CN105622869A - Preparation method of wood fiber temperature sensitive type semi-interpenetrating network gel material - Google Patents
Preparation method of wood fiber temperature sensitive type semi-interpenetrating network gel material Download PDFInfo
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- 229920002522 Wood fibre Polymers 0.000 title claims abstract description 37
- 239000000463 material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002025 wood fiber Substances 0.000 title abstract 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 87
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 60
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000178 monomer Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011521 glass Substances 0.000 claims abstract description 14
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004964 aerogel Substances 0.000 claims abstract description 12
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 12
- 238000004108 freeze drying Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 27
- 244000068988 Glycine max Species 0.000 claims description 24
- 235000010469 Glycine max Nutrition 0.000 claims description 24
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 18
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 13
- 239000012978 lignocellulosic material Substances 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000010902 straw Substances 0.000 claims description 5
- 229920005610 lignin Polymers 0.000 claims description 4
- 239000002028 Biomass Substances 0.000 claims description 3
- 239000002023 wood Substances 0.000 claims description 2
- 244000025254 Cannabis sativa Species 0.000 claims 1
- 229920001131 Pulp (paper) Polymers 0.000 claims 1
- 235000012054 meals Nutrition 0.000 claims 1
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 abstract description 11
- 239000003999 initiator Substances 0.000 abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 abstract 2
- 239000000499 gel Substances 0.000 description 38
- 229920002678 cellulose Polymers 0.000 description 15
- 239000001913 cellulose Substances 0.000 description 15
- 239000000017 hydrogel Substances 0.000 description 7
- 239000002608 ionic liquid Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 230000008961 swelling Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000003203 everyday effect Effects 0.000 description 3
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 2
- 239000004342 Benzoyl peroxide Substances 0.000 description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000011121 hardwood Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000001165 hydrophobic group Chemical group 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000011122 softwood Substances 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001408 amides Chemical group 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000006166 lysate Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012857 repacking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- -1 terpene compound Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- WTHDKMILWLGDKL-UHFFFAOYSA-N urea;hydrate Chemical compound O.NC(N)=O WTHDKMILWLGDKL-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a preparation method of a wood fiber temperature sensitive type semi-interpenetrating network gel material, and belongs to the field of wood fiber materials. The invention aims at providing a sensitive type wood fiber gel material preparation method which is simple in process and low in production cost. The preparation method comprises the following steps: feeding a certain amount of a wood fiber/LiCl/DMSO solution into a glass tube with a plug, then sequentially adding a certain amount of temperature sensitive type monomer N-isopropylacrylamide and a cross-linking agent N, N-methylene bisacrylamide, stirring for 10 min at room temperature, adding 2, 2'-azobisisobutyronitrile as an initiator, continuously stirring to ensure that the added reagent is completely dissolved, performing vacuum defoamation, introducing nitrogen for 30 min, leaving the glass tube to stand in a 60 DEG C water bath kettle for reaction, taking out gel after 24 h and putting the gel into absolute ethyl alcohol for soaking and washing, replacing the absolute ethyl alcohol till all unreacted monomer, formed oligomer and the solvent LiCl/DMSO in the gel are removed, finally replacing the absolute ethyl alcohol with tertiary butanol, and performing freeze drying, so as to obtain aerogel.
Description
Technical field
The invention belongs to biomass energy transformation technology field, the preparation method relating generally to a kind of wood fibre temperature sensitive type semi-interpenetrating network gel material.
