CN103709256B - A kind of the method for hydrogel and the application of this hydrogel are prepared in tea grounds modification - Google Patents
A kind of the method for hydrogel and the application of this hydrogel are prepared in tea grounds modification Download PDFInfo
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Abstract
The invention provides and a kind of the method for hydrogel and the application of hydrogel are prepared in tea grounds modification.Main preparation process is: fresh green tea branches and leaves divide into groups, complete, dry, pulverize, then extract water soluble component, filtering drying, degreasing, decolouring, obtain green tea slag for subsequent use.Green tea slag alkali electroless method extracts water insoluble dietary fiber, and pickling, obtains different tenderness tea grounds Mierocrystalline cellulose.With ionic liquid AMIMCl, modification is carried out to tea grounds Mierocrystalline cellulose, prepare the tea grounds cellulose aquagel of different tenderness.Prepared tea grounds cellulose aquagel, not only makes tea grounds turn waste into wealth, and protection of the environment; In preparation process, compared for characteristic and the relevance grade of the hydrogel prepared by tea grounds Mierocrystalline cellulose of different tenderness, inquire into the best tenderness realizing tea grounds higher value application; Meanwhile, carried out pre-test to the application of the tea grounds cellulose aquagel of preparation, this hydrogel can be used as drug release carrier, for the high-valued deep processing and utilization of tea grounds provides point of penetration.
Description
Technical field
The present invention relates to natural fiber hydrogel, being specially a kind of take tea grounds as preparation method and the application thereof of the hydrogel of main raw material, belongs 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 tea output 135.8 ten thousand tons, accounts 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, a large amount of discarded tea grounds all can be produced.The tea grounds that these tea drink and production of instant tea enterprise produce every year reaches 1.6 hundred million kilograms, if directly these discarded tea grounds are used as refuse treatment, not only waste the potential resources wherein contained, and easily causes 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, cause concern and the attention of various circles of society.
In tea grounds, dietary fiber content enriches, and based on insoluble dietary fibre, the content of insoluble dietary fibre is 14.55% ~ 23.38%, in various kinds of foods, be in higher level.Alkalescence extraction method extracts food fibre from tea grounds, is the important channel of an Appropriate application tea grounds.Cellulosic research and utilization, mainly comprise: the research of cellulosic structure, cellulosic pre-treatment, cellulose modifiedly prepare flocculation agent, cellulose modifiedly prepare sorbent material etc.Natural cellulose, through modified obtained novel material, can be widely used in the every field such as medicine, plastics industry.Therefore, the research of cellulose modified method is more and more subject to the attention of scientific research personnel in recent years.
Hydrogel is can be swelling in water, and keeps large quantity of moisture and undissolved cross-linked polymer.Hydrogel has three-dimensional net structure, can absorb a large amount of moisture swelling in water, and continues after swelling keep its original structure and do not dissolved.In biomedicine field, hydrogel can be used as drug release carrier.
The invention provides a kind of method that hydrogel is prepared in tea grounds modification, with the tea grounds of different tenderness for main raw material, with ionic liquid 1-allyl group-3-methylimidazolium chloride (AMIMCl) for properties-correcting agent, the obtained tea grounds cellulose aquagel that can be used as drug release carrier.
Summary of the invention
An object of the present invention is, provides a kind of method hydrogel being prepared by tea grounds modification, and this hydrogel is main raw material by the tea grounds of different tenderness, obtains with ionic liquid AMIMCl modification.
Another object of the present invention is, provides a kind of application method of tea-leaf water gel, and this tea-leaf water gel can be used as drug release carrier.
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 different tenderness, with AMIMCl ionic liquid, the tea grounds Mierocrystalline cellulose of different tenderness is carried out modification, is prepared into cellulose aquagel.
