CN102775647B - Preparation method of hemicellulose based edible film - Google Patents
Preparation method of hemicellulose based edible film Download PDFInfo
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- CN102775647B CN102775647B CN201210266588.6A CN201210266588A CN102775647B CN 102775647 B CN102775647 B CN 102775647B CN 201210266588 A CN201210266588 A CN 201210266588A CN 102775647 B CN102775647 B CN 102775647B
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- 229920002488 Hemicellulose Polymers 0.000 title claims abstract description 137
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 19
- 235000013305 food Nutrition 0.000 claims abstract description 14
- 239000000413 hydrolysate Substances 0.000 claims abstract description 13
- 239000000706 filtrate Substances 0.000 claims description 67
- 238000003756 stirring Methods 0.000 claims description 49
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 25
- 229910052799 carbon Inorganic materials 0.000 claims description 20
- IPCSVZSSVZVIGE-UHFFFAOYSA-N palmitic acid group Chemical group C(CCCCCCCCCCCCCCC)(=O)O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 230000004048 modification Effects 0.000 claims description 18
- 238000012986 modification Methods 0.000 claims description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 17
- 150000002500 ions Chemical class 0.000 claims description 17
- 229920001661 Chitosan Polymers 0.000 claims description 16
- 108010009736 Protein Hydrolysates Proteins 0.000 claims description 15
- 229920002472 Starch Polymers 0.000 claims description 14
- 239000008107 starch Substances 0.000 claims description 14
- 235000019698 starch Nutrition 0.000 claims description 14
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical group CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims description 12
- 239000004902 Softening Agent Substances 0.000 claims description 12
- 235000021314 Palmitic acid Nutrition 0.000 claims description 10
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 10
- 229940098695 palmitic acid Drugs 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 8
- 241000219000 Populus Species 0.000 claims description 6
- 239000003995 emulsifying agent Substances 0.000 claims description 6
- 229940075507 glyceryl monostearate Drugs 0.000 claims description 6
- 239000001788 mono and diglycerides of fatty acids Substances 0.000 claims description 6
- 230000008719 thickening Effects 0.000 claims description 6
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- -1 polyoxyethylene Polymers 0.000 claims description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- MEIRRNXMZYDVDW-MQQKCMAXSA-N (2E,4E)-2,4-hexadien-1-ol Chemical compound C\C=C\C=C\CO MEIRRNXMZYDVDW-MQQKCMAXSA-N 0.000 claims description 4
- 241000609240 Ambelania acida Species 0.000 claims description 4
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 4
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000010905 bagasse Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 235000002949 phytic acid Nutrition 0.000 claims description 4
- 229940068041 phytic acid Drugs 0.000 claims description 4
- 239000000467 phytic acid Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- 239000001913 cellulose Substances 0.000 claims description 3
- 229920002678 cellulose Polymers 0.000 claims description 3
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 claims description 3
- 239000004334 sorbic acid Substances 0.000 claims description 3
- 229940075582 sorbic acid Drugs 0.000 claims description 3
- 235000010199 sorbic acid Nutrition 0.000 claims description 3
- 229960005196 titanium dioxide Drugs 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 229920001285 xanthan gum Polymers 0.000 claims description 3
- 239000000230 xanthan gum Substances 0.000 claims description 3
- 229940082509 xanthan gum Drugs 0.000 claims description 3
- 235000010493 xanthan gum Nutrition 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 235000013399 edible fruits Nutrition 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 9
- 238000004806 packaging method and process Methods 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 239000012785 packaging film Substances 0.000 abstract description 2
- 229920006280 packaging film Polymers 0.000 abstract description 2
- 239000003242 anti bacterial agent Substances 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 235000008429 bread Nutrition 0.000 abstract 1
- 235000012970 cakes Nutrition 0.000 abstract 1
- 238000007872 degassing Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000004014 plasticizer Substances 0.000 abstract 1
- 241000219095 Vitis Species 0.000 description 12
- 235000009754 Vitis X bourquina Nutrition 0.000 description 12
- 235000012333 Vitis X labruscana Nutrition 0.000 description 12
- 235000014787 Vitis vinifera Nutrition 0.000 description 12
- 235000007688 Lycopersicon esculentum Nutrition 0.000 description 8
- 240000003768 Solanum lycopersicum Species 0.000 description 8
- 239000002585 base Substances 0.000 description 8
- 239000008187 granular material Substances 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 238000007605 air drying Methods 0.000 description 7
