is as follows:
A: xylogen, poly(lactic acid), poly butylene succinate, fire retardant antimonous oxide were removed moisture down in dry 9 hours at 60 ℃ respectively;
B: with the xylogen after the A step drying treatment, poly(lactic acid), poly butylene succinate, fire retardant antimonous oxide and softening agent glycerine, expanding material polycaprolactone, oxidation inhibitor four (β-(3,5 di-tert-butyl-hydroxy phenyls) propionic acid) pentaerythritol ester is even in the high speed blender and mixing according to weight percent 26%, 30%, 20%, 13.5%, 4%, 6%, 0.5% respectively, putting into twin screw extruder then reacts, product is through cooling, pelletizing, oven dry obtains the matrix material master batch; Wherein screw speed is 120rpm, 165 ℃ of extrusion temperatures;
C: with length-to-diameter ratio is that 10 jute fibre was immersed in the aqueous solution that concentration is 0.5% silane coupling agent (γ-An Bingjisanyiyangjiguiwan) after 5 hours, carries out drying treatment, obtains the consistency jute fibre of surface modification;
D: matrix material master batch that step B is obtained and the modification jute fibre that obtains of chitin and step C successively join and carry out Compound Machining in the twin screw extruder, and screw speed is 135rpm, and extrusion temperature is 180 ℃, finally obtains lignin composite material; Wherein the weight content of matrix material master batch, chitin and jute fibre is respectively 81%, 4% and 15%.
As shown in Figure 2, the every good mechanical performance of the lignin composite material of present embodiment, degradability is good.
The flame retardant resistance of utilizing the flame retardant resistance UL94V experimental technique among the embodiment 1 to test the lignin composite material of present embodiment, through test, the flame retardant resistance of the lignin composite material of present embodiment is the V0 grade.
Embodiment 3:
The embodiment of the invention 3 has proposed a kind of lignin composite material, this lignin composite material is mixed by xylogen, macromolecular compound, fiber substance, chitin, softening agent, expanding material, oxidation inhibitor, fire retardant, wherein macromolecular compound adopts polyethylene, fiber substance adopts carbon fiber, softening agent adopts diethyl phthalate, expanding material adopts polyethylene vinyl acetate, oxidation inhibitor to adopt β-(3, the 5-di-tert-butyl-hydroxy phenyl) cyclohexyl propionate, fire retardant adopts trioctyl phosphate.Concrete preparation method is as follows:
A: xylogen, polyethylene and fire retardant trioctyl phosphate were removed moisture down in dry 6 hours at 70 ℃ respectively;
B: with the xylogen after the A step drying treatment, polyethylene, fire retardant trioctyl phosphate and plasticizer phthalic acid diethyl ester, expanding material polyethylene vinyl acetate, oxidation inhibitor β-(3, the 5-di-tert-butyl-hydroxy phenyl) cyclohexyl propionate is even in the high speed blender and mixing according to weight percent 49%, 30%, 9%, 6%, 5%, 1% respectively, putting into twin screw extruder then reacts, product is through cooling, pelletizing, oven dry obtains the matrix material master batch; Wherein screw speed is 60rpm, 185 ℃ of extrusion temperatures;
C: with length-to-diameter ratio is that 20 carbon fiber was immersed in the aqueous solution that concentration is 1% silane coupling agent (N-(beta-aminoethyl)-γ TSL 8330) after 5 hours, carries out drying treatment, obtains the consistency carbon fiber of surface modification;
D: matrix material master batch that step B is obtained and the modified carbon fiber that obtains of chitin and step C successively join and carry out Compound Machining in the twin screw extruder, and screw speed is 75rpm, and extrusion temperature is 200 ℃, finally obtains lignin composite material; Wherein the weight content of matrix material master batch, chitin and jute fibre is respectively 63%, 7% and 30%.
As shown in Figure 2, the every good mechanical performance of the lignin composite material of present embodiment, degradability is good.
