CN105482130A - Preparation method of magnetic lignin sulfonate grafted hydrogel - Google Patents
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
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Abstract
The invention discloses a preparation method of magnetic lignin sulfonate grafted hydrogel. The preparation method comprises steps as follows: with acrylic acid and acrylamide as monomers, nano ferroferric oxide as a magnetic source and sodium lignin sulfonate as a graft, the magnetic hydrogel is prepared by adjusting the mass of an initiator, crosslinking agents, sodium lignin sulfonate and a magnetic ball and the mass ratio of the two monomers with an ultrasonic method. The degree of crossklinking can be adjusted by adding different quantities of the crosslinking agents in the process, the number of pores in the hydrogel and the pore size are regulated by changing the degree of crosslinking and the mass ratio of the two monomers, and the purpose of controlling the swelling property of the hydrogel is achieved. With acrylic acid and acrylamide as monomers, the magnetic hydrogel is prepared with the ultrasonic method, operation is simple, the cost is low, the hydrogel is prepared conveniently and quickly, environment pressure can be reduced, limited resources are sufficiently used, distribution of the water absorption rate of the prepared product is wide, the water absorption rate is high, and the preparation method can be widely applied in life.
Description
Technical field
The present invention relates to a kind of preparation method of magnetic hydrogel, particularly a kind of method of ultrasonic wave added synthesizing magnetic modified lignin mahogany sulfonate graft acrylic acid based aquagel.
Background technology
Hydrogel is a kind of novel high polymer material, and development starts from the sixties in 20th century.After the seventies, the open working of SAP obtains huge progress, portioned product excellent property, and Absorbable rod reaches the moisture of deadweight hundreds of times and even thousands of times, and internal moisture can also be made under certain pressure and temperature to be kept, there is excellent weathering resistance and protect fluidity.Hydrogel is now widely used in medical and health, agricultural gardening, material of construction, industry, the aspects such as artificial intelligence.
Acrylic acid series hydrogel raw material is easy to obtain, excellent property, and reactive behavior is high, and all kinds of linguistic term therefore in synthesis material are just more extensive, and mainly vinylformic acid and Mierocrystalline cellulose, each kind of starch, mineral etc. carry out grafting, modification by copolymerization.Utilize starch, Mierocrystalline cellulose and acrylic acid copolymer, reason is starch, Mierocrystalline cellulose, wide material sources and cheap, and biological degradability is better.Main starch has Tapioca Starch, flour, Semen Maydis powder, Rhizoma amorphophalli powder etc.; Mierocrystalline cellulose then can extract from paper pulp fiber, chitosan etc.Larger specific surface area is the common trait of mineral powder, and have many hydroxyls to be present in its surface, to be combined into key very suitable with acrylate copolymer, the mineral that the characteristics such as ion exchangeable, swelling property, high thermal resistance and lower shrinking percentage all possess can be used, come to react with vinylformic acid by modification by copolymerization, the acrylic acid series plural gel that such properties is good, cost is low just can prepare.In order to improve intensity and the performance of gel, reduce the harm of unconverted monomer, vinylformic acid and salt thereof can also synthesize hydrogel with the such as graft copolymerization such as polyvinyl alcohol, acrylamide.
The application of magnetic gel in target administration is comparatively extensive, and its development is also rapider in recent years.Magnetic hydrogel is the intelligent aqueous gel capable that a class has magnetic responsiveness, be generally made up of polymeric matrix and magnetic component, and magnetic component mostly is the magnetic inorganic particulate of tool, as Fe
3o
4deng metal oxide and CoFe
2o
4etc. ferrite compound.Because hemicellulose and magnetic gel all have the advantage of its uniqueness, so hemicellulose group magnetic hydrogel has many potential purposes in fixing, bioseparation, drug controlled release and the sensor of enzyme.
Summary of the invention
The object of the invention is to adopt vinylformic acid and acrylamide to be main raw material, by changing the addition of magnetic ball and sodium lignosulfonate, ultrasonic wave added method synthesizing magnetic modified lignin mahogany sulfonate graft acrylic acid based aquagel, technique is simple, raw material is easy to obtain, with low cost, of reduced contamination, time saving and energy saving, convenient and swift, and can second stage employ papermaking waste, reduce environmental stress, be suitable for suitability for industrialized production.
