CN104059239A - Method for producing preservative film by using used tea leaves - Google Patents
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- CN104059239A CN104059239A CN201410324790.9A CN201410324790A CN104059239A CN 104059239 A CN104059239 A CN 104059239A CN 201410324790 A CN201410324790 A CN 201410324790A CN 104059239 A CN104059239 A CN 104059239A
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Abstract
The invention relates to a method for preparing an edible preservative film by using used tea leaves as the raw material and the method comprises the following steps of preparing low-molecular weight hemicellulose through alkaline liquor extraction, laccase hydrolysis and ultrafiltration purification,and adding a little plasticizing agent on the basis of the cellulose to prepare the edible preservative film. The method specifically comprises the following steps: dissolving the alkaline soluble hemicellulose in the used tea leaves by use of low-concentration alkaline liquor (0.4-0.5mol/L), regulating the pH value and hydrolyzing lignin in the solution by use of laccase having the concentration of 0.02%-0.1%, concentrating by use of an ultrafiltration membrane having the molecular weight cut-off of 3000-50000g/mol, precipitating the hemicellulose by using ethanol having a high concentration (80%-90%), thus obtaining the hemicellulose, wherein the yield is between 1% and 2%; and finally, preparing the preservative film by use of the hemicellulose and plasticizers such as xylitol, sorbitol, mannitol and glycerin. The method is simple in process; the obtained preservative film has the characteristics of high mechanical resistance, high oxygen permeation resistance, water/oil resistance, high temperature resistance, easy degradability and the like.
Description
Technical field
The present invention relates to a kind of method of making preservative film of tea grounds, belong to food-processing and preservation technique field.
Background technology
Renewable lignocellulose resource is one of effective way solving the day by day exhausted and environmental problem of petrochemical industry resource.Hemicellulose is extensively present in the fine cell wall of plant, and the alkali-soluble polysaccharide that to be a class be polymerized by the glycosyl of non-glucose, mainly plays the effect that connects Mierocrystalline cellulose and xylogen, occupies 20%~35% of cell walls gross weight.
Hemicellulose complex structure, glycosyl units is of a great variety, common are D-wood sugar, L-arabinose, D-semi-lactosi, D-MANNOSE etc., the hemicellulose in natural phant source, a large amount of production for sugar industry Raw, as Xylitol, semi-lactosi etc.The structure of hemicellulose sugar unit and the diversity of composition, determined the physics and chemistry attribute plasticity-of hemicellulose, as the hemicellulose in wheat balloonflower root possesses good binding property and film forming ability.Plant hemicellulose is a kind of edible raw material of renewable, easy degraded, generally possesses the ability that good resistance oxygen, water and macromole have free passage, and therefore can use the huge application prospect existing on preservative film.
Tea grounds is still used as a kind of waste resource processing in China, reaches 1.6 ten thousand tons every year from the discarded tea grounds of tea drink and production of instant tea producer.Tea grounds after water extraction is processed, content of cellulose is abundant, accounts for 14.55%~23.38% of tea grounds dry weight, and the content of hemicellulose approximately 6%~16% is the desirable feedstock of obtaining edible hemicellulose.
In tea grounds, the composition of hemicellulose sugar unit is relatively simple, comprises glucose sugar, semi-lactosi, pectinose, wood sugar, rhamnosyl, galacturonic acid and galn, and wherein semi-lactosi, pectinose and glucose sugar occupy 82.2% of glycosyl total amount.The same with other plant class half fiber, tea-leaf dietary fiber possesses good water holding, holds the performance of perfume (or spice) and isolated microorganism, but film-forming properties is poor separately.
On existing market, popular Perserving materials great majority are still the plastics such as polyethylene (PE), polyvinyl chloride (PVC), polyvinylidene dichloride (PVDC), except deriving from non-degradable material, under certain ambient condition, as microwave, refrigerator, baking etc. also have chemical transformation and objectionable impurities to the infiltration in food, thereby be detrimental to health.
Protein, polysaccharide, lipid acid and resene etc. can by self group or the intermolecular interaction of foreign aid forms the film that possesses a fixed structure and effect, therefore, is also the main source of edible material.China Patent Publication No.: " CN 102850562 A " disclose a kind of casein food grade and glycerine of utilizing in milk by dry edible and the easy method of degraded preservative film prepared, casein food grade film-forming process is simple, fresh-keeping effect is comparatively remarkable, but the source that faces casein food grade is comparatively limited, the problems such as price is high, and film forming ductility is poor.China Patent Publication No.: " CN 102850470 A " disclose a kind of alkaline hydrogen peroxide method that utilizes from the method for tea grounds separating high-purity tea grounds half fiber, yet utilized H
2o
2the xylogen that can not go out preferably in tea grounds, must be through comparatively loaded down with trivial details macroporous resin ethanol gradient elution except colour purity, and this method object is at the hemicellulose that is only to prepare higher degree from tea grounds.
