CN106589264A - Method for preparing crylic-acid-based composite hydrogel - Google Patents
Method for preparing crylic-acid-based composite hydrogel Download PDFInfo
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- CN106589264A CN106589264A CN201610991087.2A CN201610991087A CN106589264A CN 106589264 A CN106589264 A CN 106589264A CN 201610991087 A CN201610991087 A CN 201610991087A CN 106589264 A CN106589264 A CN 106589264A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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Abstract
The invention provides a method for preparing crylic-acid-based composite hydrogel. The method comprises the steps that 1, at room temperature, a sodium hydroxide solution is placed in an ice-water bath, a crylic acid solution is moved and taken and is added into the sodium hydroxide solution drop by drop under constant stirring, and after the reaction is finished, mixed liquid A is obtained; 2, lignosulfonate, glucan, an initiator and a cross-linking agent are added into the mixed liquid A in sequence, constant stirring is carried out, the lignosulfonate, the glucan, the initiator and the cross-linking agent are completely dissolved, and mixed liquid B is obtained; 3, the obtained mixed liquid B is sealed and transferred into an ultrasonic cleaner, an ultrasonic reaction is carried out under the constant-temperature condition, the product is taken out and cut after the reaction is completed, and absolute ethyl alcohol is used for soaking treatment; 4, the soaked product is placed in a vacuum drying box to be dried, smashing is carried out, and the final product crylic-acid-based composite hydrogel is obtained and placed in a dryer to be stored. The method is simple in process, easy to operate and low in cost, and meets environmental friendliness of a synthetic process and efficient utilization of industrial waste sodium lignin sulfonate.
Description
Technical field
The present invention relates to a kind of preparation method of acrylic composite aquogel, relates generally to one kind with acrylic acid as list
Body, sodium lignin sulfonate and glucosan are complex, using the preparation method of ultrasonic method acrylic acid synthesizing base composite aquogel.
Background technology
Hydrogel is the lightly crosslinked novel high polymer functional material with tridimensional network of a class.It is absorbable to reach certainly
Tuple Radix Achyranthis Bidentatae or even thousands of times of moisture, and internal moisture can be kept under certain pressure and temperature not to be lost in, with excellent
Good weatherability and guarantor's fluidity.At present, in health care, construction material, agricultural gardening, food industry and petrochemical industry and ring
The fields such as border protection are widely applied.With social sustainable development, the hydrogel with biodegradable is received
The great attention of people, introduces cheap complex and hydrogel is modified, and reduces the cost for preparing hydrogel, produces after being combined
The water absorbent rate of thing, salt tolerance and gel strength are all greatly improved.Therefore, biomass system hydrogel receives much concern.It is wooden
Plain sodium sulfonate is one of principal by product of paper-making pulping industry, containing hydroxyl, sulfonic group and methoxyl group etc. on its molecular structure
Various functional groups, under certain condition can with many kinds of substance occur various modified-reaction such as sulfonating agent sulfonation, have it is oxidizing,
Complexing of metal ion or grafting etc..The absorption speed of hydrogel is also an important indicator for weighing its performance.Dextran molecule
Contain substantial amounts of non-ionic hydrophilic functional group hydroxyl in structure, being introduced in hydrogel can greatly improve rate of water absorption, change
The performance of kind hydrogel.
Acrylic acid seriess 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, reason is starch, cellulose, wide material sources and cheap, and biological degradability compared with
It is good.Larger specific surface area is the common trait of mineral powder, and has many hydroxyls to be present in its surface, with acrylate copolymer
With reference to very properly, the mineral that the characteristic such as ion exchangeable, dilatancy, heat-resisting quantity and relatively low shrinkage factor all possesses can add
To utilize, reacted with acrylic acid with modification by copolymerization, such properties are good, the acrylic composite aquogel of low cost
Just can prepare.
The content of the invention
The purpose of the present invention is with acrylic acid principal monomer, graft copolymerization sodium lignin sulfonate and glucosan, by ultrasound
Method acrylic acid synthesizing base composite aquogel, technique green is simple, and raw material is easy to get, with low cost and can reuse papermaking and give up
Gurry, reduces ambient pressure, is suitable to industrialized production.
