CN106893284B - The preparation method of polylactic acid/nano-cellulose composite material - Google Patents
The preparation method of polylactic acid/nano-cellulose composite material Download PDFInfo
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- CN106893284B CN106893284B CN201710212358.4A CN201710212358A CN106893284B CN 106893284 B CN106893284 B CN 106893284B CN 201710212358 A CN201710212358 A CN 201710212358A CN 106893284 B CN106893284 B CN 106893284B
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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
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
- C08L1/04—Oxycellulose; Hydrocellulose, e.g. microcrystalline cellulose
Abstract
The present invention discloses a kind of preparation method of polylactic acid/nano-cellulose composite material, comprising the following specific steps 1) preparing nano-cellulose organogel；2) the nano-cellulose organogel block prepared in step 1) is immersed in the chloroform soln of polylactic acid 24-48 hours, after taking-up gel piece is dried 2-5 hours at normal temperature in solution, it is put into vacuum oven and is dried in vacuo 10-15 hours under the conditions of 50-60 DEG C, polylactic acid/nano-cellulose composite material is obtained with hot press hot pressing, reaction condition of the present invention is mild, method applicability is strong, it is reacted without adding other additives, effectively increase nano-cellulose in the composite accounting while, also guarantee that nano-cellulose is dispersed in polylactic acid matrix.
Description
Technical field
The present invention relates to technical field of polymer processing, and in particular to a kind of polylactic acid/nano-cellulose composite material
Preparation method.
Background technique
As high molecular material is widely applied, petroleum resources, which largely consume, causes plastic garbage constantly to increase, global environment
Pollution problem aggravation.A large amount of consumption of non-renewable energy resources are so that poly-lactic acid material is more and more paid attention to.Polylactic acid can
It is that fermenting raw materials polymerization is made by corn and other natural plants, water and titanium dioxide can be resolved into completely under microbial action
Carbon, it is completely environmental-friendly.But polylactic acid matter is hard and crisp, and impact resistant strength and hydrophily are poor, limits its scope of application.
It is a kind of design method applied to fields such as material science that nano-cellulose, which is mixed in polymer,.The method is answered
It is very attractive with having a extensive future.It can have new capability or property by mixing various other polymer material preparations
The material that can enhance.Polylactic acid/nano-cellulose composite material is compared to pure poly-lactic acid material, hydrophily, biological degradability
Etc. be all significantly improved, can be widely applied to biology, the fields such as medicine and packaging.And the high-ratio surface of nano-cellulose
Long-pending and energy, nanoparticle usually have strong aggregation tendency, this makes them be difficult to be dispersed in polylactic acid.
Currently, the preparation of polylactic acid/nano-cellulose composite material is generally by being modified nano-cellulose surface
Or expanding material is added to solve dispersion problem of the nano-cellulose in polylactic acid matrix.But the above method is only preparing low account for
Polylactic acid can effectively be enhanced when the nano-cellulose composite material of ratio, nano-cellulose filler further increases the group of will form
It is poly-, lead to the declines for enhancing polylactic acid.
Summary of the invention
The shortcomings that overcoming the above prior art: the technical problem to be solved by the present invention is to provide a kind of reaction condition temperature
With method applicability is strong, is reacted without adding other additives, and nano-cellulose accounting in the composite is effectively increased
While, also guarantee the preparation of nano-cellulose polylactic acid/nano-cellulose composite material dispersed in polylactic acid matrix
Method.
