CN113292830A - Environment-friendly flame-retardant polylactic acid plastic and preparation method thereof - Google Patents
Environment-friendly flame-retardant polylactic acid plastic and preparation method thereof Download PDFInfo
- Publication number
- CN113292830A CN113292830A CN202110379813.6A CN202110379813A CN113292830A CN 113292830 A CN113292830 A CN 113292830A CN 202110379813 A CN202110379813 A CN 202110379813A CN 113292830 A CN113292830 A CN 113292830A
- Authority
- CN
- China
- Prior art keywords
- parts
- polylactic acid
- glass fiber
- environment
- friendly flame
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 78
- 239000004626 polylactic acid Substances 0.000 title claims abstract description 77
- 239000003063 flame retardant Substances 0.000 title claims abstract description 44
- 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 title claims abstract description 42
- 229920003023 plastic Polymers 0.000 title claims abstract description 42
- 239000004033 plastic Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000003365 glass fiber Substances 0.000 claims abstract description 59
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 24
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 24
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims abstract description 20
- 239000000600 sorbitol Substances 0.000 claims abstract description 20
- 229920001451 polypropylene glycol Polymers 0.000 claims abstract description 19
- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 18
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 18
- 239000001116 FEMA 4028 Substances 0.000 claims abstract description 18
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 18
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims abstract description 18
- 229920001276 ammonium polyphosphate Polymers 0.000 claims abstract description 18
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 18
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims abstract description 18
- 229960004853 betadex Drugs 0.000 claims abstract description 18
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 18
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims abstract description 17
- 229930195725 Mannitol Natural products 0.000 claims abstract description 17
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000594 mannitol Substances 0.000 claims abstract description 17
- 235000010355 mannitol Nutrition 0.000 claims abstract description 17
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 42
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 38
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000003513 alkali Substances 0.000 claims description 14
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 14
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000001125 extrusion Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000004381 surface treatment Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000007605 air drying Methods 0.000 claims description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 239000002202 Polyethylene glycol Substances 0.000 description 6
- 239000004744 fabric Substances 0.000 description 6
- 229920001223 polyethylene glycol Polymers 0.000 description 6
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical group CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical group CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920000704 biodegradable plastic Polymers 0.000 description 1
- 238000000071 blow moulding Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 229920006238 degradable plastic Polymers 0.000 description 1
- 235000013410 fast food Nutrition 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 235000021485 packed food Nutrition 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009757 thermoplastic moulding Methods 0.000 description 1
- 238000011282 treatment Methods 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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
-
- 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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides an environment-friendly flame-retardant polylactic acid plastic and a preparation method thereof, wherein the environment-friendly flame-retardant polylactic acid plastic is prepared from the following raw materials in parts by weight: 100-120 parts of polylactic acid, 10-20 parts of glass fiber, 2-4 parts of mannitol, 1-3 parts of beta-cyclodextrin, 15-20 parts of ammonium polyphosphate, 4-6 parts of melamine, 4-6 parts of polypropylene oxide, 0.2-0.8 part of sorbitol, 1-2 parts of talcum powder, 1-2 parts of stearic acid amide and 0.1-0.4 part of antioxidant. The polylactic acid plastic disclosed by the invention has the advantages of environmental friendliness and high flame retardant grade, and the influence of the addition of a flame retardant on the physical and mechanical properties of the polylactic acid body material is reduced to the greatest extent.
Description
Technical Field
The invention belongs to the technical field of degradable plastics, and particularly relates to an environment-friendly flame-retardant polylactic acid plastic and a preparation method thereof.
Background
Polylactic acid, also known as polylactide, is a polyester polymer obtained by polymerizing lactic acid as a main raw material, is a novel biodegradable material, and is prepared from a starch raw material provided by a renewable plant resource (such as corn). The starch raw material is saccharified to obtain glucose, the glucose and certain strains are fermented to prepare high-purity lactic acid, and the polylactic acid with certain molecular weight is synthesized by a chemical synthesis method. The biodegradable plastic has good biodegradability, can be completely degraded by microorganisms in the nature after being used, finally generates carbon dioxide and water, does not pollute the environment, is very favorable for protecting the environment, and is a well-known environment-friendly material. The common plastic treatment method still burns and cremates to cause a large amount of greenhouse gases to be discharged into the air, while the polylactic acid plastic is buried in the soil to be degraded, and the generated carbon dioxide directly enters organic matters of the soil or is absorbed by plants, so that the carbon dioxide is not discharged into the air and does not cause the greenhouse effect.
