CN110028624A - Preparation method and application based on hemicellulose compound temperature-sensitive gel - Google Patents

Preparation method and application based on hemicellulose compound temperature-sensitive gel Download PDF

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CN110028624A
CN110028624A CN201910302977.1A CN201910302977A CN110028624A CN 110028624 A CN110028624 A CN 110028624A CN 201910302977 A CN201910302977 A CN 201910302977A CN 110028624 A CN110028624 A CN 110028624A
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hemicellulose
bagasse
water
isopropyl acrylamide
sensitive gel
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唐晓宁
刘高喆
高欣
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F251/00Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof

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Abstract

The invention discloses a kind of preparation methods based on hemicellulose compound temperature-sensitive gel, this method grinds and sieves air-dried bagasse, obtain bagasse powder raw material, and with alkali assist hot-water extraction method, by the hemicellulose dissolution in bagasse, followed by aqueous solution micell polymerization method, n-isopropyl acrylamide and propyl acrylate are subjected to graft copolymerization, then hemicellulose is added, and with N, copolymer and hemicellulose are crosslinked by N- methylene-bisacrylamide, product is through cutting, cleaning, it is cold it is dry after obtain poly-N-isopropyl acrylamide grafted propylene propyl propionate/temperature sensitive plural gel of hemicellulose;The gel as made from this method is to the pentachlorophenol adsorption capacity with higher in organic wastewater.

Description

Preparation method and application based on hemicellulose compound temperature-sensitive gel
Technical field
The present invention relates to one kind by poly-N-isopropyl acrylamide graft copolymerization propyl acrylate and the compound system of hemicellulose The method of standby thermo-sensitive gel, belongs to high-molecular compounded and modified field of material technology.
Background technique
Sponge contains the hemicellulose of about 15-35%, and most of hemicellulose is gone in pulp stage It removes, remains in waste liquid.The calorific value of hemicellulose is 13.6 MJ/kg, is the half of lignin.Modern slurrying and paper maker Sulphate cook technique in industry usually burns the hemicellulose in waste liquid, and preparation produces required steam to utilize.This The mode of kind processing hemicellulose is not fully developed this saccharoidal property, is a kind of great wasting of resources.Currentization Stone resource is almost exhausted, particularly important to natural polymer, such as the effective use of hemicellulose.Existing preextraction hemicellulose Method mainly include physical method, chemical method and biological method.Specifically, having diluted acid extraction, water hot extraction, steam quick-fried Broken extraction, alkali extraction and dilute acid steam explosion etc..However, the process conditions that diluted acid extracts hemicellulose are difficult to control, cellulose Hydrolysis can reduce pulping yield;In steam blasting extraction process, though extractable obtain a large amount of hemicellulose, cellulose Structure can be destroyed, and be unfavorable for the promotion of paper strength.The operating cost that alkali carries take is high, and a large amount of alkali and acids chemicals need It is added in system, the adjusting for pH.Hot water extraction hemicellulose can effectively reduce cost and environmental pollution, and hot water is molten Solve extracting hemicelluloses after can also quickly with other polymer substances, for example, cellulose and lignin are separated.Hot water extraction Method has the shorter reaction time, and higher acid concentration and higher temperature etc. react advantage, favorably generate more xyloses Monomer.The concentrated extract of the hemicellulose of extraction can be separated with the mode that film filters, this is avoided that using high concentration Acid.
Hemicellulose is the second largest carbohydrate high polymer for constituting plant cell wall construction, and content is only second to fiber Element, but it is different from the cellulose of homogeneous polysaccharide.Hemicellulose is a kind of heteroglycan being made of different types of monosaccharide.These Monosaccharide mainly has xylose, glucose, mannose, galactolipin, arabinose, glucuronic acid and galacturonic acid etc.[3].In structure When at hemicellulose, uniform monosaccharide is not constituted with a kind of connection type with a kind of monosaccharide, by two or more monosaccharide with A variety of connection types constitute branched heteroglycan.Hemicellulose is a kind of carbon hydrate that content is more in plant fiber material Object, its content in needlebush are 25%~35%, and the content in leaf wood is 18%~22%, and in gramineae plant Content is 16 %~25%.In recent years, becoming increasingly conspicuous with energy problem, hemicellulose are gradually considered most rich on the earth Rich, most cheap one of renewable resource;There are significant differences for its hemicellulose level of different types of plant and structure.Its In, needlebush mainly contains polydextrose mannose, and leaf wood and grass as raw material mainly contain xylan and polyglucuronic acid Branch, and the xylan branch in leaf wood is mainly acetyl group.