Technical solution of the invention is as follows: a kind of preparation method of polylactic acid/nano-cellulose composite material, special
Sign is: comprising the following specific steps
1) it prepares nano-cellulose organogel: nano-cellulose powder being added in 0-20 DEG C of deionized water, at ultrasound
Reason obtains nano-cellulose suspension, and oil bath heating is to 70-80 DEG C after standing 24-48 hours, ultrasound defoaming, after being cooled to room temperature
Organic solvent is added, stands, until forming supernatant liquor and lower layer's gel layer, removes supernatant liquor, organic solvent replacement is added
Supernatant liquor after replacing 5-8 times altogether, removes upper layer organic solvent layer every 12-24 hours replacement upper layer organic solvent layers；It takes
Lower layer's gel layer rinses 2-3 acquisition nano-cellulose organogel with organic solvent out, and nano-cellulose organogel is cut
It is placed at fritter spare in 4 DEG C of environment；
2) the nano-cellulose organogel block prepared in step 1) is immersed in 24- in the chloroform soln of polylactic acid
It 48 hours, after taking-up gel piece is dried 2-5 hours at normal temperature in solution, is put into vacuum oven in 50-60 DEG C of condition
Then the dry gel piece finished is paved with hot pressing die, with hot press in upper and lower plates 155- by lower vacuum drying 10-15 hours
160 DEG C, hot pressing under the conditions of pressure 2000-2200psi obtains polylactic acid/nano-cellulose composite material.
The mass percent concentration of nano-cellulose is 4%-15% in the nano-cellulose suspension.
The organic solvent is one of ethyl alcohol, acetone, isopropanol.
As optimization, in step 1), the volume ratio of lower layer's gel layer and supernatant liquor is 1 ︰ 4-5.
As optimization, the mass percent concentration of polylactic acid is 2%-15% in the chloroform soln of the polylactic acid.
The beneficial effects of the present invention are: the present invention is prepared for the nanometer with three-dimensional net structure using sol-gel method
Cellulose organogel block, then will prepare composite material in gel piece immersion polylactic acid enables nano-cellulose in composite wood
Fine dispersion is obtained relative to polylactic acid in material, while improving the accounting of nano-cellulose in composite material, preparation process item
Part is mild, easy to operate, the polylactic acid/nano-cellulose composite material and pure poly-lactic acid material phase obtained by the preparation method
Than, elongation at break and impact strength obtain biggish raising, and the present invention prepares raw material and derives from renewable energy,
Degradable green, no environmental pressure meet environmental-friendly theory, have good development prospect in medical packaging field.
Detailed description of the invention
Fig. 1 is 2K times of SEM figure of composite material prepared by the embodiment of the present invention three.
Fig. 2 is 5K times of SEM figure of composite material prepared by the embodiment of the present invention three.
Specific embodiment
The present invention is described in further details with specific embodiment below, but the present invention is not only limited in detail below in fact
Apply example.
Embodiment one
A kind of preparation method of polylactic acid/nano-cellulose composite material, comprising the following specific steps
1) it prepares nano-cellulose organogel: nano-cellulose powder being added in 0-20 DEG C of deionized water, at ultrasound
Reason obtains nano-cellulose suspension, and the mass percent concentration of nano-cellulose is 4%- in the nano-cellulose suspension
15%, to 70-80 DEG C, ultrasound defoaming is added organic solvent, stands oil bath heating after being cooled to room temperature after standing 24-48 hours,
Until forming supernatant liquor and lower layer's gel layer, the volume ratio of lower layer's gel layer and supernatant liquor is 1 ︰ 4-5, and removal upper layer is clear
Liquid is added organic solvent and replaces supernatant liquor, every 12-24 hours replacement upper layer organic solvent layers, after replacing 5-8 times altogether, goes
Except upper layer organic solvent layer；It takes out lower layer's gel layer and rinses 2-3 acquisition nano-cellulose organogel with organic solvent, will receive
The fritter that rice cellulose organogel is cut into 12mmX12mmX12mm is placed in spare in 4 DEG C of environment；
2) the nano-cellulose organogel block prepared in step 1) is immersed in 24- in the chloroform soln of polylactic acid
48 hours, the mass percent concentration of polylactic acid was 2%-15% in the chloroform soln of the polylactic acid, was taken out from solution
After gel piece is dried 2-5 hours at normal temperature, it is put into vacuum oven and is dried in vacuo 10-15 hours under the conditions of 50-60 DEG C,
Then the gel piece dry finished is paved with hot pressing die, with hot press at 155-160 DEG C of upper and lower plates, pressure 2000-2200psi
Under the conditions of hot pressing, obtain polylactic acid/nano-cellulose composite material.The organic solvent is ethyl alcohol, acetone, one in isopropanol
Kind.
