CN105801890A - Method for preparing high-toughness konjac glucomannan preservative film - Google Patents
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- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0087—Glucomannans or galactomannans; Tara or tara gum, i.e. D-mannose and D-galactose units, e.g. from Cesalpinia spinosa; Tamarind gum, i.e. D-galactose, D-glucose and D-xylose units, e.g. from Tamarindus indica; Gum Arabic, i.e. L-arabinose, L-rhamnose, D-galactose and D-glucuronic acid units, e.g. from Acacia Senegal or Acacia Seyal; Derivatives thereof
- C08B37/009—Konjac gum or konjac mannan, i.e. beta-D-glucose and beta-D-mannose units linked by 1,4 bonds, e.g. from Amorphophallus species; Derivatives thereof
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- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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Abstract
The invention discloses a method for preparing a high-toughness konjac glucomannan preservative film, and belongs to the field of preservative films.The method includes the steps that konjac glucomannan is extracted from konjaku flour, chitosan is added into konjac glucomannan extracting liquid for swelling, modified nanometer montmorillonite powder and glycerol are added to obtain raw film liquid, the raw film liquid is concentrated to be evenly smeared on a glass plate, modification is carried out through deacylation, and the high-toughness konjac glucomannan preservative film is obtained.According to the method, montmorillonite is modified in the preparing process, the dispersity of the montmorillonite in water is high without gathering, and the toughness of the film is improved by adding the modified montmorillonite powder; as konjac glucomannan and chitosan are jointly mixed, the elasticity and the strength of the film can be improved, and antibacterial performance is also improved; the film is modified through deacylation, volatilization of water and consumption of nutrient substances can be inhibited, the speed, passing through the surfaces of fresh products, of oxygen is limited, and therefore the retention period of the fresh products is prolonged.
Description
Technical field
The preparation method that the invention discloses a kind of high tenacity Rhizoma amorphophalli glucomannan preservative film, belongs to preservative film field.
Background technology
Rhizoma amorphophalli glucomannan is a kind of natural macromolecule amylose, comprises glucose and mannose in its molecule, and β-Isosorbide-5-Nitrae-glycosidic bond connects.As a kind of renewable natural resources, Rhizoma amorphophalli glucomannan source is sufficient, biodegradable, has the multifrequency nature such as gelation, film property.Rhizoma amorphophalli glucomannan is big because of its solution viscosity, and stability is high, and antibiotic property is strong, and conjunctiva is careful, smooth character and be taken as the active component of antistaling agent.Fresh food is through the process of KGM antistaling agent, surface forms thin film and closes fresh goods surface pores, formation has tight infiltrative closed environment, moisture evaporation and nutrient substance consumption can be suppressed, restriction oxygen, by fresh goods superficial velocity, weakens fresh goods respiratory intensity, may also suppress the intrusion of pathogenic bacteria and mycete simultaneously and spread, play anti-corrosive fresh-keeping effect, thus extending fresh goods storage life.Such material has impressionability, can be developed into as Novel non-toxic, non-harmful edible food packaging film.
Research about konjac glncomanan film is a lot of in recent years, under certain condition, Rhizoma amorphophalli glucomannan has good film property, but film forming is discontinuous, scrub resistance is poor, the problem such as film formation time length, film strength are low, antibacterial ability is poor and wettability is big, therefore masking again after being generally modified, to improve film property, film-strength, water-resistance and poisture-penetrability.