Summary of the invention
The object of the present invention is to provide and a kind ofly from tea grounds, extract hemicellulose, and take that it prepares the method for the food fresh keeping membrane of edibility as main 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 method of making preservative film of tea grounds, it is characterized in that, and comprise the steps:
(1) by the tea grounds through high-temperature water extracted, 100
oc~120
oCunder environment, dry 2h, through pulverizing, rear mistake 200~300 mesh sieves, make tea powder.
(2) the KOH solution that the ratio that the tea powder of step (1) being produced is 1:15 according to feed liquid mass ratio is 0.4~0.5mol/L with concentration mixes, 45~50
oc extracts 5h, and rear filtration is got filtrate and obtained crude fibre alkaline solution; The KOH of this concentration extracts solvent polymerization degree hemicellulose on the low side, if excessive concentration 1mol/L, the hemicellulose polymerization degree is high, and film forming ability tea, just a little as Mierocrystalline cellulose and xylogen.
(3) by the resulting crude fibre alkaline solution of step (2), add acetic acid to regulate and make pH between 4.8~5.5, according to V/V, be in 100:1 and the mass concentration laccase acetum that is 0.02%~0.1%, in 45
ounder C, be incubated 2h, obtain thick hemicellulose solution; The tea grounds main component of removing polyphenol and water soluble component due to alkaline extraction is hemicellulose, xylogen and protein (on a small quantity), and the Main Function in this step is laccase hydrolytic lignin, controlled hydrolysis degree, not complete hydrolysis.
(4) thick half fiber solution of step (3) gained is passed through to spiral wound filter core, ultra-filtration membrane throttling molecular weight is 3000~50000g/mol, and working pressure is 100Kpa, obtains hemicellulose concentrated solution; The hemicellulose of certain polymerization degree that screening is crossed by preorder step process and xylogen hydrolysing component.
(5) by step (4) gained hemicellulose concentrated solution, adding dehydrated alcohol to alcohol concn is 80%~90%, mix, and static 12h, rear filtration or centrifugal, filter residue is higly branched chain hemicellulose goods.
(6) step (5) gained hemicellulose goods are dissolved in to 30% aqueous glycerin solution with the concentration of 0.5-2mg/ml, adding mass concentration is 5%~30% edibility softening agent, the volume ratio of softening agent and aqueous glycerin solution is 1:6-1:10, rear stirring 30~45min, and in 50~60
oc carries out crosslinking reaction.
(7) by step (6) gained solution according to 0.01~0.1g/cm
2build on smooth metal grinding tool, 100
oc baking 1h obtains edibility hemicellulose preservative film.
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), ultra-filtration membrane throttling molecular weight is 25000g/mol.
As preferably, in step (6), the mass concentration of softening agent is 25%.
As preferably, in step (7), gained solution is according to 0.05g/cm
2build on smooth metal grinding tool.
As preferably, the edibility softening agent described in step (6) is Xylitol or sorbyl alcohol or N.F,USP MANNITOL.
The alkaline solution that concentration is lower can access the more hemicellulose of side chain, molecular weight is relatively little, film-forming properties is high, and the alkali of high density can increase the dissolving power of straight chain hemicellulose, laccase is oxidized to the phenol unit of xylogen phenoxy group and loses crosslinked ability, the xylogen of the partially stabilized form of degrading.
Beneficial effect of the present invention is: this product contains a certain amount of low molecule hydrolyzate with laccase hydrolytic lignin the thick tea hemicellulose that obtains by ultrafiltration and high alcohol concn precipitation, side chain is more, the ability that possesses good film-forming properties, antioxygen seepage force and deadening microorganism, after adding softening agent, can promote tensile stress and moistureproof ability; The features such as the edibility half fiber preservative film tool anti-machine capability prepared by technique scheme is high, antioxygen seepage force is strong, waterproof oil resistance, high temperature resistant and easy degraded, complete processing is simple.
Embodiment
Embodiment mono-, comprises the steps:
(1) step of raw material pulverizing, the tea grounds 100g by through high-temperature water extracted, is placed in baking oven 110
ounder C environment, dry 2h, through pulverizing, rear mistake 300 mesh sieves, make tea powder standby.
