CN115160707B - Polyvinyl chloride wood-plastic composite material and preparation method thereof - Google Patents
Polyvinyl chloride wood-plastic composite material and preparation method thereof Download PDFInfo
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- CN115160707B CN115160707B CN202210774409.3A CN202210774409A CN115160707B CN 115160707 B CN115160707 B CN 115160707B CN 202210774409 A CN202210774409 A CN 202210774409A CN 115160707 B CN115160707 B CN 115160707B
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- 239000004800 polyvinyl chloride Substances 0.000 title claims abstract description 48
- 229920000915 polyvinyl chloride Polymers 0.000 title claims abstract description 48
- 239000000463 material Substances 0.000 title claims abstract description 33
- 229920001587 Wood-plastic composite Polymers 0.000 title claims abstract description 31
- 239000011155 wood-plastic composite Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 39
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical class O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 claims abstract description 38
- 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 claims abstract description 30
- 239000003063 flame retardant Substances 0.000 claims abstract description 30
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 26
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 19
- 229920001046 Nanocellulose Polymers 0.000 claims abstract description 17
- 239000007822 coupling agent Substances 0.000 claims abstract description 17
- 239000000314 lubricant Substances 0.000 claims abstract description 9
- 239000002023 wood Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 50
- 238000010438 heat treatment Methods 0.000 claims description 45
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 42
- 239000011240 wet gel Substances 0.000 claims description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 38
- 238000001035 drying Methods 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 23
- -1 silicon nitride compound Chemical class 0.000 claims description 21
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 19
- 229910001308 Zinc ferrite Inorganic materials 0.000 claims description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims description 19
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical group O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 claims description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 17
- LUNMJRJMSXZSLC-UHFFFAOYSA-N 2-cyclopropylethanol Chemical compound OCCC1CC1 LUNMJRJMSXZSLC-UHFFFAOYSA-N 0.000 claims description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 14
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 14
- 239000004209 oxidized polyethylene wax Substances 0.000 claims description 14
- 235000013873 oxidized polyethylene wax Nutrition 0.000 claims description 14
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 13
- 239000001301 oxygen Substances 0.000 claims description 13
- 229910052760 oxygen Inorganic materials 0.000 claims description 13
- 229920002050 silicone resin Polymers 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 12
- UMFJXASDGBJDEB-UHFFFAOYSA-N triethoxy(prop-2-enyl)silane Chemical compound CCO[Si](CC=C)(OCC)OCC UMFJXASDGBJDEB-UHFFFAOYSA-N 0.000 claims description 12
- 238000002485 combustion reaction Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 9
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 7
- 229910018487 Ni—Cr Inorganic materials 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 7
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 239000008187 granular material Substances 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 238000011068 loading method Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000001125 extrusion Methods 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 229920003192 poly(bis maleimide) Polymers 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 238000000643 oven drying Methods 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- LFRDHGNFBLIJIY-UHFFFAOYSA-N trimethoxy(prop-2-enyl)silane Chemical group CO[Si](OC)(OC)CC=C LFRDHGNFBLIJIY-UHFFFAOYSA-N 0.000 claims description 2
- 239000004566 building material Substances 0.000 abstract description 2
- 241000219000 Populus Species 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 239000002131 composite material Substances 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 239000004743 Polypropylene Substances 0.000 description 5
- 238000009835 boiling Methods 0.000 description 5
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000005484 gravity Effects 0.000 description 5
- 238000003760 magnetic stirring Methods 0.000 description 5
- 229920001155 polypropylene Polymers 0.000 description 5
- 239000011863 silicon-based powder Substances 0.000 description 5
- 239000000779 smoke Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L97/00—Compositions of lignin-containing materials
- C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the field of building materials, in particular to a polyvinyl chloride wood-plastic composite material and a preparation method thereof, and the polyvinyl chloride wood-plastic composite material comprises the following components in parts by weight: 80-100 parts of polyvinyl chloride, 20-30 parts of allyl silicone modified bismaleimide, 20-30 parts of nanocrystalline cellulose, 60-80 parts of wood powder, 1-2 parts of lubricant, 2-4 parts of flame retardant, 3-5 parts of ACR impact resistance agent and 3-5 parts of titanate coupling agent.
Description
Technical Field
The invention relates to the field of building materials, in particular to a polyvinyl chloride wood-plastic composite material and a preparation method thereof.
