CN108410024A - A kind of preparation method of nano-cellulose/oxidized starch biomembrane - Google Patents
A kind of preparation method of nano-cellulose/oxidized starch biomembrane Download PDFInfo
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- CN108410024A CN108410024A CN201810272895.2A CN201810272895A CN108410024A CN 108410024 A CN108410024 A CN 108410024A CN 201810272895 A CN201810272895 A CN 201810272895A CN 108410024 A CN108410024 A CN 108410024A
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- 239000001254 oxidized starch Substances 0.000 title claims abstract description 105
- 235000013808 oxidized starch Nutrition 0.000 title claims abstract description 105
- 238000002360 preparation method Methods 0.000 title claims abstract description 84
- 229920002678 cellulose Polymers 0.000 title claims abstract description 82
- 239000001913 cellulose Substances 0.000 title claims abstract description 72
- 229920002472 Starch Polymers 0.000 claims abstract description 48
- 239000008107 starch Substances 0.000 claims abstract description 48
- 235000019698 starch Nutrition 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- 235000010980 cellulose Nutrition 0.000 claims abstract description 40
- 239000013081 microcrystal Substances 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 230000003647 oxidation Effects 0.000 claims abstract description 11
- 239000004014 plasticizer Substances 0.000 claims abstract description 7
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims abstract description 4
- 238000007872 degassing Methods 0.000 claims abstract description 4
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims abstract description 4
- 239000008108 microcrystalline cellulose Substances 0.000 claims abstract description 4
- 229940016286 microcrystalline cellulose Drugs 0.000 claims abstract description 4
- 238000007766 curtain coating Methods 0.000 claims abstract description 3
- 229920002261 Corn starch Polymers 0.000 claims description 40
- 239000008120 corn starch Substances 0.000 claims description 40
- 229940099112 cornstarch Drugs 0.000 claims description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 22
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 20
- 239000000835 fiber Substances 0.000 claims description 14
- 235000011187 glycerol Nutrition 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 238000004806 packaging method and process Methods 0.000 claims description 7
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 6
- 239000012286 potassium permanganate Substances 0.000 claims description 5
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 4
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 4
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 3
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 2
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 2
- -1 sorbierite Chemical compound 0.000 claims description 2
- 239000000811 xylitol Substances 0.000 claims description 2
- 235000010447 xylitol Nutrition 0.000 claims description 2
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 2
- 229960002675 xylitol Drugs 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 239000002121 nanofiber Substances 0.000 claims 1
- 239000002070 nanowire Substances 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 210000002700 urine Anatomy 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000003643 water by type Substances 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 11
- 239000011521 glass Substances 0.000 description 10
- 239000002904 solvent Substances 0.000 description 10
- 238000001291 vacuum drying Methods 0.000 description 10
- 229920001046 Nanocellulose Polymers 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- 239000000463 material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- BXKDSDJJOVIHMX-UHFFFAOYSA-N edrophonium chloride Chemical compound [Cl-].CC[N+](C)(C)C1=CC=CC(O)=C1 BXKDSDJJOVIHMX-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- ANOBYBYXJXCGBS-UHFFFAOYSA-L stannous fluoride Chemical compound F[Sn]F ANOBYBYXJXCGBS-UHFFFAOYSA-L 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
- B65D65/46—Applications of disintegrable, dissolvable or edible materials
- B65D65/466—Bio- or photodegradable packaging materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/18—Oxidised starch
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2303/04—Starch derivatives
- C08J2303/10—Oxidised starch
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
- C08J2401/04—Oxycellulose; Hydrocellulose
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
Abstract
The present invention relates to a kind of preparation methods of nano-cellulose/oxidized starch biomembrane, belong to the preparing technical field of Biodegradable film.The preparation method includes：S1：a）It is under room temperature, starch is soluble in water；b）Catalyst nano microcrystalline cellulose is added in starch solution, is stirred evenly, water-bath carries out pre-gelatinized processing；c）Starch oxidation agent reaction is added；d）Adjust reaction system pH, terminate after reaction with absolute ethyl alcohol and deionized water repeatedly washed product to get oxidized starch；S2：Oxidized starch in S1 is soluble in water, plasticizer and nano micro crystal cellulose is added to be uniformly mixed, film liquid is obtained into after water-bath, it finally will mixing vibration be de-gassed in ultrasonic cleaner at film liquid, using solution curtain coating mode by the film forming after degassing process be prepared into biomembrane to get.Preparation method prepared by the present invention is simple and convenient to operate, is highly practical, manufacturing cost is low, and the biomembrane biodegradable of preparation, the feature of environmental protection are good.