Sugarcane is the important sugar crop of China, and bagasse is the main waste (accounting for 24%~27%) of sugar industry, It is a kind of important renewable biomass raw material.Sugarcane is the sugaring raw material of Largest In China, southern sugarcane district sugarcane total output 7000t, the bagasse yield generated every year is about 2000t, utilizes space and potentiality with very big.With other crop material phases Than hemicellulose level is higher in bagasse.Since bagasse converts and utilizes the limitation of technology, current most of bagasse quilts It directly burns or passes into disuse, utilization rate is very low, not only results in waste of resources, but also bring environmental pollution.In recent years, Attention due to country to agricultural waste utilization, Comprehensive Utilization of Bagasse aspect also obtain quick development.Due to biology The fast development of matter trans-utilization engineering technology, it has been found that bagasse is not only natural macromolecular material, green chemical Treasure-house, wherein the biomass energy that is also richly stored with.Therefore, how to have been obtained using bagasse production renewable energy bigger Concern.Is produced from the second largest province Yunnan of sugar as China, there are about the bagasses of 170t within 1 year.Bagasse is product of the sugarcane by squeezing, Also belong to the scope of crop material.It is up to 25 %~30% of hemicellulose in bagasse, can be used as the desirable feedstock of hemicellulose.
Hydrogel is the cross-linked polymer using water as decentralized medium, when its into the water when can absorb a large amount of moisture, It is swollen rapidly and is not dissolved.Based on good characteristics such as hydrogel high-efficiency water-absorbing, water conservation and biodegradables, cured in biology It is used widely in the fields such as medicine, food, agricultural, environment.The preparation method of hemicellulose based aquagel can generally speaking be divided into Chemical crosslink technique and physical crosslinking method.In contrast, chemical gel is more more stable than physical gel.Hydrogel is that one kind can be in water It is swollen and undissolved three-dimensional network shape hydrophilic polymer, since a large amount of hydrophilic radicals are contained in inside, can absorb and keep big Moisture is measured, and the presence of cross-linked network can make it that original shape be kept to be not dissolved after water absorption and swelling.Hydrogel is hydrophilic Property but polymer not soluble in water, the multicomponent system being made of high molecular three-dimensional network and water.According to hydrogel to the external world The response condition of stimulation can be divided into conventional hydrogels and intelligent aqueous gel.Intelligent aqueous gel is that one kind can produce environmental stimuli The hydrogel of raw sensitive response.Typical environmental stimuli has temperature, pH value, solvent, salinity, light, electric field, chemical substance etc.. Due to progress in Intelligent Hydrogel chemical converter, memory cell switch, sensor, the control delivery systme of drug, artificial muscle, The potential application of the embedding of chemical storage device, molecule separation system, organized enzyme etc., thus to the research of intelligent aqueous gel Through the big hot spot for becoming functional polymer research field.And temperature-sensitive hydrogel is that one kind can be by quick stereomutation The progress in Intelligent Hydrogel material that extraneous temperature change is responded.This kind of hydrogel can occur discontinuous within specified temperatures Volume-phase transition, this temperature is referred to as lower critical solution temperature (LCST).When temperature is lower than LCST, hydrogel is in molten Swollen state, however, when being higher than the temperature, the rapid dehydration shrinkage of hydrogel, to show the responsiveness to temperature.Poly- (N- N-isopropylacrylamide) (PNIPA) hydrogel is to study most commonly used temperature-sensitive hydrogel at present, the LCST in pure water Temperature is 32 DEG C, close with body temperature, thus is had broad application prospects in biomedical materials field.From 1986 Since Pelton synthesizes n-isopropyl acrylamide, has become and studied widest temperature sensitive type polymer at present.2018 It is crosslinking agent that Hu Yaoqiang seminar, which develops using n-isopropyl acrylamide as monomer, N,N methylene bis acrylamide, over cure Sour potassium is initiator, prepares thermo-sensitive gel using no emulsion polymerization;2018 Nian Duan head seminars are different with houghite and N- Propylacrylamide is raw material, and organic-inorganic PNIPA/LDHs temperature sensitivity Compound Water has been made using free radical polymerization Gel, the results showed that, the invertibity variation of collosol and gel can be achieved at 33 DEG C or so for PNIPA/LDHs composite hydrogel;, Chu etc. Graphene oxide is introduced into PNIPA hydrogel, obtains and extends with temperature sensitivity and the high of near-infrared response performance Property hydrogel.But for hemicellulose, hemicellulose and the compound preparation hydrophobicity of n-isopropyl acrylamide are temperature sensitive solidifying Glue has not been reported.
