CN105622869B - A kind of preparation method of wood fibre temperature sensitive type semi-interpenetrating network gel material - Google Patents
A kind of preparation method of wood fibre temperature sensitive type semi-interpenetrating network gel material Download PDFInfo
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- CN105622869B CN105622869B CN201510852212.7A CN201510852212A CN105622869B CN 105622869 B CN105622869 B CN 105622869B CN 201510852212 A CN201510852212 A CN 201510852212A CN 105622869 B CN105622869 B CN 105622869B
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Abstract
The present invention relates to a kind of preparation method of wood fibre temperature sensitive type semi-interpenetrating network gel material, belong to lignocellulosic material field.Purpose is to provide for a kind of preparation method for the responsive type wood fibre gel rubber material that technique is simple, production cost is low.A certain amount of wood fibre/LiCl/DMSO solution is taken to be filled in band in glass tube, then a certain amount of temperature sensitive monomer N N-isopropylacrylamides and crosslinking agent N are sequentially added, N methylene-bisacrylamides, azo-bis-isobutyl cyanide is added as initiator after stirring 10min at room temperature, continue stirring so that the reagent added is completely dissolved rear vacuum defoamation, nitrogen 30min is passed through again, and glass tube is statically placed in 60 DEG C of water-baths and reacted, gel is taken out after 24h and is put into washing by soaking in absolute ethyl alcohol, absolute ethyl alcohol is changed until removing all unreacted monomers and the oligomer formed in gel, and solvent LiCl/DMSO.Finally absolute ethyl alcohol therein is displaced with the tert-butyl alcohol to be freeze-dried again, obtain aeroge.
Description
Technical field
The invention belongs to biomass energy transformation technology field, relates generally to a kind of wood fibre temperature sensitive type semi-intercrossing network
The preparation method of gel rubber material.
Background technology
In recent years, the research on the gel of the one pack systems such as cellulose, hemicellulose or lignin is a lot, but for
The research of the full constituent wood fibre responsive to temperature type gel of each composition rare report is not separated.Responsive to temperature type gel is main
It is due to contain a certain proportion of hydrophobic/hydrophilic group on its macromolecular chain so that gel is sent out as ambient temperature changes
Raw volume phase transition.Such as in poly-N-isopropyl acrylamide system, amide groups-NHCO is hydrophilic radical, and isopropyl-CH
(CH3) it is hydrophobic grouping.When ambient temperature is relatively low, the hydrophilic radical in gel network structure passes through hydrogen bond and outside moisture
With reference to gel water absorption and swelling;When temperature is higher, hydrogen bond action between hydrophilic radical and water weakens, hydrophobic grouping it is mutual
Effect enhancing, gel then gradually taper up.In the preparation process of temperature-sensitive type gel, the monomer that is commonly used is polyvinyl alcohol,
Polyethylene glycol oxide (PEO), NIPA (NIPAAm) and N, N- acrylamide (DEAAm) etc..
