CN106589264B - A kind of preparation method of acrylic composite hydrogel - Google Patents
A kind of preparation method of acrylic composite hydrogel Download PDFInfo
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- CN106589264B CN106589264B CN201610991087.2A CN201610991087A CN106589264B CN 106589264 B CN106589264 B CN 106589264B CN 201610991087 A CN201610991087 A CN 201610991087A CN 106589264 B CN106589264 B CN 106589264B
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- hydroxide solution
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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 present invention provides a kind of preparation methods of acrylic composite hydrogel, include the following steps: (1) that at room temperature, sodium hydroxide solution is placed in ice-water bath, pipettes acrylic acid solution and be added dropwise in sodium hydroxide solution under constant stirring, after completion of the reaction, mixed liquor A is obtained；Step 2 sequentially adds lignosulfonates, glucan, initiator and crosslinking agent into mixed liquor A, is stirred continuously, and makes it dissolve completely, obtains mixed liquid B；Step 3 seals obtained mixed liquid B in transfer ultrasonic cleaner, under constant temperature conditions ultrasonic reaction, takes out product after the reaction was completed and shreds, and is handled with soaked in absolute ethyl alcohol；Step 4 dries the product placement after immersion treatment in a vacuum drying oven, and pulverization process obtains final product acrylic composite hydrogel, is placed in drier and saves.Present invention process is simple, easily operated, low in cost, realizes the greenization of synthesis technology and the efficient utilization of trade waste sodium lignin sulfonate.
Description
Technical field
The present invention relates to a kind of preparation methods of acrylic composite hydrogel, and it is single for relating generally to one kind with acrylic acid
Body, sodium lignin sulfonate and glucan are compound, utilize the preparation method of ultrasonic method acrylic acid synthesizing base composite hydrogel.
Background technique
Hydrogel is a kind of lightly crosslinked novel high polymer functional material with tridimensional network.It is absorbable to reach certainly
It weighs hundreds times or even thousands of times of moisture, and is able to maintain internal moisture under certain pressure and temperature and is not lost, have excellent
Good weatherability and liquid retention.Currently, 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 compound and is modified to hydrogel, reduces the cost for preparing hydrogel, produces after compound
Water absorbent rate, salt tolerance and the gel strength of object are all greatly improved.Therefore, biomass system hydrogel is concerned.It is wooden
Plain sodium sulfonate is one of the principal by product of paper-making pulping industry, and hydroxyl, sulfonic group and methoxyl group etc. are contained on molecular structure
Various functional groups, can occur under certain condition with many kinds of substance a variety of 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 measuring its performance.Dextran molecule
Contain a large amount of non-ionic hydrophilic functional group hydroxyl in structure, rate of water absorption can be greatly improved by being introduced into hydrogel, be changed
The performance of kind hydrogel.
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.Benefit
With starch, cellulose and acrylic acid copolymer, the reason is that starch, cellulose, from a wealth of sources and cheap, and biological degradability compared with
It is good.Biggish specific surface area is the common trait of mineral powder, and is present in its surface there are many hydroxyl, with acrylate copolymer
In conjunction with very properly, the mineral that the characteristics such as ion exchangeable, dilatancy, heat-resisting quantity and lower shrinking percentage all have can add
To utilize, reacted with modification by copolymerization with acrylic acid, the acrylic composite hydrogel that such properties are good, at low cost
It can prepare.
Summary of the invention
The purpose of the present invention is pass through ultrasound with acrylic acid principal monomer, graft copolymerization sodium lignin sulfonate and glucan
Method acrylic acid synthesizing base composite hydrogel, technique green is simple, and raw material is easy to get, low in cost and can to reuse papermaking useless
Gurry reduces environmental pressure, is suitable for industrialized production.
