CN109852015A - A kind of cooperative flame retardant poly lactic acid nano composite material and preparation method thereof - Google Patents
A kind of cooperative flame retardant poly lactic acid nano composite material and preparation method thereof Download PDFInfo
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- CN109852015A CN109852015A CN201811516451.5A CN201811516451A CN109852015A CN 109852015 A CN109852015 A CN 109852015A CN 201811516451 A CN201811516451 A CN 201811516451A CN 109852015 A CN109852015 A CN 109852015A
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 64
- 239000004626 polylactic acid Substances 0.000 title claims abstract description 61
- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 58
- 239000000463 material Substances 0.000 title claims abstract description 54
- 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 43
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 25
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims abstract description 16
- 230000000979 retarding effect Effects 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims description 18
- 239000012745 toughening agent Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 11
- 238000001125 extrusion Methods 0.000 claims description 9
- 238000005469 granulation Methods 0.000 claims description 9
- 230000003179 granulation Effects 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 239000003963 antioxidant agent Substances 0.000 claims description 6
- 230000003078 antioxidant effect Effects 0.000 claims description 6
- -1 graphite Alkene Chemical class 0.000 claims description 6
- 229920001432 poly(L-lactide) Polymers 0.000 claims description 5
- BZQKBFHEWDPQHD-UHFFFAOYSA-N 1,2,3,4,5-pentabromo-6-[2-(2,3,4,5,6-pentabromophenyl)ethyl]benzene Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1CCC1=C(Br)C(Br)=C(Br)C(Br)=C1Br BZQKBFHEWDPQHD-UHFFFAOYSA-N 0.000 claims description 4
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 4
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 4
- 229920002961 polybutylene succinate Polymers 0.000 claims description 4
- 239000004631 polybutylene succinate Substances 0.000 claims description 4
- 229920001610 polycaprolactone Polymers 0.000 claims description 4
- 239000004632 polycaprolactone Substances 0.000 claims description 4
- WSQZNZLOZXSBHA-UHFFFAOYSA-N 3,8-dioxabicyclo[8.2.2]tetradeca-1(12),10,13-triene-2,9-dione Chemical compound O=C1OCCCCOC(=O)C2=CC=C1C=C2 WSQZNZLOZXSBHA-UHFFFAOYSA-N 0.000 claims description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
- 229930182843 D-Lactic acid Natural products 0.000 claims description 2
- JVTAAEKCZFNVCJ-UWTATZPHSA-N D-lactic acid Chemical compound C[C@@H](O)C(O)=O JVTAAEKCZFNVCJ-UWTATZPHSA-N 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229940022769 d- lactic acid Drugs 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims 1
- 239000010439 graphite Substances 0.000 claims 1
- 239000000654 additive Substances 0.000 abstract description 4
- 230000000996 additive effect Effects 0.000 abstract description 4
- 239000012752 auxiliary agent Substances 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 abstract 2
- 235000014655 lactic acid Nutrition 0.000 abstract 1
- 239000004310 lactic acid Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- 239000004416 thermosoftening plastic Substances 0.000 description 2
- UZBRNILSUGWULW-UHFFFAOYSA-N 3,8-dioxabicyclo[8.2.2]tetradeca-1(12),10,13-triene-2,9-dione;hexanedioic acid Chemical compound OC(=O)CCCCC(O)=O.O=C1OCCCCOC(=O)C2=CC=C1C=C2 UZBRNILSUGWULW-UHFFFAOYSA-N 0.000 description 1
- 206010054949 Metaplasia Diseases 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 compound 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
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000071 blow moulding Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical compound O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Biological Depolymerization Polymers (AREA)
Abstract
The invention discloses a kind of cooperative flame retardant poly lactic acid nano composite materials and preparation method thereof.This composite material is made of the raw material of following parts by weight of component: 70~90wt% of polylactic acid, 5~20wt% of bromide fire retardant, 2~10wt% of fire retarding synergist, 0.1~5wt% of graphene oxide, 0~2wt% of other auxiliary agents.On the one hand the present invention can generate cooperative flame retardant effect with halogenated flame retardant as fire retarding synergist using graphene, to reduce the dosage of halogenated flame retardant, on the other hand since the nano flame retardant synergist additive amount of the invention used is few, it can be dispersed in polylactic acid matrix in material processing, so that lactic acid composite material is having excellent flame retardant property, mechanical property is improved simultaneously.
