CN103709256A - Method for preparing hydrogel by modifying tea grounds, and applications of hydrogel - Google Patents
Method for preparing hydrogel by modifying tea grounds, and applications of hydrogel Download PDFInfo
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Abstract
The invention provides a method for preparing hydrogel by modifying tea grounds, and applications of the hydrogel. The method mainly comprises the preparation steps of: grouping fresh and green tea branches and leaves, fixing, drying and crushing, extracting water-soluble components, filtering and drying, degreasing, decolorizing to obtain green tea grounds for later use; extracting water-insoluble dietary fiber from the green tea grounds by adopting an alkaline chemical method, and pickling to obtain different tendernesses of tea ground cellulose; modifying the tea ground cellulose by using ionic liquid AMIMC1 to prepare different tendernesses of tea ground cellulose hydrogel. The prepared tea ground cellulose hydrogel not only changes tea grounds into valuables, but also can protect the environment; in the preparation process, the best tenderness for performing high-value utilization to the tea grounds can be realized by comparing and discussing the characteristics and applicability of the hydrogel prepared by the different tendernesses of tea ground cellulose. In addition, the applications of the prepared tea ground cellulose hydrogel is primarily discussed, the hydrogel can be used as a medicament release carrier, and provide an entry point for the high-value and deep processing utilization of the tea grounds.
Description
Technical field
The present invention relates to natural fiber hydrogel, be specially a kind of preparation method and application thereof of take the hydrogel that tea grounds is main raw material, belong to environment protection, the high-valued deep processing and utilization of agricultural-food and natural macromolecule modification technology.
Background technology
Nearly ten years, China's tea industry high speed development---within 2009, Chinese tea place cultivated area reaches 1,800,000 hectares, accounts for 45% of the world, and 135.8 ten thousand tons of tea output, account for 1/3 of world's total amount.Cultivated area and the tea yield of China all rank first in the world.Meanwhile, the industry fast developments such as China's tea drink, tea-polyphenol, instant tea, wherein, tea drink becomes the third-largest beverage, is only second to water and soda pop.No matter be the extraction of tea drink, instant tea or tea-polyphenol, all can produce a large amount of discarded tea grounds.Nearly 1.6 hundred million kilograms of the annual tea grounds producing of these tea drink and production of instant tea enterprise, if directly these discarded tea grounds are used as to refuse treatment, have not only wasted the potential resources wherein containing, and have easily caused environmental pollution.Therefore, how to develop the comprehensive utilization of tea grounds, make it to become new type resource and be used, in protection of the environment source utilization ratio, caused concern and the attention of various circles of society.
In tea grounds, dietary fiber content is abundant, take insoluble dietary fibre as main, and the content of insoluble dietary fibre is 14.55%～23.38%, in various kinds of foods in higher level.Alkalescence extraction method is extracted food fibre from tea grounds, is an important channel that rationally utilizes tea grounds.Cellulosic research and utilization, mainly comprise: the research of cellulosic structure, cellulosic pre-treatment, cellulose modified flocculation agent, the cellulose modified sorbent material etc. of preparing prepared.Natural cellulose is resulting novel material after modification, can be widely used in the every field such as medicine, plastics industry.Therefore, the research of cellulose modified method in recent years is more and more subject to scientific research personnel's attention.
Hydrogel is can swelling in water, and keeps large quantity of moisture and undissolved cross-linked polymer.Hydrogel has three-dimensional net structure, in water, can absorb a large amount of moisture swellings, and after swelling, continue to keep its original structure and not dissolved.In biomedicine field, hydrogel can be used as drug release carrier.
The invention provides a kind of tea grounds modification and prepare the method for hydrogel, the tea grounds of the tender degree of difference of take is main raw material, the ionic liquid 1-allyl group-3-Methylimidazole hydrochloride (AMIMCl) of take is properties-correcting agent, makes the tea grounds cellulose aquagel of useful as drug release vehicle.
Summary of the invention
One of object of the present invention is, a kind of method of being prepared by tea grounds modification to hydrogel is provided, and this hydrogel is main raw material by the tea grounds of the tender degree of difference, with ionic liquid AMIMCl modification, makes.