Description
Technical field
The invention belongs to the preparing technical field of Biodegradable film more particularly to a kind of nano-cellulose/oxidized starch
The preparation method of biomembrane.
Background technology
Starch is the carbohydrate that plant is formed through photosynthesis, as a kind of important stored energy form of plant,
Yield is only second to cellulose, is a kind of pure natural and renewable resource of abundance.Oxidized starch has low viscous compared to ative starch
The advantages that degree, high cohesive force, transparency are good and are not easy gel, carbonyl and carboxy functional group are inserted into starch chain and replaced
The hydrophilic hydroxyl groups of starch make starch hydrophobicity improve.
Cellulose is a kind of natural green high molecular material, is renewable resource.Nano-cellulose can be from multiple fiber
It is usually separated in source, including plant, animal, bacterium and algae etc., nano micro crystal cellulose has high-purity, highly crystalline
The characteristics such as degree, high elastic modulus, high intensity, also with nano particle characteristic, have both biomaterial lightweight, it is degradable,
The characteristics of biocompatibility and recyclability, makes it show huge application prospect in high-performance composite materials.
In recent years, with the attention higher and higher to environmental problem, degradable packing material has become solution petroleum base
The direction of the only way and food packaging development in future of food packaging problem.Therefore, it is necessary to by nano-cellulose and starch
It is combined together the laminated film for preparing degradable, a kind of stability is high, film of environmental protection meets production life instantly to provide
Demand living, and widen the application range of nano-cellulose.
Invention content
For the above-mentioned prior art the problem of, the present invention is intended to provide a kind of nano-cellulose/oxidized starch life
The preparation method of object film, compared with prior art, biomembrane prepared by the present invention is with oxidized starch, nano micro crystal cellulose and sweet
Oil is primary raw material, and step is simple and convenient to operate, is highly practical, manufacturing cost is low, the biomembrane biodegradable of preparation,
The feature of environmental protection is good；Meanwhile the present invention not only regard nano-cellulose as catalyst, but also as hardening agent, the synthesis of biomembrane reduces
The use of chemicals, and starch is influenced small.
An object of the present invention is to provide a kind of preparation method of oxidized starch.
The second object of the present invention is to provide a kind of preparation method of nano-cellulose/oxidized starch biomembrane.
The third object of the present invention is to provide the preparation method of above-mentioned oxidized starch biomembrane, nano-cellulose/oxidation and forms sediment
The application of the preparation method of powder biomembrane and its biomembrane of preparation.
For achieving the above object, the invention discloses following technical proposals：
First, the invention discloses a kind of preparation methods of oxidized starch, specifically, the preparation method includes following step
Suddenly：
A) under room temperature, starch is soluble in water；
B) catalyst nano microcrystalline cellulose is added in starch solution, is stirred evenly, water-bath carries out at pre-gelatinized
Reason；
C) starch oxidation agent reaction is added；
D) adjust reaction system pH, terminate after reaction with absolute ethyl alcohol and deionized water repeatedly washed product to get oxidation
Starch.
In step a), the starch is cornstarch.
In step b), the content of the catalyst is the 0.5%-5 of the starch weight of over dry.
In step b), the fibre length of the nano micro crystal cellulose is 100-800nm.
In step b), the time of the stirring is 8-10h.
In step b), the water-bath refers to：2h is reacted at 75 DEG C first, is then cooled to 50 DEG C.
In step c), the starch oxidation agent includes H2O2、KMnO4Or NaClO.
Preferably, the H2O2Feed postition be：Throughput is 10-15g/ml, time 60min.
