CN107245232A - A kind of PHBV composites being modified based on bacteria cellulose - Google Patents
A kind of PHBV composites being modified based on bacteria cellulose Download PDFInfo
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- CN107245232A CN107245232A CN201710555880.2A CN201710555880A CN107245232A CN 107245232 A CN107245232 A CN 107245232A CN 201710555880 A CN201710555880 A CN 201710555880A CN 107245232 A CN107245232 A CN 107245232A
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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
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/12—Applications used for fibers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2312/00—Crosslinking
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Abstract
The present invention provides a kind of PHBV composites being modified based on bacteria cellulose, and the composite includes the micron order bamboo shoots bacteria cellulose and poly butyric of modification without acid esters PHBV, and specific preparation method is：By bamboo shoots bacteria cellulose, vacuum freeze drying is crushed through micronizer, sieving, obtains micron order bamboo shoots bacteria cellulose；Micron order bamboo shoots bacteria cellulose is added in distilled water, high-speed stirred, silane coupler and azodiisobutyronitrile, heating response is added dropwise, modified bamboo shoots bacterial cellulose solution is obtained；Poly butyric is added in dichloromethane without acid esters PHBV and stirred, is mixed with modified bamboo shoots bacterial cellulose solution, N HOSu NHSs are added dropwise, stirring, solvent flashing, solidification obtains the PHBV composites being modified based on bacteria cellulose.PHBV composites prepared by the present invention are modified PHBV using bacteria cellulose, improve the toughness and hydrophily of PHBV composites.
Description
Technical field
The invention belongs to PHBV technical field of composite materials, and in particular to a kind of to be answered based on the PHBV that bacteria cellulose is modified
Condensation material.
Background technology
In recent years, with rise in oil price caused by the increasingly depleted of petroleum resources, and petrochemical industry source plastics
Difficult degradation caused by environmental pollution so that domestic and international researcher starts to be directed to grinding for the degradation plastic of non-petroleum sources
Study carefully.The biopolymer of industrialized production mainly has PHA PH A, polylactic acid PLA, biological polyethylene, life at present
Thing nylon etc..Poly-β-hybroxybutyric acid-beta-hydroxy valerate P HBV are a member in PHA extended familys, be using starch as raw material,
The green bio material of fermenting and producing, it is many excellent with biodegradability, biocompatibility, piezoelectricity, optical activity etc.
Good characteristic, has wide practical use in fields such as biomedicine, agricultural, daily lifes.
But PHBV easily generates large-sized spherocrystal, with spherocrystal center to external expansion formed many circular crackings with
And many splittings are formed along spherulitic growth direction, so as to cause PHBV quality very crisp, and there is the meeting during room temperature storage
The problem of generation secondary crystallization, it is therefore desirable to be modified to PHBV.It is a kind of siliceous disclosed in Chinese patent CN 104530672B
The preparation method of micrometer fibers toughness reinforcing PHBV composites, by the silica fibre and hydrogen-oxygen using rice straw, wheat straw and reed as raw material
Change sodium water solution blending, after disperseing through polyethylene glycol, broken, separation, vacuum drying obtain siliceous micrometer fibers, will be siliceous micro-
Rice fiber and PHBV melt blendings, extrusion granulating obtain product.PHBV composite woods disclosed in Chinese patent CN 103525048B
Material and its preparation method and application, by the chloroform of the resin containing PHBV or 2,2,2- trifluoroethanol solution and polyamide-amide are tree-like
Polymer Solution is mixed, and is stood after heating stirring, and plastic film mulch, solvent flashing obtains PHBV composites.Can by above-mentioned prior art
Know, by adding micro nanometer fiber or grafting polymer material in PHBV materials, making to form three-dimensional netted hole in PHBV
Structure, destroys PHBV regularity, declines its crystallinity, so as to improve the toughness of PHBV composites.Wherein, physics is added
Method is more easy, and is produced without accessory substance, but is the dispersiveness and consumption of additive the drawbacks of physics adding method
Have a great impact to the modified effect of PHBV composites, the compatibility for improving additive and PHBV seems particularly significant.
The content of the invention
, will be micro- the technical problem to be solved in the present invention is to provide a kind of PHBV composites being modified based on bacteria cellulose
Nanoscale bamboo shoots bacteria cellulose is crosslinked using n-hydroxysuccinimide and PHBV, prepared after coupling agent modified
PHBV composites.Bacteria cellulose is combined by PHBV composites prepared by the present invention with PHBV, improves PHBV composites
Toughness and hydrophily.