Another object of the present invention is, a kind of application method of tea-leaf water gel is provided, this tea-leaf water gel useful as drug release vehicle.
The present invention is achieved through the following technical solutions above-mentioned purpose.
First, invention utilizes alkali electroless method to extract water insoluble dietary fiber from the tea grounds of the tender degree of difference, with AMIMCl ionic liquid, the tea grounds Mierocrystalline cellulose of the tender degree of difference is carried out to modification, is prepared into cellulose aquagel.
The invention provides a kind of method of being prepared by tea grounds modification to hydrogel, comprise the following steps:
(1) fresh green tea branches and leaves are carried out to steam beating, dry, pulverize, sieve, obtain pretreated tealeaves;
(2) extract the water soluble component in pretreated tealeaves, filter, dry, in degreasing reagent, soaking and stirring is carried out after degreasing, washing, then decolour with decolouring reagent, washing, dries, and obtains degreasing, decolouring green tea slag;
(3) degreasing step (2) being obtained, decolouring green tea slag evenly mix with aqueous sodium hydroxide solution, water-bath, and suction filtration, washing, the green tea slag after obtaining alkali and carrying, the green tea slag after alkali is carried carries out acidolysis, suction filtration, washing, oven dry, obtains tea grounds Mierocrystalline cellulose;
(4) adopt heating-cooling-washing process, tea grounds Mierocrystalline cellulose is mixed with 10～30g modifying agent, heated and stirred is dissolved, obtain tea grounds cellulose colloid sample, after by formed tea grounds cellulose colloid sample cool to room temperature, washing, thoroughly after washing tea grounds cellulose aquagel; Described modifying agent is ionic liquid 1-allyl group-3-Methylimidazole hydrochloride (AMIMCl); The cellulosic consumption of described tea grounds is with 3%～10% of AMIMCl consumption calculating.
In aforesaid method, by fresh green tea branches and leaves according to the tender degree of difference by Tender to being always divided into successively a leaf, two leaves, three leaves, Lao Ye and tea stalk, the described fresh green tea branches and leaves of step (1) are a kind of in a leaf, two leaves, three leaves, Lao Ye, tea stalk, to obtain different tender degree tea grounds, by the tender degree tea grounds of difference, make different tender degree tea grounds Mierocrystalline celluloses, and then make different tender degree tea grounds cellulose aquagels.
In aforesaid method, the water soluble component extracting in pretreated tealeaves described in step (2) is specially: pretreated tealeaves is mixed for 1:20～1:40 in mass ratio with water, in water temperature, be to soak 2～4 times under 70～100 ℃ of conditions, each soak time 10～40min.
In aforesaid method, described in step (2), degreasing reagent is sherwood oil, and the described soaking and stirring time is 1～3 hour; Described decolouring reagent is acetone.
In aforesaid method, described in step (3), aqueous sodium hydroxide solution massfraction is 1%～5%, the solid-liquid ratio of degreasing, decolouring green tea slag and aqueous sodium hydroxide solution is 1:10～1:30g:mL, and the bath temperature of described water-bath is 30～60 ℃, and the water-bath time is 1～2 hour.
In aforesaid method, described in step (3), acidolysis concrete steps are: the green tea slag after alkali is carried mixes by solid-liquid ratio 1:10～1:30g:mL with the vitriol oil, in temperature, are acidolysis 1～2 hour under 40～70 ℃ of conditions.
In aforesaid method, described in step (4), the temperature of stirring and dissolving is 80～150 ℃, and the stirring and dissolving time is 10～20h.
In aforesaid method, described in step (4), the method for washing is: with the ionic liquid in distilled water displacement washing tea grounds cellulose colloid.
Tea grounds cellulose aquagel of the present invention compared with prior art, has the following advantages:
(1) tea grounds cellulose aquagel of the present invention, main raw material used is green tea slag, belongs to waste, is prepared into hydrogel, in protection of the environment, has improved again resource utilization, for the high-valued deep processing and utilization of tea grounds provides point of penetration.