Summary of the invention
nullThe technical problem that present invention mainly solves: the single film made for current Rhizoma amorphophalli glucomannan also exists many deficiencies，As film forming is discontinuous，Film formation time is long、Film strength is low、Antibacterial ability difference and the problem such as wettability is big，The preparation method providing a kind of high tenacity Rhizoma amorphophalli glucomannan preservative film，The present invention extracts Rhizoma amorphophalli glucomannan from Rhizoma amorphophalli powder，Chitosan is added in Rhizoma amorphophalli glucomannan extracting solution swelling，And add modified nanometer Montmorillonitum powder and glycerol obtains the thick liquid of film，After being concentrated, uniform application is on a glass，High tenacity Rhizoma amorphophalli glucomannan preservative film is obtained by deacylated tRNA base is modified，Montmorillonite is modified by the present invention in preparation，Make its dispersibility in water high and not easily reunite，The toughness of film is improved by adding modified nano montmorillonite powder，Rhizoma amorphophalli glucomannan and chitosan blend can be improved elasticity and the intensity of film，Anti-microbial property is also improved，Thin film is carried out again de-acyl modified，Moisture evaporation and nutrient substance consumption can be suppressed，Restriction oxygen is by fresh goods superficial velocity，Thus extending fresh goods storage life.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) weighing 15～20g konjaku powder and pour in 1L beaker, add 400～500mL dehydrated alcohol, move in 45～55 DEG C of water-baths, stirring moistening 30～40min obtains suspension, is moved into by suspension in colloid mill, grinds 15～25min；
(2) grinding pours abrasive material into buchner funnel after terminating, remove alcohol-soluble free sugar for 3～5 times by dehydrated alcohol filtering and washing and carry out remove impurity process, collect the fine powder after remove impurity and be dissolved in 300～400mL distilled water, with horizontal centrifuge with the centrifugal 20～30min of 4000～6000r/min rotating speed, separation obtains supernatant, it is Rhizoma amorphophalli glucomannan extracting solution, standby；
(3) weigh 10～15g montmorillonite to put into super grinder grinds to form the powder that particle diameter is 2～4 μm, powder after grinding is joined in 100～200mL distilled water, be placed on shaking table vibrate mixing 10～20min obtain montmorillonite powder suspension, the suspension obtained is put in the oil bath pan of 90～100 DEG C, add the follow-up continuous insulated and stirred 4～6h of 2～4g stearic acid while stirring, after filtration, dry to obtain modified nano montmorillonite powder；
(4) it is that 3～5g chitosan is joined in the Rhizoma amorphophalli glucomannan extracting solution that step (2) is standby by 1:10 by solid-to-liquid ratio, after standing swelling 30～50min, add the above-mentioned prepared modified nano montmorillonite powder of 0.5～0.8g and mixed liquor gross mass 7～9% glycerol, pour ultrasonic disperse instrument into after 200～300W power ultrasonic dispersion 10～15min, again with concentration be 0.5mol/L phosphoric acid solution regulate pH to 3～5, obtain the thick liquid of film；
(5) thick for above-mentioned film liquid is moved in vacuum concentration pot, reduce pressure inside the tank to 900～1000Pa, be evaporated to the 1/3 of its original volume, obtain dense thick coating liquid, it is loaded into coating machine to smear uniformly on a glass, puts into baking oven dry 6～8h at 55～65 DEG C；
(6) glass plate of dried load thin film is immersed in the sodium hydroxide solution that concentration is 0.5mol/L; sonic oscillation dipping 2～3h carries out de-acyl modified; modified terminate after at 60～65 DEG C vacuum drying 1～2h, namely obtain high tenacity Rhizoma amorphophalli glucomannan preservative film after taking off film.
The method of the application of the present invention: fruit is deposited and preservative film prepared by the present invention can be used in process to preserve, such as fragrant pear is stored, store 20～40 days at normal temperatures, the rotting rate of fragrant pear reaches 38.5～42.1%, and in edible fruit, vitamin C reduces by 180～220mg/100g, use preservative film that fragrant pear Surface coating is stored, storing 20～40 days at normal temperatures, the rotting rate of fragrant pear reaches 15.2～23.5%, and vitamin C reduces by 120～160mg/100g；The thickness of the preservative film of the present invention is 15～20 μm, and hot strength is 55.8～65.9MPa, and elongation at break is 13.8～17.5%, and moisture-vapor transmission is 16.4～18.2g/m224h, oxygen permeating amount is 47.1368～48.3650cm3/m2·24h·0.1MPa。
The invention has the beneficial effects as follows:
(1) abundant raw material source of the present invention, preparation technology is simple, easy to use；
(2) montmorillonite is modified by the present invention in preparation so that it is in water, dispersibility is high and not easily reunite, and improves the toughness of film by adding modified nano montmorillonite powder；
(3) Rhizoma amorphophalli glucomannan and chitosan blend can improve elasticity and the intensity of film, and anti-microbial property is also improved；
(4) being carried out by thin film de-acyl modified again, can suppress moisture evaporation and nutrient substance consumption, restriction oxygen is by fresh goods superficial velocity, thus extending fresh goods storage life.