Background technology
In recent years, the research about the gel of the one pack systems such as cellulose, hemicellulose or lignin is a lot, but for not separating the research rare report of the full constituent wood fibre responsive to temperature type gel of each composition. Responsive to temperature type gel is mainly due to containing a certain proportion of hydrophobic/hydrophilic group on its macromolecular chain so that gel, along with ambient temperature change, volume phase transition occurs. As, in poly-N-isopropyl acrylamide system, amide groups-NHCO is hydrophilic group, and isopropyl-CH (CH3) for hydrophobic group. When ambient temperature is relatively low, the hydrophilic group in gel network structure is combined with outside moisture by hydrogen bond, gel water absorption and swelling; When temperature is higher, the hydrogen bond action between hydrophilic group and water weakens, and the Interaction enhanced of hydrophobic group, gel then gradually tapers up. In the preparation process of temperature-sensitive type gel, commonly used monomer is polyvinyl alcohol, polyethylene glycol oxide (PEO), NIPA (NIPAAm) and N, N-acrylamide (DEAAm) etc.
Patent CN102702566A discloses a kind of method utilizing ionic liquid to prepare lignocellulose aerogel, mainly adopts wood powder and ionic liquid body to prepare lignocellulose aerogel. Patent CN103146017A discloses a kind of method that rapid solution lignocellulose prepares aeroge, and it prepares raw material that raw material adopts to patent CN102702566A similar is all adopt lignocellulosic material and ionic liquid to prepare lignocellulose aerogel. Adopt ionic liquid to prepare aeroge and greatly add cost, and the preparation process complex process of ionic liquid. Monomer and initiator are added in hydrogel solution by the present invention, can synthesize semi-intercrossing network (Semi-IPN) hydrogel, if being simultaneously introduced cross-linking agent also can prepare full interpenetrating networks (Full-IPN) hydrogel after initiation reaction. Semi-intercrossing network and full interpenetrating networks are distinctive in that the straight chain/branched polymer of semi-intercrossing network can be separated under the premise not destroying chemical bond from polymer network. Having a lot of excellent performance by the hydrogel that the design of this inierpeneirating network structure is prepared, the network structure of controllable gel controls absorption and the release performance of medicine, can introduce natural polymer and make gel have biocompatibility. Polysaccharide polymer is rich reserves in nature, good biocompatibility, and biodegradable, is therefore the class important biomolecule macromole preparing interpenetrating net polymer hydrogel. A lot of scholars utilize wood fibre to isolate cellulose therein, hemicellulose or lignin and prepare inierpeneirating network structure or semi-interpenetrating network aqueous gel. Chang et al. is in alkali urea water solution system (NaOH/Urea), cellulose network is prepared for cross-linking agent with epoxychloropropane (ECH), add cross-linking agent methylene-bisacrylamide (BIS), under the initiation of Ammonium persulfate. on cellulose crosslinked network structure basis cross-linked polymeric N-isopropylacrylamide (NIPAAm) again, thus preparing full inierpeneirating network structure hydrogel. Wherein there are two converging networks simultaneously, have well-regulated loose structure, good mechanical strength and thermo-responsive. Wang [151] et al. adds NIPA monomer after utilizing LiCl/DMAc system to dissolve cellulose, with N, N-methylene-bisacrylamide (MBA) is cross-linking agent, synthesize containing poly-N,N-DMAA (DMAm) and cellulosic half interpenetrating network structure hydrogel under benzoyl peroxide (BPO) causes. The thermogravimetric testing result display semi-interpenetrating network polymer of this gel only has a heat decomposition temperature, and this illustrates there is good chemistry connection in gel structure between DMAm segment and cellulose chain segment.
Summary of the invention
In order to overcome the deficiency of background technology, the preparation method that the invention provides a kind of wood fibre temperature sensitive type semi-interpenetrating network gel material. Mainly solve existing method and prepare the problems such as lignocellulose aerogel complex process, difficulty be big.
The technical solution adopted in the present invention is: the preparation method of a kind of wood fibre temperature sensitive type semi-interpenetrating network gel material, comprises the following steps:
(1) take a certain amount of lignocellulosic material, adopt microphyte pulverizer to be ground into powder.