Technical scheme of the present invention is as follows:
(1) get magnetic ball under room temperature in sealed vessel, add ultrasonic disperse under nitrogen protection after distilled water, at interval of 10min with hand dynamic 1min until magnetic ball is dispersed; Obtain magnetic ball solution, for subsequent use;
(2) take sodium lignosulfonate, be dissolved in distilled water completely, obtain lignosulfonic acid sodium solution, for subsequent use;
(3) sodium hydroxide is added in distilled water, make it dissolve completely under stirring, cool to room temperature; Under ice-water bath, vinylformic acid is dropwise added in sodium hydroxide solution, and constantly stirs, question response completely after, add linking agent and be stirred to it and dissolve completely, and then add acrylamide and be stirred to it and dissolve completely; Obtain solution A;
(4) the magnetic ball solution of step (1) gained and step (2) gained lignosulfonic acid sodium solution are joined in step (3) gained solution A, stir and make it dispersed, add initiator, stir and make it dissolve completely, obtain solution B, logical nitrogen protection after sealing;
(5) solution B is placed in ultrasound environments, controls water temperature at 40-50 DEG C, until it reacts completely under nitrogen protection;
(6) gel of synthesis is cut into the fritter that specification is 0.3*0.3*0.3mm, washs 2h by soaked in absolute ethyl alcohol, repeat 3-4 time, after vacuum-drying, sealing is preserved.
Further, in step (1), described magnetic ball is ferriferrous oxide nano magnetic ball, and described magnetic spherolite footpath is 100nm.
Further, in step (2), described sulfonated lignin are sodium lignosulfonate, and in described lignosulfonic acid sodium solution, the concentration of sodium lignosulfonate is 0.02 ~ 0.1g/mL.
Further, in step (3), the sodium hydroxide concentration be dissolved in distilled water is 0.2 ~ 0.4g/mL.
Further, in step (3), described linking agent is N, N '-methylene-bisacrylamide; In step (4), described initiator is ammonium persulphate.
Described magnetic ball: the amount ratio of sodium lignosulfonate, sodium hydroxide, vinylformic acid, linking agent, acrylamide, initiator is 0.05-0.5g:0.1-0.5g:1-2g:5mL:0.01-0.03g:0.1-0.7g:0.05-0.2 g.
In step (6), described vacuum drying temperature is 60 ~ 80 DEG C.
The synthetic method of the nano ferriferrous oxide microballoon that the present invention utilizes is:
The Fe (Cl) of 0.008mol is got under room temperature
36H
2the NaAc3H of O and 0.04mol
2o, is dissolved in the ethylene glycol of 35mL respectively, adds 0.5g sodium lignosulfonate again, stirring and dissolving after mixing, then magnetic agitation makes it dispersed in 20 minutes; Above-mentioned solution is moved in autoclave, at 220 DEG C of temperature, reacts 8h, be cooled to room temperature; By the centrifugation of gained precipitation mixture, precipitate with deionized water cleans 3 times, then uses washes of absolute alcohol 3 times, centrifugation; Solid after being separated is put into the dry 12h of vacuum drying oven, and the temperature of described vacuum drying oven is set as 60 DEG C.
This is tested reagent used and is all analytical pure, is commercially available.
Beneficial effect of the present invention:
The present invention take vinylformic acid as monomer, by regulating magnetic ball, linking agent and the amount of initiator and the mass ratio of monomer, utilizes ultrasonic wave added legal system for magnetic modified water gel.Its operational condition is easy to control, and equipment is simple, and preparation cost is low, and made product swelling behavior is good, and pattern is better, is easy to realize industrialization.And can environmental pressure be reduced, make full use of limited resources.
Accompanying drawing explanation
Fig. 1 is the surface scan Electronic Speculum figure of vacuum drying sodium lignosulfonate magnetic hydrogel sample;
Fig. 2 is the transverse section scanning electron microscope (SEM) photograph of vacuum drying sodium lignosulfonate magnetic hydrogel sample, and wherein spherical particle thing is the spheroid figure that Z 250 is formed in gel inside;
Fig. 3 is the surperficial partial enlarged drawing of vacuum drying sodium lignosulfonate magnetic hydrogel sample;
Fig. 4 is the transverse section partial enlarged drawing of vacuum drying sodium lignosulfonate magnetic hydrogel sample.