Detailed description of the invention
First weighing 15～20g konjaku powder and pour in 1L beaker, add 400～500mL dehydrated alcohol, move in 45～55 DEG C of water-baths, stirring moistening 30～40min obtains suspension, is moved into by suspension in colloid mill, grinds 15～25min；Grinding pours abrasive material into buchner funnel after terminating, remove alcohol-soluble free sugar for 3～5 times by dehydrated alcohol filtering and washing and carry out remove impurity process, collect the fine powder after remove impurity and be dissolved in 300～400mL distilled water, with horizontal centrifuge with the centrifugal 20～30min of 4000～6000r/min rotating speed, separation obtains supernatant, it is Rhizoma amorphophalli glucomannan extracting solution, standby；Weigh 10～15g montmorillonite to put into super grinder grinds to form the powder that particle diameter is 2～4 μm, powder after grinding is joined in 100～200mL distilled water, be placed on shaking table vibrate mixing 10～20min obtain montmorillonite powder suspension, the suspension obtained is put in the oil bath pan of 90～100 DEG C, add the follow-up continuous insulated and stirred 4～6h of 2～4g stearic acid while stirring, after filtration, dry to obtain modified nano montmorillonite powder；It is that 3～5g chitosan is added in standby Rhizoma amorphophalli glucomannan extracting solution by 1:10 by solid-to-liquid ratio, after standing swelling 30～50min, add the above-mentioned prepared modified nano montmorillonite powder of 0.5～0.8g and mixed liquor gross mass 7～9% glycerol, pour ultrasonic disperse instrument into after 200～300W power ultrasonic dispersion 10～15min, again with concentration be 0.5mol/L phosphoric acid solution regulate pH to 3～5, obtain the thick liquid of film；Thick for above-mentioned film liquid is moved in vacuum concentration pot, reduce pressure inside the tank to 900～1000Pa, be evaporated to the 1/3 of its original volume, obtain dense thick coating liquid, it is loaded into coating machine to smear uniformly on a glass, puts into baking oven dry 6～8h at 55～65 DEG C；The glass plate of dried load thin film is immersed in the sodium hydroxide solution that concentration is 0.5mol/L; sonic oscillation dipping 2～3h carries out de-acyl modified; modified terminate after at 60～65 DEG C vacuum drying 1～2h, namely obtain high tenacity Rhizoma amorphophalli glucomannan preservative film after taking off film.