Background
The wood-plastic composite material is a novel material prepared by taking wood flour and plastic as main raw materials, has the characteristics of unique texture of raw wood, good mechanical property and dimensional stability, good water resistance, wear resistance and chemical corrosion resistance, is not afraid of worm-eating, is easy to color, has low maintenance requirement, long service life, is easy to form, can be processed for a plurality of times and the like, can solve the environmental problem caused by waste plastic, can improve the utilization rate of agricultural and forestry waste, saves materials, and simultaneously obtains industrial products with high practical value.
As an interior decoration material, a large amount of dense smoke or toxic gas generated during combustion is avoided, a large amount of black smoke and toxic and harmful gas are generated during combustion of the polyvinyl chloride wood-plastic composite material, smoke is possibly choked during fire disaster, and research on flame-retardant smoke-suppression modification of the polyvinyl chloride composite material is paid importance, and a large number of documents report the flame-retardant smoke-suppression effect at present, but the flame-retardant smoke-suppression effect is generally not ideal.
Disclosure of Invention
The invention aims to: aiming at the technical problems, the invention provides a polyvinyl chloride wood-plastic composite material and a preparation method thereof.
The technical scheme adopted is as follows:
the polyvinyl chloride wood-plastic composite material comprises the following components in parts by weight:
80-100 parts of polyvinyl chloride, 20-30 parts of allyl silicone modified bismaleimide, 20-30 parts of nanocrystalline cellulose, 60-80 parts of wood powder, 1-2 parts of lubricant, 2-4 parts of flame retardant, 3-5 parts of ACR impact resistant agent and 3-5 parts of titanate coupling agent.
Further, the composition comprises the following components in parts by weight:
100 parts of polyvinyl chloride, 25 parts of allyl silicone modified bismaleimide, 20 parts of nanocrystalline cellulose, 70 parts of wood powder, 2 parts of lubricant, 3 parts of flame retardant, 3 parts of ACR impact resistance agent and 5 parts of titanate coupling agent.
Further, the preparation method of the allyl silicone modified bismaleimide comprises the following steps:
mixing allyl silicone resin and bismaleimide under the protection of nitrogen, heating to 130-150 ℃ for reaction for 30-50min to obtain a prepolymer, defoaming the prepolymer, heating to 150-160 ℃ for curing for 1-2h, heating to 170-180 ℃ for curing for 1-2h, heating to 190-200 ℃ for curing for 1-2h, crushing the obtained solid, sieving with a 400-800 mesh sieve, and drying.
Further, the preparation method of the allyl silicone resin comprises the following steps:
adding allylalkoxysilane into cyclohexane, stirring uniformly, then dripping dilute hydrochloric acid solution, heating to 60-70 ℃ after dripping, reacting for 8-10h, heating to reflux to remove small molecular fraction, and finally distilling under reduced pressure to remove unreacted allylalkoxysilane, thus obtaining the allylsilicone resin.
Further, the allylalkoxysilane is allyltrimethoxysilane or allyltriethoxysilane.
Further, the mass ratio of the allyl silicone resin to the bismaleimide is 1:1-3.
Further, the lubricant comprises oxidized polyethylene wax and pentaerythritol tetrabenzoate, wherein the mass ratio of the oxidized polyethylene wax to the pentaerythritol tetrabenzoate is 3-5:1.
further, the flame retardant is a zinc ferrite/silicon nitride compound.
Further, the preparation method of the zinc ferrite/silicon nitride compound comprises the following steps:
s1: adding ferric nitrate and citric acid into water, stirring to dissolve completely, adding ammonia water dropwise to pH 7-8 while stirring, stirring for 5-10 hr to obtain wet gel A, suction filtering, and drying at 120-150deg.C for 8-15 hr;
s2: adding zinc nitrate and citric acid into water, stirring to dissolve completely, adding ammonia water dropwise while stirring to pH of the system to 4-5, stirring for 5-10h to obtain wet gel B, suction filtering to obtain wet gel B, and drying at 120-150deg.C for 8-15 h;
s3: mixing silica powder, dried wet gel A and wet gel B, ball milling in ethanol medium for 5-10 hr, oven drying, loading into graphite barrel with holes, and vacuumizing to 0.5X10 -4 -1×10 -4 And (3) under the pressure of MPa, filling mixed gas consisting of 4-6MPa of high-purity nitrogen and high-purity oxygen, taking mixed powder of titanium powder and carbon powder as an ignition agent, and igniting by heating a nickel-chromium wire through direct current to perform self-propagating combustion so as to form a zinc ferrite/silicon nitride compound.