In step c), the content of the starch oxidation agent is the 3-5% of the starch weight of over dry.
In step d), the adjusting reaction system pH refers to：Reaction is adjusted with the NaOH of the HCl and 0.1mol/L of 0.1mol/L
The pH to 8-10 of system.
Secondly, the invention discloses a kind of preparation methods of nano-cellulose/oxidized starch biomembrane, including：It will be above-mentioned
Oxidized starch prepared by the preparation method of oxidized starch is soluble in water, and plasticizer is then added and nano micro crystal cellulose mixing is equal
It is even, it is obtained after water-bath uniformly at film liquid, it finally will mixing vibration be de-gassed place in ultrasonic cleaner at film liquid
Reason, using solution curtain coating mode by the film forming after degassing process be prepared into biomembrane to get.
The content of the nano micro crystal cellulose is the 1-10% of the oxidized starch weight of over dry.
The content of the plasticizer is the 20-30% of the oxidized starch weight of over dry.
The plasticizer includes：Glycerine, ethylene glycol, butanediol, sorbierite, xylitol, formamide, caprolactam, urea
Or tristerin etc..
The water-bath refers to：3h is reacted at 70 DEG C.
Finally, the invention discloses above-mentioned nano-cellulose/preparation method of oxidized starch biomembrane and its lifes of preparation
Application of the object film in food packaging.
The method have the characteristics that：(1) present invention is not only using nanocrystalline cellulose as the increasing in biomembrane building-up process
Strong agent, while by using nanocrystalline cellulose as the catalyst for preparing oxidized starch, not only significantly simplifying the oxidation of starch
Step, reduces the use of chemicals, and uses nanocrystalline cellulose very small on the influence of the whiteness of starch as catalyst, has
Help obtain cleaner and beautiful biomembrane.(2) present invention prepares biomembrane with oxidized starch instead of common starch, because
After starch surface hydroxyl is oxidized to carbonyl and carboxyl for oxidant so that starch has better heat resistance and degradability
Can, to increase service life of the biomembrane as packaging bag when and discard after automatic degradation capability.(3) nanocrystalline cellulose
As catalyst, it due to small, can enter inside starch, to increase the gap between starch molecule, be conducive to oxygen
The entrance of agent, and oxidation reaction is made to not only occur on starch molecule surface, and it is happened at the inside of starch molecule；Compared to general
Logical catalyst, when same catalyst additive amount, nanocrystalline cellulose helps oxidation effectiveness to become apparent from；(4) oxidized starch compared to
Ative starch has the advantages that be more soluble in water, stability are good, melt fluidity is preferable, easily form a film, viscosity is low etc., the physics after film forming
Intensity is good.
Compared with prior art, the present invention achieves following advantageous effect：Biomembrane prepared by the present invention with oxidized starch,
Nano micro crystal cellulose (CNC) and glycerine are primary raw material, and step is simple and convenient to operate, is highly practical, manufacturing cost is low, system
Standby biomembrane biodegradable, the feature of environmental protection are good；Meanwhile the present invention not only regard nano-cellulose as catalyst, but also as strong
Agent, the synthesis of biomembrane not only reduce the use of chemicals, and do not influence the whiteness to starch.
Specific implementation mode
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific implementation mode, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or combination thereof.
As described in background, with the attention higher and higher to environmental problem, degradable packing material has become
Solve the problems, such as the direction of the only way and food packaging development in future of oil based food packaging；Therefore, the present invention proposes a kind of
The preparation method of nano-cellulose/oxidized starch biomembrane；In conjunction with specific implementation mode, invention is further explained.
Embodiment 1
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, includes the following steps：
1) preparation of oxidized starch：A) under room temperature, 10g cornstarch is dissolved in 30ml deionized waters；B) by 0.5%
(fibre length of nano micro crystal cellulose is in 100-300nm for the nano micro crystal cellulose of (relative to over dry cornstarch quality)
Between) be added in starch solution, 2h is reacted in 75 DEG C of water-baths after stirring 8h, is then cooled to 50 DEG C；C) it is (opposite to be added 4%
In over dry cornstarch quality) NaClO progress oxidation reactions；Reaction is adjusted with the NaOH of the HCl and 0.1mol/L of 0.1mol/L
The pH to 8 of system, in stirring after 2h by with reaction terminating oxidation reaction, it is anti-with absolute ethyl alcohol and deionized water after reaction terminating
Multiple washed product is to get oxidized starch.
