CN102775647A - Preparation method of hemicellulose based edible film - Google Patents
Preparation method of hemicellulose based edible film Download PDFInfo
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- CN102775647A CN102775647A CN2012102665886A CN201210266588A CN102775647A CN 102775647 A CN102775647 A CN 102775647A CN 2012102665886 A CN2012102665886 A CN 2012102665886A CN 201210266588 A CN201210266588 A CN 201210266588A CN 102775647 A CN102775647 A CN 102775647A
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- semicellulose
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- hemicellulose
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- edible film
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- 229920002488 Hemicellulose Polymers 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000000413 hydrolysate Substances 0.000 claims abstract description 15
- 235000013305 food Nutrition 0.000 claims abstract description 14
- 238000007872 degassing Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 3
- 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 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
- 150000002500 ions Chemical class 0.000 claims description 17
- 229920001661 Chitosan Polymers 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 16
- 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
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- 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
- 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
- -1 polyoxyethylene Polymers 0.000 claims description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 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
- 238000004519 manufacturing process Methods 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
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- 229920002678 cellulose Polymers 0.000 claims description 3
- 239000001913 cellulose Substances 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
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 235000013399 edible fruits Nutrition 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 6
- 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
- 239000004014 plasticizer Substances 0.000 abstract 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 13
- 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 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
- 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
- 238000005516 engineering process Methods 0.000 description 5
- 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
- 239000012528 membrane Substances 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 241001092070 Eriobotrya Species 0.000 description 3
- 235000009008 Eriobotrya japonica Nutrition 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- 238000000151 deposition 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
- 238000004062 sedimentation Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 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
- 230000002349 favourable effect Effects 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- 235000008935 nutritious Nutrition 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 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
- 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
- 239000000706 filtrate Substances 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
- 230000003014 reinforcing effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 235000015067 sauces Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229960005196 titanium dioxide Drugs 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
- General Preparation And Processing Of Foods (AREA)
- Jellies, Jams, And Syrups (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 the food product pack field, compare other stationery and plastic wrapping, edible packing membrane has incomparable advantage, and it has characteristics such as edible, health, nutrition, environmental protection, convenience.The traditional technology and the limitation of prescription make the edible film of preparation have some limitation, such as: membrane prepare raw material consumption is big, operational path is comparatively complicated, makes industriallization 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 the scale operation utilization.
At present to the base material major part of edible film round expansion such as starch, Sunlover 10, lipid materials; But be prone to crisp, big legume protein film forming after the starch film forming intensity difference and protein denaturation take place easily; Lipid material polarity again is very weak and not soluble in water; Be difficult to shortcomings such as film forming, make that above film suitability is not strong.The present invention adopts nutritious and the base material of the natural hemicellulose polysaccharide of nourishing function as edible film is arranged; And on the basis of traditional filming technology; The not high characteristic of intensity after the strong and film forming is carried out modification to semicellulose, and is improved with regard to the membrane prepare technology after the modification to the polyose substrate hydrophilic; Improve semicellulose film strength and hydrophobic nature greatly, further satisfied 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; Deficiencies such as this method has overcome that existing edible film kind is single, intensity is low, poor transparency, elongation are little, barrier property difference; Adopt semicellulose/modification semicellulose as the edible film base-material; Be aided with other auxiliary agent again, prepare the hemicellulose group edible film that has satisfied the edible food package requirement, half-and-half cellulosic diversification and industrial applications are significant.
Technical scheme of the present invention is following:
(1) adds entry at semicellulose or in the modification semicellulose of sig water predissolve 5～40min; Stirring and dissolving under 50～70 ℃, 300～500rpm; Treatment time 30～40min makes hemicellulose hydrolysate, wherein during the predissolve of modification semicellulose; The addition of alkali is 0.04～0.08% of a modification semicellulose quality, and the mass ratio of water and semicellulose or modification semicellulose is for being 50:1～100:1;
(2) granulated active carbon of adding cellulosic hydrolysate quality 5～20% in cellulosic hydrolysate, the activated carbon granule size is 1.5～3mm for particle diameter, behind reaction 20～30min, filters, and collects and filtrate;
(3) in filtrating, add the chitosan of filtrating quality 0.3～0.6% and the acetic acid soln of filtrating quality 0.1～0.2%, under 300～800rpm, stir;
(4) fluidizer of adding filtrating quality 0.4～1% in the solution that step (3) makes stirs, and regulating pH value then is 2～3, adopts the ordinary method degassing;
(5) in the solution that step (4) makes, add emulsifying agent and hydrophober, be heated to 60 ℃～80 ℃, the back that stirs is incubated 5～10min down for 60～80 ℃, and wherein the addition of emulsifying agent and hydrophober is 0.3～0.6% of the filtrating quality;
(6) with step (5) solution film-forming, descended dry 4～8 hours at 80 ℃ after the moulding, promptly get the hemicellulose group edible film.
