CN105482130B - A kind of preparation method of lignosulphonates magnetic hydrogel - Google Patents
A kind of preparation method of lignosulphonates magnetic hydrogel Download PDFInfo
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Abstract
The present invention discloses a kind of preparation method of lignosulphonates magnetic hydrogel.Step is：Using acrylic acid and acrylamide as monomer, using nano ferriferrous oxide as magnetic source, using sodium lignin sulfonate as graft, by adjusting initiator, crosslinking agent, sodium lignin sulfonate and the quality of magnetic ball and the mass ratio of two kinds of monomers, magnetic hydrogel is prepared using ultrasonic method.Adding different amounts of crosslinking agent in the process can play the role of regulating and controlling the degree of cross linking, regulate and control the quantity of gel mesoporous and the size in aperture by changing the mass ratio of crosslinking degree and two kinds of monomers, to achieve the purpose that control gel swelling.The present invention prepares magnetic hydrogel using acrylic acid and acrylamide as monomer, using ultrasonic method, easy to operate, of low cost, it is convenient and efficient, and environmental pressure can be reduced, make full use of limited resources, made product water absorbent rate distribution is wide, and rate of water absorption is high, can be widely used in life.
Description
Technical field
The present invention relates to a kind of preparation method of magnetic hydrogel, more particularly to a kind of ultrasonic wave added synthesizing magnetic innovation wood
The method of mahogany sulfonate grafted propylene acidic group hydrogel.
Background technology
Hydrogel is a kind of novel high polymer material, and development starts from the 1960s.After the seventies, the opening work of SAP
Work obtains huge progress, and portioned product function admirable can absorb the moisture for reaching hundreds times or even thousands of times of dead weight, and certain
Pressure and temperature under internal moisture can also be made to be maintained, have excellent weatherability and protect fluidity.Hydrogel is extensive
Applied to medical and health, agricultural gardening, construction material, industry, artificial intelligence etc..
Acrylic acid series hydrogel raw material is easily obtained, function admirable, and reactivity is high, therefore each in terms of synthesis material
Class linguistic term is just more extensive, mainly acrylic acid and cellulose, each kind of starch, mineral etc. be grafted, modification by copolymerization.Profit
With starch, cellulose and acrylic acid copolymer, the reason is that starch, cellulose, derive from a wealth of sources and cheaply, and biological degradability compared with
It is good.Main starch has tapioca starch, flour, corn flour, konjaku flour etc.；Cellulose then can be from paper pulp fiber, chitosan etc.
Extraction.Larger specific surface area is the common trait of mineral powder, and is present in its surface there are many hydroxyl, with acroleic acid polymerization
Object combination bonding is very suitable, the mineral that the characteristics such as ion exchangeable, dilatancy, heat-resisting quantity and lower shrinking percentage all have
It can be used, be reacted with acrylic acid with modification by copolymerization, the acrylic acid series that such properties are good, at low cost is compound
Gel can prepare.In order to improve the intensity and performance of gel, the harm of unconverted monomer is reduced, acrylic acid and its salt are also
Hydrogel can be synthesized with the graft copolymerizations such as such as polyvinyl alcohol, acrylamide.
Application of the magnetic gel in terms of target administration is wide, its development is also relatively rapider in recent years.Magnetic hydrogel
It is a kind of intelligent aqueous gel with magnetic responsiveness, is generally made of polymer substrate and magnetic component, and magnetic component is mostly
Have magnetic inorganic particulate, such as Fe3O4Equal metal oxides and CoFe2O4Etc. ferrites compound.Because of hemicellulose
There is its uniqueness with magnetic gel, so hemicellulose group magnetic hydrogel is in the fixation of enzyme, bio-separation, drug control
There are many potential purposes for system release and sensor etc..
Invention content
The purpose of the present invention is using acrylic acid and acrylamide for primary raw material, by changing magnetic ball and sulfomethylated lignin
The additive amount of sour sodium, ultrasonic wave added method synthesizing magnetic modified lignin mahogany sulfonate grafted propylene acidic group hydrogel is simple for process, former
Expect it is readily available, it is of low cost, it is of reduced contamination, it is time saving and energy saving, it is convenient and efficient, and can secondary use papermaking waste, subtract
Subenvironment pressure is suitable for industrialized production.