2) preparation of biomembrane：Oxidized starch in 5g steps 1) is dissolved in 100ml deionized waters, it is sweet that 1g is then added
Oil and 0.05g nano micro crystal celluloses are uniformly mixed, and obtain uniformly forming a film at film liquid after reacting 3h in 70 DEG C of water-bath
Liquid mixing vibration 30min in ultrasonic cleaner is de-gassed, and weighs into film liquid with 0.15g/cm2It is cast in smooth
On glass plate, equal solvent volatilize naturally after through vacuum drying (60 DEG C) to constant weight to get.
Embodiment 2
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, includes the following steps：
1) preparation of oxidized starch：A) under room temperature, 10g cornstarch is dissolved in 30ml deionized waters；B) by 1.5%
(fibre length of nano micro crystal cellulose is in 100-300nm for the nano micro crystal cellulose of (relative to over dry cornstarch quality)
Between) be added in starch solution, 2h is reacted in 75 DEG C of water-baths after stirring 8h, is then cooled to 50 DEG C；C) it is (opposite to be added 4%
In over dry cornstarch quality) NaClO progress oxidation reactions；Reaction is adjusted with the NaOH of the HCl and 0.1mol/L of 0.1mol/L
The pH to 8 of system, in stirring after 2h by with reaction terminating oxidation reaction, it is anti-with absolute ethyl alcohol and deionized water after reaction terminating
Multiple washed product is to get oxidized starch.
2) preparation of biomembrane：Oxidized starch in 5g steps 1) is dissolved in 100ml deionized waters, 1.5g is then added
Butanediol and 0.25g nano micro crystal celluloses are uniformly mixed, and are obtained uniformly at film liquid after 3h is reacted in 70 DEG C of water-bath, will
At film liquid, mixing vibration 30min is de-gassed in ultrasonic cleaner, weighs into film liquid with 0.15g/cm2It is cast in light
On sliding glass plate, equal solvent volatilize naturally after through vacuum drying (60 DEG C) to constant weight to get.
Embodiment 3
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, includes the following steps：
1) preparation of oxidized starch：A) under room temperature, 10g cornstarch is dissolved in 30ml deionized waters；B) by 2.0%
(fibre length of nano micro crystal cellulose is in 100-300nm for the nano micro crystal cellulose of (relative to over dry cornstarch quality)
Between) be added in starch solution, 2h is reacted in 75 DEG C of water-baths after stirring 10h, is then cooled to 50 DEG C；C) it is (opposite to be added 5%
In over dry cornstarch quality) NaClO progress oxidation reactions；Reaction is adjusted with the NaOH of the HCl and 0.1mol/L of 0.1mol/L
The pH to 8 of system, in stirring after 2h by with reaction terminating oxidation reaction, it is anti-with absolute ethyl alcohol and deionized water after reaction terminating
Multiple washed product is to get oxidized starch.
2) preparation of biomembrane：Oxidized starch in 5g steps 1) is dissolved in 100ml deionized waters, 1.5g is then added
Glycerine and 0.25g nano micro crystal celluloses are uniformly mixed, and are reacted and are obtained after 3h uniformly into film liquid in 70 DEG C of water-bath, will be at
Film liquid mixing vibration 30min in ultrasonic cleaner is de-gassed, and weighs into film liquid with 0.15g/cm2It is cast in smooth
Glass plate on, equal solvent volatilize naturally after through vacuum drying (60 DEG C) to constant weight to get.