The invention provides a kind of method hydrogel being prepared by tea grounds modification, comprise the following steps:
(1) steam beating is carried out to fresh green tea branches and leaves, dry, pulverize, sieve, obtain pretreated tealeaves;
(2) extract the water soluble component in pretreated tealeaves, filter, dry, after in degreasing agent, soaking and stirring carries out degreasing, washing, then decolour with decolouring reagent, washing, dries, and obtains degreasing, decolouring green tea slag;
(3) degreasing step (2) obtained, decolouring green tea slag and aqueous sodium hydroxide solution Homogeneous phase mixing, water-bath, suction filtration, washing, obtain alkali carry after green tea slag, the green tea slag after being carried by alkali carries out acidolysis, suction filtration, washing, and oven dry, obtains tea grounds Mierocrystalline cellulose;
(4) adopt heating-cooling-washing process, mixed by tea grounds Mierocrystalline cellulose 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-methylimidazolium chloride (AMIMCl); The cellulosic consumption of described tea grounds is with 3% ~ 10% of AMIMCl Dosage calculation.
In aforesaid method, by fresh green tea branches and leaves according to different tenderness by Tender to being always divided into a leaf, two leaves, three leaves, Lao Ye and tea stalk successively, the described fresh green tea branches and leaves of step (1) are the one in a leaf, two leaves, three leaves, Lao Ye, tea stalk, to obtain different tenderness tea grounds, different tenderness tea grounds Mierocrystalline cellulose is obtained by different tenderness tea grounds, and then obtained different tenderness tea grounds cellulose aquagel.
In aforesaid method, described in step (2), the water soluble component extracted in pretreated tealeaves is specially: mixed for 1:20 ~ 1:40 in mass ratio with water by pretreated tealeaves, soak 2 ~ 4 times under water temperature is 70 ~ 100 DEG C of conditions, each soak time 10 ~ 40min.
In aforesaid method, described in step (2), degreasing agent 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, decolour 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 DEG C, and water bath time is 1 ~ 2 hour.
In aforesaid method, described in step (3), acidolysis concrete steps are: the green tea slag after being carried by alkali mixes by solid-liquid ratio 1:10 ~ 1:30g:mL with the vitriol oil, acidolysis 1 ~ 2 hour under temperature is 40 ~ 70 DEG C of conditions.
In aforesaid method, described in step (4), the temperature of stirring and dissolving is 80 ~ 150 DEG C, 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, while protection of the environment, turn improves 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, the green tea slag Mierocrystalline cellulose obtained by tealeaves different sites that main raw material used is a leaf of And Development of Tea Shoot, two leaves, three leaves, Lao Ye and tea stalk etc. have different tenderness, due to the demand of variant production in industrial production and technique, the tealeaves of Tea Processing enterprise to different tenderness has different demand degree.By characteristic and the relevance grade of the hydrogel prepared by the tea grounds Mierocrystalline cellulose that contrasts different tenderness, the best tenderness realizing tea grounds higher value application can be inquired into.
(3) the tea grounds Mierocrystalline cellulose of different tenderness is carried out modification by the present invention AMIMCl ionic liquid, is prepared into tea grounds cellulose aquagel, and carried out pre-test to the application of tea grounds cellulose aquagel, 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) addressed in embodiment adopts conventional gravimetric method to survey.After this hydrogel drying, weigh, to be soaked under room temperature in water and after swollen reaches swollen equilibrium state in 3 days, take out sample in water and dry the surface-moisture of colloid with filter paper, and weighing.ESR is by following formulae discovery:
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 addressed in embodiment and medicine add up release rate, are with sodium salicylate (NaSA) as model drug, for medicine carrying and the releasing research of prepared hydrogel.Be soaked in the bottle that the 100mLNaSA aqueous solution (10%, w/w) is housed under dried hydrogel room temperature.For research medicine-delivery power, in drug incorporation, take out the NaSA aqueous solution in 10mL medicine carrying at interval of certain hour, adopt ultra-violet and visible spectrophotometer to measure NaSA in solution and remain content, meanwhile, in erlenmeyer flask, the distilled water of equivalent is added to keep liquor capacity constant.After medicine carrying terminates, take out the sample of medicine carrying, with distilled water flushing twice and 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 (w/w) of the NaSA aqueous solution after the medicine carrying t time;
V--the volume of the NaSA aqueous solution;
M--the quality of hydrogel before medicine carrying;
For drugs release dynamics, medicine carrying hydrogel and 100mL distilled water (as release medium) are placed in 37 DEG C of constant incubator vibration treatment in erlenmeyer flask.In dispose procedure, take out 5mL release medium at interval of certain hour and be used for determination of drug concentration, meanwhile, add the distilled water of equivalent in erlenmeyer flask to keep release medium constancy of volume.Medicine adds up release rate (%) according to following Equation for Calculating:
Medicine adds up release rate (%)=W
t/ W
total× 100%
In formula, W
t--during time t, medicine adds up the amount discharged;
W
total--the amount that hydrogel Chinese traditional medicine always loads.