(2) tea grounds cellulose aquagel of the present invention, main raw material used is the prepared green tea slag of the tealeaves different sites Mierocrystalline cellulose that a leaf, two leaves, three leaves, Lao Ye and the tea stalk etc. of And Development of Tea Shoot have different tender degree, due to the demand of variant production in industrial production and technique, there are different demand degree in Tea Processing enterprise to the tealeaves of the tender degree of difference.By contrasting characteristic and the relevance grade of the prepared hydrogel of the tea grounds Mierocrystalline cellulose of different tender degree, can inquire into the tender degree of the best of realizing tea grounds higher value application.
(3) the present invention carries out modification with AMIMCl ionic liquid by the tea grounds Mierocrystalline cellulose of the tender degree of difference, is prepared into tea grounds cellulose aquagel, and the application of tea grounds cellulose aquagel has been carried out to pre-test, and this hydrogel can be used as drug release carrier.
(4) reaction conditions gentleness of the present invention is easy to control, and modification procedure is simple, and processing unit is few, easy handling.
Embodiment
Below in conjunction with embodiment, the present invention is described in more detail:
The balance moisture expansivity (ESR) of addressing in embodiment is to adopt conventional gravimetric analysis method to survey.After this hydrogel is dry, weigh, under room temperature, be soaked in water and swollen reaches after swollen equilibrium state for 3 days, in water, take out sample and with filter paper, dry the surface-moisture of colloid, and weigh.ESR calculates by following formula:
ESR(%)＝(W
s-W
d)/W
d×100
In formula, W
s--the weight of hydrogel under balance swollen state;
W
d--the weight of dried hydrogel before swollen;
The carrying drug ratio of addressing in embodiment and medicine accumulative total release rate are as model drug, for medicine carrying and the releasing research of prepared hydrogel with sodium salicylate (NaSA).Under dried hydrogel room temperature, be soaked in be equipped with the 100mL NaSA aqueous solution (10%, in bottle w/w).For research medicine-delivery power, in medicine carrying process, at interval of certain hour, take out the NaSA aqueous solution in 10mL medicine carrying, adopt ultra-violet and visible spectrophotometer to measure NaSA residue content in solution, meanwhile, in erlenmeyer flask, add the distilled water of equivalent to keep liquor capacity constant.After medicine carrying finishes, take out the sample of medicine carrying, use twice of distilled water flushing oven drying to constant weight.In hydrogel, NaSA carrying drug ratio (%) is according to following Equation for Calculating:
NaSA carrying drug ratio (%)=[(C
o-C
t) V/m] * (4-2)
In formula, C
o--the concentration (w/w) of the NaSA aqueous solution before medicine carrying;
C
t--the concentration of the NaSA aqueous solution (w/w) after the medicine carrying t time;
V--the volume of the NaSA aqueous solution;
The quality of hydrogel before m--medicine carrying;
For drugs release dynamics, medicine carrying hydrogel and 100mL distilled water (as release medium) are placed in 37 ℃ of constant incubator vibration treatment in erlenmeyer flask.In dispose procedure, at interval of certain hour, take out 5mL release medium for determination of drug concentration, meanwhile, in erlenmeyer flask, add the distilled water of equivalent to keep release medium constancy of volume.Medicine accumulative total release rate (%) is according to following Equation for Calculating:
Medicine accumulative total release rate (%)=W
t/ W
total* 100%
In formula, W
t--the amount that during time t, medicine accumulative total discharges;
W
total--the total amount of loading of hydrogel Chinese traditional medicine.
Embodiment 1:
(1) fresh green tea one leaf is carried out to steam beating, dry, pulverize, sieve, obtain pretreated tealeaves;
(2) by pretreated tealeaves and water 1:25,70 ℃ of water temperatures, immersion 2 times in mass ratio, each soak time 10min, extracts water soluble component, filters, and dries.Take sherwood oil as solvent, and soaking and stirring is carried out after degreasing for 1 hour, washing, then with acetone decolouring, wash, dry, obtain degreasing, decolouring green tea slag.
