CN104693706A - Heat resistance increased impact resistant polylactic acid modified material and preparation method thereof - Google Patents
Heat resistance increased impact resistant polylactic acid modified material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polylactic acid modified material comprising the following components by weight: 100 parts of polylactic acid, 20-30 parts of modified calcium carbonate, 10-20 parts of a plasticizer, 1.0-2.0 parts of an ultraviolet absorbent, 0.5-1.0 part of an antioxidant, 8-15 parts of an impact resistant modifying agent and 4-8 parts of a processing aid. The preparation method is as follows: mixing the 100 parts of polylactic acid, 8-15 parts of the impact resistant modifying agent and 4-8 parts of the processing aid in a high mixing machine for 3 to 5 minutes, adding the 20-30 parts of modified calcium carbonate, 10-20 parts of the plasticizer, 1.0-2.0 parts of the ultraviolet absorbent and 0.5-1.0 part of the antioxidant into the high mixing machine for mixing for 5-8 minutes, wherein the high mixing machine mixing temperature is 80 to 90 DEG C; cooling the mixture to 50 DEG C below, adding into a double screw extruder from a main feeding port, wherein the extrusion temperature is 180 to 220 DEG C, extruding to obtain the polylactic acid modified material, cooling with water, cutting, drying, sealing and packaging. The mechanical strength of the polylactic acid modified material can be improved, heat resistance can be improved, and the polylactic acid impact resistant property can be greatly improved.
Description
Technical field
The present invention relates to field of high polymer material modification and processing technique field, be specifically related to a kind of heat-resisting enhancing shock resistance modified polylactic acid material and preparation method thereof.
Background technology
Along with industrial production and scientific and technical development, plastics are absolutely necessary in people's daily life, and based on our population base, China is plastics consumption big country in the whole world.But conventional plastic goods simultaneously also pollute environment easily bringing people, general plastics needed the upper century-old even longer time could be degradable, result in serious " white pollution ".Meanwhile, traditional plastic raw materials all derives from the Nonrenewable resources such as oil, and the traditional plastics industry of the exhaustion along with fossil resources also receives threat.Therefore, the eco-friendly biodegradable polymkeric substance petroleum replacing base plastic prod of Devoting Major Efforts To Developing, has become the focus of current research exploitation.
In the bio-degradable plastics developed at present, poly(lactic acid) is a kind of bio-based plastics that can be degradable.Because poly(lactic acid) can be generated by renewable resources fermentations such as W-Gums, there is again excellent biodegradability, make it be subject to paying close attention to more and more widely in alternative petrochemical industry macromolecular material, can be used for the fields such as biomedicine, packaging, clothes, agroforestry, catering trade.Although poly(lactic acid) has excellent degradability and biocompatibility, the crisp poor toughness of poly(lactic acid) matter, lack flexible and elasticity, very easily flexural deformation, heat resisting temperature is too low, strongly limit its development and use range, so need to carry out modification to poly(lactic acid).
Traditional polylactic acid modified method is by poly(lactic acid) and other superpolymer or adds mineral filler, by simply mixing, complete processing is without specific requirement, some performance of poly(lactic acid) can only be improved, be difficult to the shock resistance simultaneously improving poly(lactic acid), heat-resisting and mechanical property etc., therefore common poly(lactic acid) is difficult to the application requiring meeting various industry, as automobile, household electrical appliances, the industries such as building, to the requirement that plastic material has some higher, in the mechanical property of material, even to reach or close to the level of engineering plastics, and in the engineering process of poly-lactic acid material, the most scabrous problem is ensureing that material has higher toughness, higher resistance toheat is also needed while excellent mechanical stretching performance, therefore also need constantly to carry out modification to improve over-all properties to poly-lactic acid material.
Summary of the invention
In order to overcome the defect of prior art, the object of this invention is to provide one and there is heat-resisting enhancing shock resistance modified polylactic acid material.