Technical scheme is as follows：
（1）It takes magnetic ball in sealing container at room temperature, ultrasonic disperse under nitrogen protection after distilled water is added, at interval of
10min shakes with hands 1min until magnetic ball is evenly dispersed；Magnetic ball solution is obtained, it is spare；
（2）Sodium lignin sulfonate is weighed, is completely dissolved in distilled water, lignin sulfonic acid sodium solution is obtained, it is spare；
（3）Sodium hydroxide is added in distilled water, is made it completely dissolved under stirring, is cooled to room temperature；It, will under ice-water bath
Acrylic acid is added dropwise in sodium hydroxide solution, and is stirred continuously, and after complete reaction, crosslinking agent is added and stirs to it completely
Dissolving, then adds acrylamide and stirs to it and be completely dissolved；Obtain solution A；
（4）By step（1）The magnetic ball solution and step of gained（2）Gained lignin sulfonic acid sodium solution is added to step（3）
In acquired solution A, stirring keeps its evenly dispersed, and initiator is added, and stirring makes it completely dissolved, and obtains solution B, and nitrogen is led to after sealing
Protection；
（5）Solution B is placed in ultrasound environments, control water temperature is under 40-50 DEG C, nitrogen protection up to the reaction was complete for it；
（6）The gel of synthesis is cut into the fritter that specification is 0.3*0.3*0.3mm, washs 2h with soaked in absolute ethyl alcohol, weight
It is 3-4 times multiple, it is sealed after vacuum drying.
Further, step（1）In, the magnetic ball is ferriferrous oxide nano magnetic ball, and the magnetic spherolite diameter is
100nm。
Further, step（2）In, the lignosulfonates are sodium lignin sulfonate, the sodium lignin sulfonate
A concentration of 0.02 ~ 0.1g/mL of sodium lignin sulfonate in solution.
Further, step（3）In, sodium hydroxide is dissolved in a concentration of 0.2 ~ 0.4 g/mL in distilled water.
Further, step（3）In, the crosslinking agent is N, N '-methylene-bisacrylamides；Step（4）In, it is described
Initiator be ammonium persulfate.
The magnetic ball：The amount ratio of sodium lignin sulfonate, sodium hydroxide, acrylic acid, crosslinking agent, acrylamide, initiator
For 0.05-0.5g：0.1-0.5g ：1-2g：5mL：0.01-0.03g：0.1-0.7g：0.05-0.2g.
Step（6）In, the vacuum drying temperature is 60 ~ 80 DEG C.
The synthetic method of nano ferriferrous oxide microballoon that the present invention is utilized is：
The Fe (Cl) of 0.008mol is taken at room temperature3•6H2The NaAc 3H of O and 0.04mol2O is dissolved in the second of 35mL respectively
0.5g sodium lignin sulfonates, stirring and dissolving, then magnetic agitation are added in glycol, after mixing is allowed to evenly dispersed within 20 minutes；It will
Above-mentioned solution moves into autoclave, reacts 8h at a temperature of 220 DEG C, is cooled to room temperature；Gained precipitation mixture is centrifuged,
Precipitation is cleaned 3 times with deionized water, then with washes of absolute alcohol 3 times, is centrifuged；Solid after separation is put into vacuum drying
Dry 12h, the temperature of the vacuum drying chamber are set as 60 DEG C in case.
This experiment reagent used is all that analysis is pure, is commercially available.
Beneficial effects of the present invention：
The present invention is using acrylic acid as monomer, by adjusting magnetic ball, crosslinking agent and the amount of initiator and the mass ratio of monomer,
Magnetic modified hydrogel is prepared using ultrasonic wave added method.Its operating condition is easily controllable, and equipment is simple, and manufacturing cost is low, made
Product swelling behavior is good, and pattern is preferable, it is easy to accomplish industrialization.And environmental pressure can be reduced, make full use of limited resources.