(2) step that Mierocrystalline cellulose is slightly carried, the KOH solution that the ratio that the tea powder that step (1) is produced is 1:15 according to feed liquid mass ratio is 0.4mol/L with concentration mixes, and KOH solution is 1500ml, 45
oc extracts 5h, and rear filtration is got filtrate and obtained crude fibre alkaline solution; The KOH of this concentration extracts solvent polymerization degree hemicellulose on the low side, if excessive concentration 1mol/L, the hemicellulose polymerization degree is high, and film forming ability tea, just a little as Mierocrystalline cellulose and xylogen.
(3) step of hydrolytic lignin, by the resulting crude fibre alkaline solution of step (2), adds acetic acid to regulate to make pH to 5, according to V/V, is that in 100:1 and the mass concentration laccase acetum that is 0.05%, laccase acetum is 15ml, after in 45
owater-bath 2h in C, obtains thick hemicellulose solution; The tea grounds main component of removing polyphenol and water soluble component due to alkaline extraction is hemicellulose, xylogen and protein (on a small quantity), and the Main Function in this step is laccase hydrolytic lignin, controlled hydrolysis degree, not complete hydrolysis.
(4) step that molecular retention is slightly carried, by thick half fiber solution of step (3) gained, by spiral wound filter core, ultra-filtration membrane throttling molecular weight is 25000g/mol, working pressure is 100Kpa, obtains hemicellulose concentrated solution, about 150ml; The hemicellulose of certain polymerization degree that screening is crossed by preorder step process and xylogen hydrolysing component.
(5) prepare the step of higly branched chain hemicellulose goods, by step (4) gained hemicellulose concentrated solution, adding dehydrated alcohol to ethanol volumetric concentration is 85%, mix static 12h, rear filtration or centrifugal, filter residue is higly branched chain hemicellulose goods, about 1.8g.
(6) prepare the step of preservative film solution, step (5) gained hemicellulose goods are dissolved in to 30% aqueous glycerin solution with the volumetric concentration of 1mg/ml, and adding mass concentration is 20% Xylitol, and the volume ratio of softening agent and aqueous glycerin solution is 1:6, rear stirring 30min, and in 55
oc water-bath, crosslinking reaction.
(7) prepare the step of preservative film, by step (6) gained solution according to 0.05g/cm
2build on smooth metal grinding tool, 100
oc baking 1h obtains edibility hemicellulose preservative film.
This product contains a certain amount of low molecule hydrolyzate with laccase hydrolytic lignin the thick tea hemicellulose that obtains by ultrafiltration and high alcohol concn precipitation, side chain is more, the ability that possesses good film-forming properties, antioxygen seepage force and deadening microorganism, after adding softening agent, can promote tensile stress and moistureproof ability; The features such as the edibility half fiber preservative film tool anti-machine capability prepared by technique scheme is high, antioxygen seepage force is strong, waterproof oil resistance, high temperature resistant and easy degraded, complete processing is simple.
Embodiment bis-, following steps, consist of:
(1) by the tea grounds through high-temperature water extracted, 100
oc~120
oCunder environment, dry 2h, through pulverizing, rear mistake 200~300 mesh sieves, make tea powder.
(2) the KOH solution that the ratio that the tea powder of step (1) being produced is 1:15 according to feed liquid mass ratio is 0.4~0.5mol/L with concentration mixes, 45~50
oc extracts 5h, and rear filtration is got filtrate and obtained crude fibre alkaline solution; The KOH of this concentration extracts solvent polymerization degree hemicellulose on the low side, if excessive concentration 1mol/L, the hemicellulose polymerization degree is high, and film forming ability tea, just a little as Mierocrystalline cellulose and xylogen.
(3) by the resulting crude fibre alkaline solution of step (2), add acetic acid to regulate and make pH between 4.8~5.5, according to V/V, be in 100:1 and the mass concentration laccase acetum that is 0.02%~0.1%, in 45
ounder C, be incubated 2h, obtain thick hemicellulose solution; The tea grounds main component of removing polyphenol and water soluble component due to alkaline extraction is hemicellulose, xylogen and protein (on a small quantity), and the Main Function in this step is laccase hydrolytic lignin, controlled hydrolysis degree, not complete hydrolysis.
