CN107417934A - It is a kind of that there is power to cause the high-strength of optics anisotropic approach, high-ductility cellulose aquagel and preparation method thereof - Google Patents
It is a kind of that there is power to cause the high-strength of optics anisotropic approach, high-ductility cellulose aquagel and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of high-strength, high-ductility cellulose aquagel preparation method that optics anisotropic approach is caused with power, the cellulose gel of low chemical crosslinking density is first prepared, gained cellulose gel then is positioned over into 0.1 ~ 25min in the non-solvent of cellulose carries out rapid physical crosslinking；Obtained cellulose gel is utilized into pure water, obtains high-strength, the tough cellulose aquagel of the low chemical crosslinking density of the sensitive cause optics anisotropic approach of power.The stress sensitive that the cellulose aquagel that the present invention is prepared applies to the external world, the obvious optics opposite sex is shown, be a kind of potential soft material of intelligence.
Description
Technical field
The present invention relates to a kind of preparation method and application of cellulose aquagel, belong to chemical, high molecular functional material
Material field.
Background technology
Macromolecule hydrogel is that have chemically or physically structure, can absorb large quantity of moisture but polymer not soluble in water
With water composition, the multicomponent system with three-dimensional crosslinked network structure（Chem. Soc. Rev., 2013. 42, 7391-
7420 ; Chem. Soc. Rev., 2013. 42, 7335-7372）.However, although by repeatedly improvement, the work(of hydrogel
Can constantly extend, lift the mechanical strength of hydrogel and toughness be always researcher bottleneck, some fields such as body bone tissue
The applications such as reparation, the soft substance sensor of intelligence or membrane filtration need hydrogel not only to possess preferable toughness and intensity, and
Hydrogel is more wanted to have both feature.At present, the shortcomings that conventional hydrogels mechanical strength is poor is studied to more by a series of
Mend, wherein most representational have Nanometer composite hydrogel（Adv. Mater., 2002. 14, 1120-1124; Angew. Chem. Int. Ed., 2005. 44, 6500-6504）, double-network hydrogel（J. Am. Chem. Soc., 2001.
123, 5582-5583; Adv. Mater., 2003. 15, 1155-1158; Adv. Funct. Mater., 2004.
14, 1124-1128）, microgel enhancing hydrogel（Macromolecules, 2012. 45, 5218-5228;Macromolecules, 2012. 45, 9445-9451）, ion enhancing hydrogel（Nature. 2012.489,133-136）
With the double cross-linked hydrogels of physical chemistry（Adv. Mater., 2016. 28, 5844-5849；Adv. Funct. Mater.,
2016. 26, 6279-6287）.Wherein polysaccharide hydrogel is a kind of with biocompatibility, biological degradability and nontoxic excellent
The material of benign matter, therefore turn into study hotspot.The patent of invention of the patent No. 200810197646.8 is prepared using epoxychloropropane
Cellulose chemistry gel, adding the mol ratio of large excess of epoxychloropropane and cellulose glucose unit makes hydroxyl on cellulose
Base forms a large amount of chemical crosslinking points by abundant reaction so that obtained hydrogel has enough elastic expansion water storages.It is but such
Type complete swelling cellulose aquagel mechanical property is poor, and stretching and compressive strength only have tens KPa, and significantly limit should
With.The A of patent No. CN 104448396 patent of invention prepares cellulose gel using epoxychloropropane, is re-introduced into physical crosslinking
Network, it is prepared into a kind of elongation at break<80%, stretch the cellulose gel with the several MPa of compressive strength.Physical crosslinking side
It is also appropriate to improve the toughness of gel while the addition of formula is greatly improved the intensity of cellulose gel, but also show
The moisture content and light transmittance that reduce hydrogel write, because excessive physical crosslinking point is to form three-dimensional by hydrogen bond and crystallization
Network structure, make cellulose molecular chain limitation of movement.Cai etc. develops a kind of synthetic method of double cross connection cellulose aquagel.
