CN104927321B - A kind of packaging material preparation method of PHBV composite membrane - Google Patents
A kind of packaging material preparation method of PHBV composite membrane Download PDFInfo
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Abstract
The present invention provides a kind of packaging material preparation method of PHBV composite membrane, comprises the following steps：(1) serpentine is obtained serpentine powder body with superfine grinding after ball mill ball milling, sodium stearate is dissolved in deionized water mix homogeneously modification liquid is obtained, serpentine powder body is added modification liquid, it is placed in water bath with thermostatic control stirring, take out, filter, it is placed in drying baker and dries to constant weight, obtain modified snake stone powder；(2) PHBV of 80 90 weight portions is added in twin-roll plastic mixing mill and plastify, the compatilizer of the modified snake stone powder of 26 weight portions and 4 weight portions is sequentially added twin-roll plastic mixing mill and continues plasticizing, thin logical 8 times, obtain compound；(3) PTFE of the compatilizer of compound and 4 weight portions, 48 weight portions is added melt blending in banbury, move to double screw extruder extruding pelletization, obtain pellet, pellet cast film machine casting film-forming obtains packaging material PHBV composite membrane.The composite membrane that the present invention prepares has preferable thermostability and toughness, can apply to multiple occasions.
Description
Technical field：
The present invention relates to a kind of packaging material, more particularly to a kind of packaging material preparation method of PHBV composite membrane.
Background technology：
Increasingly in short supply with petroleum resources, the gradually aggravation of white pollution and greenhouse effect, with renewable biomass money
Source is that the bioabsorbable polymer material of raw material becomes the focus that current Material Field develops.Bioabsorbable polymer material is a class environment friend
Good type new material, mainly with plant as raw material, obtains such as PHA (PHA), polylactic acid (PIA) by Microbe synthesis
Deng be then by Microbe synthesis monomer again chemosynthesis and obtain.PHBV (PHBV) is one of PHA,
It is 3-hydroxybutyrate ester and the copolymer of 3- hydroxyl valerate, having good biological degradability, biocompatibility and biology can
The characteristics such as absorbability, longer bio-absorbable cycle, therefore can be applicable to such as medical material (suture, nail), thin-film material
The field such as (mulch film, shopping bag, compost bag), disposable product (pen, tableware), packaging material (particularly packaging for foodstuff).
For example, Publication No. CN101508791B, publication date are 2012.10.03, apply for the fragrant Chinese patent of artificial Xing Jin
Disclose " a kind of production method of biodegradable plastic film ", specifically provide one kind and produced using Ecoflex and PHBV
The method of biodegradable plastic film, by 5～50%PHBV poly butyric valeric acid copolyesters and 50～95%Ecoflex fat
Fat race aromatic series atactic polyester mix homogeneously, the more additional CaCO accounting for said mixture gross weight 5%3, this invention have as
Lower beneficial effect：Its process is simple, easily operated, the thin film being produced, in the presence of soil microorganism, can resolve into completely
Water, carbon dioxide and Organic substance, pollution-free, can be widely applied to agricultural mulching, packaging bag (packaging for foodstuff, industrial packaging) etc.,
It is a kind of environment-friendly products of green.But, there is certain defect in this thin film：When being applied to packaging material, its in thermostability and
The performance of toughness aspect is undesirable, reduces its range of application.
Content of the invention：
It is to provide a kind of preparation method of packaging material PHBV composite membrane that the present invention will solve this technology book, prepares
Composite membrane there is preferable thermostability and toughness, can apply to multiple occasions.
For solving this above-mentioned technology book, the technical scheme is that：
A kind of packaging material preparation method of PHBV composite membrane, comprises the following steps：
(1) serpentine is obtained serpentine powder body with superfine grinding after ball mill ball milling, sodium stearate is dissolved in deionization
Water mix homogeneously is obtained modification liquid, and serpentine powder body is added modification liquid, is placed in water bath with thermostatic control and stirs 30 minutes, taking-up, mistake
Filter, is placed in drying baker and dries to constant weight, obtain modified snake stone powder；
(2) PHBV of 80-90 weight portion is added in twin-roll plastic mixing mill and plastify 2 minutes, by the modified snake of 2-6 weight portion
The compatilizer of stone powder and 4 weight portions sequentially adds twin-roll plastic mixing mill and continues plasticizing 8 minutes, thin logical 8 times, obtains compound；
(3) PTFE of the compatilizer of compound and 4 weight portions, 4-8 weight portion is added 12 points of melt blending in banbury
Clock, moves to double screw extruder extruding pelletization, obtains pellet, and pellet cast film machine casting film-forming obtains packaging material and uses
PHBV composite membrane.