Patent CN102702566A discloses a kind of method that lignocellulose aerogel is prepared using ionic liquid, mainly
It is that lignocellulose aerogel is prepared using wood powder and ionic liquid body.Patent CN103146017A discloses a kind of quick dissolving
The method that lignocellulosic prepares aeroge, its preparing raw material is similar to raw material used by patent CN102702566A all to adopt
Lignocellulose aerogel is prepared with lignocellulosic material and ionic liquid.Aeroge is prepared using ionic liquid greatly to increase
Cost, and the preparation process complex process of ionic liquid are added.The present invention adds monomer and initiator in hydrogel solution,
Semi-intercrossing network (Semi-IPN) hydrogel can be synthesized after initiation reaction, if full interpenetrating networks can also be prepared by adding crosslinking agent simultaneously
(Full-IPN) hydrogel.The difference of semi-intercrossing network and full interpenetrating networks is straight chain/branched polymer of semi-intercrossing network
It can be separated on the premise of chemical bond is not destroyed from polymer network.Designed by this inierpeneirating network structure made
Standby hydrogel has many excellent performances, the absorption of the network structure control medicine of controllable gel and release performance, can
Introducing natural polymer causes gel to have biocompatibility.Polysaccharide polymer rich reserves in nature, bio-compatible
Property is good and biodegradable, therefore is a kind of important biomolecule macromolecular for preparing interpenetrating net polymer hydrogel.Many scholars
Cellulose, hemicellulose or lignin therein, which are isolated, using wood fibre prepares inierpeneirating network structure or Semi-IPN net
Network hydrogel.Chang et al. is prepared in alkali urea water solution system (NaOH/Urea) with epoxychloropropane (ECH) for crosslinking agent
Cellulose network, addition crosslinking agent methylene-bisacrylamide (BIS), in cellulose crosslinked network under the initiation of ammonium persulfate
Cross-linked polymeric N-isopropylacrylamide (NIPAAm) again on architecture basics, so as to which full inierpeneirating network structure hydrogel be made.Wherein
Simultaneously there is two converging networks, have well-regulated loose structure, good mechanical strength and thermo-responsive.Wang[151]
Et al. using LiCl/DMAc systems dissolving cellulose after add NIPA monomer, with N, N- di-2-ethylhexylphosphine oxides third
Acrylamide (MBA) is crosslinking agent, has been synthesized under benzoyl peroxide (BPO) initiation and has contained poly- N,N-DMAA
(DMAm) and cellulose half interpenetrating network structure hydrogel.The thermogravimetric testing result of the gel shows semi-interpenetrating network polymer
Only there is a heat decomposition temperature, this explanation has good chemistry in gel structure between DMAm segments and cellulose chain segment
Connection.
The content of the invention
In order to overcome the shortcomings of background technology, the invention provides a kind of wood fibre temperature sensitive type semi-interpenetrating network gel material
The preparation method of material.It is main to solve the problems such as existing method prepares lignocellulose aerogel complex process, difficulty is big.
The technical solution adopted in the present invention is:A kind of preparation side of wood fibre temperature sensitive type semi-interpenetrating network gel material
Method, comprise the following steps:
(1) a certain amount of lignocellulosic material is taken, powder is ground into using microphyte pulverizer.
(2) a certain amount of lignocellulosic powder is screened, ethylenediamine solution is immersed and filters at room temperature after magnetic agitation 24h
And be freeze-dried, obtain the lignocellulosic after ethylenediamine processing;
(3) LiCl/DMSO mixed solutions are prepared, then take the lignocellulosic powder of a certain amount of ethylenediamine pretreatment molten
In the solution, it is placed in after magnetic agitation 24h in 60 DEG C of constant temperature blender with magnetic force continues to obtain homogeneous glue after stirring 2h at room temperature
Thick lignocellulosic/LiCl/DMSO solution;
(4) take a certain amount of lignocellulosic/LiCl/DMSO solution to be filled in band in glass tube, then sequentially add certain
Measure temperature sensitive monomer NIPA (NIPAAm) and crosslinking agent N, N- methylene-bisacrylamide (MBA);
(5) nitrogen 30min is passed through, and glass tube is statically placed in 60 DEG C of water-baths and reacted, gel is taken out after 24h and is put into nothing
Washing by soaking in water-ethanol, absolute ethyl alcohol is changed until removing all unreacted monomers and the oligomer formed in gel,
And solvent LiCl/DMSO;
(6) displace absolute ethyl alcohol therein with the tert-butyl alcohol to be freeze-dried again, obtain the Semi-IPN net of wood fibre temperature sensitive type
Network aerogel material;
According in a kind of preparation method technical scheme of wood fibre temperature sensitive type semi-interpenetrating network gel material, step (1)
Described in lignocellulosic material be mainly soybean stalk, hardwood pulp, Straw Pulp, softwood pulp etc. all contain lignin
With the biomass material of cellulose.