Description
Technical field
The invention belongs to polymeric material fields, and in particular to a kind of cooperative flame retardant poly lactic acid nano composite material and its system
Preparation Method.
Background technique
Polylactic acid (PLA) is a kind of polymer with excellent biocompatibility and biodegradable, is derived from
Renewable resource crops (such as corn), most prominent advantage are biodegradabilities, can be by life micro- in nature after use
Object is degradable, ultimately generates carbon dioxide and water, free from environmental pollution, to protection environmental benefits.Polylactic acid has good machinery
Performance and physical property are suitable for the various processing methods such as blow molding, thermoplastic, easy to process.Polylactic acid is having many advantageous properties
While there is also some disadvantages, be such as readily burned, use scope is restricted, it is therefore desirable to be assigned by method of modifying poly-
Lactic acid flame retardant property.
Adding type fire retardant be blended with high molecular material be material it is flame-retardant modified can common method.Halogen containing flame-retardant have compared with
High flame retardant property is usually used in the flame-retardant modified of thermoplastic macromolecule material.However the additive amount of halogen flame is high, to mechanics
Performance is affected.Graphene is the tightly packed a kind of carbonaceous new material at single layer bi-dimensional cellular shape lattice structure of carbon atom,
With the characteristics such as high-intensitive, high conductivity and high-specific surface area.Recent studies suggest that in a polymer matrix at nano-dispersion
Graphene can effectively improve mechanical property, electric property, thermal stability and barrier property of nanocomposite etc..Polymerization
Object/graphene nanocomposite material flame retardant property causes domestic and foreign scholars' extensive concern.The collaboration of fire retardant and graphene
Effect improves the flame retardant effect to polymer, reduces the additive amount of fire retardant, provides one kind newly to improve flame retarding efficiency
Approach.
Summary of the invention
The purpose of the present invention is to provide a kind of cooperative flame retardant poly lactic acid nano composite materials and preparation method thereof, reduce resistance
Agent dosage is fired, flame retarding efficiency is improved, improves mechanical property.This method simple economy, abundant raw material are easy to get, and are easy to industrial metaplasia
It produces.
The present invention provides a kind of cooperative flame retardant poly lactic acid nano composite materials and preparation method thereof, by including following weight
The raw material of part component is made:
Preferably, the polylactic acid is poly-L-lactic acid, poly- D lactic acid or their blend, and weight average molecular weight is 1~200,000.
Preferably, the bromide fire retardant is brominated epoxy resin, decabromodiphenylethane, brominated Polystyrene etc..
Preferably, the fire retarding synergist is environmentally friendly grade antimony oxide.
Preferably, the graphene is graphene oxide, graphene or graphene microchip.
Preferably, the toughener is mainly poly butylene succinate (PBS), polycaprolactone (PCL), polyadipate
Butylene terephthalate (PBAT).
Preferably, other described auxiliary agents are mainly antioxidant, and antioxidant is mainly hindered phenol or sulphur ester antioxidant.
The preparation method of above-mentioned cooperative flame retardant poly lactic acid nano composite material, the specific steps are as follows:
(1) each raw material is weighed according to the ratio；
(2) by polylactic acid particle within the scope of 60-200 DEG C, constant temperature or gradually heating are crystallized 1-20 hours, obtain crystallinity
Polylactic acid particle greater than 60%；
(3) bromide fire retardant, fire retarding synergist, toughener, graphene are dried to 6-12h in 80 DEG C of baking ovens.