Description of the drawings
Fig. 1 is the surface scan electron microscope of vacuum drying sodium lignin sulfonate magnetic hydrogel sample；
Fig. 2 is the cross section scanning electron microscope (SEM) photograph of vacuum drying sodium lignin sulfonate magnetic hydrogel sample, wherein spherical
Particulate matter is the sphere figure that ferroso-ferric oxide is formed inside gel；
Fig. 3 is the surface partial enlarged view of vacuum drying sodium lignin sulfonate magnetic hydrogel sample；
Fig. 4 is the cross section partial enlarged view of vacuum drying sodium lignin sulfonate magnetic hydrogel sample.
Specific implementation method
With reference to specific implementation example, the present invention will be further described, so that those skilled in the art more fully understand
The present invention, but the invention is not limited in following embodiments.
Embodiment 1
It is that the magnetic ball of 100nm or so is placed in sealing container to take 0.05g grain sizes at room temperature, is added after 5-10mL distilled water
Ultrasound is evenly dispersed to its under logical nitrogen protection, weighs 0.1g sodium lignin sulfonates and is completely dissolved in 5mL distilled water, accurately weighs
1.8942g sodium hydroxides are dissolved in the clean small beaker containing 5mL distilled water, and 5mL third is then accurately measured under ice-water bath
Olefin(e) acid stirs in drop and is added dropwise in sodium hydroxide solution, weighs 0.0116g crosslinking agents and 0.7000g after complete reaction
Acrylamide is added thereto, and stirring is completely dissolved up to it, will be added in above-mentioned solution containing evenly dispersed magnetic ball solution,
Stirring keeps its evenly dispersed, weighs 0.145g initiators, is added in solution, stirring makes it completely dissolved, and above-mentioned solution is placed in
In ultrasound environments, control water temperature is at 43 DEG C, up to the reaction was complete for it under nitrogen protection.It is 0.3* that the gel of synthesis, which is cut into specification,
The fritter of 0.3*0.3mm washs 2h with soaked in absolute ethyl alcohol, repeats 3-4 times, be sealed after vacuum drying.
Embodiment 2
It is that the magnetic ball of 100nm or so is placed in sealing container to take 0.1g grain sizes at room temperature, is added after 5-10mL distilled water
Ultrasound is evenly dispersed to its under logical nitrogen protection, weighs 0.2g sodium lignin sulfonates and is completely dissolved in 5mL distilled water, accurately weighs
1.6028g sodium hydroxides are dissolved in the clean small beaker containing 5mL distilled water, and 5mL third is then accurately measured under ice-water bath
Olefin(e) acid stirs in drop and is added dropwise in sodium hydroxide solution, weighs 0.0232g crosslinking agents and 0.3015g after complete reaction
Acrylamide is added thereto, and stirring is completely dissolved up to it, will be added in above-mentioned solution containing evenly dispersed magnetic ball solution,
Stirring keeps its evenly dispersed, weighs 0.116g initiators, is added in solution, stirring makes it completely dissolved, and above-mentioned solution is placed in
In ultrasound environments, control water temperature is at 45 DEG C, up to the reaction was complete for it under nitrogen protection.It is 0.3* that the gel of synthesis, which is cut into specification,
The fritter of 0.3*0.3mm washs 2h with soaked in absolute ethyl alcohol, repeats 3-4 times, be sealed after vacuum drying.
Embodiment 3
It is that the magnetic ball of 100nm or so is placed in sealing container to take 0.15g grain sizes at room temperature, is added after 5-10mL distilled water
Ultrasound is evenly dispersed to its under logical nitrogen protection, weighs 0.3g sodium lignin sulfonates and is completely dissolved in 5mL distilled water, accurately weighs
2.0400 g sodium hydroxides are dissolved in the clean small beaker containing 5mL distilled water, and 5mL third is then accurately measured under ice-water bath
Olefin(e) acid stirs in drop and is added dropwise in sodium hydroxide solution, weighs 0.0174g crosslinking agents and 0.1005g after complete reaction
Acrylamide is added thereto, and stirring is completely dissolved up to it, will be added in above-mentioned solution containing evenly dispersed magnetic ball solution,
Stirring keeps its evenly dispersed, weighs 0.087g initiators, is added in solution, stirring makes it completely dissolved, and above-mentioned solution is placed in
In ultrasound environments, control water temperature is at 50 DEG C, up to the reaction was complete for it under nitrogen protection.It is 0.3* that the gel of synthesis, which is cut into specification,
The fritter of 0.3*0.3mm washs 2h with soaked in absolute ethyl alcohol, repeats 3-4 times, be sealed after vacuum drying.