Pentachlorophenol (PCP) is a kind of persistence organic pollutant, is widely used as fungicide, algicide, insecticide, weeding Agent and timber preservative, it was reported that they can cause the mutation of allergy, stimulation, dermatitis, cancer and human gene.Pentachlorophenol It can be detected in surface water, deposit, aquatile, topsoil and human milk, and since it has biology product The features such as tired property and environmental persistence, the negative effect to the mankind and animals and plants health is still a crucial environmental problem. In addition, pentachlorophenol can be with long-distance migration and there are a very long time in environment, as the accumulation of their concentration can be to fish Class, wild animal and the mankind cause undesirable health effect, it is therefore necessary to remove pentachlorophenol before organic wastewater discharges.Mesh Preceding to have developed many methods removal PCP, such as absorption aoxidizes, microbial degradation, due to its water solubility, by with Upper traditional physics and chemical method cannot effectively remove them, therefore absorption is considered as a kind of relative efficiency removal The method of PCP.
The organic wastewater pollution problem in conjunction with caused by modern industry, the application, which is described in detail to prepare using bagasse as raw material, efficiently to inhale The process flow of the thermo-sensitive gel of Annex V chlorophenol;It is not only to make up n-isopropyl acrylamide class thermo-sensitive gel in organic wastewater The vacancy of adsorption treatment research, and the comprehensive utilization ratio of bagasse resource is improved, it is that the high value added utilization of bagasse rises To positive impetus.
Summary of the invention
The new way of high value added utilization is provided for resourceful Bagasse Material, while in efficiently removal organic wastewater Pentachlorophenol, the present invention provides a kind of preparation method based on hemicellulose compound temperature-sensitive gel, this method utilizes resource Abundant bagasse obtains half fiber with ethyl alcohol precipitating, centrifuge separation and freeze-drying by sodium hydroxide water hot extraction's method for raw material Dimension element, using aqueous solution micell polymerization method by n-isopropyl acrylamide graft copolymerization propyl acrylate, and is cross-linked to form temperature sensitive Hydrogel product further expands the application field of Bagasse Hemicellulose and thermo-sensitive gel.
The process technology scheme for realizing that the object of the invention is taken is as follows:
1. being ground to the bagasse raw material after air-drying, screening process, qualified bagasse powder raw material is obtained;
2. dissolve out using the method that alkali assists hot-water extraction by hemicellulose in bagasse powder raw material, and with alcohol precipitating, film divides From and washing, obtain hemicellulose after freeze-drying;
3. utilizing aqueous solution micell polymerization method, n-isopropyl acrylamide and propyl acrylate are subjected to graft copolymerization, after And hemicellulose being added, and with N, copolymer and hemicellulose are crosslinked by N- methylene-bisacrylamide, and reaction terminates, and are coagulated Glue cut, cleaned, be lyophilized after to obtain poly-N-isopropyl acrylamide grafted propylene propyl propionate/hemicellulose temperature sensitive compound solidifying Glue (PNIPA-co-PA/Hemic).