(4) substance after being dried in (2) the step of weighing up and (3) is first put into super mixer and carries out dry-mixed 3-
5min。
(5) mixture obtained in step (4) is added twin-screw extrude, carries out melting extrusion granulation, extruder
Temperature of each section is as follows: 140~150 DEG C of an area, two 150~160 DEG C of areas, three 160~170 DEG C of areas, four 160~170 DEG C of areas, 5th area
160~170 DEG C, six 160~170 DEG C of areas, seven 165~175 DEG C of areas, 160~170 DEG C of head temperature, 12~18MPa of pressure, object
Material stops 1~2min in an extruder
The beneficial effects of the present invention are: (1) bromide fire retardant thermal stability is high, flame retarding efficiency is high, and fire retardant is not easy to migrate,
Suitable for introducing graphene and bromide fire retardant progress to the stringent household electrical appliances of various performance requirements, electronics and automobile and other industries (2)
Compositional flame-retardant modified polylactic resin can make material obtain excellent mechanical property while improving Flame Retardancy energy
Energy.The dispersion of nanoscale can be reached as long as a small amount of graphene is added, hence it is evident that reduce heat release when polymer combustion
Rate peak value reduces usage amount of the bromide fire retardant in polylactic acid；(3) raw material is easy to get extensively, and it is quick that the processing is simple, is suitable for
Large-scale industrial production.
Specific embodiment
The present invention can be further elucidated above by the acquisition of following preferred embodiment, but these embodiments are merely to illustrate,
The scope of the present invention is not made and defining.
The various raw material that following embodiment of the present invention uses, not doing specified otherwise is commercial product.
In the composite-material formula of embodiment and comparative example, polylactic acid is poly-L-lactic acid, weight average molecular weight 100,000~30
Ten thousand；Bromide fire retardant is decabromodiphenylethane (Albemarle Corporation, the U.S.)；Fire retarding synergist is antimony oxide；Toughener is to gather oneself
Diacid butylene terephthalate (PBAT), trade mark C1200, graphene are homemade graphene oxide, other auxiliary agents use
Be antioxidant 1010.
Embodiment 1
In one embodiment of the invention, this kind of cooperative flame retardant poly lactic acid nano composite material, by as follows according to weight
The raw material of percentage forms:
(1) by polylactic acid particle within the scope of 60-200 DEG C, constant temperature or gradually heating are crystallized 1-20 hours, obtain crystallinity
Polylactic acid particle greater than 60%；
(2) bromide fire retardant, fire retarding synergist, toughener, graphene are dried to 6-12h in 80 DEG C of baking ovens.
(3) substance after being dried in (1) the step of weighing up and (2) is first put into super mixer and carries out dry-mixed 3-
5min。
(4) mixture obtained in step (3) is added twin-screw extrude, carries out melting extrusion granulation, extruder
Temperature of each section is as follows: 140~150 DEG C of an area, two 150~160 DEG C of areas, three 160~170 DEG C of areas, four 160~170 DEG C of areas, 5th area
160~170 DEG C, six 160~170 DEG C of areas, seven 165~175 DEG C of areas, 160~170 DEG C of head temperature, 12~18MPa of pressure, object
Material stops 1~2min in an extruder
Obtained cooperative flame retardant poly lactic acid nano composite material material performance is shown in Table 1.
Embodiment 2
In one embodiment of the invention, this kind of cooperative flame retardant poly lactic acid nano composite material, by as follows according to weight
The raw material of percentage forms:
(1) by polylactic acid particle within the scope of 60-200 DEG C, constant temperature or gradually heating are crystallized 1-20 hours, obtain crystallinity
Polylactic acid particle greater than 60%；
(2) bromide fire retardant, fire retarding synergist, toughener, graphene are dried to 6-12h in 80 DEG C of baking ovens.
