CN105754309A - Preparation method of PHA (polyhydroxyalkanoate)-based composite - Google Patents
Preparation method of PHA (polyhydroxyalkanoate)-based composite Download PDFInfo
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- CN105754309A CN105754309A CN201610173165.8A CN201610173165A CN105754309A CN 105754309 A CN105754309 A CN 105754309A CN 201610173165 A CN201610173165 A CN 201610173165A CN 105754309 A CN105754309 A CN 105754309A
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- 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
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Abstract
The invention provides a preparation method of a PHA (polyhydroxyalkanoate)-based composite. The method comprises steps as follows: (1) chestnut shell powder is prepared; (2) potassium feldspar powder is dried and evenly mixed with stearic acid and the chestnut shell powder, the mixture is transferred to a high-speed kneader, subjected to primary stirring to be at 65 DEG C, subjected to secondary stirring, heated to 70 DEG C, continuously subjected to secondary stirring and cooled to the room temperature, and modified powder is obtained; (3) PHA is dried, crushed and added to a high-speed mixer with the modified powder to be mixed for 12 min, a mixture is obtained and added to a twin-screw extruder, melting, blending, extrusion, cooling and granulation are performed, and the PHA-based composite is obtained. The prepared composite has good mechanical properties and heat resistance and the wider application range.
Description
Technical field:
The present invention relates to a kind of composite, the preparation method particularly relating to a kind of polyhydroxyalkanoate based composites.
Background technology:
Polyhydroxyalkanoate (English is abbreviated as PHA) is polyester in a kind of born of the same parents synthesized by a lot of antibacterials, existing primarily as the Stored Matter of carbon source and the energy in vivo, it has the biodegradability not available for physicochemical characteristic and synthetic plastic, the biocompatibility that are similar to synthetic plastic.Natural or synthesis biodegradable macromolecular material often has significantly high water vapo(u)r transmission, and this is disadvantageous in food fresh keeping, and PHA then has good barrier properties for gases so that it is possible application is in the fresh goods fresh-keeping packaging of long period.Another aspect, PHA also has good hydrolytic stability, the cup be made up of PHA is machine-washed 20 circulations with the automatic bowl of 75 DEG C, and its shape and molecular weight are all without changing.Additionally, with other TPO, polyaromatic base polymer ratio, PHA also has good ultraviolet stability.PHA is alternatively arranged as the source of biodegradable environmentally friendly solvent, if ethyl hydroxy acid EHB (ethyl3 hydroxy butyrate) is water miscible, has low volatility, it is possible to for cleaning agent, adhesive, dyestuff, ink solvent.Performance excellent above makes PHA can be applied in the fields such as packaging material, jointing material, sprayed on material and dress material, utensil class material, electronic product, durable consumer goods, agricultural products, automated production, chemical mediator and solvent.
Publication number is CN102850741A, publication date is 2013.01.02, apply for the Chinese patent of artificial Jiangsu million new material Science and Technology Ltd. discloses " a kind of polyhydroxyalkanoate biodegradable composites and preparation method thereof and application ", this composite includes following components by weight ratio: homopolymerization polyhydroxyalkanoate 30-80 part, copolymerization polyhydroxyalkanoate 20-70 part, Plant fiber's 15-40 part, coupling agent 1.5-6 part, antioxidant 0.5-10 part, processing aid 1-6 part.Polyhydroxyalkanoate biodegradable composites prepared by this invention can substitute the general-purpose plastics such as tradition modified polypropene completely, and has fully bio-degradable characteristic, can 100% recovery.But, this composite yet suffers from certain defect: mechanical property is not ideal enough, and heat resistance is poor, therefore constrains its range of application.
Summary of the invention:
The preparation method that the technical problem to be solved in the present invention is to provide a kind of polyhydroxyalkanoate based composites, the composite prepared has good mechanical property and heat resistance, and range of application is wider.
