CN108164940A - A kind of preparation method of shock resistance poly-lactic acid material - Google Patents
A kind of preparation method of shock resistance poly-lactic acid material Download PDFInfo
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- CN108164940A CN108164940A CN201611115340.4A CN201611115340A CN108164940A CN 108164940 A CN108164940 A CN 108164940A CN 201611115340 A CN201611115340 A CN 201611115340A CN 108164940 A CN108164940 A CN 108164940A
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- polylactic acid
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- acid material
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- 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
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- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- 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
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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- Biological Depolymerization Polymers (AREA)
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Abstract
The invention discloses a kind of modified polylactic acid material, by being made comprising forming for following parts by weight：100 parts of polylactic acid, 10 30 parts of modified calcium carbonate, 10 20 parts of plasticizer, 0.5 1.5 parts of antioxidant, 8 20 parts of anti-impact modifier.Preparation method is as follows：By 100 parts of polylactic acid, 8 10 parts of anti-impact modifiers and 48 parts of processing aids were in high-speed mixer and mixing 35 minutes, then by 10 30 parts of modified calcium carbonates, 10 20 parts of plasticizer, 0.5 1.5 parts of antioxidant are added to high mixer 58 minutes, and blending owner's charge door is added in double screw extruder, and extrusion temperature is 180 200 DEG C, modified polylactic acid material is obtained after extrusion, water cooled, pelletizing and then drying pack.The modified polylactic acid material of the present invention improves mechanical strength and shock resistance.
Description
Technical field
The present invention relates to field of high polymer material modification and processing technique field, and in particular to a kind of shock resistance gathers breast
Sour modified material and preparation method thereof.
Background technology
In the biodegradable plastics developed at present, polylactic acid is a kind of biology base modeling that can be degradable
Material.It is generated, and with excellent biodegradability, make since polylactic acid can be fermented by renewable resources such as cornstarch
Its in petrochemical industry high molecular material is substituted by more and more extensive concern, available for biomedicine, packaging, clothes, agriculture and forestry,
The fields such as catering trade.Although polylactic acid has excellent degradability and biocompatibility, the crisp poor toughness of polylactic acid matter lacks
Flexible and elasticity, easily flexural deformation, temperature is excessively low, strongly limits its development and use scope, so needing to poly-
Lactic acid is modified；
Traditional polylactic acid modified method is by polylactic acid and other high polymers or adds in inorganic filler, by being simply kneaded, adds
Work technique can only improve certain performances of polylactic acid, it is difficult to improve the impact resistance and machinery of polylactic acid simultaneously without specific requirement
Performance etc., therefore common polylactic acid is difficult to meet the application requirement of various industries, such as vehicle appliance, building industry, to plastics material
Material has some higher requirements, in the mechanical performance of material or even to reach or the level close to engineering plastics, and in poly- breast
In the engineering process of sour material, it is most difficult to solve the problems, such as be to ensure material with higher toughness, excellent machine
Tool tensile property also needs to higher performance simultaneously, therefore also needs to constantly be modified poly-lactic acid material comprehensive to improve
Close performance；
The defects of to improve the prior art, the object of the present invention is to provide one kind to have shock resistance modified polylactic acid material；
Compared with prior art, beneficial effects of the present invention are as follows：The shock resistance modified polylactic acid material of the present invention is using addition
Modified calcium carbonate improves the interaction between common polarity inorganic and nonpolar polylactic acid matrix, makes inorganic carbonate
Calcium uniformly disperses in organic polylactic acid matrix, greatly improves the mechanical strength of polylactic acid.The anti-impact modifier of addition
The impact flexibility of polylactic acid is improved, and reduces the strong of material without destroying the crystal structure of polylactic acid in process
Degree；Effective addition of antioxidant enhances the weather resistance of polylactic acid, extends the service life of polylactic acid article.Thus, this
Invention improves the toughness and mechanical strength of poly-lactic acid material（Toughness improves 15-20Mpa/ impact strengths
Improve 10-15KJ/m2）The higher field of comprehensive performance demand is can be widely used in, and preparation is simple, be suitble to work
Industry metaplasia is produced.