The invention also provides a preparation method of the polyvinyl chloride wood-plastic composite material, which comprises the following steps:
adding wood powder, titanate coupling agent, nanocrystalline cellulose and flame retardant into a high-speed mixer for premixing treatment, adding polyvinyl chloride, allyl silicone modified bismaleimide, lubricant and ACR impact resistance agent after uniformly mixing, heating to 40-50 ℃, stirring for 20-30min, putting the mixture into a double-screw extruder for melting, blending and extruding, and cooling and drying the obtained granules to obtain the modified bismaleimide.
The invention has the beneficial effects that:
the invention provides a polyvinyl chloride wood-plastic composite material, which can improve the mechanical strength of the material after allyl silicone modified bismaleimide is added, and introduces silicon atoms, so that the carbon formation can be promoted during combustion, the carbon residue rate is improved, the zinc ferrite/silicon nitride composite material has good thermal stability as a flame retardant, zinc oxide and ferric oxide generated in the thermal decomposition process can promote carbonization of a material matrix, and form a staggered flocculent protective carbon layer on the surface together with silicon nitride particles, so that the polyvinyl chloride wood-plastic composite material is used as a protective barrier to prevent further combustion, has the effects of flame retardance and smoke suppression, can be used as a stress concentrator to induce a large number of silver lines between the matrix when external force acts, so as to absorb a large number of impact energy, and simultaneously, the stress field between the silver lines is mutually interfered, so that the end stress of the silver lines is reduced, the further development of the silver lines is hindered, and the effect of shock resistance and toughening is played.
Detailed Description
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1:
the polyvinyl chloride wood-plastic composite material comprises the following components in parts by weight:
100 parts of polyvinyl chloride, 25 parts of allyl silicone modified bismaleimide, 20 parts of nanocrystalline cellulose, 70 parts of poplar powder, 1 part of oxidized polyethylene wax, 1 part of pentaerythritol tetrabenzoate, 3 parts of flame retardant, 3 parts of ACR impact resistance agent and 5 parts of titanate coupling agent.
The preparation method of the allyl silicone modified bismaleimide comprises the following steps:
204g of allyl triethoxysilane and 252g of cyclohexane are sequentially added into a three-port bottle provided with a thermometer and a condensation reflux device, 54.8g of 1.5wt% dilute hydrochloric acid solution is slowly added dropwise after magnetic stirring, the temperature is raised to 65 ℃ after the dripping is finished for reaction for 10 hours, the temperature is raised to reflux, a water separator is adopted to separate and remove small molecular fraction hydrochloric acid, water and generated ethanol by utilizing the difference of specific gravity of the solvent under the boiling state, the process lasts for 10 hours, finally the allyl triethoxysilane remained in the system is distilled out by adopting a rotary evaporator under 120 ℃ and minus 0.09MPa, and the allyl silicone resin and N, N '-4,4' -diphenylmethane bismaleimide are prepared under the protection of nitrogen according to the mass ratio of 1:1, heating to 150 ℃ for reaction for 50min to obtain a prepolymer, defoaming the prepolymer, heating to 150 ℃ for curing for 1h, heating to 170 ℃ for curing for 1h, heating to 200 ℃ for curing for 2h, crushing the obtained solid, sieving with a 800-mesh screen, and drying.
The flame retardant is a zinc ferrite/silicon nitride compound, and the preparation method comprises the following steps:
adding 80g of ferric nitrate and 20g of citric acid into 200mL of water, stirring to dissolve completely, dropwise adding ammonia water to the system pH to 7 while stirring, continuously stirring for 10 hours after the dropwise adding to obtain wet gel A, suction-filtering the obtained wet gel A, drying at 120 ℃ for 12 hours for later use, adding 40g of zinc nitrate and 20g of citric acid into water, stirring to dissolve completely, dropwise adding ammonia water to the system pH to 5 while stirring, continuously stirring for 10 hours after the dropwise adding to obtain wet gel B, suction-filtering the obtained wet gel B, drying at 120 ℃ for 12 hours for later use, mixing 50g of silicon powder, the dried wet gel A and the wet gel B, ball-milling in an ethanol medium for 10 hours, drying, loading into a graphite barrel with holes, and vacuumizing to 1X 10 -4 And (3) under the pressure of MPa, filling mixed gas consisting of 6MPa high-purity nitrogen and high-purity oxygen, wherein the volume ratio of the high-purity nitrogen to the high-purity oxygen is 4:1, titanium powder and carbon powder are mixed according to a mass ratio of 4: the mixed powder formed by the step 1 is used as an ignition agent, and the direct current is used for heating the nickel-chromium wire to ignite for self-propagating combustion, so that a zinc ferrite/silicon nitride compound is formed.