For solving above-mentioned technical problem, the technical scheme is that
The preparation method of a kind of polyhydroxyalkanoate based composites, comprises the following steps:
(1) being soaked in hydrochloric acid solution by chestnut shell 24 hours, take out and be placed in vacuum drying oven and dry to constant weight at 70 DEG C, put into grinding in ball grinder 5 hours after smashing with pulverizer together with abrading-ball, being cooled to room temperature after taking-up, to obtain chestnut shell powder standby；
(2) feldspar in powder is dried 8 hours at 80 DEG C, the chestnut shell powder obtained with stearic acid and step (1) is mixed homogeneously, move in high-speed kneading machine, one-level stirring makes two grades of stirrings into after 65 DEG C, temperature continues two grades after rising to 70 DEG C and stirs 40 minutes, obtains modified powder after being cooled to room temperature；
(3) polyhydroxyalkanoate is pulverized after dry 5 hours at 90 DEG C, add together with the modified powder obtained with step (2) in high-speed mixer and mix 12 minutes, obtain compound, add mixture into melted, blended in double screw extruder, extrusion, cooling, pelletizing, obtain polyhydroxyalkanoate based composites.
Preferably, in step of the present invention (1), the volume fraction of hydrochloric acid solution is 12%.
Preferably, in step of the present invention (1), the diameter of abrading-ball is 2mm.
Preferably, in step of the present invention (1), the weight ratio of chestnut shell and abrading-ball is 3.5:1.
Preferably, in step of the present invention (2), feldspar in powder, chestnut shell powder, stearic weight ratio are 100:50:1.
Preferably, in step of the present invention (2), mixing speed during one-level stirring is 600rpm.
Preferably, in step of the present invention (2), mixing speed during two grades of stirrings is 1200rpm.
Preferably, in step of the present invention (3), count by weight, polyhydroxyalkanoate 70-75 part, modified powder 25-30 part.
Preferably, in step of the present invention (3), the mixing speed of high-speed mixer is 1400rpm.
Preferably, in step of the present invention (3), the melt temperature of double screw extruder is 160-190 DEG C, and screw speed is 400rpm.
Compared with prior art, the method have the advantages that
null1) chestnut shell is the shell of Semen Castaneae，Belong to recyclability vegetable material，There is good mechanical performance and degradation property，But there is more impurity in its surface，And the compatibility between PHA matrix is not good，And granule is bigger，Dispersing uniformity is poor，Therefore the present invention first passes through hydrochloric acid and eliminates the impurity on chestnut shell surface，Again through ball mill, chestnut shell ball milling become the only small chestnut shell powder of particle diameter，Then pass through stearic acid and chestnut shell powder has been carried out surface treatment，With stearic acid, the hydroxyl on chestnut shell powder surface there occurs that chemical bonding reacts，Stearic organic group and PHA matrix can form chemical bond simultaneously，The compatibility between chestnut shell powder and PHA matrix is made to obtain very big improvement，The interface bond strength formed have also been obtained large increase，Make chestnut shell powder that PHA matrix can be played good potentiation，Thus substantially increasing the mechanical property of composite；Additionally, chestnut shell itself has certain antibacterial and anti-inflammation functions, the anti-microbial property of composite therefore also can be effectively improved.
2) potash feldspar is a kind of aluminium silicate mineral with lamellar structure, its heat resistance is fine, good interface cohesion can be formed with PHA matrix after stearic acid surface processes, and stearic acid enters between the lamella of potash feldspar, lamella is strutted the spacing increasing lamella, the macromolecular chain making PHA can enter potash feldspar lamella, form the good intercalation synthesis structure in interface, when being subject to high temperature action, potash feldspar lamella can play good heat iris action, it is substantially reduced the heat impact on PHA, thus being greatly improved the heat resistance of composite；Additionally, the hardness of potash feldspar is significantly high, wearability is fine, therefore also can be effectively improved the anti-wear performance of composite.
Detailed description of the invention:
Describing the present invention in detail below in conjunction with specific embodiment, illustrative examples and explanation in this present invention are used for explaining the present invention, but not as a limitation of the invention.
