CN102268105A - Environment-friendly hemicellulose water absorbent and preparation method thereof - Google Patents
Environment-friendly hemicellulose water absorbent and preparation method thereof Download PDFInfo
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- CN102268105A CN102268105A CN 201110228447 CN201110228447A CN102268105A CN 102268105 A CN102268105 A CN 102268105A CN 201110228447 CN201110228447 CN 201110228447 CN 201110228447 A CN201110228447 A CN 201110228447A CN 102268105 A CN102268105 A CN 102268105A
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Abstract
The invention discloses an environment-friendly hemicellulose water absorbent and a preparation method thereof. The preparation method of the water absorbent comprises: dry-grinding bambusa textilt into powder, extracting under vacuum by using mixed solvent of toluene and ethanol, adding sodium chlorite and distilled water into residues, regulating the pH value, extracting under vacuum, filtering, washing the filter residue with alcohol, drying, extracting with KOH solution, filtering, regulating the pH value to 5.5, precipitating in ethanol, washing the precipitate with alcohol, drying and obtaining hemicelluloses; and dissolving the hemicelluloses in distilled water, adding an initiator, acrylic acid and cross-linking agent in an atmosphere of inert gas, uniformly mixing, heating, cooling, washing a coarse product, drying under vacuum, and obtaining the hemicellulose water absorbent. The water absorbent prepared by the invention has high biocompatibility, high water absorption efficiency, high sustained-release and water-holding capacity and bright prospect and is free from toxin and biodegradable. In the invention, the process is simple, the reaction conditions are easy to control, the industrialization is easy, and environment pollution in a production process is avoided.
Description
Technical field
The invention belongs to the water-absorbing material field, relate to hemicellulose modification and High hydrophilous resin, be specifically related to a kind of environment-friendly type hemicellulose water-retaining agent and preparation method thereof.
Background technology
Hydrogel is a kind of wetting ability but water-fast high molecular polymer.They can be swelling to balance rapidly in water, and still can keep its shape and three-dimensional space network structure, and the deswelling that can dewater under certain condition again is a class set suction, water conservation, slowly-releasing is in one and develop functional high molecule material rapidly.Be widely used in fields such as industry, agricultural, medicine and biological engineering material.
High absorbency material is different with traditional water-absorbing material.Traditional water-absorbing material water-retaining capacity is little, can only absorb several times to tens times water of sole mass, and water retention capacity is also poor.And high-absorbent material can absorb the hundred times of sole mass and even thousands of times water, not only has good water absorbing properties, and has remarkable water retention capacity.
In recent years, hemicellulose is studied as the biomass-based material of preparation and a series of novel degradable polymkeric substance.The Application Areas of exploitation mainly comprises food and biomedical sector at present.The film that the hemicellulose of modifications such as plasticizing, esterification, graft polymerization forms increases significantly than unmodified membrane at aspects such as barrier, mechanical mechanics properties, laminated film particularly, being expected to is becoming the novel environment friendly material aspect packaging material for food and the food/edibility coating film.In addition, hemicellulose can be used for biomedical sector with its biological activity and biocompatibility, especially the key areas of medicament slow release and organizational project.Gel as xylan and chitosan formation is expected to be applied to aspects such as drug release; The hemicellulose hydrogel has tempting application prospect in fields such as protein load and release, colon position targeting drug releases.
At present, the report that does not prepare the environment-friendly type super strength water absorbent as yet relevant for hemicellulose.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of environment-friendly type water-retaining agent and preparation method thereof is provided.Water-retaining agent of the present invention is nontoxic, and is biodegradable, has suction efficiently, slowly-releasing and water retention capacity.Preparation method of the present invention is simple and easy to control, and cost is low, is easy to industrialization.
Purpose of the present invention realizes by following scheme:
A kind of environment-friendly type hemicellulose water-retaining agent, structural formula is as follows:
M in the formula, n, x, p 〉=1.
