CN104098879A - Flame-retardant polylactic acid composition and preparation method thereof - Google Patents
Flame-retardant polylactic acid composition and preparation method thereof Download PDFInfo
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- CN104098879A CN104098879A CN201310121199.9A CN201310121199A CN104098879A CN 104098879 A CN104098879 A CN 104098879A CN 201310121199 A CN201310121199 A CN 201310121199A CN 104098879 A CN104098879 A CN 104098879A
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Abstract
The invention specifically relates to a flame-retardant polylactic acid composition and a preparation method thereof, belonging to the technical field of materials. The preparation method comprises the following steps: (1) putting thermoplastic elastomer and processing oil in a ratio of 2: 1 into a high-speed mixer and carrying out high speed mixing; (2) uniformly mixing the mixture obtained in the step (1), a polylactic acid resin, a fire retardant, an assistant fire retardant, an anti-dropping agent and a nucleation promoter under stirring in the manner of dry mixing, then introducing the obtained mixture into a double-screw extruder by using a volumetric feeder, carrying out fusing and mulling, cooling an extruded strip obtained after fusing and mulling with cold water so as to obtain a solid strip and preparing cylindrical particles by using a granulator; and (3) drying the resin composition particles at 80 DEG C in a hot air circulating oven for more than 4 h, preparing a test sample strip by using an injection molding machine and carrying out performance test. The flame-retardant polylactic acid composition prepared by using the method has toughness, strength and flame resistance.
Description
[technical field]
The invention belongs to material technology field, be specifically related to a kind of flame-proof polylactic acid composition and method of making the same.
[background technology]
Poly(lactic acid) (PLA) is a kind of bioabsorbable polymer material taking Biological resources as raw material, can degradablely be carbonic acid gas and water.The production process of poly(lactic acid) does not rely on petroleum resources, and the environmental pressure causing in manufacturing processed is little, has good compostability, biological degradability, has good mechanical property and processing characteristics in addition, thereby obtains in a lot of fields applying more and more widely.
But of poly(lactic acid) itself is not fire-retardant, when burning, molten drop phenomenon can occur.In some special field, as electronic apparatus, automotive trim etc., conventional poly(lactic acid) can not meet service requirements, need to carry out flame-retardant modified to it.
The flame-retardant modified of poly(lactic acid) can add reactive flame retardant and additive flame retardant.Reactive flame retardant large usage quantity, relate to the change of polymerization process condition, more complicated, thereby flame-retardant modified common employing additive flame retardant to poly(lactic acid), and this method is simple, is a kind of most economical method.
Additive flame retardant adds in poly(lactic acid), is mix with resin matrix and exist with the dispersing morphology of physics, thus performance fire retardation.The fire retardant of poly(lactic acid) comprises bromine system, chlorine system, phosphorus system, nitrogen system, silicon system and inorganic combustion inhibitor.Halogen containing flame-retardant is because toxicity is larger, in the time of burning, produces the toxic products such as Dioxins, causes secondary pollution and abandoned.Inorganic combustion inhibitor is that its loading level of flame retardant effect that reaches good must be very high, generally fill out momentum and be greater than 40%, large like this loading level can cause the physical property of poly(lactic acid) greatly to reduce, thereby the flame-retardant modified of poly(lactic acid) is mainly main with phosphorus system, nitrogen system, silicon, but the fire retardants such as ammonium polyphosphate, primary ammonium phosphate, melamine phosphate, polysiloxane promote comparatively effective to the flame retardant effect of poly(lactic acid), but especially very large on the impact of toughness on the over-all properties of poly(lactic acid), make product because crossing the crisp practical value that do not have.
In view of this, be necessary to develop a kind of flame-proof polylactic acid composition in fact, this flame-proof polylactic acid composition is the poly (lactic acid) composition of taking into account toughness, intensity and flame retardant resistance.
[summary of the invention]
Therefore, the object of this invention is to provide a kind of flame-proof polylactic acid composition and method of making the same, making the flame-proof polylactic acid composition obtaining is the poly (lactic acid) composition of taking into account toughness, intensity and flame retardant resistance.
In order to achieve the above object, flame-proof polylactic acid composition of the present invention, calculates by weight, and it comprises following component:
70～150 parts of polylactic resin;
1～40 part of fire retardant;
0～20 part of auxiliary flame retardant;
1～30 part of thermoplastic elastomer;
0.1～30 part of nucleation accelerating agent.
Alternatively, described polylactic resin is L-type or D type polylactic resin.