The mechanical property and the physical property are good. The polylactic acid is suitable for various processing methods such as blow molding, thermoplastic molding and the like, is convenient to process and has wide application. Can be used for processing various plastic products from industry to civilian use, packaged food, fast food lunch boxes, non-woven fabrics, industrial and civilian cloth. And then the fabric is processed into agricultural fabrics, health care fabrics, cleaning rags, sanitary products, outdoor ultraviolet-proof fabrics, tent cloth, floor mat surfaces and the like, and the market prospect is very good.
However, polylactic acid itself is a flammable material, and has an oxygen index of 20%, and thus, due to its flammable characteristics, the application range of polylactic acid is limited to some extent. At present, many researches on the flame retardance of polylactic acid are reported, and the flame retardants reported at present mainly comprise phosphorus-nitrogen flame retardants, metal compounds, intumescent flame retardant systems and the like. However, when the existing flame retardant is added into polylactic acid, the flame retardant property of the polylactic acid is improved, and the physical and mechanical properties of the polylactic acid body material are also influenced to a certain extent.
Disclosure of Invention
The polylactic acid plastic has the advantages of environmental protection and high flame retardant grade, and simultaneously reduces the influence of the addition of a flame retardant on the physical and mechanical properties of a polylactic acid body material to the maximum extent.
The technical scheme of the invention is realized as follows:
an environment-friendly flame-retardant polylactic acid plastic is prepared from the following raw materials in parts by weight: 100-120 parts of polylactic acid, 10-20 parts of glass fiber, 2-4 parts of mannitol, 1-3 parts of beta-cyclodextrin, 15-20 parts of ammonium polyphosphate, 4-6 parts of melamine, 4-6 parts of polypropylene oxide, 0.2-0.8 part of sorbitol, 1-2 parts of talcum powder, 1-2 parts of stearic acid amide and 0.1-0.4 part of antioxidant.
Wherein the glass fiber is prepared by the following surface treatments:
1) adding glass fiber into mixed alkali solution, stirring for 1-2h at normal temperature, filtering, washing with 0.5-2% acetic acid, washing with a large amount of deionized water, and drying at low temperature to obtain surface hydroxylated glass fiber;
(2) adjusting the pH value of 75% alcohol by volume to 4-5 with acetic acid, adding surface hydroxylated glass fiber, stirring, adding silane coupling agent 2-4% of glass fiber weight and caprolactam 0.3-0.8%, heating to 40-60 deg.C, stirring for 1-3h, taking out, and air drying.
The mixed alkali mixed solution is a mixed solution of potassium hydroxide and potassium carbonate, wherein the mass percentage concentration of the potassium hydroxide is 0.5-1.5%, and the mass percentage concentration of the potassium carbonate is 1.0-2.0%.
Wherein the antioxidant is 1010, 168 or 800.
A preparation method of environment-friendly flame-retardant polylactic acid plastic comprises the following steps:
(1) adding polylactic acid, polypropylene oxide and sorbitol into a reaction kettle, heating to 140-170 ℃, and then continuously stirring for 25-35 min;
(2) adding glass fiber, mannitol, beta-cyclodextrin, ammonium polyphosphate, melamine, talcum powder, stearic acid amide and antioxidant, fully and uniformly stirring, placing in a double-screw extruder for melt extrusion, and drying the extruded material to remove moisture to obtain the product.
Wherein the drying temperature is 50 +/-5 DEG C
The invention has the beneficial effects that:
(1) the glass fiber after surface treatment is added in the invention, and the glass fiber is blended with the polylactic acid, so that the strength of the polylactic acid is improved, and the original biodegradability of the polylactic acid can be maintained. In order to enable the glass fiber and the polylactic acid to have better compatible effect, the surface of the glass fiber is chemically treated, the surface chemical property of the glass fiber is changed, and the compatibility of the glass fiber and the polylactic acid is obviously improved.