Specific implementation method
Below in conjunction with concrete embodiment, the present invention will be further described, and to make those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
Embodiment 1
Getting 0.05g particle diameter under room temperature is that the magnetic ball of about 100nm is placed in sealed vessel, ultrasonic dispersed to it under logical nitrogen protection after adding 5-10mL distilled water, taking 0.1g sodium lignosulfonate is dissolved in 5mL distilled water completely, accurately take in the clean small beaker that 1.8942g sodium hydroxide is dissolved in containing 5mL distilled water, then under ice-water bath, 5mL vinylformic acid is accurately measured, drip while stir and dropwise add in sodium hydroxide solution, question response completely after take 0.0116g linking agent and 0.7000g acrylamide adds wherein, stir until it dissolves completely, to join in above-mentioned solution containing homodisperse magnetic ball solution, stirring makes it dispersed, take 0.145g initiator, add in solution, stirring makes it dissolve completely, above-mentioned solution is placed in ultrasound environments, control water temperature at 43 DEG C, until it reacts completely under nitrogen protection.The gel of synthesis is cut into the fritter that specification is 0.3*0.3*0.3mm, washs 2h by soaked in absolute ethyl alcohol, repeat 3-4 time, after vacuum-drying, sealing is preserved.
Embodiment 2
Getting 0.1g particle diameter under room temperature is that the magnetic ball of about 100nm is placed in sealed vessel, ultrasonic dispersed to it under logical nitrogen protection after adding 5-10mL distilled water, taking 0.2g sodium lignosulfonate is dissolved in 5mL distilled water completely, accurately take in the clean small beaker that 1.6028g sodium hydroxide is dissolved in containing 5mL distilled water, then under ice-water bath, 5mL vinylformic acid is accurately measured, drip while stir and dropwise add in sodium hydroxide solution, question response completely after take 0.0232g linking agent and 0.3015g acrylamide adds wherein, stir until it dissolves completely, to join in above-mentioned solution containing homodisperse magnetic ball solution, stirring makes it dispersed, take 0.116g initiator, add in solution, stirring makes it dissolve completely, above-mentioned solution is placed in ultrasound environments, control water temperature at 45 DEG C, until it reacts completely under nitrogen protection.The gel of synthesis is cut into the fritter that specification is 0.3*0.3*0.3mm, washs 2h by soaked in absolute ethyl alcohol, repeat 3-4 time, after vacuum-drying, sealing is preserved.
Embodiment 3
Getting 0.15g particle diameter under room temperature is that the magnetic ball of about 100nm is placed in sealed vessel, ultrasonic dispersed to it under logical nitrogen protection after adding 5-10mL distilled water, taking 0.3g sodium lignosulfonate is dissolved in 5mL distilled water completely, accurately take in the clean small beaker that 2.0400g sodium hydroxide is dissolved in containing 5mL distilled water, then under ice-water bath, 5mL vinylformic acid is accurately measured, drip while stir and dropwise add in sodium hydroxide solution, question response completely after take 0.0174g linking agent and 0.1005g acrylamide adds wherein, stir until it dissolves completely, to join in above-mentioned solution containing homodisperse magnetic ball solution, stirring makes it dispersed, take 0.087g initiator, add in solution, stirring makes it dissolve completely, above-mentioned solution is placed in ultrasound environments, control water temperature at 50 DEG C, until it reacts completely under nitrogen protection.The gel of synthesis is cut into the fritter that specification is 0.3*0.3*0.3mm, washs 2h by soaked in absolute ethyl alcohol, repeat 3-4 time, after vacuum-drying, sealing is preserved.