Technical scheme is as follows：
A kind of preparation method of acrylic composite aquogel, comprises the steps：
Under step 1, room temperature, sodium hydroxide solution is placed in ice-water bath, pipette acrylic acid solution in the case where being stirred continuously by
It is added dropwise in sodium hydroxide solution and is reacted, after completion of the reaction, obtains mixed liquor A；
Step 2, in mixed liquor A lignosulfonates, glucosan, initiator and cross-linking agent are sequentially added, are stirred continuously,
Make its dissolving complete, obtain mixed liquid B；
Step 3, by the mixed liquid B for obtaining sealing transfer ultrasonic cleaner in, the ultrasonic reaction under constant temperature, reaction
After the completion of take out and product and shred, and processed with soaked in absolute ethyl alcohol；
Step 4, the product after immersion treatment is placed in vacuum drying oven and is dried, pulverization process obtains final product
Acrylic composite aquogel, is positioned in exsiccator and preserves.
In step 1, when preparing mixed liquor A, the concentration of the sodium hydroxide solution for being used is 9.8mmol/L, is used
The concentration of acrylic acid solution is 14.57mol/L；The acrylic acid solution for being used is 1 with the volume ratio of sodium hydroxide solution：1, institute
The response time stated is 10min.
In step 2, when preparing mixed liquid B, the lignosulfonates that used, glucosan, initiator, cross-linking agent with mix
The amount ratio of liquid A is 0.05～0.2g：0.1～0.4g：0.06～0.12g：0.0085～0.017g：10mL.
In step 2, prepare mixed liquid B when, the lignosulfonates for being used be sodium lignin sulfonate, the initiation for being used
Agent is Ammonium persulfate., and the cross-linking agent for being used is N,N methylene bis acrylamide.
In step 3, described constant temperature is 60～70 DEG C, and ultrasonic time is 2h, is with the time of soaked in absolute ethyl alcohol
12h。
Beneficial effect：
The present invention, by adding sodium lignin sulfonate, glucosan, cross-linking agent and initiator, is utilized with acrylic acid as monomer
Ultrasonic method prepares acrylic composite aquogel.As a result show that technological process is simple, easily operated, with low cost, while also real
The greenization of synthesis technique and the efficient utilization of trade waste sodium lignin sulfonate are showed.Prepared swelling behavior absorption
It is functional, it is adapted to industrialized production.
Description of the drawings
Fig. 1 is the infrared figure of the sample of embodiment 2；
Fig. 2 is the scanning electron microscope (SEM) photograph of the sample of embodiment 2.
Specific embodiment
With reference to example is embodied as, the present invention will be further described.
Embodiment 1
Room temperature calls 1.96g sodium hydroxide in the following text in small beaker, adds 5mL deionized waters it is fully dissolved, and is placed in frozen water
In bath, the acrylic acid solution for accurately pipetting 5mL 14.57mol/L is dropwise slowly added in sodium hydroxide solution in the case where being stirred continuously
Take out after reaction 10min, fully reaction and put at room temperature, 0.05g sodium lignin sulfonates, 0.1g Portugals are then sequentially added in order
Polysaccharide, 0.06g Ammonium persulfate .s, 0.0085g N,N methylene bis acrylamides are stirred continuously so as to after dissolving completely, sealing
Transfer is put in KQ-100B type ultrasonic cleaners, and control water temperature is taken out product in 60～70 DEG C of temperature, after ultrasonic reaction 2h and cut
Broken frustillatum, uses soaked in absolute ethyl alcohol 12h；Product after immersion treatment is placed in vacuum drying oven and is dried to constant weight,
Pulverization process is carried out with pulverizer, preservation in exsiccator is then collected and place.
Embodiment 2
Room temperature calls 1.96g sodium hydroxide in the following text in small beaker, adds 5mL deionized waters it is fully dissolved, and is placed in frozen water
In bath, the acrylic acid solution for accurately pipetting 5mL 14.57mol/L is dropwise slowly added in sodium hydroxide solution in the case where being stirred continuously
Take out after reaction 10min, fully reaction and put at room temperature, 0.05g sodium lignin sulfonates, 0.2g Portugals are then sequentially added in order
Polysaccharide, 0.08g Ammonium persulfate .s, 0.0085g N,N methylene bis acrylamides are stirred continuously so as to after dissolving completely, sealing
Transfer is put in KQ-100B type ultrasonic cleaners, and control water temperature is taken out product in 60～70 DEG C of temperature, after ultrasonic reaction 2h and cut
Broken frustillatum, uses soaked in absolute ethyl alcohol 12h；Product after immersion treatment is placed in vacuum drying oven and is dried to constant weight,
Pulverization process is carried out with pulverizer, preservation in exsiccator is then collected and place.