This method using cellulose, bases and aqueous solution of urea as raw material, by be continuously chemically crosslinked with alcohol induced physical crosslinking, obtain
Double cross connection cellulose aquagel is arrived.Confirmed by test, the mechanical strength of this type hydrogel significantly larger than passes through single friendship
The cellulose aquagel of connection, elongation at break are up to 80%, and shortcoming is the preparation process first step chemical crosslinking time and second
Walking the alcohol induced physical crosslinking time, time-consuming（Highest 24h/ 48h respectively）, material preparation efficiency is greatly reduced, increases work
The difficulty of industryization application；After introducing substantial amounts of physical cross-linked network simultaneously, cellulose crystallity significantly improves, and sacrifices hydrogel
Optical transmittance, while substantial amounts of crystallization greatly limits cellulosic molecule chain movement so that the tension failure elongation of material
Rate lifting is very limited.In addition, this type cellulose aquagel is without because the double crosslinking Treatments of this alternating chemistries physics
And show other features (Adv. Funct. Mater.,2016. 26, 6279-6287)。
The content of the invention
The technical problems to be solved by the invention are to provide a kind of functional fiber hydrogel, by controlling chemistry to hand over
Join dot density and physical crosslinking time, not only greatly shorten gel preparation time, greatly lift the toughness of cellulose aquagel,
The thixotropy of the sensitive sensing external force of cellulose aquagel is more assigned, applies external force induction gel micro-structural orientation, it is different to produce optics
Sexual behaviour.
Technical scheme can be realized by following technical measures：
A kind of high-strength, high-ductility cellulose aquagel preparation method that optics anisotropic approach is caused with power, comprises the following steps：
（1）Under conditions of less than cellulose gel temperature, chemical cross-linking agent and regenerated cellulose solution are mixed, crosslinking
It is 0.05 that agent active function, which is rolled into a ball with the mol ratio of cellulose glucose unit,:1 ~ 1:1, mixing speed is 100 ~ 1000rpm, is stirred
It is 0.5 ~ 5h to mix the time, obtains uniform mixed solution；
（2）By step（1）Obtained solution centrifugal deaeration, crosslinking more than 30min is stood, obtains the fiber of low chemical crosslinking density
Plain gel；
（3）By step（2）Gained cellulose gel is positioned over 0.1 ~ 25min in the non-solvent of cellulose and carries out rapid physical friendship
Connection；
（4）By step（3）Obtained cellulose gel utilizes pure water, obtains the sensitive low chemistry for causing optics anisotropic approach of power
High-strength, the tough cellulose aquagel of crosslink density.
Preferably, step（1）Described in the mol ratio of cross linker active functional group and cellulose glucose unit be 1:
1.33 ~ 1:9.28；Step（3）The time of middle physical crosslinking is 0.1 ~ 15min.
Preferably, step（1）Described in chemical cross-linking agent be epoxide and/or aldehyde compound.
Preferably, step（1）Described in chemical cross-linking agent for epoxychloropropane, epoxy chlorobutane, one kind of glutaraldehyde
It is or a variety of.
Preferably, step（1）Described in regenerated cellulose source, be cotton linter pulp, degreasing cotton pulp, straw pulp, wood pulp,
Bagasse pulp, alginate fibre element, ascidian cellulose, the one or more of tunicin, the degree of polymerization is 200 ~ 2000.
Preferably, step（1）Described in the mass fraction of regenerated cellulose solution be 2 ~ 7 wt%.
Preferably, step（2）The middle temperature for standing crosslinking is 0 ~ 80 DEG C, stands time and temperature and the environment temperature of crosslinking
Relevant, temperature is higher, and it is shorter to be crosslinked the required time.
Preferably, step（3）Described in the non-solvent of cellulose be acidic aqueous solution or ethanol.