The present invention also provides a kind of preparation method of environment-friendly type hemicellulose water-retaining agent, may further comprise the steps:
(1) pulverizes after the bambusa textile drying, with volume ratio is that the toluene of 21 ~ 4:1 and ethanol mixed solvent are at 90 ~ 100 ℃ of extracting 4 ~ 8h, in residue, add Textone and distilled water, with hydrochloric acid or vinegar acid for adjusting pH value is that 2 ~ 3h is extracted at 70 ~ 80 ℃ in 3.8～4.0 backs, filter, filter residue 95%(wt.) washing with alcohol is 2 ~ 3 times, in 50 ~ 60 ℃ of down dry 12 ~ 16h, obtains the bambusa textile of delignification;
(2) bambusa textile of the delignification that step (1) is obtained extracts 8～12 h with 8 ~ 10%(wt.) KOH solution at 20～30 ℃, filter, filtrate is 5.5 with the vinegar acid for adjusting pH value, add 95%(wt. again) ethanol, leave standstill 8 ~ 10h and obtain precipitation, filter, precipitation is with acidifying 70%(volume fraction) washing with alcohol 2 ~ 3 times, in 50 ~ 60 ℃ of down dry 12 ~ 16h, obtain xylan class hemicellulose;
(3) the xylan class hemicellulose that step (2) is obtained adds in the distilled water, dissolves fully to it in 60～90 ℃ of heating 5～30min, obtains xylan class hemicellulose solution;
(4) in rare gas element, in the xylan class hemicellulose solution that step (3) obtains, add initiator, add vinylformic acid and linking agent again, after stirring, in 20 ~ 40 ℃ of heating 10 ~ 40h, cooling obtains crude product;
(5) crude product that step (4) is obtained is washed with distilled water to washings and is neutral, to constant weight, obtains the hemicellulose water-retaining agent in 50 ~ 60 ℃ of vacuum-drying 20 ~ 24h.
In the step of the present invention (1), the mass volume ratio of described bambusa textile powder and mixed solvent is 1:(15 ~ 25) g mL
-1The mass ratio of described Textone and residue is (1.2 ~ 1.8): 1; Mass volume ratio 1 (15 ~ 25) the g mL of described residue and distilled water
-1
In the step of the present invention (2), the mass volume ratio of the bambusa textile of described delignification and 8 ~ 10%(wt.) KOH solution is 1 (15～25) g mL
-1Described 95%(wt.) volume ratio of ethanol and filtrate is 3:1.
In the step of the present invention (3), the mass volume ratio of described xylan class hemicellulose and distilled water is 1:(10～50) g mL
-1
In the step of the present invention (4), described initiator is the mixture of ammonium persulphate and Tetramethyl Ethylene Diamine; The mass ratio of described initiator and xylan class hemicellulose is (2 ~ 18): 100; The mass volume ratio of described ammonium persulphate and Tetramethyl Ethylene Diamine is 1:1 g mL
-1
In the step of the present invention (4), described vinylformic acid is the vinylformic acid of degree of neutralization 70%, and the mass ratio of described vinylformic acid and xylan class hemicellulose is (1 ~ 20): 1.
In the step of the present invention (4), described linking agent is
N,
N'-methylene-bisacrylamide, the mass ratio of described linking agent and xylan class hemicellulose is (1 ~ 5): 20.
In the step of the present invention (4), described rare gas element is a nitrogen.
The present invention compared with prior art has following beneficial effect:
(1) water-retaining agent of the present invention is nontoxic, biodegradable, has higher water-retaining capacity, and water-retaining capacity reaches 90 ~ 822 times of own wt;
(2) preparation method's technology of the present invention is simple, and the reaction conditions gentleness is easy to operate, is easy to industrialization;
(3) as reaction medium, generative process does not produce environmental pollution to preparation method of the present invention with water.
Embodiment
The invention will be further described below in conjunction with embodiment, but the scope of protection of present invention is not limited to this.