(3) by degreasing, decolouring green tea slag, be that 1%NaOH solution is by solid-liquid ratio 1:10(g:mL with massfraction) mix 30 ℃ of water-baths of constant temperature 1 hour, suction filtration, washing.Again with the vitriol oil by solid-liquid ratio 1:10(g:mL) mix, 40 ℃ of acidolysis of constant temperature 1 hour, suction filtration, washing, dries, and obtains a leaf tea grounds Mierocrystalline cellulose;
(4) adopt heating-cooling-washing process, by 3%(with the calculating of AMIMCl consumption) a leaf tea grounds Mierocrystalline cellulose and 10g AMIMCl stirring and dissolving 10h at 80 ℃.By formed tea grounds cellulose colloid sample cool to room temperature.Then, with the ionic liquid in distilled water displacement washing tea grounds cellulose colloid.Thoroughly, after washing, obtain a leaf tea grounds cellulose aquagel.
(5) a leaf tea grounds cellulose aquagel is measured, balance moisture expansivity is 133.24 ± 8.22%, and balance carrying drug ratio is 12.83%, and drug release rate is 62.7%.
Embodiment 2:
(1) fresh green tea two leaves are carried out to steam beating, dry, pulverize, sieve, obtain pretreated tealeaves;
(2) by pretreated tealeaves and water 1:25,80 ℃ of water temperatures, immersion 2 times in mass ratio, each soak time 15min, extracts water soluble component, filters, and dries.Take sherwood oil as solvent, and soaking and stirring is carried out after degreasing for 1.5 hours, washing, then with acetone decolouring, wash, dry, obtain degreasing, decolouring green tea slag.
(3) by degreasing, decolouring green tea slag, be that 2%NaOH solution is by solid-liquid ratio 1:15(g:mL with massfraction) mix 35 ℃ of water-baths of constant temperature 1.5 hours, suction filtration, washing.Again with the vitriol oil by solid-liquid ratio 1:15(g:mL) mix, 50 ℃ of acidolysis of constant temperature 1 hour, suction filtration, washing, dries, and obtains two leaf tea grounds Mierocrystalline celluloses;
(4) adopt heating-cooling-washing process, by 5%(with the calculating of AMIMCl consumption) two leaf tea grounds Mierocrystalline celluloses and 15g AMIMCl stirring and dissolving 12h at 90 ℃.After heating for dissolving, formed tea grounds cellulose colloid sample cool to room temperature.Then, with the ionic liquid in distilled water displacement washing tea grounds cellulose colloid.Thoroughly, after washing, obtain two leaf tea grounds cellulose aquagels.
(5) two leaf tea grounds cellulose aquagels are measured, balance moisture expansivity is 310.86 ± 4.18%, and balance carrying drug ratio is 13.18%, and drug release rate is 65.0%.
Embodiment 3:
(1) fresh green tea three leaves are carried out to steam beating, dry, pulverize, sieve, obtain pretreated tealeaves;
(2) by pretreated tealeaves and water 1:30,90 ℃ of water temperatures, immersion 3 times in mass ratio, each soak time 20min, extracts water soluble component, filters, and dries.Take sherwood oil as solvent, and soaking and stirring is carried out after degreasing for 1.5 hours, washing, then with acetone decolouring, wash, dry, obtain degreasing, decolouring green tea slag.
(3) by degreasing, decolouring green tea slag, be that 3%NaOH solution is by solid-liquid ratio 1:20(g:mL with massfraction) mix 40 ℃ of water-baths of constant temperature 1.5 hours, suction filtration, washing.Again with the vitriol oil by solid-liquid ratio 1:20(g:mL) mix, 60 ℃ of acidolysis of constant temperature 1 hour, suction filtration, washing, dries, and obtains three-leaf tea slag Mierocrystalline cellulose;
(4) adopt heating-cooling-washing process, by 7%(with the calculating of AMIMCl consumption) three-leaf tea slag Mierocrystalline cellulose and 20g AMIMCl stirring and dissolving 14h at 100 ℃.After heating for dissolving, formed tea grounds cellulose colloid sample cool to room temperature.Then, with the ionic liquid in distilled water displacement washing tea grounds cellulose colloid.Thoroughly, after washing, obtain three-leaf tea slag cellulose aquagel.