Embodiment 4
It is that the magnetic ball of 100nm or so is placed in sealing container to take 0.2g grain sizes at room temperature, is added after 5-10mL distilled water
Ultrasound is evenly dispersed to its under logical nitrogen protection, weighs 0.4g sodium lignin sulfonates and is completely dissolved in 5mL distilled water, accurately weighs
1.7485g sodium hydroxides are dissolved in the clean small beaker containing 5mL distilled water, and 5mL third is then accurately measured under ice-water bath
Olefin(e) acid stirs in drop and is added dropwise in sodium hydroxide solution, weighs 0.0116g crosslinking agents and 0.5025g after complete reaction
Acrylamide is added thereto, and stirring is completely dissolved up to it, will be added in above-mentioned solution containing evenly dispersed magnetic ball solution,
Stirring keeps its evenly dispersed, weighs 0.174g initiators, is added in solution, stirring makes it completely dissolved, and above-mentioned solution is placed in
In ultrasound environments, control water temperature is at 40 DEG C, up to the reaction was complete for it under nitrogen protection.It is 0.3* that the gel of synthesis, which is cut into specification,
The fritter of 0.3*0.3mm washs 2h with soaked in absolute ethyl alcohol, repeats 3-4 times, be sealed after vacuum drying.
Embodiment 5
It is that the magnetic ball of 100nm or so is placed in sealing container to take 0.05g grain sizes at room temperature, is added after 5-10mL distilled water
Ultrasound is evenly dispersed to its under logical nitrogen protection, weighs 0.5g sodium lignin sulfonates and is completely dissolved in 5mL distilled water, accurately weighs
1.8942g sodium hydroxides are dissolved in the clean small beaker containing 5mL distilled water, and 5mL third is then accurately measured under ice-water bath
Olefin(e) acid stirs in drop and is added dropwise in sodium hydroxide solution, weighs 0.0116g crosslinking agents and 0.5025g after complete reaction
Acrylamide is added thereto, and stirring is completely dissolved up to it, will be added in above-mentioned solution containing evenly dispersed magnetic ball solution,
Stirring keeps its evenly dispersed, weighs 0.116g initiators, is added in solution, stirring makes it completely dissolved, and above-mentioned solution is placed in
In ultrasound environments, control water temperature is at 45 DEG C, up to the reaction was complete for it under nitrogen protection.It is 0.3* that the gel of synthesis, which is cut into specification,
The fritter of 0.3*0.3mm washs 2h with soaked in absolute ethyl alcohol, repeats 3-4 times, be sealed after vacuum drying.
As can be seen from Figure 1, there are some sizes on the surface of vacuum drying sodium lignin sulfonate magnetic hydrogel sample not
One hole.
As can be seen from Figure 2, there are many spherical in the cross section of vacuum drying sodium lignin sulfonate magnetic hydrogel sample
Particulate matter, there is also some irregular gaps.
From figure 3, it can be seen that after the surface amplification of vacuum drying sodium lignin sulfonate magnetic hydrogel sample, can be observed
Aperture is apparent and intensive.
As can be seen from Figure 4, after the inside amplification of vacuum drying sodium lignin sulfonate magnetic hydrogel sample, can be observed
Particulate matter is more obvious.
Swelling ratio of the sample in distilled water reaches 545g/g.