Another object of the present invention is to provide a kind of preparation method of above-mentioned heat-resisting enhancing shock resistance modified polylactic acid material.
To achieve these goals, technical scheme of the present invention is as follows:
The invention provides a kind of heat-resisting enhancing shock resistance modified polylactic acid material, be made up of the component comprising following weight part:
Described poly(lactic acid) comprises the Poly-L-lactic acid and dextrorotation poly(lactic acid) that mass ratio is 4:1 ~ 4:2.
Described modified calcium carbonate is made up of the component of following weight part: 100 parts, calcium carbonate, promotor 3 ~ 5 parts, stearic acid 5 ~ 8 parts, 10 ~ 20 parts, calcium oxide.
Described promotor comprises the carboxylated polyethylene wax and polyacrylamide that mass ratio is 1:1.
Described softening agent be selected from hexanaphthene-1,2-dicarboxyl dinonyl, diphenyl phthalate or SA dibutylester one or more.
Described UV light absorber be selected from 4-benzoyloxy-2,2,6,6-tetramethyl piperidine, tricresyl phosphite (1,2,2,6,6-pentamethvl) ester or Whitfield's ointment-4-tertiary butyl phenyl ester one or more.
Described oxidation inhibitor be selected from thio-2 acid octadecyl ester, [β-(3,5 di-t-butyl 4-hydroxy-pheny) propionic acid] pentaerythritol ester or Tyox B one or more.
Described anti-impact modifier be selected from maleic anhydride grafted ethene/propylene copolymer, the multipolymer of maleic anhydride grafted ethene-propylenediene terpolymer, vinylbenzene and divinyl or ethene and acrylonitrile copolymer one or more.
Described processing aid be selected from stearic acid, Zinic stearas, calcium stearate or erucicamide one or more.
Present invention also offers a kind of preparation method of above-mentioned heat-resisting enhancing shock resistance modified polylactic acid material, comprise the following steps:
By 100 parts of poly(lactic acid), 8 ~ 15 parts of anti-impact modifiers and 4 ~ 8 parts of processing aids high-speed mixer and mixing 3 ~ 5 minutes, then 20 ~ 30 parts of modified calcium carbonates, 10 ~ 20 parts of softening agent, 1.0 ~ 2.0 parts of UV light absorber are joined high mixer with 0.5 ~ 1.0 part of oxidation inhibitor and mix 5 ~ 8 minutes, wherein the mixing temperature of high mixer is 80 ~ 90 DEG C; Said mixture is cooled to less than 50 DEG C, joins in twin screw extruder by main charging opening, extrusion temperature is 180 ~ 220 DEG C, obtains modified polylactic acid material after extruding, through water-cooled, pelletizing, then dry, pack.
Described poly(lactic acid) is the poly(lactic acid) matrix of the blended composition of ratio being 4:1 ~ 4:2 with mass ratio by Poly-L-lactic acid and dextrorotation poly(lactic acid), pulverizes 500 mesh sieves, and obtains polylactic acid powder.
The preparation method of described modified calcium carbonate comprises the following steps: first add in high-speed mixer by 100 parts of calcium carbonate, at 100 ~ 110 DEG C of dry 30min, add 5 ~ 8 parts of stearic acid, 3 ~ 5 parts of promotor and 10 ~ 20 parts of calcium oxide again, obtain modified calcium carbonate after high-speed mixing 10 ~ 15min, described promotor comprises the carboxylated polyethylene wax and polyacrylamide that mass ratio is 1:1.
The screw slenderness ratio of described twin screw extruder is 30:1, and screw speed is 80 ~ 120r/min.
