CN114106537A - Degradable PPC composite board and preparation method thereof - Google Patents
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Abstract
The invention discloses a degradable PPC composite board and a preparation method thereof; the preparation method comprises the following steps: s1: grafting L-lactide on the surfaces of silicon dioxide and sisal fibers, and uniformly mixing the L-lactide with basalt fibers and polylactic acid to obtain a polylactic acid layer; s2: uniformly mixing the carbon dioxide base, the polylactic acid and other additives to obtain a carbon dioxide base layer; s3: grafting citric acid on the surface of lignin, introducing a phosphorus element, and uniformly mixing with wood fiber to obtain a lignin layer; s4: pre-pressing, hot-drying and hot-rolling the polylactic acid layer, the carbon dioxide base layer and the lignin layer to obtain the PPC composite board; the PCC composite board prepared by the invention is formed by hot pressing three layers of boards, has excellent mechanical strength, thermal stability and flame retardance, is made of degradable materials, can protect the environment, improves the global greenhouse effect, accords with the national policy, has strong equipment universality, and can be produced by the original equipment for producing PP and PC materials.
Description
Technical Field
The invention relates to the technical field of composite boards, in particular to a degradable PPC composite board and a preparation method thereof.
Background
The release of plastic tokens is forbidden, disposable hotel tools such as toothbrushes, combs and other plastic products are forbidden, the development of full-biodegradable high-strength injection molding special materials is urgent, and most of the existing markets mainly use common PP plastics which are not degradable, and the recycled finished products are large, so that the environmental pollution is caused.
Disclosure of Invention
The invention aims to provide a degradable PPC composite board and a preparation method thereof, and aims to solve the problems in the background art.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of a degradable PPC composite board comprises the following steps:
s1: dissolving silicon dioxide and sisal fibers in a toluene solution, uniformly mixing, heating to 100 ℃, introducing nitrogen, adding the toluene solution of L-lactide and stannous octoate, reacting at 160 ℃ for 12-48h, performing suction filtration, washing with trichloromethane, drying, adding a nano cellulose ethanol solution with the pH value of 4-5, uniformly mixing, continuously adding a silane coupling agent and basalt fibers, uniformly mixing, reacting for 2-3h, washing with water, dissolving in an acetamide solution, uniformly mixing with polylactic acid at 60-70 ℃, performing vacuum defoaming, drying, uniformly mixing with a composite compatilizer, extruding by an extruder, granulating, and performing hot pressing to obtain a polylactic acid double-screw layer;
s2: uniformly mixing carbon dioxide base, polylactic acid, a butanediol adipate-butanediol terephthalate copolymer, a BASF chain extender, a dispersing agent, a lubricating agent and a filler, and carrying out extrusion, grain cutting and hot pressing by a double-screw extruder to obtain a carbon dioxide base layer;
s3: dissolving sodium hypophosphite in a citric acid aqueous solution, adding lignin nanoparticles, drying, standing for 12-15h, drying at 60 ℃ for 45h, standing at 130 ℃ for 5h, centrifuging for 5-10min, washing with water, drying, adding di (2-ethylhexyl) phosphate into a mixed ethanol solution, reacting for 5-8h, carrying out reduced pressure distillation, carrying out suction filtration, washing with water, drying, dissolving in water, adding 4, 4' -diaminodiphenylmethane, mixing uniformly, adding dried wood fibers, reacting for 5-10min, and carrying out extrusion, grain cutting and hot pressing by using a double-screw extruder to obtain a lignin layer;
s4: and pre-pressing, hot-drying and hot-rolling the polylactic acid layer, the carbon dioxide base layer and the lignin layer to obtain the PPC composite board.
Further, before use, the sisal fibers are soaked in an aqueous solution of sodium hydroxide, reacted for 1-2 hours, washed by water, kept stand, dried and dried;
before being used, the basalt fiber is soaked in a mixed solution of a graphene oxide aqueous solution and a polyethylene glycol aqueous solution, reacted for 0.5-1h, and dried.
Further, the preparation process of the composite compatilizer comprises the following steps: uniformly mixing chloroform, dimethyl sulfoxide and polyethylene glycol monomethyl ether, adding acetic anhydride, precipitating with glacial ethyl ether, dissolving with chloroform, repeating for three times, filtering, and drying to obtain hydroformylation polyethylene glycol monomethyl ether;
dissolving chitosan in a mixed solution of acetic acid and methanol, adding hydroformylation polyethylene glycol monomethyl ether, reacting for 24-30h, adding sodium cyanoborohydride, reacting for 40-50h, dialyzing in water for 48h, centrifuging, drying and grinding to obtain modified chitosan, dissolving polylactic acid in an N, N-dimethylformamide solution, slowly dropwise adding toluene diisocyanate, heating to 50-60 ℃, introducing nitrogen, reacting for 0.5h, adding the N, N-dimethylformamide solution of the modified chitosan, reacting for 8-10h at 90-100 ℃, precipitating with ice water, performing suction filtration, washing, drying, extracting with an acetone solution for 48h, and drying.