The invention also provides a preparation method of the polyvinyl chloride wood-plastic composite material, which comprises the following steps:
adding poplar powder, titanate coupling agent, nanocrystalline cellulose and flame retardant into a high-speed mixer for premixing treatment, adding polyvinyl chloride, allyl silicone modified bismaleimide, oxidized polyethylene wax, pentaerythritol tetrabenzoate and ACR impact resistance agent after uniformly mixing, heating to 50 ℃, stirring for 30min, putting the mixture into a double-screw extruder for melt blending extrusion, and cooling and drying the obtained granules to obtain the modified polypropylene composite material.
Example 2:
the polyvinyl chloride wood-plastic composite material comprises the following components in parts by weight:
100 parts of polyvinyl chloride, 30 parts of allyl silicone modified bismaleimide, 30 parts of nanocrystalline cellulose, 80 parts of poplar powder, 1 part of oxidized polyethylene wax, 1 part of pentaerythritol tetrabenzoate, 4 parts of flame retardant, 5 parts of ACR impact resistance agent and 5 parts of titanate coupling agent.
The preparation method of the allyl silicone modified bismaleimide comprises the following steps:
204g of allyl triethoxysilane and 252g of cyclohexane are sequentially added into a three-port bottle provided with a thermometer and a condensation reflux device, 54.8g of 1.5wt% dilute hydrochloric acid solution is slowly added dropwise after magnetic stirring, the temperature is raised to 70 ℃ after the dripping is finished for reaction for 10 hours, the temperature is raised to reflux, a water separator is adopted to separate and remove small molecular fraction hydrochloric acid, water and generated ethanol by utilizing the difference of specific gravity of the solvent under the boiling state, the process lasts for 10 hours, finally the allyl triethoxysilane remained in the system is distilled out by adopting a rotary evaporator under 120 ℃ and minus 0.09MPa, and the allyl silicone resin and N, N '-4,4' -diphenylmethane bismaleimide are prepared under the protection of nitrogen according to the mass ratio of 1:3, heating to 150 ℃ for reaction for 50min to obtain a prepolymer, heating to 160 ℃ for curing for 2h, heating to 180 ℃ for curing for 2h, heating to 200 ℃ for curing for 2h after the prepolymer is defoamed, crushing the obtained solid, sieving with a 800-mesh screen, and drying.
The flame retardant is a zinc ferrite/silicon nitride compound, and the preparation method comprises the following steps:
adding 80g of ferric nitrate and 20g of citric acid into 200mL of water, stirring to dissolve completely, dropwise adding ammonia water to the system pH to 8 while stirring, continuously stirring for 10 hours after the dropwise adding to obtain wet gel A, filtering the obtained wet gel A, drying at 150 ℃ for 15 hours for later use, adding 40g of zinc nitrate and 20g of citric acid into water, stirring to dissolve completely, dropwise adding ammonia water to the system pH to 5 while stirring, continuously stirring for 10 hours after the dropwise adding to obtain wet gel B, drying at 150 ℃ for later use after the dropwise adding to obtain wet gel B, mixing 50g of silicon powder, the dried wet gel A and the wet gel B, ball-milling for 10 hours in an ethanol medium, drying, loading into a graphite barrel with holes, and vacuumizing to 1X 10 -4 MPa, and 6MPa high-purity nitrogen and high-purity oxygen are filled againThe volume ratio of the high-purity nitrogen to the high-purity oxygen is 4:1, titanium powder and carbon powder are mixed according to a mass ratio of 4: the mixed powder formed by the step 1 is used as an ignition agent, and the direct current is used for heating the nickel-chromium wire to ignite for self-propagating combustion, so that a zinc ferrite/silicon nitride compound is formed.
The invention also provides a preparation method of the polyvinyl chloride wood-plastic composite material, which comprises the following steps:
adding poplar powder, titanate coupling agent, nanocrystalline cellulose and flame retardant into a high-speed mixer for premixing treatment, adding polyvinyl chloride, allyl silicone modified bismaleimide, oxidized polyethylene wax, pentaerythritol tetrabenzoate and ACR impact resistance agent after uniformly mixing, heating to 50 ℃, stirring for 30min, putting the mixture into a double-screw extruder for melt blending extrusion, and cooling and drying the obtained granules to obtain the modified polypropylene composite material.
