CN108384173A - A kind of high molecular weight height founds the preparation method of structure lactic acid composite material - Google Patents
A kind of high molecular weight height founds the preparation method of structure lactic acid composite material Download PDFInfo
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- CN108384173A CN108384173A CN201810318395.8A CN201810318395A CN108384173A CN 108384173 A CN108384173 A CN 108384173A CN 201810318395 A CN201810318395 A CN 201810318395A CN 108384173 A CN108384173 A CN 108384173A
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- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
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Abstract
The present invention relates to technical field of polymer materials, are related to a kind of preparation method of the vertical structure lactic acid composite material of high molecular weight height.The present invention provides a kind of preparation method of the vertical structure lactic acid composite material of high molecular weight height, specially：Modified Poly L-lactic acid is obtained with poly- L-lactic acid in 100~200 DEG C of 1~6min of melt blending；Modified Poly L-lactic acid and the ratio of poly- L-lactic acid are：90~70：10~30；Modified Poly L-lactic acid is made using linear Poly L-lactic acid, peroxidating diisopropyl ammonia, pentaerythritol triacrylate and tetraethylthiuram disulfide as raw material by melt blending.Extruding-out process can be used in the method for the present invention, and time 5min is blended, is conducive to industrialized production；And the method for the present invention is realized when Poly L-lactic acid and poly- L-lactic acid ratio are 70：It has just been completely formed Stereocomplex crystalline substance in the case of 30, that is, further reduced the dosage of poly- L-lactic acid.
Description
Technical field
The present invention relates to technical field of polymer materials, and in particular to a kind of vertical structure lactic acid composite material of high molecular weight height
Preparation method.
Background technology
Polylactic acid (PLA) is a kind of important synthesis high molecular material of fully biodegradable, there is good bio-compatible
Property, preferable mechanical strength and hot formability are nontoxic, nonirritant, thus are considered as that most promising biodegradable is high
Molecular material.Be for polylactic acid biggest advantage can be from carbohydrate be decomposed into, as metabolism is arranged in inside of human body
Go out external.Plastics result in the focus that the problem of environmental pollution has become world's extensive concern, this sustainable development at present
The Biodegradable polymer material of exhibition has become the research and development direction paid close attention to jointly in the world.Although polylactic acid has very
More advantages, however some performances of polylactic acid itself are there is still a need for improving, with lower melt strength and crystal property,
Therefore it cannot meet the processing such as requirement to polylactic acid performance, such as blown film, wire drawing at present.Its heat resistance is poor, only about
There are 58 DEG C or so.The serious application range for limiting polylactic acid of these disadvantages, exists to further expand polylactic acid
Commercial and industrial application value, it is necessary to be modified to it.
It is largely poly- with poly- dextrorotation using poly- l-lactic acid (PLA) to improve its heat resistance and crystal property
Lactic acid (PDLA) is blended to improve its heat resistance, while can improve its crystal property to a certain extent.PLA/
PDLA blendings can form a kind of special crystal structure and be called Stereocomplex crystalline substance, with special crystal structure, fusing point ratio
Respective polymer is higher by 50 DEG C or so, and the heat resistance of polylactic acid, Mechanics of Machinery can be improved in this special Stereocomplex crystalline substance
Performance, anti-hydrolytic performance etc..
However the formation of this Stereocomplex crystalline substance receives the influence of PLA and PDLA components, the different of component ratio can shape
It is brilliant at the Stereocomplex of different content.It is under normal circumstances 1 in ratio：Vertical structure can be completely formed in the case of 1 (weight ratio)
Composite crystal.The main machining method for currently forming Stereocomplex crystalline substance is solution casting method and melt blended method, research work
Show that solution casting method is more advantageous to form stereoscopic composite compared with melt blending method, and on the molecular weight of obtained polylactic acid
Higher is limited, and this method is easy to operate, but post-processing is complex, cost is higher, and yield is relatively low, is not easy to large-scale industry
Production.