Embodiment 4
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, includes the following steps：
1) preparation of oxidized starch：A) under room temperature, 10g cornstarch is dissolved in 30ml deionized waters；B) by 2.0%
(fibre length of nano micro crystal cellulose is in 300-500nm for the nano micro crystal cellulose of (relative to over dry cornstarch quality)
Between) be added in starch solution, 2h is reacted in 75 DEG C of water-baths after stirring 10h, is then cooled to 50 DEG C；C) it is (opposite to be added 3%
In over dry cornstarch quality) KMnO4Carry out oxidation reaction；Reaction is adjusted with the NaOH of the HCl and 0.1mol/L of 0.1mol/L
The pH to 8 of system, in stirring after 2h by with reaction terminating oxidation reaction, it is anti-with absolute ethyl alcohol and deionized water after reaction terminating
Multiple washed product is to get oxidized starch.
2) preparation of biomembrane：Oxidized starch in 5g steps 1) is dissolved in 100ml deionized waters, 1.5g is then added
Glycerine and 0.15g nano micro crystal celluloses are uniformly mixed, and are reacted and are obtained after 3h uniformly into film liquid in 70 DEG C of water-bath, will be at
Film liquid mixing vibration 30min in ultrasonic cleaner is de-gassed, and weighs into film liquid with 0.15g/cm2It is cast in smooth
Glass plate on, equal solvent volatilize naturally after through vacuum drying (60 DEG C) to constant weight to get.
Embodiment 5
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, includes the following steps：
1) preparation of oxidized starch：A) under room temperature, 10g cornstarch is dissolved in 30ml deionized waters；B) by 3.0%
(fibre length of nano micro crystal cellulose is in 300-500nm for the nano micro crystal cellulose of (relative to over dry cornstarch quality)
Between) be added in starch solution, 2h is reacted in 75 DEG C of water-baths after stirring 10h, is then cooled to 50 DEG C；C) it is (opposite to be added 3%
In over dry cornstarch quality) KMnO4Carry out oxidation reaction；Reaction is adjusted with the NaOH of the HCl and 0.1mol/L of 0.1mol/L
The pH to 8 of system, in stirring after 2h by with reaction terminating oxidation reaction, it is anti-with absolute ethyl alcohol and deionized water after reaction terminating
Multiple washed product is to get oxidized starch.
2) preparation of biomembrane：Oxidized starch in 5g steps 1) is dissolved in 100ml deionized waters, 1.5g is then added
Glycerine and 0.15g nano micro crystal celluloses are uniformly mixed, and are reacted and are obtained after 3h uniformly into film liquid in 70 DEG C of water-bath, will be at
Film liquid mixing vibration 30min in ultrasonic cleaner is de-gassed, and weighs into film liquid with 0.15g/cm2It is cast in smooth
Glass plate on, equal solvent volatilize naturally after through vacuum drying (60 DEG C) to constant weight to get.
Embodiment 6
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, includes the following steps：
1) preparation of oxidized starch：A) under room temperature, 10g cornstarch is dissolved in 30ml deionized waters；B) by 3.0%
(fibre length of nano micro crystal cellulose is in 300-500nm for the nano micro crystal cellulose of (relative to over dry cornstarch quality)
Between) be added in starch solution, 2h is reacted in 75 DEG C of water-baths after stirring 10h, is then cooled to 50 DEG C；C) it is (opposite to be added 5%
In over dry cornstarch quality) KMnO4Carry out oxidation reaction；Reaction is adjusted with the NaOH of the HCl and 0.1mol/L of 0.1mol/L
The pH to 8 of system, in stirring after 2h by with reaction terminating oxidation reaction, it is anti-with absolute ethyl alcohol and deionized water after reaction terminating
Multiple washed product is to get oxidized starch.
2) preparation of biomembrane：Oxidized starch in 5g steps 1) is dissolved in 100ml deionized waters, 1.0g is then added
Glycerine and 0.3g nano micro crystal celluloses are uniformly mixed, and are reacted and are obtained after 3h uniformly into film liquid in 70 DEG C of water-bath, will be at
Film liquid mixing vibration 30min in ultrasonic cleaner is de-gassed, and weighs into film liquid with 0.15g/cm2It is cast in smooth
Glass plate on, equal solvent volatilize naturally after through vacuum drying (60 DEG C) to constant weight to get.