In order to solve the above technical problems, the technical scheme is that：
A kind of PHBV composites being modified based on bacteria cellulose, it is described to be answered based on the P HBV that bacteria cellulose is modified
Condensation material includes the micron order bamboo shoots bacteria cellulose and poly butyric of modification without acid esters PHBV, the micron order bamboo of the modification
Bamboo shoot bacteria cellulose is the micron order bamboo shoots bacteria cellulose of cross-linking silane coupling agent, and the micron order bamboo shoots bacterium of the modification is fine
Dimension is plain and poly butyric is connected without n-hydroxysuccinimide crosslinking is passed through between acid esters PHBV.
As the preferred of above-mentioned technical proposal, preparation method comprises the following steps：
(1) by bamboo shoots bacteria cellulose vacuum freeze drying, crushed through micronizer, sieve, obtain micron order bamboo shoots
Bacteria cellulose；
(2) the micron order bamboo shoots bacteria cellulose for preparing step (1) is added in distilled water, high-speed stirred, and silicon is added dropwise
Alkane coupling agent and azodiisobutyronitrile, heating response obtain modified bamboo shoots bacterial cellulose solution；
(3) poly butyric is added in dichloromethane without acid esters PHBV and stirred, the modification prepared with step (2)
Bamboo shoots bacterial cellulose solution mixing, be added dropwise n-hydroxysuccinimide, stirring, solvent flashing, solidification obtain be based on bacterium
Cellulose modified PHBV composites.
As the preferred of above-mentioned technical proposal, in the step (1), the temperature of vacuum freeze drying is -10--20 DEG C, when
Between be 24h.
As the preferred of above-mentioned technical proposal, in the step (1), a diameter of 50- of micron order bamboo shoots bacteria cellulose
100μm。
As the preferred of above-mentioned technical proposal, in the step (2), the speed of high-speed stirred is 2000-2500r/min,
Time is 30min.
As the preferred of above-mentioned technical proposal, in the step (2), micron order bamboo shoots bacteria cellulose, silane coupler
Mass ratio with azodiisobutyronitrile is 10:1:0.2-0.4.
As the preferred of above-mentioned technical proposal, in the step (2), the temperature of heating response is 70-90 DEG C, and the time is 4-
6h。
As the preferred of above-mentioned technical proposal, in the step (3), bamboo shoots of the poly butyric without acid esters PHBV, modification
The mass ratio of bacteria cellulose and n-hydroxysuccinimide is 20-30:10-15:5-7.
As the preferred of above-mentioned technical proposal, in the step (3), the temperature of stirring is 40-50 DEG C, and the time of stirring is
48h。
As the preferred of above-mentioned technical proposal, in the step (3), the PHB V composite woods being modified based on bacteria cellulose
Material can be fiber, film-form or bulk material.
Compared with prior art, the invention has the advantages that：
(1) it is thin that what prepared by the present invention includes modified micron order bamboo shoots based on the PHBV composites that bacteria cellulose is modified
Fungin and poly butyric are without acid esters PHBV, and the wide material sources of bamboo shoots bacteria cellulose, crystallinity is high high with the degree of polymerization, tool
There are high tensile strength and a modulus of elasticity, and hydrophilic power due to bamboo shoots bacteria cellulose and hold that oily power is good, bamboo shoots bacterium is fine
Dimension element can adsorb poly butyric without acid esters PHBV, reduce the generation in PHBV crack, improve poly butyric without acid esters
The toughness and elasticity of PHBV composites, and micron order bamboo shoots bacteria cellulose is by cross-linking silane coupling agent, enhances thin
Compatibility performance between fungin and PHBV, improves dispersive property of the micron order bacteria cellulose in PHBV, then will change
Property micron order bamboo shoots bacteria cellulose and poly butyric it is solid without being crosslinked between acid esters PHBV by n-hydroxysuccinimide
Change, significantly improve the toughness of the solidification PHBV composites of preparation, and degradability, thermoplastic processing and biocompatibility are equal
It is not affected, is conducive to improving the curing performance of PHBV composites.
(2) preparation method controllability of the invention is good, is not simple between added material bacteria cellulose and PHBV
Blending, bacteria cellulose is crosslinked with PHBV phases after modified, is crosslinked on the basis of bacteria cellulose and PHBV are sufficiently mixed, profit
Acted on the physical absorption of bacteria cellulose, expansive force and chemical crosslinking, prevent the generation in gap in PHBV materials, improve PHBV
Adhesion between segment, and bacteria cellulose has excellent degradability and bio-compatible performance, to the PHBV feature of environmental protection
Can be without influence, therefore the excellent combination property of the PHBV composites prepared improves the suitable application area of PHBV composites.