Claims (6)
1. a kind of preparation method of lignosulphonates magnetic hydrogel, which is characterized in that include the following steps：
（1）It takes magnetic ball in sealing container at room temperature, ultrasonic disperse under nitrogen protection after distilled water is added, at interval of
10min shakes with hands 1min until magnetic ball is evenly dispersed；Magnetic ball solution is obtained, it is spare；
The magnetic ball is ferriferrous oxide nano magnetic ball, and synthetic method is：
The Fe (Cl) of 0.008mol is taken at room temperature3•6H2The NaAc 3H of O and 0.04mol2O is dissolved in the ethylene glycol of 35mL respectively
In, 0.5g sodium lignin sulfonates, stirring and dissolving, then magnetic agitation are added after mixing is allowed to evenly dispersed within 20 minutes；It will be above-mentioned
Solution moves into autoclave, reacts 8h at a temperature of 220 DEG C, is cooled to room temperature；Gained precipitation mixture is centrifuged, is precipitated
It is cleaned 3 times, then with washes of absolute alcohol 3 times, is centrifuged with deionized water；Solid after separation is put into vacuum drying chamber
Dry 12h, the temperature of the vacuum drying chamber are set as 60 DEG C；
（2）Sodium lignin sulfonate is weighed, is completely dissolved in distilled water, lignin sulfonic acid sodium solution is obtained, it is spare；
（3）Sodium hydroxide is added in distilled water, is made it completely dissolved under stirring, is cooled to room temperature；Under ice-water bath, by propylene
Acid is added dropwise in sodium hydroxide solution, and is stirred continuously, and after complete reaction, addition crosslinking agent stirs completely molten to it
Solution, then adds acrylamide and stirs to it and be completely dissolved；Obtain solution A；
（4）By step（1）The magnetic ball solution and step of gained（2）Gained lignin sulfonic acid sodium solution is added to step（3）Gained
In solution A, stirring keeps its evenly dispersed, and initiator is added, and stirring makes it completely dissolved, and obtains solution B, and nitrogen is led to after sealing and is protected
Shield；
（5）Solution B is placed in ultrasound environments, control water temperature is under 40-50 DEG C, nitrogen protection up to the reaction was complete for it；
（6）The gel of synthesis is cut into the fritter that specification is 0.3*0.3*0.3mm, 2h is washed with soaked in absolute ethyl alcohol, repeats 3-4
It is secondary, it is sealed after vacuum drying；
The magnetic ball：Sodium lignin sulfonate, sodium hydroxide, acrylic acid, crosslinking agent, acrylamide, initiator amount ratio be
0.05-0.5g ：0.1-0.5g ：1-2g：5mL：0.01-0.03g：0.1-0.7g：0.05-0.2g.
2. preparation method according to claim 1, which is characterized in that step（1）In, the magnetic spherolite diameter is 100nm.
3. preparation method according to claim 1, which is characterized in that step（2）In, in the lignin sulfonic acid sodium solution
A concentration of 0.02 ~ 0.1g/mL of sodium lignin sulfonate.
4. preparation method according to claim 1, which is characterized in that step（3）In, sodium hydroxide is dissolved in distilled water
A concentration of 0.2 ~ 0.4 g/mL.
5. preparation method according to claim 1, which is characterized in that step（3）In, the crosslinking agent is N, and N '-is sub-
Bisacrylamide；Step（4）In, the initiator is ammonium persulfate.
6. preparation method according to claim 1, which is characterized in that step（6）In, the vacuum drying temperature is 60
~80℃。
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| CN106075791A (en) * | 2016-07-20 | 2016-11-09 | 周荣 | A kind of preparation method of polymolecularity aerosol extinguishing agent |
| 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 |
| CN108676121B (en) * | 2018-04-16 | 2021-02-05 | 中国林业科学研究院亚热带林业研究所 | Magnetic hemicellulose-based hydrogel |
| 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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| CN103923274A (en) * | 2014-04-01 | 2014-07-16 | 江苏大学 | Environmental-friendly lignin super absorbent resin and preparation method thereof |
| CN104845006A (en) * | 2015-05-11 | 2015-08-19 | 东华大学 | Magnetic acrylamide hydrogel and preparation method thereof |
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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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| CN103923274A (en) * | 2014-04-01 | 2014-07-16 | 江苏大学 | Environmental-friendly lignin super absorbent resin and preparation method thereof |
| CN104925870A (en) * | 2015-05-08 | 2015-09-23 | 江苏大学 | Solvothermal method for preparing nano-grade ferroferric oxide |
| CN104845006A (en) * | 2015-05-11 | 2015-08-19 | 东华大学 | Magnetic acrylamide hydrogel and preparation method thereof |
| 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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