Above method concrete operations are as follows:
(1) melting process of bagasse: bagasse is after air-drying processing, wherein air-drying the moisture of raw material because of different ground Area, different seasons and air humidity are different and generate certain difference, general moisture control in the range of 3~30%, Air dry matter is ground, and is crossed after the screening of 40 ~ 200 mesh sieve as bagasse powder raw material;
(2) treatment process of bagasse hemicellulose: bagasse powder raw material, water, sodium hydroxide being mixed, are put into reactor tank, 30 ~ 90 min are reacted under conditions of 150 ~ 200 DEG C, wherein the mass ratio of over dry bagasse powder and water is 1:5 ~ 1:10, over dry sugarcane The mass ratio of ground-slag end and sodium hydroxide is 100:1 ~ 100:10, and after reaction, reactor tank cools down rapidly in water, reactant It is separated by solid-liquid separation, dehydrated alcohol precipitating is poured into filtrate, then filtered with the film of 0.35 ~ 0.65 nm, dehydrated alcohol washing is frozen Bagasse hemicellulose is obtained after dry
(3) synthesis of PNIPA-co-PA/Hemic thermo-sensitive gel
By n-isopropyl acrylamide and N, the mass ratio of N- methylene-bisacrylamide is the ratio of 15:1 ~ 30:1, and N- is different Propylacrylamide and N, N- methylene-bisacrylamide are dissolved in deionized water, are transferred in reaction vessel, then by third Dispersion and dissolution is added into reaction vessel in olefin(e) acid propyl ester and hemicellulose, after leading to 15 ~ 30min of nitrogen purge gas, then successively adds Enter neopelex, ammonium persulfate, tetramethylethylenediamine, sealed reaction vessel, in 45 ~ 65 DEG C of constant temperature water bath device React 12 ~ 36 h;Hydrogel obtained is taken out, 24 ~ 48h is impregnated after stripping and slicing in dehydrated alcohol, impregnates 3 in deionized water ~ 8 days, every 10 ~ 15h replaced a water, is made after freeze-drying and is based on hemicellulose compound temperature-sensitive gel PNIPA-co-PA/Hemic, Wherein the mass volume ratio g:mL of n-isopropyl acrylamide and deionized water is 3:8 ~ 1:5, and neopelex adds Dosage is the 3 ~ 8% of deionized water quality, and ammonium persulfate: tetramethylethylenediamine: the mass ratio of n-isopropyl acrylamide is 0.02:0.01:1~0.2:0.1:1;
The additive amount of the propyl acrylate is the 5 ~ 20% of the quality of n-isopropyl acrylamide;The additive amount of hemicellulose is The 3 ~ 15% of the quality of n-isopropyl acrylamide.
The present invention by hemicellulose compound temperature-sensitive gel application is based on made from the above method in removal another object is that have In machine waste water in pentachlorophenol.
The beneficial effects of the present invention are: tradition, harmful, method complicated for operation have been cast aside in bagasse hemicellulose extraction, turn To cleaning, efficient, the easy new way of operation;Reagent itself does not generate any harmful substance to environment during the reaction, and And the Action advantage of the complementary purification hemicellulose of plurality of reagents is concentrated.Using aqueous solution micell polymerization method, synthesis is poly- N-isopropyl acrylamide graft copolymerization acrylic acid is total to propyl ester (PNIPAM-PA), and it is carried out hemicellulose it is compound, crosslinking make With the hydrophobic water gel for obtaining that there is temperature-sensing property;The synthesis macromolecule composite natral high-molecular gel has synthesis macromolecule The general character of class adsorbent material, can be in multiple industries such as petrochemical industry refining, agriculture weeding, weaving, leather manufacture, paper and timber processing Good application prospect is played in terms of the processing of generated pentachlorophenol organic liquid waste.Meanwhile the temperature sensitive suction of the hemicellulose group It is excellent that attached gel is also equipped with temperature sense performance, hypotoxicity, good absorption property, environment friendly and cheap price etc. Gesture, is novel, the green functional material of one kind of mainstream development now, this attractive gel is embodied as bagasse high value added utilization One feasible scheme is provided, while also providing certain application foundation for the functionalization exploitation of waste agronomic crop.
Specific embodiment
Below with reference to embodiment, invention is further described in detail, but the scope of the present invention is not limited in described Hold.