- 235000001014 amino acid Nutrition 0.000 description 7
- 150000001413 amino acids Chemical class 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 230000000873 masking effect Effects 0.000 description 7
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 7
- 239000004926 polymethyl methacrylate Substances 0.000 description 7
- 238000002834 transmittance Methods 0.000 description 7
- 235000018102 proteins Nutrition 0.000 description 6
- 108090000623 proteins and genes Proteins 0.000 description 6
- 102000004169 proteins and genes Human genes 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- LTVDFSLWFKLJDQ-UHFFFAOYSA-N α-tocopherolquinone Chemical compound CC(C)CCCC(C)CCCC(C)CCCC(C)(O)CCC1=C(C)C(=O)C(C)=C(C)C1=O LTVDFSLWFKLJDQ-UHFFFAOYSA-N 0.000 description 6
- 230000004888 barrier function Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 244000061508 Eriobotrya japonica Species 0.000 description 3
- 235000009008 Eriobotrya japonica Nutrition 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 238000012869 ethanol precipitation Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 239000005022 packaging material Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 235000008935 nutritious Nutrition 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 108010073771 Soybean Proteins Proteins 0.000 description 1
- 239000012754 barrier agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 235000021374 legumes Nutrition 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 235000015067 sauces Nutrition 0.000 description 1
- 235000019710 soybean protein Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
-
- 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
Landscapes
- Jellies, Jams, And Syrups (AREA)
- General Preparation And Processing Of Foods (AREA)
Abstract
The invention discloses a preparation method of a hemicellulose based edible film. The method includes taking hemicellulose or modified hemicellulose as a base material, adding additives such as an antibacterial agent, a plasticizer and a separator into hydrolysate of the base material, dissolving, mixing evenly, homogenizing, degassing, preparing a film, drying finally, and preparing the edible food packaging film with a certain intensity and water-solubility. The preparation method is simple, easy to industrialize, good in film formation and high in intensity; and the formed film has good separating performance and water resistance, and can satisfy packaging requirements of bread, cakes, fruit and other food.
Description
Technical field
The invention belongs to plant chemical industry and packaging material for food field, particularly a kind of preparation method of hemicellulose group edible film.
Background technology
In food product pack field, compare other stationery and plastic wrapping, edible packing membrane has unrivaled advantage, and it has the characteristics such as edible, health, nutrition, environmental protection, convenience.Traditional technique and the limitation of formula, make the having some limitations property of edible film of preparation, such as: film preparation raw material consumption is large, operational path is comparatively complicated, makes industrialization be difficult to utilization and extention; Prepared film bad mechanical strength, barrier property is low, heat sealability is bad, the not high reason of transparency, causes the application space of edible film and scope to diminish, can not scale operation utilization.
At present to the base material major part of edible film round expansion such as starch, soybean protein, lipid materials, but after starch film forming, easily there is intensity difference and protein denaturation in crisp, large legume protein film forming easily, lipid material again polarity is very weak and not soluble in water, be difficult to the shortcomings such as film forming, make above film suitability not strong.The present invention adopts nutritious and has the natural hemicellulose polysaccharide of nourishing function as the base material of edible film, and on the basis of traditional filming technology, the not high characteristic of intensity after strong and film forming for polyose substrate hydrophilic, hemicellulose is carried out to modification, and improve with regard to the film preparation technique after modification, greatly improve hemicellulose film strength and hydrophobic nature, further met the needs of production and life food fresh keeping and packing.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of hemicellulose group edible film, the method has overcome the deficiencies such as existing edible film kind is single, intensity is low, poor transparency, elongation is little, barrier property is poor, adopt hemicellulose/modification hemicellulose as edible film base-material, be aided with again other auxiliary agent, prepare the hemicellulose group edible film that has met edible food package requirement, half-and-half cellulosic diversification and industrial applications are significant.