(3) substance after being dried in (1) the step of weighing up and (2) is first put into super mixer and carries out dry-mixed 3-
5min。
(4) mixture obtained in step (3) is added twin-screw extrude, carries out melting extrusion granulation, extruder
Temperature of each section is as follows: 140~150 DEG C of an area, two 150~160 DEG C of areas, three 160~170 DEG C of areas, four 160~170 DEG C of areas, 5th area
160~170 DEG C, six 160~170 DEG C of areas, seven 165~175 DEG C of areas, 160~170 DEG C of head temperature, 12~18MPa of pressure, object
Material stops 1~2min in an extruder
Obtained cooperative flame retardant poly lactic acid nano composite material material performance is shown in Table 1.
Embodiment 3
In one embodiment of the invention, this kind of cooperative flame retardant poly lactic acid nano composite material, by as follows according to weight
The raw material of percentage forms:
(1) by polylactic acid particle within the scope of 60-200 DEG C, constant temperature or gradually heating are crystallized 1-20 hours, obtain crystallinity
Polylactic acid particle greater than 60%；
(2) bromide fire retardant, fire retarding synergist, toughener, graphene are dried to 6-12h in 80 DEG C of baking ovens.
(3) substance after being dried in (1) the step of weighing up and (2) is first put into super mixer and carries out dry-mixed 3-
5min。
(4) mixture obtained in step (3) is added twin-screw extrude, carries out melting extrusion granulation, extruder
Temperature of each section is as follows: 140~150 DEG C of an area, two 150~160 DEG C of areas, three 160~170 DEG C of areas, four 160~170 DEG C of areas, 5th area
160~170 DEG C, six 160~170 DEG C of areas, seven 165~175 DEG C of areas, 160~170 DEG C of head temperature, 12~18MPa of pressure, object
Material stops 1~2min in an extruder
Obtained cooperative flame retardant poly lactic acid nano composite material material performance is shown in Table 1.
Embodiment 4
In one embodiment of the invention, this kind of cooperative flame retardant poly lactic acid nano composite material, by as follows according to weight
The raw material of percentage forms:
(1) by polylactic acid particle within the scope of 60-200 DEG C, constant temperature or gradually heating are crystallized 1-20 hours, obtain crystallinity
Polylactic acid particle greater than 60%；
(2) bromide fire retardant, fire retarding synergist, toughener, graphene are dried to 6-12h in 80 DEG C of baking ovens.
(3) substance after being dried in (1) the step of weighing up and (2) is first put into super mixer and carries out dry-mixed 3-
5min。
(4) mixture obtained in step (3) is added twin-screw extrude, carries out melting extrusion granulation, extruder
Temperature of each section is as follows: 140~150 DEG C of an area, two 150~160 DEG C of areas, three 160~170 DEG C of areas, four 160~170 DEG C of areas, 5th area
160~170 DEG C, six 160~170 DEG C of areas, seven 165~175 DEG C of areas, 160~170 DEG C of head temperature, 12~18MPa of pressure, object
Material stops 1~2min in an extruder
Obtained cooperative flame retardant poly lactic acid nano composite material material performance is shown in Table 1.
Embodiment 5
In one embodiment of the invention, this kind of cooperative flame retardant poly lactic acid nano composite material, by as follows according to weight
The raw material of percentage forms:
(1) by polylactic acid particle within the scope of 60-200 DEG C, constant temperature or gradually heating are crystallized 1-20 hours, obtain crystallinity
Polylactic acid particle greater than 60%；
(2) bromide fire retardant, fire retarding synergist, toughener are dried to 6-12h in 80 DEG C of baking ovens.
(3) substance after being dried in (1) the step of weighing up and (2) is first put into super mixer and carries out dry-mixed 3-
5min。
(4) mixture obtained in step (3) is added twin-screw extrude, carries out melting extrusion granulation, extruder
Temperature of each section is as follows: 140~150 DEG C of an area, two 150~160 DEG C of areas, three 160~170 DEG C of areas, four 160~170 DEG C of areas, 5th area
160~170 DEG C, six 160~170 DEG C of areas, seven 165~175 DEG C of areas, 160~170 DEG C of head temperature, 12~18MPa of pressure, object
Material stops 1~2min in an extruder
Obtained cooperative flame retardant poly lactic acid nano composite material material performance is shown in Table 1.
