CN105131185B - Pineapple bran hemicellulose group pH responsive types porous aquagel and its preparation method and application - Google Patents
Pineapple bran hemicellulose group pH responsive types porous aquagel and its preparation method and application Download PDFInfo
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Abstract
The invention belongs to technical field of polymer materials, discloses a kind of pineapple bran hemicellulose group pH responsive types porous aquagel and its preparation method and application.Methods described is, by pre-processing, recycling alkali lye is classified hemicellulose in extraction process extraction pretreatment pineapple bran, washing, is freeze-dried, obtains hemicellulose first by pineapple bran；Hemicellulose is dissolved in deionized water, pore-foaming agent is added, heating stirring, it is well mixed and is completely dissolved, obtain solution I；Monomer and initiator are added into solution I, continues to stir, adds crosslinking agent, it is in clear state to stir to system dissolving perfect solution, stands, washing by soaking, freeze-drying, obtains pineapple bran hemicellulose group pH responsive type porous aquagels.The preparation method of the present invention is simple, and raw material sources enrich；The pore size of prepared porous aquagel is controllable and has good texture characteristic, mechanical property and pH sensitiveness, can be applied to field of medicaments and adsorbing domain.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of pineapple bran hemicellulose group pH responsive types are porous
Hydrogel and preparation method and application.
Background technology
Pineapple bran is dropped in the environment as caused main waste material in pineapple process, has both caused largely to provide
Source wastes, and can also aggravate environmental.Study and show to contain substantial amounts of hemicellulose in pineapple bran, this is the depth of pineapple bran
Processing and comprehensive utilization provide an attemptable direction.Hemicellulose is a kind of glycan of low molecule amount, primary structure
Unit has the neutral sugars such as D- xyloses, L-arabinose, D- galactolipins and a small amount of uronic acid composition, contains among the structure of hemicellulose
There are many activity hydroxies, basis is provided for the modification of hemicellulose, so as to widen the application of hemicellulose and field.
Hydrogel is a kind of hydrophilic polymer, and it can absorb substantial amounts of moisture, and itself will not dissolve, and is had steady
Fixed three-dimensional net structure.Different according to the responsiveness to external environment, hydrogel can be divided into conventional hydrogels and environment is quick
Perceptual hydrogel.Enviromental sensitive hydrogel can ring to the minor variations of environment, such as temperature, pH value, magnetic field, electric field generation
Should, it is widely used in the fields such as drug controlled release, immobilised enzymes and organizational project.
The content of the invention
In order to overcome shortcoming and defect in the prior art, it is an object of the invention to provide a kind of pineapple bran hemicellulose group
The preparation method of pH responsive type porous aquagels.
Another object of the present invention is to provide the porous aquagel being prepared by above-mentioned preparation method.The present invention's is more
The features such as hole hydrogel has good mechanical property and swelling behavior, and pore size is controllable, three-dimensional net structure is stable.
It is still another object of the present invention to provide the application of above-mentioned porous aquagel.Hydrogel prepared by the present invention can be made
Field of medicaments is applied to for drug release carrier, wound dressing etc., adsorbent can also be used as to be applied to chemical industry, environment guarantor
The fields such as shield.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of pineapple bran hemicellulose group pH responsive type porous aquagels, specifically includes following steps：
A：By pineapple bran by pre-processing, hemicellulose in recycling alkali lye classification extraction process extraction pretreatment pineapple bran,
Washing, freeze-drying, obtain hemicellulose；
B：Hemicellulose is dissolved in deionized water, pore-foaming agent is added, heating stirring, makes it well mixed and completely molten
Solution, obtains solution I；Monomer and initiator are added into solution I, continues to stir, adds crosslinking agent, stir to system and dissolved
Whole soln is in clear state, is stood, washing by soaking, freeze-drying, it is porous to obtain pineapple bran hemicellulose group pH responsive types
Hydrogel.
Pretreatment described in step A, which refers to smash pineapple bran, sieves, and is then carried out with sodium chlorite solution in 70-80 DEG C
Delignification pre-processes 3~5h, and it is 3.8-4.0 to adjust pH value of solution during delignification processing；The pineapple bran and chlorous acid
The mass volume ratio of sodium solution is 1g:(15-25)mL；The mass percent of sodium chlorite is 5%- in the sodium chlorite solution
10%；The material of the regulation pH is acetic acid.