Further, the carbon dioxide-based layer requires materials including, by weight: 5-10 parts of carbon dioxide base, 20-25 parts of polylactic acid, 60-70 parts of butanediol adipate-butanediol terephthalate copolymer, 0.1-0.3 part of BASF chain extender, 0.2-0.3 part of dispersant, 0.1-0.3 part of lubricant and 3-5 parts of filler.
Further, the temperature of a cylinder of the double-screw extruder is 160-180 ℃, the temperature of a die head is 170 ℃, and the length-diameter ratio is 52: 1, cooling by air cooling.
Further, the silane coupling agent is gamma-aminopropyltriethoxysilane.
Further, the dispersant is ethylene bis stearamide; the lubricant is one or more of polyethylene wax, calcium stearate, paraffin and stearic acid amide; the filler is one or more of calcium carbonate and talcum powder.
Further, the PCC composite board is prepared by the preparation method of the degradable PPC composite board.
Further, the materials required for the polylactic acid layer include, by weight: 10-20 parts of silicon dioxide, 10-20 parts of sisal fiber, 300 parts of toluene 200-lactide, 10-20 parts of L-lactide, 0.1-0.5 part of stannous octoate, 5-15 parts of nano-cellulose, 1-5 parts of silane coupling agent, 8-16 parts of basalt fiber, 20-40 parts of acetamide, 5-15 parts of polylactic acid and 1-8 parts of composite compatilizer.
Further, the materials required by the composite compatilizer comprise, by weight: 40-60 parts of chloroform, 10-20 parts of dimethyl sulfoxide, 5-15 parts of polyethylene glycol monomethyl ether, 10-15 parts of acetic anhydride, 20-40 parts of glacial ethyl ether, 1-5 parts of chitosan, 10-20 parts of acetic acid, 10-20 parts of methanol, 8-15 parts of hydroformylation polyethylene glycol monomethyl ether, 1-5 parts of sodium cyanoborohydride, 40-60 parts of N, N-dimethylformamide, 5-15 parts of modified chitosan, 5-8 parts of polylactic acid and 1-10 parts of toluene diisocyanate.
Further, the materials required by the lignin layer comprise, by weight: 1-5 parts of sodium hypophosphite, 5-20 parts of citric acid, 1-5 parts of lignin, 20-30 parts of ethanol, 10-20 parts of di (2-ethylhexyl) phosphate, 20-30 parts of water, 1-5 parts of 4, 4' -diaminodiphenylmethane and 5-10 parts of wood fiber.
Compared with the prior art, the invention has the following beneficial effects: (1) the L-lactide is grafted on the surface of the silicon dioxide, so that the silicon dioxide can be uniformly dispersed in the polylactic acid, the thermal stability of the composite board is improved, the degradation rate of the polylactic acid is delayed, and the service life of the composite board is prolonged. The alkali treatment of the sisal fiber can remove small molecular substances on the surface, then the L-lactide is grafted on the surface of the sisal fiber, the compatibility of the sisal fiber with polylactic acid and basalt fiber is improved, the bending strength of the composite board is enhanced, the sisal fiber is fibrillated, the addition of the L-lactide can generate small molecular weight polylactic acid on the surface of the sisal fiber, the contact area between the polylactic acid can be increased when the polylactic acid is mixed with the polylactic acid, the sisal fiber and the basalt fiber are mixed to fill the polylactic acid, the polylactic acid and the sisal fiber can generate a synergistic effect, the basalt fiber can delay the fracture of the composite board when the composite board is under external stress, thereby avoiding the composite board from being damaged, the compatibility of the basalt fiber and the polylactic acid is good, no pore exists in the prepared board, the water absorption rate of the composite board can be reduced, and the thermal stability and the comprehensive performance of the composite board can be enhanced by adding the basalt fibers.
(2) The method has the advantages that the graphene oxide aqueous solution is used for treating the basalt fiber, the binding property of the basalt fiber and the polylactic acid is improved, the roughness of the surface of the composite board is improved, the polyethylene glycol can reduce the agglomeration of the graphene oxide, the addition of the graphene oxide can improve the impact strength of the composite board, the holes in the surface of the composite board are reduced, and the mechanical property of the composite board is further improved.
