CN104059239B - A kind of tea grounds makes the method for preservative film - Google Patents
A kind of tea grounds makes the method for preservative film Download PDFInfo
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- CN104059239B CN104059239B CN201410324790.9A CN201410324790A CN104059239B CN 104059239 B CN104059239 B CN 104059239B CN 201410324790 A CN201410324790 A CN 201410324790A CN 104059239 B CN104059239 B CN 104059239B
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Abstract
The present invention relates to a kind of with tea grounds as raw material, by alkali liquor extraction, laccase hydrolyzes, ultrafiltration purification is prepared low-molecular-weight half fiber, and based on this cellulose, added the method that a small amount of plastic agent prepares edible freshness-keeping thin coat.The method dissolves alkali solubility hemicellulose in tea grounds according to low-concentration alkali liquor (0.4 0.5mol/L), again with by regulation pH value and the lignin in the laccase hydrating solution using concentration to be 0.02%～0.1%, it is 3000～50000g/mol to concentrate by ultrafiltration molecular cut off, use the ethanol precipitation hemicellulose of high concentration (80%～90%), yield is between 1% ~ 2%, and prepares preservative film with plasticizers such as this hemicellulose and xylitol, sorbitol, mannitol and glycerol.This technique is simple, made preservative film tool resistance to mechanical ability height, the oil resistance strong, waterproof of antioxygen penetration, the feature such as high temperature resistant and degradable.
Description
Technical field
The present invention relates to a kind of method that tea grounds makes preservative film, belong to food processing and technical field of preservation of fresh.
Background technology
Renewable lignocellulose resource is to solve one of day by day exhausted effective way with environmental problem of fossil resources.Hemicellulose is widely present in the fine cell wall of plant, is the alkali-soluble polysaccharide that is polymerized by the glycosyl of non-glucose of a class, primarily serves connection cellulose and the effect of lignin, occupies the 20%～35% of cell wall gross weight.
Hemicellulose structure is complicated, and glycosyl units is of a great variety, common are D-xylose, L-arabinose, D-galactose, D-MANNOSE etc., the hemicellulose of natural botanical source, is largely used to the production of raw material in sugar industry, such as xylitol, galactose etc..The structure of hemicellulose sugar unit and the multiformity of composition, determine physics and the chemical attribute plasticity of hemicellulose, as the hemicellulose in Semen Tritici aestivi Radix Platycodonis possesses good cohesive and film forming ability.Plant hemicellulose is a kind of renewable, degradable edible raw material, typically is provided with preferably hindering the ability that oxygen, water and macromole have free passage, therefore can use application prospect huge present on preservative film.
Tea grounds still processes as a kind of waste resource in China, reaches 1.6 ten thousand tons from the tea grounds that tea beverage and production of instant tea producer are discarded every year.Tea grounds after water extraction processes, content of cellulose enriches, and accounts for the 14.55%～23.38% of tea grounds dry weight, and the content of hemicellulose about 6%～16%, is the desirable feedstock obtaining edible hemicellulose.
In tea grounds, the composition of hemicellulose sugar unit is relatively easy, and including glucose sugar, galactose, arabinose, xylose, rhamnose, galacturonic acid and aminogalactose, wherein galactose, arabinose and glucose sugar occupy the 82.2% of glycosyl total amount.The same with other plant class half fiber, tea-leaf dietary fiber possesses preferable water holding, holds perfume (or spice) and the performance of isolation microorganism, but individually film property is poor.
On existing market, popular Perserving materials great majority are still that the plastics such as polyethylene (PE), polrvinyl chloride (PVC), polyvinylidene chloride (PVDC), in addition to deriving from non-degradable material, under certain ambient condition, also have the infiltration in food of chemical change and harmful substance such as microwave, refrigerator, baking etc., thus be detrimental to health.