The preparation method of the modified temperature-sensitive hydrogel of embodiment 1:PNIPA-co-PA/Hemic, concrete operations are as follows:
(1) melting process of bagasse
Bagasse is after air-drying processing, and moisture content 3%, air dry matter is ground, and is after the screening of the sieve of 40 ~ 60 mesh Bagasse powder raw material;
(2) treatment process of bagasse hemicellulose
By 1.03g bagasse powder raw material (if air-drying raw material moisture is 3%, 1 g of over dry Bagasse Material, then 1/(100-3) %= 1.03 g bagasse powder raw materials), water, sodium hydroxide mixing, be put into reactor tank, react 90min under conditions of 150 DEG C, Middle 1.00 g of over dry bagasse powder, the dosage of water are 5.00 g, 0.01 g of dosage of sodium hydroxide;After reaction, reactor tank It cools down in water rapidly, reactant is separated by solid-liquid separation using 350 mesh industry screen cloths, dehydrated alcohol precipitating is poured into filtrate, is adopted It is washed with the filtering of the film of 0.35 nm and dehydrated alcohol, after freeze-drying, obtains bagasse hemicellulose;
(3) synthesis of PNIPA-co-PA/Hemic thermo-sensitive gel
The n-isopropyl acrylamide of 3.00 g and 0.20 g N,N methylene bis acrylamide are dissolved in the deionization of 8 mL It in water, is transferred in reaction tube, then by 0.15 g propyl acrylate (matter of 5 wt% relative to n-isopropyl acrylamide Measure, then 3 × 5%=0.15g propyl acrylate) and 0.09 g hemicellulose (3% quality relative to n-isopropyl acrylamide, then 3 × 3%=0.09 g), is transferred in test tube and disperses and dissolve;Then, after leading to nitrogen purge gas 15min, 0.24 is being sequentially added G neopelex (SDBS, 3% relative to water in system, then 8 × 3%=0.24 g neopelex), 0.06 g ammonium persulfate (APS) and 0.03 g tetramethylethylenediamine (TEMED), plug test tube with plug;In 45 DEG C of water-bath 36h is reacted in thermostat;The hydrogel of preparation is taken out, is cut into a thickness of the disk of 0.20 cm;Then it is soaked in dehydrated alcohol 24 h are steeped, are impregnated 3 days in deionized water, every 10 h replaces a water, and it is temperature sensitive solidifying that PNIPA-co-PA/Hemic is obtained after freeze-drying Glue;
(4) absorption property of thermo-sensitive gel
Pentachlorophenol determining adsorption method: 0.1 mol/L HCl is mixed into pentachlorophenol solution, and pH value is adjusted to 3; To measure gel adsorption effect, 100 mg PNIPA-co-PA/Hemic thermo-sensitive gels are added 0.05 mmol/L's of 50mL In PCP simulated wastewater for 24 hours;The concentration of pentachlorophenol before and after adsorption treatment is measured by high performance liquid chromatography;It obtains PNIPA-co-PA/Hemic thermo-sensitive gel has stronger adsorption capacity to pentachlorophenol, and adsorption rate is up to 75%.
The preparation method of the modified temperature-sensitive hydrogel of embodiment 2:PNIPA-co-PA/Hemic, concrete operations are as follows:
(1) melting process of bagasse:
Bagasse is after air-drying processing, and moisture content 15%, air dry matter is ground, after the screening of the sieve of 100 ~ 120 mesh For bagasse powder raw material;
(2) treatment process of bagasse hemicellulose:
By 1.18 g bagasse powder raw materials (if air-drying raw material moisture is 15%, over dry bagasse powder 1g, then 1/(100-15) %= 1.18 g bagasse powder raw materials), water, sodium hydroxide mixing, be put into reactor tank, react 60min under conditions of 180 DEG C, Middle 1.00 g of over dry bagasse powder, the dosage of water are 7.00 g, and the dosage of sodium hydroxide is 0.05 g, after reaction, reaction Tank cools down rapidly in water, is separated by solid-liquid separation reactant using 400 mesh industry screen cloths, absolute alcohol precipitating is poured into filtrate, Bagasse hemicellulose is obtained using the film filtering and dehydrated alcohol washing, Leng Ganhou of 0.50 nm;
(3) synthesis of PNIPA-co-PA/Hemic thermo-sensitive gel:
By the n-isopropyl acrylamide of 3.00 g and 0.15 g N,N methylene bis acrylamide be dissolved in 10 mL go from It in sub- water, is transferred in reaction tube, then by 0.36g propyl acrylate (12% matter relative to n-isopropyl acrylamide Measure, then 3 × 12%=0.36g propyl acrylate) and 0.30g hemicellulose (10% quality relative to n-isopropyl acrylamide, Then 3 × 10%=0.30g), it is transferred in test tube and disperses and dissolve;Then, it after leading to 20 min of nitrogen purge gas, sequentially adds (SDBS, 5% relative to water in system, then 10 × 5%=0.50g dodecyl benzene sulfonic acid for 0.50g neopelex Sodium), 0.21 g ammonium persulfate (APS) and 0.18 g tetramethylethylenediamine (TEMED), plug test tube with plug;At 50 DEG C 20h is reacted in constant temperature water bath device;The hydrogel of preparation is taken out, is cut into a thickness of the disk of 0.40 cm;Then, in anhydrous second 36 h are impregnated in alcohol, are impregnated 5 days in deionized water, and every 12 h replaces a water, and Leng Ganhou obtains PNIPA-co-PA/Hemic Thermo-sensitive gel;
(4) absorption property of thermo-sensitive gel
Pentachlorophenol determining adsorption method: 0.1mol/L HCl is mixed into pentachlorophenol solution, and pH value is adjusted to 3; To measure gel adsorption effect, 100 mg PNIPA-co-PA/Hemic thermo-sensitive gels are added 50 mL, 0.05 mmol/L's In PCP simulated wastewater for 24 hours;The concentration of pentachlorophenol before and after adsorption treatment is measured by high performance liquid chromatography;It obtains PNIPA-co-PA/Hemic thermo-sensitive gel has stronger adsorption capacity to pentachlorophenol, and adsorption rate is up to 99%.
The preparation method of the modified temperature-sensitive hydrogel of embodiment 3:PNIPA-co-PA/Hemic, concrete operations are as follows:
(1) melting process of bagasse:
Bagasse is after air-drying processing, and moisture content 30%, air dry matter is ground, after the screening of the sieve of 180 ~ 200 mesh For bagasse powder raw material;
(2) treatment process of bagasse hemicellulose:
By 1.43 g bagasse powder raw materials (if air-drying raw material moisture is 30%, over dry bagasse powder 1g, then 1/(100-30) %= 1.43 g bagasse powder raw materials), water, sodium hydroxide mixing, be put into reactor tank, react 30min under conditions of 200 DEG C, Middle 1.00 g of over dry bagasse powder, the dosage of water are 10.00 g, and the dosage of sodium hydroxide is 0.10 g;After reaction, it reacts Tank cools down rapidly in water, is separated by solid-liquid separation reactant using 500 mesh industry screen cloths, dehydrated alcohol precipitating is poured into filtrate, Bagasse hemicellulose is obtained using the film filtering and dehydrated alcohol washing, Leng Ganhou of 0.65 nm;
(3) synthesis of PNIPA-co-PA/Hemic thermo-sensitive gel:
By the n-isopropyl acrylamide of 3.00 g and 0.10 g N,N methylene bis acrylamide be dissolved in 15 mL go from It in sub- water, is transferred in reaction tube, then by 0.60 g propyl acrylate (20% matter relative to n-isopropyl acrylamide Measure, then 3 × 20%=0.60 g propyl acrylate) and 0.45 g hemicellulose (15% matter relative to n-isopropyl acrylamide Amount, then 3 × 15%=0.45 g), is transferred in test tube and disperses and dissolve;Then, it after leading to 30 min of nitrogen purge gas, sequentially adds (SDBS, 8% relative to water in system, then 10 × 8%=0.80 g dodecyl benzene sulfonic acid for 0.80 g neopelex Sodium), 0.60 g ammonium persulfate (APS) and 0.30 g tetramethylethylenediamine (TEMED), plug test tube with plug;At 65 DEG C 15h is reacted in constant temperature water bath device;The hydrogel of preparation is taken out, is cut into a thickness of the disk of 0.60 cm;Then in dehydrated alcohol 48 h of middle immersion impregnate 8 days in deionized water, and every 15 h replaces a water, and Leng Ganhou obtains PNIPA-co-PA/Hemic temperature Quick gel;
(4) absorption property of thermo-sensitive gel
Pentachlorophenol determining adsorption method: 0.1 mol/L HCl is mixed into pentachlorophenol solution, and pH value is adjusted to 3; To measure gel adsorption effect, 100 mg PNIPA-co-PA/Hemic thermo-sensitive gels are added 50 mL, 0.05 mmol/L's In PCP simulated wastewater for 24 hours;Wherein the concentration of the pentachlorophenol before and after adsorption treatment is measured by high performance liquid chromatography.? PNIPA-co-PA/Hemic thermo-sensitive gel has stronger adsorption capacity to pentachlorophenol out, and adsorption rate is up to 88%.