Alternatively, fire retardant chemical formula is [OC6H3 (CH3) 2] 2P (O) OC6H4OP (O) [OC6H3 (CH3) 2] 2, and this fire retardant is preferably 15～30 weight parts.
Alternatively, described auxiliary flame retardant is melamine pyrophosphate salt or ammonium polyphosphate.
Alternatively, the weight ratio of described fire retardant and auxiliary flame retardant is 2～10.
Alternatively, described flame-proof polylactic acid composition also comprises the anti-dripping agent of 0～0.8 weight part, and this anti-vertical agent is fluoro-containing composition or fluoropolymer, is wherein preferably tetrafluoroethylene, is preferably 0.1～0.5 weight part.
Alternatively, described thermoplastic elastomer is styrene-ethylene-butadiene-styrene copolymer compound, styrene-ethylene-propylene-styrene copolymerisation thing, styrene-butadiene-styrene co-polymer, styrene-isoprene-phenylethene co-polymer, styrene butadiene rubbers, ethylene-propylene rubber, divinyl rubber, synthetic polyisoprene, paracril, acryl rubber, ethene-acryl rubber, silicon rubber, fluorine unpigmented rubber, vulcanized rubber, dynamic perduren, natural rubber, ethylene-propylene-butylene elastomerics, polyolefin elastomerics, polyvinyl chloride based elastomers, polyamide-based elastomerics, polyester based elastomers, polyester-polyethers based elastomers, polyurethane series elastomerics, mixture a kind of or that formed by above thermoplastic elastomer in fluorine prime system elastomerics, be preferably styrene-ethylene-butadiene-styrene copolymer compound.
Alternatively, described crystallization promoter is the mixture a kind of or that be made up of above crystallization promoter in talcum powder, mica, polynite, barium sulfate, calcium carbonate, silicon-dioxide, aluminium hydroxide, aluminum oxide, aluminium carbonate, be preferably talcum powder, be preferably 0.5～15 weight part.
Alternatively, described flame-proof polylactic acid composition also comprises the processing aid of 1～10 weight part, and this processing aid is a kind of or its mixture in expanding material, chainextender, antioxidant, UV light stabilizing agent, resistant to hydrolysis stablizer, thermo-stabilizer, agent for slow releasing, static inhibitor, wetting agent, tinting material, lubricant.
The present invention also provides a kind of preparation method of flame-proof polylactic acid composition, and the method comprises the following steps:
(1) by weight with the ratio of 2:1, thermoplastic elastomer and treated oil being positioned in high-speed mixer and doing high-speed mixing, until treated oil and thermoplastic elastomer reach even admixture, take out for subsequent use;
(2) mixture in proportion step (1) being obtained and polylactic resin, fire retardant, auxiliary flame retardant, nucleation accelerating agent first stir to be dry mixed mode, import and under the condition of 180～210 ° of C, carry out the melting processing of mixing in twin screw extruder with positive displacement feeder afterwards, melting mix processing after gained extrude bar be cooled to through cold water solid-state, with tablets press make cylindrical particle;
(3) by above-mentioned resin combination particle under the condition of 80 ° of C, dry more than 4 hours in Hotaircirculatingoven, then use Jet forming machine to be made into test bars, and performance test.
Alternatively, in described step (1): treated oil is the mixture a kind of or that be made up of above treated oil in paraffinic base series treated oil, aromatic series series treated oil, epoxy soybean oil, glycerine, be preferably paraffinic base series treated oil, its molecular weight is between 100～3000.
Compared to prior art, flame-proof polylactic acid composition and method of making the same of the present invention, make the poly (lactic acid) composition obtaining take into account toughness, intensity and flame retardant resistance, and meet environmental requirement, wherein flame retardant rating all can reach 1.6mmV-0, can be widely used in mechanism's part products such as electronics, household electrical appliances, automotive trim.
[embodiment]
The invention is further illustrated by the following examples, and the raw material wherein using in comparative example and embodiment is specially:
(1) polylactic resin: NatureWorks company of U.S. system, specification: 4032D.
(2) condensation polymer type non-halogen phosphoric acid ester combustion inhibitor: Japanese Daihachi Chemical Industry Co., Ltd. system, specification: PX-200, chemical formula is [OC
6h
3(CH
3)
2]
2p (O) OC
6h
4oP (O) [OC
6h
3(CH
3)
2]
2.