(5) three-leaf tea slag cellulose aquagel is measured, balance moisture expansivity is 146.12 ± 3.45%, and balance carrying drug ratio is 14.07%, and drug release rate is 65.5%.
Embodiment 4:
(1) fresh green tea Lao Ye leaf is carried out to steam beating, dry, pulverize, sieve, obtain pretreated tealeaves;
(2) by pretreated tealeaves and water 1:35,100 ℃ of water temperatures, immersion 3 times in mass ratio, each soak time 30min, extracts water soluble component, filters, and dries.Take sherwood oil as solvent, and soaking and stirring is carried out after degreasing for 2 hours, washing, then with acetone decolouring, wash, dry, obtain degreasing, decolouring green tea slag.
(3) by degreasing, decolouring green tea slag, be that 4%NaOH solution is by solid-liquid ratio 1:30(g:mL with massfraction) mix 50 ℃ of water-baths of constant temperature 2 hours, suction filtration, washing.Again with the vitriol oil by solid-liquid ratio 1:25(g:mL) mix, 60 ℃ of acidolysis of constant temperature 2 hours, suction filtration, washing, dries, and obtains Lao Ye tea grounds Mierocrystalline cellulose;
(4) adopt heating-cooling-washing process, by 8%(with the calculating of AMIMCl consumption) Lao Ye tea grounds Mierocrystalline cellulose and 30g AMIMCl stirring and dissolving 18h at 80 ℃.After heating for dissolving, formed tea grounds cellulose colloid sample cool to room temperature.Then, with the ionic liquid in distilled water displacement washing tea grounds cellulose colloid.Thoroughly, after washing, obtain Lao Ye tea grounds cellulose aquagel.
(5) Lao Ye tea grounds cellulose aquagel is measured, balance moisture expansivity is 307.38 ± 35.07%, and balance carrying drug ratio is 14.54%, and drug release rate is 51.5%.
Embodiment 5:
(1) fresh green tea tea stalk is carried out to steam beating, dry, pulverize, sieve, obtain pretreated tealeaves;
(2) by pretreated tealeaves and water 1:40,100 ℃ of water temperatures, immersion 4 times in mass ratio, each soak time 40min, extracts water soluble component, filters, and dries.Take sherwood oil as solvent, and soaking and stirring is carried out after degreasing for 3 hours, washing, then with acetone decolouring, wash, dry, obtain degreasing, decolouring green tea slag.
(3) by degreasing, decolouring green tea slag, be that 5%NaOH solution is by solid-liquid ratio 1:30(g:mL with massfraction) mix 60 ℃ of water-baths of constant temperature 2 hours, suction filtration, washing.Again with the vitriol oil by solid-liquid ratio 1:30(g:mL) mix, 70 ℃ of acidolysis of constant temperature 2 hours, suction filtration, washing, dries, and obtains tea stalk tea grounds Mierocrystalline cellulose;
(4) adopt heating-cooling-washing process, by 10%(with the calculating of AMIMCl consumption) tea stalk tea grounds Mierocrystalline cellulose and 30g AMIMCl stirring and dissolving 20h at 90 ℃.After heating for dissolving, formed tea grounds cellulose colloid sample cool to room temperature.Then, with the ionic liquid in distilled water displacement washing tea grounds cellulose colloid.Thoroughly, after washing, obtain tea stalk tea grounds cellulose aquagel.
(5) tea stalk tea grounds cellulose aquagel is measured, balance moisture expansivity is 217.72 ± 5.73%, and balance carrying drug ratio is 14.90%, and drug release rate is 71.4%.
