CN106478963B - Flaxseed gum/cellulose composite hydrogel and preparation method thereof - Google Patents
Flaxseed gum/cellulose composite hydrogel and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to flaxseed gum/cellulose composite hydrogels, it is by concretionary dual network porous aquagel after flaxseed gum solution and cellulose solution mixing crosslinking, and wherein the mass ratio of flaxseed gum and cellulose is 1:1~1:9.Composite hydrogel produced by the present invention has preferable mechanical stability; the porous network structure for being 25~38 μm with average pore size; water holding capacity under the conditions of 40 DEG C was up to 14 days; show good water suction and water retention property; and it is biodegradable under certain humidity, temperature and microorganism existence condition; belong to environment-friendly material, is easy to functionalization and expands and apply, can be widely used in the fields such as bio-medical material, environmental protection and water-keeping material.
Description
Technical field
The present invention relates to polymeric material fields, and in particular to flaxseed gum/cellulose composite hydrogel and its preparation side
Method.
Background technique
Arid is a global problem, arid, the soil erosion of semiarid zone, desertification, soil alkaline
The environmental problems such as change, not only directly affect the production capacity of dry farming system, but also injured ecological safety.Arid is
As the agricultural problem of most serious in worldwide, therefore, the arviculture for studying arid area is being total to for facing mankind
Same project.In recent years, for example hydrophilic high molecular material of super water-absorbent material is because can play the role of maintaining moisture and chemical fertilizer
It is received significant attention with promoting crop growth.
Hydrogel is one for being physically or chemically crosslinked and being formed by the high molecular material with hydrophilic radical through appropriateness
Kind has the functional polymer material of three-dimensional network porous structure and height swelling behavior.It being capable of sensing external environment stimulation
(such as temperature, pH, ionic strength) and sensitivity response can be made, due to its excellent water imbibition, water-retaining property and environmental response
Property, hydrogel shows wide application prospect in fields such as drug delivery system, wastewater treatment, agriculturals.Past tens
Nian Li, hydrogel are widely used in the utilization rate for being used to improve water in agricultural.
As the increasingly depleted and people of fossil resources are to the pay attention to day by day of environmental protection, with natural macromolecular material
The hydrogel that (such as starch, chitosan, cellulose) is prepared as a raw material can be dropped because of its good biocompatibility and biology
Solution property and extensive source and receive more and more attention, however, these material swelling behaviors are unsatisfactory, it is often necessary to
Raw material is modified and to form correspondingly derivative and achievees the purpose that improving performance, such as with cellulose derivative carboxymethyl cellulose
Element and carboxyethyl cellulose etc. are the hydrogel of raw material preparation, although hydrogel performance increases, these are from original
The modified angle of material is set out, and improves its swelling behavior to realize；Preparation process is complicated simultaneously, higher cost.
And flaxseed gum limits its application as excellent water-keeping material due to showing Weak Gels.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of linseed in view of the deficiency of the prior art
Glue/cellulose composite hydrogel and preparation method thereof, gained composite hydrogel have good mechanical stability, water suction and water conservation
Performance.
The present invention be solve the problems, such as it is set forth above used by technical solution are as follows:
Flaxseed gum/cellulose composite hydrogel is by coagulating after flaxseed gum solution and cellulose solution mixing crosslinking
Gu hydrogel made of is 25~38 μm of porous network structure with average pore size, wherein the matter of flaxseed gum and cellulose
Amount is than being preferably 1:1~1:9.
According to the above scheme, the viscosity average molecular weigh of the cellulose is 30,000~370,000 dalton.
According to the above scheme, the mixing crosslinking carries out in the solution.
According to the above scheme, the crosslinking is using epoxychloropropane as crosslinking agent, every 100g flaxseed gum solution and fiber
0.5~5mL epoxychloropropane is added in the mixed solution of plain solution.
Above-mentioned flaxseed gum/cellulose composite hydrogel preparation method, key step are as follows:
1) flaxseed gum solution and cellulose solution are prepared respectively, are placed in 1~7 DEG C of condition storage；
It 2) is 1:1~1:9 by the mass ratio of flaxseed gum and cellulose, by flaxseed gum solution obtained by step 1) and fiber
Plain solution is uniformly mixed, and epoxychloropropane is then added and carries out cross-linking reaction, it is molten to obtain flaxseed gum/cellulose composite cross-linked polymer
Liquid；
3) flaxseed gum/cellulose composite cross-linked polymer solution obtained by step 2) is poured into mold and is solidified to get arriving
Flaxseed gum/cellulose composite hydrogel.