(2) The flame retardant added in the invention is an intumescent flame retardant, beta-cyclodextrin is a carbon source, ammonium polyphosphate is an acid source, melamine is an air source, a carbonaceous foam layer can be generated on the surface during combustion, the effects of heat insulation, oxygen isolation, smoke suppression, drip prevention and the like are achieved, the flame retardant has excellent flame retardant performance, low smoke, low toxicity and no corrosive gas is generated, and the environment-friendly performance of the polyester plastics is ensured by adding the flame retardant.
(3) The polypropylene oxide and the sorbitol are added into the polylactic acid to blend and modify the polylactic acid, when the polylactic acid is impacted, the polypropylene oxide and the sorbitol can absorb or disperse impact energy, so that the toughness of the polylactic acid is improved, and the sorbitol also plays a role of a plasticizer in the composition.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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
The embodiment provides an environment-friendly flame-retardant polylactic acid plastic which is prepared from the following raw materials in parts by weight: 110 parts of polylactic acid, 15 parts of glass fiber, 3 parts of mannitol, 2 parts of beta-cyclodextrin, 18 parts of ammonium polyphosphate, 5 parts of melamine, 5 parts of polypropylene oxide, 0.5 part of sorbitol, 1.5 parts of talcum powder, 1.5 parts of stearic acid amide and 0.25 part of antioxidant; the antioxidant is antioxidant 1010.
Wherein the glass fiber is prepared by the following surface treatments:
1) adding glass fiber into mixed alkali solution, stirring for 1.5h at normal temperature, filtering, washing with 1.2% acetic acid, washing with a large amount of deionized water, and drying at low temperature to obtain surface hydroxylated glass fiber; the synthetic alkali solution is a mixed solution of potassium hydroxide and potassium carbonate, wherein the mass percentage concentration of the potassium hydroxide is 1.0%, and the mass percentage concentration of the potassium carbonate is 1.5%;
(2) adjusting the pH value of 75% alcohol by volume to 4-5 with acetic acid, adding surface hydroxylated glass fiber, stirring, adding silane coupling agent 3% of glass fiber weight and caprolactam 0.55%, heating to 50 deg.C, stirring for 2h, taking out, and air drying.
The preparation method of the environment-friendly flame-retardant polylactic acid plastic comprises the following steps:
(1) adding polylactic acid, polypropylene oxide and sorbitol into a reaction kettle, heating to 155 ℃, and continuing stirring for 30 min;
(2) adding glass fiber, mannitol, beta-cyclodextrin, ammonium polyphosphate, melamine, talcum powder, stearic acid amide and antioxidant, fully stirring uniformly, putting into a double-screw extruder for melt extrusion, drying the extruded material to remove water, wherein the drying temperature is 50 +/-5 ℃, and thus obtaining the polyethylene glycol terephthalate.
Example 2
The embodiment provides an environment-friendly flame-retardant polylactic acid plastic which is prepared from the following raw materials in parts by weight: 100 parts of polylactic acid, 20 parts of glass fiber, 2 parts of mannitol, 3 parts of beta-cyclodextrin, 15 parts of ammonium polyphosphate, 6 parts of melamine, 4 parts of polypropylene oxide, 0.8 part of sorbitol, 1 part of talcum powder, 2 parts of stearic acid amide and 0.1 part of antioxidant; the antioxidant is 1010, 168 or 800.
Wherein the glass fiber is prepared by the following surface treatments:
1) adding glass fiber into mixed alkali solution, stirring for 1h at normal temperature, filtering, washing with 2% acetic acid, washing with a large amount of deionized water, and drying at low temperature to obtain surface hydroxylated glass fiber; the synthetic alkali solution is a mixed solution of potassium hydroxide and potassium carbonate, the mass percentage concentration of the potassium hydroxide is 0.5%, and the mass percentage concentration of the potassium carbonate is 2.0%;
(2) adjusting the pH value of 75% alcohol by volume to 4 with acetic acid, adding the glass fiber with hydroxylated surface, stirring, adding silane coupling agent 4% of the weight of the glass fiber and caprolactam 0.3%, heating to 60 ℃, stirring for 1h, taking out, and drying to obtain the final product.