(2) screen a certain amount of lignocellulose powder, filter and lyophilization after immersing ethylenediamine solution at room temperature magnetic agitation 24h, obtain the lignocellulose after ethylenediamine processes;
(3) preparation LiCl/DMSO mixed solution, then the lignocellulose powder taking a certain amount of ethylenediamine pretreatment is dissolved in this solution, and under room temperature, magnetic agitation 24h obtains the lignocellulose/LiCl/DMSO solution of homogeneous thickness after being placed in 60 DEG C of constant temperature blender with magnetic force to continue stirring 2h;
(4) a certain amount of lignocellulose/LiCl/DMSO solution is taken in band plug glass tubing, then a certain amount of temperature sensitive monomer NIPA (NIPAAm) and cross-linking agent N,N methylene bis acrylamide (MBA) it are sequentially added into;
(5) nitrogen 30min is passed into, and glass tubing is statically placed in 60 DEG C of water-baths and reacts, taking out gel after 24h and put into washing by soaking in dehydrated alcohol, changing dehydrated alcohol until removing all unreacted monomers and the oligomer formed in gel, and solvent LiCl/DMSO;
(6) displace dehydrated alcohol therein lyophilization again with the tert-butyl alcohol, obtain wood fibre temperature sensitive type semi-intercrossing network aerogel material;
In preparation method technical scheme according to a kind of wood fibre temperature sensitive type semi-interpenetrating network gel material, the lignocellulosic material described in step (1) is mainly soybean stalk, hardwood pulp, Straw Pulp, softwood pulp etc., and all contain lignin and cellulosic biomass material.
In preparation method technical scheme according to a kind of wood fibre temperature sensitive type semi-interpenetrating network gel material, the lignocellulose powder filtered out described in step (2) is 40-80 order;
In preparation method technical scheme according to a kind of wood fibre temperature sensitive type semi-interpenetrating network gel material, it is characterized in that the concentration of the LiCl/DMSO mixed solution described in step (3) is 8%, the concentration of the lignocellulose powder added in LiCl/DMSO mixed solution is 1-5%.
The invention difference from existing technology is in that, the present invention achieves following technique effect: take a certain amount of wood fibre/LiCl/DMSO solution in band plug glass tubing, then a certain amount of temperature sensitive monomer NIPA (NIPAAm) and cross-linking agent N it are sequentially added into, N-methylene-bisacrylamide (MBA), azo-bis-isobutyl cyanide (AIBN) is added as initiator after stirring 10min under room temperature, continuing stirring makes the reagent added be completely dissolved final vacuum deaeration, pass into nitrogen 30min again, and glass tubing is statically placed in 60 DEG C of water-baths and reacts, take out gel after 24h and put into washing by soaking in dehydrated alcohol, change dehydrated alcohol until removing all unreacted monomers and the oligomer formed in gel, and solvent LiCl/DMSO. finally displace dehydrated alcohol therein lyophilization again with the tert-butyl alcohol, obtain aeroge. aeroge preparation method technique provided by the invention is simple, condition is gentleer, and production cost is low, the aerogel material environmental protection obtained. below in conjunction with accompanying drawing, the invention will be further described.
Accompanying drawing explanation
The electromicroscopic photograph of Fig. 1 wood fibre temperature sensitive type semi-intercrossing network aeroge, a wood fibre cellulose content is 1%, and b wood fibre cellulose content is 3%, and c wood fibre cellulose content is 5%
The infrared spectrum of Fig. 2 temperature sensitive type wood fibre gel, Stem-T-1 represents the gel rubber material that wood fibre cellulose content is 1%, and Stem-T-3 represents the gel rubber material that wood fibre cellulose content is 3%, and Stem-T-5 represents the gel rubber material that wood fibre cellulose content is 5%
Fig. 3 wood fibre gel equilibrium swelling ratio at different temperatures, Stem-T-1 represents gel rubber material that wood fibre cellulose content is 1% equilibrium swelling ratio at different temperatures, Stem-T-3 represents gel rubber material that wood fibre cellulose content is 3% equilibrium swelling ratio at different temperatures, and Stem-T-5 represents gel rubber material that wood fibre cellulose content is 5% equilibrium swelling ratio at different temperatures
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, technical matters step, it is embodied as condition and material, technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only a part of embodiment of the present invention, rather than whole embodiments. Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not paying creative work premise, broadly fall into the scope of protection of the invention.