According in a kind of preparation method technical scheme of wood fibre temperature sensitive type semi-interpenetrating network gel material, step (2)
Described in the lignocellulosic powder filtered out be 40-80 mesh;
According in a kind of preparation method technical scheme of wood fibre temperature sensitive type semi-interpenetrating network gel material, its feature exists
The concentration of LiCl/DMSO mixed solutions described in step (3) is the wooden fibre added in 8%, LiCl/DMSO mixed solutions
The concentration for tieing up plain powder is 1-5%.
The invention difference from existing technology is that the present invention achieves following technique effect:Take a certain amount of wooden
Fiber/LiCl/DMSO solution is filled in glass tube in band, then sequentially adds a certain amount of temperature sensitive monomer NIPA
(NIPAAm) azo-bis-isobutyl cyanide is added after and crosslinking agent N, N- methylene-bisacrylamide (MBA), stirring 10min at room temperature
(AIBN) initiator is used as, continues stirring and causes the reagent of addition to be completely dissolved rear vacuum defoamation, then be passed through nitrogen 30min, and
Glass tube is statically placed in 60 DEG C of water-baths and reacted, gel is taken out after 24h and is put into washing by soaking in absolute ethyl alcohol, changes anhydrous second
Alcohol is until remove all unreacted monomers and the oligomer formed, and solvent LiCl/DMSO in gel.Finally use tertiary fourth
Alcohol displaces absolute ethyl alcohol therein and is freeze-dried again, obtains aeroge.Aeroge preparation method technique letter provided by the invention
List, condition are gentleer, and production cost is low, obtained aerogel material environmental protection.The present invention is made furtherly below in conjunction with the accompanying drawings
It is bright.
Brief description of the drawings
The electromicroscopic photograph of Fig. 1 wood fibre temperature sensitive type semi-intercrossing network aeroges, a wood fibres cellulose content are 1%, b wood
Matter content of cellulose is that 3%, c wood fibres cellulose content is 5%
The infrared spectrum of Fig. 2 temperature sensitive type wood fibre gels, Stem-T-1 represent the gel that wood fibre cellulose content is 1%
Material, Stem-T-3 represent the gel rubber material that wood fibre cellulose content is 3%, and Stem-T-5 represents that wood fibre cellulose content is
5% gel rubber material
The equilibrium swelling ratio of Fig. 3 wood fibres gel at different temperatures, Stem-T-1 represent that wood fibre cellulose content is
The equilibrium swelling ratio of 1% gel rubber material at different temperatures, Stem-T-3 represent the gel material that wood fibre cellulose content is 3%
The equilibrium swelling ratio of material at different temperatures, the gel rubber material that Stem-T-5 expression wood fibre cellulose contents are 5% is in not equality of temperature
Equilibrium swelling ratio under degree
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, technical matters step, condition and material is embodied, to this hair
Technical scheme in bright embodiment is clearly and completely described, it is clear that described embodiment is only a present invention part
Embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not paying wound
The every other embodiment obtained under the premise of the property made work, belongs to the scope of protection of the invention.
The present invention can be soybean stalk, hardwood pulp, Straw Pulp, softwood pulp etc. using lignocellulosic material.With
Lower embodiment illustrates by lignocellulosic material of soybean stalk.Soybean stalk raw material crushes by microphyte pulverizer
Into powder, and the soybean stalk powder of 40-80 mesh is filtered out, soybean stalk pretreatment of raw material of the invention is in ethylenediamine solution
Magnetic agitation, lysate use concentration as 8%LiCl/DMSO mixed solutions.Thermo-sensitive additive is temperature sensitive monomer N- isopropyls
Base acrylamide (NIPAAm) and crosslinking agent N, N- methylene-bisacrylamide (MBA), it is mutual to be made wood fibre temperature sensitive type half
Wear network aerogel material.