(3) The preparation of the composite compatilizer is that after the surface of chitosan is grafted with hydroformylation polyethylene glycol monomethyl ether, the surface of chitosan is grafted with polyacetic acid again, firstly, polyethylene glycol is subjected to hydroformylation reaction, so that the cross-linking phenomenon can be avoided, sodium cyanoborohydride can reduce imine into amino, so that the grafted chitosan is more stable, and the grafting of the polyacetic acid is facilitated.
(4) After lignin is modified, the lignin is mixed with wood fiber to prepare a lignin layer, so that the flame retardance of the composite board is enhanced, citric acid is grafted on the surface of the lignin and generates chelation with phosphorus to coat the phosphorus to enhance the stability of the performance of the phosphorus, meanwhile, the introduction of the phosphorus does not influence the mechanical strength of the composite board, the surface of the lignin layer can be roughened due to the addition of the phosphorus, the tightness between fibers can be enhanced, the distribution of the phosphorus in the board is wide, when the composite board is heated, the phosphorus can expand to block air and combustible parts and is difficult to decompose by heating, the glass transition temperature of the composite board is increased, so that the flame retardance of the composite board is improved, in addition, the lignin contains machine oxides of non-metal elements such as Si and the like, and after the phosphorus is introduced, a combined effect can be achieved, and the heat release rate of the composite board is reduced, further enhancing the flame retardance of the composite board.
The PCC composite board prepared by the invention is formed by hot pressing three layers of boards, has excellent mechanical strength, thermal stability and flame retardance, is made of degradable materials, can protect the environment, improves the global greenhouse effect, accords with the national policy, has strong equipment universality, and can be produced by the original equipment for producing PP and PC materials.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1: s1: soaking sisal fibers in an aqueous solution of 18% sodium hydroxide, reacting for 1h, washing with water, standing, airing and drying;
s2: uniformly mixing 0.1g/L aqueous solution of graphene oxide and 0.0005g/L aqueous solution of polyethylene glycol, reacting at 50 ℃ for 24h, standing to room temperature, centrifuging for 5min, washing with water, drying, dissolving in water, soaking basalt fiber in the solution, and drying;
s3: uniformly mixing 20 parts of chloroform, 10 parts of dimethyl sulfoxide and 5 parts of polyethylene glycol monomethyl ether, adding 10 parts of acetic anhydride, precipitating with 20 parts of glacial ethyl ether, dissolving with 20 parts of chloroform, repeating the steps for three times, and performing suction filtration and drying to obtain hydroformylation polyethylene glycol monomethyl ether;
dissolving 1 part of chitosan in a mixed solution of 10 parts of acetic acid and 10 parts of methanol, adding 8 parts of hydroformylation polyethylene glycol monomethyl ether, reacting for 24 hours, adding 1 part of sodium cyanoborohydride, reacting for 40 hours, dialyzing in water, reacting for 48 hours, centrifuging, drying and grinding to obtain modified chitosan, dissolving 5 parts of polylactic acid in 40 parts of N, N-dimethylformamide solution, slowly dropwise adding 1 part of toluene diisocyanate, heating to 50 ℃, introducing nitrogen, reacting for 0.5 hour, adding 5 parts of N, N-dimethylformamide solution of modified chitosan, reacting for 8-10 hours at 90 ℃, precipitating, filtering, washing and drying by using ice water, extracting for 48 hours by using an acetone solution, and drying to obtain the composite compatilizer;
s4: dissolving 10 parts of silicon dioxide and 10 parts of dried sisal fibers in 200 parts of toluene solution, uniformly mixing, heating to 100 ℃, introducing nitrogen, adding 10 parts of toluene solution of L-lactide and 0.1 part of stannous octoate, reacting at 160 ℃ for 12 hours, performing suction filtration, washing with trichloromethane, drying, adding 5 parts of nano cellulose ethanol solution with the pH value of 4, uniformly mixing, continuously adding 1 part of gamma-aminopropyltriethoxysilane and 8 parts of dried basalt fibers, uniformly mixing, reacting for 2 hours, washing with water, dissolving in 20 parts of acetamide solution, uniformly mixing with 5 parts of polylactic acid at 60 ℃, performing deaeration in vacuum, uniformly mixing with 1 part of composite compatilizer after drying, and performing extrusion, grain cutting and hot pressing by using a double-screw extruder to obtain a polylactic acid layer;
s5: uniformly mixing 5 parts of carbon dioxide base, 20 parts of polylactic acid, 60 parts of butanediol adipate-butanediol terephthalate copolymer, 0.1 part of BASF chain extender, 0.2 part of ethylene bis stearamide, 0.1 part of calcium stearate and 3 parts of talcum powder, and extruding, granulating and hot-pressing by using a double-screw extruder to obtain a carbon dioxide base layer;
s6: dissolving 1 part of sodium hypophosphite into an aqueous solution of 5 parts of citric acid, adding 1 part of lignin nanoparticles, drying, standing for 12h, drying at 60 ℃ for 45h, standing at 130 ℃ for 5h, centrifuging for 5min, washing with water, drying, mixing with 20 parts of an ethanol solution, adding 10 parts of di (2-ethylhexyl) phosphate, reacting for 5h, carrying out reduced pressure distillation, carrying out suction filtration, washing with water, drying, dissolving in 20 parts of water, adding 1 part of 4, 4' -diaminodiphenylmethane, mixing uniformly, adding 5 parts of dried wood fibers, reacting for 5min, and carrying out extrusion, grain cutting and hot pressing by using a double-screw extruder to obtain a lignin layer;
s7: and pre-pressing, hot-drying and hot-rolling the polylactic acid layer, the carbon dioxide base layer and the lignin layer to obtain the PPC composite board.