Example 3:
the polyvinyl chloride wood-plastic composite material comprises the following components in parts by weight:
80 parts of polyvinyl chloride, 20 parts of allyl silicone modified bismaleimide, 20 parts of nanocrystalline cellulose, 60 parts of poplar powder, 1 part of oxidized polyethylene wax, 1 part of pentaerythritol tetrabenzoate, 2 parts of flame retardant, 3 parts of ACR impact resistance agent and 3 parts of titanate coupling agent.
The preparation method of the allyl silicone modified bismaleimide comprises the following steps:
204g of allyl triethoxysilane and 252g of cyclohexane are sequentially added into a three-port bottle provided with a thermometer and a condensation reflux device, 54.8g of 1.5wt% dilute hydrochloric acid solution is slowly added dropwise after magnetic stirring, the temperature is raised to 60 ℃ for reaction for 8 hours after the dripping, the temperature is raised to reflux, a water separator is adopted to separate and remove small molecular fraction hydrochloric acid, water and generated ethanol by utilizing the difference of specific gravity of the solvent under the boiling state, the process lasts for 10 hours, finally the allyl triethoxysilane remained in the system is distilled out by adopting a rotary evaporator under 120 ℃ and minus 0.09MPa, so that allyl silicone resin can be obtained, and the allyl silicone resin and N, N '-4,4' -diphenylmethane bismaleimide are subjected to the mass ratio of 1 under the protection of nitrogen: 1, heating to 130 ℃ for reaction for 30min to obtain a prepolymer, defoaming the prepolymer, heating to 150 ℃ for curing for 1h, heating to 170 ℃ for curing for 1h, heating to 190 ℃ for curing for 1h, crushing the obtained solid, sieving with a 400-mesh sieve, and drying.
The flame retardant is a zinc ferrite/silicon nitride compound, and the preparation method comprises the following steps:
adding 80g of ferric nitrate and 20g of citric acid into 200mL of water, stirring to dissolve completely, dropwise adding ammonia water to the system pH to 7 while stirring, continuously stirring for 5 hours after dropwise adding to obtain wet gel A, suction-filtering the obtained wet gel A, drying at 120 ℃ for 8 hours for later use, adding 40g of zinc nitrate and 20g of citric acid into water, stirring to dissolve completely, dropwise adding ammonia water to the system pH to 4 while stirring, continuously stirring for 5 hours after dropwise adding to obtain wet gel B, suction-filtering the obtained wet gel B, drying at 120 ℃ for 8 hours for later use, mixing 50g of silicon powder, the dried wet gel A and the wet gel B, ball-milling in an ethanol medium for 5 hours, drying, loading into a graphite barrel with holes, and vacuumizing to 0.5X10 -4 4MPa, and 4MPa of mixed gas consisting of high-purity nitrogen and high-purity oxygen is filled, wherein the volume ratio of the high-purity nitrogen to the high-purity oxygen is 4:1, titanium powder and carbon powder are mixed according to a mass ratio of 4: the mixed powder formed by the step 1 is used as an ignition agent, and the direct current is used for heating the nickel-chromium wire to ignite for self-propagating combustion, so that a zinc ferrite/silicon nitride compound is formed.
The invention also provides a preparation method of the polyvinyl chloride wood-plastic composite material, which comprises the following steps:
adding poplar powder, titanate coupling agent, nanocrystalline cellulose and flame retardant into a high-speed mixer for premixing treatment, adding polyvinyl chloride, allyl silicone modified bismaleimide, oxidized polyethylene wax, pentaerythritol tetrabenzoate and ACR impact resistance agent after uniformly mixing, heating to 40 ℃, stirring for 20min, putting the mixture into a double-screw extruder for melt blending extrusion, and cooling and drying the obtained granules to obtain the modified polypropylene composite material.
Example 4:
the polyvinyl chloride wood-plastic composite material comprises the following components in parts by weight:
100 parts of polyvinyl chloride, 20 parts of allyl silicone modified bismaleimide, 30 parts of nanocrystalline cellulose, 60 parts of poplar powder, 1 part of oxidized polyethylene wax, 1 part of pentaerythritol tetrabenzoate, 4 parts of flame retardant, 3 parts of ACR impact resistance agent and 5 parts of titanate coupling agent.