Technical scheme is as follows:
A kind of preparation method of acrylic composite hydrogel, includes the following steps:
Step 1, at room temperature, sodium hydroxide solution is placed in ice-water bath, pipette acrylic acid solution under constant stirring by
It is added dropwise in sodium hydroxide solution and is reacted, after completion of the reaction, obtain mixed liquor A；
Step 2 sequentially adds lignosulfonates, glucan, initiator and crosslinking agent into mixed liquor A, is stirred continuously,
It makes it dissolve completely, obtains mixed liquid B；
Step 3 seals obtained mixed liquid B in transfer ultrasonic cleaner, under constant temperature conditions ultrasonic reaction, reaction
Product is taken out after the completion and is shredded, and is handled with soaked in absolute ethyl alcohol；
Step 4 dries the product placement after immersion treatment in a vacuum drying oven, and pulverization process obtains final product
Acrylic composite hydrogel, is placed in drier and saves.
In step 1, when preparing mixed liquor A, the concentration of used sodium hydroxide solution is 9.8mmol/L, used
The concentration of acrylic acid solution is 14.57mol/L；The volume ratio of used acrylic acid solution and sodium hydroxide solution is 1:1, institute
The reaction time stated is 10min.
In step 2, when preparing mixed liquid B, used lignosulfonates, glucan, initiator, crosslinking agent and 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, when preparing mixed liquid B, used lignosulfonates are sodium lignin sulfonate, used initiation
Agent is ammonium persulfate, and used crosslinking agent is N, N- methylene-bisacrylamide.
In step 3, the constant temperature is 60~70 DEG C, ultrasonic time 2h, is with the time of soaked in absolute ethyl alcohol
12h。
The utility model has the advantages that
The present invention, by addition sodium lignin sulfonate, glucan, crosslinking agent and initiator, is utilized using acrylic acid as monomer
Ultrasonic method prepares acrylic composite hydrogel.Process flow is simple, easily operated, low in cost as the result is shown, while also real
The greenization of synthesis technology and the efficient utilization of trade waste sodium lignin sulfonate are showed.Prepared swelling behavior absorption
It is functional, it is suitble to industrialized production.
Detailed description of the invention
Fig. 1 is the infrared figure of 2 sample of embodiment；
Fig. 2 is the scanning electron microscope (SEM) photograph of 2 sample of embodiment.
Specific embodiment
Below with reference to specific implementation example, the present invention will be further described.
Embodiment 1
Room temperature calls 1.96g sodium hydroxide in the following text in small beaker, and 5mL deionized water, which is added, dissolves it sufficiently, is placed in ice water
In bath, the acrylic acid solution for accurately pipetting 5mL 14.57mol/L is slowly added in sodium hydroxide solution dropwise under constant stirring
10min is reacted, sufficiently takes out and is placed at room temperature after reaction, then sequentially add 0.05g sodium lignin sulfonate, the Portugal 0.1g in order
Glycan, 0.06g ammonium persulfate, 0.0085g N, N- methylene-bisacrylamide are stirred continuously, after making it dissolve completely, sealing
Transfer is set in KQ-100B type ultrasonic cleaner, and control water temperature is taken out product and cut after 60~70 DEG C of temperature, ultrasonic reaction 2h
Broken frustillatum, with soaked in absolute ethyl alcohol 12h；By the product placement after immersion treatment, drying to constant weight in a vacuum drying oven,
Pulverization process is carried out with pulverizer, then collects and places in drier and save.
Embodiment 2
Room temperature calls 1.96g sodium hydroxide in the following text in small beaker, and 5mL deionized water, which is added, dissolves it sufficiently, is placed in ice water
In bath, the acrylic acid solution for accurately pipetting 5mL 14.57mol/L is slowly added in sodium hydroxide solution dropwise under constant stirring
10min is reacted, sufficiently takes out and is placed at room temperature after reaction, then sequentially add 0.05g sodium lignin sulfonate, the Portugal 0.2g in order
Glycan, 0.08g ammonium persulfate, 0.0085g N, N- methylene-bisacrylamide are stirred continuously, after making it dissolve completely, sealing
Transfer is set in KQ-100B type ultrasonic cleaner, and control water temperature is taken out product and cut after 60~70 DEG C of temperature, ultrasonic reaction 2h
Broken frustillatum, with soaked in absolute ethyl alcohol 12h；By the product placement after immersion treatment, drying to constant weight in a vacuum drying oven,
Pulverization process is carried out with pulverizer, then collects and places in drier and save.