Preferably, the acidic aqueous solution is hydrochloric acid, sulfuric acid, acetic acid, phosphoric acid, acetic acid, phytic acid, nitric acid, the one of benzoic acid
Kind is a variety of, and the concentration of the acidic aqueous solution is 0.01 ~ 8 mol/L.
A kind of high-strength, high-ductility cellulose aquagel that optics anisotropic approach is caused with power, is prepared using the above method.
Compared with prior art, the stress sensitive that the cellulose aquagel that the present invention is prepared applies to the external world, shows
Go out the obvious optics opposite sex, be a kind of potential soft material of intelligence.
Brief description of the drawings
Using accompanying drawing, the invention will be further described, but the embodiment in accompanying drawing does not form any limit to the present invention
System.
Accompanying drawing 1 is the standby obtained cellulose aquagel of embodiment 1 under photo in kind under being acted on by external force and corresponding polarisation
Photo, for optics polarisation photograph taking under the polaroid of two intersections, hydrogel is each in the obvious iris of stress generation
Anisotropy behavior；
Accompanying drawing 2 is under conditions of embodiment 2, changes chemical cross-linking agent active function groups/cellulose hydroxyl group mol ratio content, system
Load-deformation curve of the standby obtained cellulose aquagel under stretch mode, is surveyed using U.S. INSTRON electron mechanicses material
Tested under the stretch mode of test-run a machine；
Accompanying drawing 3 is the AFM height map under the cellulose aquagel hygrometric state condition that embodiment 2 obtains；
Accompanying drawing 4 is that embodiment 3 is obtained causes atomic force of the optics foreign fiber hydrogel under maximum tension deformation with power
Microscope height map and corresponding phasor；
Accompanying drawing 5 is the compression stress that there is power to cause optics foreign fiber hydrogel to apply the external world that embodiment 3 is prepared
The polarisation photo of stimuli responsive.
Accompanying drawing 6 is to observe hydrogel stress under hydrogel translucency and polarisation under the different acid treatment times in embodiment 1-6
Its optics opposite sex is iris anisotropy behavior figure under state.
Embodiment
Following examples further illustrate present disclosure, but should not be construed limitation of the present invention.Do not carrying on the back
In the case of from spirit of the invention and essence, the modifications or substitutions made to the inventive method, step or condition belong to this
The scope of invention.
The preparation of regenerated cellulose：
The preparation method of cellulose solution referring toMacromolecules, 2008. 23, 9345-9351.Cellulose solvent is put
The precooling in refrigerator, cellulose is put into the good solvent of precooling, the cellulose solution obtained after being stirred vigorously.Gained cellulose
Solution sloughs bubble and undissolved impurity after being centrifuged under temperature control, high speed rotating speed, finally gives transparent cellulose solution.
Embodiment 1
The regenerated cellulose solution that concentration is 5 wt% is prepared.Epoxychloropropane is added at 10 DEG C（Epoxychloropropane is lived
Property functional group and cellulose glucose unit mol ratio=1：2.32）, mould, room temperature are transferred to after stirring after evacuation and centrifugal degassing
Part chemical crosslinking cellulose gel is obtained after placing 8h, gel is then placed in 2 mol/L sulfuric acid solutions 0.1min quickly eventually
Only chemical crosslink reaction and physical cross-linked network is introduced, being finally washed to neutrality and obtaining hydrogel has high light transmittance, high tenacity
Optics opposite sex behavior is caused with obvious power, i.e., state hydrogel is forced under polarisation and produces obvious iris polarisation behavior.
Embodiment 2
The regenerated cellulose solution that concentration is 5 wt% is prepared.Epoxychloropropane is added at 10 DEG C（Epoxychloropropane is lived
Property functional group and cellulose glucose unit mol ratio=1：2.32）, mould, room temperature are transferred to after stirring after evacuation and centrifugal degassing
Part chemical crosslinking cellulose gel is obtained after placing 8h, gel is then placed in 2 mol/L sulfuric acid solution 5min Quick stops
Chemical crosslink reaction simultaneously introduces physical cross-linked network, be finally washed to neutrality obtain hydrogel have high light transmittance, high tenacity and
Obvious power causes optics opposite sex behavior, i.e., state hydrogel is forced under polarisation and produces obvious iris polarisation behavior.