Claims (5)

1. a kind of preparation method based on hemicellulose compound temperature-sensitive gel, it is characterised in that carry out as follows:
1. being ground to the bagasse raw material after air-drying, screening process, qualified bagasse powder raw material is obtained;
2. dissolve out using the method that alkali assists hot-water extraction by hemicellulose in bagasse powder raw material, and with alcohol precipitating, film divides From and washing, obtain hemicellulose after freeze-drying;
3. utilizing aqueous solution micell polymerization method, n-isopropyl acrylamide and propyl acrylate are subjected to graft copolymerization, after And hemicellulose being added, and with N, copolymer and hemicellulose are crosslinked by N- methylene-bisacrylamide, and reaction terminates, and are coagulated Glue cut, cleaned, be lyophilized after to obtain poly-N-isopropyl acrylamide grafted propylene propyl propionate/hemicellulose temperature sensitive compound solidifying Glue.
2. the preparation method based on hemicellulose compound temperature-sensitive gel according to claim 1, it is characterised in that concrete operations It is as follows:
1. bagasse is after air-drying processing, moisture control 3~30%, ground by air dry matter, crosses 40 ~ 200 mesh sieve sieve It is bagasse powder raw material after choosing;
2. by bagasse powder raw material, water, sodium hydroxide mix, be put into reactor tank, under conditions of 150 ~ 200 DEG C react 30 ~ 90 min, wherein the mass ratio of over dry bagasse powder and water is 1:5 ~ 1:10, the mass ratio of over dry bagasse powder and sodium hydroxide For 100:1 ~ 100:10, after reaction, reactor tank cools down rapidly in water, and reactant is separated by solid-liquid separation, and nothing is poured into filtrate Then water-ethanol precipitating is filtered with the film of 0.35 ~ 0.65 nm, dehydrated alcohol washing obtains bagasse hemicellulose after freeze-drying;
3. pressing n-isopropyl acrylamide and N, the mass ratio of N- methylene-bisacrylamide is the ratio of 15:1 ~ 30:1, by N- N-isopropylacrylamide and N, N- methylene-bisacrylamide are dissolved in deionized water, are transferred in reaction vessel, then will Dispersion and dissolution is added into reaction vessel in propyl acrylate and hemicellulose, after leading to 15 ~ 30min of nitrogen purge gas, then successively Neopelex, ammonium persulfate, tetramethylethylenediamine, sealed reaction vessel, in 45 ~ 65 DEG C of constant temperature water bath device is added 12 ~ 36 h of middle reaction;Hydrogel obtained is taken out, 24 ~ 48h is impregnated after stripping and slicing in dehydrated alcohol, soaks in deionized water Bubble 3 ~ 8 days, every 10 ~ 15h replace a water, are made after freeze-drying and are based on hemicellulose compound temperature-sensitive gel, wherein N- isopropyl third The mass volume ratio g:mL of acrylamide and deionized water is 3:8 ~ 1:5, and the additive amount of neopelex is deionized water 3 ~ 8 % of quality, ammonium persulfate: tetramethylethylenediamine: the mass ratio of n-isopropyl acrylamide is 0.02:0.01:1 ~ 0.2: 0.1:1。
3. the preparation method according to claim 2 based on hemicellulose compound temperature-sensitive gel, it is characterised in that: acrylic acid The additive amount of propyl ester is the 5 ~ 20% of the quality of n-isopropyl acrylamide.
4. the preparation method according to claim 2 based on hemicellulose compound temperature-sensitive gel, it is characterised in that: hemicellulose The additive amount of element is the 3 ~ 15% of the quality of n-isopropyl acrylamide.
5. compound based on hemicellulose made from the preparation method based on hemicellulose compound temperature-sensitive gel described in claim 1-4 Application of the thermo-sensitive gel in removal organic wastewater in pentachlorophenol.
CN201910302977.1A 2019-04-16 2019-04-16 Preparation method and application based on hemicellulose compound temperature-sensitive gel Pending CN110028624A (en)

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