The temperature of a charging barrel of the double-screw extruder is 160 ℃, the temperature of a die head is 170 ℃, and the length-diameter ratio is 52: 1, cooling by air cooling.
Example 2: s1: soaking sisal fibers in an aqueous solution of 18% sodium hydroxide, reacting for 1.5h, washing with water, standing, airing and drying;
s2: uniformly mixing 0.1g/L aqueous solution of graphene oxide and 0.0005g/L aqueous solution of polyethylene glycol, reacting at 55 ℃ for 24h, standing to room temperature, centrifuging for 8min, washing with water, drying, dissolving in water, soaking basalt fiber in the solution, and drying;
s3: uniformly mixing 25 parts of chloroform, 15 parts of dimethyl sulfoxide and 10 parts of polyethylene glycol monomethyl ether, adding 12 parts of acetic anhydride, precipitating with 30 parts of glacial ethyl ether, dissolving with 25 parts of chloroform, repeating the steps for three times, and performing suction filtration and drying to obtain hydroformylation polyethylene glycol monomethyl ether;
dissolving 3 parts of chitosan into a mixed solution of 15 parts of acetic acid and 15 parts of methanol, adding 10 parts of hydroformylation polyethylene glycol monomethyl ether, reacting for 28 hours, adding 2 parts of sodium cyanoborohydride, reacting for 45 hours, dialyzing in water, reacting for 48 hours, centrifuging, drying and grinding to obtain modified chitosan, dissolving 6 parts of polylactic acid into 50 parts of N, N-dimethylformamide solution, slowly dropwise adding 8 parts of toluene diisocyanate, heating to 55 ℃, introducing nitrogen, reacting for 0.5 hour, adding 10 parts of N, N-dimethylformamide solution of modified chitosan, reacting for 8-10 hours at 95 ℃, precipitating, filtering, washing and drying by using ice water, extracting for 48 hours by using an acetone solution, and drying to obtain the composite compatilizer;
s4: dissolving 15 parts of silicon dioxide and 15 parts of dried sisal fibers in 250 parts of toluene solution, uniformly mixing, heating to 100 ℃, introducing nitrogen, adding 15 parts of toluene solution of L-lactide and 0.3 part of stannous octoate, reacting at 160 ℃ for 30 hours, performing suction filtration, washing with trichloromethane, drying, adding 10 parts of nano cellulose ethanol solution with the pH value of 4, uniformly mixing, continuously adding 3 parts of gamma-aminopropyltriethoxysilane and 13 parts of dried basalt fibers, uniformly mixing, reacting for 2.5 hours, washing with water, dissolving in 30 parts of acetamide solution, uniformly mixing with 10 parts of polylactic acid at 65 ℃, performing vacuum deaeration, drying, uniformly mixing with 5 parts of composite compatilizer, and performing extrusion, grain cutting and hot pressing by using a double-screw extruder to obtain a polylactic acid layer;
s5: uniformly mixing 8 parts of carbon dioxide base, 22 parts of polylactic acid, 65 parts of butanediol adipate-butanediol terephthalate copolymer, 0.2 part of BASF chain extender, 0.25 part of ethylene bis stearamide, 0.2 part of calcium stearate and 4 parts of talcum powder, and extruding, granulating and hot-pressing by using a double-screw extruder to obtain a carbon dioxide base layer;
s6: dissolving 3 parts of sodium hypophosphite in 12 parts of citric acid aqueous solution, adding 3 parts of lignin nanoparticles, drying, standing for 13h, drying at 60 ℃ for 45h, standing at 130 ℃ for 5h, centrifuging for 8min, washing with water, drying, mixing with 25 parts of ethanol solution, adding 15 parts of di (2-ethylhexyl) phosphate, reacting for 6h, distilling under reduced pressure, filtering, washing with water, drying, dissolving in 25 parts of water, adding 3 parts of 4, 4' -diaminodiphenylmethane, mixing uniformly, adding 8 parts of dried wood fiber, reacting for 8min, and extruding, granulating and hot-pressing by using a double-screw extruder to obtain a lignin layer;
s7: and pre-pressing, hot-drying and hot-rolling the polylactic acid layer, the carbon dioxide base layer and the lignin layer to obtain the PPC composite board.