Embodiment 1
The preparation method of a kind of polyhydroxyalkanoate based composites, comprises the following steps:
(1) chestnut shell is soaked in the hydrochloric acid solution that volume fraction is 12% 24 hours, taking-up is placed in vacuum drying oven and dries to constant weight at 70 DEG C, after smashing with pulverizer with diameter be put into grinding in ball grinder 5 hours together with 2mm abrading-ball, the weight ratio of chestnut shell and abrading-ball is 3.5:1, and being cooled to room temperature after taking-up, to obtain chestnut shell powder standby；
(2) feldspar in powder is dried 8 hours at 80 DEG C, the chestnut shell powder obtained with stearic acid and step (1) is mixed homogeneously, move in high-speed kneading machine, feldspar in powder, chestnut shell powder, stearic weight ratio are 100:50:1, one-level stirring (mixing speed is 600rpm) makes two grades of stirrings (mixing speed is 1200rpm) into after 65 DEG C, temperature continues two grades after rising to 70 DEG C and stirs 40 minutes, obtains modified powder after being cooled to room temperature；
(3) count by weight, 75 parts of polyhydroxyalkanoates are pulverized after dry 5 hours at 90 DEG C, adding mixing speed in high-speed mixer together with the modified powder obtained with 25 parts of steps (2) is mix 12 minutes under 1400rpm, obtain compound, add mixture into melted, blended in double screw extruder, extrusion, cooling, pelletizing, the melt temperature of double screw extruder is 160-190 DEG C, and screw speed is 400rpm, obtains polyhydroxyalkanoate based composites.
Embodiment 2
The preparation method of a kind of polyhydroxyalkanoate based composites, comprises the following steps:
(1) chestnut shell is soaked in the hydrochloric acid solution that volume fraction is 12% 24 hours, taking-up is placed in vacuum drying oven and dries to constant weight at 70 DEG C, after smashing with pulverizer with diameter be put into grinding in ball grinder 5 hours together with 2mm abrading-ball, the weight ratio of chestnut shell and abrading-ball is 3.5:1, and being cooled to room temperature after taking-up, to obtain chestnut shell powder standby；
(2) feldspar in powder is dried 8 hours at 80 DEG C, the chestnut shell powder obtained with stearic acid and step (1) is mixed homogeneously, move in high-speed kneading machine, feldspar in powder, chestnut shell powder, stearic weight ratio are 100:50:1, one-level stirring (mixing speed is 600rpm) makes two grades of stirrings (mixing speed is 1200rpm) into after 65 DEG C, temperature continues two grades after rising to 70 DEG C and stirs 40 minutes, obtains modified powder after being cooled to room temperature；
(3) count by weight, 72 parts of polyhydroxyalkanoates are pulverized after dry 5 hours at 90 DEG C, adding mixing speed in high-speed mixer together with the modified powder obtained with 28 parts of steps (2) is mix 12 minutes under 1400rpm, obtain compound, add mixture into melted, blended in double screw extruder, extrusion, cooling, pelletizing, the melt temperature of double screw extruder is 160-190 DEG C, and screw speed is 400rpm, obtains polyhydroxyalkanoate based composites.
Embodiment 3
The preparation method of a kind of polyhydroxyalkanoate based composites, comprises the following steps:
(1) chestnut shell is soaked in the hydrochloric acid solution that volume fraction is 12% 24 hours, taking-up is placed in vacuum drying oven and dries to constant weight at 70 DEG C, after smashing with pulverizer with diameter be put into grinding in ball grinder 5 hours together with 2mm abrading-ball, the weight ratio of chestnut shell and abrading-ball is 3.5:1, and being cooled to room temperature after taking-up, to obtain chestnut shell powder standby；
(2) feldspar in powder is dried 8 hours at 80 DEG C, the chestnut shell powder obtained with stearic acid and step (1) is mixed homogeneously, move in high-speed kneading machine, feldspar in powder, chestnut shell powder, stearic weight ratio are 100:50:1, one-level stirring (mixing speed is 600rpm) makes two grades of stirrings (mixing speed is 1200rpm) into after 65 DEG C, temperature continues two grades after rising to 70 DEG C and stirs 40 minutes, obtains modified powder after being cooled to room temperature；
(3) count by weight, 74 parts of polyhydroxyalkanoates are pulverized after dry 5 hours at 90 DEG C, adding mixing speed in high-speed mixer together with the modified powder obtained with 26 parts of steps (2) is mix 12 minutes under 1400rpm, obtain compound, add mixture into melted, blended in double screw extruder, extrusion, cooling, pelletizing, the melt temperature of double screw extruder is 160-190 DEG C, and screw speed is 400rpm, obtains polyhydroxyalkanoate based composites.