Example 1
First weighing 15g konjaku powder and pour in 1L beaker, add 400mL dehydrated alcohol, move in 45 DEG C of water-baths, stirring moistening 30min obtains suspension, is moved into by suspension in colloid mill, grinds 15min；Grinding pours abrasive material into buchner funnel after terminating, remove alcohol-soluble free sugar for 3 times by dehydrated alcohol filtering and washing and carry out remove impurity process, collect the fine powder after remove impurity and be dissolved in 300mL distilled water, with horizontal centrifuge with the centrifugal 20min of 4000r/min rotating speed, separation obtains supernatant, it is Rhizoma amorphophalli glucomannan extracting solution, standby；Weigh 10g montmorillonite to put into super grinder grinds to form the powder that particle diameter is 2 μm, powder after grinding is joined in 100mL distilled water, it is placed on shaking table vibration mixing 10min and obtains montmorillonite powder suspension, the suspension obtained is put in the oil bath pan of 90 DEG C, add the follow-up continuous insulated and stirred 4h of 2g stearic acid while stirring, after filtration, dry to obtain modified nano montmorillonite powder；It is that 3g chitosan is added in standby Rhizoma amorphophalli glucomannan extracting solution by 1:10 by solid-to-liquid ratio, after standing swelling 30min, add the above-mentioned prepared modified nano montmorillonite powder of 0.5g and mixed liquor gross mass 7% glycerol, pour ultrasonic disperse instrument into after 200W power ultrasonic dispersion 10min, again with concentration be 0.5mol/L phosphoric acid solution regulate pH to 3, obtain the thick liquid of film；Thick for above-mentioned film liquid is moved in vacuum concentration pot, reduce pressure inside the tank to 900Pa, be evaporated to the 1/3 of its original volume, obtain dense thick coating liquid, be loaded into coating machine and smear uniformly on a glass, put into baking oven dry 6h at 55 DEG C；The glass plate of dried load thin film being immersed in the sodium hydroxide solution that concentration is 0.5mol/L, sonic oscillation dipping 2h carries out de-acyl modified, modified terminate after at 60 DEG C vacuum drying 1h, namely obtain high tenacity Rhizoma amorphophalli glucomannan preservative film after taking off film.
Fruit meat and fish dishes is deposited and preservative film prepared by the present invention can be used in process to preserve, such as fragrant pear is stored, store 20 days at normal temperatures, the rotting rate of fragrant pear reaches 38.5%, and in edible fruit, vitamin C reduces 180mg/100g, use preservative film that fragrant pear Surface coating is stored, storing 20 days at normal temperatures, the rotting rate of fragrant pear reaches 15.2%, and vitamin C reduces 120mg/100g；The thickness of the preservative film of the present invention is 15 μm, and hot strength is 55.8MPa, and elongation at break is 13.8%, and moisture-vapor transmission is 16.4g/m224h, oxygen permeating amount is 47.1368cm3/m2·24h·0.1MPa。
Example 2
First weighing 17g konjaku powder and pour in 1L beaker, add 450mL dehydrated alcohol, move in 50 DEG C of water-baths, stirring moistening 35min obtains suspension, is moved into by suspension in colloid mill, grinds 20min；Grinding pours abrasive material into buchner funnel after terminating, remove alcohol-soluble free sugar for 4 times by dehydrated alcohol filtering and washing and carry out remove impurity process, collect the fine powder after remove impurity and be dissolved in 350mL distilled water, with horizontal centrifuge with the centrifugal 25min of 5000r/min rotating speed, separation obtains supernatant, it is Rhizoma amorphophalli glucomannan extracting solution, standby；Weigh 13g montmorillonite to put into super grinder grinds to form the powder that particle diameter is 3 μm, powder after grinding is joined in 150mL distilled water, it is placed on shaking table vibration mixing 15min and obtains montmorillonite powder suspension, the suspension obtained is put in the oil bath pan of 95 DEG C, add the follow-up continuous insulated and stirred 5h of 3g stearic acid while stirring, after filtration, dry to obtain modified nano montmorillonite powder；It is that 4g chitosan is added in standby Rhizoma amorphophalli glucomannan extracting solution by 1:10 by solid-to-liquid ratio, after standing swelling 40min, add the above-mentioned prepared modified nano montmorillonite powder of 0.6g and mixed liquor gross mass 8% glycerol, pour ultrasonic disperse instrument into after 250W power ultrasonic dispersion 13min, again with concentration be 0.5mol/L phosphoric acid solution regulate pH to 4, obtain the thick liquid of film；Thick for above-mentioned film liquid is moved in vacuum concentration pot, reduce pressure inside the tank to 950Pa, be evaporated to the 1/3 of its original volume, obtain dense thick coating liquid, be loaded into coating machine and smear uniformly on a glass, put into baking oven dry 7h at 60 DEG C；The glass plate of dried load thin film being immersed in the sodium hydroxide solution that concentration is 0.5mol/L, sonic oscillation dipping 2.5h carries out de-acyl modified, modified terminate after at 63 DEG C vacuum drying 1.5h, namely obtain high tenacity Rhizoma amorphophalli glucomannan preservative film after taking off film.