Embodiment 3
The regenerated cellulose solution that concentration is 5 wt% is prepared.Epoxychloropropane is added at 10 DEG C（Epoxychloropropane is lived
Property functional group and cellulose glucose unit mol ratio=1：2.32）, mould, room temperature are transferred to after stirring after evacuation and centrifugal degassing
Part chemical crosslinking cellulose gel is obtained after placing 8h, gel is then placed in 2 mol/L sulfuric acid solutions 15min quickly eventually
Only chemical crosslink reaction and physical cross-linked network is introduced, being finally washed to neutrality and obtaining hydrogel has high light transmittance, high tenacity
Optics opposite sex behavior is caused with obvious power, i.e., state hydrogel is forced under polarisation and produces obvious iris polarisation behavior.
Embodiment 4
The regenerated cellulose solution that concentration is 5 wt% is prepared.Epoxychloropropane is added at 10 DEG C（Epoxychloropropane is lived
Property functional group and cellulose glucose unit mol ratio=1：2.32）, mould, room temperature are transferred to after stirring after evacuation and centrifugal degassing
Part chemical crosslinking cellulose gel is obtained after placing 8h, gel is then placed in 2 mol/L sulfuric acid solutions 20min quickly eventually
Only chemical crosslink reaction and physical cross-linked network is introduced, being finally washed to neutrality and obtaining cellulose aquagel has certain printing opacity
Property, high-ductility and power cause optics opposite sex behavior, i.e., state hydrogel is forced under polarisation and produces iris polarisation behavior.
Embodiment 5
The regenerated cellulose solution that concentration is 5 wt% is prepared.Epoxychloropropane is added at 10 DEG C（Epoxychloropropane is lived
Property functional group and cellulose glucose unit mol ratio=1：2.32）, mould, room temperature are transferred to after stirring after evacuation and centrifugal degassing
Part chemical crosslinking cellulose gel is obtained after placing 8h, gel is then placed in 2 mol/L sulfuric acid solutions 25min quickly eventually
Only chemical crosslink reaction and physical cross-linked network is introduced, being finally washed to neutrality and obtaining cellulose aquagel has low light transmission, height
Tough property, hydrogel still there is power to cause optics opposite sex behavior, i.e., iris polarisation caused by state hydrogel are forced under polarisation
Behavior.
Embodiment 6
The regenerated cellulose solution that concentration is 5 wt% is prepared.Epoxychloropropane is added at 10 DEG C（Epoxychloropropane is lived
Property functional group and cellulose glucose unit mol ratio=1：2.32）, mould, room temperature are transferred to after stirring after evacuation and centrifugal degassing
Part chemical crosslinking cellulose gel is obtained after placing 8h, gel is then placed in 2 mol/L sulfuric acid solution 30min terminationizations
Learn cross-linking reaction and introduce physical cross-linked network, be finally washed to neutrality and obtain light tight, high-ductility cellulose aquagel sample,
Hydrogel causes optics opposite sex behavior without power, i.e., state hydrogel is forced under polarisation and does not produce iris polarisation behavior.
Embodiment 7
The regenerated cellulose solution that concentration is 6 wt% is prepared, epoxychloropropane is added at 0 DEG C（Epoxychloropropane activity
Functional group and cellulose glucose unit mol ratio=1：9.28）, mould is transferred to after stirring after evacuation and centrifugal degassing, stirring is equal
Even and evacuation and centrifugal degassing, shift stand the obtained loose chemical cross-linked cellulose gels of crosslinking 60min at 0 DEG C in mould afterwards, so
Gel is placed in 5min Quick stops chemical crosslink reaction in 1 mol/L hydrochloric acid solution afterwards and introduces physical cross-linked network, water
Being washed till neutrality and obtain cellulose aquagel, there is certain translucency, high-ductility and power to cause optics opposite sex behavior, i.e., is forced under polarisation
State hydrogel produces iris polarisation behavior.