The temperature of the double-screw extruder barrel is 170 ℃, the temperature of the die head is 170 ℃, and the length-diameter ratio is 52: 1, cooling by air cooling.
Example 3: s1: soaking sisal fibers in an aqueous solution of 18 sodium hydroxide, reacting for 2 hours, washing with water, standing, airing and drying;
s2: uniformly mixing 0.1g/L aqueous solution of graphene oxide and 0.0005g/L aqueous solution of polyethylene glycol, reacting at 60 ℃ for 24h, standing to room temperature, centrifuging for 10min, washing with water, drying, dissolving in water, soaking basalt fiber in the solution, and drying;
s3: uniformly mixing 30 parts of chloroform, 20 parts of dimethyl sulfoxide and 15 parts of polyethylene glycol monomethyl ether, adding 15 parts of acetic anhydride, precipitating with 40 parts of glacial ethyl ether, dissolving with 30 parts of chloroform, repeating the steps for three times, and performing suction filtration and drying to obtain hydroformylation polyethylene glycol monomethyl ether;
dissolving 5 parts of chitosan into a mixed solution of 20 parts of acetic acid and 20 parts of methanol, adding 15 parts of hydroformylation polyethylene glycol monomethyl ether, reacting for 30 hours, adding 5 parts of sodium cyanoborohydride, reacting for 50 hours, carrying out dialysis reaction in water for 48 hours, centrifuging, drying and grinding to obtain modified chitosan, dissolving 8 parts of polylactic acid into 60 parts of N, N-dimethylformamide solution, slowly dropwise adding 10 parts of toluene diisocyanate, heating to 60 ℃, introducing nitrogen, reacting for 0.5 hour, adding 15 parts of N, N-dimethylformamide solution of modified chitosan, reacting for 10 hours at 100 ℃, precipitating, carrying out suction filtration, washing and drying by using ice water, extracting for 48 hours by using acetone solution, and drying to obtain the composite compatilizer;
s4: dissolving 20 parts of silicon dioxide and 20 parts of dried sisal fibers in 300 parts of toluene solution, uniformly mixing, heating to 100 ℃, introducing nitrogen, adding 20 parts of toluene solution of L-lactide and 0.5 part of stannous octoate, reacting for 48 hours at 160 ℃, performing suction filtration, washing with trichloromethane, drying, adding 15 parts of nano cellulose ethanol solution with the pH value of 5, uniformly mixing, continuously adding 5 parts of gamma-aminopropyltriethoxysilane and 16 parts of dried basalt fibers, uniformly mixing, reacting for 3 hours, washing with water, dissolving in 40 parts of acetamide solution, uniformly mixing with 15 parts of polylactic acid at 70 ℃, performing deaeration in vacuum, uniformly mixing with 8 parts of composite compatilizer after drying, and performing extrusion, grain cutting and hot pressing by using a double-screw extruder to obtain a polylactic acid layer;
s5: uniformly mixing 10 parts of carbon dioxide base, 25 parts of polylactic acid, 70 parts of butanediol adipate-butanediol terephthalate copolymer, 0.3 part of BASF chain extender, 0.3 part of ethylene bis stearamide, 0.3 part of calcium stearate and 5 parts of talcum powder, and extruding, granulating and hot-pressing by using a double-screw extruder to obtain a carbon dioxide base layer;
s6: dissolving 5 parts of sodium hypophosphite in 20 parts of citric acid aqueous solution, adding 5 parts of lignin nanoparticles, drying, standing for 15h, drying at 60 ℃ for 45h, standing at 130 ℃ for 5h, centrifuging for 10min, washing with water, drying, mixing with 30 parts of ethanol solution, adding 20 parts of di (2-ethylhexyl) phosphate, reacting for 8h, carrying out reduced pressure distillation, carrying out suction filtration, washing with water, drying, dissolving in 30 parts of water, adding 5 parts of 4, 4' -diaminodiphenylmethane, mixing uniformly, adding 10 parts of dried wood fiber, reacting for 10min, and carrying out extrusion, grain cutting and hot pressing by using a double-screw extruder to obtain a lignin layer;
s7: and pre-pressing, hot-drying and hot-rolling the polylactic acid layer, the carbon dioxide base layer and the lignin layer to obtain the PPC composite board.