Technical solution of the present invention is as follows:
(1) at hemicellulose or in the modification hemicellulose of sig water predissolve 5～40min, add water, stirring and dissolving under 50～70 ℃, 300～500rpm, treatment time 30～40min, make hemicellulose hydrolysate, wherein during the predissolve of modification hemicellulose, the addition of alkali is 0.04～0.08% of modification hemicellulose quality, and the mass ratio of water and hemicellulose or modification hemicellulose is for being 50:1～100:1;
(2) in cellulosic hydrolysate, add the granulated active carbon of cellulosic hydrolysate quality 5～20%, activated carbon granule is big or small for particle diameter is 1.5～3mm, after reaction 20～30min, filters, and collects filtrate;
(3) in filtrate, add the chitosan of filtrate quality 0.3～0.6% and the acetic acid solution of filtrate quality 0.1～0.2%, under 300～800rpm, stir;
(4) fluidizer that adds filtrate quality 0.4～1% in the solution making in step (3), stirs, and then regulating pH value is 2～3, adopts ordinary method degassed;
(5) in the solution making in step (4), add emulsifying agent and hydrophober, be heated to 60 ℃～80 ℃, after stirring, at 60～80 ℃, be incubated 5～10min, wherein the addition of emulsifying agent and hydrophober is 0.3～0.6% of filtrate quality;
(6) with step (5) solution film-forming, after moulding, at 80 ℃, be dried 4～8 hours, obtain hemicellulose group edible film.
In the present invention, hemicellulose molecule amount is 10000～50000, and modified-cellulose is a kind of in acetylated hemicellulose, positively charged ion hemicellulose.
In the present invention, sig water is that mass percent concentration is 0.2～0.8% NaOH solution or KOH solution.
In the present invention, when Mierocrystalline cellulose or predissolve modification hydrolysis of hemicellulose, under ultrasound condition or in homogeneous instrument, carry out.
In the present invention, softening agent is that softening agent is a kind of in glycerine, sorbyl alcohol, ethylene glycol, polyoxyethylene glycol, and its addition is 0.4～1% of filtrate quality.
In the present invention, emulsifying agent is glyceryl monostearate or starch, and addition is 0.3～0.6% of filtrate quality.
In the present invention, hydrophober is Palmiticacid or stearic acid, and its addition is 0.3～0.6% of filtrate quality.
A kind of in adding thickening material Xylo-Mucine, polynite, xanthan gum in the present invention in the preparation of hemicellulose group edible film, addition is 0.2～1.0% of filtrate quality.
A kind of in adding food antiseptic-germicide nano titanium oxide, phytic acid, Sorbic Acid in the present invention in the preparation of hemicellulose group edible film, addition is the 0.01-0.1% of filtrate quality.Chitosan not only has anti-microbial effect or a kind of good fruit glaze agent, the anti-microbial property that chitosan and nano titanium oxide, phytic acid, Sorbic Acid can reinforcing membrane.
Described in the present invention, adopting modification hemicellulose is raw material while preparing film, after film is dry, take film off, by (water temperature is 10～30 ℃) after film cooling bath 5～20min, then dries at 40～60 ℃, can obtain high-clarity hemicellulose film.
In the present invention, the preparation of positively charged ion hemicellulose adopts ordinary method, by every gram of hemicellulose (adopting alcohol deposition method to obtain hemicellulose after the extracting of raw material alkali), adding 30-50ml ethanolic soln mixes hemicellulose and ethanolic soln, ethanolic soln mass percent concentration is 40%～60%, in water bath with thermostatic control, stir and be warming up to 55 ℃～65 ℃, drip sodium hydroxide solution (mass percent concentration is 6%), sodium hydroxide addition is 5～7% of hemicellulose quality, and stir-activating 30min, then the cationic etherifying agent 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride (CHPTMAC) that adds hemicellulose quality 25%～35%, be warming up to temperature of reaction 45-65 ℃, stirring reaction 2～5 hours, after reaction finishes, with acetic acid neutralization, ethanol precipitation, filtration, washing, at 40～50 ℃, vacuum-drying is 24 hours, can obtain positively charged ion hemicellulose.
The present invention adopts hemicellulose or modification hemicellulose as base material, and in the hydrolyzed solution of base material, add the additives such as antiseptic-germicide, softening agent, barrier agent, be prepared into a kind of edible food packaging film, in existing food as internal packing (as: inner packaging material of the food such as sauce packet, coffee, candied haws on a stick) and outer packaging (as: housing material of the food such as fruit, cake), this film is with its good barrier property and good mechanical property, can meet the requirement of internal packing and outer packaging in food.
The more original edible film of the present invention is compared, and adopts hemicellulose or modification hemicellulose as the base-material of preparing of film, have nutritious, preparation is simple, only with a small amount of base-material and auxiliary agent, can meet the requirements such as intensity and transparency; Technique and formula are simple, and base-material and auxiliary dosage are few, are convenient to suitability for industrialized production and promote; Compare as glutinous rice film with like product on market in addition, intensity, barrier property, mechanical property and transparency are higher, are more suitable for as packaging material for food.