In Fig. 1, in 3420cm-1Locate as O-H stretching vibration absworption peaks, 2940cm-1Locate as C-H stretching vibration absworption peaks,
1700cm-1Locate as the absworption peak of C=O in carboxyl functional group, 1170cm-1- SO in place's sodium lignin sulfonate3The absworption peak of H,
850cm-1Locate the characteristic absorption peak for glucosan.
In Fig. 2, there is substantial amounts of pore space structure in hydrogel surface, hydrogel water suction and absorption property characteristic it is main just from
In this surface hole defect structure.
Embodiment 3
Room temperature calls 1.96g sodium hydroxide in the following text in small beaker, adds 5mL deionized waters it is fully dissolved, and is placed in frozen water
In bath, the acrylic acid solution for accurately pipetting 5mL 14.57mol/L is dropwise slowly added in sodium hydroxide solution in the case where being stirred continuously
Take out after reaction 10min, fully reaction and put at room temperature, 0.15g sodium lignin sulfonates, 0.3g Portugals are then sequentially added in order
Polysaccharide, 0.1g Ammonium persulfate .s, 0.0145g N,N methylene bis acrylamides are stirred continuously so as to after dissolving completely, and sealing turns
In dislocation KQ-100B type ultrasonic cleaners, control water temperature is taken out product in 60～70 DEG C of temperature, after ultrasonic reaction 2h and is shredded
Frustillatum, uses soaked in absolute ethyl alcohol 12h；Product after immersion treatment is placed in vacuum drying oven and is dried to constant weight, used
Pulverizer carries out pulverization process, then collects and place preservation in exsiccator.
Embodiment 4
Room temperature calls 1.96g sodium hydroxide in the following text in small beaker, adds 5mL deionized waters it is fully dissolved, and is placed in frozen water
In bath, the acrylic acid solution for accurately pipetting 5mL 14.57mol/L is dropwise slowly added in sodium hydroxide solution in the case where being stirred continuously
Take out after reaction 10min, fully reaction and put at room temperature, 0.1g sodium lignin sulfonates, 0.2g Portugals are then sequentially added in order
Polysaccharide, 0.12g Ammonium persulfate .s, 0.0115g N,N methylene bis acrylamides are stirred continuously so as to after dissolving completely, sealing
Transfer is put in KQ-100B type ultrasonic cleaners, and control water temperature is taken out product in 60～70 DEG C of temperature, after ultrasonic reaction 2h and cut
Broken frustillatum, uses soaked in absolute ethyl alcohol 12h；Product after immersion treatment is placed in vacuum drying oven and is dried to constant weight,
Pulverization process is carried out with pulverizer, preservation in exsiccator is then collected and place.
Embodiment 5
Room temperature calls 1.96g sodium hydroxide in the following text in small beaker, adds 5mL deionized waters it is fully dissolved, and is placed in frozen water
In bath, the acrylic acid solution for accurately pipetting 5mL 14.57mol/L is dropwise slowly added in sodium hydroxide solution in the case where being stirred continuously
Take out after reaction 10min, fully reaction and put at room temperature, 0.2g sodium lignin sulfonates, 0.4g Portugals are then sequentially added in order
Polysaccharide, 0.12g Ammonium persulfate .s, 0.017g N,N methylene bis acrylamides are stirred continuously so as to after dissolving completely, and sealing turns
In dislocation KQ-100B type ultrasonic cleaners, control water temperature is taken out product in 60～70 DEG C of temperature, after ultrasonic reaction 2h and is shredded
Frustillatum, uses soaked in absolute ethyl alcohol 12h；Product after immersion treatment is placed in vacuum drying oven and is dried to constant weight, used
Pulverizer carries out pulverization process, then collects and place preservation in exsiccator.