The preparation method of the environment-friendly flame-retardant polylactic acid plastic comprises the following steps:
(1) adding polylactic acid, polypropylene oxide and sorbitol into a reaction kettle, heating to 140 ℃, and continuing stirring for 35 min;
(2) adding glass fiber, mannitol, beta-cyclodextrin, ammonium polyphosphate, melamine, talcum powder, stearic acid amide and antioxidant, fully stirring uniformly, putting into a double-screw extruder for melt extrusion, drying the extruded material to remove water, wherein the drying temperature is 50 +/-5 ℃, and thus obtaining the polyethylene glycol terephthalate.
Example 3
The embodiment provides an environment-friendly flame-retardant polylactic acid plastic which is prepared from the following raw materials in parts by weight: 120 parts of polylactic acid, 10 parts of glass fiber, 4 parts of mannitol, 1 part of beta-cyclodextrin, 20 parts of ammonium polyphosphate, 4 parts of melamine, 6 parts of polypropylene oxide, 0.2 part of sorbitol, 2 parts of talcum powder, 1 part of stearic acid amide and 0.4 part of antioxidant; the antioxidant is 1010, 168 or 800.
Wherein the glass fiber is prepared by the following surface treatments:
1) adding glass fiber into mixed alkali solution, stirring for 2h at normal temperature, filtering, washing with 0.5% acetic acid, washing with a large amount of deionized water, and drying at low temperature to obtain surface hydroxylated glass fiber; the synthetic alkali solution is a mixed solution of potassium hydroxide and potassium carbonate, wherein the mass percentage concentration of the potassium hydroxide is 1.5 percent, and the mass percentage concentration of the potassium carbonate is 1.0 percent;
(2) adjusting the pH value of 75% alcohol by volume to 5 with acetic acid, adding the glass fiber with hydroxylated surface, stirring, adding silane coupling agent 2% of the weight of the glass fiber and caprolactam 0.8%, heating to 40 ℃, stirring for 3h, taking out, and drying to obtain the final product.
The preparation method of the environment-friendly flame-retardant polylactic acid plastic comprises the following steps:
(1) adding polylactic acid, polypropylene oxide and sorbitol into a reaction kettle, heating to 140-170 ℃, and then continuously stirring for 25 min;
(2) adding glass fiber, mannitol, beta-cyclodextrin, ammonium polyphosphate, melamine, talcum powder, stearic acid amide and antioxidant, fully stirring uniformly, putting into a double-screw extruder for melt extrusion, drying the extruded material to remove water, wherein the drying temperature is 50 +/-5 ℃, and thus obtaining the polyethylene glycol terephthalate.
Example 4
The embodiment provides an environment-friendly flame-retardant polylactic acid plastic which is prepared from the following raw materials in parts by weight: 105 parts of polylactic acid, 18 parts of glass fiber, 2.5 parts of mannitol, 1.5 parts of beta-cyclodextrin, 18 parts of ammonium polyphosphate, 4.5 parts of melamine, 5.5 parts of polypropylene oxide, 0.3 part of sorbitol, 1.8 parts of talcum powder, 1.2 parts of stearic acid amide and 0.15 part of antioxidant; the antioxidant is antioxidant 168.
Wherein the glass fiber is prepared by the following surface treatments:
1) adding glass fiber into mixed alkali solution, stirring for 1.5h at normal temperature, filtering, washing with 1.5% acetic acid, washing with a large amount of deionized water, and drying at low temperature to obtain surface hydroxylated glass fiber; the synthetic alkali solution is a mixed solution of potassium hydroxide and potassium carbonate, the mass percentage concentration of the potassium hydroxide is 0.8%, and the mass percentage concentration of the potassium carbonate is 1.2%;
(2) adjusting the pH value of 75% alcohol by volume to 4.2 with acetic acid, adding surface hydroxylated glass fiber, stirring, adding silane coupling agent 3.5% of glass fiber weight and caprolactam 0.4%, heating to 45 deg.C, stirring for 2.5h, taking out, and air drying.
The preparation method of the environment-friendly flame-retardant polylactic acid plastic comprises the following steps:
(1) adding polylactic acid, polypropylene oxide and sorbitol into a reaction kettle, heating to 170 ℃, and then continuously stirring for 25-35 min;
(2) adding glass fiber, mannitol, beta-cyclodextrin, ammonium polyphosphate, melamine, talcum powder, stearic acid amide and antioxidant, fully stirring uniformly, putting into a double-screw extruder for melt extrusion, drying the extruded material to remove water, wherein the drying temperature is 50 +/-5 ℃, and thus obtaining the polyethylene glycol terephthalate.