Protein, polysaccharide, fatty acid and resinae etc. can form the film possessed the most structurally and functionally by the intermolecular interaction of self group or foreign aid, therefore, are also the main sources of edible material.China Patent Publication No.: " CN
102850562 A " disclose and a kind of utilize casein and glycerol in milk to prepare edible and the method for degradable preservative film by being dried; casein film-forming process is simple, and fresh-keeping effect is more notable, but the source facing casein is relatively limited; the problems such as price is high, and film forming ductility is poor.China Patent Publication No.: " CN 102850470 A " discloses and a kind of utilizes alkaline hydrogen peroxide method from the method for tea grounds separating high-purity tea grounds half fiber, but utilize H2O2Can not preferably go out the lignin in tea grounds, must be through relatively complicated macroporous resin ethanol gradient elution except colour purity, this method purpose is being only that the hemicellulose preparing higher degree from tea grounds.
Summary of the invention
It is an object of the invention to provide a kind of hemicellulose that extracts from tea grounds, and the method preparing the food fresh keeping membrane of edibility with it for primary raw material, to make up or to overcome weak point of the prior art.
For achieving the above object, the technical solution used in the present invention is as follows: a kind of tea grounds makes the method for preservative film, it is characterised in that comprise the steps:
(1) by the tea grounds through high-temperature water extracted, under 100 DEG C～120 DEG C of environment, 2h is dried, size-reduced, rear mistake 200～300 mesh sieve, make tea powder.
(2) tea powder that step (1) is produced is mixed with the KOH solution that concentration is 0.4mol/L～0.5mol/L according to the ratio that feed liquid mass ratio is 1:15, extract 5h at 45 DEG C～50 DEG C, filter afterwards, take filtrate and obtain crude fibre aqueous slkali；The KOH of this concentration extracts and dissolves the hemicellulose that the degree of polymerization is on the low side, if excessive concentration 1mol/L, the hemicellulose degree of polymerization is high, and film forming ability is poor, is just somewhat like cellulose and lignin.
(3) by the crude fibre aqueous slkali obtained by step (2), add acetic acid regulation make pH between 4.8～5.5, after according to V/V be 100:1 add mass concentration be 0.02%～0.1% laccase acetum, at 45 DEG C be incubated 2h, obtain thick hemicellulose solution；Owing to the tea grounds of alkaline extraction removing polyphenol and water soluble ingredient is mainly composed of hemicellulose, lignin and protein (on a small quantity), the Main Function in this step is laccase hydrolytic lignin, controls hydrolysis degree, not complete hydrolysis.
(4) by thick for step (3) gained half fiber solution by roll-to-roll ultrafiltration filter element, ultrafilter membrane molecular cut off is 3000～50000g/mol, and operation pressure is 100KPa, obtains hemicellulose concentrated solution；The hemicellulose of certain degree of polymerization that screening was processed by previous step and lignin hydrolysing component.
(5) by step (4) gained hemicellulose concentrated solution, adding dehydrated alcohol to concentration of alcohol is 80%～90%, mix homogeneously, stands 12h, and rear filtration or centrifugal, filtering residue is highly branched chain hemicellulose goods.
(6) step (5) gained hemicellulose goods are dissolved in the concentration of 0.5mg/ml～2mg/ml the glycerine water solution of 30%, add the edibility plasticizer aqueous solution that mass concentration is 5%～30%, edibility plasticizer aqueous solution is 1:6～1:10 with the volume ratio of glycerine water solution, rear stirring 30min～45min, and carry out cross-linking reaction in 50 DEG C～60 DEG C.
(7) by step (6) gained solution according to 0.01g/cm2～0.1g/cm2Pour on smooth metal grinding tool, i.e. obtain edibility hemicellulose preservative film at 100 DEG C of baking 1h.
As preferably, in step (2), the concentration of KOH is 0.4mol/L.
As preferably, in step (3), the mass concentration of laccase acetum is 0.05%.
As preferably, in step (4), ultrafilter membrane molecular cut off is 25000g/mol.
As preferably, in step (6), the mass concentration of edibility plasticizer is 25%.
As preferably, in step (7), gained solution is according to 0.05g/cm2Pour on smooth metal grinding tool.
As preferably, the edibility plasticizer described in step (6) is xylitol or sorbitol or mannitol.