The semicellulose molecular weight is 10000～50000 among the present invention, and modified-cellulose is a kind of in acetylated hemicellulose, the positively charged ion semicellulose.
Sig water is that mass percent concentration is 0.2～0.8% NaOH solution or KOH solution among the present invention.
When Mierocrystalline cellulose or predissolve modification hydrolysis of hemicellulose, under ultrasound condition or in the homogeneous appearance, carry out among the present invention.
Softening agent is that softening agent is a kind of in glycerine, sorbyl alcohol, terepthaloyl moietie, the polyoxyethylene glycol among the present invention, and its addition is 0.4～1% of the filtrating quality.
Emulsifying agent is glyceryl monostearate or starch among the present invention, and addition is 0.3～0.6% of the filtrating quality.
Hydrophober is Palmiticacid or Triple Pressed Stearic Acid among the present invention, and its addition is 0.3～0.6% of the filtrating quality.
A kind of in adding thickening material Xylo-Mucine, polynite, the XG 550 in the preparation of hemicellulose group edible film among the present invention, addition is 0.2～1.0% of the filtrating quality.
A kind of in interpolation food antiseptic-germicide nano titanium oxide, phytic acid, the Sorbic Acid in the preparation of hemicellulose group edible film among the present invention, addition is the 0.01-0.1% of filtrating quality.It still is a kind of good fruit glaze agent that chitosan not only has anti-microbial effect, but the anti-microbial property of chitosan and nano titanium oxide, phytic acid, Sorbic Acid reinforcing membrane.
When adopting the modification semicellulose to be the feedstock production film described in the present invention, after the film drying, take film off, with (water temperature is 10～30 ℃) behind film cooling bath 5～20min, 40～60 ℃ of oven dry down can obtain high-clarity semicellulose film again.
Ordinary method is adopted in the preparation of positively charged ion semicellulose among the present invention; Adding the 30-50ml ethanolic soln by every gram semicellulose (adopting alcohol deposition method to obtain semicellulose after the extracting of raw material alkali) mixes semicellulose and ethanolic soln; The ethanolic soln mass percent concentration is 40%～60%; In water bath with thermostatic control, stir and be warming up to 55 ℃～65 ℃, dropping sodium solution (mass percent concentration is 6%), the sodium hydroxide addition is 5～7% of a semicellulose quality; And stir-activating 30min; The cationic etherifying agent 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride (CHPTMAC) that adds semicellulose quality 25%～35% then is warming up to temperature of reaction 45-65 ℃, stirring reaction 2～5 hours; After reaction finished, with acetic acid neutralization, ethanol sedimentation, filtration, washing 40～50 ℃ of following vacuum-dryings 24 hours, can obtain the positively charged ion semicellulose.
The present invention adopts semicellulose or modification semicellulose as base material; And in the hydrolyzed solution of base material, add 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 materials of food such as sauce packet, coffee, candied haws on a stick) and outer packaging (as: outer package of food materials such as fruit, cake); This film is with its good barrier property and favorable mechanical performance, can satisfy the requirement of internal packing and outer packaging in the food.
The more original edible film of the present invention is compared, and adopts semicellulose or the modification semicellulose preparation base-material as film, have nutritious, preparation is simple, only can satisfy requirements such as intensity and transparency with a spot of base-material and auxiliary agent; Technology is simple with prescription, and base-material and auxiliary dosage are few, is convenient to suitability for industrialized production and promotes; In addition with market on like product such as glutinous rice film compare, intensity, barrier property, mechanical property and transparency are higher, are more suitable for as packaging material for food.
Embodiment
Through embodiment the present invention is done further explain below, but protection domain of the present invention is not limited to said content, the method like no specified otherwise among the embodiment all adopts ordinary method.