Embodiment 1:
(1) fresh green tea one leaf is carried out steam beating, dry, pulverize, sieve, obtain pretreated tealeaves;
(2) by pretreated tealeaves and water in mass ratio 1:25, water temperature 70 DEG C, soak 2 times, each soak time 10min, extract water soluble component, filter, dry.Take sherwood oil as solvent, after soaking and stirring carries out degreasing in 1 hour, washing, then with acetone decolouring, wash, dry, obtain degreasing, decolouring green tea slag.
(3) be that 1%NaOH solution is by solid-liquid ratio 1:10(g:mL by degreasing, decolouring green tea slag with massfraction) mix, constant temperature 30 DEG C of water-baths 1 hour, suction filtration, wash.Again with the vitriol oil by solid-liquid ratio 1:10(g:mL) mix, constant temperature 40 DEG C of acidolysis 1 hour, suction filtration, washing, dry, obtain a leaf tea grounds Mierocrystalline cellulose;
(4) adopt heating-cooling-washing process, by 3%(with AMIMCl Dosage calculation) a leaf tea grounds Mierocrystalline cellulose and 10gAMIMCl stirring and dissolving 10h at 80 DEG C.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.After thorough washing, obtain a leaf tea grounds cellulose aquagel.
(5) measure a leaf tea grounds cellulose aquagel, 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 leaf is carried out steam beating, dry, pulverize, sieve, obtain pretreated tealeaves;
(2) by pretreated tealeaves and water in mass ratio 1:25, water temperature 80 DEG C, soak 2 times, each soak time 15min, extract water soluble component, filter, dry.Take sherwood oil as solvent, after soaking and stirring carries out degreasing in 1.5 hours, washing, then with acetone decolouring, wash, dry, obtain degreasing, decolouring green tea slag.
(3) be that 2%NaOH solution is by solid-liquid ratio 1:15(g:mL by degreasing, decolouring green tea slag with massfraction) mix, constant temperature 35 DEG C of water-baths 1.5 hours, suction filtration, wash.Again with the vitriol oil by solid-liquid ratio 1:15(g:mL) mix, constant temperature 50 DEG C of acidolysis 1 hour, suction filtration, washing, dry, obtain two leaf tea grounds Mierocrystalline celluloses;
(4) adopt heating-cooling-washing process, by 5%(with AMIMCl Dosage calculation) two leaf tea grounds Mierocrystalline celluloses and 15gAMIMCl stirring and dissolving 12h at 90 DEG C.After heating for dissolving, the tea grounds cellulose colloid sample cool to room temperature formed.Then, with the ionic liquid in distilled water displacement washing tea grounds cellulose colloid.After thorough washing, obtain two leaf tea grounds cellulose aquagels.
(5) measure two leaf tea grounds cellulose aquagels, 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 leaf is carried out steam beating, dry, pulverize, sieve, obtain pretreated tealeaves;
(2) by pretreated tealeaves and water in mass ratio 1:30, water temperature 90 DEG C, soak 3 times, each soak time 20min, extract water soluble component, filter, dry.Take sherwood oil as solvent, after soaking and stirring carries out degreasing in 1.5 hours, washing, then with acetone decolouring, wash, dry, obtain degreasing, decolouring green tea slag.
(3) be that 3%NaOH solution is by solid-liquid ratio 1:20(g:mL by degreasing, decolouring green tea slag with massfraction) mix, constant temperature 40 DEG C of water-baths 1.5 hours, suction filtration, wash.Again with the vitriol oil by solid-liquid ratio 1:20(g:mL) mix, constant temperature 60 DEG C of acidolysis 1 hour, suction filtration, washing, dry, obtain three-leaf tea slag Mierocrystalline cellulose;
(4) adopt heating-cooling-washing process, by 7%(with AMIMCl Dosage calculation) three-leaf tea slag Mierocrystalline cellulose and 20gAMIMCl stirring and dissolving 14h at 100 DEG C.After heating for dissolving, the tea grounds cellulose colloid sample cool to room temperature formed.Then, with the ionic liquid in distilled water displacement washing tea grounds cellulose colloid.After thorough washing, obtain three-leaf tea slag cellulose aquagel.