(4) thick half fiber solution of step (3) gained is passed through to spiral wound filter core, ultra-filtration membrane throttling molecular weight is 3000~50000g/mol, and working pressure is 100Kpa, obtains hemicellulose concentrated solution; The hemicellulose of certain polymerization degree that screening is crossed by preorder step process and xylogen hydrolysing component.
(5) by step (4) gained hemicellulose concentrated solution, adding dehydrated alcohol to alcohol concn is 80%~90%, mix, and static 12h, rear filtration or centrifugal, filter residue is higly branched chain hemicellulose goods.
(6) step (5) gained hemicellulose goods are dissolved in to 30% aqueous glycerin solution with the concentration of 0.5-2mg/ml, adding mass concentration is 5%~30% edibility softening agent, the volume ratio of softening agent and aqueous glycerin solution is 1:6-1:10, rear stirring 30~45min, and in 50~60
oc carries out crosslinking reaction.
(7) by step (6) gained solution according to 0.01~0.1g/cm
2build on smooth metal grinding tool, 100
oc baking 1h obtains edibility hemicellulose preservative film.
This product contains a certain amount of low molecule hydrolyzate with laccase hydrolytic lignin the thick tea hemicellulose that obtains by ultrafiltration and high alcohol concn precipitation, side chain is more, the ability that possesses good film-forming properties, antioxygen seepage force and deadening microorganism, after adding softening agent, can promote tensile stress and moistureproof ability; The features such as the edibility half fiber preservative film tool anti-machine capability prepared by technique scheme is high, antioxygen seepage force is strong, waterproof oil resistance, high temperature resistant and easy degraded, complete processing is simple.
Embodiment tri-, comprise the steps:
(1) step of raw material pulverizing, the tea grounds 100g by through high-temperature water extracted, is placed in baking oven 110
ounder C environment, dry 2h, through pulverizing, rear mistake 250 mesh sieves, make tea powder standby.
(2) step that Mierocrystalline cellulose is slightly carried, the KOH solution that the ratio that the tea powder that step (1) is produced is 1:15 according to feed liquid mass ratio is 0.5mol/L with concentration mixes, and KOH solution is 1500ml, 45
oc extracts 5h, and rear filtration is got filtrate and obtained crude fibre alkaline solution; The KOH of this concentration extracts solvent polymerization degree hemicellulose on the low side, if excessive concentration 1mol/L, the hemicellulose polymerization degree is high, and film forming ability tea, just a little as Mierocrystalline cellulose and xylogen.
(3) step of hydrolytic lignin, by the resulting crude fibre alkaline solution of step (2), adds acetic acid to regulate and makes pH to 5.5, according to V/V, be in 100:1 and the mass concentration laccase acetum that is 0.1%, laccase acetum is 15ml, and this enzyme solution pH is 5.5, after in 45
owater-bath 2h in C, obtains thick hemicellulose solution; The tea grounds main component of removing polyphenol and water soluble component due to alkaline extraction is hemicellulose, xylogen and protein (on a small quantity), and the Main Function in this step is laccase hydrolytic lignin, controlled hydrolysis degree, not complete hydrolysis.
(4) step that molecular retention is slightly carried, by thick half fiber solution of step (3) gained, by spiral wound filter core, ultra-filtration membrane throttling molecular weight is 3000~20000g/mol, working pressure is 100Kpa, obtains hemicellulose concentrated solution, about 150ml; The hemicellulose of certain polymerization degree that screening is crossed by preorder step process and xylogen hydrolysing component.
(5) prepare the step of higly branched chain hemicellulose goods, by step (4) gained hemicellulose concentrated solution, adding dehydrated alcohol to alcohol concn is 85%, mix, and static 12h, rear filtration or centrifugal, filter residue is higly branched chain hemicellulose goods, about 1.8g.
(6) prepare the step of preservative film solution, step (5) gained hemicellulose goods are dissolved in to 30% aqueous glycerin solution with the concentration of 1mg/ml, and adding mass concentration is 25% N.F,USP MANNITOL, and the volume ratio of softening agent and aqueous glycerin solution is 1:10, rear stirring 30min, and in 55
oc water-bath, crosslinking reaction.
(7) prepare the step of preservative film, by step (6) gained solution according to 0.05g/cm
2build on smooth metal grinding tool, 100
oc baking 1h obtains edibility hemicellulose preservative film.