Embodiment 4
The preparation method of a kind of polyhydroxyalkanoate based composites, comprises the following steps:
(1) chestnut shell is soaked in the hydrochloric acid solution that volume fraction is 12% 24 hours, taking-up is placed in vacuum drying oven and dries to constant weight at 70 DEG C, after smashing with pulverizer with diameter be put into grinding in ball grinder 5 hours together with 2mm abrading-ball, the weight ratio of chestnut shell and abrading-ball is 3.5:1, and being cooled to room temperature after taking-up, to obtain chestnut shell powder standby；
(2) feldspar in powder is dried 8 hours at 80 DEG C, the chestnut shell powder obtained with stearic acid and step (1) is mixed homogeneously, move in high-speed kneading machine, feldspar in powder, chestnut shell powder, stearic weight ratio are 100:50:1, one-level stirring (mixing speed is 600rpm) makes two grades of stirrings (mixing speed is 1200rpm) into after 65 DEG C, temperature continues two grades after rising to 70 DEG C and stirs 40 minutes, obtains modified powder after being cooled to room temperature；
(3) count by weight, 73 parts of polyhydroxyalkanoates are pulverized after dry 5 hours at 90 DEG C, adding mixing speed in high-speed mixer together with the modified powder obtained with 27 parts of steps (2) is mix 12 minutes under 1400rpm, obtain compound, add mixture into melted, blended in double screw extruder, extrusion, cooling, pelletizing, the melt temperature of double screw extruder is 160-190 DEG C, and screw speed is 400rpm, obtains polyhydroxyalkanoate based composites.
Embodiment 5
The preparation method of a kind of polyhydroxyalkanoate based composites, comprises the following steps:
(1) chestnut shell is soaked in the hydrochloric acid solution that volume fraction is 12% 24 hours, taking-up is placed in vacuum drying oven and dries to constant weight at 70 DEG C, after smashing with pulverizer with diameter be put into grinding in ball grinder 5 hours together with 2mm abrading-ball, the weight ratio of chestnut shell and abrading-ball is 3.5:1, and being cooled to room temperature after taking-up, to obtain chestnut shell powder standby；
(2) feldspar in powder is dried 8 hours at 80 DEG C, the chestnut shell powder obtained with stearic acid and step (1) is mixed homogeneously, move in high-speed kneading machine, feldspar in powder, chestnut shell powder, stearic weight ratio are 100:50:1, one-level stirring (mixing speed is 600rpm) makes two grades of stirrings (mixing speed is 1200rpm) into after 65 DEG C, temperature continues two grades after rising to 70 DEG C and stirs 40 minutes, obtains modified powder after being cooled to room temperature；
(3) count by weight, 70 parts of polyhydroxyalkanoates are pulverized after dry 5 hours at 90 DEG C, adding mixing speed in high-speed mixer together with the modified powder obtained with 30 parts of steps (2) is mix 12 minutes under 1400rpm, obtain compound, add mixture into melted, blended in double screw extruder, extrusion, cooling, pelletizing, the melt temperature of double screw extruder is 160-190 DEG C, and screw speed is 400rpm, obtains polyhydroxyalkanoate based composites.
Embodiment 6
The preparation method of a kind of polyhydroxyalkanoate based composites, comprises the following steps:
(1) chestnut shell is soaked in the hydrochloric acid solution that volume fraction is 12% 24 hours, taking-up is placed in vacuum drying oven and dries to constant weight at 70 DEG C, after smashing with pulverizer with diameter be put into grinding in ball grinder 5 hours together with 2mm abrading-ball, the weight ratio of chestnut shell and abrading-ball is 3.5:1, and being cooled to room temperature after taking-up, to obtain chestnut shell powder standby；
(2) feldspar in powder is dried 8 hours at 80 DEG C, the chestnut shell powder obtained with stearic acid and step (1) is mixed homogeneously, move in high-speed kneading machine, feldspar in powder, chestnut shell powder, stearic weight ratio are 100:50:1, one-level stirring (mixing speed is 600rpm) makes two grades of stirrings (mixing speed is 1200rpm) into after 65 DEG C, temperature continues two grades after rising to 70 DEG C and stirs 40 minutes, obtains modified powder after being cooled to room temperature；
(3) count by weight, 71 parts of polyhydroxyalkanoates are pulverized after dry 5 hours at 90 DEG C, adding mixing speed in high-speed mixer together with the modified powder obtained with 29 parts of steps (2) is mix 12 minutes under 1400rpm, obtain compound, add mixture into melted, blended in double screw extruder, extrusion, cooling, pelletizing, the melt temperature of double screw extruder is 160-190 DEG C, and screw speed is 400rpm, obtains polyhydroxyalkanoate based composites.