Embodiment
Describe the present invention in detail below in conjunction with specific embodiment, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1：
(1) by bamboo shoots bacteria cellulose at -10 DEG C vacuum freeze drying 24h, crushed through micronizer, sieve, obtain
To a diameter of 50 μm of micron order bamboo shoots bacteria cellulose.
(2) micron order bamboo shoots bacteria cellulose is added in distilled water, with 2000r/min speed high-speed stirred
30min, is 10 according to the mass ratio of micron order bamboo shoots bacteria cellulose, silane coupler and azodiisobutyronitrile:1:0.2, drop
Plus silane coupler and azodiisobutyronitrile, the heating response 4h at 70 DEG C, obtain modified bamboo shoots bacterial cellulose solution.
(3) according to poly butyric without acid esters PHBV, the bamboo shoots bacteria cellulose of modification and n-hydroxysuccinimide
Mass ratio is 20:10:5, poly butyric is added in dichloromethane without acid esters PHBV and stirred, it is thin with modified bamboo shoots
Fungin solution is mixed, and n-hydroxysuccinimide is added dropwise, 48h is stirred at 40 DEG C, solvent flashing, solidification obtain fiber,
The PHBV composites being modified based on bacteria cellulose of film-form or bulk.
Embodiment 2：
(1) by bamboo shoots bacteria cellulose at -20 DEG C vacuum freeze drying 24h, crushed through micronizer, sieve, obtain
To a diameter of 100 μm of micron order bamboo shoots bacteria cellulose.
(2) micron order bamboo shoots bacteria cellulose is added in distilled water, with 2500r/min speed high-speed stirred
30min, is 10 according to the mass ratio of micron order bamboo shoots bacteria cellulose, silane coupler and azodiisobutyronitrile:1:0.4, drop
Plus silane coupler and azodiisobutyronitrile, the heating response 6h at 90 DEG C, obtain modified bamboo shoots bacterial cellulose solution.
(3) according to poly butyric without acid esters PHBV, the bamboo shoots bacteria cellulose of modification and n-hydroxysuccinimide
Mass ratio is 30:15:7, poly butyric is added in dichloromethane without acid esters PHBV and stirred, it is thin with modified bamboo shoots
Fungin solution is mixed, and n-hydroxysuccinimide is added dropwise, 48h is stirred at 50 DEG C, solvent flashing, solidification obtain fiber,
The PHBV composites being modified based on bacteria cellulose of film-form or bulk.
Embodiment 3：
(1) by bamboo shoots bacteria cellulose at -15 DEG C vacuum freeze drying 24h, crushed through micronizer, sieve, obtain
To a diameter of 60 μm of micron order bamboo shoots bacteria cellulose.
(2) micron order bamboo shoots bacteria cellulose is added in distilled water, with 2200r/min speed high-speed stirred
30min, is 10 according to the mass ratio of micron order bamboo shoots bacteria cellulose, silane coupler and azodiisobutyronitrile:1:0.3, drop
Plus silane coupler and azodiisobutyronitrile, the heating response 5h at 80 DEG C, obtain modified bamboo shoots bacterial cellulose solution.
(3) according to poly butyric without acid esters PHBV, the bamboo shoots bacteria cellulose of modification and n-hydroxysuccinimide
Mass ratio is 25:13:6, poly butyric is added in dichloromethane without acid esters PHBV and stirred, it is thin with modified bamboo shoots
Fungin solution is mixed, and n-hydroxysuccinimide is added dropwise, 48h is stirred at 45 DEG C, solvent flashing, solidification obtain fiber,
The PHBV composites being modified based on bacteria cellulose of film-form or bulk.
Embodiment 4：
(1) by bamboo shoots bacteria cellulose at -13 DEG C vacuum freeze drying 24h, crushed through micronizer, sieve, obtain
To a diameter of 75 μm of micron order bamboo shoots bacteria cellulose.
(2) micron order bamboo shoots bacteria cellulose is added in distilled water, with 2400r/min speed high-speed stirred
30min, is 10 according to the mass ratio of micron order bamboo shoots bacteria cellulose, silane coupler and azodiisobutyronitrile:1:0.25, drop
Plus silane coupler and azodiisobutyronitrile, the heating response 4.5h at 75 DEG C, obtain modified bamboo shoots bacterial cellulose solution.