Embodiment
Below by embodiment, the present invention is described in further detail, but protection domain of the present invention is not limited to described content, in embodiment, method if no special instructions all adopts ordinary method.
Embodiment 1: the preparation method of hemicellulose group edible film, and concrete operations are as follows:
(1) first in the container with heating and stirring device, add hemicellulose (molecular weight is 20000), then add therein water, stirring and dissolving under 70 ℃, 300rpm then, treatment time 40min, make hemicellulose hydrolysate, the mass ratio 50:1 of water and hemicellulose;
(2) in hemicellulose hydrolysate, add the granulated active carbon of hemicellulose hydrolysate quality 15%, activated carbon granule particle diameter is being between 1.5～3mm, after reaction 20min, filters, and collects filtrate;
(3) in filtrate, add the chitosan of filtrate quality 0.5% and the acetic acid solution of filtrate quality 0.1%, under 300rpm, stir and chitosan is dissolved completely;
(4) the softening agent glycerine that adds filtrate quality 0.5% in the solution making in step (3), stirs, and then regulator solution pH value is 2.5, degassed 5min;
(5) in the solution making in step (4), add glyceryl monostearate and Palmiticacid, be heated to 60 ℃, stir at latter 80 ℃ and be incubated 5min, wherein the addition of glyceryl monostearate and Palmiticacid is 0.3% of filtrate quality;
(6) step (5) solution is poured on to masking on poly (methyl methacrylate) plate, after moulding, forced air drying at 80 ℃ 4 hours, obtains hemicellulose group edible film.
Gained half fiber base edible film tensile strength can reach that 30MPa, elongation reach 20%, transmittance reaches 60%, water vapour transmission coefficient can reach 0.30g.mm/m
2.h.KPa.With this edible film liquid, tomato is carried out to coating-film fresh-keeping experiment, the V-c content in tomato has reduced by 28%, and aminoacids content increases by 12%, and total reducing sugar reduces by 23%, compare with the tomato of not filming, this organize fresh-keeping tomato shelf life extension more than 3-4 days.
Embodiment 2: the preparation method of hemicellulose group edible film, and concrete operations are as follows:
(1) first in the container with heating and stirring device, add hemicellulose (molecular weight is 15000), and add therein water, stirring and dissolving under 70 ℃, 500rpm then, treatment time 30min, make hemicellulose hydrolysate, the mass ratio of water and hemicellulose is 50:1;
(2) in hemicellulose hydrolysate, add the granulated active carbon of hemicellulose hydrolysate quality 10%, activated carbon granule particle diameter is being between 1.5～3mm, after reaction 30min, filters, and collects filtrate;
(3) in filtrate, add the chitosan of filtrate quality 0.3% and the acetic acid solution of filtrate quality 0.1%, under 500rpm, stir and chitosan is dissolved completely;
(4) the softening agent sorbyl alcohol that adds filtrate quality 0.5% in the solution making in step (3), stirs, and then regulator solution pH value is 3, degassed;
(5) in the solution making in step (4), add starch and stearic acid, be heated to 70 ℃, stir at latter 70 ℃ and be incubated 7min, wherein starch and stearic addition are 0.5% of filtrate quality;
(6) step (5) solution is poured on to masking on poly (methyl methacrylate) plate, after moulding, forced air drying at 80 ℃ 4 hours, obtains hemicellulose group edible film.
Gained half fiber base edible film tensile strength can reach that 28MPa, elongation reach 20%, transmittance reaches 70%, water vapour transmission coefficient can reach 0.35g.mm/m2.h.KPa.With this edible film liquid, tomato is carried out to coating-film fresh-keeping experiment, the V-c content in tomato has reduced by 24%, and aminoacids content increases by 19%, and total reducing sugar reduces by 20%, compare with the tomato of not filming, this organize fresh-keeping tomato shelf life extension more than 4-5 days.