Example 5
The embodiment provides an environment-friendly flame-retardant polylactic acid plastic which is prepared from the following raw materials in parts by weight: 115 parts of polylactic acid, 12 parts of glass fiber, 3.5 parts of mannitol, 1.2 parts of beta-cyclodextrin, 18 parts of ammonium polyphosphate, 4.5 parts of melamine, 5.5 parts of polypropylene oxide, 0.3 part of sorbitol, 1.2 parts of talcum powder, 1.8 parts of stearic acid amide and 0.35 part of antioxidant; the antioxidant is 1010, 168 or 800.
Wherein the glass fiber is prepared by the following surface treatments:
1) adding glass fiber into mixed alkali solution, stirring for 1.5h at normal temperature, filtering, washing with 1.0% acetic acid, washing with a large amount of deionized water, and drying at low temperature to obtain surface hydroxylated glass fiber; the synthetic alkali solution is a mixed solution of potassium hydroxide and potassium carbonate, wherein the mass percentage concentration of the potassium hydroxide is 1.2%, and the mass percentage concentration of the potassium carbonate is 1.8%;
(2) adjusting the pH value of 75% alcohol by volume to 4.8 with acetic acid, adding surface hydroxylated glass fiber, stirring, adding silane coupling agent 2.5% of glass fiber weight and caprolactam 0.7%, heating to 55 deg.C, stirring for 2h, taking out, and air drying.
The preparation method of the environment-friendly flame-retardant polylactic acid plastic comprises the following steps:
(1) adding polylactic acid, polypropylene oxide and sorbitol into a reaction kettle, heating to 145 ℃, and continuing stirring for 30 min;
(2) adding glass fiber, mannitol, beta-cyclodextrin, ammonium polyphosphate, melamine, talcum powder, stearic acid amide and antioxidant, fully stirring uniformly, putting into a double-screw extruder for melt extrusion, drying the extruded material to remove water, wherein the drying temperature is 50 +/-5 ℃, and thus obtaining the polyethylene glycol terephthalate.
Performance testing
The properties of the polylactic acid plastic prepared in examples 1 to 5 were measured, and the test standards and the test results are shown in the following table.
TABLE 1 mechanical Properties test results of polylactic acid plastics of examples 1 to 5
The data show that the polylactic acid plastic prepared by the invention has good tensile strength, elongation at break and notch impact strength on the basis of good flame retardant property.
Comparative example 1
This example provides an environmentally friendly flame retardant polylactic acid plastic, which has the same raw materials and preparation method as example 1 except that no glass fiber is added.
Comparative example 2
This example provides an environment-friendly flame-retardant polylactic acid plastic, which is prepared by adding no polypropylene oxide and no sorbitol to the raw materials of this example, and the preparation method comprises the following steps:
adding polylactic acid into a reaction kettle, adding glass fiber, mannitol, beta-cyclodextrin, ammonium polyphosphate, melamine, talcum powder, stearic acid amide and an antioxidant, fully and uniformly stirring, placing in a double-screw extruder for melt extrusion, drying the extruded material to remove water, and drying at the temperature of 50 +/-5 ℃ to obtain the polylactic acid.
Comparative example 3
The embodiment provides an environment-friendly flame-retardant polylactic acid plastic, wherein sorbitol is not added in the raw materials of the embodiment, and the preparation method comprises the following steps:
(1) adding polylactic acid and polypropylene oxide into a reaction kettle, heating to 155 ℃, and continuing stirring for 30 min;
(2) adding glass fiber, mannitol, beta-cyclodextrin, ammonium polyphosphate, melamine, talcum powder, stearic acid amide and antioxidant, fully stirring uniformly, putting into a double-screw extruder for melt extrusion, drying the extruded material to remove water, wherein the drying temperature is 50 +/-5 ℃, and thus obtaining the polyethylene glycol terephthalate.
Performance testing
The properties of the polylactic acid plastic prepared in comparative examples 1 to 3 were measured, and the test standards and test results are shown in the following table.