Embodiment 1
Soybean stalk stalk part is taken, after the crushing of microphyte pulverizer, filters out the powder of straw of 40-80 mesh for experiment
Use.Soybean stalk powder extracted through benzene -ol mixed liquor (2: 1, v/v) remove after 24h resin acid therein, terpene compound and
The organic solvent extract such as aliphatic acid.Powder of straw is fully volatilized moisture in soybean stalk powder and residual prior to ventilation after extracting
The a small amount of organic solvent stayed, is then dried in vacuo.
Embodiment 2
Dry soybean stalk stalk raw material 10g is weighed, is ground into 40-80 mesh powders, immerses 200ml ethylenediamine solutions
Filter and be freeze-dried after magnetic agitation 24h at room temperature, obtain the soybean stalk stalk powder of ethylenediamine pretreatment.
Embodiment 3
Preparation contains 8%LiCl/DMSO solution, then takes the soybean stalk powder of a certain amount of ethylenediamine pretreatment to be dissolved in this
In solution, the concentration of soybean stalk powder is 1%, is placed in 60 DEG C of constant temperature blender with magnetic force continues after magnetic agitation 24h at room temperature
Homogeneous sticky stalk/LiCl/DMSO solution is obtained after stirring 2h.
Soybean stalk powder/LiCl/DMSO solution that the concentration for taking a certain amount of soybean stalk powder is 1% fills in glass tube in band
In, then sequentially add a certain amount of temperature sensitive monomer NIPA (NIPAAm) and crosslinking agent N, N- di-2-ethylhexylphosphine oxide third
Acrylamide (MBA), add azo-bis-isobutyl cyanide (AIBN) after stirring 10min at room temperature and be used as initiator, continue stirring and cause
The reagent of addition is completely dissolved rear vacuum defoamation, then is passed through nitrogen 30min, and glass tube is statically placed in 60 DEG C of water-baths instead
Should, after 24h take out gel be put into washing by soaking in absolute ethyl alcohol, change absolute ethyl alcohol daily, until remove gel in it is all not
The monomer of reaction and the oligomer formed, and solvent LiCl/DMSO.Finally absolute ethyl alcohol therein is displaced with the tert-butyl alcohol
It is freeze-dried again, obtains the wood fibre temperature sensitive type semi-intercrossing network aerogel material that lignocellulosic material concentration is 1%.
Embodiment 4
Preparation contains 8%LiCl/DMSO solution, then takes the soybean stalk powder of a certain amount of ethylenediamine pretreatment to be dissolved in this
In solution, the concentration of soybean stalk powder is 3%, is placed in 60 DEG C of constant temperature blender with magnetic force continues after magnetic agitation 24h at room temperature
Homogeneous sticky stalk/LiCl/DMSO solution is obtained after stirring 2h.
Soybean stalk powder/LiCl/DMSO solution that the concentration for taking a certain amount of soybean stalk powder is 1% fills in glass tube in band
In, then sequentially add a certain amount of temperature sensitive monomer NIPA (NIPAAm) and crosslinking agent N, N- di-2-ethylhexylphosphine oxide third
Acrylamide (MBA), add azo-bis-isobutyl cyanide (AIBN) after stirring 10min at room temperature and be used as initiator, continue stirring and cause
The reagent of addition is completely dissolved rear vacuum defoamation, then is passed through nitrogen 30min, and glass tube is statically placed in 60 DEG C of water-baths instead
Should, after 24h take out gel be put into washing by soaking in absolute ethyl alcohol, change absolute ethyl alcohol daily, until remove gel in it is all not
The monomer of reaction and the oligomer formed, and solvent LiCl/DMSO.Finally absolute ethyl alcohol therein is displaced with the tert-butyl alcohol
It is freeze-dried again, obtains the wood fibre temperature sensitive type semi-intercrossing network aerogel material that lignocellulosic material concentration is 3%.
Embodiment 5
Preparation contains 8%LiCl/DMSO solution, then takes the soybean stalk powder of a certain amount of ethylenediamine pretreatment to be dissolved in this
In solution, the concentration of soybean stalk powder is 5%, is placed in 60 DEG C of constant temperature blender with magnetic force continues after magnetic agitation 24h at room temperature
Homogeneous sticky stalk/LiCl/DMSO solution is obtained after stirring 2h.