The classification extraction process of alkali lye described in step A is divided into three-level extracting, the quality percentage of alkali lye described in extracting per one-level
Specific concentration is 1%-20%, and the temperature of the extracting is 60-80 DEG C, and the time of extracting is 2-5h；It is described pretreatment pineapple bran with
Per one-level, the mass volume ratio of extracting alkali lye is 1g:(10-30)mL；The alkali lye is the NaOH aqueous solution, the KOH aqueous solution or second
Alcohol-NaOH.
Washing described in step A refers to be washed 3-6 times repeatedly with the ethanol solution that volume fraction is 70%, and the freezing is dry
Dry condition is to be freeze-dried 30h in -50 DEG C.
It is 2%-10% that hemicellulose described in step B, which is dissolved in the mass concentration after deionized water,；The pore-foaming agent is poly-
One or more of ethylene glycol or sodium alginate, the molecular weight of the polyethylene glycol is 1000-8000；The pore-foaming agent dosage is
The 0%-15% of hemicellulose and monomer gross mass, the temperature of the heating stirring is 40-60 DEG C；Heating is stirred described in step B
It is 300-600rpm to mix speed.
Monomer described in step B is acrylamide, acrylic acid, one or more of propene sulfonic acid, the monomer dosage with
The mass ratio of hemicellulose dosage is 2:1-10:1.The initiator is ammonium persulfate, potassium peroxydisulfate, the NSC 18620 hydrochloric acid of azo two
One kind in salt, the initiator amount are hemicellulose and the 1%-2% of monomer gross mass.
The time for continuing stirring described in step B is 5-10min, and the crosslinking agent is N-N methylene-bisacrylamides, ring
Ethylene Oxide or glutaraldehyde, the dosage of crosslinking agent are hemicellulose and the 1%-5% of monomer gross mass.
Washing by soaking refers to wash 3-7d with distilled water immersion described in step B, and a water is changed every 8-24h；It is described cold
Freezing dry condition is：30h is freeze-dried in -50 DEG C.
Time of repose described in step B is 2-4h.
The pineapple bran hemicellulose group pH responsive types porous aquagel is prepared by above-mentioned preparation method.
The pineapple bran hemicellulose group pH responsive types porous aquagel is in drug release carrier, the medicine neck of wound dressing
Domain, and chemical industry, field of environment protection as adsorbent.
Compared with prior art, the invention has the advantages that and beneficial effect：
(1) it is processing of farm products waste material pineapple bran that hydrogel of the invention is raw materials used, abundance, cheap, can
Turned waste into wealth with realizing, be advantageous to higher value application agricultural byproducts, promote recycling economy development；
(2) present invention prepare hydrogel process route is simple, equipment requirement is low, be easy to implement industrialized production；
(3) present invention can be by changing the dosage and molecular weight of pore-foaming agent, and crosslinking agent and monomer dosage are porous to adjust
The pore size of hydrogel, and the three-dimensional net structure for forming hydrogel is stable, has good texture characteristic and mechanical property；
(4) by introducing alkalescence or acidic-group on hemicellulose skeleton, so that the hydrogel being prepared
With pH sensitiveness, hydrogel has been widened in biology, the application of medicine and other fields.
Brief description of the drawings
Fig. 1 is the SEM figures of pineapple bran hemicellulose group pH responsive type porous aquagels prepared by embodiment 1；
Fig. 2 is the SEM figures of pineapple bran hemicellulose group pH responsive type porous aquagels prepared by embodiment 2；
Fig. 3 is the SEM figures of pineapple bran hemicellulose group pH responsive type porous aquagels prepared by embodiment 3；
Fig. 4 is the SEM figures of pineapple bran hemicellulose group pH sensitive hydrogels prepared by embodiment 4.
Embodiment
It is described further and describes below in conjunction with implementation of the drawings and examples to the present invention, but the embodiment party of the present invention
Formula is not limited to this.