TABLE 2 mechanical Property test results of comparative examples 1 to 3 polylactic acid plastics
As can be seen from the above data, the polylactic acid plastic prepared in comparative example 1 has slightly reduced flame retardant property, and has significantly reduced tensile strength, elongation at break and notch impact strength compared with example 1. Compared with the polylactic acid plastic prepared in the example 1, the flame retardant property of the polylactic acid plastic prepared in the comparative example 2 is slightly reduced, and the tensile strength, the elongation at break and the notch impact strength are all obviously reduced. Compared with the polylactic acid plastic prepared in the example 1, the flame retardant property of the polylactic acid plastic prepared in the comparative example 2 is slightly reduced, and the tensile strength, the elongation at break and the notch impact strength are all obviously reduced. The tensile strength, elongation at break and notched impact strength were less reduced than in comparative example 2.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements, etc. made within the spirit and principles of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. The environment-friendly flame-retardant polylactic acid plastic is characterized by being prepared from the following raw materials in parts by weight: 100-120 parts of polylactic acid, 10-20 parts of glass fiber, 2-4 parts of mannitol, 1-3 parts of beta-cyclodextrin, 15-20 parts of ammonium polyphosphate, 4-6 parts of melamine, 4-6 parts of polypropylene oxide, 0.2-0.8 part of sorbitol, 1-2 parts of talcum powder, 1-2 parts of stearic acid amide and 0.1-0.4 part of antioxidant.
2. The environment-friendly flame-retardant polylactic acid plastic according to claim 1, wherein: the glass fiber is prepared by the following surface treatments:
1) adding glass fiber into mixed alkali solution, stirring for 1-2h at normal temperature, filtering, washing with 0.5-2% acetic acid, washing with a large amount of deionized water, and drying at low temperature to obtain surface hydroxylated glass fiber;
(2) adjusting the pH value of 75% alcohol by volume to 4-5 with acetic acid, adding surface hydroxylated glass fiber, stirring, adding silane coupling agent 2-4% of glass fiber weight and caprolactam 0.3-0.8%, heating to 40-60 deg.C, stirring for 1-3h, taking out, and air drying.
3. The environment-friendly flame-retardant polylactic acid plastic according to claim 2, wherein: the mixed alkali mixed solution is a mixed solution of potassium hydroxide and potassium carbonate, the mass percentage concentration of the potassium hydroxide is 0.5-1.5%, and the mass percentage concentration of the potassium carbonate is 1.0-2.0%.
4. The environment-friendly flame-retardant polylactic acid plastic according to claim 1, wherein: the antioxidant is 1010, 168 or 800.
5. The preparation method of the environment-friendly flame-retardant polylactic acid plastic according to any one of claims 1 to 4, which is characterized by comprising the following steps:
(1) adding polylactic acid, polypropylene oxide and sorbitol into a reaction kettle, heating to 140-170 ℃, and then continuously stirring for 25-35 min;
(2) adding glass fiber, mannitol, beta-cyclodextrin, ammonium polyphosphate, melamine, talcum powder, stearic acid amide and antioxidant, fully and uniformly stirring, placing in a double-screw extruder for melt extrusion, and drying the extruded material to remove moisture to obtain the product.