(3) according to poly butyric without acid esters PHBV, the bamboo shoots bacteria cellulose of modification and n-hydroxysuccinimide
Mass ratio is 26:13:5, poly butyric is added in dichloromethane without acid esters PHBV and stirred, it is thin with modified bamboo shoots
Fungin solution is mixed, and n-hydroxysuccinimide is added dropwise, 48h is stirred at 43 DEG C, solvent flashing, solidification obtain fiber,
The PHBV composites being modified based on bacteria cellulose of film-form or bulk.
Embodiment 5：
(1) by bamboo shoots bacteria cellulose at -20 DEG C vacuum freeze drying 24h, crushed through micronizer, sieve, obtain
To a diameter of 60 μm of micron order bamboo shoots bacteria cellulose.
(2) micron order bamboo shoots bacteria cellulose is added in distilled water, with 2500r/min speed high-speed stirred
30min, is 10 according to the mass ratio of micron order bamboo shoots bacteria cellulose, silane coupler and azodiisobutyronitrile:1:0.2, drop
Plus silane coupler and azodiisobutyronitrile, the heating response 6h at 85 DEG C, obtain modified bamboo shoots bacterial cellulose solution.
(3) according to poly butyric without acid esters PHBV, the bamboo shoots bacteria cellulose of modification and n-hydroxysuccinimide
Mass ratio is 30:14:5, poly butyric is added in dichloromethane without acid esters PHBV and stirred, it is thin with modified bamboo shoots
Fungin solution is mixed, and n-hydroxysuccinimide is added dropwise, 48h is stirred at 45 DEG C, solvent flashing, solidification obtain fiber,
The PHBV composites being modified based on bacteria cellulose of film-form or bulk.
Embodiment 6：
(1) by bamboo shoots bacteria cellulose at -17 DEG C vacuum freeze drying 24h, crushed through micronizer, sieve, obtain
To a diameter of 95 μm of micron order bamboo shoots bacteria cellulose.
(2) micron order bamboo shoots bacteria cellulose is added in distilled water, with 2000r/min speed high-speed stirred
30min, is 10 according to the mass ratio of micron order bamboo shoots bacteria cellulose, silane coupler and azodiisobutyronitrile:1:0.3, drop
Plus silane coupler and azodiisobutyronitrile, the heating response 6h at 70 DEG C, obtain modified bamboo shoots bacterial cellulose solution.
(3) according to poly butyric without acid esters PHBV, the bamboo shoots bacteria cellulose of modification and n-hydroxysuccinimide
Mass ratio is 20:15:6, poly butyric is added in dichloromethane without acid esters PHBV and stirred, it is thin with modified bamboo shoots
Fungin solution is mixed, and n-hydroxysuccinimide is added dropwise, 48h is stirred at 50 DEG C, solvent flashing, solidification obtain fiber,
The PHBV composites being modified based on bacteria cellulose of film-form or bulk.
Comparative example 1：
It is 20 according to mass ratio of the poly butyric without acid esters PHBV, bamboo shoots bacteria cellulose:10, by poly butyric without
Acid esters PHBV, which is added in dichloromethane, to stir, and is mixed with bamboo shoots bacterial cellulose solution, and stirring is equal, solvent flashing, Gu
Change the PHBV composites being modified based on bacteria cellulose for obtaining fiber, film-form or bulk.
Comparative example 2：
It is 20 according to mass ratio of the poly butyric without acid esters PHBV, cellulose:10, by poly butyric without acid esters PHBV
It is added in dichloromethane and stirs, mixed with cellulose solution, stirring is equal, solvent flashing, solidification obtains fiber, film-form
Or it is block based on cellulose modified PHBV composites.