(3) auxiliary flame retardant melamine pyrophosphate salt: Hai great Chemical Co., Ltd. of Qingdao City system, specification 11-2.
(4) an anti-vertical agent tetrafluoroethylene: GuangZhou, China Shang Neng polymkeric substance Science and Technology Ltd. system, specification: Shinepoly SN3300.
(5) thermoplastic elastic body styrene-ethylene-butadiene-styrene co-polymer: Taiwan rubber limited-liability company system, specification: SEBS6151.
(6) paraffinic base treated oil: Sun Oil Company of U.S. system, specification: Sunpar 2280.
(7) talcum powder: Kunshan Run Shi Chemical Co., Ltd. system, specification: RS-888A.
Comparative example 1
It in comparative example 1, is the pure polylactic resin of 100 weight parts.
Embodiment 1
(1) by weight with the ratio of 2:1, styrene-ethylene-butadiene-styrene copolymer compound and paraffin treated oil being positioned over and doing high-speed mixing in high-speed mixer, within approximately 10 minutes, post-treatment oil reaches even admixture with styrene-ethylene-butadiene-styrene copolymer compound, takes out for subsequent use;
(2) get mixture 20 weight parts that step (1) obtains and polylactic resin 100 weight parts, phosphate flame retardant 20 weight parts, talcum powder 5 weight parts first stir to be dry mixed mode, import and under the condition of 180～210 ° of C, carry out the melting processing of mixing in twin screw extruder with positive displacement feeder afterwards, melting mix processing after gained extrude bar be cooled to through cold water solid-state, with tablets press make cylindrical particle;
(3) by above-mentioned resin combination particle under the condition of 80 ° of C, dry more than 4 hours in Hotaircirculatingoven, then use Jet forming machine to be made into test bars, and performance test.
Embodiment 2
(1) by weight with the ratio of 2:1, styrene-ethylene-butadiene-styrene copolymer compound and paraffin treated oil being positioned over and doing high-speed mixing in high-speed mixer, within approximately 10 minutes, post-treatment oil reaches even admixture with styrene-ethylene-butadiene-styrene copolymer compound, takes out for subsequent use;
(2) get mixture 20 weight parts that step (1) obtains and polylactic resin 100 weight parts, phosphate flame retardant 30 weight parts, talcum powder 5 weight parts first stir to be dry mixed mode, import and under the condition of 180～210 ° of C, carry out the melting processing of mixing in twin screw extruder with positive displacement feeder afterwards, melting mix processing after gained extrude bar be cooled to through cold water solid-state, with tablets press make cylindrical particle;
(3) by above-mentioned resin combination particle under the condition of 80 ° of C, dry more than 4 hours in Hotaircirculatingoven, then use Jet forming machine to be made into test bars, and performance test.
Embodiment 3
(1) by weight with the ratio of 2:1, styrene-ethylene-butadiene-styrene copolymer compound and paraffin treated oil being positioned over and doing high-speed mixing in high-speed mixer, within approximately 10 minutes, post-treatment oil reaches even admixture with styrene-ethylene-butadiene-styrene copolymer compound, takes out for subsequent use;
(2) get mixture 20 weight parts that step (1) obtains and polylactic resin 100 weight parts, phosphate flame retardant 20 weight parts, auxiliary flame retardant melamine pyrophosphate salt 5 weight parts, talcum powder 5 weight parts first stir to be dry mixed mode, import and under the condition of 180～210 ° of C, carry out the melting processing of mixing in twin screw extruder with positive displacement feeder afterwards, melting mix processing after gained extrude bar be cooled to through cold water solid-state, with tablets press make cylindrical particle;
(3) by above-mentioned resin combination particle under the condition of 80 ° of C, dry more than 4 hours in Hotaircirculatingoven, then use Jet forming machine to be made into test bars, and performance test.
Embodiment 4
(1) by weight with the ratio of 2:1, styrene-ethylene-butadiene-styrene copolymer compound and paraffin treated oil being positioned over and doing high-speed mixing in high-speed mixer, within approximately 10 minutes, post-treatment oil reaches even admixture with styrene-ethylene-butadiene-styrene copolymer compound, takes out for subsequent use;
(2) get mixture 20 weight parts that step (1) obtains and polylactic resin 100 weight parts, phosphate flame retardant 20 weight parts, auxiliary flame retardant melamine pyrophosphate salt 5 weight parts, talcum powder 5 weight parts, anti-dripping agent tetrafluoroethylene 0.4 weight part first stirs to be dry mixed mode, import and under the condition of 180～210 ° of C, carry out the melting processing of mixing in twin screw extruder with positive displacement feeder afterwards, melting mix processing after gained extrude bar be cooled to through cold water solid-state, with tablets press make cylindrical particle;
(3) by above-mentioned resin combination particle under the condition of 80 ° of C, dry more than 4 hours in Hotaircirculatingoven, then use Jet forming machine to be made into test bars, and performance test.