This product contains a certain amount of low molecule hydrolyzate with laccase hydrolytic lignin the thick tea hemicellulose that obtains by ultrafiltration and high alcohol concn precipitation, side chain is more, the ability that possesses good film-forming properties, antioxygen seepage force and deadening microorganism, after adding softening agent, can promote tensile stress and moistureproof ability; The features such as the edibility half fiber preservative film tool anti-machine capability prepared by technique scheme is high, antioxygen seepage force is strong, waterproof oil resistance, high temperature resistant and easy degraded, complete processing is simple.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; 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 all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (7)
1. of tea grounds, make a method for preservative film, it is characterized in that, comprise the steps:
(1) by the tea grounds through high-temperature water extracted, 100
oc~120
oCunder environment, dry 2h, through pulverizing, rear mistake 200~300 mesh sieves, make tea powder;
(2) the KOH solution that the ratio that the tea powder of step (1) being produced is 1:15 according to feed liquid mass ratio is 0.4~0.5mol/L with concentration mixes, 45~50
oc extracts 5h, and rear filtration is got filtrate and obtained crude fibre alkaline solution;
(3) by the resulting crude fibre alkaline solution of step (2), add acetic acid to regulate and make pH between 4.8~5.5, according to V/V, be in 100:1 and the mass concentration laccase acetum that is 0.02%~0.1%, in 45
ounder C, be incubated 2h, obtain thick hemicellulose solution;
(4) thick half fiber solution of step (3) gained is passed through to spiral wound filter core, ultra-filtration membrane throttling molecular weight is 3000~50000g/mol, and working pressure is 100Kpa, obtains hemicellulose concentrated solution;
(5) by step (4) gained hemicellulose concentrated solution, adding dehydrated alcohol to alcohol concn is 80%~90%, mix, and static 12h, rear filtration or centrifugal, filter residue is higly branched chain hemicellulose goods;
(6) step (5) gained hemicellulose goods are dissolved in to 30% aqueous glycerin solution with the concentration of 0.5-2mg/ml, adding mass concentration is 5%~30% edibility softening agent, the volume ratio of softening agent and aqueous glycerin solution is 1:6-1:10, rear stirring 30~45min, and in 50~60
oc carries out crosslinking reaction;
(7) by step (6) gained solution according to 0.01~0.1g/cm
2build on smooth metal grinding tool, 100
oc baking 1h obtains edibility hemicellulose preservative film.
2. method of making preservative film of tea grounds according to claim 1, is characterized in that: in step (2), the concentration of KOH is 0.4mol/L.
3. method of making preservative film of tea grounds according to claim 1, is characterized in that: in step (3), the mass concentration of laccase acetum is 0.05%.
4. method of making preservative film of tea grounds according to claim 1, is characterized in that: in step (4), ultra-filtration membrane throttling molecular weight is 25000g/mol.
5. method of making preservative film of tea grounds according to claim 1, is characterized in that: in step (6), the mass concentration of softening agent is 25%.
6. method of making preservative film of tea grounds according to claim 1, is characterized in that: in step (7), gained solution is according to 0.05g/cm
2build on smooth metal grinding tool.
7. method of making preservative film of tea grounds according to claim 1, is characterized in that: the softening agent described in step (6) is Xylitol or sorbyl alcohol or N.F,USP 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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CN104059239B CN104059239B (en) | 2016-11-30 |
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Cited By (3)
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---|---|---|---|---|
CN108395724A (en) * | 2018-03-12 | 2018-08-14 | 安徽农业大学 | A kind of preparation method of tea grounds/cellulose preservative film |
CN109293959A (en) * | 2018-09-30 | 2019-02-01 | 安徽农业大学 | Tea grounds modified oxidized cellulose composite membrane and the preparation method and application thereof |
CN109320786A (en) * | 2016-12-11 | 2019-02-12 | 金福珍 | A kind of edible mushroom packaging material |
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JP2000504058A (en) * | 1996-04-09 | 2000-04-04 | イー.カショギ インダストリーズ | Compositions with highly ungelatinized contents |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109320786A (en) * | 2016-12-11 | 2019-02-12 | 金福珍 | A kind of edible mushroom packaging material |
CN108395724A (en) * | 2018-03-12 | 2018-08-14 | 安徽农业大学 | A kind of preparation method of tea grounds/cellulose preservative film |
CN109293959A (en) * | 2018-09-30 | 2019-02-01 | 安徽农业大学 | Tea grounds modified oxidized cellulose composite membrane and the preparation method and application thereof |
CN109293959B (en) * | 2018-09-30 | 2021-07-30 | 安徽农业大学 | Tea-residue-modified oxidized cellulose composite membrane and preparation method and application thereof |
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