(5) measure three-leaf tea slag cellulose aquagel, 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 steam beating, dry, pulverize, sieve, obtain pretreated tealeaves;
(2) by pretreated tealeaves and water in mass ratio 1:35, water temperature 100 DEG C, soak 3 times, each soak time 30min, extract water soluble component, filter, dry.Take sherwood oil as solvent, after soaking and stirring carries out degreasing in 2 hours, washing, then with acetone decolouring, wash, dry, obtain degreasing, decolouring green tea slag.
(3) be that 4%NaOH solution is by solid-liquid ratio 1:30(g:mL by degreasing, decolouring green tea slag with massfraction) mix, constant temperature 50 DEG C of water-baths 2 hours, suction filtration, wash.Again with the vitriol oil by solid-liquid ratio 1:25(g:mL) mix, constant temperature 60 DEG C of acidolysis 2 hours, suction filtration, washing, dry, obtain Lao Ye tea grounds Mierocrystalline cellulose;
(4) adopt heating-cooling-washing process, by 8%(with AMIMCl Dosage calculation) Lao Ye tea grounds Mierocrystalline cellulose and 30gAMIMCl stirring and dissolving 18h at 80 DEG C.After heating for dissolving, the tea grounds cellulose colloid sample cool to room temperature formed.Then, with the ionic liquid in distilled water displacement washing tea grounds cellulose colloid.After thorough washing, obtain Lao Ye tea grounds cellulose aquagel.
(5) measure Lao Ye tea grounds cellulose aquagel, 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 steam beating, dry, pulverize, sieve, obtain pretreated tealeaves;
(2) by pretreated tealeaves and water in mass ratio 1:40, water temperature 100 DEG C, soak 4 times, each soak time 40min, extract water soluble component, filter, dry.Take sherwood oil as solvent, after soaking and stirring carries out degreasing in 3 hours, washing, then with acetone decolouring, wash, dry, obtain degreasing, decolouring green tea slag.
(3) be that 5%NaOH solution is by solid-liquid ratio 1:30(g:mL by degreasing, decolouring green tea slag with massfraction) mix, constant temperature 60 DEG C of water-baths 2 hours, suction filtration, wash.Again with the vitriol oil by solid-liquid ratio 1:30(g:mL) mix, constant temperature 70 DEG C of acidolysis 2 hours, suction filtration, washing, dry, obtain tea stalk tea grounds Mierocrystalline cellulose;
(4) adopt heating-cooling-washing process, by 10%(with AMIMCl Dosage calculation) tea stalk tea grounds Mierocrystalline cellulose and 30gAMIMCl stirring and dissolving 20h at 90 DEG C.After heating for dissolving, the tea grounds cellulose colloid sample cool to room temperature formed.Then, with the ionic liquid in distilled water displacement washing tea grounds cellulose colloid.After thorough washing, obtain tea stalk tea grounds cellulose aquagel.
(5) measure tea stalk tea grounds cellulose aquagel, balance moisture expansivity is 217.72 ± 5.73%, and balance carrying drug ratio is 14.90%, and drug release rate is 71.4%.