Embodiment 1
A kind of preparation method of pineapple bran hemicellulose group pH responsive type porous aquagels, specifically includes following steps：
(1) pineapple bran is after it crushed 40 mesh, is carried out with the sodium chlorite solution that mass fraction is 5% at 70 DEG C de- wooden
The mass volume ratio of element pretreatment 3h, pineapple bran and sodium chlorite solution are 1g:15mL, acetic acid is used after adding sodium chlorite solution
It is 3.8 to adjust pH value of solution, obtains pre-processing pineapple bran；
(2) pretreatment pineapple bran is stripped using NaOH aqueous solution classification extraction process, the classification extraction process is divided into
Three-level extracts, and one-level extracting alkali lye mass concentration is 2%, two level extracting alkali lye mass concentration is 5%, three-level extracting alkali lye quality
Concentration is 10%, and the pretreatment pineapple bran is 1g with the mass volume ratio that alkali lye is extracted per one-level:10mL, the extracting temperature per one-level
Spend for 60 DEG C, be 5h per one-level extraction times, washed repeatedly 5 times with the ethanol that volume fraction is 70% after having extracted, in -50 DEG C
30h is freeze-dried, obtains hemicellulose；
(3) accurately weigh the hemicelluloses of 0.5g after purification to be dissolved in 10mL distilled water, adding 0.35g molecular weight is
1000 polyethylene glycol pore-foaming agent, (rotating speed of stirring is 300rpm) is stirred in 40 DEG C of oil baths, is well mixed and is completely dissolved, obtain
To solution I；3g monomeric acrylamides and 0.035g initiator ammonium persulfates are added into solution I, continues after stirring 5min, adds
0.035g crosslinking agent N-N methylene-bisacrylamides, continuing stirring makes system dissolving perfect solution be in clear state, stops
Stirring, 2h is stood, with distilled water washing by soaking 3d repeatedly, a water is changed every 8h, be freeze-dried 30h in -50 DEG C, obtain pineapple
Slag hemicellulose group pH responsive type porous aquagels.
Embodiment 2
A kind of preparation method of pineapple bran hemicellulose group pH responsive type porous aquagels, specifically includes following steps：
(1) pineapple bran carries out de- wood at 70 DEG C after it crushed 40 mesh with the sodium chlorite solution that mass fraction is 7.5%
The mass volume ratio of quality pretreatment 3h, pineapple bran and sodium chlorite solution are 1g:20mL, vinegar is used after adding sodium chlorite solution
Acid-conditioning solution pH is 3.9, obtains pre-processing pineapple bran；
(2) pretreatment pineapple bran is stripped using NaOH aqueous solution classification extraction process, the classification extraction process is divided into
Three-level extracts, and one-level extracting alkali lye mass concentration is 2%, two level extracting alkali lye mass concentration is 5%, three-level extracting alkali lye quality
Concentration is 10%, and the pretreatment pineapple bran is 1g with the mass volume ratio that alkali lye is extracted per one-level:20mL, the extracting temperature per one-level
Spend for 70 DEG C, be 3h per one-level extraction times, washed repeatedly 5 times with the ethanol that volume fraction is 70% after having extracted, in -50 DEG C
30h is freeze-dried, obtains hemicellulose；
(3) accurately weigh the hemicelluloses of 0.5g after purification to be dissolved in 10mL distilled water, adding 0.55g molecular weight is
6000 polyethylene glycol pore-foaming agent, (rotating speed of stirring is 400rpm) is stirred in 50 DEG C of oil baths, is well mixed and is completely dissolved, obtain
To solution I；5g monomeric acrylamides and 0.11g initiator ammonium persulfates are added into solution I, continues after stirring 5min, adds
0.275g crosslinking agent N-N methylene-bisacrylamides, continuing stirring makes system dissolving perfect solution be in clear state, stops
Stirring, 3h is stood, with distilled water washing by soaking 5d repeatedly, a water is changed every 12h, be freeze-dried 30h in -50 DEG C, obtain spinach
Trailing plants slag hemicellulose group pH responsive type porous aquagels.