In view of the foregoing drawbacks, the Chinese patent application of Publication No. CN102532837A discloses a kind of high-molecular-weight poly breast
The preparation method of sour stereoscopic composite, specific method are：By poly- l-lactic acid and poly- dextrorotation polylactic acid by weight 80：20~
20：80 are mixed, and mixed material is mixed in torque rheometer at 140~210 DEG C, that is, complete high-molecular-weight poly
The preparation of lactic acid stereoscopic composite；But in the documents only when Poly L-lactic acid and poly- L-lactic acid ratio be 50~
60：When 40~50, it can just be completely formed Stereocomplex crystalline substance；And it is to be blended in torque rheometer in documents, altogether
It is 15min to do time, i.e. the method for documents is only applicable to laboratory applications, and it is longer that the time is blended；In view of the poly- right side
It is expensive to revolve lactic acid, although documents realize Poly L-lactic acid：Poly- L-lactic acid=60：It is just obtained in the case of 40
Full Stereocomplex is brilliant, but if the dosage of poly- L-lactic acid can be further decreased, then entire production cost is just lower；In addition,
The formation of this Stereocomplex crystalline substance, can directly form powdered product in PDLA high-contents, be unfavorable for mechanical property and each side
The raising of face performance.
Invention content
In view of the foregoing drawbacks, the present invention provides the preparation method of a kind of high vertical structure, poly-lactic acid in high molecular weight composite material, this
Extruding-out process can be used in the method for invention, and time 5min is blended, is more conducive to industrialized production；And the present invention
Method is realized when Poly L-lactic acid and poly- L-lactic acid ratio are 70：Stereocomplex crystalline substance has just been completely formed in the case of 30,
The dosage that further reduced poly- L-lactic acid further reduced entire production cost.
Technical scheme of the present invention：
The present invention provides the preparation method of a kind of high vertical structure, poly-lactic acid in high molecular weight composite material, the preparation methods
For：Modified Poly L-lactic acid is obtained into high molecular weight height in 100~200 DEG C of 1~6min of melt blending with poly- L-lactic acid and founds structure
Lactic acid composite material；Wherein, modified Poly L-lactic acid and the ratio of poly- L-lactic acid are：Modified poly- l-lactic acid 90~70
Parts by weight, poly- 10~30 parts by weight of dextrorotation polylactic acid；
Also, the modified Poly L-lactic acid is prepared using following methods：
By linear Poly L-lactic acid, peroxidating diisopropyl ammonia, pentaerythritol triacrylate and tetraethyl Ji Qiulan
Nurse obtains modified Poly L-lactic acid in 180~200 DEG C of 3~5min of melt blending；The ratio of each raw material is：Linear Poly L-lactic acid
(PLA) 100 parts by weight, 0.6 parts by weight of peroxidating diisopropyl ammonia (DCP), pentaerythritol triacrylate (PETA) 0.1~0.4
Parts by weight, 0.05~0.12 parts by weight of tetraethylthiuram disulfide (TETDS).
Further, in the above method, modified Poly L-lactic acid using screw extruder melt altogether with poly- L-lactic acid
Mixed, screw speed is 20~80rpm (preferably 50rpm).
Further, before modified poly- l-lactic acid is mixed with poly- dextrorotation polylactic acid, using vacuum drying, drying time be for
8~48h, 60~80 DEG C of drying temperature make its equal water content be less than 250ppm.
Preferably, in the preparation method of the modified Poly L-lactic acid, each raw material proportioning is：100 weight of polylactic acid (PLA)
Part, 0.6 parts by weight of peroxidating diisopropyl ammonia (DCP), 0.4 parts by weight of pentaerythritol triacrylate (PETA), tetraethyl
0.12 parts by weight of base thiuram (TETDS).
Further, in the above method, in the preparation method of the modified Poly L-lactic acid, melt blending uses Screw Extrusion
Machine, screw speed are 30~150rpm (preferably 50rpm).
Beneficial effects of the present invention：
1) using the preparation method of the high Stereocomplex crystalline substance of high molecular weight of the present invention, molecular weight can be made to be higher than
105The Stereocomplex that the even whole contents of high-content are formed in the poly- l-lactic acid of g/mol is brilliant.
It 2), can be in poly- l-lactic acid and the poly- right side using the preparation method of high molecular weight Stereocomplex crystalline substance of the present invention
Rotation polylactic acid is non-equal than (70:30), the time is only the crystal that all Stereocomplexes are formed under conditions of 5 minutes, is compared
In current research, ratios, the limitation of long duration such as breach.
3) present invention can use extrusion molding, be conducive to industrialized production.
4) the present invention provides a kind of new preparation high molecular weight, the preparation method of high vertical structure lactic acid composite material, energy
Blocky poly-lactic acid material is accessed, the mechanical property and crystal property of composite material can be further significantly improved.