Preferably, in step (1) of the present invention, the particle diameter of serpentine powder body is 3 μm.
Preferably, in step (1) of the present invention, the weight of serpentine powder body and sodium stearate is than for 20:1.
Preferably, in step (1) of the present invention, the temperature of water bath with thermostatic control is 80 DEG C.
Preferably, in step (1) of the present invention, the temperature of drying baker is 80 DEG C.
Preferably, in step (2) of the present invention, the temperature of plasticizing is 140 DEG C.
Preferably, in step (2) of the present invention, compatilizer is epoxy soybean oil.
Preferably, in step (3) of the present invention, the temperature of melt blending is 170 DEG C, and rotating speed is 60rpm.
Preferably, in step (4) of the present invention, the extrusion temperature of double screw extruder is 180-205 DEG C, and rotating speed is
800rpm.
Preferably, in step (4) of the present invention, packaging material are 0.1mm with the thickness of PHBV composite membrane.
Compared with prior art, the invention has the advantages that：
(1) serpentine is the silicate mineral with layer structure, has preferable thermostability and mechanical property, is making
During powder body, its surface occurs hydroxyl and unsaturated bond so that showing very strong polarity, with the low pole of PHBV not
Compatible, therefore the present invention carries out surface modification as surface modifier to it using sodium stearate, and sodium stearate is molten in the hot water
The anion that solution ionization produces and the surface of snake stone powder are fully contacted and there occurs coupling reaction, greatly reduce surface polarity
And increase the interlamellar spacing of snake stone powder, improve itself compatibility and PHBV between, the another aspect present invention passes through melting and inserts
The mode of layer defines exfoliated composite construction, and the macromolecular chain of PHBV inserts between the lamella of snake stone powder and produces preferably
Interface interaction, when composite membrane be subject to percussion when, snake stone powder becomes stress because of itself preferable strength and stiffness
Centrostigma, runs into snake stone powder lamella and can stop or shift, snake stone powder absorbs big stroke simultaneously during micro-crack extension
Can, thus substantially increasing the toughness of composite membrane；When composite membrane is in hot environment, snake stone powder lamella can play heat-insulated
Effect and itself there is preferable thermostability, therefore can the effectively impact to composite membrane for the trap heat, thus effectively improve answer
Close heat distortion temperature and the thermostability of film.
(2) PTFE is the english abbreviation of politef, has good heat-resisting quantity, resistance to acids and bases and solvent resistant
Property, with the help of compatilizer epoxy soybean oil, the compatibility between PTFE and PHBV matrix is greatly improved, thus
Define preferable compatibility blending, can further improve the thermostability of composite membrane, also can effectively improve the acid and alkali-resistance of composite membrane
Property and solvent resistance.
Specific embodiment：
To describe the present invention, the illustrative examples of the here present invention and explanation below in conjunction with specific embodiment in detail
It is used for explaining the present invention, but not as a limitation of the invention.