Embodiment 8
The regenerated cellulose solution that concentration is 6 wt% is prepared.Epoxychloropropane is added at 0 DEG C（Epoxychloropropane activity
Functional group and cellulose glucose unit mol ratio=1：1.33）, mould is transferred to after stirring after evacuation and centrifugal degassing, room temperature is put
Part chemical crosslinking cellulose gel is obtained after putting 4h, gel is then placed in 2 mol/L sulfuric acid solution 10min Quick stops
Chemical crosslink reaction simultaneously introduces physical cross-linked network, is finally washed to and neutral obtain transparent high tenacity there is power to cause the optics opposite sex
Cellulose aquagel.
Embodiment 9
The regenerated cellulose solution that concentration is 6 wt% is prepared.According to crosslinking agent and cellulose glucose unit at 0 DEG C
Mol ratio is 1:1.33 add epoxychloropropane, rear to stir the fully dispersed chemical cross-linking agents of 2 h, after be transferred in mould and be positioned over
Loose chemical cross-linked cellulose gel is prepared in 2h in 60 DEG C of baking ovens, and then gel is transferred in 2mol/L acetums
20min Quick stops chemically react and introduce physical cross-linked network, are finally washed to and neutral obtain transparent high tenacity and have power
Cause the cellulose aquagel of the optics opposite sex.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than the present invention is protected
The limitation of scope is protected, although being explained in detail with reference to preferred embodiment to the present invention, one of ordinary skill in the art should
Understand, technical scheme can be modified or equivalent substitution, without departing from the essence of technical solution of the present invention
And scope.
Claims (10)
- A kind of 1. high-strength, high-ductility cellulose aquagel preparation method that optics anisotropic approach is caused with power, it is characterised in that bag Include following steps：（1）Under conditions of less than cellulose gel temperature, chemical cross-linking agent and regenerated cellulose solution are mixed, crosslinking It is 0.05 that agent active function, which is rolled into a ball with the mol ratio of cellulose glucose unit,:1 ~ 1:1, mixing speed is 100 ~ 1000rpm, is stirred It is 0.5 ~ 5h to mix the time, obtains uniform mixed solution；（2）By step（1）Obtained solution centrifugal deaeration, crosslinking more than 30min is stood, obtains the fiber of low chemical crosslinking density Plain gel；（3）By step（2）Gained cellulose gel is positioned over 0.1 ~ 25min in the non-solvent of cellulose and carries out rapid physical friendship Connection；（4）By step（3）Obtained cellulose gel utilizes pure water, obtain power it is sensitive cause optics anisotropic approach it is high-strength, High-ductility cellulose aquagel.
- 2. preparation method according to claim 1, it is characterised in that step（1）Described in cross linker active functional group Mol ratio with cellulose glucose unit is 1:1.33 ~ 1:9.28；Step（3）The time of middle physical crosslinking be 0.1 ~ 15min。
- 3. preparation method according to claim 1, it is characterised in that step（1）Described in chemical cross-linking agent be epoxy Compound and/or aldehyde compound.
- 4. preparation method according to claim 1, it is characterised in that step（1）Described in chemical cross-linking agent be epoxy One or more in chloropropane, epoxy chlorobutane, glutaraldehyde.
- 5. preparation method according to claim 1, it is characterised in that step（1）Described in regenerated cellulose source, be Cotton linter pulp, degreasing cotton pulp, straw pulp, wood pulp, bagasse pulp, alginate fibre element, ascidian cellulose, one kind of tunicin Or it is a variety of, the degree of polymerization is 200 ~ 2000.
- 6. preparation method according to claim 1, it is characterised in that step（1）Described in regenerated cellulose solution Mass fraction is 2 ~ 7 wt%.