Embodiment 1: the preparation method of hemicellulose group edible film, and concrete operations are following:
(1) in having the container of heating and stirring device, adds earlier semicellulose (molecular weight is 20000); Add entry then therein, stirring and dissolving under 70 ℃, 300rpm then, treatment time 40min; Make hemicellulose hydrolysate, the mass ratio 50:1 of water and semicellulose;
(2) granulated active carbon of adding hemicellulose hydrolysate quality 15% in hemicellulose hydrolysate, the activated carbon granule particle diameter is being between 1.5～3mm, behind the reaction 20min, filters, and collects filtrating;
(3) in filtrating, add the chitosan of filtrating quality 0.5% and the acetic acid soln of filtrating quality 0.1%, under 300rpm, stir and make the chitosan dissolving fully;
(4) the softening agent glycerine of adding filtrating quality 0.5% in the solution that step (3) makes stirs, and regulator solution pH value is 2.5 then, degassing 5min;
(5) in the solution that step (4) makes, add glyceryl monostearate and Palmiticacid, be heated to 60 ℃, stir back 80 ℃ and be incubated 5min down, wherein the addition of glyceryl monostearate and Palmiticacid is 0.3% of the filtrating quality;
(6) step (5) solution is poured on makes film on the poly (methyl methacrylate) plate, 80 ℃ of following forced air dryings 4 hours, promptly get the hemicellulose group edible film after the moulding.
Gained half fiber base edible film tensile strength can reach that 30MPa, elongation reach 20%, transmittance reaches 60%, the water vapour transmission coefficient can reach 0.30g.mm/m
2.h.KPa.With this edible film liquid tomato is carried out coating-film fresh-keeping experiment, the V-c content in the 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 following:
(1) in having the container of heating and stirring device, adds earlier semicellulose (molecular weight is 15000); And add entry therein, stirring and dissolving under 70 ℃, 500rpm then, treatment time 30min; Make hemicellulose hydrolysate, the mass ratio of water and semicellulose is 50:1;
(2) granulated active carbon of adding hemicellulose hydrolysate quality 10% in hemicellulose hydrolysate, the activated carbon granule particle diameter is being between 1.5～3mm, behind the reaction 30min, filters, and collects filtrating;
(3) in filtrating, add the chitosan of filtrating quality 0.3% and the acetic acid soln of filtrating quality 0.1%, under 500rpm, stir and make the chitosan dissolving fully;
(4) the softening agent sorbyl alcohol of adding filtrating quality 0.5% in the solution that step (3) makes stirs, and the regulator solution pH value is 3 then, the degassing;
(5) in the solution that step (4) makes, add starch and Triple Pressed Stearic Acid, be heated to 70 ℃, stir back 70 ℃ and be incubated 7min down, wherein starch and stearic addition are 0.5% of the filtrating quality;
(6) step (5) solution is poured on makes film on the poly (methyl methacrylate) plate, 80 ℃ of following forced air dryings 4 hours, promptly get the hemicellulose group edible film after the moulding.
Gained half fiber base edible film tensile strength can reach that 28MPa, elongation reach 20%, transmittance reaches 70%, the water vapour transmission coefficient can reach 0.35g.mm/m2.h.KPa.With this edible film liquid tomato is carried out coating-film fresh-keeping experiment, the V-c content in the 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 following:
(1) earlier in having the container of heating and stirring device, adds acetylated hemicellulose, add 0.08% NaOH solution (mass percent concentration is 0.2%) of acetylated hemicellulose quality, predissolve 10min; Add entry more therein; The mass ratio of water and acetylated hemicellulose is 80:1, at 60 ℃, 400rpm, ultrasound condition (ultrasonic frequency 40kHz, power 120W) ultrasonic 20min down, stirs afterwards then; Treatment time 10min makes hemicellulose hydrolysate;
(2) granulated active carbon of adding hemicellulose hydrolysate quality 5% in hemicellulose hydrolysate, the activated carbon granule particle diameter is being between 1.5～3mm, behind the reaction 25min, filters, and collects filtrating;
(3) in filtrating, add the chitosan of filtrating quality 0.4% and the acetic acid soln of filtrating quality 0.15%, under 600rpm, stir and make the chitosan dissolving fully;
(4) the softening agent terepthaloyl moietie of adding filtrating quality 1% in the solution that step (3) makes stirs, and the regulator solution pH value is 3 then, the degassing;
(5) in the solution that step (4) makes, add starch and Palmiticacid, be heated to 65 ℃, stir back 70 ℃ and be incubated 6min down, wherein the addition of starch and Palmiticacid is 0.4% of the filtrating quality;
(6) step (5) solution be poured on make film on the poly (methyl methacrylate) plate, after the moulding 80 ℃ of following forced air dryings 6 hours;
(7) dried film is put into after cooling bath handles 10min again, 60 ℃ of oven dry down can obtain high-clarity semicellulose film, and wherein cold water temperature is 10 ℃.