Embodiment 3
A kind of preparation method of pineapple bran hemicellulose group pH responsive type porous aquagels, specifically includes following steps：
(1) pineapple bran carries out de- wood at 70 DEG C after it crushed 40 mesh with the sodium chlorite solution that mass fraction is 10%
The mass volume ratio of quality pretreatment 3h, pineapple bran and sodium chlorite solution are 1g:25mL, vinegar is used after adding sodium chlorite solution
Acid-conditioning solution pH is 4.0, obtains pre-processing pineapple bran；
(2) pretreatment pineapple bran is stripped using NaOH aqueous solution classification extraction process, the classification extraction process is divided into
Three-level extracts, and one-level extracting alkali lye mass concentration is 2%, two level extracting alkali lye mass concentration is 5%, three-level extracting alkali lye quality
Concentration is 10%, and the pretreatment pineapple bran is 1g with the mass volume ratio that alkali lye is extracted per one-level:30mL, the extracting temperature per one-level
Spend for 80 DEG C, be 2h per one-level extraction times, washed repeatedly 5 times with the ethanol that volume fraction is 70% after having extracted, in -50 DEG C
30h is freeze-dried, obtains hemicellulose；
(3) accurately weigh the hemicelluloses of 0.5g after purification to be dissolved in 10mL distilled water, adding 0.225g molecular weight is
8000 polyethylene glycol pore-foaming agent, (rotating speed of stirring is 500rpm) is stirred in 60 DEG C of oil baths, is well mixed and is completely dissolved, obtain
To solution I；1g monomeric acrylamides and 0.0225g initiator ammonium persulfates are added into solution I, continues after stirring 5min, adds
Enter 0.03g crosslinking agent N-N methylene-bisacrylamides, continuing stirring makes system dissolving perfect solution be in clear state, stops
Only stir, stand 4h, with distilled water washing by soaking 7d repeatedly, a water is changed every 24h, be freeze-dried 30h in -50 DEG C, obtain
Pineapple bran hemicellulose group pH responsive type porous aquagels.
Embodiment 4
A kind of preparation method of pineapple bran hemicellulose group pH sensitive hydrogels, specifically includes following steps：
(1) pineapple bran carries out de- wood at 70 DEG C after it crushed 40 mesh with the sodium chlorite solution that mass fraction is 10%
The mass volume ratio of quality pretreatment 3h, pineapple bran and sodium chlorite solution are 1g:20mL, vinegar is used after adding sodium chlorite solution
Acid-conditioning solution pH is 3.8, obtains pre-processing pineapple bran；
(2) pretreatment pineapple bran is stripped using NaOH aqueous solution classification extraction process, the classification extraction process is divided into
Three-level extracts, and one-level extracting alkali lye mass concentration is 2%, two level extracting alkali lye mass concentration is 5%, three-level extracting alkali lye quality
Concentration is 10%, and the pretreatment pineapple bran is 1g with the mass volume ratio that alkali lye is extracted per one-level:30mL, the extracting temperature per one-level
Spend for 80 DEG C, be 2h per one-level extraction times, washed repeatedly 5 times with the ethanol that volume fraction is 70% after having extracted, in -50 DEG C
30h is freeze-dried, obtains hemicellulose；
(3) accurately weigh the hemicelluloses of 0.5g after purification to be dissolved in 10mL distilled water, in 45 DEG C of oil baths stirring (stirrings
Rotating speed be 500rpm), it is well mixed and be completely dissolved, obtain solution I；Into solution I add 3g monomeric acrylamides and
0.035g initiator ammonium persulfates, continue after stirring 5min, add 0.035g crosslinking agent N-N methylene-bisacrylamides, continue
Stirring makes system dissolving perfect solution be in clear state, stops stirring, standing 4h, with distilled water washing by soaking 7d repeatedly,
A water is changed every 24h, 30h is freeze-dried in -50 DEG C, obtains pineapple bran hemicellulose group pH sensitive hydrogels.