After testing, it is prepared by the PHBV composites being modified based on bacteria cellulose and comparative example that prepared by embodiment 1-6
PHBV composites mechanical property, heat resistance, the result of degradability it is as follows：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative example 1 | Comparative example 2 | |
| Tensile strength (MPa) | 6.8 | 7.4 | 7.0 | 6.9 | 7.1 | 7.3 | 5.3 | 5.1 |
| Thermal degradation temperature (DEG C) | 285 | 283 | 280 | 284 | 281 | 280 | 275 | 272 |
| Contact angle (°) | 103 | 98 | 100 | 106 | 100 | 102 | 110 | 113 |
| Elongation at break (%) | 32 | 45 | 39 | 40 | 42 | 36 | 13 | 7 |
| Degradable rate (%) | 100 | 98 | 100 | 99 | 100 | 100 | 100 | 100 |
As seen from the above table, what prepared by the present invention is keeping degradable rate based on the PHBV composites that bacteria cellulose is modified
On the basis of, significantly improve the toughness and heat resistance of PHBV composites.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. a kind of PHBV composites being modified based on bacteria cellulose, it is characterised in that：It is described to be modified based on bacteria cellulose
PHBV composites include modified micron order bamboo shoots bacteria cellulose and poly butyric without acid esters PHBV, the modification
Micron order bamboo shoots bacteria cellulose is the micron order bamboo shoots bacteria cellulose of cross-linking silane coupling agent, the micron order bamboo of the modification
Bamboo shoot bacteria cellulose and poly butyric are without passing through n-hydroxysuccinimide crosslinking connection between acid esters PHBV.
2. a kind of PHBV composites being modified based on bacteria cellulose according to claim 1, it is characterised in that prepare
Method comprises the following steps：
(1) by bamboo shoots bacteria cellulose vacuum freeze drying, crushed through micronizer, sieve, obtain micron order bamboo shoots bacterium
Cellulose；
(2) the micron order bamboo shoots bacteria cellulose for preparing step (1) is added in distilled water, high-speed stirred, silane is added dropwise even
Join agent and azodiisobutyronitrile, heating response, obtain modified bamboo shoots bacterial cellulose solution；
(3) poly butyric is added in dichloromethane without acid esters PHBV and stirred, the bamboo of the modification prepared with step (2)
Bamboo shoot bacterial cellulose solution is mixed, and n-hydroxysuccinimide is added dropwise, and stirring, solvent flashing, solidification obtains being based on bacterial fibers
The modified PHBV composites of element.
3. a kind of PHBV composites being modified based on bacteria cellulose according to claim 2, it is characterised in that：It is described
In step (1), the temperature of vacuum freeze drying is -10--20 DEG C, and the time is 24h.
4. a kind of PHBV composites being modified based on bacteria cellulose according to claim 2, it is characterised in that：It is described
In step (1), a diameter of 50-100 μm of micron order bamboo shoots bacteria cellulose.
5. a kind of PHBV composites being modified based on bacteria cellulose according to claim 2, it is characterised in that：It is described
In step (2), the speed of high-speed stirred is 2000-2500r/min, and the time is 30min.
6. a kind of PHBV composites being modified based on bacteria cellulose according to claim 2, it is characterised in that：It is described
In step (2), the mass ratio of micron order bamboo shoots bacteria cellulose, silane coupler and azodiisobutyronitrile is 10:1:0.2-
0.4。
7. a kind of PHBV composites being modified based on bacteria cellulose according to claim 2, it is characterised in that：It is described
In step (2), the temperature of heating response is 70-90 DEG C, and the time is 4-6h.
8. a kind of PHBV composites being modified based on bacteria cellulose according to claim 2, it is characterised in that：It is described
In step (3), bamboo shoots bacteria cellulose and the mass ratio of n-hydroxysuccinimide of the poly butyric without acid esters PHBV, modification
For 20-30:10-15:5-7.
9. a kind of PHBV composites being modified based on bacteria cellulose according to claim 2, it is characterised in that：It is described
In step (3), the temperature of stirring is 40-50 DEG C, and the time of stirring is 48h.
10. a kind of PHBV composites being modified based on bacteria cellulose according to claim 2, it is characterised in that：Institute
State in step (3), the PHBV composites being modified based on bacteria cellulose can be fiber, film-form or bulk material.
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Cited By (3)
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| CN109735593A (en) * | 2018-12-29 | 2019-05-10 | 武汉理工大学 | A simple and rapid method for producing PHB/bacterial cellulose composites |
| CN110128803A (en) * | 2019-04-24 | 2019-08-16 | 广东省医疗器械研究所 | A kind of preparation method of modified BCW/PHBV composite material |
| CN110564120A (en) * | 2019-08-27 | 2019-12-13 | 江苏理工学院 | Cellulose derivative modified poly (beta-hydroxybutyrate valerate) composite material and preparation method thereof |
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| CN110564120A (en) * | 2019-08-27 | 2019-12-13 | 江苏理工学院 | Cellulose derivative modified poly (beta-hydroxybutyrate valerate) composite material and preparation method thereof |
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