Compared with prior art, beneficial effect of the present invention is as follows:
Heat-resisting enhancing shock resistance modified polylactic acid material of the present invention adopts and adds modified calcium carbonate, improve the interaction between common polarity inorganic and nonpolar poly(lactic acid) matrix, make inorganic carbonate calcium dispersed in organic poly(lactic acid) matrix, greatly improve thermotolerance and the physical strength of poly-lactic acid material.The anti-impact modifier added improves the impelling strength of poly(lactic acid), and in the course of processing, does not destroy the crystalline structure of poly(lactic acid) and reduce the intensity of material; The efficient combination of UV light absorber and oxidation inhibitor adds, and enhances the weather resistance of poly(lactic acid), extends the work-ing life of polylactic acid article.Thus, the present invention not only makes the thermotolerance of poly-lactic acid material obviously promote, and also drastically increases toughness and physical strength, can be widely used in over-all properties and require higher field, and preparation is simple, be applicable to suitability for industrialized production.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation.
GB(GB is adopted in following examples) measure the properties of material, if no special instructions, the number of component is parts by weight.
Embodiment 1
(1) calcium carbonate pre-treatment: first 100 parts, calcium carbonate is added in high-speed mixer, at 100 ~ 110 DEG C of dry 30min, then add stearic acid 6 parts, promotor 5 parts, 15 parts, calcium oxide, high-speed mixing 10min, obtains modified calcium carbonate; Promotor comprises the carboxylated polyethylene wax and polyacrylamide that mass ratio is 1:1.
(2) the poly(lactic acid) matrix of Poly-L-lactic acid 75 parts and dextrorotation poly(lactic acid) 25 parts of blended compositions is pulverized 500 mesh sieves, obtain polylactic acid powder;
(3) by polylactic acid powder 100 parts, maleic anhydride grafted ethene-propylenediene terpolymer 10 parts and Zinic stearas 4 parts high-speed mixer and mixing 3 minutes, then by modified calcium carbonate 20 parts, hexanaphthene-1,2-dicarboxyl dinonyl 15 parts, tricresyl phosphite (1,2,2,6,6-pentamethvl) ester 1.2 parts joins high mixer with Tyox B 1.0 parts and mixes 5 minutes, and wherein the mixing temperature of high mixer is at 90 DEG C;
(4) after mixing, said mixture is cooled to less than 50 DEG C, twin screw extruder is joined by main charging opening, extrusion temperature is 190 ~ 210 DEG C, screw slenderness ratio is 30:1, and screw speed is 100r/min, obtains modified polylactic acid material after extruding, through water-cooled, pelletizing, then dry, pack.
Modified polylactic acid material is injection molded into sample, tests its correlated performance, the results are shown in Table 1.
Embodiment 2
(1) modified calcium carbonate pre-treatment: first 100 parts, calcium carbonate is added in high-speed mixer, at 100 ~ 110 DEG C of dry 30min, then add stearic acid 5 parts, promotor 3 parts, 10 parts, calcium oxide, high-speed mixing 12min, obtains modified calcium carbonate; Promotor comprises the carboxylated polyethylene wax and polyacrylamide that mass ratio is 1:1.
(2) the poly(lactic acid) matrix of Poly-L-lactic acid 80 parts and dextrorotation poly(lactic acid) 20 parts of blended compositions is pulverized 500 mesh sieves, obtain polylactic acid powder;
(3) by the multipolymer 8 parts of polylactic acid powder 100 parts, vinylbenzene and divinyl and erucicamide 6 parts high-speed mixer and mixing 4 minutes, then by modified calcium carbonate 22 parts, SA dibutylester 12 parts, Whitfield's ointment-4-tertiary butyl phenyl ester 1.0 parts and [β-(3,5 di-t-butyl 4-hydroxy-pheny) propionic acid] pentaerythritol ester 0.8 part joins high mixer and mixes 6 minutes, and wherein the mixing temperature of high mixer is at 80 DEG C;
(4) after mixing, said mixture is cooled to less than 50 DEG C, twin screw extruder is joined by main charging opening, extrusion temperature is 180 ~ 200 DEG C, screw slenderness ratio is 30:1, and screw speed is 120r/min, obtains modified polylactic acid material after extruding, through water-cooled, pelletizing, then dry, pack.