- 7. preparation method according to claim 1, it is characterised in that step（2）The middle temperature for standing crosslinking is 0 ~ 80 DEG C.
- 8. preparation method according to claim 1, it is characterised in that step（3）Described in the non-solvent of cellulose be Acidic aqueous solution or ethanol.
- 9. preparation method according to claim 8, it is characterised in that the acidic aqueous solution be hydrochloric acid, sulfuric acid, acetic acid, Phosphoric acid, acetic acid, phytic acid, nitric acid, the one or more of benzoic acid, the concentration of the acidic aqueous solution is 0.01 ~ 8 mol/L.
- 10. a kind of high-strength, high-ductility cellulose aquagel that optics anisotropic approach is caused with power, it is characterised in that will using right The preparation method described in any one of 1-9 is asked to be prepared.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109440212A (en) * | 2018-11-28 | 2019-03-08 | 五邑大学 | The preparation method of the highly oriented tough regenerated celulose fibre of height and the highly oriented tough regenerated celulose fibre of height |
| CN109485906A (en) * | 2018-11-28 | 2019-03-19 | 五邑大学 | Height-oriented cellulose aerogels and preparation method thereof |
| CN111378182A (en) * | 2019-01-01 | 2020-07-07 | 翁秋梅 | Force-induced responsive polymer with single-hybrid network structure |
| CN111378181A (en) * | 2019-01-01 | 2020-07-07 | 翁秋梅 | Force-induced responsive polymer with single-hybrid network structure |
| CN111592665A (en) * | 2020-05-25 | 2020-08-28 | 广西大学 | Preparation method of carbonized lignin/cellulose conductive hydrogel with pressure sensitivity characteristic |
| CN112759787A (en) * | 2020-12-30 | 2021-05-07 | 鹤山市绿湖生物能源有限公司 | Preparation method of thick-wall regenerated cellulose sponge |
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| CN104387597A (en) * | 2014-11-28 | 2015-03-04 | 武汉大学 | Chemical and physical double-cross-linking high-strength chitin gel material and preparation method thereof |
| CN104448396A (en) * | 2014-11-28 | 2015-03-25 | 武汉大学 | Chemical and physical crosslinking based dual-network cellulose gel system material |
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| CN101128488A (en) * | 2004-12-29 | 2008-02-20 | 路易吉·安布罗西奥 | Biodegradable, super absorbent polymer hydrogels and a method for their preparation |
| CN104387597A (en) * | 2014-11-28 | 2015-03-04 | 武汉大学 | Chemical and physical double-cross-linking high-strength chitin gel material and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109440212A (en) * | 2018-11-28 | 2019-03-08 | 五邑大学 | The preparation method of the highly oriented tough regenerated celulose fibre of height and the highly oriented tough regenerated celulose fibre of height |
| CN109485906A (en) * | 2018-11-28 | 2019-03-19 | 五邑大学 | Height-oriented cellulose aerogels and preparation method thereof |
| CN109440212B (en) * | 2018-11-28 | 2021-05-11 | 五邑大学 | Preparation method of high-orientation high-toughness regenerated cellulose fiber and high-orientation high-toughness regenerated cellulose fiber |
| CN109485906B (en) * | 2018-11-28 | 2021-11-23 | 五邑大学 | Highly oriented cellulose aerogel and method for producing same |
| CN111378182A (en) * | 2019-01-01 | 2020-07-07 | 翁秋梅 | Force-induced responsive polymer with single-hybrid network structure |
| CN111378181A (en) * | 2019-01-01 | 2020-07-07 | 翁秋梅 | Force-induced responsive polymer with single-hybrid network structure |
| CN111592665A (en) * | 2020-05-25 | 2020-08-28 | 广西大学 | Preparation method of carbonized lignin/cellulose conductive hydrogel with pressure sensitivity characteristic |
| CN112759787A (en) * | 2020-12-30 | 2021-05-07 | 鹤山市绿湖生物能源有限公司 | Preparation method of thick-wall regenerated cellulose sponge |
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