Employing through the edible film tensile strength of the modification semicellulose of prehydrolysis preparation can reach that 38MPa, elongation reach 30%, transmittance reaches 85%, the water vapour transmission coefficient can reach 0.18g.mm/m
2.h.KPa.With this edible film liquid grape is carried out the coating-film fresh-keeping experiment, the V-c content in the 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 following:
(1) in having the container of heating and stirring device, adds poplar positively charged ion semicellulose earlier; Add 0.04% NaOH solution (mass percent concentration is 0.8%) of positively charged ion semicellulose quality, predissolve 5min adds entry more therein; The mass ratio of water and positively charged ion semicellulose is 60:1; 65 ℃, 350rpm stirring, treatment time 35min makes hemicellulose hydrolysate then;
Wherein the preparation method of poplar positively charged ion semicellulose is following:
At first adopt alcohol deposition method to make semicellulose after with the alkali extracting poplar; Add the ratio of 50ml ethanolic soln in every gram semicellulose semicellulose and ethanolic soln are mixed, the ethanolic soln mass percent concentration is 40%, in water bath with thermostatic control, stirs and is warming up to 60 ℃; Dropping sodium solution (mass percent concentration is 6%); The sodium hydroxide addition is 5% of a semicellulose quality, and stir-activating 30min, adds the cationic etherifying agent 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride (CHPTMAC) of semicellulose quality 30% then; Be warming up to 65 ℃ of temperature of reaction, stirring reaction 2 hours; After reaction finished, with acetic acid neutralization, ethanol sedimentation, filtration, washing 45 ℃ of following vacuum-dryings 24 hours, can obtain poplar positively charged ion semicellulose;
(2) granulated active carbon of adding hemicellulose hydrolysate quality 20% in hemicellulose hydrolysate, the activated carbon granule particle diameter is being between 1.5～3mm, behind the reaction 20min, filters, and collects filtrating;
(3) in filtrating, add the chitosan of filtrating quality 0.6% and the acetic acid soln of filtrating quality 0.2%, under 800rpm, stir and make the chitosan dissolving fully;
(4) in the solution that step (3) makes, add the softening agent polyoxyethylene glycol of filtrating quality 0.4% and the thickening material Xylo-Mucine of filtrating quality 0.5%, stir, the regulator solution pH value is 3 then, the degassing;
(5) in the solution that step (4) makes, add glyceryl monostearate and Palmiticacid, be heated to 80 ℃, stir back 60 ℃ and be incubated 10min down, wherein the addition of starch and Palmiticacid is 0.6% of the filtrating quality;
(6) step (5) solution be poured on make film on the poly (methyl methacrylate) plate, after the moulding 80 ℃ of following forced air dryings 8 hours;
(7) dried film is put into after cooling bath handles 5min again, 50 ℃ of oven dry down can obtain high-clarity semicellulose film, and wherein cold water temperature is 20 ℃.
Adopt that the edible film tensile strength of positively charged ion semicellulose preparation can reach that 33MPa, elongation reach 28%, transmittance reaches 86%, the water vapour transmission coefficient can reach 0.16g.mm/m
2.h.KPa.With this edible film liquid grape is carried out the coating-film fresh-keeping experiment, the V-c content in the 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 following:
(1) in having the container of heating and stirring device, adds earlier semicellulose (molecular weight is 25000); And add entry therein, stirring and dissolving under 50 ℃, 350rpm then, treatment time 35min; Make hemicellulose hydrolysate, the mass ratio of water and semicellulose is 100:1;
(2) granulated active carbon of adding hemicellulose hydrolysate quality 12% in hemicellulose hydrolysate, the activated carbon granule particle diameter is being between 1.5～3mm, behind the reaction 20min, filters, and collects filtrating;
(3) in filtrating, add the chitosan of filtrating quality 0.3%, the acetic acid soln of filtrating quality 0.1%, the nano titanium oxide of filtrating quality 0.05%, under 500rpm, stir;
(4) in the solution that step (3) makes, add the softening agent sorbyl alcohol of filtrating quality 0.5% and the thickening material polynite of filtrating quality 0.2%, stir, the regulator solution pH value is 2 then, the degassing;
(5) in the solution that step (4) makes, add starch and Triple Pressed Stearic Acid, be heated to 75 ℃, stir back 65 ℃ and be incubated 8min down, wherein starch and stearic addition are 0.4% of filtrating quality;
(6) step (5) solution is poured on makes film on the poly (methyl methacrylate) plate, 80 ℃ of following forced air dryings 5 hours, promptly get the hemicellulose group edible film after the moulding.