Embodiment 1
A kind of packaging material preparation method of PHBV composite membrane, comprises the following steps：
(1) superfine grinding after serpentine ball mill ball milling is obtained the serpentine powder body that particle diameter is 3 μm, by sodium stearate
It is dissolved in deionized water mix homogeneously and modification liquid be obtained, the weight of serpentine powder body and sodium stearate ratio is for 20:1, by snake stone powder
Body adds modification liquid, is placed in the water bath with thermostatic control that temperature is 80 DEG C and stirs 30 minutes, takes out, filters, being placed in temperature is 80 DEG C
Dry in drying baker to constant weight, obtain modified snake stone powder；
(2) plastify 2 minutes at adding the PHBV of 85 weight portions 140 DEG C in twin-roll plastic mixing mill, by the modified Serpentiss of 5 weight portions
The epoxy soybean oil of stricture of vagina stone powder and 4 weight portions sequentially adds twin-roll plastic mixing mill and continues plasticizing 8 minutes, thin logical 8 times, is mixed
Material；
(3) PTFE of the compatilizer of compound and 4 weight portions, 6 weight portions being added temperature in banbury is 170 DEG C, turns
Speed is melt blending 12 minutes under 60rpm, moves to double screw extruder extruding pelletization, obtains pellet, and extrusion temperature is 180-205
DEG C, rotating speed is 800rpm, and pellet cast film machine casting film-forming obtains the packaging material that thickness is 0.1mm and is combined with PHBV
Film.
Embodiment 2
A kind of packaging material preparation method of PHBV composite membrane, comprises the following steps：
(1) superfine grinding after serpentine ball mill ball milling is obtained the serpentine powder body that particle diameter is 3 μm, by sodium stearate
It is dissolved in deionized water mix homogeneously and modification liquid be obtained, the weight of serpentine powder body and sodium stearate ratio is for 20:1, by snake stone powder
Body adds modification liquid, is placed in the water bath with thermostatic control that temperature is 80 DEG C and stirs 30 minutes, takes out, filters, being placed in temperature is 80 DEG C
Dry in drying baker to constant weight, obtain modified snake stone powder；
(2) plastify 2 minutes at adding the PHBV of 88 weight portions 140 DEG C in twin-roll plastic mixing mill, by the modification of 2.5 weight portions
The epoxy soybean oil of snake stone powder and 4 weight portions sequentially adds twin-roll plastic mixing mill and continues plasticizing 8 minutes, thin logical 8 times, is mixed
Close material；
(3) PTFE of the compatilizer of compound and 4 weight portions, 5 weight portions being added temperature in banbury is 170 DEG C, turns
Speed is melt blending 12 minutes under 60rpm, moves to double screw extruder extruding pelletization, obtains pellet, and extrusion temperature is 180-205
DEG C, rotating speed is 800rpm, and pellet cast film machine casting film-forming obtains the packaging material that thickness is 0.1mm and is combined with PHBV
Film.
Embodiment 3
A kind of packaging material preparation method of PHBV composite membrane, comprises the following steps：
(1) superfine grinding after serpentine ball mill ball milling is obtained the serpentine powder body that particle diameter is 3 μm, by sodium stearate
It is dissolved in deionized water mix homogeneously and modification liquid be obtained, the weight of serpentine powder body and sodium stearate ratio is for 20:1, by snake stone powder
Body adds modification liquid, is placed in the water bath with thermostatic control that temperature is 80 DEG C and stirs 30 minutes, takes out, filters, being placed in temperature is 80 DEG C
Dry in drying baker to constant weight, obtain modified snake stone powder；
(2) plastify 2 minutes at adding the PHBV of 84 weight portions 140 DEG C in twin-roll plastic mixing mill, by the modified Serpentiss of 4 weight portions
The epoxy soybean oil of stricture of vagina stone powder and 4 weight portions sequentially adds twin-roll plastic mixing mill and continues plasticizing 8 minutes, thin logical 8 times, is mixed
Material；
(3) PTFE of the compatilizer of compound and 4 weight portions, 7 weight portions being added temperature in banbury is 170 DEG C, turns
Speed is melt blending 12 minutes under 60rpm, moves to double screw extruder extruding pelletization, obtains pellet, and extrusion temperature is 180-205
DEG C, rotating speed is 800rpm, and pellet cast film machine casting film-forming obtains the packaging material that thickness is 0.1mm and is combined with PHBV
Film.