Claims (7)
1. prepared by tea grounds modification a method for hydrogel, it is characterized in that, described hydrogel is that main raw material preparation obtains by the tea grounds of different tenderness, comprises the following steps:
(1) steam beating is carried out to fresh green tea branches and leaves, dry, pulverize, sieve, obtain pretreated tealeaves; By fresh green tea branches and leaves according to different tenderness by Tender to being always divided into a leaf, two leaves, three leaves, Lao Ye and tea stalk successively, described fresh green tea branches and leaves are the one in a leaf, two leaves, three leaves, Lao Ye, tea stalk, to obtain different tenderness tea grounds, different tenderness tea grounds Mierocrystalline cellulose is obtained by different tenderness tea grounds, and then obtained different tenderness tea grounds cellulose aquagel;
(2) extract the water soluble component in pretreated tealeaves, filter, dry, after in degreasing agent, soaking and stirring carries out degreasing, washing, then decolour with decolouring reagent, washing, dries, and obtains degreasing, decolouring green tea slag;
(3) degreasing step (2) obtained, decolouring green tea slag and aqueous sodium hydroxide solution Homogeneous phase mixing, water-bath, suction filtration, washing, obtain alkali carry after green tea slag, the green tea slag after being carried by alkali carries out acidolysis, suction filtration, washing, and oven dry, obtains tea grounds Mierocrystalline cellulose; Described acidolysis concrete steps are: the green tea slag after being carried by alkali mixes by solid-liquid ratio 1:10 ~ 1:30g:mL with the vitriol oil, acidolysis 1 ~ 2 hour under temperature is 40 ~ 70 DEG C of conditions;
(4) adopt heating-cooling-washing process, mixed by tea grounds Mierocrystalline cellulose 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-methylimidazolium chloride (AMIMCl); The cellulosic consumption of described tea grounds is with 3% ~ 10% of AMIMCl Dosage calculation.
2. a kind of method hydrogel being prepared by tea grounds modification according to claim 1, it is characterized in that, described in step (2), the water soluble component extracted in pretreated tealeaves is specially: mixed for 1:20 ~ 1:40 in mass ratio with water by pretreated tealeaves, soak 2 ~ 4 times under water temperature is 70 ~ 100 DEG C of conditions, each soak time 10 ~ 40min.
3. a kind of method hydrogel being prepared by tea grounds modification according to claim 1, is characterized in that, described in step (2), degreasing agent is sherwood oil, and the described soaking and stirring time is 1 ~ 3 hour; Described decolouring reagent is acetone.
4. a kind of method hydrogel being prepared by tea grounds modification 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, decolour green tea slag and aqueous sodium hydroxide solution is 1:10 ~ 1:30g:mL, the bath temperature of described water-bath is 30 ~ 60 DEG C, and water bath time is 1 ~ 2 hour.
5. a kind of method hydrogel being prepared by tea grounds modification according to claim 1, is characterized in that, described in step (4), the temperature of stirring and dissolving is 80 ~ 150 DEG C, and the stirring and dissolving time is 10 ~ 20h.
6. a kind of method hydrogel being prepared by tea grounds modification 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.
7. a kind of natural tea grounds cellulose aquagel obtained by a kind of method hydrogel being prepared by tea grounds modification according to claim 1 is as the application of drug release carrier.
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| CN105131185B (en) * | 2015-09-17 | 2017-12-01 | 华南理工大学 | Pineapple bran hemicellulose group pH responsive types porous aquagel and its preparation method and application |
| CN105707907A (en) * | 2016-03-03 | 2016-06-29 | 中国林业科学研究院林产化学工业研究所 | Method for preparing insoluble dietary fiber from olea europaea pomace |
| CN106071641A (en) * | 2016-06-28 | 2016-11-09 | 郭舒洋 | A kind of tealeaf residue resource prepares the preparation method of anticorrosion granule |
| CN106589411B (en) * | 2016-11-28 | 2019-05-14 | 华南理工大学 | A kind of pineapple bran carboxymethyl cellulose/polyvinyl alcohol/mesoporous silicon oxide composite hydrogel and the preparation method and application thereof |
| KR20200049222A (en) * | 2018-10-31 | 2020-05-08 | (주)아모레퍼시픽 | Granular Composition Comprising Dietary Fiber from Green Tea and Method for Preparing the Same |
| KR102633916B1 (en) * | 2018-10-31 | 2024-02-06 | (주)아모레퍼시픽 | Granular Composition Comprising Dietary Fiber 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 |
| US20210267242A1 (en) * | 2020-02-28 | 2021-09-02 | Amorepacific Corporation | Snowpowder, granular composition comprising sugar alcohol and method for preparing the same |
| CN112868451A (en) * | 2021-01-11 | 2021-06-01 | 霍山玉锦生态农业科技有限公司 | Green pollution-free tea ecological planting method |
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