Invention content
It is a further object of the present invention to provide a kind of preparation methods of above-mentioned shock resistance modified polylactic acid material
To achieve these goals, technical scheme is as follows：
The present invention provides a kind of shock resistance modified polylactic acid materials, are made of the component comprising following parts by weight：
100 parts of polylactic acid
10 ~ 30 parts of modified calcium carbonate
10 ~ 20 parts of plasticizer
0.5 ~ 1.0 part of antioxidant
8 ~ 15 parts of anti-impact modifier
4 ~ 8 parts of processing aid
It is 4 that the polylactic acid, which includes mass ratio,:1~4:2 l-lactic acid and dextrorotation polylactic acid；
The modified calcium carbonate is made of the component of following parts by weight：100 parts of calcium carbonate, 3 ~ 5 parts of accelerating agent, 5 ~ 8 parts of stearic acid,
10 ~ 20 parts of calcium oxide；
It is 1 that the accelerating agent, which includes mass ratio,:1 carboxylated polyethylene wax and polyacrylamide；
The plasticizer is in two different nonyl fat of hexamethylene -1,2- dicarboxyls, neck phthalic acid hexichol fat or sebacic acid dibutyl ester
One or more；
The antioxidant is selected from 18 fat of thio-2 acid, [β-(3,5 di-t-butyl 4- hydroxy-phenies) propionic acid] Ji Shusi alcohol esters
Or one or more of one kind in the fat of thiodipropionic acid dilauryl osmanthus；
The anti-impact modifier is selected from maleic anhydride grafted ethene/propylene copolymer, maleic anhydride grafted ethene-propylene-two
Alkene terpolymer, the copolymer of styrene and butadiene or the one or more of ethylene and acrylonitrile copolymer；
One or more of the processing aid in stearic acid zinc stearate calcium stearate or erucyl amide.
The present invention also provides a kind of preparation methods of above-mentioned shock resistance modified polylactic acid material, include the following steps：
By 100 parts of polylactic acid, 8 ~ 15 parts of anti-impact modifiers and 4 ~ 8 parts of processing aids in high-speed mixer and mixing 3 ~ 5 minutes, then
20 ~ 30 parts of modified calcium carbonates, 10 ~ 20 parts of plasticizer, 1.0 ~ 2.0 parts of ultra-violet absorbers and 0.5 ~ 1.0 part of antioxidant are added
Enter to high mixer and mix 5 ~ 8 points 50 DEG C hereinafter, there is main charge door to be added in double screw extruder, extrusion temperature is 180 ~ 220
DEG C, modified polylactic acid material is obtained after extrusion, water cooled, pelletizing and then drying pack；
The polylactic acid is using mass ratio as 4 by l-lactic acid and dextrorotation polylactic acid:1~4:The poly- breast of 2 ratio blending composition
Acidic group body crushed 500 mesh sieve, obtain polylactic acid powder；
The screw slenderness ratio of the double screw extruder is 30:1, screw speed is 80 ~ 120r/min.
Specific embodiment
With reference to embodiment, the present invention is described in further detail：
The properties of material are measured in following embodiment using GB (national standard), unless otherwise instructed, the number of component is attached most importance to
Measure number.
Embodiment 1
（1）Modified calcium carbonate pre-processes：First by 100 parts of addition high-speed mixers of calcium carbonate, in 100 ~ 110 DEG C of dry 30min,
Add 9 parts of stearic acid, 3 parts of accelerating agent.13 parts of calcium oxide, mixed at high speed 15min obtain modified calcium carbonate；Accelerating agent includes
Mass ratio 1:1 carboxylated polyethylene wax and polyacrylamide；
(2) 70 parts of polylactic acid matrixes formed with the 30 parts of blendings of dextrorotation polylactic acid of l-lactic acid be crushed into 500 mesh sieve, obtained poly-
Lactic acid powder；
(3) by 100 parts of polylactic acid powder, 8 parts with calcium stearate of 6 parts of ethylene and acrylonitrile copolymer 1 divides in high-speed mixer and mixing 5
Clock, then by 24 parts of modified calcium carbonate, 10 parts of hexamethylene -1,2- dicarboxyl dinonyl, 1.5 parts of tris phosphite and thio two
0.5 part of propionic acid dilauryl is added to high mixer and mixes 8 minutes, and wherein the mixing temperature of high mixer is at 80 DEG C；
(4) after mixing, appeal mixture is cooled to 50 DEG C hereinafter, being added to double screw extruder, extrusion temperature by main charge door
Spend is 190 ~ 210 DEG C.Screw slenderness ratio is 30:1, screw speed 100r/min obtain modified polylactic acid material after extrusion, pass through
Water cooling, pelletizing and then drying, pack；
Modified polylactic acid material is molded into sample, tests its correlated performance：
Tensile strength 36.4（Mpa）Examination criteria ISO527-2:2012
Notch impact strength 19.2（KJ/m²）Examination criteria ISO179-2:2010
Elongation at break 97.5（%）Examination criteria ISO527-2.