Embodiment 7
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, includes the following steps：
1) preparation of oxidized starch：A) under room temperature, 10g cornstarch is dissolved in 30ml deionized waters；B) by 4.0%
(fibre length of nano micro crystal cellulose is in 300-500nm for the nano micro crystal cellulose of (relative to over dry cornstarch quality)
Between) be added in starch solution, 2h is reacted in 75 DEG C of water-baths after stirring 10h, is then cooled to 50 DEG C；C) being passed through throughput is
The H of 13g/ml2O260min carries out oxidation reaction；The pH of reaction system is adjusted with the NaOH of the HCl and 0.1mol/L of 0.1mol/L
To 8, in stirring after 2h by with reaction terminating oxidation reaction, wash production repeatedly with absolute ethyl alcohol and deionized water after reaction terminating
Object is to get oxidized starch.
2) preparation of biomembrane：Oxidized starch in 5g steps 1) is dissolved in 100ml deionized waters, 1.0g is then added
Glycerine and 0.3g nano micro crystal celluloses are uniformly mixed, and are reacted and are obtained after 3h uniformly into film liquid in 70 DEG C of water-bath, will be at
Film liquid mixing vibration 30min in ultrasonic cleaner is de-gassed, and weighs into film liquid with 0.15g/cm2It is cast in smooth
Glass plate on, equal solvent volatilize naturally after through vacuum drying (60 DEG C) to constant weight to get.
Embodiment 8
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, includes the following steps：
1) preparation of oxidized starch：A) under room temperature, 10g cornstarch is dissolved in 30ml deionized waters；B) by 4.0%
(fibre length of nano micro crystal cellulose is in 300-500nm for the nano micro crystal cellulose of (relative to over dry cornstarch quality)
Between) be added in starch solution, 2h is reacted in 75 DEG C of water-baths after stirring 10h, is then cooled to 50 DEG C；C) being passed through throughput is
The H of 10g/ml2O260min carries out oxidation reaction；The pH of reaction system is adjusted with the NaOH of the HCl and 0.1mol/L of 0.1mol/L
To 8, in stirring after 2h by with reaction terminating oxidation reaction, wash production repeatedly with absolute ethyl alcohol and deionized water after reaction terminating
Object is to get oxidized starch.
2) preparation of biomembrane：Oxidized starch in 5g steps 1) is dissolved in 100ml deionized waters, 1.0g is then added
Glycerine and 0.4g nano micro crystal celluloses are uniformly mixed, and are reacted and are obtained after 3h uniformly into film liquid in 70 DEG C of water-bath, will be at
Film liquid mixing vibration 30min in ultrasonic cleaner is de-gassed, and weighs into film liquid with 0.15g/cm2It is cast in smooth
Glass plate on, equal solvent volatilize naturally after through vacuum drying (60 DEG C) to constant weight to get.
Embodiment 9
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, includes the following steps：
1) preparation of oxidized starch：A) under room temperature, 10g cornstarch is dissolved in 30ml deionized waters；B) by 4.0%
(fibre length of nano micro crystal cellulose is in 500-800nm for the nano micro crystal cellulose of (relative to over dry cornstarch quality)
Between) be added in starch solution, 2h is reacted in 75 DEG C of water-baths after stirring 10h, is then cooled to 50 DEG C；C) being passed through throughput is
15g.ml-1H2O260min carries out oxidation reaction；Reaction system is adjusted with the NaOH of the HCl and 0.1mol/L of 0.1mol/L
PH to 8, in stirring after 2h by with reaction terminating oxidation reaction, washed repeatedly with absolute ethyl alcohol and deionized water after reaction terminating
Product is to get oxidized starch.
2) preparation of biomembrane：Oxidized starch in 5g steps 1) is dissolved in 100ml deionized waters, 1.0g is then added
Glycerine and 0.5g nano micro crystal celluloses are uniformly mixed, and are reacted and are obtained after 3h uniformly into film liquid in 70 DEG C of water-bath, will be at
Film liquid mixing vibration 30min in ultrasonic cleaner is de-gassed, and weighs into film liquid with 0.15g/cm2It is cast in smooth
Glass plate on, equal solvent volatilize naturally after through vacuum drying (60 DEG C) to constant weight to get.