The temperature of the double-screw extruder charging barrel is 180 ℃, the temperature of the die head is 170 ℃, and the length-diameter ratio is 52: 1, cooling by air cooling.
Comparative example
Comparative example 1: s1: soaking sisal fibers in an aqueous solution of 18% sodium hydroxide, reacting for 1h, washing with water, standing, airing and drying;
s2: uniformly mixing 0.1g/L aqueous solution of graphene oxide and 0.0005g/L aqueous solution of polyethylene glycol, reacting at 50 ℃ for 24h, standing to room temperature, centrifuging for 5min, washing with water, drying, dissolving in water, soaking basalt fiber in the solution, and drying;
s3: uniformly mixing 20 parts of chloroform, 10 parts of dimethyl sulfoxide and 5 parts of polyethylene glycol monomethyl ether, adding 10 parts of acetic anhydride, precipitating with 20 parts of glacial ethyl ether, dissolving with 20 parts of chloroform, repeating the steps for three times, and performing suction filtration and drying to obtain hydroformylation polyethylene glycol monomethyl ether;
dissolving 1 part of chitosan in a mixed solution of 10 parts of acetic acid and 10 parts of methanol, adding 8 parts of hydroformylation polyethylene glycol monomethyl ether, reacting for 24 hours, adding 1 part of sodium cyanoborohydride, reacting for 40 hours, dialyzing in water, reacting for 48 hours, centrifuging, drying and grinding to obtain modified chitosan, dissolving 5 parts of polylactic acid in 40 parts of N, N-dimethylformamide solution, slowly dropwise adding 1 part of toluene diisocyanate, heating to 50 ℃, introducing nitrogen, reacting for 0.5 hour, adding 5 parts of N, N-dimethylformamide solution of modified chitosan, reacting for 8-10 hours at 90 ℃, precipitating, filtering, washing and drying by using ice water, extracting for 48 hours by using an acetone solution, and drying to obtain the composite compatilizer;
s4: dissolving 10 parts of silicon dioxide and 10 parts of dried sisal fibers in 200 parts of toluene solution, adding 5 parts of nano-cellulose ethanol solution with the pH value of 4, mixing uniformly, then continuously adding 1 part of gamma-aminopropyltriethoxysilane and 8 parts of dried basalt fibers, mixing uniformly, reacting for 2 hours, washing with water, dissolving in 20 parts of acetamide solution, mixing uniformly with 5 parts of polylactic acid at 60 ℃, carrying out vacuum defoaming, drying, mixing uniformly with 1 part of composite compatilizer, and carrying out extrusion, grain cutting and hot pressing by a double-screw extruder to obtain a polylactic acid layer;
s5: uniformly mixing 5 parts of carbon dioxide base, 20 parts of polylactic acid, 60 parts of butanediol adipate-butanediol terephthalate copolymer, 0.1 part of BASF chain extender, 0.2 part of ethylene bis stearamide, 0.1 part of calcium stearate and 3 parts of talcum powder, and extruding, granulating and hot-pressing by using a double-screw extruder to obtain a carbon dioxide base layer;
s6: dissolving 1 part of sodium hypophosphite into an aqueous solution of 5 parts of citric acid, adding 1 part of lignin nanoparticles, drying, standing for 12h, drying at 60 ℃ for 45h, standing at 130 ℃ for 5h, centrifuging for 5min, washing with water, drying, mixing with 20 parts of an ethanol solution, adding 10 parts of di (2-ethylhexyl) phosphate, reacting for 5h, carrying out reduced pressure distillation, carrying out suction filtration, washing with water, drying, dissolving in 20 parts of water, adding 1 part of 4, 4' -diaminodiphenylmethane, mixing uniformly, adding 5 parts of dried wood fibers, reacting for 5min, and carrying out extrusion, grain cutting and hot pressing by using a double-screw extruder to obtain a lignin layer;
s7: and pre-pressing, hot-drying and hot-rolling the polylactic acid layer, the carbon dioxide base layer and the lignin layer to obtain the PPC composite board.
The temperature of a charging barrel of the double-screw extruder is 160 ℃, the temperature of a die head is 170 ℃, and the length-diameter ratio is 52: 1, cooling by air cooling.