Embodiment 4
A kind of packaging material preparation method of PHBV composite membrane, comprises the following steps：
(1) superfine grinding after serpentine ball mill ball milling is obtained the serpentine powder body that particle diameter is 3 μm, by sodium stearate
It is dissolved in deionized water mix homogeneously and modification liquid be obtained, the weight of serpentine powder body and sodium stearate ratio is for 20:1, by snake stone powder
Body adds modification liquid, is placed in the water bath with thermostatic control that temperature is 80 DEG C and stirs 30 minutes, takes out, filters, being placed in temperature is 80 DEG C
Dry in drying baker to constant weight, obtain modified snake stone powder；
(2) plastify 2 minutes at adding the PHBV of 80 weight portions 140 DEG C in twin-roll plastic mixing mill, by the modified Serpentiss of 6 weight portions
The epoxy soybean oil of stricture of vagina stone powder and 4 weight portions sequentially adds twin-roll plastic mixing mill and continues plasticizing 8 minutes, thin logical 8 times, is mixed
Material；
(3) PTFE of the compatilizer of compound and 4 weight portions, 8 weight portions being added temperature in banbury is 170 DEG C, turns
Speed is melt blending 12 minutes under 60rpm, moves to double screw extruder extruding pelletization, obtains pellet, and extrusion temperature is 180-205
DEG C, rotating speed is 800rpm, and pellet cast film machine casting film-forming obtains the packaging material that thickness is 0.1mm and is combined with PHBV
Film.
Embodiment 5
A kind of packaging material preparation method of PHBV composite membrane, comprises the following steps：
(1) superfine grinding after serpentine ball mill ball milling is obtained the serpentine powder body that particle diameter is 3 μm, by sodium stearate
It is dissolved in deionized water mix homogeneously and modification liquid be obtained, the weight of serpentine powder body and sodium stearate ratio is for 20:1, by snake stone powder
Body adds modification liquid, is placed in the water bath with thermostatic control that temperature is 80 DEG C and stirs 30 minutes, takes out, filters, being placed in temperature is 80 DEG C
Dry in drying baker to constant weight, obtain modified snake stone powder；
(2) plastify 2 minutes at adding the PHBV of 90 weight portions 140 DEG C in twin-roll plastic mixing mill, by the modified Serpentiss of 2 weight portions
The epoxy soybean oil of stricture of vagina stone powder and 4 weight portions sequentially adds twin-roll plastic mixing mill and continues plasticizing 8 minutes, thin logical 8 times, is mixed
Material；
(3) PTFE of the compatilizer of compound and 4 weight portions, 4 weight portions being added temperature in banbury is 170 DEG C, turns
Speed is melt blending 12 minutes under 60rpm, moves to double screw extruder extruding pelletization, obtains pellet, and extrusion temperature is 180-205
DEG C, rotating speed is 800rpm, and pellet cast film machine casting film-forming obtains the packaging material that thickness is 0.1mm and is combined with PHBV
Film.
Embodiment 6
A kind of packaging material preparation method of PHBV composite membrane, comprises the following steps：
(1) superfine grinding after serpentine ball mill ball milling is obtained the serpentine powder body that particle diameter is 3 μm, by sodium stearate
It is dissolved in deionized water mix homogeneously and modification liquid be obtained, the weight of serpentine powder body and sodium stearate ratio is for 20:1, by snake stone powder
Body adds modification liquid, is placed in the water bath with thermostatic control that temperature is 80 DEG C and stirs 30 minutes, takes out, filters, being placed in temperature is 80 DEG C
Dry in drying baker to constant weight, obtain modified snake stone powder；
(2) plastify 2 minutes at adding the PHBV of 87 weight portions 140 DEG C in twin-roll plastic mixing mill, by the modified Serpentiss of 3 weight portions
The epoxy soybean oil of stricture of vagina stone powder and 4 weight portions sequentially adds twin-roll plastic mixing mill and continues plasticizing 8 minutes, thin logical 8 times, is mixed
Material；
(3) PTFE of the compatilizer of compound and 4 weight portions, 5.5 weight portions to be added temperature in banbury be 170 DEG C,
Rotating speed is melt blending 12 minutes under 60rpm, moves to double screw extruder extruding pelletization, obtains pellet, and extrusion temperature is 180-
205 DEG C, rotating speed is 800rpm, and pellet cast film machine casting film-forming obtains the packaging material that thickness is 0.1mm multiple with PHBV
Close film.