Embodiment 3: the preparation method of hemicellulose group edible film, and concrete operations are as follows:
(1) first in the container with heating and stirring device, add acetylated hemicellulose, 0.08% the NaOH solution (mass percent concentration is 0.2%) that adds acetylated hemicellulose quality, predissolve 10min, add therein again water, the mass ratio of water and acetylated hemicellulose is 80:1, then, at 60 ℃, 400rpm, the lower ultrasonic 20min of ultrasound condition (ultrasonic frequency 40kHz, power 120W), stirs afterwards, treatment time 10min, makes hemicellulose hydrolysate;
(2) in hemicellulose hydrolysate, add the granulated active carbon of hemicellulose hydrolysate quality 5%, activated carbon granule particle diameter is being between 1.5～3mm, after reaction 25min, filters, and collects filtrate;
(3) in filtrate, add the chitosan of filtrate quality 0.4% and the acetic acid solution of filtrate quality 0.15%, under 600rpm, stir and chitosan is dissolved completely;
(4) the softening agent ethylene glycol that adds filtrate quality 1% in the solution making in step (3), stirs, and then regulator solution pH value is 3, degassed;
(5) in the solution making in step (4), add starch and Palmiticacid, be heated to 65 ℃, stir at latter 70 ℃ and be incubated 6min, wherein the addition of starch and Palmiticacid is 0.4% of filtrate quality;
(6) step (5) solution is poured on to masking on poly (methyl methacrylate) plate, after moulding forced air drying at 80 ℃ 6 hours;
(7) dried film is put into cooling bath again and processed after 10min, dry at 60 ℃, can obtain high-clarity hemicellulose film, wherein cold water temperature is 10 ℃.
The edible film tensile strength that employing is prepared through the modification hemicellulose of prehydrolysis can reach that 38MPa, elongation reach 30%, transmittance reaches 85%, water vapour transmission coefficient can reach 0.18g.mm/m
2.h.KPa.With this edible film liquid, grape is carried out to coating-film fresh-keeping experiment, the V-c content in fruit has reduced by 22%, and aminoacids content increases by 16%, total reducing sugar reduces by 22%, protein reduces by 27%, compare with the grape of not filming, this organize fresh-keeping grape shelf life extension more than 3-4 days.
Embodiment 4: the preparation method of hemicellulose group edible film, and concrete operations are as follows:
(1) first in the container with heating and stirring device, add poplar positively charged ion hemicellulose, 0.04% the NaOH solution (mass percent concentration is 0.8%) that adds positively charged ion hemicellulose quality, predissolve 5min, add therein again water, the mass ratio of water and positively charged ion hemicellulose is 60:1, then 65 ℃, 350rpm stirring, treatment time 35min, makes hemicellulose hydrolysate;
Wherein the preparation method of poplar positively charged ion hemicellulose is as follows:
First by poplar with adopting alcohol deposition method to make hemicellulose after alkali extracting, in every gram of hemicellulose, adding the ratio of 50ml ethanolic soln mixes hemicellulose and ethanolic soln, ethanolic soln mass percent concentration is 40%, in water bath with thermostatic control, stir and be warming up to 60 ℃, drip sodium hydroxide solution (mass percent concentration is 6%), sodium hydroxide addition is 5% of hemicellulose quality, and stir-activating 30min, then the cationic etherifying agent 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride (CHPTMAC) that adds hemicellulose quality 30%, be warming up to 65 ℃ of temperature of reaction, stirring reaction 2 hours, after reaction finishes, with acetic acid neutralization, ethanol precipitation, filtration, washing, at 45 ℃, vacuum-drying is 24 hours, can obtain poplar positively charged ion hemicellulose,
(2) in hemicellulose hydrolysate, add the granulated active carbon of hemicellulose hydrolysate quality 20%, activated carbon granule particle diameter is being between 1.5～3mm, after reaction 20min, filters, and collects filtrate;
(3) in filtrate, add the chitosan of filtrate quality 0.6% and the acetic acid solution of filtrate quality 0.2%, under 800rpm, stir and chitosan is dissolved completely;
(4) in the solution making in step (3), add the softening agent polyoxyethylene glycol of filtrate quality 0.4% and the thickening material Xylo-Mucine of filtrate quality 0.5%, stir, then regulator solution pH value is 3, degassed;
(5) in the solution making in step (4), add glyceryl monostearate and Palmiticacid, be heated to 80 ℃, stir at latter 60 ℃ and be incubated 10min, wherein the addition of starch and Palmiticacid is 0.6% of filtrate quality;
(6) step (5) solution is poured on to masking on poly (methyl methacrylate) plate, after moulding forced air drying at 80 ℃ 8 hours;
(7) dried film is put into cooling bath again and processed after 5min, dry at 50 ℃, can obtain high-clarity hemicellulose film, wherein cold water temperature is 20 ℃.