Description of the drawings
Fig. 1 is polydactyl acid point in unmodified linear Poly L-lactic acid and embodiment 2~4 used in the embodiment of the present invention
The curve of son amount distribution.Polylactic acid molecule amount it can be seen from the molecular weight distribution curve of Fig. 1 after modification has occurred
Significant change, weight average molecular weight is by 1.6 × 105G/mol has been increased to 3.9 × 105g/mol.And molecular weight distribution obviously becomes
Width, this explanation is by after extrusion reaction of the present invention, having obtained long-chain branch polylactic acid.
Fig. 2 is the DSC melting curves of the embodiment of the present invention 1~4 and comparative example 1~2.By the data of Fig. 2 and table 1 it is found that
Under conditions of the weight ratios such as the poly- l-lactic acid of long-chain branch and poly- dextrorotation polylactic acid be non-, method using the present invention can be made
The standby Stereocomplex crystalline substance compound with high-content, and the fusing point of obtained Stereocomplex crystalline substance material is up to 223.9 DEG C；It is special
The weight ratio for not being the poly- l-lactic acid of long-chain branch and poly- dextrorotation polylactic acid is 70：Under conditions of 30, preparation using the present invention
Method can be completely formed Stereocomplex crystalline substance product；And it is found by comparative example 1~2, in the content of poly- dextrorotation polylactic acid
When being 30%, the stereoscopic composite of higher amount can be obtained by extrusion reaction.
Specific implementation mode：
The specific implementation mode of the present invention is further described with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
Embodiment 1
The preparation method of lactic acid composite material includes the following steps：
1) by polylactic acid, dry 48h, temperature are 80 DEG C in vacuum drying oven；
2) 90 parts by weight of poly- l-lactic acid being dried and poly- 10 parts by weight of dextrorotation polylactic acid are blended uniformly, so
Afterwards blending granulation is carried out with extruder, the temperature of the temperature of extruder from mouth mold to barrel is 200,200,200,200,
200,200,200,200,200,160,100 DEG C, screw speed 50rpm, the time from barrel to mouth mold is 6min；
3) sample obtained by uses DSC to be heated to 240 DEG C, isothermal 5min from 40 DEG C with 10 DEG C/min, then with 10 DEG C/
Min cools to 40 DEG C from 240 DEG C, and the result is shown in table 1 and Fig. 2.
Embodiment 2
The preparation method that high molecular weight height founds structure lactic acid composite material includes the following steps：
1) by polylactic acid, dry 48h, temperature are 80 DEG C in vacuum drying oven；
2) by 0.6 parts by weight of 100 parts by weight of poly- l-lactic acid and peroxidating diisopropyl ammonia being dried, Ji Wusi
0.4 parts by weight of alcohol triacrylate, 0.12 parts by weight of tetraethylthiuram disulfide be blended it is uniform, then use extruder into
Row, which is blended, to be granulated, and the poly- l-lactic acid of modified long-chain branch is obtained；Temperature of the temperature of extruder from mouth mold to barrel is 200,
200,200,200,200,200,200,200,200,160,100 DEG C, screw speed 50rpm, the time from barrel to mouth mold
For 6min；
3) poly- 90 parts by weight of l-lactic acid of long-chain branch and poly- 10 parts by weight of dextrorotation polylactic acid are blended uniform, then with reaction
Extruder carries out blending granulation, and the temperature of the temperature of extruder from mouth mold to barrel is 200,200,200,200,200,200,
200,200,200,160,100 DEG C, screw speed 50rpm, the time from barrel to mouth mold is 6min；
4) sample obtained by uses DSC to be heated to 240 DEG C, isothermal 5min from 40 DEG C with 10 DEG C/min, then with 10 DEG C/
Min cools to 40 DEG C from 240 DEG C, and the result is shown in table 1 and Fig. 2.
Embodiment 3
The preparation method that high molecular weight height founds structure lactic acid composite material includes the following steps：
1) by polylactic acid, dry 48h, temperature are 80 degree in vacuum drying oven；
2) by 0.6 parts by weight of 100 parts by weight of poly- l-lactic acid and peroxidating diisopropyl ammonia being dried, Ji Wusi
0.4 parts by weight of alcohol triacrylate, 0.12 parts by weight of tetraethylthiuram disulfide be blended it is uniform, then use extruder into
Row, which is blended, to be granulated, and the poly- l-lactic acid of modified long-chain branch is obtained；Temperature of the temperature of extruder from mouth mold to barrel is 200,
200,200,200,200,200,200,200,200,160,100 DEG C, screw speed 50rpm, the time from barrel to mouth mold
For 6min；
3) poly- 80 parts by weight of l-lactic acid of long-chain branch and poly- 20 parts by weight of dextrorotation polylactic acid are blended uniform, then with reaction
Extruder carries out blending granulation, and the temperature of the temperature of extruder from mouth mold to barrel is 200,200,200,200,200,200,
200,200,200,160,100 DEG C, screw speed 50rpm, the time from barrel to mouth mold is 6min；
4) sample obtained by uses DSC to be heated to 240 DEG C, isothermal 5min from 40 DEG C with 10 DEG C/min, then with 10 DEG C/
Min cools to 40 DEG C from 240 DEG C, and the result is shown in table 1 and Fig. 2.