The relatively low aqueous slkali of concentration can obtain the hemicellulose that side chain is more, molecular weight is relatively small, film property is high, and the alkali of high concentration can increase the solvability of straight chain hemicellulose, the phenol unit of lignin is oxidized to phenoxy group and loses crosslinking ability by laccase, the lignin of partially stabilized form of degrading.
The invention have the benefit that this product laccase hydrolytic lignin the inferior tea hemicellulose obtained by ultrafiltration and high concentration of alcohol precipitation contain a certain amount of low molecule hydrolysate, side chain is more, possess good film property, antioxygen penetration and the ability of deadening microorganism, after adding plasticizer, it is possible to promote tensile stress and moisture protection；Having resistance to mechanical ability height, the oil resistance strong, waterproof of antioxygen penetration, the feature such as high temperature resistant and degradable by edibility half fiber preservative film prepared by technique scheme, processing technique is simple.
Detailed description of the invention
Embodiment one, comprises the steps:
(1) step of raw material pulverizing, by the tea grounds 100g through high-temperature water extracted, is placed in baking oven under 110 DEG C of environment drying 2h, size-reduced, and rear mistake 300 mesh sieve makes tea powder standby.
(2) step that cellulose slightly carries, tea powder step (1) produced mixes with the KOH solution that concentration is 0.4mol/L according to the ratio that feed liquid mass ratio is 1:15, and KOH solution is 1500ml, extracts 5h at 45 DEG C, rear filtration, takes filtrate and obtains crude fibre aqueous slkali；The KOH of this concentration extracts and dissolves the hemicellulose that the degree of polymerization is on the low side, if excessive concentration 1mol/L, the hemicellulose degree of polymerization is high, and film forming ability is poor, is just somewhat like cellulose and lignin.
(3) step of hydrolytic lignin, by the crude fibre aqueous slkali obtained by step (2), add acetic acid regulation and make pH to 5, after according to V/V be 100:1 add mass concentration be 0.05% laccase acetum, laccase acetum is 15ml, after in 45 DEG C water-bath 2h, obtain thick hemicellulose solution；Owing to the tea grounds of alkaline extraction removing polyphenol and water soluble ingredient is mainly composed of hemicellulose, lignin and protein (on a small quantity), the Main Function in this step is laccase hydrolytic lignin, controls hydrolysis degree, not complete hydrolysis.
(4) step that molecular retention slightly carries, by thick for step (3) gained half fiber solution by roll-to-roll ultrafiltration filter element, ultrafilter membrane molecular cut off is 25000g/mol, and operation pressure is 100KPa, obtains hemicellulose concentrated solution, about 150ml；The hemicellulose of certain degree of polymerization that screening was processed by previous step and lignin hydrolysing component.
(5) preparing the step of highly branched chain hemicellulose goods, by step (4) gained hemicellulose concentrated solution, adding dehydrated alcohol to ethanol volumetric concentration is 85%, mix homogeneously, stands 12h, and rear filtration or centrifugal, filtering residue is highly branched chain hemicellulose goods, about 1.8g.
(6) step of preservative film solution is prepared, step (5) gained hemicellulose goods are dissolved in the volumetric concentration of 1mg/ml the glycerine water solution of 30%, add the xylitol aqueous solution that mass concentration is 25%, xylitol aqueous solution is 1:6 with the volume ratio of glycerine water solution, rear stirring 30min, and in 55 DEG C of water-baths, cross-linking reaction.
(7) step of preservative film is prepared, by step (6) gained solution according to 0.05g/cm2Pour on smooth metal grinding tool, i.e. obtain edibility hemicellulose preservative film at 100 DEG C of baking 1h.
This product contains a certain amount of low molecule hydrolysate with laccase hydrolytic lignin and by ultrafiltration and the high concentration of alcohol inferior tea hemicellulose that obtains of precipitation, side chain is more, possess good film property, antioxygen penetration and the ability of deadening microorganism, after adding plasticizer, it is possible to promote tensile stress and moisture protection；Having resistance to mechanical ability height, the oil resistance strong, waterproof of antioxygen penetration, the feature such as high temperature resistant and degradable by edibility half fiber preservative film prepared by technique scheme, processing technique is simple.