The flame retardant resistance of utilizing the flame retardant resistance UL94V experimental technique among the embodiment 1 to test the lignin composite material of present embodiment, through test, the flame retardant resistance of the lignin composite material of present embodiment is the V1 grade.
Embodiment 4:
The embodiment of the invention 4 has proposed a kind of lignin composite material; this lignin composite material is mixed by xylogen, macromolecular compound, fiber substance, chitin, softening agent, expanding material, oxidation inhibitor, fire retardant; wherein macromolecular compound adopts polyethylene; fiber substance adopts glass fibre; softening agent adopts the acetylize tributyl citrate; expanding material adopts maleic anhydride graft copolymer, and oxidation inhibitor adopts Tyox B, fire retardant adopting montmorillonite.
Concrete, the lignin composite material preparation method that the invention process 4 proposes is as follows:
A: xylogen, polyethylene and fire retardant polynite were removed moisture down in dry 3 hours at 80 ℃ respectively;
B: the xylogen after the A step drying treatment, polyethylene, fire retardant polynite and softening agent acetylize tributyl citrate, expanding material maleic anhydride graft copolymer, oxidation inhibitor Tyox B is even in the high speed blender and mixing according to weight percent 60%, 15%, 5%, 8%, 10%, 2% respectively, putting into twin screw extruder then reacts, product is through cooling, pelletizing, oven dry obtains the matrix material master batch; Wherein screw speed is 15rpm, 200 ℃ of extrusion temperatures;
C: with length-to-diameter ratio is that 30 glass fibre soaks in concentration to be in the aqueous solution of 2% silane coupling agent (N-(beta-aminoethyl)-γ TSL 8330) after 5 hours, to carry out drying treatment, obtain the consistency glass fibre of surface modification;
D: matrix material master batch that step B is obtained and the modified glass-fiber that obtains of chitin and step C successively join and carry out Compound Machining in the twin screw extruder, and screw speed is 35rpm, and extrusion temperature is 220 ℃, finally obtains lignin composite material; Wherein the weight content of matrix material master batch, chitin and jute fibre is respectively 50%, 10% and 40%.
As shown in Figure 2, the every good mechanical performance of the lignin composite material of present embodiment, degradability is good.
The flame retardant resistance of utilizing the flame retardant resistance UL94V experimental technique among the embodiment 1 to test the lignin composite material of present embodiment, through test, the flame retardant resistance of the lignin composite material of present embodiment is the V2 grade.
The lignin composite material that the present invention proposes has the following advantages: water-absorbent is little, good mechanical performance and degradable, and the lignin composite material preparation method that the present invention proposes is simple, easy to process, this lignin composite material can be widely used in a plurality of fields such as automobile, aviation, building and electronic apparatus.
The above only is preferred embodiment of the present invention, and is in order to restriction the present invention, within the spirit and principles in the present invention not all, any modification of being done, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. lignin composite material, it is characterized in that this matrix material is by xylogen, macromolecular compound, fiber substance, chitin, softening agent, expanding material, oxidation inhibitor, fire retardant mixes, wherein the shared weight percent of each composition is as follows: the content of xylogen is 2.5%～56.4%, the content of macromolecular compound is 10%～70.5%, the content of fire retardant is 2.5%～16.92%, the content of softening agent is 0.5%～7.52%, the content of expanding material is 0.5%～9.4%, the content of oxidation inhibitor is 0.05%～1.88%, the content of chitin is 1%～10%, and the content of fiber is 5%～40%.
2. lignin composite material according to claim 1 is characterized in that described xylogen is the high pure alkali xylogen.
3. lignin composite material according to claim 1, it is characterized in that described macromolecular compound is artificial synthetic macromolecular compound and/or natural high moleculer eompound, wherein the synthetic macromolecular compound is one or more in polyethylene, polypropylene, poly(lactic acid), the poly butylene succinate, and natural high moleculer eompound is one or more in starch, polycaprolactone, poly-beta-hydroxy-butyrate, poly-butyric ester, the poly-valerate.