Embodiment 2
（1）Modified calcium carbonate pre-processes：First by 100 parts of addition high-speed mixers of calcium carbonate, in 100 ~ 110 DEG C of dry 30min,
Add 10 parts of stearic acid, 4 parts of accelerating agent.18 parts of calcium oxide, mixed at high speed 10min obtain modified calcium carbonate；Accelerating agent includes
Mass ratio 1:1 carboxylated polyethylene wax and polyacrylamide；
(2) 75 parts of polylactic acid matrixes formed with the 25 parts of blendings of dextrorotation polylactic acid of l-lactic acid be crushed into 500 mesh sieve, obtained poly-
Lactic acid powder；
(3) by 100 parts of polylactic acid powder, 8 parts with calcium stearate of 3 parts of ethylene and acrylonitrile copolymer 1 divides in high-speed mixer and mixing 5
Clock, then by 28 parts of modified calcium carbonate, 12 parts of hexamethylene -1,2- dicarboxyl dinonyl, 1.5 parts of tris phosphite and thio two
0.5 part of propionic acid dilauryl is added to high mixer and mixes 8 minutes, and wherein the mixing temperature of high mixer is at 80 DEG C；
(4) after mixing, appeal mixture is cooled to 50 DEG C hereinafter, being added to double screw extruder, extrusion temperature by main charge door
Spend is 180 ~ 210 DEG C.Screw slenderness ratio is 30:1, screw speed 120r/min obtain modified polylactic acid material after extrusion, pass through
Then water cooling, pelletizing are dried, pack；
Modified polylactic acid material is molded into sample, tests its correlated performance,
Tensile strength 41.2（Mpa）Examination criteria ISO527-2:2012
Notch impact strength 19.7（KJ/m²）Examination criteria ISO179-2:2010
Elongation at break 89.6（%）Examination criteria ISO527-2.
Embodiment 3
(1) modified calcium carbonate pre-processes：First by 100 parts of addition high-speed mixers of calcium carbonate, in 100 ~ 110 DEG C of dry 30min,
Add 8 parts of stearic acid, 8 parts of accelerating agent.15 parts of calcium oxide, mixed at high speed 15min obtain modified calcium carbonate；Accelerating agent includes
Mass ratio 1:1 carboxylated polyethylene wax and polyacrylamide；
(2) 80 parts of polylactic acid matrixes formed with the 20 parts of blendings of dextrorotation polylactic acid of l-lactic acid be crushed into 500 mesh sieve, obtained poly-
Lactic acid powder；
(3) by 100 parts of polylactic acid powder, ethylene is with 10 parts of 6 parts of acrylonitrile copolymer 1 and calcium stearate in high-speed mixer and mixing 8
Minute, then by 25 parts of modified calcium carbonate, 10 parts of hexamethylene -1,2- dicarboxyl dinonyl, 1.5 parts of tris phosphite with it is thio
0.5 part of dipropionic acid dilauryl is added to high mixer and mixes 8 minutes, and wherein the mixing temperature of high mixer is at 80 DEG C；
(4) after mixing, appeal mixture is cooled to 50 DEG C hereinafter, being added to double screw extruder, extrusion temperature by main charge door
Spend is 190 ~ 220 DEG C.Screw slenderness ratio is 30:1, screw speed 110r/min obtain modified polylactic acid material after extrusion, pass through
Then water cooling, pelletizing are dried, pack；
Modified polylactic acid material is molded into sample, tests its correlated performance：
Tensile strength 36.5（Mpa）Examination criteria ISO527-2:2012
Notch impact strength 38.3（KJ/m²）Examination criteria ISO179-2:2010
Elongation at break 155.5%）Examination criteria ISO527-2.