Embodiment two, comprises the steps of:
(1) by the tea grounds through high-temperature water extracted, under 100 DEG C～120 DEG C of environment, 2h is dried, size-reduced, rear mistake 200～300 mesh sieve, make tea powder.
(2) tea powder that step (1) is produced is mixed with the KOH solution that concentration is 0.4mol/L～0.5mol/L according to the ratio that feed liquid mass ratio is 1:15, extract 5h at 45 DEG C～50 DEG C, filter afterwards, take filtrate and obtain crude fibre aqueous slkali；The KOH of this concentration extracts and dissolves the hemicellulose that the degree of polymerization is on the low side, if excessive concentration 1mol/L, the hemicellulose degree of polymerization is high, and film forming ability is poor, is just somewhat like cellulose and lignin.
(3) by the crude fibre aqueous slkali obtained by step (2), add acetic acid regulation make pH between 4.8～5.5, after according to V/V be 100:1 add mass concentration be 0.02%～0.1% laccase acetum, at 45 DEG C be incubated 2h, obtain thick hemicellulose solution；Owing to the tea grounds of alkaline extraction removing polyphenol and water soluble ingredient is mainly composed of hemicellulose, lignin and protein (on a small quantity), the Main Function in this step is laccase hydrolytic lignin, controls hydrolysis degree, not complete hydrolysis.
(4) by thick for step (3) gained half fiber solution by roll-to-roll ultrafiltration filter element, ultrafilter membrane molecular cut off is 3000g/mol～50000g/mol, and operation pressure is 100KPa, obtains hemicellulose concentrated solution；The hemicellulose of certain degree of polymerization that screening was processed by previous step and lignin hydrolysing component.
(5) by step (4) gained hemicellulose concentrated solution, adding dehydrated alcohol to concentration of alcohol is 80%～90%, mix homogeneously, stands 12h, and rear filtration or centrifugal, filtering residue is highly branched chain hemicellulose goods.
(6) step (5) gained hemicellulose goods are dissolved in the concentration of 0.5mg/ml～2mg/ml the glycerine water solution of 30%, adding mass concentration is the sorbitol aqueous solution of 25%, sorbitol aqueous solution is 1:6～1:10 with the volume ratio of glycerine water solution, rear stirring 30min～45min, and carry out cross-linking reaction in 50 DEG C～60 DEG C.
(7) by step (6) gained solution according to 0.01g/cm2～0.1g/cm2Pour on smooth metal grinding tool, i.e. obtain edibility hemicellulose preservative film at 100 DEG C of baking 1h.
This product contains a certain amount of low molecule hydrolysate with laccase hydrolytic lignin and by ultrafiltration and the high concentration of alcohol inferior tea hemicellulose that obtains of precipitation, side chain is more, possess good film property, antioxygen penetration and the ability of deadening microorganism, after adding plasticizer, it is possible to promote tensile stress and moisture protection；Having resistance to mechanical ability height, the oil resistance strong, waterproof of antioxygen penetration, the feature such as high temperature resistant and degradable by edibility half fiber preservative film prepared by technique scheme, processing technique is simple.
Embodiment three, comprises the steps:
(1) step of raw material pulverizing, by the tea grounds 100g through high-temperature water extracted, is placed in baking oven under 110 DEG C of environment drying 2h, size-reduced, and rear mistake 250 mesh sieve makes tea powder standby.
(2) step that cellulose slightly carries, tea powder step (1) produced mixes with the KOH solution that concentration is 0.5mol/L according to the ratio that feed liquid mass ratio is 1:15, and KOH solution is 1500ml, extracts 5h at 45 DEG C, rear filtration, takes filtrate and obtains crude fibre aqueous slkali；The KOH of this concentration extracts and dissolves the hemicellulose that the degree of polymerization is on the low side, if excessive concentration 1mol/L, the hemicellulose degree of polymerization is high, and film forming ability is poor, is just somewhat like cellulose and lignin.