Embodiment two
A kind of preparation method of polylactic acid/nano-cellulose composite material, comprising the following specific steps
1) it prepares nano-cellulose organogel: nano-cellulose powder being added in 0 DEG C of deionized water, be ultrasonically treated
To nano-cellulose suspension, the mass percent concentration of nano-cellulose is 10% in the nano-cellulose suspension, is stood
Oil bath heating is to 80 DEG C after 24 hours, and ultrasound defoaming is added ethyl alcohol, stands after being cooled to room temperature, until formed supernatant liquor and
The volume ratio of lower layer's gel layer, lower layer's gel layer and supernatant liquor is 1 ︰ 4-5, removes supernatant liquor, and ethyl alcohol is added and replaces upper layer
Clear liquid after replacing 8 times altogether, removes upper layer ethyl alcohol every 12 hours replacement upper layer ethyl alcohol；Lower layer's gel layer is taken out to be rinsed with ethyl alcohol
2-3 acquisition nano-cellulose organogel, is placed in 4 for the fritter that nano-cellulose organogel is cut into 12mmX12mmX12mm
It is spare in DEG C environment；
2) the nano-cellulose organogel block prepared in step 1) is immersed in 48 in the chloroform soln of polylactic acid
Hour, the mass percent concentration of polylactic acid is 15% in the chloroform soln of the polylactic acid, and gel piece is taken out from solution
After drying 2 hours at normal temperature, it is put into vacuum oven under the conditions of 60 DEG C and is dried in vacuo 15 hours, then finish drying
Gel piece be paved with hot pressing die, with hot press hot pressing under the conditions of 160 DEG C of upper and lower plates, pressure 2200psi, obtain polylactic acid/
Nano-cellulose composite material.
Embodiment three
A kind of preparation method of polylactic acid/nano-cellulose composite material, comprising the following specific steps
1) it prepares nano-cellulose organogel: nano-cellulose powder being added in 0 DEG C of deionized water, be ultrasonically treated
To nano-cellulose suspension, the mass percent concentration of nano-cellulose is 8% in the nano-cellulose suspension, is stood
Oil bath heating is to 70 DEG C after 24 hours, and ultrasound defoaming is added ethyl alcohol, stands after being cooled to room temperature, until formed supernatant liquor and
The volume ratio of lower layer's gel layer, lower layer's gel layer and supernatant liquor is 1 ︰ 5, removes supernatant liquor, and it is clear that ethyl alcohol replacement upper layer is added
Liquid after replacing 5 times altogether, removes upper layer ethyl alcohol every 48 hours replacement upper layer ethyl alcohol；It takes out lower layer's gel layer and rinses 3 with ethyl alcohol
Secondary acquisition nano-cellulose organogel, is placed in 4 DEG C for the fritter that nano-cellulose organogel is cut into 12mmX12mmX12mm
It is spare in environment；
2) the nano-cellulose organogel block prepared in step 1) is immersed in 48 in the chloroform soln of polylactic acid
Hour, the mass percent concentration of polylactic acid is 15% in the chloroform soln of the polylactic acid, and gel piece is taken out from solution
After drying 2 hours at normal temperature, it is put into vacuum oven under the conditions of 60 DEG C and is dried in vacuo 15 hours, then finish drying
Gel piece be paved with hot pressing die, with hot press hot pressing under the conditions of 160 DEG C of upper and lower plates, pressure 2000psi, obtain polylactic acid/
Nano-cellulose composite material.
Prepared polylactic acid/nano-cellulose composite material as shown in Figs. 1-2 can be bright from figure by sem analysis
Aobvious to find out, NCC is uniformly dispersed in PLA, and composite material section is coarse and uneven, is in ductile rupture feature.From high magnification numbe
Figure in as can be seen that NCC and PLA nano-cellulose and two-phase cohere the aggregation that nano-cellulose is closely not observed, receive
Rice cellulose is substantially wrapped by, and the caking property of the two is fine.