According to the above scheme, the flaxseed gum mass percentage in the flaxseed gum solution is 0.5~4wt.%；It is described
The mass percentage of cellulose is 1~5wt.% in cellulose solution.
According to the above scheme, in the step 2), in the mixed solution of every 100g flaxseed gum solution and cellulose solution, ring
The additional amount of oxygen chloropropane is 0.5~5mL.
According to the above scheme, in the step 2), the time of cross-linking reaction is 10~120min.
According to the above scheme, in the step 2), further include the steps that evacuation and centrifugal degassing cleans after cross-linking reaction.
According to the above scheme, in the step 3), setting temperature is 4~60 DEG C, and setting time is 0.5~12h.
According to the above scheme, the flaxseed gum and cellulose are dissolved into the mixed aqueous solution of urea and alkali.Wherein, the urine
Alkali is sodium hydroxide and lithium hydroxide etc. in the mixed aqueous solution of element and alkali.Preferably, the mixed aqueous solution of urea and alkali is
Aqueous solution containing 6~10wt.%NaOH and 2~20wt.% urea；Or the aqueous solution be containing 4~9wt.%LiOH and 4~
The aqueous solution of 30wt.%.
It is further preferred that the preparation method of the flaxseed gum solution is: flaxseed gum is added to urea and alkali
In mixed aqueous solution, the stirring and dissolving at 20~25 DEG C, evacuation and centrifugal degassing, cleaning is made flaxseed gum solution.Wherein, centrifugation uses
Revolving speed is 6000~7500rpm, and the time is 10~20min.Most preferably, sodium hydroxide in the mixed aqueous solution of urea and alkali
Concentration is 7wt.%, and the concentration of urea is 12wt.%；Alternatively, the concentration of lithium hydroxide is in the mixed aqueous solution of urea and alkali
9wt.%, the concentration of urea are 12wt.%.
It is further preferred that the preparation method of the cellulose solution is: the mixed aqueous solution of urea and alkali is cooled in advance-
5~-20 DEG C, cellulose stirring and dissolving is then added, evacuation and centrifugal degassing, cleaning is made cellulose solution.Wherein, centrifugation uses revolving speed
For 6000~7500rpm, the time is 10~20min.Most preferably, in the mixed aqueous solution of urea and alkali sodium hydroxide concentration
For 7wt.%, the concentration of urea is 12wt.%；Alternatively, the concentration of lithium hydroxide is in the mixed aqueous solution of urea and alkali
9wt.%, the concentration of urea are 12wt.%.
Compared with prior art, the beneficial effects of the present invention are:
(1) select natural polymer flaxseed gum and cellulose for raw material in selection of the present invention, in combination with flaxseed gum
Super water-absorbent can and cellulose high-intensitive network structure, avoid to material modification, acquired flaxseed gum/cellulose is multiple
Heshui gel has good mechanical stability, good water suction and water retention property；Meanwhile the present invention overcomes flaxseed gum by
In its Weak Gels, to limit its limitation applied as excellent water-keeping material；
(2) preparation method of the present invention dissolves flaxseed gum and cellulose using green solvent, and anti-by being simply crosslinked
Flaxseed gum/cellulose composite hydrogel should be prepared, preparation process is simple, waste liquid is easy recycling, not will cause ring
Border pollution；
(3) the raw materials used in the present invention is from a wealth of sources, cheap, biodegradable, environmentally friendly, is easy to functionalization and opens up
Exhibition and application, can be widely used in the fields such as bio-medical material, environmental protection and water-keeping material.
Detailed description of the invention
In Fig. 1, a, c are respectively that 1 gained flaxseed gum of embodiment/cellulose composite hydrogel is swollen the macro of front and back in water
Shape appearance figure is seen, b, d are respectively the macro morphology figure that 5 gained cellulose aquagel of embodiment is swollen front and back in water；
Fig. 2 is the scanning electricity after embodiment 2 and the obtained flaxseed gum of embodiment 5/cellulose composite hydrogel water suction
Mirror figure；
In Fig. 3, a, b, c are respectively embodiment 1, embodiment 3, the obtained flaxseed gum of embodiment 5/cellulose Compound Water
The equilibrium swelling ratio of gel in water；
In Fig. 4, a, b, c are respectively embodiment 1, embodiment 3, the obtained flaxseed gum of embodiment 5/cellulose Compound Water
The water retention of gel in water.