Performance test：
(1) the texture properties evaluation of hydrogel
The hydrogel in embodiment 1,2,3,4 is chosen, TPA analyses are carried out using 5g power.Each hydrogel sample is (straight
Footpath about 2.5cm, high about 1cm) undergo two second compressions, decrement 30%, speed is 5mm-1 before compression, and speed is during compression
1mm s-1, speed is 5mm s-1 after compression, and used compression probe pops one's head in (P36-R) for cylindrical stainless steel.It is resulting
Different hydrogels texture data it is as shown in table 1：
Table 1：Hydrogel texture data prepared by embodiment 1~4
| Sample number into spectrum | Hardness (g) | Elasticity | Cohesion (- gs) | Stickiness (g) | Recovery |
| Embodiment 1 | 4305.472±424.378 | 0.945±0.097 | 0.969±0.097 | 4125.326±449.531 | 0.951±0.105 |
| Embodiment 2 | 5029.374±825.373 | 0.749±0.068 | 0.836±0.072 | 4986.291±793.496 | 0.763±0.068 |
| Embodiment 3 | 477.794±62.532 | 0.938±0.122 | 0.824±0.064 | 393.783±73.273 | 0.660±0.044 |
| Embodiment 4 | 3843.848±396.756 | 0.943±0.093 | 0.999±0.103 | 3838.305±423.976 | 0.930±0.098 |
By texture data find the environment sensitive type porous aquagel for preparing of the present invention have good texture characteristic and
Mechanical property.
(2) the swelling behavior evaluation of hydrogel
The hydrogel in embodiment 1,2,3,4 is chosen, a certain amount of dried hydrogel sample is weighed, is soaked in respectively
About 48 hours in the cushioning liquid that pH is 2.0,4.0,6.0,8.0,10.0 and 12.0, after hydrogel reaches swelling equilibrium, claim it
Weight, calculating are the water absorption and swelling rate (percentage of hydrogel water absorption and its own weight of the hydrogel under different pH environment
Than), test result is as shown in table 2：
Table 2：Swelling behavior test data prepared by embodiment 1~4
| pH2.0 | pH4.0 | pH6.0 | pH8.0 | pH10.0 | pH12.0 | |
| Embodiment 1 | 912% | 915% | 943% | 1002% | 1109% | 1702% |
| Embodiment 2 | 540% | 532% | 520% | 540% | 596% | 987% |
| Embodiment 3 | 1128% | 1030% | 1069% | 1143% | 1575% | 2046% |
| Embodiment 4 | 743% | 785% | 769% | 799% | 943% | 1432% |
Can be seen that the environment sensitive type porous aquagel of the invention prepared by the data of swelling ratio has good pH
Sensitiveness and swellability.
(3) ESEM (SEM) analysis of hydrogel
The hydrogel in embodiment 1,2,3,4 is chosen, dried hydrogel sample is fixed in copper dish with conducting resinl
Metal spraying processing is carried out, then observes the surface topography of hydrogel, multiplication factor 1000 under 10K accelerating potentials with ESEM
Times, structural characterization is as shown in figures 1-4.Analyze hydrogel sample SEM photograph in different embodiments to find, the water-setting of embodiment 1,2,3
There is clear and uniform cavernous structure on the surface of glue sample, and embodiment 4 is the hydrogel sample surface that pore-foaming agent dosage is 0
Obvious pore structure is hardly visible, simply shows intensive buckle condition, being indicated above pore-foaming agent can make hydrogel show shape
Into uniform cavernous structure.Meanwhile the change of the factor such as crosslinking agent, monomer dosage also can be to pore structure size and intensive journey
Degree has an impact.
The above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not to the present invention
Embodiment restriction.For those of ordinary skill in the field, can also make on the basis of the above description
Other various forms of changes or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all the present invention
All any modification, equivalent and improvement made within spirit and principle etc., should be included in the protection of the claims in the present invention
Within the scope of.