The above is only feature implementation examples of the invention, are not limited in any way to the scope of the present invention.It is all to use together
The technical solution formed Deng exchange or equivalence replacement, all falls within rights protection scope of the present invention.
Claims (3)
1. a kind of preparation method of polylactic acid/nano-cellulose composite material, it is characterised in that: comprising the following specific steps
1) it prepares nano-cellulose organogel: nano-cellulose powder being added in 0-20 DEG C of deionized water, be ultrasonically treated
To nano-cellulose suspension, to 70-80 DEG C, ultrasound defoaming is added oil bath heating after being cooled to room temperature after standing 24-48 hours
Organic solvent is stood, until forming supernatant liquor and lower layer's gel layer, removes supernatant liquor, and organic solvent is added and replaces upper layer
Clear liquid after replacing 5-8 times altogether, removes upper layer organic solvent layer every 12-24 hours replacement upper layer organic solvent layers；Under taking-up
Layer gel layer rinses 2-3 acquisition nano-cellulose organogel with organic solvent, nano-cellulose organogel is cut into small
Block is placed in spare in 4 DEG C of environment；
2) that the nano-cellulose organogel block prepared in step 1) is immersed in 24-48 in the chloroform soln of polylactic acid is small
When, after taking-up gel piece is dried 2-5 hours at normal temperature in solution, it is put into vacuum oven under the conditions of 50-60 DEG C true
Sky is 10-15 hours dry, and the dry gel piece finished is then paved with hot pressing die, with hot press at 155-160 DEG C of upper and lower plates,
Hot pressing under the conditions of pressure 2000-2200psi, obtains polylactic acid/nano-cellulose composite material；
The mass percent concentration of nano-cellulose is 4%-15% in the nano-cellulose suspension；
The mass percent concentration of polylactic acid is 2%-15% in the chloroform soln of the polylactic acid.
2. the preparation method of polylactic acid/nano-cellulose composite material according to claim 1, it is characterised in that: described
Organic solvent is one of ethyl alcohol, acetone, isopropanol.
3. the preparation method of polylactic acid/nano-cellulose composite material according to claim 1, it is characterised in that: step
1) in, the volume ratio of lower layer's gel layer and supernatant liquor is 1 ︰ 4-5.
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| CN109880180B (en) * | 2019-03-13 | 2021-03-02 | 广州谱睿汀新材料科技有限公司 | Nano-cellulose/cellulose compound, reinforced polylactic acid 3D printing material and preparation method thereof |
| CN112092419B (en) * | 2019-06-18 | 2022-04-19 | 中国科学技术大学 | Preparation method of bacterial cellulose composite board with tubular structure |
| CN113311025B (en) * | 2021-07-13 | 2023-06-27 | 浙江农林大学 | Preparation method of novel intelligent gas sensing material suitable for indoor ammonia gas detection |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102666669A (en) * | 2009-09-14 | 2012-09-12 | 诺丁汉大学 | Cellulose nanoparticle aerogels, hydrogels and organogels |
| CN103044871A (en) * | 2012-11-26 | 2013-04-17 | 浙江大学宁波理工学院 | Preparation method of polylactic acid/nano-cellulose composite material |
| CN105837861A (en) * | 2016-04-03 | 2016-08-10 | 苏鑫 | Composite natural polymer gel material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102666669A (en) * | 2009-09-14 | 2012-09-12 | 诺丁汉大学 | Cellulose nanoparticle aerogels, hydrogels and organogels |
| CN103044871A (en) * | 2012-11-26 | 2013-04-17 | 浙江大学宁波理工学院 | Preparation method of polylactic acid/nano-cellulose composite material |
| CN105837861A (en) * | 2016-04-03 | 2016-08-10 | 苏鑫 | Composite natural polymer gel material |
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