Comparative example 2: s1: soaking sisal fibers in an aqueous solution of 18% sodium hydroxide, reacting for 1h, washing with water, standing, airing and drying;
s2: uniformly mixing 0.1g/L aqueous solution of graphene oxide and 0.0005g/L aqueous solution of polyethylene glycol, reacting at 50 ℃ for 24h, standing to room temperature, centrifuging for 5min, washing with water, drying, dissolving in water, soaking basalt fiber in the solution, and drying;
s3: uniformly mixing 20 parts of chloroform, 10 parts of dimethyl sulfoxide and 5 parts of polyethylene glycol monomethyl ether, adding 10 parts of acetic anhydride, precipitating with 20 parts of glacial ethyl ether, dissolving with 20 parts of chloroform, repeating the steps for three times, and performing suction filtration and drying to obtain hydroformylation polyethylene glycol monomethyl ether;
dissolving 1 part of chitosan in a mixed solution of 10 parts of acetic acid and 10 parts of methanol, adding 8 parts of hydroformylation polyethylene glycol monomethyl ether, reacting for 24 hours, adding 1 part of sodium cyanoborohydride, reacting for 40 hours, dialyzing in water, reacting for 48 hours, centrifuging, drying and grinding to obtain modified chitosan, dissolving 5 parts of polylactic acid in 40 parts of N, N-dimethylformamide solution, slowly dropwise adding 1 part of toluene diisocyanate, heating to 50 ℃, introducing nitrogen, reacting for 0.5 hour, adding 5 parts of N, N-dimethylformamide solution of modified chitosan, reacting for 8-10 hours at 90 ℃, precipitating, filtering, washing and drying by using ice water, extracting for 48 hours by using an acetone solution, and drying to obtain the composite compatilizer;
s4: dissolving 10 parts of silicon dioxide and 10 parts of dried sisal fibers in 200 parts of toluene solution, uniformly mixing, heating to 100 ℃, introducing nitrogen, adding 10 parts of toluene solution of L-lactide and 0.1 part of stannous octoate, reacting at 160 ℃ for 12 hours, performing suction filtration, washing with trichloromethane, drying, adding 5 parts of nano cellulose ethanol solution with the pH value of 4, uniformly mixing, continuously adding 1 part of gamma-aminopropyltriethoxysilane and 8 parts of dried basalt fibers, uniformly mixing, reacting for 2 hours, washing with water, dissolving in 20 parts of acetamide solution, uniformly mixing with 5 parts of polylactic acid at 60 ℃, performing deaeration in vacuum, uniformly mixing with 1 part of composite compatilizer after drying, and performing extrusion, grain cutting and hot pressing by using a double-screw extruder to obtain a polylactic acid layer;
s5: uniformly mixing 5 parts of carbon dioxide base, 20 parts of polylactic acid, 60 parts of butanediol adipate-butanediol terephthalate copolymer, 0.1 part of BASF chain extender, 0.2 part of ethylene bis stearamide, 0.1 part of calcium stearate and 3 parts of talcum powder, and extruding, granulating and hot-pressing by using a double-screw extruder to obtain a carbon dioxide base layer;
s6: dissolving 1 part of lignin in 20 parts of water, adding 1 part of 4, 4' -diaminodiphenylmethane, uniformly mixing, adding 5 parts of dried wood fiber, reacting for 5min, and performing extrusion, grain cutting and hot pressing by using a double-screw extruder to obtain a lignin layer;
s7: and pre-pressing, hot-drying and hot-rolling the polylactic acid layer, the carbon dioxide base layer and the lignin layer to obtain the PPC composite board.
The temperature of a charging barrel of the double-screw extruder is 160 ℃, the temperature of a die head is 170 ℃, and the length-diameter ratio is 52: 1, cooling by air cooling.
Experimental data
Tensile strength: according to GB/T1040.2-2006 determination of tensile Properties of plastics.
Bending property: according to GB1449-2005, Experimental method for bending Properties of fiber reinforced plastics.
Impact strength: according to GB/T1843-2008 "determination of Izod impact Strength".
Water absorption: the sample was soaked in water, taken out 7 days later, and weighed before and after water absorption.
Flame retardancy: according to the UL-94 standard.
And (4) conclusion: 1. compared with the comparative example 1, the examples 1 to 3 show that the mechanical strength and the water absorption of the PCC composite board can be effectively improved by grafting the L-lactide on the surfaces of the silicon dioxide and the sisal fibers, and the mechanical strength of the PCC composite board is not influenced by the introduction of the phosphorus element in the lignin layer.
2. Comparing examples 1-3 with comparative example 2, it is shown that the flame retardancy of the PCC composite board can be improved by introducing phosphorus after the lignin is epoxidized.