Claims (5)
- A kind of 1. preparation method of pineapple bran hemicellulose group pH responsive type porous aquagels, it is characterised in that：Specifically include with Lower step：A：By pineapple bran by pre-processing, hemicellulose in recycling alkali lye classification extraction process extraction pretreatment pineapple bran, washing, Freeze-drying, obtains hemicellulose；B：Hemicellulose is dissolved in deionized water, pore-foaming agent is added, heating stirring, it is well mixed and is completely dissolved, Obtain solution I；Monomer and initiator are added into solution I, continues to stir, adds crosslinking agent, is stirred complete to system dissolving Solution is in clear state, is stood, washing by soaking, freeze-drying, obtains the porous water of pineapple bran hemicellulose group pH responsive types Gel；Pore-foaming agent described in step B is one or more of polyethylene glycol or sodium alginate, and the molecular weight of the polyethylene glycol is 1000-8000；Monomer described in step B is one or more of acrylamide, acrylic acid, propene sulfonic acid；Described initiator is over cure One kind in sour ammonium, potassium peroxydisulfate, azo-bis-isobutyrate hydrochloride；Crosslinking agent described in step B is N-N methylene bisacrylamide acyls Amine, expoxy propane or glutaraldehyde；The classification extraction process of alkali lye described in step A is divided into three-level extracting, and per one-level, the mass percent of alkali lye is dense described in extracting Spend for 1%-20%, the temperature of the extracting is 60-80 DEG C, and the time of extracting is 2-5h；The pretreatment pineapple bran and every one-level The mass volume ratio for extracting alkali lye is 1g:（10-30）mL；Pretreatment described in step A, which refers to smash pineapple bran, sieves, and then carries out de- wood in 70-80 DEG C with sodium chlorite solution Element 3 ~ 5h of pretreatment, it is 3.8-4.0 to adjust pH value of solution during delignification processing；The pineapple bran and sodium chlorite solution Mass volume ratio be 1g:（15-25）mL；The mass percent of sodium chlorite is 5%-10% in the sodium chlorite solution；Institute The material for stating regulation pH is acetic acid；Pore-foaming agent dosage described in step B is the 0%-15% of hemicellulose and monomer gross mass, the monomer dosage and hemicellulose The mass ratio of plain dosage is 2:1-10:1；The initiator amount is hemicellulose and the 1%-2% of monomer gross mass；The crosslinking Agent dosage is hemicellulose and the 1%-5% of monomer gross mass.
- 2. the preparation method of pineapple bran hemicellulose group pH responsive type porous aquagels, its feature exist according to claim 1 In：The alkali lye is the NaOH aqueous solution, the KOH aqueous solution or ethanol-NaOH.
- 3. the preparation method of pineapple bran hemicellulose group pH responsive type porous aquagels, its feature exist according to claim 1 In：It is 2%-10% that hemicellulose described in step B, which is dissolved in the mass concentration after deionized water,；The temperature of the heating stirring is 40-60℃；Heating stirring speed described in step B is 300-600rpm；The time for continuing stirring described in step B is 5- 10min；Time of repose described in step B is 2-4h；Washing by soaking refers to wash 3-7d with distilled water immersion described in step B, and a water is changed every 8-24h；The freezing is dry Dry condition is：30h is freeze-dried in -50 DEG C；Washing described in step A refers to be washed 3-6 times repeatedly with the ethanol solution that volume fraction is 70%, the freeze-drying Condition is to be freeze-dried 30h in -50 DEG C.
- 4. the pineapple bran hemicellulose group pH responsive types that one kind is prepared as the preparation method described in any one of claim 1 ~ 3 Porous aquagel.
- 5. pineapple bran hemicellulose group pH responsive types porous aquagel is in drug release carrier, wound according to claim 4 Application in dressing and absorbent fields.
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| CN107759735B (en) * | 2016-08-22 | 2020-07-28 | 华南理工大学 | Water-insoluble hemicellulose grafted polyacrylamide and preparation and application thereof |
| 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 |
| CN108047353A (en) * | 2017-12-20 | 2018-05-18 | 南京林业大学 | A kind of method of hemicellulose in separation in situ and recycling strong alkali solution |
| DE102017130893A1 (en) * | 2017-12-21 | 2019-06-27 | Paul Hartmann Ag | pH regulating wound dressing |
| CN108530585B (en) * | 2018-04-17 | 2020-08-11 | 广西大学 | PH-responsive plant fiber functional material and preparation method and application thereof |
| CN108713967A (en) * | 2018-06-01 | 2018-10-30 | 叶建民 | A kind of sound absorption curtain fabric |
| CN110240673B (en) * | 2019-06-19 | 2022-03-22 | 天津科技大学 | Poplar steam blasting liquid hemicellulose-based hydrogel and preparation method thereof |
| CN112705170B (en) * | 2020-12-16 | 2022-03-29 | 华南理工大学 | Efficient shaddock peel lignin-based hydrogel adsorbent and preparation method and application thereof |
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