The edible film tensile strength that adopts positively charged ion hemicellulose to prepare can reach that 33MPa, elongation reach 28%, transmittance reaches 86%, water vapour transmission coefficient can reach 0.16g.mm/m
2.h.KPa.With this edible film liquid, grape is carried out to coating-film fresh-keeping experiment, the V-c content in fruit has reduced by 27%, and aminoacids content increases by 18%, total reducing sugar reduces by 20%, protein reduces by 36%, compare with the grape of not filming, this organize fresh-keeping grape shelf life extension more than 3-4 days.
Embodiment 5: the preparation method of hemicellulose group edible film, and concrete operations are as follows:
(1) first in the container with heating and stirring device, add hemicellulose (molecular weight is 25000), and add therein water, stirring and dissolving under 50 ℃, 350rpm then, treatment time 35min, make hemicellulose hydrolysate, the mass ratio of water and hemicellulose is 100:1;
(2) in hemicellulose hydrolysate, add the granulated active carbon of hemicellulose hydrolysate quality 12%, activated carbon granule particle diameter is being between 1.5～3mm, after reaction 20min, filters, and collects filtrate;
(3) in filtrate, add the chitosan of filtrate quality 0.3%, the nano titanium oxide of the acetic acid solution of filtrate quality 0.1%, filtrate quality 0.05% stirs under 500rpm;
(4) in the solution making in step (3), add the softening agent sorbyl alcohol of filtrate quality 0.5% and the thickening material polynite of filtrate quality 0.2%, stir, then regulator solution pH value is 2, degassed;
(5) in the solution making in step (4), add starch and stearic acid, be heated to 75 ℃, stir at latter 65 ℃ and be incubated 8min, wherein starch and stearic addition are 0.4% of filtrate quality;
(6) step (5) solution is poured on to masking on poly (methyl methacrylate) plate, after moulding, forced air drying at 80 ℃ 5 hours, obtains hemicellulose group edible film.
Gained half fiber base edible film tensile strength can reach that 32MPa, elongation reach 25%, transmittance reaches 75%, water vapour transmission coefficient can reach 0.25g.mm/m2.h.KPa, with this edible film liquid, loquat is carried out to coating-film fresh-keeping experiment, V-c content in fruit has reduced by 52%, aminoacids content increases by 17%, compare with the loquat of not filming, this organize fresh-keeping loquat shelf life extension more than 7 days, and there is no TiO
2group relatively, adds TiO
2favourable to fruit freshness preserving afterwards.
Embodiment 6: the preparation method of hemicellulose group edible film, and concrete operations are as follows:
(1) first in the container with heating and stirring device, add hemicellulose (molecular weight is 30000), and add therein water, stirring and dissolving under 55 ℃, 450rpm then, treatment time 30min, make hemicellulose hydrolysate, the mass ratio of water and hemicellulose is 70:1;
(2) in hemicellulose hydrolysate, add the granulated active carbon of hemicellulose hydrolysate quality 12%, activated carbon granule particle diameter is being between 1.5～3mm, after reaction 25min, filters, and collects filtrate;
(3) in filtrate, add the chitosan of filtrate quality 0.4%, the phytic acid of the acetic acid solution of filtrate quality 0.2%, filtrate quality 0.01% stirs under 500rpm;
(4) in the solution making in step (3), add the softening agent glycerine of filtrate quality 0.5% and the thickening material xanthan gum of filtrate quality 0.2%, stir, then regulator solution pH value is 2, degassed;
(5) in the solution making in step (4), add starch and stearic acid, be heated to 80 ℃, stir at latter 60 ℃ and be incubated 10min, wherein starch and stearic addition are 0.5% of filtrate quality;
(6) step (5) solution is poured on to masking on poly (methyl methacrylate) plate, after moulding, forced air drying at 80 ℃ 5 hours, obtains hemicellulose group edible film.
Gained half fiber base edible film tensile strength can reach that 36MPa, elongation reach 35%, transmittance reaches 78%, water vapour transmission coefficient can reach 0.32g.mm/m2.h.KPa.With this edible film liquid, grape is carried out to coating-film fresh-keeping experiment, the V-c content in fruit has reduced by 18%, and aminoacids content increases by 25%, and total reducing sugar reduces by 18%, and protein reduces by 23%, compare with the grape of not filming, this organize fresh-keeping grape shelf life extension more than 5 days.