Modified polylactic acid material is injection molded into sample, tests its correlated performance, the results are shown in Table 1.
Embodiment 3
(1) modified calcium carbonate pre-treatment: first 100 parts, calcium carbonate is added in high-speed mixer, at 100 ~ 110 DEG C of dry 30min, then add stearic acid 8 parts, promotor 4 parts, 15 parts, calcium oxide, high-speed mixing 15min, obtains modified calcium carbonate; Promotor comprises the carboxylated polyethylene wax and polyacrylamide that mass ratio is 1:1.
(2) the poly(lactic acid) matrix of Poly-L-lactic acid 67 parts and dextrorotation poly(lactic acid) 33 parts of blended compositions is pulverized 500 mesh sieves, obtain polylactic acid powder;
(3) by polylactic acid powder 100 parts, ethene and acrylonitrile copolymer 15 parts and calcium stearate 8 parts high-speed mixer and mixing 5 minutes, then by modified calcium carbonate 25 parts, hexanaphthene-1,2-dicarboxyl dinonyl 10 parts, tricresyl phosphite (1,2,2,6,6-pentamethvl) ester 1.5 parts joins high mixer with Tyox B 0.5 part and mixes 8 minutes, and wherein the mixing temperature of high mixer is at 80 DEG C;
(4) after mixing, said mixture is cooled to less than 50 DEG C, twin screw extruder is joined by main charging opening, extrusion temperature is 190 ~ 210 DEG C, screw slenderness ratio is 30:1, and screw speed is 100r/min, obtains modified polylactic acid material after extruding, through water-cooled, pelletizing, then dry, pack.
Modified polylactic acid material is injection molded into sample, tests its correlated performance, the results are shown in Table 1.
Embodiment 4
(1) modified calcium carbonate pre-treatment: first 100 parts, calcium carbonate is added in high-speed mixer, at 100 ~ 110 DEG C of dry 30min, then add stearic acid 6 parts, promotor 5 parts, 15 parts, calcium oxide, high-speed mixing 15min, obtains modified calcium carbonate; Promotor comprises the carboxylated polyethylene wax and polyacrylamide that mass ratio is 1:1.
(2) the poly(lactic acid) matrix of Poly-L-lactic acid 72 parts and dextrorotation poly(lactic acid) 28 parts of blended compositions is pulverized 500 mesh sieves, obtain polylactic acid powder;
(3) by polylactic acid powder 100 parts, maleic anhydride grafted ethene-propylenediene terpolymer 10 parts and Zinic stearas 6 parts high-speed mixer and mixing 4 minutes, then by modified calcium carbonate 30 parts, hexanaphthene-1,2-dicarboxyl dinonyl 20 parts, Whitfield's ointment-4-tertiary butyl phenyl ester 2.0 parts and [β-(3,5 di-t-butyl 4-hydroxy-pheny) propionic acid] pentaerythritol ester 0.8 part joins high mixer and mixes 8 minutes, and wherein the mixing temperature of high mixer is at 85 DEG C;
(4) after mixing, said mixture is cooled to less than 50 DEG C, twin screw extruder is joined by main charging opening, extrusion temperature is 200 ~ 220 DEG C, screw slenderness ratio is 30:1, and screw speed is 80r/min, obtains modified polylactic acid material after extruding, through water-cooled, pelletizing, then dry, pack.
Modified polylactic acid material is injection molded into sample, tests its correlated performance, the results are shown in Table 1.
Embodiment 5
(1) modified calcium carbonate pre-treatment: first 100 parts, calcium carbonate is added in high-speed mixer, at 100 ~ 110 DEG C of dry 30min, then add stearic acid 8 parts, promotor 4 parts, 20 parts, calcium oxide, high-speed mixing 12min, obtains modified calcium carbonate; Promotor comprises the carboxylated polyethylene wax and polyacrylamide that mass ratio is 1:1.