The preparation method of the allyl silicone modified bismaleimide comprises the following steps:
204g of allyl triethoxysilane and 252g of cyclohexane are sequentially added into a three-port bottle provided with a thermometer and a condensation reflux device, 54.8g of 1.5wt% dilute hydrochloric acid solution is slowly added dropwise after magnetic stirring, the temperature is raised to 60 ℃ for reaction for 10 hours after the dripping, the temperature is raised to reflux, a water separator is adopted to separate and remove small molecular fraction hydrochloric acid, water and generated ethanol by utilizing the difference of specific gravity of the solvent under the boiling state, the process lasts for 10 hours, finally the allyl triethoxysilane remained in the system is distilled out by adopting a rotary evaporator under 120 ℃ and minus 0.09MPa, so that allyl silicone resin can be obtained, and the allyl silicone resin and N, N '-4,4' -diphenylmethane bismaleimide are subjected to the mass ratio of 1 under the protection of nitrogen: 1, heating to 150 ℃ for reaction for 30min to obtain a prepolymer, defoaming the prepolymer, heating to 160 ℃ for curing for 1h, heating to 180 ℃ for curing for 1h, heating to 200 ℃ for curing for 1h, crushing the obtained solid, sieving with a 800-mesh screen, and drying.
The flame retardant is a zinc ferrite/silicon nitride compound, and the preparation method comprises the following steps:
adding 80g of ferric nitrate and 20g of citric acid into 200mL of water, stirring to dissolve completely, dropwise adding ammonia water to the system pH to 7 while stirring, continuously stirring for 10 hours after the dropwise adding to obtain wet gel A, suction-filtering the obtained wet gel A, drying at 120 ℃ for 15 hours for later use, adding 40g of zinc nitrate and 20g of citric acid into water, stirring to dissolve completely, dropwise adding ammonia water to the system pH to 4 while stirring, continuously stirring for 10 hours after the dropwise adding to obtain wet gel B, suction-filtering the obtained wet gel B, drying at 120 ℃ for later use, mixing 50g of silicon powder, the dried wet gel A and the wet gel B, ball-milling in an ethanol medium for 5 hours, drying, loading into a graphite barrel with holes, and vacuumizing to 1X 10 -4 4MPa, and 4MPa of mixed gas consisting of high-purity nitrogen and high-purity oxygen is filled, wherein the volume ratio of the high-purity nitrogen to the high-purity oxygen is 4:1, titanium powder and carbon powder are mixed according to a mass ratio of 4:1 as an ignition agent, and igniting a direct-current heating nickel-chromium wire to perform self-propagating combustion to form a zinc ferrite/silicon nitride compound。
The invention also provides a preparation method of the polyvinyl chloride wood-plastic composite material, which comprises the following steps:
adding poplar powder, titanate coupling agent, nanocrystalline cellulose and flame retardant into a high-speed mixer for premixing treatment, adding polyvinyl chloride, allyl silicone modified bismaleimide, oxidized polyethylene wax, pentaerythritol tetrabenzoate and ACR impact resistance agent after uniformly mixing, heating to 50 ℃, stirring for 20min, putting the mixture into a double-screw extruder for melt blending extrusion, and cooling and drying the obtained granules to obtain the modified polypropylene composite material.
Example 5:
the polyvinyl chloride wood-plastic composite material comprises the following components in parts by weight:
80 parts of polyvinyl chloride, 30 parts of allyl silicone modified bismaleimide, 20 parts of nanocrystalline cellulose, 80 parts of poplar powder, 1 part of oxidized polyethylene wax, 1 part of pentaerythritol tetrabenzoate, 2 parts of flame retardant, 5 parts of ACR impact resistance agent and 3 parts of titanate coupling agent.
The preparation method of the allyl silicone modified bismaleimide comprises the following steps:
204g of allyl triethoxysilane and 252g of cyclohexane are sequentially added into a three-port bottle provided with a thermometer and a condensation reflux device, 54.8g of 1.5wt% dilute hydrochloric acid solution is slowly added dropwise after magnetic stirring, the temperature is raised to 70 ℃ for reaction for 8 hours after the dripping, the temperature is raised to reflux, a water separator is adopted to separate and remove small molecular fraction hydrochloric acid, water and generated ethanol by utilizing the difference of specific gravity of the solvent under the boiling state, the process lasts for 10 hours, finally the allyl triethoxysilane remained in the system is distilled out by adopting a rotary evaporator under 120 ℃ and minus 0.09MPa, so that allyl silicone resin can be obtained, and the allyl silicone resin and N, N '-4,4' -diphenylmethane bismaleimide are subjected to the mass ratio of 1 under the protection of nitrogen: 3, heating to 130 ℃ for reaction for 50min to obtain a prepolymer, defoaming the prepolymer, heating to 150 ℃ for curing for 2h, heating to 170 ℃ for curing for 2h, heating to 190 ℃ for curing for 2h, crushing the obtained solid, sieving with a 400-mesh sieve, and drying.