Embodiment 4
The preparation method that high molecular weight height founds structure lactic acid composite material includes the following steps：
1) by polylactic acid, dry 48h, temperature are 80 degree in vacuum drying oven；
2) by 0.6 parts by weight of 100 parts by weight of poly- l-lactic acid and peroxidating diisopropyl ammonia being dried, Ji Wusi
0.4 parts by weight of alcohol triacrylate, 0.12 parts by weight of tetraethylthiuram disulfide be blended it is uniform, then use extruder into
Row, which is blended, to be granulated, and the poly- l-lactic acid of modified long-chain branch is obtained；Temperature of the temperature of extruder from mouth mold to barrel is 200,
200,200,200,200,200,200,200,200,160,100 DEG C, screw speed 50rpm, the time from barrel to mouth mold
For 6min；
3) poly- 70 parts by weight of l-lactic acid of long-chain branch and poly- 30 parts by weight of dextrorotation polylactic acid are blended uniform, then with reaction
Extruder carries out blending granulation, and the temperature of the temperature of extruder from mouth mold to barrel is 200,200,200,200,200,200,
200,200,200,160,100 DEG C, screw speed 50rpm, the time from barrel to mouth mold is 6min；
4) sample obtained by uses DSC to be heated to 240 DEG C, isothermal 5min from 40 DEG C with 10 DEG C/min, then with 10 DEG C/
Min cools to 40 DEG C from 240 DEG C, and the result is shown in table 1 and Fig. 2.
Comparative example 1
The preparation method of lactic acid composite material includes the following steps：
1) by polylactic acid, dry 48h, temperature are 80 DEG C in vacuum drying oven；
2) by 0.6 parts by weight of 100 parts by weight of poly- l-lactic acid and peroxidating diisopropyl ammonia being dried, Ji Wusi
0.4 parts by weight of alcohol triacrylate, 0.12 parts by weight of tetraethylthiuram disulfide be blended it is uniform, then use extruder into
Row, which is blended, to be granulated, and the poly- l-lactic acid of modified long-chain branch is obtained；Temperature of the temperature of extruder from mouth mold to barrel is 200,
200,200,200,200,200,200,200,200,160,100 DEG C, screw speed 50rpm, the time from barrel to mouth mold
For 6min；
3) poly- 70 parts by weight of l-lactic acid of long-chain branch and poly- 30 parts by weight of dextrorotation polylactic acid are blended uniform, then use two
Chloromethanes solution, churned mechanically method make mixture be completely dissolved, and experimental temperature is 25 DEG C, and mixing time is for 24 hours.
4) it is finally put into ancient customs baking oven, solvent is volatilized, and product is dried in vacuo for 24 hours, drying temperature 60
℃.The sample of gained uses DSC to be heated to 240 DEG C, isothermal 5min from 40 DEG C with 10 DEG C/min, then with 10 DEG C/min from 240
DEG C 40 DEG C are cooled to, the result is shown in table 1 and Fig. 2.
Comparative example 2
The preparation method of lactic acid composite material includes the following steps：
1) by polylactic acid, dry 48h, temperature are 80 DEG C in vacuum drying oven；
2) 70 parts by weight of poly- l-lactic acid that will be dried, poly- 30 parts by weight of dextrorotation polylactic acid and peroxidating two are different
Third ammonia, 0.6 parts by weight, 0.4 parts by weight of pentaerythritol triacrylate, 0.12 parts by weight of tetraethylthiuram disulfide are blended equal
It is even, blending granulation then is carried out with extruder, obtains the poly- l-lactic acid of modified long-chain branch；The temperature of extruder is from mouth
The temperature of mould to barrel is 200,200,200,200,200,200,200,200,200,160,100 DEG C, and screw speed is
50rpm, the time from barrel to mouth mold are 6min；
3) sample obtained by uses DSC to be heated to 240 DEG C, isothermal 5min from 40 DEG C with 10 DEG C/min, then with 10 DEG C/
Min cools to 40 DEG C from 240 DEG C, and the result is shown in table 1 and Fig. 2.