The present invention adopts lignocellulosic material can be soybean stalk, hardwood pulp, Straw Pulp, softwood pulp etc. Following example illustrate with soybean stalk for lignocellulosic material. Soybean stalk raw material is ground into powder through microphyte pulverizer, and filters out the soybean stalk powder of 40-80 order, and the soybean stalk pretreatment of raw material of the present invention is in ethylenediamine solution magnetic agitation, and lysate adopts concentration to be 8%LiCl/DMSO mixed solution. Thermo-sensitive additive is temperature sensitive monomer NIPA (NIPAAm) and cross-linking agent N,N methylene bis acrylamide (MBA), has prepared wood fibre temperature sensitive type semi-intercrossing network aerogel material.
Embodiment 1
Take soybean stalk stem stalk part, after microphyte pulverizer is pulverized, filter out the powder of straw of 40-80 order for experiment. Soybean stalk powder removes the organic solvent extracts such as resinic acid therein, terpene compound and fatty acid after benzene-ol mixed liquor (2: 1, v/v) extracting 24h. After extracting, powder of straw is fully volatilized prior to ventilation a small amount of organic solvent of the moisture in soybean stalk powder and residual, then vacuum drying.
Embodiment 2
Weigh dry soybean stalk stem stalk raw material 10g, be ground into the powder of 40-80 order, filter and lyophilization after immersing 200ml ethylenediamine solution at room temperature magnetic agitation 24h, obtain the soybean stalk stalk powder end of ethylenediamine pretreatment.
Embodiment 3
Preparation is containing 8%LiCl/DMSO solution, then the soybean stalk powder taking a certain amount of ethylenediamine pretreatment is dissolved in this solution, the concentration of soybean stalk powder is 1%, and under room temperature, magnetic agitation 24h obtains the stem stalk/LiCl/DMSO solution of homogeneous thickness after being placed in 60 DEG C of constant temperature blender with magnetic force to continue stirring 2h.
Take the soybean stalk that concentration the is 1% powder/LiCl/DMSO solution of a certain amount of soybean stalk powder in band plug glass tubing, then a certain amount of temperature sensitive monomer NIPA (NIPAAm) and cross-linking agent N it are sequentially added into, N-methylene-bisacrylamide (MBA), azo-bis-isobutyl cyanide (AIBN) is added as initiator after stirring 10min under room temperature, continuing stirring makes the reagent added be completely dissolved final vacuum deaeration, pass into nitrogen 30min again, and glass tubing is statically placed in 60 DEG C of water-baths and reacts, take out gel after 24h and put into washing by soaking in dehydrated alcohol, every day changes dehydrated alcohol, until all unreacted monomers and the oligomer that formed in removal gel, and solvent LiCl/DMSO. finally displace dehydrated alcohol therein lyophilization again with the tert-butyl alcohol, obtain the wood fibre temperature sensitive type semi-intercrossing network aerogel material that lignocellulosic material concentration is 1%.
Embodiment 4
Preparation is containing 8%LiCl/DMSO solution, then the soybean stalk powder taking a certain amount of ethylenediamine pretreatment is dissolved in this solution, the concentration of soybean stalk powder is 3%, and under room temperature, magnetic agitation 24h obtains the stem stalk/LiCl/DMSO solution of homogeneous thickness after being placed in 60 DEG C of constant temperature blender with magnetic force to continue stirring 2h.