Fruit meat and fish dishes is deposited and preservative film prepared by the present invention can be used in process to preserve, such as fragrant pear is stored, store 30 days at normal temperatures, the rotting rate of fragrant pear reaches 39.3%, and in edible fruit, vitamin C reduces 200mg/100g, use preservative film that fragrant pear Surface coating is stored, storing 30 days at normal temperatures, the rotting rate of fragrant pear reaches 18.6%, and vitamin C reduces 140mg/100g；The thickness of the preservative film of the present invention is 17 μm, and hot strength is 60.2MPa, and elongation at break is 15.6%, and moisture-vapor transmission is 17.5g/m224h, oxygen permeating amount is 47.8964cm3/m2·24h·0.1MPa。
Example 3
First weighing 20g konjaku powder and pour in 1L beaker, add 500mL dehydrated alcohol, move in 55 DEG C of water-baths, stirring moistening 40min obtains suspension, is moved into by suspension in colloid mill, grinds 25min；Grinding pours abrasive material into buchner funnel after terminating, remove alcohol-soluble free sugar for 5 times by dehydrated alcohol filtering and washing and carry out remove impurity process, collect the fine powder after remove impurity and be dissolved in 400mL distilled water, with horizontal centrifuge with the centrifugal 30min of 6000r/min rotating speed, separation obtains supernatant, it is Rhizoma amorphophalli glucomannan extracting solution, standby；Weigh 15g montmorillonite to put into super grinder grinds to form the powder that particle diameter is 4 μm, powder after grinding is joined in 200mL distilled water, it is placed on shaking table vibration mixing 20min and obtains montmorillonite powder suspension, the suspension obtained is put in the oil bath pan of 100 DEG C, add the follow-up continuous insulated and stirred 6h of 4g stearic acid while stirring, after filtration, dry to obtain modified nano montmorillonite powder；It is that 5g chitosan is added in standby Rhizoma amorphophalli glucomannan extracting solution by 1:10 by solid-to-liquid ratio, after standing swelling 50min, add the above-mentioned prepared modified nano montmorillonite powder of 0.8g and mixed liquor gross mass 9% glycerol, pour ultrasonic disperse instrument into after 300W power ultrasonic dispersion 15min, again with concentration be 0.5mol/L phosphoric acid solution regulate pH to 5, obtain the thick liquid of film；Thick for above-mentioned film liquid is moved in vacuum concentration pot, reduce pressure inside the tank to 1000Pa, be evaporated to the 1/3 of its original volume, obtain dense thick coating liquid, be loaded into coating machine and smear uniformly on a glass, put into baking oven dry 8h at 65 DEG C；The glass plate of dried load thin film being immersed in the sodium hydroxide solution that concentration is 0.5mol/L, sonic oscillation dipping 3h carries out de-acyl modified, modified terminate after at 65 DEG C vacuum drying 2h, namely obtain high tenacity Rhizoma amorphophalli glucomannan preservative film after taking off film.