Gained half fiber base edible film tensile strength can reach that 32MPa, elongation reach 25%, transmittance reaches 75%, the water vapour transmission coefficient can reach 0.25g.mm/m2.h.KPa; With this edible film liquid loquat is carried out the coating-film fresh-keeping experiment; V-c content in the fruit has reduced by 52%, and aminoacids content increases by 17%, compares with the loquat of not filming; This organize fresh-keeping loquat shelf life extension more than 7 days and do not have a TiO
2Group relatively adds TiO
2The back is favourable to fruit freshness preserving.
Embodiment 6: the preparation method of hemicellulose group edible film, and concrete operations are following:
(1) in having the container of heating and stirring device, adds earlier semicellulose (molecular weight is 30000); And add entry therein, stirring and dissolving under 55 ℃, 450rpm then, treatment time 30min; Make hemicellulose hydrolysate, the mass ratio of water and semicellulose is 70:1;
(2) granulated active carbon of adding hemicellulose hydrolysate quality 12% in hemicellulose hydrolysate, the activated carbon granule particle diameter is being between 1.5～3mm, behind the reaction 25min, filters, and collects filtrating;
(3) in filtrating, add the chitosan of filtrating quality 0.4%, the acetic acid soln of filtrating quality 0.2%, the phytic acid of filtrating quality 0.01%, under 500rpm, stir;
(4) in the solution that step (3) makes, add the softening agent glycerine of filtrating quality 0.5% and the thickening material XG 550 of filtrating quality 0.2%, stir, the regulator solution pH value is 2 then, the degassing;
(5) in the solution that step (4) makes, add starch and Triple Pressed Stearic Acid, be heated to 80 ℃, stir back 60 ℃ and be incubated 10min down, wherein starch and stearic addition are 0.5% of filtrating quality;
(6) step (5) solution is poured on makes film on the poly (methyl methacrylate) plate, 80 ℃ of following forced air dryings 5 hours, promptly get the hemicellulose group edible film after the moulding.
Gained half fiber base edible film tensile strength can reach that 36MPa, elongation reach 35%, transmittance reaches 78%, the water vapour transmission coefficient can reach 0.32g.mm/m2.h.KPa.With this edible film liquid grape is carried out coating-film fresh-keeping experiment, the V-c content in the 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 following:
(1) in having the container of heating and stirring device, adds earlier bagasse positively charged ion semicellulose, add 0.06% NaOH solution (mass percent concentration is 0.5%) of positively charged ion semicellulose quality, predissolve 40min; Add entry more therein, the mass ratio of water and positively charged ion semicellulose is 90:1, then 60 ℃, 450rpm stirring; Treatment time 40min makes hemicellulose hydrolysate;
Wherein the preparation method of bagasse positively charged ion semicellulose is following:
At first adopt alcohol deposition method to make semicellulose after with the alkali extracting bagasse; Add the ratio of 30ml ethanolic soln in every gram semicellulose semicellulose and ethanolic soln are mixed, the ethanolic soln mass percent concentration is 60%, in water bath with thermostatic control, stirs and is warming up to 65 ℃; Drip potassium hydroxide solution (mass percent concentration is 6%); The sodium hydroxide addition is 6% of a semicellulose quality, and stir-activating 30min, adds the cationic etherifying agent 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride (CHPTMAC) of semicellulose quality 35% then; Be warming up to 45 ℃ of temperature of reaction, stirring reaction 5 hours; After reaction finished, with acetic acid neutralization, ethanol sedimentation, filtration, washing 50 ℃ of following vacuum-dryings 24 hours, can obtain poplar positively charged ion semicellulose;
(2) granulated active carbon of adding hemicellulose hydrolysate quality 20% in hemicellulose hydrolysate, the activated carbon granule particle diameter is being between 1.5～3mm, behind the reaction 20min, filters, and collects filtrating;
(3) in filtrating, add the chitosan of filtrating quality 0.6% and the acetic acid soln of filtrating quality 0.2%, under 800rpm, stir and make the chitosan dissolving fully;
(4) in the solution that step (3) makes, add the softening agent polyoxyethylene glycol of filtrating quality 0.4% and the thickening material Xylo-Mucine of filtrating quality 0.5%, stir, the regulator solution pH value is 3 then, the degassing;
(5) in the solution that step (4) makes, add glyceryl monostearate and Palmiticacid, be heated to 80 ℃, stir back 60 ℃ and be incubated 10min down, wherein the addition of starch and Palmiticacid is 0.6% of the filtrating quality;