Embodiment 10
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, includes the following steps：
1) preparation of oxidized starch：A) under room temperature, 10g cornstarch is dissolved in 30ml deionized waters；B) by 5.0%
(fibre length of nano micro crystal cellulose is in 500-800nm for the nano micro crystal cellulose of (relative to over dry cornstarch quality)
Between) be added in starch solution, 2h is reacted in 75 DEG C of water-baths after stirring 10h, is then cooled to 50 DEG C；C) it is (opposite to be added 4%
In over dry cornstarch quality) NaClO progress oxidation reactions；Reaction is adjusted with the NaOH of the HCl and 0.1mol/L of 0.1mol/L
The pH to 8 of system, in stirring after 2h by with reaction terminating oxidation reaction, it is anti-with absolute ethyl alcohol and deionized water after reaction terminating
Multiple washed product is to get oxidized starch.
2) preparation of biomembrane：Oxidized starch in 5g steps 1) is dissolved in 100ml deionized waters, 1.5g is then added
Ethylene glycol and 0.3g nano micro crystal celluloses are uniformly mixed, and are obtained uniformly at film liquid after 3h is reacted in 70 DEG C of water-bath, will
At film liquid, mixing vibration 30min is de-gassed in ultrasonic cleaner, weighs into film liquid with 0.15g/cm2It is cast in light
On sliding glass plate, equal solvent volatilize naturally after through vacuum drying (60 DEG C) to constant weight to get.
Comparative example 1
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, with embodiment 1, difference lies in do not include step
1), in the preparation of step 2) biomembrane, oxidized starch is replaced with inoxidized cornstarch.
Comparative example 2
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, with embodiment 2, difference lies in do not include step
1), in the preparation of step 2) biomembrane, oxidized starch is replaced with inoxidized cornstarch.
Comparative example 3
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, with embodiment 3, difference lies in do not include step
1), in the preparation of step 2) biomembrane, oxidized starch is replaced with inoxidized cornstarch.
Comparative example 4
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, with embodiment 4, difference lies in do not include step
1), in the preparation of step 2) biomembrane, oxidized starch is replaced with inoxidized cornstarch.
Comparative example 5
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, with embodiment 5, difference lies in do not include step
1), in the preparation of step 2) biomembrane, oxidized starch is replaced with inoxidized cornstarch.
Comparative example 6
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, with embodiment 6, difference lies in do not include step
1), in the preparation of step 2) biomembrane, oxidized starch is replaced with inoxidized cornstarch.
Comparative example 7
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, with embodiment 7, difference lies in do not include step
1), in the preparation of step 2) biomembrane, oxidized starch is replaced with inoxidized cornstarch.
Comparative example 8
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, with embodiment 8, difference lies in do not include step
1), in the preparation of step 2) biomembrane, oxidized starch is replaced with inoxidized cornstarch.
Comparative example 9
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, with embodiment 9, difference lies in do not include step
1), in the preparation of step 2) biomembrane, oxidized starch is replaced with inoxidized cornstarch.
Comparative example 10
A kind of preparation method of nano-cellulose/oxidized starch biomembrane, with embodiment 10, difference lies in do not include step
It is rapid 1), in the preparation of step 2) biomembrane, with inoxidized cornstarch replace oxidized starch.
Performance test：
Using tensile strength and break elongation rate as performance testing index, measure nano-cellulose prepared by embodiment 1-10/
The mechanical property of oxidized starch biomembrane.Test method is：Above-mentioned biomembrane will be first cut into the strip of 8cm × 1.5cm, dry
48h is balanced in dry device, is measured by tensilon, test result is as shown in table 1.