Fruit meat and fish dishes is deposited and preservative film prepared by the present invention can be used in process to preserve, such as fragrant pear is stored, store 40 days at normal temperatures, the rotting rate of fragrant pear reaches 42.1%, and in edible fruit, vitamin C reduces 220mg/100g, use preservative film that fragrant pear Surface coating is stored, storing 40 days at normal temperatures, the rotting rate of fragrant pear reaches 23.5%, and vitamin C reduces 160mg/100g；The thickness of the preservative film of the present invention is 20 μm, and hot strength is 65.9MPa, and elongation at break is 17.5%, and moisture-vapor transmission is 18.2g/m224h, oxygen permeating amount is 48.3650cm3/m2·24h·0.1MPa。
Claims (1)
1. the preparation method of a high tenacity Rhizoma amorphophalli glucomannan preservative film, it is characterised in that concrete preparation process is:
(1) weighing 15～20g konjaku powder and pour in 1L beaker, add 400～500mL dehydrated alcohol, move in 45～55 DEG C of water-baths, stirring moistening 30～40min obtains suspension, is moved into by suspension in colloid mill, grinds 15～25min；
(2) grinding pours abrasive material into buchner funnel after terminating, remove alcohol-soluble free sugar for 3～5 times by dehydrated alcohol filtering and washing and carry out remove impurity process, collect the fine powder after remove impurity and be dissolved in 300～400mL distilled water, with horizontal centrifuge with the centrifugal 20～30min of 4000～6000r/min rotating speed, separation obtains supernatant, it is Rhizoma amorphophalli glucomannan extracting solution, standby；
(3) weigh 10～15g montmorillonite to put into super grinder grinds to form the powder that particle diameter is 2～4 μm, powder after grinding is joined in 100～200mL distilled water, be placed on shaking table vibrate mixing 10～20min obtain montmorillonite powder suspension, the suspension obtained is put in the oil bath pan of 90～100 DEG C, add the follow-up continuous insulated and stirred 4～6h of 2～4g stearic acid while stirring, after filtration, dry to obtain modified nano montmorillonite powder；
(4) it is that 3～5g chitosan is joined in the Rhizoma amorphophalli glucomannan extracting solution that step (2) is standby by 1:10 by solid-to-liquid ratio, after standing swelling 30～50min, add the above-mentioned prepared modified nano montmorillonite powder of 0.5～0.8g and mixed liquor gross mass 7～9% glycerol, pour ultrasonic disperse instrument into after 200～300W power ultrasonic dispersion 10～15min, again with concentration be 0.5mol/L phosphoric acid solution regulate pH to 3～5, obtain the thick liquid of film；
(5) thick for above-mentioned film liquid is moved in vacuum concentration pot, reduce pressure inside the tank to 900～1000Pa, be evaporated to the 1/3 of its original volume, obtain dense thick coating liquid, it is loaded into coating machine to smear uniformly on a glass, puts into baking oven dry 6～8h at 55～65 DEG C；
(6) glass plate of dried load thin film is immersed in the sodium hydroxide solution that concentration is 0.5mol/L; sonic oscillation dipping 2～3h carries out de-acyl modified; modified terminate after at 60～65 DEG C vacuum drying 1～2h, namely obtain high tenacity Rhizoma amorphophalli glucomannan preservative film after taking off film.
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2016
- 2016-04-14 CN CN201610228905.3A patent/CN105801890A/en not_active Withdrawn
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| US11560487B2 (en) | 2020-09-22 | 2023-01-24 | Swimc Llc | Coating compositions containing low molecular weight chitosan composition |
| CN113388169A (en) * | 2020-12-15 | 2021-09-14 | 合肥工业大学 | Preparation method of high-temperature-resistant lysozyme composite preservative film for food |
| CN113024859A (en) * | 2021-03-02 | 2021-06-25 | 林香春 | Edible antibacterial medicine packaging film and preparation method thereof |
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| CN112890071A (en) * | 2021-03-11 | 2021-06-04 | 武汉科亿华科技有限公司 | Salicylic acid konjak preservative film and preparation method thereof |
| CN112890071B (en) * | 2021-03-11 | 2024-02-23 | 武汉科亿华科技有限公司 | Salicylic acid konjak preservative film and preparation method thereof |
| CN113085293A (en) * | 2021-03-30 | 2021-07-09 | 西南科技大学 | Preparation method of konjac glucomannan fresh-keeping film |
| CN113085293B (en) * | 2021-03-30 | 2022-03-22 | 西南科技大学 | Preparation method of konjac glucomannan fresh-keeping film |
| CN116874890A (en) * | 2023-06-29 | 2023-10-13 | 贵州电子科技职业学院 | Antibacterial preservative film based on konjak glucomannan and preparation method thereof |
| CN116874890B (en) * | 2023-06-29 | 2024-06-04 | 贵州电子科技职业学院 | Antibacterial preservative film based on konjak glucomannan and preparation method thereof |
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