Embodiment 7: the preparation method of hemicellulose group edible film, and concrete operations are as follows:
(1) first in the container with heating and stirring device, add bagasse positively charged ion hemicellulose, 0.06% the NaOH solution (mass percent concentration is 0.5%) that adds positively charged ion hemicellulose quality, predissolve 40min, add therein water, the mass ratio of water and positively charged ion hemicellulose is 90:1 again, then 60 ℃, 450rpm stirring, treatment time 40min, makes hemicellulose hydrolysate;
Wherein the preparation method of bagasse positively charged ion hemicellulose is as follows:
First by bagasse with adopting alcohol deposition method to make hemicellulose after alkali extracting, in every gram of hemicellulose, adding the ratio of 30ml ethanolic soln mixes hemicellulose and ethanolic soln, ethanolic soln mass percent concentration is 60%, in water bath with thermostatic control, stir and be warming up to 65 ℃, drip potassium hydroxide solution (mass percent concentration is 6%), sodium hydroxide addition is 6% of hemicellulose quality, and stir-activating 30min, then the cationic etherifying agent 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride (CHPTMAC) that adds hemicellulose quality 35%, be warming up to 45 ℃ of temperature of reaction, stirring reaction 5 hours, after reaction finishes, with acetic acid neutralization, ethanol precipitation, filtration, washing, at 50 ℃, vacuum-drying is 24 hours, can obtain poplar positively charged ion hemicellulose,
(2) in hemicellulose hydrolysate, add the granulated active carbon of hemicellulose hydrolysate quality 20%, activated carbon granule particle diameter is being between 1.5～3mm, after reaction 20min, filters, and collects filtrate;
(3) in filtrate, add the chitosan of filtrate quality 0.6% and the acetic acid solution of filtrate quality 0.2%, under 800rpm, stir and chitosan is dissolved completely;
(4) in the solution making in step (3), add the softening agent polyoxyethylene glycol of filtrate quality 0.4% and the thickening material Xylo-Mucine of filtrate quality 0.5%, stir, then regulator solution pH value is 3, degassed;
(5) in the solution making in step (4), add glyceryl monostearate and Palmiticacid, be heated to 80 ℃, stir at latter 60 ℃ and be incubated 10min, wherein the addition of starch and Palmiticacid is 0.6% of filtrate quality;
(6) step (5) solution is poured on to masking on poly (methyl methacrylate) plate, after moulding, forced air drying at 80 ℃ 8 hours, obtains hemicellulose group edible film;
The edible film tensile strength that adopts positively charged ion hemicellulose to prepare can reach that 34MPa, elongation reach 29%, transmittance reaches 87%, water vapour transmission coefficient can reach 0.20g.mm/m
2.h.KPa.With this edible film liquid, grape is carried out to coating-film fresh-keeping experiment, the V-c content in fruit has reduced by 40%, and aminoacids content increases by 17%, total reducing sugar reduces by 20%, protein reduces by 28%, compare with the grape of not filming, this organize fresh-keeping grape shelf life extension more than 3-4 days.
Claims (9)
1. a preparation method for hemicellulose group edible film, is characterized in that concrete steps are as follows:
(1) ratio that is 50～100:1 according to the mass ratio of water and hemicellulose or modification hemicellulose, at hemicellulose or in the modification hemicellulose of sig water predissolve 5～40min, add water, stirring and dissolving under 50～70 ℃, 300～500rpm, treatment time 30～40min, make hemicellulose hydrolysate, wherein during the predissolve of modification hemicellulose, the addition of alkali is 0.04～0.08% of modification hemicellulose quality;
(2) in cellulosic hydrolysate, add the granulated active carbon of hemicellulose hydrolysate quality 5～20%, after reaction 20～30min, filter, and collect filtrate;
(3) in filtrate, add the chitosan of filtrate quality 0.3～0.6% and the acetic acid solution of filtrate quality 0.1～0.2%, under 300～800rpm, stir;
(4) softening agent that adds filtrate quality 0.4～1% in the solution making in step (3), stirs, and then regulates pH value to be 2～3, degassed;
(5) in the solution making in step (4), add emulsifying agent and hydrophober, be heated to 60～80 ℃, after stirring, at 60～80 ℃, be incubated 5～10min, wherein the addition of emulsifying agent and hydrophober is 0.3～0.6% of filtrate quality;
(6) with step (5) solution film-forming, after moulding, at 80 ℃, be dried 4～8 hours, obtain hemicellulose group edible film;
Wherein said sig water is that mass percent concentration is 0.2～0.8% NaOH solution or KOH solution.
2. the preparation method of hemicellulose group edible film according to claim 1; it is characterized in that: hemicellulose molecule amount is 10000～50000, modified-cellulose is a kind of in acetylated hemicellulose, bagasse positively charged ion hemicellulose, poplar positively charged ion hemicellulose.