The mechanical property of nano-cellulose/oxidized starch biomembrane prepared by 1 embodiment 1-10 of table
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Tensile strength/% | 7.0 | 10.7 | 11.3 | 8.1 | 8.67 | 12.3 | 12.99 | 12.25 | 11.02 | 14.68 |
| Elongation after fracture/MPa | 55.8 | 40.8 | 36.9 | 49.8 | 45.6 | 29.8 | 28.7 | 29.2 | 31.4 | 24.7 |
The mechanical property of nano-cellulose/oxidized starch biomembrane prepared by 2 comparative example 1-10 of table
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Tensile strength/% | 4.31 | 3.97 | 4.22 | 4.89 | 5.08 | 3.55 | 4.67 | 5.32 | 5.15 | 3.74 |
| Elongation after fracture/MPa | 22.3 | 21.5 | 20.7 | 23.8 | 19.6 | 18.8 | 21.9 | 22.7 | 17.3 | 19.1 |
As can be seen from Table 1 and Table 2, it after method using the present invention handles cornstarch, intensity and has no progeny
Elongation has obtained significantly being promoted.
The foregoing is merely the preferred embodiments of the application, are not intended to limit this application, for those skilled in the art
For member, the application can have various modifications and variations.Any modification made by within the spirit and principles of this application,
Equivalent replacement, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. a kind of preparation method of oxidized starch, which is characterized in that the preparation method comprises the following steps：
A) under room temperature, starch is soluble in water；
B) catalyst nano microcrystalline cellulose is added in starch solution, is stirred evenly, water-bath carries out pre-gelatinized processing；
C) starch oxidation agent reaction is added；
D) adjust reaction system pH, terminate after reaction with absolute ethyl alcohol and deionized water repeatedly washed product to get oxidized starch.
2. the preparation method of oxidized starch as described in claim 1, which is characterized in that the content of the catalyst is over dry
The 0.5%-5% of starch weight；Preferably, the starch is cornstarch.
3. the preparation method of oxidized starch as described in claim 1, which is characterized in that the fiber of the nano micro crystal cellulose
Length is 100-800nm；Preferably, the time of the stirring is 8-10h.
4. the preparation method of oxidized starch as described in claim 1, which is characterized in that the water-bath refers to：First 75
DEG C reaction 2h, be then cooled to 50 DEG C.
5. the preparation method of oxidized starch according to any one of claims 1-4, which is characterized in that the starch oxidation agent packet
Include H2O2、KMnO4Or NaClO；Preferably, the H2O2Feed postition be：Throughput is 10-15g/ml, time 60min；It is excellent
Choosing, the content of the starch oxidation agent is the 3-5% of the starch weight of over dry.
6. the preparation method of oxidized starch as claimed in claim 5, which is characterized in that the adjusting reaction system pH refers to：With
The NaOH of the HCl and 0.1mol/L of 0.1mol/L adjust the pH to 8-10 of reaction system.
7. a kind of preparation method of nano-cellulose/oxidized starch biomembrane, which is characterized in that will be any in claim 1-6
Oxidized starch prepared by the preparation method of the oxidized starch described in is soluble in water, and plasticizer and nano microcrystalline fiber is then added
Element be uniformly mixed, obtained after water-bath uniformly at film liquid, finally will at film liquid in ultrasonic cleaner mixing vibration into
Row degassing process, using solution curtain coating mode by the film forming after degassing process be prepared into biomembrane to get.
8. the preparation method of nano-cellulose as claimed in claim 5/oxidized starch biomembrane, which is characterized in that described to receive
The content of rice microcrystalline cellulose is the 1-10% of the oxidized starch weight of over dry；
Preferably, the content of the plasticizer is the 20-30% of the oxidized starch weight of over dry；
Preferably, the plasticizer includes：Glycerine, ethylene glycol, butanediol, sorbierite, xylitol, formamide, caprolactam, urine
Element or tristerin；
Preferably, the water-bath refers to：3h is reacted at 70 DEG C.
9. nanofiber prepared by the preparation method of nano-cellulose as claimed in claim 7 or 8/oxidized starch biomembrane
Element/oxidized starch biomembrane.
10. the preparation method of oxidized starch as claimed in any one of claims 1 to 6, Nanowire as claimed in claim 7 or 8
Tie up the preparation method of element/oxidized starch biomembrane, nano-cellulose as claimed in claim 9/oxidized starch biomembrane is being eaten
Application in product packaging.
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