Embodiment 4
Getting 0.2g particle diameter under room temperature is that the magnetic ball of about 100nm is placed in sealed vessel, ultrasonic dispersed to it under logical nitrogen protection after adding 5-10mL distilled water, taking 0.4g sodium lignosulfonate is dissolved in 5mL distilled water completely, accurately take in the clean small beaker that 1.7485g sodium hydroxide is dissolved in containing 5mL distilled water, then under ice-water bath, 5mL vinylformic acid is accurately measured, drip while stir and dropwise add in sodium hydroxide solution, question response completely after take 0.0116g linking agent and 0.5025g acrylamide adds wherein, stir until it dissolves completely, to join in above-mentioned solution containing homodisperse magnetic ball solution, stirring makes it dispersed, take 0.174g initiator, add in solution, stirring makes it dissolve completely, above-mentioned solution is placed in ultrasound environments, control water temperature at 40 DEG C, until it reacts completely under nitrogen protection.The gel of synthesis is cut into the fritter that specification is 0.3*0.3*0.3mm, washs 2h by soaked in absolute ethyl alcohol, repeat 3-4 time, after vacuum-drying, sealing is preserved.
Embodiment 5
Getting 0.05g particle diameter under room temperature is that the magnetic ball of about 100nm is placed in sealed vessel, ultrasonic dispersed to it under logical nitrogen protection after adding 5-10mL distilled water, taking 0.5g sodium lignosulfonate is dissolved in 5mL distilled water completely, accurately take in the clean small beaker that 1.8942g sodium hydroxide is dissolved in containing 5mL distilled water, then under ice-water bath, 5mL vinylformic acid is accurately measured, drip while stir and dropwise add in sodium hydroxide solution, question response completely after take 0.0116g linking agent and 0.5025g acrylamide adds wherein, stir until it dissolves completely, to join in above-mentioned solution containing homodisperse magnetic ball solution, stirring makes it dispersed, take 0.116g initiator, add in solution, stirring makes it dissolve completely, above-mentioned solution is placed in ultrasound environments, control water temperature at 45 DEG C, until it reacts completely under nitrogen protection.The gel of synthesis is cut into the fritter that specification is 0.3*0.3*0.3mm, washs 2h by soaked in absolute ethyl alcohol, repeat 3-4 time, after vacuum-drying, sealing is preserved.
As can be seen from Figure 1, there are some holes not of uniform size in the surface of vacuum drying sodium lignosulfonate magnetic hydrogel sample.
As can be seen from Figure 2, there is many spherical particle things in the transverse section of vacuum drying sodium lignosulfonate magnetic hydrogel sample, also there are some irregular gaps.
As can be seen from Figure 3, after the surface amplification of vacuum drying sodium lignosulfonate magnetic hydrogel sample, can be observed aperture obvious and intensive.
As can be seen from Figure 4, after the inside amplification of vacuum drying sodium lignosulfonate magnetic hydrogel sample, can be observed particulate matter more obvious.
The swelling ratio of sample in distilled water reaches 545g/g.
Claims (7)
1. a preparation method for Sulfite lignin magnetic hydrogel, is characterized in that, comprises the steps:
(1) get magnetic ball under room temperature in sealed vessel, add ultrasonic disperse under nitrogen protection after distilled water, at interval of 10min with hand dynamic 1min until magnetic ball is dispersed; Obtain magnetic ball solution, for subsequent use;
(2) take sodium lignosulfonate, be dissolved in distilled water completely, obtain lignosulfonic acid sodium solution, for subsequent use;
(3) sodium hydroxide is added in distilled water, make it dissolve completely under stirring, cool to room temperature; Under ice-water bath, vinylformic acid is dropwise added in sodium hydroxide solution, and constantly stirs, question response completely after, add linking agent and be stirred to it and dissolve completely, and then add acrylamide and be stirred to it and dissolve completely; Obtain solution A;
(4) the magnetic ball solution of step (1) gained and step (2) gained lignosulfonic acid sodium solution are joined in step (3) gained solution A, stir and make it dispersed, add initiator, stir and make it dissolve completely, obtain solution B, logical nitrogen protection after sealing;
(5) solution B is placed in ultrasound environments, controls water temperature at 40-50 DEG C, until it reacts completely under nitrogen protection;
(6) gel of synthesis is cut into the fritter that specification is 0.3*0.3*0.3mm, washs 2h by soaked in absolute ethyl alcohol, repeat 3-4 time, after vacuum-drying, sealing is preserved.