The PCC composite board prepared by the invention has excellent mechanical strength, flame retardance, low water absorption and degradability.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A preparation method of a degradable PPC composite board is characterized by comprising the following steps: the method comprises the following steps:
s1: dissolving silicon dioxide and sisal fibers in a toluene solution, uniformly mixing, heating to 100 ℃, introducing nitrogen, adding the toluene solution of L-lactide and stannous octoate, reacting at 160 ℃ for 12-48h, performing suction filtration, washing with trichloromethane, drying, adding a nano cellulose ethanol solution with the pH value of 4-5, uniformly mixing, continuously adding a silane coupling agent and basalt fibers, uniformly mixing, reacting for 2-3h, washing with water, dissolving in an acetamide solution, uniformly mixing with polylactic acid at 60-70 ℃, performing vacuum defoaming, drying, uniformly mixing with a composite compatilizer, extruding by an extruder, granulating, and performing hot pressing to obtain a polylactic acid double-screw layer;
s2: uniformly mixing carbon dioxide base, polylactic acid, a butanediol adipate-butanediol terephthalate copolymer, a BASF chain extender, a dispersing agent, a lubricating agent and a filler, and carrying out extrusion, grain cutting and hot pressing by a double-screw extruder to obtain a carbon dioxide base layer;
s3: dissolving sodium hypophosphite in a citric acid aqueous solution, adding lignin nanoparticles, drying, standing for 12-15h, drying at 60 ℃ for 45h, standing at 130 ℃ for 5h, centrifuging for 5-10min, washing with water, drying, adding di (2-ethylhexyl) phosphate into a mixed ethanol solution, reacting for 5-8h, carrying out reduced pressure distillation, carrying out suction filtration, washing with water, drying, dissolving in water, adding 4, 4' -diaminodiphenylmethane, mixing uniformly, adding dried wood fibers, reacting for 5-10min, and carrying out extrusion, grain cutting and hot pressing by using a double-screw extruder to obtain a lignin layer;
s4: and pre-pressing, hot-drying and hot-rolling the polylactic acid layer, the carbon dioxide base layer and the lignin layer to obtain the PPC composite board.
2. The preparation method of the degradable PPC composite board according to claim 1, wherein the preparation method comprises the following steps: before use, the sisal fibers are soaked in an aqueous solution of sodium hydroxide, reacted for 1-2 hours, washed by water, kept stand, dried and dried;
before being used, the basalt fiber is soaked in a mixed solution of a graphene oxide aqueous solution and a polyethylene glycol aqueous solution, reacted for 0.5-1h, and dried.
3. The preparation method of the degradable PPC composite board according to claim 1, wherein the preparation method comprises the following steps: the preparation process of the composite compatilizer comprises the following steps: uniformly mixing chloroform, dimethyl sulfoxide and polyethylene glycol monomethyl ether, adding acetic anhydride, precipitating with glacial ethyl ether, dissolving with chloroform, repeating for three times, filtering, and drying to obtain hydroformylation polyethylene glycol monomethyl ether;
dissolving chitosan in a mixed solution of acetic acid and methanol, adding hydroformylation polyethylene glycol monomethyl ether, reacting for 24-30h, adding sodium cyanoborohydride, reacting for 40-50h, dialyzing in water for 48h, centrifuging, drying and grinding to obtain modified chitosan, dissolving polylactic acid in an N, N-dimethylformamide solution, slowly dropwise adding toluene diisocyanate, heating to 50-60 ℃, introducing nitrogen, reacting for 0.5h, adding the N, N-dimethylformamide solution of the modified chitosan, reacting for 8-10h at 90-100 ℃, precipitating with ice water, performing suction filtration, washing, drying, extracting with an acetone solution for 48h, and drying.
4. The preparation method of the degradable PPC composite board according to claim 1, wherein the preparation method comprises the following steps: the carbon dioxide base layer comprises the following materials in parts by weight: 5-10 parts of carbon dioxide base, 20-25 parts of polylactic acid, 60-70 parts of butanediol adipate-butanediol terephthalate copolymer, 0.1-0.3 part of BASF chain extender, 0.2-0.3 part of dispersant, 0.1-0.3 part of lubricant and 3-5 parts of filler.
5. The preparation method of the degradable PPC composite board according to claim 1, wherein the preparation method comprises the following steps: the temperature of a charging barrel of the double-screw extruder is 160-180 ℃, the temperature of a die head is 170 ℃, and the length-diameter ratio is 52: 1, cooling by air cooling.
6. The preparation method of the degradable PPC composite board according to claim 1, wherein the preparation method comprises the following steps: the silane coupling agent is gamma-aminopropyl triethoxysilane.
7. The preparation method of the degradable PPC composite board as claimed in claim 4, wherein the preparation method comprises the following steps: the dispersing agent is ethylene bis stearamide; the lubricant is one or more of polyethylene wax, calcium stearate, paraffin and stearic acid amide; the filler is one or more of calcium carbonate and talcum powder.
8. The PCC composite board prepared by the preparation method of the degradable PPC composite board according to any one of claims 1-7.
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