(3) step of hydrolytic lignin, by the crude fibre aqueous slkali obtained by step (2), add acetic acid regulation and make pH to 5.5, after according to V/V be 100:1 add mass concentration be 0.1% laccase acetum, laccase acetum is 15ml, this enzymatic solution pH is 5.5, after in 45 DEG C water-bath 2h, obtain thick hemicellulose solution；Owing to the tea grounds of alkaline extraction removing polyphenol and water soluble ingredient is mainly composed of hemicellulose, lignin and protein (on a small quantity), the Main Function in this step is laccase hydrolytic lignin, controls hydrolysis degree, not complete hydrolysis.
(4) step that molecular retention slightly carries, by thick for step (3) gained half fiber solution by roll-to-roll ultrafiltration filter element, ultrafilter membrane molecular cut off is 3000g/mol～20000g/mol, and operation pressure is 100KPa, obtains hemicellulose concentrated solution, about 150ml；The hemicellulose of certain degree of polymerization that screening was processed by previous step and lignin hydrolysing component.
(5) preparing the step of highly branched chain hemicellulose goods, by step (4) gained hemicellulose concentrated solution, adding dehydrated alcohol to concentration of alcohol is 85%, mix homogeneously, stands 12h, and rear filtration or centrifugal, filtering residue is highly branched chain hemicellulose goods, about 1.8g.
(6) step of preservative film solution is prepared, step (5) gained hemicellulose goods are dissolved in the concentration of 1mg/ml the glycerine water solution of 30%, adding mass concentration is the Osmitrol of 25%, Osmitrol is 1:10 with the volume ratio of glycerine water solution, rear stirring 30min, and in 55 DEG C of water-baths, cross-linking reaction.
(7) step of preservative film is prepared, by step (6) gained solution according to 0.05g/cm2Pour on smooth metal grinding tool, i.e. obtain edibility hemicellulose preservative film at 100 DEG C of baking 1h.
This product contains a certain amount of low molecule hydrolysate with laccase hydrolytic lignin and by ultrafiltration and the high concentration of alcohol inferior tea hemicellulose that obtains of precipitation, side chain is more, possess good film property, antioxygen penetration and the ability of deadening microorganism, after adding plasticizer, it is possible to promote tensile stress and moisture protection；Having resistance to mechanical ability height, the oil resistance strong, waterproof of antioxygen penetration, the feature such as high temperature resistant and degradable by edibility half fiber preservative film prepared by technique scheme, processing technique is simple.
The ultimate principle of the present invention, principal character and advantages of the present invention have more than been shown and described.Skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; the principle that the present invention is simply described described in above-described embodiment and description; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements both fall within scope of the claimed invention.Claimed scope is defined by appending claims and equivalent thereof.
Claims (7)
1. the method making preservative film with tea grounds, it is characterised in that comprise the steps:
(1) by the tea grounds through high-temperature water extracted, under 100 DEG C～120 DEG C of environment, dry 2h, cross 200～300 mesh sieves after crushed, make tea powder；
(2) tea powder that step (1) is produced is mixed with the KOH solution that concentration is 0.4～0.5mol/L according to the ratio that feed liquid mass ratio is 1:15, extract 5h at 45 DEG C～50 DEG C, filter afterwards, take filtrate and obtain crude fibre aqueous slkali；
(3) by the crude fibre aqueous slkali obtained by step (2), add acetic acid regulation make pH between 4.8～5.5, after according to V/V be 100:1 add mass concentration be 0.02%～0.1% laccase acetum, at 45 DEG C be incubated 2h, obtain thick hemicellulose solution；
(4) by thick for step (3) gained half fiber solution by roll-to-roll ultrafiltration filter element, ultrafilter membrane molecular cut off is 3000g/mol～50000g/mol, and operation pressure is 100KPa, obtains hemicellulose concentrated solution；
(5) by step (4) gained hemicellulose concentrated solution, adding dehydrated alcohol to concentration of alcohol is 80%～90%, mix homogeneously, stands 12h, and rear filtration or centrifugal, filtering residue is highly branched chain hemicellulose goods；
(6) step (5) gained hemicellulose goods are dissolved in the concentration of 0.5mg/ml～2mg/ml the glycerine water solution of 30%, add the edibility plasticizer aqueous solution that mass concentration is 5%～30%, edibility plasticizer aqueous solution is 1:6～1:10 with the volume ratio of glycerine water solution, rear stirring 30min～45min, and carry out cross-linking reaction in 50 DEG C～60 DEG C；
(7) by step (6) gained solution according to 0.01g/cm2～0.1g/cm2Pour on smooth metal grinding tool, i.e. obtain edibility hemicellulose preservative film at 100 DEG C of baking 1h.