2. preparation method according to claim 1, is characterized in that, in step (1), described magnetic ball is ferriferrous oxide nano magnetic ball, and described magnetic spherolite footpath is 100nm.
3. preparation method according to claim 1, is characterized in that, in step (2), described sulfonated lignin are sodium lignosulfonate, and in described lignosulfonic acid sodium solution, the concentration of sodium lignosulfonate is 0.02 ~ 0.1g/mL.
4. preparation method according to claim 1, is characterized in that, in step (3), the sodium hydroxide concentration be dissolved in distilled water is 0.2 ~ 0.4g/mL.
5. preparation method according to claim 1, is characterized in that, in step (3), described linking agent is N, N '-methylene-bisacrylamide; In step (4), described initiator is ammonium persulphate.
6. preparation method according to claim 1, it is characterized in that, described magnetic ball: the amount ratio of sodium lignosulfonate, sodium hydroxide, vinylformic acid, linking agent, acrylamide, initiator is 0.05-0.5g:0.1-0.5g:1-2g:5mL:0.01-0.03g:0.1-0.7g:0.05-0.2 g.
7. preparation method according to claim 1, is characterized in that, in step (6), described vacuum drying temperature is 60 ~ 80 DEG C.
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| CN201610024534.7A CN105482130B (en) | 2016-01-15 | 2016-01-15 | A kind of preparation method of lignosulphonates magnetic hydrogel |
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Cited By (6)
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| CN106075791A (en) * | 2016-07-20 | 2016-11-09 | 周荣 | A kind of preparation method of polymolecularity aerosol extinguishing agent |
| CN106589264A (en) * | 2016-11-10 | 2017-04-26 | 江苏大学 | Method for preparing crylic-acid-based composite hydrogel |
| CN107245132A (en) * | 2017-06-22 | 2017-10-13 | 安徽省德邦瓷业有限公司 | A kind of method that is once grafted chemical modification of sunflower seed shell lignin |
| CN107501691A (en) * | 2017-09-25 | 2017-12-22 | 安徽依采妮纤维材料科技有限公司 | A kind of preparation method of sodium lignin sulfonate filled plastics composite |
| CN108676121A (en) * | 2018-04-16 | 2018-10-19 | 中国林业科学研究院亚热带林业研究所 | A kind of magnetism hemicellulose based aquagel |
| CN113509907A (en) * | 2021-03-09 | 2021-10-19 | 大连工业大学 | Preparation of lignin-based composite hydrogel and application of lignin-based composite hydrogel in heavy metal ion adsorption and luminescent materials |
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| CN105153351A (en) * | 2015-07-31 | 2015-12-16 | 莆田学院 | Citric acid-polyacrylate magnetic hydrogel, preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106075791A (en) * | 2016-07-20 | 2016-11-09 | 周荣 | A kind of preparation method of polymolecularity aerosol extinguishing agent |
| CN106589264A (en) * | 2016-11-10 | 2017-04-26 | 江苏大学 | Method for preparing crylic-acid-based composite hydrogel |
| CN106589264B (en) * | 2016-11-10 | 2019-01-08 | 江苏大学 | A kind of preparation method of acrylic composite hydrogel |
| CN107245132A (en) * | 2017-06-22 | 2017-10-13 | 安徽省德邦瓷业有限公司 | A kind of method that is once grafted chemical modification of sunflower seed shell lignin |
| CN107501691A (en) * | 2017-09-25 | 2017-12-22 | 安徽依采妮纤维材料科技有限公司 | A kind of preparation method of sodium lignin sulfonate filled plastics composite |
| CN108676121A (en) * | 2018-04-16 | 2018-10-19 | 中国林业科学研究院亚热带林业研究所 | A kind of magnetism hemicellulose based aquagel |
| CN113509907A (en) * | 2021-03-09 | 2021-10-19 | 大连工业大学 | Preparation of lignin-based composite hydrogel and application of lignin-based composite hydrogel in heavy metal ion adsorption and luminescent materials |
| CN113509907B (en) * | 2021-03-09 | 2024-03-22 | 大连工业大学 | Preparation of lignin-based composite hydrogel and application of lignin-based composite hydrogel in heavy metal ion adsorption and luminescent materials |
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