Embodiment 1
(1) pulverizes after the 50g bambusa textile drying, toluene and ethanol 21 are mixed and obtain mixed solvent by volume, in the bambusa textile powder, add the 1200mL mixed solvent, in Soxhlet extractor in 96 ℃ of extracting 6h, add the 75g Textone to the 50g residue, adding 1000mL distilled water, is 3.8 with 6mol/L vinegar acid for adjusting pH value, extracts 2h at 75 ℃, filter, filter residue 95%(wt.) washing with alcohol is 2 times, in 60 ℃ of following dry 14h, obtains the bambusa textile of delignification;
(2) the bambusa textile 400mL 10%(wt. of the delignification that 20g step (1) is obtained) KOH solution extracts 10h at 23 ℃, filters; The filtrate that obtains is 5.5 with 6mol/L vinegar acid for adjusting pH value, adds 1200mL 95%(wt. again) ethanol, leave standstill 10h, filter, the precipitation that obtains acidifying 70%(volume fraction) washing with alcohol is 2 times, and dry 12h under 60 ℃ obtains xylan class hemicellulose;
(3) the xylan class hemicellulose that 6g step (2) is obtained adds 180mL distilled water, to dissolving fully, obtains xylan class hemicellulose solution in 85 ℃ of heating 15 min;
(4) in nitrogen, 0.3g ammonium persulphate and 0.3mL Tetramethyl Ethylene Diamine are added in the xylan class hemicellulose solution that step (3) obtains, add the vinylformic acid and the 0.6g of 6g degree of neutralization 70% again
N,
N'-methylene-bisacrylamide, after stirring, in 30 ℃ of heating 24h, cooling obtains crude product;
(5) crude product that step (4) is obtained is washed with distilled water to washings and is neutral, to constant weight, obtains the hemicellulose water-retaining agent in 50 ℃ of vacuum-drying 24h.
Measuring method and condition: under 25 ℃ of room temperatures, get a certain amount of hemicellulose water-retaining agent, abundant swelling and reach balance in distilled water when promptly hemicellulose water-retaining agent quality no longer increases, is taken out, and weighs.
Water-retaining agent water retention=remaining mass/hemicellulose water-retaining agent quality.
After measured, the water-retaining agent of embodiment 1 preparation can absorb the water of 822 times of own wts.
Embodiment 2
(1) pulverizes after the 60g bambusa textile drying, toluene and ethanol 41 are mixed and obtain mixed solvent by volume, in the bambusa textile powder, add the 900mL mixed solvent, in Soxhlet extractor in 90 ℃ of extracting 8h, add the 60g Textone to the 50g residue, adding 750mL distilled water, is 3.8 with 6mol/L vinegar acid for adjusting pH value, extracts 2.5h at 80 ℃, filter, filter residue is with 95% washing with alcohol 3 times, in 50 ℃ of dry 16h down, obtains the bambusa textile of delignification;
(2) the bambusa textile 300mL 10%(wt. of the delignification that 20g step (1) is obtained) KOH solution extracts 12h at 20 ℃, filters; The filtrate that obtains is 5.5 with 6mol/L vinegar acid for adjusting pH value, adds 900mL 95%(wt. again) ethanol, leave standstill 8h, filter, the precipitation that obtains is with acidifying 70%(volume fraction) washing with alcohol 3 times, in 50 ℃ of dry 16h down, obtain xylan class hemicellulose;
(3) the xylan class hemicellulose that 6g step (2) is obtained adds 300mL distilled water, to dissolving fully, obtains xylan class hemicellulose solution in 60 ℃ of heating 30 min;
(4) in nitrogen, 0.54g ammonium persulphate and 0.54mL Tetramethyl Ethylene Diamine are added in the xylan class hemicellulose solution that step (3) obtains, add the vinylformic acid and the 0.3g of 72g degree of neutralization 70% again
N,
N'-methylene-bisacrylamide, after stirring, in 20 ℃ of heating 40h, cooling obtains crude product;
(5) crude product that step (4) is obtained is washed with distilled water to washings and is neutral, to constant weight, obtains the hemicellulose water-retaining agent in 60 ℃ of vacuum-drying 20 h.
After measured, the water-retaining agent of embodiment 2 preparations can absorb the water of 240 times of own wts.