Claims (5)
1. a kind of preparation method of acrylic composite aquogel, it is characterised in that comprise the steps：
Under step 1, room temperature, sodium hydroxide solution is placed in ice-water bath, pipettes acrylic acid solution and dropwise add in the case where being stirred continuously
Enter in sodium hydroxide solution and reacted, after completion of the reaction, obtain mixed liquor A；
Step 2, in mixed liquor A lignosulfonates, glucosan, initiator and cross-linking agent are sequentially added, are stirred continuously so as to
Dissolving is complete, obtains mixed liquid B；
Step 3, by the mixed liquid B for obtaining sealing transfer ultrasonic cleaner in, the ultrasonic reaction under constant temperature, reaction is completed
Product is taken out afterwards and is shredded, and processed with soaked in absolute ethyl alcohol；
Step 4, the product after immersion treatment is placed in vacuum drying oven and is dried, pulverization process obtains final product propylene
Acidic group composite aquogel, is positioned in exsiccator and preserves.
2. the preparation method of a kind of acrylic composite aquogel according to claim 1, it is characterised in that in step 1,
When preparing mixed liquor A, the concentration of the sodium hydroxide solution for being used is 9.8mmol/L, the concentration of the acrylic acid solution for being used
For 14.57mol/L；The acrylic acid solution for being used is 1 with the volume ratio of sodium hydroxide solution：1, the described response time is
10min。
3. the preparation method of a kind of acrylic composite aquogel according to claim 1, it is characterised in that in step 2,
When preparing mixed liquid B, the amount ratio of the lignosulfonates, glucosan, initiator, cross-linking agent and the mixed liquor A that are used is
0.05～0.2g：0.1～0.4g：0.06～0.12g：0.0085～0.017g：10mL.
4. a kind of preparation method of acrylic composite aquogel according to claim 1 and 2, it is characterised in that step 2
In, when preparing mixed liquid B, the lignosulfonates for being used are sodium lignin sulfonate, and the initiator for being used is Ammonium persulfate.,
The cross-linking agent for being used is N,N methylene bis acrylamide.
5. the preparation method of a kind of acrylic composite aquogel according to claim 1, it is characterised in that in step 3,
Described constant temperature is 60～70 DEG C, and ultrasonic time is 2h, is 12h with the time of soaked in absolute ethyl alcohol.
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| CN201610991087.2A CN106589264B (en) | 2016-11-10 | 2016-11-10 | A kind of preparation method of acrylic composite hydrogel |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109232815A (en) * | 2018-07-20 | 2019-01-18 | 江苏大学 | A kind of preparation method and applications of acrylic acid complex polysaccharide class hydrogel |
| CN111261878A (en) * | 2020-01-23 | 2020-06-09 | 同济大学 | Catalyst slurry containing aqueous gel, catalyst layer and fuel cell electrode produced therefrom |
| CN113053578A (en) * | 2021-03-24 | 2021-06-29 | 上海上力特种电缆有限公司 | Water-blocking powder for waterproof cable, preparation method of water-blocking powder and waterproof cable |
| 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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- 2016-11-10 CN CN201610991087.2A patent/CN106589264B/en not_active Expired - Fee Related
Patent Citations (2)
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| WO2004066704A2 (en) * | 2003-01-17 | 2004-08-12 | Cornell Research Foundation, Inc. | Injectable hydrogel microspheres from aqueous two-phase system |
| CN105482130A (en) * | 2016-01-15 | 2016-04-13 | 江苏大学 | Preparation method of magnetic lignin sulfonate grafted hydrogel |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232815A (en) * | 2018-07-20 | 2019-01-18 | 江苏大学 | A kind of preparation method and applications of acrylic acid complex polysaccharide class hydrogel |
| CN111261878A (en) * | 2020-01-23 | 2020-06-09 | 同济大学 | Catalyst slurry containing aqueous gel, catalyst layer and fuel cell electrode produced therefrom |
| 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 |
| CN113053578A (en) * | 2021-03-24 | 2021-06-29 | 上海上力特种电缆有限公司 | Water-blocking powder for waterproof cable, preparation method of water-blocking powder and waterproof cable |
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