Comparative example 1
In a comparative example of the invention, it is made of the raw material as follows according to weight percent:
Polylactic acid 94.9wt%
Toughener 5wt%
Other auxiliary agents 0.1wt%
As a preferred solution of the present invention, polylactic acid is poly-L-lactic acid, weight average molecular weight 100,000~300,000；Toughener is poly-
Adipic acid butylene terephthalate (PBAT), trade mark C1200.
(1) by polylactic acid particle within the scope of 60-200 DEG C, constant temperature or gradually heating are crystallized 1-20 hours, obtain crystallinity
Polylactic acid particle greater than 60%；
(2) toughener is dried to 6-12h in 80 DEG C of baking ovens.
(3) mixture obtained in step (1) and (2) is added twin-screw extrude, carries out melting extrusion granulation, squeezed
Machine temperature of each section is as follows out: 140~150 DEG C of an area, two 150~160 DEG C of areas, three 160~170 DEG C of areas, four 160~170 DEG C of areas,
Five 160~170 DEG C of areas, six 160~170 DEG C of areas, seven 165~175 DEG C of areas, 160~170 DEG C of head temperature, pressure 12~
18MPa, material stop 1~2min in an extruder
Obtained poly-lactic acid material material performance is shown in Table 1.
Comparative example 2
In a comparative example of the invention, this kind of cooperative flame retardant poly lactic acid nano composite material, by as follows according to weight
The raw material of percentage forms:
As a preferred solution of the present invention, polylactic acid is poly-L-lactic acid, weight average molecular weight 100,000~300,000；Bromide fire retardant
For decabromodiphenylethane (Albemarle Corporation, the U.S.)；Fire retarding synergist is antimony oxide；Toughener is polyadipate terephthaldehyde
Sour fourth diester (PBAT), trade mark C1200.
(1) by polylactic acid particle within the scope of 60-200 DEG C, constant temperature or gradually heating are crystallized 1-20 hours, obtain crystallinity
Polylactic acid particle greater than 60%；
(2) bromide fire retardant, fire retarding synergist, toughener are dried to 6-12h in 80 DEG C of baking ovens.
(3) substance after being dried in (1) the step of weighing up and (2) is first put into super mixer and carries out dry-mixed 3-
5min。
(4) mixture obtained in step (3) is added twin-screw extrude, carries out melting extrusion granulation, extruder
Temperature of each section is as follows: 140~150 DEG C of an area, two 150~160 DEG C of areas, three 160~170 DEG C of areas, four 160~170 DEG C of areas, 5th area
160~170 DEG C, six 160~170 DEG C of areas, seven 165~175 DEG C of areas, 160~170 DEG C of head temperature, 12~18MPa of pressure, object
Material stops 1~2min in an extruder
Obtained cooperative flame retardant poly lactic acid nano composite material material performance is shown in Table 1.
1 cooperative flame retardant poly lactic acid nano composite material physical property of table:
In above embodiments, with the increase of bromide fire retardant additive amount, the tensile strength and impact strength of compound system
It reduces.When bromine system is fire-retardant and graphene is used in compounding, mechanical property increases, while with the increase of graphene content, anti-flammability
It can increase substantially.It is worth mentioning that embodiment 3, not only obtains good tensile strength and impact strength, is also equipped with
Good flame retardant property.Present invention obtains the preferable flame-retardant polylactic acid materials of mechanical property.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by those familiar with the art, all answers
It is included within the scope of protection of the present invention.Therefore, the protection scope that protection scope of the present invention should be defined with claim
Subject to.
Claims (8)
1. a kind of cooperative flame retardant poly lactic acid nano composite material, it is characterised in that: by the raw material including following weight percent meter
It is made:
2. a kind of cooperative flame retardant poly lactic acid nano composite material according to claim 1, it is characterised in that: the polylactic acid
For poly-L-lactic acid, poly- D lactic acid or their blend, weight average molecular weight is 10,000~500,000.