Embodiment 3
(1) pulverizes after the 60g bambusa textile drying, toluene and ethanol 31 mixing are by volume obtained mixed solvent, in the bambusa textile powder, add the 1500mL mixed solvent, in Soxhlet extractor in 100 ℃ of extracting 4h, adding the 90g Textone to the 50g residue, add 1250mL distilled water, is 4.8 with 1mol/L salt acid for adjusting pH value, extract 3h at 70 ℃, filter, filter residue is with 95% washing with alcohol 2 times, in 60 ℃ times dry 16h,, obtain the bambusa textile of delignification;
(2) the bambusa textile 500mL 9%(wt. of the delignification that 20g step (1) is obtained) KOH solution extracts 8h at 30 ℃, filters; The filtrate that obtains is 5.5 with 6 mol/L vinegar acid for adjusting pH value, adds 1500mL 95%(wt. again) ethanol, leave standstill 9h, filter, the precipitation that obtains acidifying 70%(volume fraction) washing with alcohol is 2 times, and dry 14h under 55 ℃ obtains xylan class hemicellulose;
(3) the xylan class hemicellulose that 6g step (2) is obtained adds 60mL distilled water, to dissolving fully, obtains xylan class hemicellulose solution in 90 ℃ of heating 5 min;
(4) in nitrogen, 0.06g ammonium persulphate and 0.06mL Tetramethyl Ethylene Diamine are added in the xylan class hemicellulose solution that step (3) obtains, add the vinylformic acid and the 1.5g of 120g degree of neutralization 70% again
N,
N'-methylene-bisacrylamide, after stirring, in 40 ℃ of heating 10 h, cooling obtains crude product;
(5) crude product that step (4) is obtained is washed with distilled water to washings and is neutral, to constant weight, obtains the hemicellulose water-retaining agent in 55 ℃ of vacuum-drying 22h.
After measured, the water-retaining agent of embodiment 3 preparations can absorb the water of 99 times of own wts.
Claims (9)
1. environment-friendly type hemicellulose water-retaining agent is characterized in that structural formula is as follows:
M in the formula, n, x, p 〉=1.
2. the preparation method of the described environment-friendly type hemicellulose of claim 1 water-retaining agent is characterized in that may further comprise the steps:
(1) pulverizes after the bambusa textile drying, with volume ratio is that the toluene of 21 ~ 4:1 and ethanol mixed solvent are at 90 ~ 100 ℃ of extracting 4 ~ 8h, in residue, add Textone and distilled water, with hydrochloric acid or vinegar acid for adjusting pH value is that 2 ~ 3h is extracted at 70 ~ 80 ℃ in 3.8～4.0 backs, filter, filter residue 95%(wt.) washing with alcohol is 2 ~ 3 times, in 50 ~ 60 ℃ of down dry 12 ~ 16h, obtains the bambusa textile of delignification;
(2) bambusa textile of the delignification that step (1) is obtained extracts 8～12 h with 8 ~ 10%(wt.) KOH solution at 20～30 ℃, filter, filtrate is 5.5 with the vinegar acid for adjusting pH value, add 95%(wt. again) ethanol, leave standstill 8 ~ 10h and obtain precipitation, filter, precipitation is with acidifying 70%(volume fraction) washing with alcohol 2 ~ 3 times, in 50 ~ 60 ℃ of down dry 12 ~ 16h, obtain xylan class hemicellulose;
(3) the xylan class hemicellulose that step (2) is obtained adds in the distilled water, dissolves fully to it in 60～90 ℃ of heating 5～30min, obtains xylan class hemicellulose solution;
(4) in rare gas element, in the xylan class hemicellulose solution that step (3) obtains, add initiator, add vinylformic acid and linking agent again, after stirring, in 20 ~ 40 ℃ of heating 10 ~ 40h, cooling obtains crude product;
(5) crude product that step (4) is obtained is washed with distilled water to washings and is neutral, to constant weight, obtains the hemicellulose water-retaining agent in 50 ~ 60 ℃ of vacuum-drying 20 ~ 24h.