Tea grounds the most according to claim 1 makes the method for preservative film, it is characterised in that: in step (2), the concentration of KOH is 0.4mol/L.
Tea grounds the most according to claim 1 makes the method for preservative film, it is characterised in that: in step (3), the mass concentration of laccase acetum is 0.05%.
Tea grounds the most according to claim 1 makes the method for preservative film, it is characterised in that: in step (4), ultrafilter membrane molecular cut off is 25000g/mol.
Tea grounds the most according to claim 1 makes the method for preservative film, it is characterised in that: in step (6), the mass concentration of edibility plasticizer is 25%.
Tea grounds the most according to claim 1 makes the method for preservative film, it is characterised in that: in step (7), gained solution is according to 0.05g/cm2Pour on smooth metal grinding tool.
Tea grounds the most according to claim 1 makes the method for preservative film, it is characterised in that: the edibility plasticizer described in step (6) is xylitol or sorbitol or mannitol.
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| CN201410324790.9A CN104059239B (en) | 2014-07-09 | A kind of tea grounds makes the method for preservative film |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410324790.9A CN104059239B (en) | 2014-07-09 | A kind of tea grounds makes the method for preservative film |
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| CN104059239A CN104059239A (en) | 2014-09-24 |
| CN104059239B true CN104059239B (en) | 2016-11-30 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5817381A (en) * | 1996-11-13 | 1998-10-06 | Agricultural Utilization Research Institute | Cellulose fiber based compositions and film and the process for their manufacture |
| CN1761703A (en) * | 2003-03-21 | 2006-04-19 | 西洛芬股份公司 | Polymeric film or coating comprising hemicellulose |
| CN102850470A (en) * | 2012-10-08 | 2013-01-02 | 江南大学 | Method for separating and purifying water-soluble hemicellulose from green tea leaves |
| CN103275358A (en) * | 2013-05-20 | 2013-09-04 | 吉林大学 | Method for preparing chitosan-based composite preservative film or coating |
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5817381A (en) * | 1996-11-13 | 1998-10-06 | Agricultural Utilization Research Institute | Cellulose fiber based compositions and film and the process for their manufacture |
| CN1761703A (en) * | 2003-03-21 | 2006-04-19 | 西洛芬股份公司 | Polymeric film or coating comprising hemicellulose |
| CN102850470A (en) * | 2012-10-08 | 2013-01-02 | 江南大学 | Method for separating and purifying water-soluble hemicellulose from green tea leaves |
| CN103275358A (en) * | 2013-05-20 | 2013-09-04 | 吉林大学 | Method for preparing chitosan-based composite preservative film or coating |
Non-Patent Citations (1)
| Title |
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| "半纤维素改性制备膜材料";刘光华 等;《纤维素科学与技术》;20090630;第17卷(第2期);第60-68页 * |
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Effective date of registration: 20230704 Address after: 311500 No. 788, baiyunyuan East Road, Tonglu Economic Development Zone, Hangzhou, Zhejiang Patentee after: Zhejiang yifutang Tea Industry Co.,Ltd. Address before: 310052 Floor 2, Building 1, No. 351, Changhe Road, Binjiang District, Hangzhou, Zhejiang Patentee before: HANGZHOU EFUTON TEA Co.,Ltd. |