Take the soybean stalk that concentration the is 1% powder/LiCl/DMSO solution of a certain amount of soybean stalk powder in band plug glass tubing, then a certain amount of temperature sensitive monomer NIPA (NIPAAm) and cross-linking agent N it are sequentially added into, N-methylene-bisacrylamide (MBA), azo-bis-isobutyl cyanide (AIBN) is added as initiator after stirring 10min under room temperature, continuing stirring makes the reagent added be completely dissolved final vacuum deaeration, pass into nitrogen 30min again, and glass tubing is statically placed in 60 DEG C of water-baths and reacts, take out gel after 24h and put into washing by soaking in dehydrated alcohol, every day changes dehydrated alcohol, until all unreacted monomers and the oligomer that formed in removal gel, and solvent LiCl/DMSO. finally displace dehydrated alcohol therein lyophilization again with the tert-butyl alcohol, obtain the wood fibre temperature sensitive type semi-intercrossing network aerogel material that lignocellulosic material concentration is 3%.
Embodiment 5
Preparation is containing 8%LiCl/DMSO solution, then the soybean stalk powder taking a certain amount of ethylenediamine pretreatment is dissolved in this solution, the concentration of soybean stalk powder is 5%, and under room temperature, magnetic agitation 24h obtains the stem stalk/LiCl/DMSO solution of homogeneous thickness after being placed in 60 DEG C of constant temperature blender with magnetic force to continue stirring 2h.
Take the soybean stalk that concentration the is 1% powder/LiCl/DMSO solution of a certain amount of soybean stalk powder in band plug glass tubing, then a certain amount of temperature sensitive monomer NIPA (NIPAAm) and cross-linking agent N it are sequentially added into, N-methylene-bisacrylamide (MBA), azo-bis-isobutyl cyanide (AIBN) is added as initiator after stirring 10min under room temperature, continuing stirring makes the reagent added be completely dissolved final vacuum deaeration, pass into nitrogen 30min again, and glass tubing is statically placed in 60 DEG C of water-baths and reacts, take out gel after 24h and put into washing by soaking in dehydrated alcohol, every day changes dehydrated alcohol, until all unreacted monomers and the oligomer that formed in removal gel, and solvent LiCl/DMSO. finally displace dehydrated alcohol therein lyophilization again with the tert-butyl alcohol, obtain 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 detailed description of the invention, but the invention thought of the present invention is not limited to that invention, the repacking of any utilization inventive concept, all will include in this patent scope of patent protection.
Claims (4)
1. the preparation method of a wood fibre temperature sensitive type semi-interpenetrating network gel material, it is characterised in that comprise the following steps:
(1) take a certain amount of lignocellulosic material, adopt microphyte pulverizer to be ground into powder;
(2) screen a certain amount of lignocellulose powder, filter and lyophilization after immersing ethylenediamine (EDA) solution at room temperature magnetic agitation 24h, obtain the lignocellulose after ethylenediamine processes;
(3) preparation LiCl/DMSO mixed solution, then the lignocellulose powder taking a certain amount of ethylenediamine pretreatment is dissolved in this solution, and under room temperature, magnetic agitation 24h obtains the lignocellulose/LiCl/DMSO solution of homogeneous thickness after being placed in 60 DEG C of constant temperature blender with magnetic force to continue stirring 2h;
(4) a certain amount of lignocellulose/LiCl/DMSO solution is taken in band plug glass tubing, then a certain amount of temperature sensitive monomer NIPA (NIPAAm) and cross-linking agent N,N methylene bis acrylamide (MBA) it are sequentially added into;
(5) nitrogen 30min is passed into, and glass tubing is statically placed in 60 DEG C of water-baths and reacts, taking out gel after 24h and put into washing by soaking in dehydrated alcohol, changing dehydrated alcohol until removing all unreacted monomers and the oligomer formed in gel, and solvent LiCl/DMSO;
(6) displace dehydrated alcohol therein lyophilization again with the tert-butyl alcohol (TBA), obtain wood fibre temperature sensitive type semi-intercrossing network aerogel material.