Embodiment 4
(1) modified calcium carbonate pre-processes：First by 100 parts of addition high-speed mixers of calcium carbonate, in 100 ~ 110 DEG C of dry 30min,
Add 6 parts of stearic acid, 5 parts of accelerating agent.20 parts of calcium oxide, mixed at high speed 20min obtain modified calcium carbonate；Accelerating agent includes
Mass ratio 1:1 carboxylated polyethylene wax and polyacrylamide；
(2) 65 parts of polylactic acid matrixes formed with the 35 parts of blendings of dextrorotation polylactic acid of l-lactic acid be crushed into 500 mesh sieve, obtained poly-
Lactic acid powder；
(3) by 100 parts of polylactic acid powder, 6 parts with calcium stearate of 2 parts of ethylene and acrylonitrile copolymer 1 divides in high-speed mixer and mixing 4
Clock, then by 26 parts of modified calcium carbonate, 8 parts of hexamethylene -1,2- dicarboxyl dinonyl, 1.5 parts of tris phosphite and thio two
0.5 part of propionic acid dilauryl is added to high mixer and mixes 8 minutes, and wherein the mixing temperature of high mixer is at 80 DEG C；
(4) after mixing, appeal mixture is cooled to 50 DEG C hereinafter, being added to double screw extruder, extrusion temperature by main charge door
Spend is 190 ~ 220 DEG C.Screw slenderness ratio is 30:1, screw speed 130r/min obtain modified polylactic acid material after extrusion, pass through
Water cooling, pelletizing and then drying pack；
Modified polylactic acid material is molded into sample, tests its correlated performance：
Tensile strength 49.5（Mpa）Examination criteria ISO527-2:2012
Notch impact strength 26.6（KJ/m²）Examination criteria ISO179-2:2010
Elongation at break 142.4（%）Examination criteria ISO527-2.
Embodiment 5
(1) modified calcium carbonate pre-processes：First by 100 parts of addition high-speed mixers of calcium carbonate, in 100 ~ 110 DEG C of dry 30min,
Add 12 parts of stearic acid, 6 parts of accelerating agent.12 parts of calcium oxide, mixed at high speed 15min obtain modified calcium carbonate；Accelerating agent includes
Mass ratio 1:1 carboxylated polyethylene wax and polyacrylamide；
(2) 72 parts of polylactic acid matrixes formed with the 28 parts of blendings of dextrorotation polylactic acid of l-lactic acid be crushed into 500 mesh sieve, obtained poly-
Lactic acid powder；
(3) by 100 parts of polylactic acid powder, 8 parts with calcium stearate of 0 part of ethylene and acrylonitrile copolymer 1 divides in high-speed mixer and mixing 5
Clock, then by 20 parts of modified calcium carbonate, 10 parts of hexamethylene -1,2- dicarboxyl dinonyl, 1.5 parts of tris phosphite and thio two
0.5 part of propionic acid dilauryl is added to high mixer and mixes 8 minutes, and wherein the mixing temperature of high mixer is at 80 DEG C；
(4) after mixing, appeal mixture is cooled to 50 DEG C hereinafter, being added to double screw extruder, extrusion temperature by main charge door
Spend is 180 ~ 210 DEG C.Screw slenderness ratio is 30:1, screw speed 100r/min obtain modified polylactic acid material after extrusion, pass through
Water cooling, pelletizing and then drying pack；
Modified polylactic acid material is molded into sample, tests its correlated performance：
Tensile strength 45.5（Mpa）Examination criteria ISO527-2:2012
Notch impact strength 27.7KJ/m2）Examination criteria ISO179-2:2010
Elongation at break 149.5（%）Examination criteria ISO527-2.
It can be seen that by each item data in above-mentioned each example, embodiment 4 and 5 keeps the good anti-impact of modified polylactic acid material
Toughness, mechanics mechanical strength and higher vicat softening temperature are hit, comprehensive performance reaches best.By comparing example 1 and example 3
Comparison, discovery do not add its notch impact strength of the modified polylactic acid material of anti-impact modifier and elongation declines to a great extent；
By comparing the comparison of example 2 and embodiment 4, it is notable that the modified polylactic acid material of modified calcium carbonate its tensile strength is not added in discovery
Attenuation.
Claims (9)
1. a kind of shock resistance modified polylactic acid material, it is characterised in that：By being made comprising forming for following parts by weight：
100 parts of polylactic acid
10-30 parts of modified calcium carbonate
10-20 parts of plasticizer
0.5-1.0 parts of antioxidant
8-15 parts of anti-impact modifier
4-8 parts of processing aid.
2. shock resistance modified polylactic acid material according to claim 1, it is characterised in that：The polylactic acid includes mass ratio
It is 4:1—4:2 l-lactic acid and dextrorotation polylactic acid.