After tested, composite and mechanical property and the heat resistance of comparative example that embodiment 1-6 prepares are as shown in the table, wherein:
Comparative example is publication number is the Chinese patent of CN102850741A,
Mechanical property tests the hot strength of detected materials, bending strength according to ASTMD638,
Heat resistance tests the heat distortion temperature of detected materials according to ASTMD648:
As seen from the above table, the hot strength of the composite that the present invention prepares, bending strength are all better than comparative example, and it is all fine that heat distortion temperature is then much higher than comparative example, mechanical property and heat resistance.
Above-described embodiment is illustrative principles of the invention and effect thereof only, not for the restriction present invention.Above-described embodiment all under the spirit and category of the present invention, can be modified or change by any those skilled in the art.Therefore, art has usually intellectual such as modifying without departing from all equivalences completed under disclosed spirit and technological thought or change, must be contained by the claim of the present invention.
Claims (10)
1. the preparation method of a polyhydroxyalkanoate based composites, it is characterised in that: comprise the following steps:
(1) being soaked in hydrochloric acid solution by chestnut shell 24 hours, take out and be placed in vacuum drying oven and dry to constant weight at 70 DEG C, put into grinding in ball grinder 5 hours after smashing with pulverizer together with abrading-ball, being cooled to room temperature after taking-up, to obtain chestnut shell powder standby；
(2) feldspar in powder is dried 8 hours at 80 DEG C, the chestnut shell powder obtained with stearic acid and step (1) is mixed homogeneously, move in high-speed kneading machine, one-level stirring makes two grades of stirrings into after 65 DEG C, temperature continues two grades after rising to 70 DEG C and stirs 40 minutes, obtains modified powder after being cooled to room temperature；
(3) polyhydroxyalkanoate is pulverized after dry 5 hours at 90 DEG C, add together with the modified powder obtained with step (2) in high-speed mixer and mix 12 minutes, obtain compound, add mixture into melted, blended in double screw extruder, extrusion, cooling, pelletizing, obtain polyhydroxyalkanoate based composites.
2. the preparation method of a kind of polyhydroxyalkanoate based composites according to claim 1, it is characterised in that: in described step (1), the volume fraction of hydrochloric acid solution is 12%.
3. the preparation method of a kind of polyhydroxyalkanoate based composites according to claim 1, it is characterised in that: in described step (1), the diameter of abrading-ball is 2mm.
4. the preparation method of a kind of polyhydroxyalkanoate based composites according to claim 1, it is characterised in that: in described step (1), the weight ratio of chestnut shell and abrading-ball is 3.5:1.
5. the preparation method of a kind of polyhydroxyalkanoate based composites according to claim 1, it is characterised in that: in described step (2), feldspar in powder, chestnut shell powder, stearic weight ratio are 100:50:1.
6. the preparation method of a kind of polyhydroxyalkanoate based composites according to claim 1, it is characterised in that: in described step (2), mixing speed during one-level stirring is 600rpm.
7. the preparation method of a kind of polyhydroxyalkanoate based composites according to claim 1, it is characterised in that: in described step (2), mixing speed during two grades of stirrings is 1200rpm.
8. the preparation method of a kind of polyhydroxyalkanoate based composites according to claim 1, it is characterised in that: in described step (3), count by weight, polyhydroxyalkanoate 70-75 part, modified powder 25-30 part.
9. the preparation method of a kind of polyhydroxyalkanoate based composites according to claim 1, it is characterised in that: in described step (3), the mixing speed of high-speed mixer is 1400rpm.
10. the preparation method of a kind of polyhydroxyalkanoate based composites according to claim 1, it is characterised in that: in described step (3), the melt temperature of double screw extruder is 160-190 DEG C, and screw speed is 400rpm.
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| WO2024112195A1 (en) * | 2022-11-21 | 2024-05-30 | Rosiro Intellectual Property B.V. | Polymer composite comprising micronized feldspar |
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Application publication date: 20160713 |
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| RJ01 | Rejection of invention patent application after publication |