Specific embodiment
The technical issues of in order to better understand the present invention solved, technical solution and technical effect, below in conjunction with reality
Example and attached drawing are applied, the contents of the present invention are further described, but should not be construed as limiting the invention.
Cellulose is cotton linters cellulose in following embodiments, its viscosity average molecular weigh is 30,000~370,000 dalton.
Embodiment 1
Flaxseed gum/cellulose composite hydrogel is by coagulating after flaxseed gum solution and cellulose solution mixing crosslinking
Gu hydrogel made of is~38 μm of porous network structure with average pore size, wherein the quality of flaxseed gum and cellulose
Than for 1:1.
Above-mentioned flaxseed gum/cellulose composite hydrogel preparation method, the specific steps are as follows:
1) 3g flaxseed gum is added to the combination solution of 97g urea containing 7wt.%NaOH and 12wt.%, the magnetic at 25 DEG C
Power stirs 2h, under the conditions of 7500rpm, is centrifuged 15min, obtains flaxseed gum solution, is placed in 4 DEG C of condition storages；
2) combination solution of 97g urea containing 7wt.%NaOH and 12wt.% is cooled to -12.5 DEG C in advance, cotton is added immediately
Short velvet fiber element 3g, mechanical stirring 4min are centrifuged 15min, obtain cellulose solution, be placed in 4 DEG C of items under the conditions of 7500rpm
Part storage；
3) according to flaxseed gum and cellulose weight ratios 1:1, by step 1) and 2) in the flaxseed gum solution, the fibre that prepare
Plain solution mixing is tieed up, 15min is stirred, epoxychloropropane 4mL is added, continuing to stir 30min, to obtain flaxseed gum/cellulose compound
Hydrogel is centrifuged 5min then under the conditions of 3000rpm；
4) solution after centrifugation is poured into mold, 30min solidification forming under the conditions of being placed in 60 DEG C, washing obtains linseed
Glue/cellulose composite hydrogel.
Embodiment 2
Flaxseed gum/cellulose composite hydrogel is by coagulating after flaxseed gum solution and cellulose solution mixing crosslinking
Gu hydrogel made of is~35 μm of porous network structure with average pore size, wherein the quality of flaxseed gum and cellulose
Than for 1:3.
Above-mentioned flaxseed gum/cellulose composite hydrogel preparation method, the specific steps are as follows:
1) 3g flaxseed gum is added to the combination solution of 97g urea containing 7wt.%NaOH and 12wt.%, the magnetic at 25 DEG C
Power stirs 2h, under the conditions of 7500rpm, is centrifuged 15min, obtains flaxseed gum solution, is placed in 4 DEG C of condition storages；
2) combination solution of 97g urea containing 7wt.%NaOH and 12wt.% is cooled to -12.5 DEG C in advance, cotton is added immediately
Short velvet fiber element 3g, mechanical stirring 4min are centrifuged 15min, obtain cellulose solution, be placed in 4 DEG C of items under the conditions of 7500rpm
Part storage；
3) according to flaxseed gum and cellulose weight ratios 1:3, by step 1) and 2) in the flaxseed gum solution, the fibre that prepare
Plain solution mixing is tieed up, 15min is stirred, epoxychloropropane 6mL is added, continuing to stir 30min, to obtain flaxseed gum/cellulose compound
Hydrogel is centrifuged 5min under the conditions of 3000rpm；
4) solution after step 3) centrifugation is poured into mold, 30min solidification forming, washing obtain under the conditions of being placed in 60 DEG C
Flaxseed gum/cellulose composite hydrogel.
Embodiment 3
Flaxseed gum/cellulose composite hydrogel is by coagulating after flaxseed gum solution and cellulose solution mixing crosslinking
Gu hydrogel made of is~33 μm of porous network structure with average pore size, wherein the quality of flaxseed gum and cellulose
Than for 1:5.