3. the preparation method of hemicellulose group edible film according to claim 1, is characterized in that: when hemicellulose or predissolve modification hydrolysis of hemicellulose, under ultrasound condition or in homogeneous instrument, carry out.
4. the preparation method of hemicellulose group edible film according to claim 1, is characterized in that: softening agent is a kind of in glycerine, sorbyl alcohol, ethylene glycol, polyoxyethylene glycol.
5. the preparation method of hemicellulose group edible film according to claim 1, is characterized in that: emulsifying agent is glyceryl monostearate or starch.
6. the preparation method of hemicellulose group edible film according to claim 1, is characterized in that: hydrophober is Palmiticacid or stearic acid.
7. the preparation method of hemicellulose group edible film according to claim 1, is characterized in that: a kind of add thickening material Xylo-Mucine, polynite, xanthan gum in the preparation of hemicellulose group edible film in, addition is 0.2～1.0% of filtrate quality.
8. the preparation method of hemicellulose group edible film according to claim 1, is characterized in that: a kind of add food antiseptic-germicide nano titanium oxide, phytic acid, Sorbic Acid in the preparation of hemicellulose group edible film in, addition is the 0.01-0.1% of filtrate quality.
9. the preparation method of hemicellulose group edible film according to claim 1, it is characterized in that: adopting modification hemicellulose is that raw material is while preparing film, at film, be dried afterwards, take off film, by after film cooling bath 5～20min, at 40～60 ℃, dry, can obtain the hemicellulose film that transparency is high, wherein water temperature is 10～30 ℃.
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| CN103272570B (en) * | 2013-06-14 | 2014-10-01 | 湖北省潜江市华山水产食品有限公司 | Preparation method and application of hemicellulose/chitosan/nano TiO2 hybrid material |
| CN104945641B (en) * | 2014-03-25 | 2017-12-22 | 北京林业大学 | A kind of preparation method of hemicellulose group organic/inorganic composite film material |
| CN104262658A (en) * | 2014-09-30 | 2015-01-07 | 广西大学 | Preparation method for degradable polysaccharide-based hemicellulose composite biomembrane |
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| CN107936551A (en) * | 2017-11-29 | 2018-04-20 | 王雪畅 | A kind of composite membrane based on bamboo and wood hemicellulose/γ polyglutamic acids and its preparation method and application |
| CN107915855B (en) * | 2017-12-23 | 2020-07-14 | 金华市联宾塑料制品有限公司 | Novel green degradable high-elasticity membrane material |
| CN108610517B (en) * | 2018-05-08 | 2020-12-15 | 昆明理工大学 | Preparation method of nanocellulose-reinforced hemicellulose-based composite membrane |
| CN109081930B (en) * | 2018-07-09 | 2021-03-26 | 北京林业大学 | Functional edible film based on hemicellulose and chitosan and preparation method thereof |
| CN111434709A (en) * | 2019-01-14 | 2020-07-21 | 新疆大学 | Preparation method of hexahydro β -acid/cyclodextrin inclusion compound-chitosan antibacterial film |
| CN109942847A (en) * | 2019-02-15 | 2019-06-28 | 北京林业大学 | A kind of hemicellulose with high-flexibility and mechanical strength/chitosan-based composite membrane and preparation method thereof |
| TWI728643B (en) * | 2020-01-07 | 2021-05-21 | 財團法人亞洲大學 | Method for making edible film from bamboo shoot husk extract and passion fruit husk extract |
| MX2023003016A (en) | 2020-09-22 | 2023-04-10 | Swimc Llc | Chitosan-containing coating compositions. |
| CN112619322A (en) * | 2021-01-15 | 2021-04-09 | 王忠良 | Air filtering membrane replacing melt-blown fabric and preparation method thereof |
| CN113336873B (en) * | 2021-06-03 | 2022-11-22 | 北京林业大学 | Preparation method of green degradable high-transparency xylan film material |
| CN115678112B (en) * | 2022-10-28 | 2023-09-19 | 武汉轻工大学 | Preparation method of complex cellulose carboxymethylation and composite membrane thereof |
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| CN1036140C (en) * | 1992-12-18 | 1997-10-15 | 中国国际科技促进会 | Vegetable fibre film product and its process |
| SE0300801D0 (en) * | 2003-03-21 | 2003-03-21 | Paul Gatenholm | Polymeric film or coating comprising hemicellulose |
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