(2) the poly(lactic acid) matrix of Poly-L-lactic acid 70 parts and dextrorotation poly(lactic acid) 30 parts of blended compositions is pulverized 500 mesh sieves, obtain polylactic acid powder;
(3) by the copolymer 12 parts of polylactic acid powder 100 parts, vinylbenzene and divinyl and calcium stearate 8 parts high-speed mixer and mixing 5 minutes, then by modified calcium carbonate 28 parts, SA dibutylester 18 parts, tricresyl phosphite (1,2,2,6,6-pentamethvl) ester 1.5 parts joins high mixer with Tyox B 0.6 part and mixes 5 minutes, and wherein the mixing temperature of high mixer is at 90 DEG C;
(4) after mixing, said mixture is cooled to less than 50 DEG C, twin screw extruder is joined by main charging opening, extrusion temperature is 190 ~ 210 DEG C, screw slenderness ratio is 30:1, and screw speed is 90r/min, obtains modified polylactic acid material after extruding, through water-cooled, pelletizing, then dry, pack.
Modified polylactic acid material is injection molded into sample, tests its correlated performance, the results are shown in Table 1.
Comparative example 1
The difference part of this comparative example and embodiment 3 is, in the preparation of mixture, do not add anti-impact modifier.All the other components, temperature of reaction, time and step are all identical.The properties of the modified polylactic acid material that this comparative example obtains is in table 1.
Comparative example 2
The difference part of this comparative example and embodiment 4 is, in the preparation of mixture, do not add modified calcium carbonate.All the other components, temperature of reaction, time and step are all identical.The properties of the modified polylactic acid material that this comparative example obtains is in table 1.
Table 1
Can be found out by data every in table 1, embodiment 4 and 5 all keeps toughness, mechanics physical strength and the higher vicat softening temperature that modified polylactic acid material is good, and over-all properties reaches best.By the contrast of comparative example 1 and embodiment 3, its notched Izod impact strength of modified polylactic acid material and the elongation that find not add anti-impact modifier decline to a great extent; By the contrast of comparative example 2 and embodiment 4, find that its tensile strength of modified polylactic acid material of not adding modified calcium carbonate significantly decays, vicat softening temperature also decreases.
Embodiment 6
(1) modified calcium carbonate pre-treatment: first 100 parts, calcium carbonate is added in high-speed mixer, at 100 ~ 110 DEG C of dry 30min, then add stearic acid 7 parts, promotor 4 parts, 18 parts, calcium oxide, high-speed mixing 12min, obtains modified calcium carbonate; Promotor comprises the carboxylated polyethylene wax and polyacrylamide that mass ratio is 1:1.
(2) the poly(lactic acid) matrix of Poly-L-lactic acid 70 parts and dextrorotation poly(lactic acid) 30 parts of blended compositions is pulverized 500 mesh sieves, obtain polylactic acid powder;
(3) by polylactic acid powder 100 parts, maleic anhydride grafted ethene/propylene copolymer 13 parts and stearic acid 7 parts high-speed mixer and mixing 5 minutes, then by modified calcium carbonate 26 parts, diphenyl phthalate 16 parts, 4-benzoyloxy-2,2,6,6-tetramethyl piperidine 1.8 parts joins high mixer with thio-2 acid octadecyl ester 0.7 part and mixes 5 minutes, and wherein the mixing temperature of high mixer is at 90 DEG C;
(4) after mixing, said mixture is cooled to less than 50 DEG C, twin screw extruder is joined by main charging opening, extrusion temperature is 190 ~ 210 DEG C, screw slenderness ratio is 30:1, and screw speed is 90r/min, obtains modified polylactic acid material after extruding, through water-cooled, pelletizing, then dry, pack.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (10)
1. a heat-resisting enhancing shock resistance modified polylactic acid material, is characterized in that: be made up of the component comprising following weight part:
2. heat-resisting enhancing shock resistance modified polylactic acid material according to claim 1, is characterized in that: described poly(lactic acid) comprises the Poly-L-lactic acid and dextrorotation poly(lactic acid) that mass ratio is 4:1 ~ 4:2.