Parameter in 1 Examples 1 to 4 of table and comparative example 1~2 obtained by DSC melting curves
Note：TccFor the temperature at cold crystallization peak, Δ HccFor cold crystallization heat content, TmFor melting peak temperature, Δ HmFor melting enthalpy,
xcFor total crystallinity.1 represents homopolymer crystal, and 2 represent Stereocomplex Jingjing body.
Claims (6)
1. high molecular weight height founds the preparation method of structure lactic acid composite material, which is characterized in that the preparation method is that：It will be modified
Poly L-lactic acid and poly- L-lactic acid in 100~200 DEG C of 1~6min of melt blending obtain high molecular weight height, and to found structure polylactic acid compound
Material；Wherein, modified Poly L-lactic acid and the ratio of poly- L-lactic acid are：Modified poly- 90~70 parts by weight of l-lactic acid, gather
10~30 parts by weight of dextrorotation polylactic acid；
Also, the modified Poly L-lactic acid is prepared using following methods：
By linear Poly L-lactic acid, peroxidating diisopropyl ammonia, pentaerythritol triacrylate and tetraethylthiuram disulfide in
180~200 DEG C of 3~5min of melt blending obtain modified Poly L-lactic acid；The ratio of each raw material is：Linear Poly L-lactic acid 100
Parts by weight, 0.6 parts by weight of peroxidating diisopropyl ammonia, 0.1~0.4 parts by weight of pentaerythritol triacrylate, tetraethyl base
0.05~0.12 parts by weight of thiuram.
2. high molecular weight height according to claim 1 founds the preparation method of structure lactic acid composite material, which is characterized in that change
Property Poly L-lactic acid and poly- L-lactic acid melt blending is carried out using screw extruder, screw speed is 20~80rpm.
3. high molecular weight height according to claim 1 or 2 founds the preparation method of structure lactic acid composite material, feature exists
In before modified poly- l-lactic acid is mixed with poly- dextrorotation polylactic acid, making its equal water content less than 250ppm using vacuum drying.
4. high molecular weight height according to claim 3 founds the preparation method of structure lactic acid composite material, which is characterized in that dry
The dry time is for 8~48h, 60~80 DEG C of drying temperature.
5. the preparation method of structure lactic acid composite material is found according to Claims 1 to 4 any one of them high molecular weight height, it is special
Sign is that in the preparation method of the modified Poly L-lactic acid, each raw material proportioning is：100 parts by weight of polylactic acid, peroxidating two are different
Third ammonia, 0.6 parts by weight, 0.4 parts by weight of pentaerythritol triacrylate, 0.12 parts by weight of tetraethylthiuram disulfide.
6. the preparation method of structure lactic acid composite material is found according to Claims 1 to 5 any one of them high molecular weight height, it is special
Sign is, in the preparation method of the modified Poly L-lactic acid, melt blending use screw extruder, screw speed be 30~
150rpm。
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| CN109337308A (en) * | 2018-08-30 | 2019-02-15 | 北京服装学院 | A kind of high Stereocomplex type poly-lactic acid material and preparation method thereof |
| CN111548615A (en) * | 2020-05-12 | 2020-08-18 | 中国科学院长春应用化学研究所 | Bidirectional stretching stereo composite polylactic acid film and preparation method thereof |
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| CN101891940A (en) * | 2009-05-21 | 2010-11-24 | 中国科学院化学研究所 | Modified polyactic acid and preparation method thereof |
| KR101820247B1 (en) * | 2016-09-29 | 2018-01-18 | 롯데케미칼 주식회사 | Resin compositions for improving clarity and thermal resistance of stereocomplexed polylactic acid |
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| CN101891940A (en) * | 2009-05-21 | 2010-11-24 | 中国科学院化学研究所 | Modified polyactic acid and preparation method thereof |
| KR101820247B1 (en) * | 2016-09-29 | 2018-01-18 | 롯데케미칼 주식회사 | Resin compositions for improving clarity and thermal resistance of stereocomplexed polylactic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109337308A (en) * | 2018-08-30 | 2019-02-15 | 北京服装学院 | A kind of high Stereocomplex type poly-lactic acid material and preparation method thereof |
| CN111548615A (en) * | 2020-05-12 | 2020-08-18 | 中国科学院长春应用化学研究所 | Bidirectional stretching stereo composite polylactic acid film and preparation method thereof |
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