Above-mentioned flaxseed gum/cellulose composite hydrogel preparation method, the specific steps are as follows:
1) 3g flaxseed gum is added to the combination solution of 97g urea containing 7wt.%NaOH and 12wt.%, the magnetic at 25 DEG C
Power stirs 2h, under the conditions of 7500rpm, is centrifuged 15min, obtains flaxseed gum solution, is placed in 4 DEG C of condition storages；
2) combination solution of 97g urea containing 7wt.%NaOH and 12wt.% is cooled to -12.5 DEG C in advance, cotton is added immediately
Short velvet fiber element 3g, mechanical stirring 4min are centrifuged 15min, obtain cellulose solution, be placed in 4 DEG C of items under the conditions of 7500rpm
Part storage；
3) by step 1) and 2) in prepare flaxseed gum solution, cellulose solution is according to linseed and cellulose
It is mixed than 1:5, stirs 15min, epoxychloropropane 8mL is added, continued stirring 30min and obtain flaxseed gum/cellulose Compound Water
Gel is centrifuged 5min under the conditions of 3000rpm；
4) solution after step 3) centrifugation is poured into mold, 30min solidification forming, washing obtain under the conditions of being placed in 60 DEG C
Flaxseed gum/cellulose composite hydrogel.
Embodiment 4
Flaxseed gum/cellulose composite hydrogel is by coagulating after flaxseed gum solution and cellulose solution mixing crosslinking
Gu hydrogel made of is~28 μm of porous network structure with average pore size, wherein the quality of flaxseed gum and cellulose
Than for 1:7.
Above-mentioned flaxseed gum/cellulose composite hydrogel preparation method, the specific steps are as follows:
1) 3g flaxseed gum is added to the combination solution of 97g urea containing 7wt.%NaOH and 12wt.%, the magnetic at 25 DEG C
Power stirs 2h, under the conditions of 7500rpm, is centrifuged 15min, obtains flaxseed gum solution, is placed in 4 DEG C of condition storages；
2) combination solution of 97g urea containing 7wt.%NaOH and 12wt.% is cooled to -12.5 DEG C in advance, cotton is added immediately
Short velvet fiber element 3g, mechanical stirring 4min are centrifuged 15min, obtain cellulose solution, be placed in 4 DEG C of items under the conditions of 7500rpm
Part storage；
3) by step 1) and 2) in prepare flaxseed gum solution, cellulose solution is according to flaxseed gum and cellulose weight
Amount is mixed than 1:7, stirs 15min, and epoxychloropropane 6mL is added, and continues to stir 30min that obtain flaxseed gum/cellulose compound
Hydrogel is centrifuged 5min under the conditions of 3000rpm；
4) solution after step 3) centrifugation is poured into mold, 30min solidification forming, washing obtain under the conditions of being placed in 60 DEG C
Flaxseed gum/cellulose composite hydrogel.
Embodiment 5
Flaxseed gum/cellulose composite hydrogel is by coagulating after flaxseed gum solution and cellulose solution mixing crosslinking
Gu hydrogel made of is~25 μm of porous network structure with average pore size, wherein the quality of flaxseed gum and cellulose
Than for 1:9.
Above-mentioned flaxseed gum/cellulose composite hydrogel preparation method, the specific steps are as follows:
1) 3g flaxseed gum is added to the combination solution of 97g urea containing 7wt.%NaOH and 12wt.%, the magnetic at 25 DEG C
Power stirs 2h, under the conditions of 7500rpm, is centrifuged 15min, obtains flaxseed gum solution, is placed in 4 DEG C of condition storages；
2) combination solution of 97g urea containing 7wt.%NaOH and 12wt.% is cooled to -12.5 DEG C in advance, cotton is added immediately
Short velvet fiber element 3g, mechanical stirring 4min are centrifuged 15min, obtain cellulose solution, be placed in 4 DEG C of items under the conditions of 7500rpm
Part storage；
3) by step 1) and 2) in prepare flaxseed gum solution, cellulose solution is according to flaxseed gum and cellulose weight
Amount is mixed than 1:9, stirs 15min, and epoxychloropropane 4mL is added, and continues to stir 30min that obtain flaxseed gum/cellulose compound
Hydrogel is centrifuged 5min under the conditions of 3000rpm；
4) solution after step 3) centrifugation is poured into mold, 30min solidification forming, washing obtain under the conditions of being placed in 60 DEG C
Flaxseed gum/cellulose composite hydrogel.
The flaxseed gum of embodiment 1 and embodiment 5/cellulose composite hydrogel is subjected to equilibrium swelling experiments comparison, such as Fig. 1 institute
Show, after swelling the flaxseed gum of embodiment 1 and embodiment 5/cellulose composite hydrogel obviously becomes larger, and embodiment 1 is answered
Heshui gel swelling ability is significantly greater than embodiment 5, and flaxseed gum content is higher in composite hydrogel, the swelling behavior shown
Also stronger.