3. preparation method according to claim 2 is characterized in that, in the step (1), the mass volume ratio of described bambusa textile powder and mixed solvent is 1:(15 ~ 25) g mL
-1The mass ratio of described Textone and residue is (1.2 ~ 1.8): 1; Mass volume ratio 1 (15 ~ 25) the g mL of described distilled water and residue
-1
4. according to claim 2 or 3 described preparation methods, it is characterized in that in the step (2), the mass volume ratio of the bambusa textile of described delignification and 8 ~ 10%(wt.) KOH solution is 1 (15～25) g mL
-1Described 95%(wt.) volume ratio of ethanol and filtrate is 3:1.
5. preparation method according to claim 4 is characterized in that, in the step (3), the mass volume ratio of described xylan class hemicellulose and distilled water is 1:(10～50) g mL
-1
6. preparation method according to claim 5 is characterized in that, in the step (4), described initiator is the mixture of ammonium persulphate and Tetramethyl Ethylene Diamine; The mass ratio of described initiator and xylan class hemicellulose is (2 ~ 18): 100;
The mass volume ratio of described ammonium persulphate and Tetramethyl Ethylene Diamine is 1:1 g mL
-1
7. preparation method according to claim 5 is characterized in that, in the step (4), described vinylformic acid is the vinylformic acid of degree of neutralization 70%, and the mass ratio of described vinylformic acid and xylan class hemicellulose is (1 ~ 20): 1.
8. preparation method according to claim 5 is characterized in that, in the step (4), described linking agent is
N,
N'-methylene-bisacrylamide, the mass ratio of described linking agent and xylan class hemicellulose is (1 ~ 5): 20.
9. according to the described preparation method of one of claim 5 ~ 8, it is characterized in that in the step (4), described rare gas element is a nitrogen.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775525A (en) * | 2012-07-16 | 2012-11-14 | 华南理工大学 | Preparation method and application of cross-linking type hemicellulose |
| CN103408805A (en) * | 2013-07-23 | 2013-11-27 | 华南理工大学 | Nano-cellulose-fiber-reinforced hemicellulose membrane and preparation method thereof |
| CN103435856A (en) * | 2013-08-20 | 2013-12-11 | 华南理工大学 | Environment-friendly internal plasticization hemicellulose membrane and preparation method thereof |
| CN103709328A (en) * | 2013-10-28 | 2014-04-09 | 北京林业大学 | Preparation method of hemicelluloses-based organic-inorganic compound hydrogel |
| CN109162094A (en) * | 2018-07-23 | 2019-01-08 | 安徽三利丝绸集团有限公司 | A kind for the treatment of process improving silk fiber moisture pick-up properties |
-
2011
- 2011-08-10 CN CN 201110228447 patent/CN102268105A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 《Journal of agricultural and food chemistry》 20110801 Xin-Wen Peng Xylan-rich Hemicelluloses-graft-Acrylic Acid Ionic Hydrogels with Rapid Responses to pH, Salt, and Organic Solvents 第59卷, 第15期 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775525A (en) * | 2012-07-16 | 2012-11-14 | 华南理工大学 | Preparation method and application of cross-linking type hemicellulose |
| CN103408805A (en) * | 2013-07-23 | 2013-11-27 | 华南理工大学 | Nano-cellulose-fiber-reinforced hemicellulose membrane and preparation method thereof |
| CN103435856A (en) * | 2013-08-20 | 2013-12-11 | 华南理工大学 | Environment-friendly internal plasticization hemicellulose membrane and preparation method thereof |
| CN103709328A (en) * | 2013-10-28 | 2014-04-09 | 北京林业大学 | Preparation method of hemicelluloses-based organic-inorganic compound hydrogel |
| CN103709328B (en) * | 2013-10-28 | 2016-04-13 | 北京林业大学 | A kind of preparation method of hemicelluloses-basedorganic-inorganic organic-inorganic compound hydrogel |
| CN109162094A (en) * | 2018-07-23 | 2019-01-08 | 安徽三利丝绸集团有限公司 | A kind for the treatment of process improving silk fiber moisture pick-up properties |
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Application publication date: 20111207 |