3. heat-resisting enhancing shock resistance modified polylactic acid material according to claim 1, is characterized in that: described modified calcium carbonate is made up of the component of following weight part: 100 parts, calcium carbonate, promotor 3 ~ 5 parts, stearic acid 5 ~ 8 parts, 10 ~ 20 parts, calcium oxide.
4. heat-resisting enhancing shock resistance modified polylactic acid material according to claim 3, is characterized in that: described promotor comprises the carboxylated polyethylene wax and polyacrylamide that mass ratio is 1:1.
5. heat-resisting enhancing shock resistance modified polylactic acid material according to claim 1, is characterized in that: described softening agent be selected from hexanaphthene-1,2-dicarboxyl dinonyl, diphenyl phthalate or SA dibutylester one or more.
6. heat-resisting enhancing shock resistance modified polylactic acid material according to claim 1, it is characterized in that: described UV light absorber is selected from 4-benzoyloxy-2,2,6,6-tetramethyl piperidine, tricresyl phosphite (1,2,2,6,6-pentamethvl) one or more in ester or Whitfield's ointment-4-tertiary butyl phenyl ester.
7. heat-resisting enhancing shock resistance modified polylactic acid material according to claim 1, it is characterized in that: described oxidation inhibitor be selected from thio-2 acid octadecyl ester, [β-(3,5 di-t-butyl 4-hydroxy-pheny) propionic acid] pentaerythritol ester or Tyox B one or more.
8. heat-resisting enhancing shock resistance modified polylactic acid material according to claim 1, is characterized in that: described anti-impact modifier be selected from maleic anhydride grafted ethene/propylene copolymer, the multipolymer of maleic anhydride grafted ethene-propylenediene terpolymer, vinylbenzene and divinyl or ethene and acrylonitrile copolymer one or more;
Or described processing aid is selected from one or more in stearic acid, Zinic stearas, calcium stearate or erucicamide.
9. a preparation method for the arbitrary described heat-resisting enhancing shock resistance modified polylactic acid material of claim 1 to 8, is characterized in that: comprise the following steps:
By 100 parts of poly(lactic acid), 8 ~ 15 parts of anti-impact modifiers and 4 ~ 8 parts of processing aids high-speed mixer and mixing 3 ~ 5 minutes, then 20 ~ 30 parts of modified calcium carbonates, 10 ~ 20 parts of softening agent, 1.0 ~ 2.0 parts of UV light absorber are joined high mixer with 0.5 ~ 1.0 part of oxidation inhibitor and mix 5 ~ 8 minutes, wherein the mixing temperature of high mixer is 80 ~ 90 DEG C; Said mixture is cooled to less than 50 DEG C, joins in twin screw extruder by main charging opening, extrusion temperature is 180 ~ 220 DEG C, obtains modified polylactic acid material after extruding, through water-cooled, pelletizing, then dry, pack.
10. the preparation method of heat-resisting enhancing shock resistance modified polylactic acid material according to claim 9, it is characterized in that: described poly(lactic acid) is the poly(lactic acid) matrix of the blended composition of ratio being 4:1 ~ 4:2 with mass ratio by Poly-L-lactic acid and dextrorotation poly(lactic acid), pulverize 500 mesh sieves, obtain polylactic acid powder;
Or the preparation method of described modified calcium carbonate comprises the following steps: first 100 parts of calcium carbonate are added in high-speed mixer, at 100 ~ 110 DEG C of dry 30min, add 5 ~ 8 parts of stearic acid, 3 ~ 5 parts of promotor and 10 ~ 20 parts of calcium oxide again, obtain modified calcium carbonate after high-speed mixing 10 ~ 15min, described promotor comprises the carboxylated polyethylene wax and polyacrylamide that mass ratio is 1:1;
Or the screw slenderness ratio of described twin screw extruder is 30:1, screw speed is 80 ~ 120r/min.
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