Flame retardant properties and the mechanical property of the composition that comparative example and each embodiment are obtained are tested, wherein testing standard is: according to the requirement of GB/T1040-2006, the tensile strength of test material under the condition of 10mm/min, according to the requirement of GB/T9341-2008, the flexural strength of test material and modulus in flexure under the condition of 2mm/min, according to the requirement of GB/T1843-2008, under the condition of thickness of test piece 4mm, carry out the shock strength of the A type breach of material, according to plastic material combustion testing in UL-94 and criteria for classification specification, under the condition of thickness of test piece 1.6mm, carry out combustion testing and the flame retardant rating classification of material, test result is as shown in table 1:
Table 1: comparative example and embodiment test result
| Test event | Comparative example 1 | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Tensile strength MPa | 64 | 45 | 44 | 47 | 47 |
| Flexural strength MPa | 91 | 78 | 77 | 77 | 80 |
| Modulus in flexure MPa | 3050 | 3410 | 3550 | 3600 | 3580 |
| Notched Izod impact strength KJ/m 2 | 2.0 | 15 | 10 | 11 | 10 |
| Flame retardant rating | V-2 | V-2 | V-0 | V-0 | V-0 |
| Drip and hang down | Be | Be | Be | Be | No |
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various amendments to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are as announcement of the present invention, and the improvement of making for the present invention or amendment all should be within protection scope of the present invention.
Claims (11)
1. a flame-proof polylactic acid composition, is characterized in that, calculates by weight, comprises following component:
2. flame-proof polylactic acid composition as claimed in claim 1, is characterized in that, described polylactic resin is L-type or D type polylactic resin.
3. flame-proof polylactic acid composition as claimed in claim 1, is characterized in that, fire retardant chemical formula is [OC6H3 (CH3) 2] 2P (O) OC6H4OP (O) [OC6H3 (CH3) 2] 2.
4. flame-proof polylactic acid composition as claimed in claim 1, is characterized in that, described auxiliary flame retardant is melamine pyrophosphate salt or ammonium polyphosphate.
5. flame-proof polylactic acid composition as claimed in claim 1, is characterized in that, the weight ratio of described fire retardant and auxiliary flame retardant is 2～10.
6. flame-proof polylactic acid composition as claimed in claim 1, is characterized in that, described flame-proof polylactic acid composition also comprises the anti-dripping agent of 0～0.8 weight part, and this anti-vertical agent is fluoro-containing composition or fluoropolymer.
7. flame-proof polylactic acid composition as claimed in claim 1, it is characterized in that, described thermoplastic elastomer is styrene-ethylene-butadiene-styrene copolymer compound, styrene-ethylene-propylene-styrene copolymerisation thing, styrene-butadiene-styrene co-polymer, styrene-isoprene-phenylethene co-polymer, styrene butadiene rubbers, ethylene-propylene rubber, divinyl rubber, synthetic polyisoprene, paracril, acryl rubber, ethene-acryl rubber, silicon rubber, fluorine unpigmented rubber, vulcanized rubber, dynamic perduren, natural rubber, ethylene-propylene-butylene elastomerics, polyolefin elastomerics, polyvinyl chloride based elastomers, polyamide-based elastomerics, polyester based elastomers, polyester-polyethers based elastomers, polyurethane series elastomerics, mixture a kind of or that formed by above thermoplastic elastomer in fluorine prime system elastomerics.
8. flame-proof polylactic acid composition as claimed in claim 1, it is characterized in that, described crystallization promoter is the mixture a kind of or that be made up of above crystallization promoter in talcum powder, mica, polynite, barium sulfate, calcium carbonate, silicon-dioxide, aluminium hydroxide, aluminum oxide, aluminium carbonate.
9. flame-proof polylactic acid composition as claimed in claim 1, it is characterized in that, described flame-proof polylactic acid composition also comprises the processing aid of 1～10 weight part, and this processing aid is a kind of or its mixture in expanding material, chainextender, antioxidant, UV light stabilizing agent, resistant to hydrolysis stablizer, thermo-stabilizer, agent for slow releasing, static inhibitor, wetting agent, tinting material, lubricant.