3. shock resistance modified polylactic acid material according to claim 1, it is characterised in that：The modified calcium carbonate is by following
The composition of parts by weight is made：100 parts of calcium carbonate, 3-5 parts of accelerating agent, 5-8 parts of stearic acid, 10-20 parts of calcium oxide.
4. impact modification poly-lactic acid material according to claim 3, it is characterised in that：The accelerating agent includes mass ratio
It is 1:1 carboxylated polyethylene wax and polyacrylamide.
5. shock resistance modified polylactic acid material according to claim 1, it is characterised in that：The plasticizer is selected from hexamethylene
One or more in alkane -1,2- dicarboxyl dinonyl, diphenyl phthalate or sebacic acid dibutyl ester.
6. shock resistance modified polylactic acid material according to claim 1, it is characterised in that：The antioxidant is selected from thio two
One or more in propionic acid octadecyl ester, pentaerythritol ester or dilauryl thiodipropionate.
7. shock resistance modified polylactic acid material according to claim 1, it is characterised in that：The anti-impact modifier is selected from
Maleic anhydride grafted ethene/propylene copolymer, maleic anhydride grafted ethene-propylenediene terpolymer, styrene and fourth two
The copolymer or ethylene of alkene and the one or more in acrylonitrile copolymer；Or the processing aid is selected from stearic acid, firmly
One or more in resin acid zinc, calcium stearate or erucyl amide.
8. the preparation method of shock resistance modified polylactic acid material according to any one of claims 1 to 7, it is characterised in that：Packet
Include following steps：
By 100 parts of polylactic acid, 8 ~ 15 parts of anti-impact modifiers are mixed 3 ~ 5 minutes in high mixer with 4 ~ 8 parts of processing aids, then will
20 ~ 30 parts of modified calcium carbonates, 10 ~ 20 parts of plasticizer, 1.0 ~ 2.0 parts of ultra-violet absorbers are added to 0.5 ~ 1.0 part of antioxidant
High mixer mixes 5 ~ 8 minutes, and the wherein mixing temperature of high mixer is 80 ~ 90 DEG C；By said mixture be cooled to 50 DEG C hereinafter, by
Main charge door is added in double screw extruder, and extrusion temperature is 180 ~ 220 DEG C, and modified polylactic acid material is obtained after extrusion, is passed through
Water cooling, pelletizing and then drying pack.
9. the preparation method of shock resistance modified polylactic acid material according to claim 8, it is characterised in that：The polylactic acid
It is using mass ratio as 4 by l-lactic acid and dextrorotation polylactic acid:1~4:The polylactic acid matrix of 2 ratio blending composition, crushed
500 mesh sieve, and obtain polylactic acid powder；Or the screw slenderness ratio of the double screw extruder is 30:1, screw speed for 80 ~
120r/min。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115260725A (en) * | 2022-09-28 | 2022-11-01 | 河北尚华塑料科技有限公司 | Environment-friendly thermoplastic elastomer material and preparation method thereof |
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| CN102391607A (en) * | 2011-08-31 | 2012-03-28 | 上海锦湖日丽塑料有限公司 | Polylactic acid/styrene resin composition and preparation method thereof |
| CN103319865A (en) * | 2013-06-08 | 2013-09-25 | 上海博疆新材料科技有限公司 | Polylactic acid alloy membrane and application thereof |
| CN104693706A (en) * | 2013-12-04 | 2015-06-10 | 滁州格美特科技有限公司 | Heat resistance increased impact resistant polylactic acid modified material and preparation method thereof |
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2016
- 2016-12-07 CN CN201611115340.4A patent/CN108164940A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102391607A (en) * | 2011-08-31 | 2012-03-28 | 上海锦湖日丽塑料有限公司 | Polylactic acid/styrene resin composition and preparation method thereof |
| CN103319865A (en) * | 2013-06-08 | 2013-09-25 | 上海博疆新材料科技有限公司 | Polylactic acid alloy membrane and application thereof |
| CN104693706A (en) * | 2013-12-04 | 2015-06-10 | 滁州格美特科技有限公司 | Heat resistance increased impact resistant polylactic acid modified material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115260725A (en) * | 2022-09-28 | 2022-11-01 | 河北尚华塑料科技有限公司 | Environment-friendly thermoplastic elastomer material and preparation method thereof |
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