The flame retardant is a zinc ferrite/silicon nitride compound, and the preparation method comprises the following steps:
adding 80g of ferric nitrate and 20g of citric acid into 200mL of water, stirring to dissolve completely, dropwise adding ammonia water to the system pH to 8 while stirring, continuously stirring for 5 hours after dropwise adding to obtain wet gel A, suction-filtering the obtained wet gel A, drying at 150 ℃ for 8 hours for later use, adding 40g of zinc nitrate and 20g of citric acid into water, stirring to dissolve completely, dropwise adding ammonia water to the system pH to 5 while stirring, continuously stirring for 5 hours after dropwise adding to obtain wet gel B, suction-filtering the obtained wet gel B, drying at 150 ℃ for 8 hours for later use, mixing 50g of silicon powder, the dried wet gel A and the wet gel B, ball-milling in an ethanol medium for 10 hours, drying, loading into a graphite barrel with holes, and vacuumizing to 0.5X10 -4 And (3) under the pressure of MPa, filling mixed gas consisting of 6MPa high-purity nitrogen and high-purity oxygen, wherein the volume ratio of the high-purity nitrogen to the high-purity oxygen is 4:1, titanium powder and carbon powder are mixed according to a mass ratio of 4: the mixed powder formed by the step 1 is used as an ignition agent, and the direct current is used for heating the nickel-chromium wire to ignite for self-propagating combustion, so that a zinc ferrite/silicon nitride compound is formed.
The invention also provides a preparation method of the polyvinyl chloride wood-plastic composite material, which comprises the following steps:
adding poplar powder, titanate coupling agent, nanocrystalline cellulose and flame retardant into a high-speed mixer for premixing treatment, adding polyvinyl chloride, allyl silicone modified bismaleimide, oxidized polyethylene wax, pentaerythritol tetrabenzoate and ACR impact resistance agent after uniformly mixing, heating to 40 ℃, stirring for 30min, putting the mixture into a double-screw extruder for melt blending extrusion, and cooling and drying the obtained granules to obtain the modified polypropylene composite material.
Comparative example 1
Comparative example 1 is substantially the same as example 1 except that no allylsilicone modified bismaleimide was added.
Comparative example 2
Comparative example 2 is substantially the same as example 1 except that N, N '-4,4' -diphenylmethane bismaleimide of equal mass is directly added instead of the prepared allylsilicone resin modified bismaleimide.
Comparative example 3
Comparative example 3 is substantially the same as example 1 except that no flame retardant was added.
Comparative example 4
Comparative example 4 is essentially the same as example 1, except that the zinc ferrite/silicon nitride composite is replaced by commercially available zinc ferrite (brand: sandwiches organism).