2. the preparation method according to a claim 1 wood fibre temperature sensitive type semi-interpenetrating network gel material, it is characterised in that the lignocellulosic material described in step (1) is mainly soybean stalk, wood powder, grass meal, wood pulp, straw pulp etc., and all include lignin and cellulosic biomass material.
3. the preparation method according to a claim 1 wood fibre temperature sensitive type semi-interpenetrating network gel material, it is characterised in that the lignocellulose powder filtered out described in step (2) is 40-80 order.
4. the preparation method according to a claim 1 wood fibre temperature sensitive type semi-interpenetrating network gel material, it is characterized in that the concentration of the LiCl/DMSO mixed solution described in step (3) is 8%, the concentration of the lignocellulose powder added in LiCl/DMSO mixed solution is 1-5%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106433671A (en) * | 2016-09-12 | 2017-02-22 | 巢湖春友种业科技有限公司 | Soil fertilizer loss rate reducible soil modifier and preparation method thereof |
| CN109134914A (en) * | 2018-07-12 | 2019-01-04 | 厦门大学 | A kind of preparation method of dual-sensitivity cellulose base aeroge |
| CN114854081A (en) * | 2022-03-25 | 2022-08-05 | 华南理工大学 | Underwater super-oleophobic lignin/cellulose high-strength aerogel and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328067A (en) * | 2001-06-29 | 2001-12-26 | 清华大学 | Process for preparing temp-sensitive porous poly(N-isopropyl acrylamide) aqueogel |
| CN1586706A (en) * | 2004-07-08 | 2005-03-02 | 东华大学 | Method for preparing quick temperature response semi-interpenetration network hydrogel |
| CN101070365A (en) * | 2007-05-22 | 2007-11-14 | 华南理工大学 | N-isopropyl acrylamide thermosensitive aquagel and its microwave radiation preparing method |
| CN102229732A (en) * | 2011-05-11 | 2011-11-02 | 东华大学 | Method for preparing semi-interpenetrating-network-structure-based pH stimulus response nano hydrogel |
-
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- 2015-11-27 CN CN201510852212.7A patent/CN105622869B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1328067A (en) * | 2001-06-29 | 2001-12-26 | 清华大学 | Process for preparing temp-sensitive porous poly(N-isopropyl acrylamide) aqueogel |
| CN1586706A (en) * | 2004-07-08 | 2005-03-02 | 东华大学 | Method for preparing quick temperature response semi-interpenetration network hydrogel |
| CN101070365A (en) * | 2007-05-22 | 2007-11-14 | 华南理工大学 | N-isopropyl acrylamide thermosensitive aquagel and its microwave radiation preparing method |
| CN102229732A (en) * | 2011-05-11 | 2011-11-02 | 东华大学 | Method for preparing semi-interpenetrating-network-structure-based pH stimulus response nano hydrogel |
Non-Patent Citations (2)
| Title |
|---|
| ZHIGUO WANG等: "Cellulose gel and aerogel from LiCl/DMSO solution", 《CELLULOSE》 * |
| 王璟: "在LiCl/DMAc体系中制备环境敏感型纤维素水凝胶", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106433671A (en) * | 2016-09-12 | 2017-02-22 | 巢湖春友种业科技有限公司 | Soil fertilizer loss rate reducible soil modifier and preparation method thereof |
| CN109134914A (en) * | 2018-07-12 | 2019-01-04 | 厦门大学 | A kind of preparation method of dual-sensitivity cellulose base aeroge |
| CN109134914B (en) * | 2018-07-12 | 2020-04-21 | 厦门大学 | Preparation method of double-sensitivity cellulose-based aerogel |
| CN114854081A (en) * | 2022-03-25 | 2022-08-05 | 华南理工大学 | Underwater super-oleophobic lignin/cellulose high-strength aerogel and preparation method and application thereof |
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