6. The preparation method of the environment-friendly flame-retardant polylactic acid plastic according to claim 5, characterized in that: the drying temperature is 50 +/-5 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110379813.6A CN113292830A (en) | 2021-04-08 | 2021-04-08 | Environment-friendly flame-retardant polylactic acid plastic and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110379813.6A CN113292830A (en) | 2021-04-08 | 2021-04-08 | Environment-friendly flame-retardant polylactic acid plastic and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113292830A true CN113292830A (en) | 2021-08-24 |
Family
ID=77319479
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110379813.6A Pending CN113292830A (en) | 2021-04-08 | 2021-04-08 | Environment-friendly flame-retardant polylactic acid plastic and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113292830A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023103116A1 (en) * | 2021-12-09 | 2023-06-15 | 王玲芝 | Special biomass color masterbatch for degradable plastic and preparation method therefor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798448A (en) * | 2010-04-06 | 2010-08-11 | 奇瑞汽车股份有限公司 | Method for preparing glass fiber-reinforced flame-retardant heat-resistant polylactic acid composite material |
| US20100256746A1 (en) * | 2009-03-23 | 2010-10-07 | Micell Technologies, Inc. | Biodegradable polymers |
| CN106243656A (en) * | 2016-09-29 | 2016-12-21 | 青岛海之源智能技术有限公司 | A kind of anti-flaming environment-friendly polylactic acid plastic and preparation method thereof |
-
2021
- 2021-04-08 CN CN202110379813.6A patent/CN113292830A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100256746A1 (en) * | 2009-03-23 | 2010-10-07 | Micell Technologies, Inc. | Biodegradable polymers |
| CN101798448A (en) * | 2010-04-06 | 2010-08-11 | 奇瑞汽车股份有限公司 | Method for preparing glass fiber-reinforced flame-retardant heat-resistant polylactic acid composite material |
| CN106243656A (en) * | 2016-09-29 | 2016-12-21 | 青岛海之源智能技术有限公司 | A kind of anti-flaming environment-friendly polylactic acid plastic and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| JIAN-XIANG FENG ET AL.: "An intumescent flame retardant system using β-cyclodextrin as a carbon source in polylactic acid (PLA)", 《POLYMERS FOR ADVANCED TECHNOLOGIES》 * |
| 刘英俊等: "《改性塑料行业指南.塑料改性理论与实践及企事业名录》", 30 September 2000 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023103116A1 (en) * | 2021-12-09 | 2023-06-15 | 王玲芝 | Special biomass color masterbatch for degradable plastic and preparation method therefor |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100374493C (en) | Flame-resistant plastic-wood composite materials and process for preparing same | |
| CN103881338B (en) | A kind of antistatic biodegradation material of novel flame-retardant and preparation method thereof | |
| CN100516135C (en) | Bio-degradable resin composite, and its filling and moulded product | |
| CN102604346B (en) | Biodegradable polylactic acid-starch flame retardant composite material and preparation method thereof | |
| WO2005066272A1 (en) | Blends of aliphatic-aromatic copolyesters with ethylene-vinyl acetate copolymers | |
| WO2007125546A1 (en) | Novel biodegradable polymer composition useful for the preparation of biodegradable plastic and a process for the preparation of said composition | |
| CN109111710B (en) | Heat-resistant PLA-based degradable plastic bottle and preparation method thereof | |
| CN105504363A (en) | Starch and plant fiber composite biodegradable polyester film-blowing grade resin and preparation method | |
| CN105694405A (en) | Halogen-free flame retardant polylactic acid toughening modification composite material and preparing method thereof | |
| CN105602216A (en) | Carbon fiber reinforced heatproof flame-retardant polylactic acid composite material and preparation method thereof | |
| CN111808334B (en) | Processing technology of biomass-based composite material for non-woven fabric with high degradability | |
| CN112920571A (en) | Modified PLA (polylactic acid) and PHA (polyhydroxyalkanoate) blending material and preparation method thereof | |
| CN113683874A (en) | Full-biomass full-degradable material and preparation method and application thereof | |
| CN102277655A (en) | Manufacturing method of biodegradable starch-based fiber | |
| CN113956630A (en) | Completely biodegradable film and preparation method thereof | |
| CN110903578A (en) | Flame-retardant polyvinyl alcohol material and preparation method thereof | |
| CN106832572A (en) | A kind of polypropylene non-woven fabric is material modified | |
| CN113292830A (en) | Environment-friendly flame-retardant polylactic acid plastic and preparation method thereof | |
| CN102070795B (en) | Biodegradation composition, and preparation method and application thereof | |
| CN113185817A (en) | Polylactic acid plastic containing composite flame retardant and preparation method thereof | |
| CN101469110A (en) | Biodegradable material composition and injection moulding product thereof | |
| Sari et al. | Properties and Food Packaging Application of Poly‐(Lactic) Acid | |
| CN106243656B (en) | A kind of anti-flaming environment-friendly polylactic acid plastic and preparation method thereof | |
| CN106217826B (en) | A kind of modified bamboo fibre lactic acid composite material of automotive trim | |
| CN114369339A (en) | Production technology and application of low-cost biodegradable material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210824 |