Claims (9)
1. prepared by tea grounds modification to a method for hydrogel, it is characterized in that, described hydrogel is that main raw material preparation obtains by the tea grounds of the tender degree of difference, comprises the following steps:
(1) fresh green tea branches and leaves are carried out to steam beating, dry, pulverize, sieve, obtain pretreated tealeaves;
(2) extract the water soluble component in pretreated tealeaves, filter, dry, in degreasing reagent, soaking and stirring is carried out after degreasing, washing, then decolour with decolouring reagent, washing, dries, and obtains degreasing, decolouring green tea slag;
(3) degreasing step (2) being obtained, decolouring green tea slag evenly mix with aqueous sodium hydroxide solution, water-bath, and suction filtration, washing, the green tea slag after obtaining alkali and carrying, the green tea slag after alkali is carried carries out acidolysis, suction filtration, washing, oven dry, obtains tea grounds Mierocrystalline cellulose;
(4) adopt heating-cooling-washing process, tea grounds Mierocrystalline cellulose is mixed with 10～30g modifying agent, heated and stirred is dissolved, obtain tea grounds cellulose colloid sample, after by formed tea grounds cellulose colloid sample cool to room temperature, washing, thoroughly after washing tea grounds cellulose aquagel; Described modifying agent is ionic liquid 1-allyl group-3-Methylimidazole hydrochloride (AMIMCl); The cellulosic consumption of described tea grounds is with 3%～10% of AMIMCl consumption calculating.
2. a kind of method of being prepared by tea grounds modification to hydrogel according to claim 1, it is characterized in that, by fresh green tea branches and leaves according to the tender degree of difference by Tender to being always divided into successively a leaf, two leaves, three leaves, Lao Ye and tea stalk, the described fresh green tea branches and leaves of step (1) are a kind of in a leaf, two leaves, three leaves, Lao Ye, tea stalk, to obtain different tender degree tea grounds, by the tender degree tea grounds of difference, make different tender degree tea grounds Mierocrystalline celluloses, and then make different tender degree tea grounds cellulose aquagels.
3. a kind of method of being prepared by tea grounds modification to hydrogel according to claim 1, it is characterized in that, the water soluble component extracting in pretreated tealeaves described in step (2) is specially: pretreated tealeaves is mixed for 1:20～1:40 in mass ratio with water, in water temperature, be to soak 2～4 times under 70～100 ℃ of conditions, each soak time 10～40min.
4. a kind of method of being prepared by tea grounds modification to hydrogel according to claim 1, is characterized in that, described in step (2), degreasing reagent is sherwood oil, and the described soaking and stirring time is 1～3 hour; Described decolouring reagent is acetone.
5. a kind of method of being prepared by tea grounds modification to hydrogel according to claim 1, it is characterized in that, described in step (3), aqueous sodium hydroxide solution massfraction is 1%～5%, the solid-liquid ratio of degreasing, decolouring green tea slag and aqueous sodium hydroxide solution is 1:10～1:30g:mL, the bath temperature of described water-bath is 30～60 ℃, and the water-bath time is 1～2 hour.
6. a kind of method of being prepared by tea grounds modification to hydrogel according to claim 1, it is characterized in that, described in step (3), acidolysis concrete steps are: the green tea slag after alkali is carried mixes by solid-liquid ratio 1:10～1:30g:mL with the vitriol oil, in temperature, are acidolysis 1～2 hour under 40～70 ℃ of conditions.
7. a kind of method of being prepared by tea grounds modification to hydrogel according to claim 1, is characterized in that, described in step (4), the temperature of stirring and dissolving is 80～150 ℃, and the stirring and dissolving time is 10～20h.
8. a kind of method of being prepared by tea grounds modification to hydrogel according to claim 1, is characterized in that, described in step (4), the method for washing is: with the ionic liquid in distilled water displacement washing tea grounds cellulose colloid.
9. by claimed in claim 1, a kind of tea grounds modification is prepared to a kind of natural tea grounds cellulose aquagel that the method for hydrogel makes as the application of drug release carrier.
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| CN111109599A (en) * | 2018-10-31 | 2020-05-08 | 株式会社爱茉莉太平洋 | Granular composition comprising dietary fiber derived from green tea and method for preparing the same |
| CN110813263A (en) * | 2019-11-27 | 2020-02-21 | 中国海洋大学 | Biomass-based hydrogel adsorbent for immobilized yeast and preparation method and application thereof |
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| CN113317540B (en) * | 2020-02-28 | 2024-02-09 | 株式会社爱茉莉太平洋 | Granular composition comprising sugar alcohol and method for preparing same |
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| CN116676799A (en) * | 2023-06-29 | 2023-09-01 | 广东食品药品职业学院 | Preparation method and application of apocynum cellulose |
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