4. lignin composite material according to claim 1, it is characterized in that described fiber substance is one or more the combination in glass fibre, carbon fiber, bamboo fibers, hemp fibre, jute fibre, sisal fibers, flax fiber, the monkey grass, and the length-to-diameter ratio of above-mentioned fiber substance is 5～30.
5. lignin composite material according to claim 1 is characterized in that described fire retardant is one or more combination wherein such as triphenyl phosphite, ammonium polyphosphate, melamine, triphenylphosphate, phosphoric acid salt, melamine cyanurate, magnesium hydroxide, aluminium hydroxide, antimonous oxide, trioctyl phosphate, tributyl phosphate, zinc borate, tetramethylolmethane or polynite.
6. lignin composite material according to claim 1 is characterized in that described softening agent is a kind of in glycerine, methane amide, dioctyl phthalate (DOP), polyoxyethylene glycol, diethyl phthalate, tributyl citrate, acetylize triethyl citrate, the methane amide acetylize tributyl citrate.
7. lignin composite material according to claim 1 is characterized in that described expanding material is a kind of in polyethylene vinyl acetate, maleic anhydride graft copolymer, polycaprolactone, polyhydroxyalkanoate, the Resins, epoxy.
8. lignin composite material according to claim 1, it is characterized in that described oxidation inhibitor is four (β-(3,5 di-tert-butyl-hydroxy phenyls) pentaerythritol ester, (3 propionic acid), the 5-di-tert-butyl-hydroxy phenyl) propionic acid octadecyl ester, β-(3, the 5-di-tert-butyl-hydroxy phenyl) cyclohexyl propionate, a kind of in the Tyox B.
9. the preparation method of lignin composite material according to claim 1, it is characterized in that comprising the steps: A: xylogen, macromolecular compound, fire retardant are carried out drying treatment, the drying treatment temperature is 50～80 ℃, and be 3～12 hours time of drying;
B: dried xylogen, macromolecular compound, fire retardant in softening agent, expanding material, oxidation inhibitor and the steps A are stirred in the exsiccant homogenizer according to certain weight proportion, it is mixed, putting into twin screw extruder then reacts, screw speed is 15rpm～180rpm, extrusion temperature is 150 ℃～200 ℃, with the product cooling and dicing of extruding, oven dry obtains the matrix material master batch; Wherein the shared weight percent of each composition is as follows: the content of xylogen is 5%～60%, the content of macromolecular compound is 20%～75%, the content of fire retardant is 5%～18%, the content of softening agent is 1%～8%, the content of expanding material is 1%～10%, and the content of oxidation inhibitor is 0.1%～2%;
C: with fiber substance concentration is that 0.1%～2% silane coupler solution is soaked, and obtains modified fibre;
D: the modified fibre that matrix material master batch that step B is obtained and chitin and step C obtain successively adds and carries out Compound Machining in the twin screw extruder, screw speed is 35rpm～200rpm, extrusion temperature is 160 ℃～220 ℃, finally obtains lignin composite material; Wherein the shared weight percent of each composition is as follows: the content of matrix material master batch is 50%～94%, and the content of chitin is 1%～10%, and the content of fiber is 5%～40%.
10. the preparation method of lignin composite material according to claim 9, it is characterized in that described silane coupling agent is a vinyl trichloro silane, vinyl three (beta-methoxy-oxyethyl group) silane, vinyltriethoxysilane, γ-metacryloxy Trimethoxy silane, β-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane, γ-glycidoxypropyltrimewasxysilane, N-(beta-aminoethyl)-γ TSL 8330, γ-An Bingjisanyiyangjiguiwan, N-phenyl-gamma-amino propyl trimethoxy silicane, a kind of in γ-methyl mercapto propyl trimethoxy silicane and the γ-r-chloropropyl trimethoxyl silane.
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