10. a preparation method for flame-proof polylactic acid composition as claimed in claim 1, is characterized in that, comprises the following steps:
(1) by weight with the ratio of 2:1, thermoplastic elastomer and treated oil being positioned in high-speed mixer and doing high-speed mixing, until treated oil and thermoplastic elastomer reach even admixture, take out for subsequent use;
(2) mixture in proportion step (1) being obtained and polylactic resin, fire retardant, auxiliary flame retardant, nucleation accelerating agent first stir to be dry mixed mode, import and under the condition of 180～210 ° of C, carry out the melting processing of mixing in twin screw extruder with positive displacement feeder afterwards, melting mix processing after gained extrude bar be cooled to through cold water solid-state, with tablets press make cylindrical particle;
(3) by above-mentioned resin combination particle under the condition of 80 ° of C, dry more than 4 hours in Hotaircirculatingoven, then use Jet forming machine to be made into test bars, and performance test.
The preparation method of 11. flame-proof polylactic acid compositions as claimed in claim 10, it is characterized in that, in described step (1): treated oil is the mixture a kind of or that be made up of above treated oil in paraffinic base series treated oil, aromatic series series treated oil, epoxy soybean oil, glycerine.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105862495A (en) * | 2016-04-28 | 2016-08-17 | 句容市鼎盛纸箱包装有限公司 | Preparation method of flame-retardant regenerated paperboard |
| CN105904778A (en) * | 2016-04-28 | 2016-08-31 | 句容市鼎盛纸箱包装有限公司 | Preparation method for degradable flame-retardant honeycomb paperboard |
| CN105924913A (en) * | 2016-04-28 | 2016-09-07 | 句容市鼎盛纸箱包装有限公司 | Preparation method of degradable moistureproof flame-retardant honeycomb paperboard |
| CN106245147A (en) * | 2016-08-02 | 2016-12-21 | 长兴德诚纺织有限公司 | A kind of flame-proof polylactic acid fabric lining |
| CN106317729A (en) * | 2016-08-25 | 2017-01-11 | 周荣 | Preparation method of thermoplastic vulcanized rubber |
| CN105038164B (en) * | 2015-08-18 | 2017-06-06 | 华南理工大学 | PLA base intermingling material and preparation method thereof and the method that expanded material is prepared by it |
| CN107383817A (en) * | 2017-08-23 | 2017-11-24 | 广东波斯科技股份有限公司 | A kind of Biodegradable low-cost flame-retardant 3D printing consumptive material and its preparation method and application |
| CN110903491A (en) * | 2019-12-12 | 2020-03-24 | 湖南绿燊环保科技有限公司 | Flame retardant, modified polylactic acid and preparation method thereof |
| CN114981358A (en) * | 2020-01-16 | 2022-08-30 | 弗洛里昂转换包装有限公司 | Polylactic acid flame retardant blend |
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Cited By (9)
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|---|---|---|---|---|
| CN105038164B (en) * | 2015-08-18 | 2017-06-06 | 华南理工大学 | PLA base intermingling material and preparation method thereof and the method that expanded material is prepared by it |
| CN105862495A (en) * | 2016-04-28 | 2016-08-17 | 句容市鼎盛纸箱包装有限公司 | Preparation method of flame-retardant regenerated paperboard |
| CN105904778A (en) * | 2016-04-28 | 2016-08-31 | 句容市鼎盛纸箱包装有限公司 | Preparation method for degradable flame-retardant honeycomb paperboard |
| CN105924913A (en) * | 2016-04-28 | 2016-09-07 | 句容市鼎盛纸箱包装有限公司 | Preparation method of degradable moistureproof flame-retardant honeycomb paperboard |
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| CN106317729A (en) * | 2016-08-25 | 2017-01-11 | 周荣 | Preparation method of thermoplastic vulcanized rubber |
| CN107383817A (en) * | 2017-08-23 | 2017-11-24 | 广东波斯科技股份有限公司 | A kind of Biodegradable low-cost flame-retardant 3D printing consumptive material and its preparation method and application |
| CN110903491A (en) * | 2019-12-12 | 2020-03-24 | 湖南绿燊环保科技有限公司 | Flame retardant, modified polylactic acid and preparation method thereof |
| CN114981358A (en) * | 2020-01-16 | 2022-08-30 | 弗洛里昂转换包装有限公司 | Polylactic acid flame retardant blend |
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