3. a kind of cooperative flame retardant poly lactic acid nano composite material according to claim 1, it is characterised in that: the bromine system
Fire retardant is for brominated epoxy resin, decabromodiphenylethane, brominated Polystyrene etc..
4. a kind of cooperative flame retardant poly lactic acid nano composite material according to claim 1, it is characterised in that: described is fire-retardant
Synergist is environmentally friendly grade antimony oxide.
5. a kind of cooperative flame retardant poly lactic acid nano composite material according to claim 1, it is characterised in that: the graphite
Alkene is graphene oxide, graphene or graphene microchip.
6. a kind of cooperative flame retardant poly lactic acid nano composite material according to claim 1, it is characterised in that: the toughening
Agent is mainly poly butylene succinate (PBS), polycaprolactone (PCL), polyadipate butylene terephthalate (PBAT).
7. a kind of cooperative flame retardant poly lactic acid nano composite material according to claim 1, it is characterised in that: described other help
Agent is mainly antioxidant, and antioxidant is mainly hindered phenol or sulphur ester antioxidant.
8. the preparation method of the cooperative flame retardant poly lactic acid nano composite material described in claim 1-7 is one of any, feature exist
In: specific step is as follows:
(1) each raw material is weighed according to the ratio
(2) by polylactic acid particle within the scope of 60-200 DEG C, constant temperature or gradually heating are crystallized 1-20 hours, are obtained crystallinity and are greater than
60% polylactic acid particle；
(3) bromide fire retardant, fire retarding synergist, toughener, graphene are dried to 6-12h in 80 DEG C of baking ovens.
(4) substance after being dried in (1) the step of weighing up and (2) is first put into super mixer and carries out dry-mixed 3-
5min。
(5) mixture obtained in step (3) is added twin-screw extrude, progress melting extrusion granulation, each section of extruder
Temperature is as follows: 140~150 DEG C of an area, two 150~160 DEG C of areas, three 160~170 DEG C of areas, four 160~170 DEG C of areas, five areas 160
~170 DEG C, six 160~170 DEG C of areas, seven 165~175 DEG C of areas, 160~170 DEG C of head temperature, 12~18MPa of pressure, material exists
1~2min is stopped in extruder.
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| CN103073862A (en) * | 2013-01-10 | 2013-05-01 | 苏州安鸿泰新材料有限公司 | Halogen-free flame-retardant polylactic acid nanocomposite and preparation method thereof |
| EP2671911A1 (en) * | 2012-06-05 | 2013-12-11 | Armacell Enterprise GmbH | A foam material with very low thermal conductivity and a process for manufacturing the foam material |
| CN106566214A (en) * | 2016-10-18 | 2017-04-19 | 安徽省卓煜新材料科技有限公司 | Synergistic flame-retardant polylactic acid nanometer composite material and preparation method thereof |
| WO2017161120A1 (en) * | 2016-03-17 | 2017-09-21 | Qed Labs Inc. | Articles with improved flame retardancy and/or melt dripping properties |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP2671911A1 (en) * | 2012-06-05 | 2013-12-11 | Armacell Enterprise GmbH | A foam material with very low thermal conductivity and a process for manufacturing the foam material |
| CN103073862A (en) * | 2013-01-10 | 2013-05-01 | 苏州安鸿泰新材料有限公司 | Halogen-free flame-retardant polylactic acid nanocomposite and preparation method thereof |
| WO2017161120A1 (en) * | 2016-03-17 | 2017-09-21 | Qed Labs Inc. | Articles with improved flame retardancy and/or melt dripping properties |
| CN106566214A (en) * | 2016-10-18 | 2017-04-19 | 安徽省卓煜新材料科技有限公司 | Synergistic flame-retardant polylactic acid nanometer composite material and preparation method thereof |
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Application publication date: 20190607 |