Performance test:
the polyvinyl chloride wood-plastic composite materials prepared in examples 1 to 5 and comparative examples 1 to 4 of the present invention were used as test samples for performance test, wherein the bending performance was tested according to GB/T9341-2000; tensile strength was measured according to GB/T1040-2006; impact properties were measured according to GB/T1043-1993; hardness testing was conducted in accordance with GB/T9342-1998, and the test results are shown in Table 1 below:
table 1:
as shown in the table 1, the polyvinyl chloride wood-plastic composite material prepared by the invention has excellent mechanical properties, high limiting oxygen index, low smoke density and excellent flame-retardant and smoke-suppressing effects.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (6)
1. The polyvinyl chloride wood-plastic composite material is characterized by comprising the following components in parts by weight:
80-100 parts of polyvinyl chloride, 20-30 parts of allyl silicone modified bismaleimide, 20-30 parts of nanocrystalline cellulose, 60-80 parts of wood powder, 1-2 parts of lubricant, 2-4 parts of flame retardant, 3-5 parts of ACR impact resistant agent and 3-5 parts of titanate coupling agent;
the preparation method of the allyl silicone modified bismaleimide comprises the following steps:
mixing allyl silicone resin and bismaleimide under the protection of nitrogen, heating to 130-150 ℃ for reaction for 30-50min to obtain a prepolymer, heating to 150-160 ℃ for curing for 1-2h after the prepolymer is defoamed, heating to 170-180 ℃ for curing for 1-2h, heating to 190-200 ℃ for curing for 1-2h, crushing the obtained solid, sieving with a 400-800 mesh sieve, and drying;
the preparation method of the allyl silicone resin comprises the following steps:
adding allylalkoxysilane into cyclohexane, stirring uniformly, then dropwise adding a dilute hydrochloric acid solution, heating to 60-70 ℃ after dripping, reacting for 8-10h, heating to reflux to remove small molecular fraction, and finally distilling under reduced pressure to remove unreacted allylalkoxysilane to obtain allylsilicone resin;
the flame retardant is a zinc ferrite/silicon nitride compound;
the preparation method of the zinc ferrite/silicon nitride compound comprises the following steps:
s1: adding ferric nitrate and citric acid into water, stirring to dissolve completely, adding ammonia water dropwise to pH 7-8 while stirring, stirring for 5-10 hr to obtain wet gel A, suction filtering, and drying at 120-150deg.C for 8-15 hr;
s2: adding zinc nitrate and citric acid into water, stirring to dissolve completely, adding ammonia water dropwise while stirring to pH of the system to 4-5, stirring for 5-10h to obtain wet gel B, suction filtering to obtain wet gel B, and drying at 120-150deg.C for 8-15 h;
s3: mixing silica powder, dried wet gel A and wet gel B, ball milling in ethanol medium for 5-10 hr, oven drying, loading into graphite barrel with holes, and vacuumizing to 0.5X10 -4 -1×10 -4 And (3) under the pressure of MPa, filling mixed gas consisting of 4-6MPa of high-purity nitrogen and high-purity oxygen, taking mixed powder of titanium powder and carbon powder as an ignition agent, and igniting by heating a nickel-chromium wire through direct current to perform self-propagating combustion so as to form a zinc ferrite/silicon nitride compound.
2. The polyvinyl chloride wood-plastic composite material according to claim 1, which is characterized by comprising the following components in parts by weight:
100 parts of polyvinyl chloride, 25 parts of allyl silicone modified bismaleimide, 20 parts of nanocrystalline cellulose, 70 parts of wood powder, 2 parts of lubricant, 3 parts of flame retardant, 3 parts of ACR impact resistance agent and 5 parts of titanate coupling agent.
3. The polyvinyl chloride wood-plastic composite of claim 1, wherein the allylalkoxysilane is allyltrimethoxysilane or allyltriethoxysilane.
4. The polyvinyl chloride wood-plastic composite according to claim 1, wherein the mass ratio of the allyl silicone to the bismaleimide is 1:1-3.
5. The polyvinyl chloride wood-plastic composite according to claim 1, wherein the lubricant comprises oxidized polyethylene wax and pentaerythritol tetrabenzoate, and the mass ratio of the oxidized polyethylene wax to the pentaerythritol tetrabenzoate is 3-5:1.
6. a method for preparing the polyvinyl chloride wood-plastic composite material according to any one of claims 1 to 5, which is characterized in that wood powder, titanate coupling agent, nanocrystalline cellulose and flame retardant are added into a high-speed mixer for premixing treatment, polyvinyl chloride, allyl silicone modified bismaleimide, lubricant and ACR impact resistant agent are added after uniform mixing, the mixture is heated to 40 to 50 ℃, stirred for 20 to 30 minutes, and then the mixture is put into a double-screw extruder for melt blending extrusion, and the obtained granules are cooled and dried, thus obtaining the polyvinyl chloride wood-plastic composite material.
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| WO2021128102A1 (en) * | 2019-12-25 | 2021-07-01 | 宁波禾隆新材料股份有限公司 | Flame-retardant wood-plastic surface layer composite, and method for preparing wood-plastic composite material having flame-retardant wood-plastic surface composite |
| CN114656729A (en) * | 2022-03-18 | 2022-06-24 | 金发科技股份有限公司 | High-flame-retardant low-temperature-resistant polyvinyl chloride composition and preparation method and application thereof |
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| EP0161432A2 (en) * | 1984-05-14 | 1985-11-21 | AlliedSignal Inc. | Flame retardant polyamide fiber and carpet |
| CN101142263A (en) * | 2005-03-17 | 2008-03-12 | 路博润高级材料公司 | Nanoparticle/Vinyl Polymer Composites |
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