After tested, embodiment 1-6 be obtained composite membrane and comparative example be obtained the heat distortion temperature of thin film and cantilever beam
Notch impact strength is as shown in the table, and wherein comparative example is the Chinese patent of Publication No. CN101508791B, heat distortion temperature
According to ASTMD648 test, Izod notched impact strength is tested according to ASTMD256：
As seen from the above table, the heat distortion temperature of the composite membrane that the present invention is obtained, Izod notched impact strength are all substantially good
The thin film being obtained in comparative example, shows preferable thermostability and toughness.
Above-described embodiment only principle of the illustrative present invention and its effect, not for the restriction present invention.Any ripe
The personage knowing this technology all can carry out modifications and changes without prejudice under the spirit and the scope of the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
All equivalent modifications becoming or change, must be covered by the claim of the present invention.
Claims (10)
1. a kind of packaging material with the preparation method of PHBV composite membrane it is characterised in that：Comprise the following steps：
(1) serpentine is obtained serpentine powder body with superfine grinding after ball mill ball milling, sodium stearate is dissolved in deionized water and mixes
Close and modification liquid is uniformly obtained, serpentine powder body is added modification liquid, be placed in water bath with thermostatic control and stir 30 minutes, take out, filter, put
Dry in drying baker to constant weight, obtain modified snake stone powder；
(2) PHBV of 80-90 weight portion is added in twin-roll plastic mixing mill and plastify 2 minutes, by the modified snake stone powder of 2-6 weight portion
And 4 the compatilizer of weight portion sequentially add twin-roll plastic mixing mill and continue plasticizing 8 minutes, thin logical 8 times, obtain compound；
(3) PTFE of the compatilizer of compound and 4 weight portions, 4-8 weight portion is added melt blending 12 minutes in banbury, move
To double screw extruder extruding pelletization, obtain pellet, pellet cast film machine casting film-forming obtains packaging material PHBV multiple
Close film.
2. a kind of packaging material according to claim 1 with the preparation method of PHBV composite membrane it is characterised in that：Described step
Suddenly, in (1), the particle diameter of serpentine powder body is 3 μm.
3. a kind of packaging material according to claim 1 with the preparation method of PHBV composite membrane it is characterised in that：Described step
Suddenly, in (1), the weight of serpentine powder body and sodium stearate is than for 20:1.
4. a kind of packaging material according to claim 1 with the preparation method of PHBV composite membrane it is characterised in that：Described step
Suddenly, in (1), the temperature of water bath with thermostatic control is 80 DEG C.
5. a kind of packaging material according to claim 1 with the preparation method of PHBV composite membrane it is characterised in that：Described step
Suddenly, in (1), the temperature of drying baker is 80 DEG C.
6. a kind of packaging material according to claim 1 with the preparation method of PHBV composite membrane it is characterised in that：Described step
Suddenly, in (2), the temperature of plasticizing is 140 DEG C.
7. a kind of packaging material according to claim 1 with the preparation method of PHBV composite membrane it is characterised in that：Described step
Suddenly, in (2), compatilizer is epoxy soybean oil.
8. a kind of packaging material according to claim 1 with the preparation method of PHBV composite membrane it is characterised in that：Described step
Suddenly in (3), the temperature of melt blending is 170 DEG C, and rotating speed is 60rpm.
9. a kind of packaging material according to claim 1 with the preparation method of PHBV composite membrane it is characterised in that：Described step
Suddenly in (3), the extrusion temperature of double screw extruder is 180-205 DEG C, and rotating speed is 800rpm.
10. a kind of packaging material according to claim 1 with the preparation method of PHBV composite membrane it is characterised in that：Described
In step (3), packaging material are 0.1mm with the thickness of PHBV composite membrane.
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| CN107383809A (en) * | 2017-06-20 | 2017-11-24 | 东莞市佳乾新材料科技有限公司 | A kind of food packaging PHBV composites and preparation method thereof |
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| CN101703805B (en) * | 2009-11-23 | 2012-10-17 | 天津工业大学 | Biocompatible and temperature-sensitive nano composite hydrogel and preparation method thereof |
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