(6) step (5) solution is poured on makes film on the poly (methyl methacrylate) plate, 80 ℃ of following forced air dryings 8 hours, promptly get the hemicellulose group edible film after the moulding;
Adopt that the edible film tensile strength of positively charged ion semicellulose preparation can reach that 34MPa, elongation reach 29%, transmittance reaches 87%, the water vapour transmission coefficient can reach 0.20g.mm/m
2.h.KPa.With this edible film liquid grape is carried out the coating-film fresh-keeping experiment, the V-c content in the 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 (10)
1. the preparation method of a hemicellulose group edible film is characterized in that concrete steps are following:
(1) mass ratio according to water and semicellulose or modification semicellulose is the ratio of 50～100:1; Add entry at semicellulose or in the modification semicellulose of sig water predissolve 5～40min; Stirring and dissolving under 50～70 ℃, 300～500rpm, treatment time 30～40min makes hemicellulose hydrolysate; Wherein during the predissolve of modification semicellulose, the addition of alkali is 0.04～0.08% of a modification semicellulose quality;
(2) granulated active carbon of adding hemicellulose hydrolysate quality 5～20% in cellulosic hydrolysate behind reaction 20～30min, filters, and collects filtrating;
(3) in filtrating, add the chitosan of filtrating quality 0.3～0.6% and the acetic acid soln of filtrating quality 0.1～0.2%, under 300～800rpm, stir;
(4) softening agent of adding filtrating quality 0.4～1% in the solution that step (3) makes stirs, and regulating pH value then is 2～3, the degassing;
(5) in the solution that step (4) makes, add emulsifying agent and hydrophober, be heated to 60～80 ℃, the back that stirs is incubated 5～10min down for 60～80 ℃, and wherein the addition of emulsifying agent and hydrophober is 0.3～0.6% of the filtrating quality;
(6), descending dry 4～8 hours, promptly get the hemicellulose group edible film after the moulding at 80 ℃ with step (5) solution film-forming.
2. according to the preparation method of the said hemicellulose group edible film of claim 1; It is characterized in that: the semicellulose molecular weight is 10000～50000, and modified-cellulose is a kind of in acetylated hemicellulose, bagasse positively charged ion semicellulose, the poplar positively charged ion semicellulose.
3. according to the preparation method of the said hemicellulose group edible film of claim 1, it is characterized in that: sig water is that mass percent concentration is 0.2～0.8% NaOH solution or KOH solution.
4. according to the preparation method of the said hemicellulose group edible film of claim 1, it is characterized in that: when semicellulose or predissolve modification hydrolysis of hemicellulose, under ultrasound condition or in the homogeneous appearance, carry out.
5. according to the preparation method of the said hemicellulose group edible film of claim 1, it is characterized in that: softening agent is a kind of in glycerine, sorbyl alcohol, terepthaloyl moietie, the polyoxyethylene glycol.
6. according to the preparation method of the said hemicellulose group edible film of claim 1, it is characterized in that: emulsifying agent is glyceryl monostearate or starch.
7. according to the preparation method of the said hemicellulose group edible film of claim 1, it is characterized in that: hydrophober is Palmiticacid or Triple Pressed Stearic Acid.
8. according to the preparation method of the said hemicellulose group edible film of claim 1, it is characterized in that: a kind of in adding thickening material Xylo-Mucine, polynite, the XG 550 in the preparation of hemicellulose group edible film, addition is 0.2～1.0% of the filtrating quality.
9. according to the preparation method of the said hemicellulose group edible film of claim 1, it is characterized in that: a kind of in interpolation food antiseptic-germicide nano titanium oxide, phytic acid, the Sorbic Acid in the preparation of hemicellulose group edible film, addition is the 0.01-0.1% of filtrating quality.
10. according to the preparation method of the said hemicellulose group edible film of claim 1, it is characterized in that: adopt the modification semicellulose to do
During the feedstock production film, after the film drying, take film off, behind film cooling bath 5～20min, 40～60 ℃ of oven dry down can obtain the high semicellulose film of transparency, and wherein water temperature is 10～30 ℃.
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