To progress scanning electron microscope sight after flaxseed gum/cellulose composite hydrogel water absorption and swelling of embodiment 2 and embodiment 5
Examine, as shown in Fig. 2, composite hydrogel shows uniform three-dimensional porous network structure, average pore size distinguish~35 μm and
~25 μm.It can thus be appreciated that: flaxseed gum content is higher in composite hydrogel, and the aperture after swelling is also bigger.
In order to further verify flaxseed gum/cellulose composite hydrogel water absorbing properties, 1,3,5 institute of embodiment is tested
Hydrogel swelling behavior, as a result as shown in figure 3, the equilibrium swelling ratio of embodiment 1,3,5 is respectively 390,153,51g/g,
It can thus be appreciated that: flaxseed gum content is bigger in composite hydrogel, and equilibrium swelling ratio is also bigger；Then, embodiment 1,3,5 is tested
The water retention property of gained hydrogel, as shown in figure 4, embodiment 1,3,5 is shown good water retention property (about 14 days), and
The content of flaxseed gum is bigger, and corresponding water retention property is also better, it was confirmed that flaxseed gum/cellulose composite hydrogel is good
Water suction and water retention property.
It is tested by simple soil degrading, flaxseed gum/cellulose composite hydrogel obtained by the present invention is placed into the soil
In, the degradation property of section observation hydrogel in different times, observation discovery flaxseed gum/cellulose composite hydrogel can be by
Microbial degradation in soil.
The above is only a preferred embodiment of the present invention, it is noted that come for those of ordinary skill in the art
It says, without departing from the concept of the premise of the invention, several modifications and variations can also be made, these belong to of the invention
Protection scope.
Claims (3)
1. flaxseed gum/cellulose composite hydrogel preparation method, it is characterised in that key step is as follows:
1) flaxseed gum solution and cellulose solution are prepared respectively, are placed in 1 ~ 7 DEG C of condition storage；
It 2) is 1:1 by the mass ratio of flaxseed gum and cellulose, by flaxseed gum solution obtained by step 1) and cellulose solution
It is uniformly mixed, epoxychloropropane is then added and carries out cross-linking reaction 30min, it is molten to obtain flaxseed gum/cellulose composite cross-linked polymer
Liquid；
3) flaxseed gum/cellulose composite cross-linked polymer solution obtained by step 2 is solidified to get flaxseed gum/cellulose is arrived
Composite hydrogel；Wherein, setting temperature is 60 DEG C, setting time 0.5h；
The flaxseed gum and cellulose are dissolved into the mixed aqueous solution of urea and alkali；Flax in the flaxseed gum solution
Seed glue mass percentage is 0.5 ~ 4wt.%；In the cellulose solution mass percentage of cellulose be 1 ~
5wt.%；In the step 2, in every 100g flaxseed gum/cellulose composite cross-linked polymer solution, the additional amount of epoxychloropropane is
4mL。
2. flaxseed gum according to claim 1/cellulose composite hydrogel preparation method, it is characterised in that the fibre
The viscosity average molecular weigh of dimension element is 30,000 ~ 370,000 dalton.
3. flaxseed gum according to claim 1/cellulose composite hydrogel preparation method, it is characterised in that the step
It is rapid 2) in, further include the steps that after cross-linking reaction evacuation and centrifugal degassing clean.
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| CN110078974A (en) * | 2019-03-22 | 2019-08-02 | 昆明理工大学 | Sesbania gum/cellulose composite water conservation hydrogel preparation method |
| CN110016160A (en) * | 2019-04-10 | 2019-07-16 | 南方医科大学 | A kind of preparation method of polysaccharide based aquagel |
| CN110463567A (en) * | 2019-08-12 | 2019-11-19 | 亿利资源集团有限公司 | A kind of soil cultivation agent and preparation method thereof |
| CN113230017A (en) * | 2021-05-10 | 2021-08-10 | 上海捷儿金科技股份有限公司 | Heat-insulating pad and application thereof |
| CN113244455B (en) * | 2021-05-17 | 2022-08-05 | 广西医科大学 | 3D printing flaxseed hydrogel support and preparation method and application thereof |
| CN113388405A (en) * | 2021-06-15 | 2021-09-14 | 鲁东大学 | Application of double-network hydrogel in soil water retention |
| CN115154407B (en) * | 2022-02-22 | 2023-04-18 | 北京华量引擎网络科技有限公司 | Chitosan flaxseed gum cross-linked hydrogel, preparation method and application thereof in gastric bulking agent |
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