Soybean stalk powder/LiCl/DMSO solution that the concentration for taking a certain amount of soybean stalk powder is 1% fills in glass tube in band
In, then sequentially add a certain amount of temperature sensitive monomer NIPA (NIPAAm) and crosslinking agent N, N- di-2-ethylhexylphosphine oxide third
Acrylamide (MBA), add azo-bis-isobutyl cyanide (AIBN) after stirring 10min at room temperature and be used as initiator, continue stirring and cause
The reagent of addition is completely dissolved rear vacuum defoamation, then is passed through nitrogen 30min, and glass tube is statically placed in 60 DEG C of water-baths instead
Should, after 24h take out gel be put into washing by soaking in absolute ethyl alcohol, change absolute ethyl alcohol daily, until remove gel in it is all not
The monomer of reaction and the oligomer formed, and solvent LiCl/DMSO.Finally absolute ethyl alcohol therein is displaced with the tert-butyl alcohol
It is freeze-dried again, obtains the wood fibre temperature sensitive type semi-intercrossing network aerogel material that lignocellulosic material concentration is 5%.
Every technical staff's notice:Although the present invention describes according to above-mentioned embodiment, of the invention
Invention thought be not limited to that invention, any repacking with inventive concept, will all include this patent protection of the patent right
In the range of.
Claims (2)
1. a kind of preparation method of wood fibre temperature sensitive type semi-intercrossing network aerogel material, it is characterised in that including following step
Suddenly:
(1) a certain amount of lignocellulosic material is taken, powder is ground into using microphyte pulverizer;
(2) a certain amount of 40-80 mesh lignocellulosic powder is screened, immerses ethylenediamine (EDA) solution magnetic agitation at room temperature
Filter and be freeze-dried after 24h, obtain the lignocellulosic after ethylenediamine processing;
(3) 8% LiCl/DMSO mixed solutions are prepared, the lignocellulosic powder for then taking 1-5% ethylenediamine to pre-process is molten
In the solution, it is placed in after magnetic agitation 24h in 60 DEG C of constant temperature blender with magnetic force continues to obtain homogeneous glue after stirring 2h at room temperature
Thick lignocellulosic/LiCl/DMSO solution;
(4) take a certain amount of lignocellulosic/LiCl/DMSO solution to be filled in band in glass tube, then sequentially add a certain amount of temperature
Quick property monomer NIPA (NIPAAm) and crosslinking agent N, N- methylene-bisacrylamide (MBA);
(5) nitrogen 30min is passed through, and glass tube is statically placed in 60 DEG C of water-baths and reacted, gel is taken out after 24h and is put into anhydrous second
Washing by soaking in alcohol, absolute ethyl alcohol is changed until removing all unreacted monomers and the oligomer formed in gel, and
Solvent LiCl/DMSO;
(6) displace absolute ethyl alcohol therein with the tert-butyl alcohol (TBA) to be freeze-dried again, obtain the Semi-IPN net of wood fibre temperature sensitive type
Network aerogel material.
2. according to a kind of preparation method of wood fibre temperature sensitive type semi-intercrossing network aerogel material of claim 1, its feature exists
Lignocellulosic material described in step (1) is soybean stalk, hardwood pulp, Straw Pulp, softwood pulp.
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CN109134914B (en) * | 2018-07-12 | 2020-04-21 | 厦门大学 | Preparation method of double-sensitivity cellulose-based aerogel |
CN114854081B (en) * | 2022-03-25 | 2023-03-21 | 华南理工大学 | Underwater super-oleophobic lignin/cellulose high-strength aerogel and preparation method and application thereof |
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CN1328067A (en) * | 2001-06-29 | 2001-12-26 | 清华大学 | Process for preparing temp-sensitive porous poly(N-isopropyl acrylamide) aqueogel |
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