In Fig. 1, in 3420cm-1Place is O-H stretching vibration absworption peak, 2940cm-1Place is C-H stretching vibration absworption peak,
1700cm-1Place is the absorption peak of C=O in carboxyl functional group, 1170cm-1Locate-SO in sodium lignin sulfonate3The absorption peak of H,
850cm-1Place is the characteristic absorption peak of glucan.
In Fig. 2, there is a large amount of hole configurations in hydrogel surface, and hydrogel water suction and absorption property characteristic mainly just come from
In this surface hole defect structure.
Embodiment 3
Room temperature calls 1.96g sodium hydroxide in the following text in small beaker, and 5mL deionized water, which is added, dissolves it sufficiently, is placed in ice water
In bath, the acrylic acid solution for accurately pipetting 5mL 14.57mol/L is slowly added in sodium hydroxide solution dropwise under constant stirring
10min is reacted, sufficiently takes out and is placed at room temperature after reaction, then sequentially add 0.15g sodium lignin sulfonate, the Portugal 0.3g in order
Glycan, 0.1g ammonium persulfate, 0.0145g N, N- methylene-bisacrylamide are stirred continuously, and after making it dissolve completely, sealing turns
In dislocation KQ-100B type ultrasonic cleaner, control water temperature is taken out product and is shredded after 60~70 DEG C of temperature, ultrasonic reaction 2h
Frustillatum, with soaked in absolute ethyl alcohol 12h；By the product placement after immersion treatment, drying to constant weight in a vacuum drying oven, uses
Pulverizer carries out pulverization process, then collects and places in drier and saves.
Embodiment 4
Room temperature calls 1.96g sodium hydroxide in the following text in small beaker, and 5mL deionized water, which is added, dissolves it sufficiently, is placed in ice water
In bath, the acrylic acid solution for accurately pipetting 5mL 14.57mol/L is slowly added in sodium hydroxide solution dropwise under constant stirring
10min is reacted, sufficiently takes out and is placed at room temperature after reaction, then sequentially add 0.1g sodium lignin sulfonate, the Portugal 0.2g in order
Glycan, 0.12g ammonium persulfate, 0.0115g N, N- methylene-bisacrylamide are stirred continuously, after making it dissolve completely, sealing
Transfer is set in KQ-100B type ultrasonic cleaner, and control water temperature is taken out product and cut after 60~70 DEG C of temperature, ultrasonic reaction 2h
Broken frustillatum, with soaked in absolute ethyl alcohol 12h；By the product placement after immersion treatment, drying to constant weight in a vacuum drying oven,
Pulverization process is carried out with pulverizer, then collects and places in drier and save.
Embodiment 5
Room temperature calls 1.96g sodium hydroxide in the following text in small beaker, and 5mL deionized water, which is added, dissolves it sufficiently, is placed in ice water
In bath, the acrylic acid solution for accurately pipetting 5mL 14.57mol/L is slowly added in sodium hydroxide solution dropwise under constant stirring
10min is reacted, sufficiently takes out and is placed at room temperature after reaction, then sequentially add 0.2g sodium lignin sulfonate, the Portugal 0.4g in order
Glycan, 0.12g ammonium persulfate, 0.017g N, N- methylene-bisacrylamide are stirred continuously, and after making it dissolve completely, sealing turns
In dislocation KQ-100B type ultrasonic cleaner, control water temperature is taken out product and is shredded after 60~70 DEG C of temperature, ultrasonic reaction 2h
Frustillatum, with soaked in absolute ethyl alcohol 12h；By the product placement after immersion treatment, drying to constant weight in a vacuum drying oven, uses
Pulverizer carries out pulverization process, then collects and places in drier and saves.
Claims (4)
1. a kind of preparation method of acrylic composite hydrogel, which comprises the steps of:
Step 1, at room temperature, sodium hydroxide solution is placed in ice-water bath, pipette acrylic acid solution under constant stirring dropwise plus
Enter in sodium hydroxide solution and reacted, after completion of the reaction, obtains mixed liquor A；
Step 2 sequentially adds lignosulfonates, glucan, initiator and crosslinking agent into mixed liquor A, is stirred continuously, makes it
Dissolution completely, obtains mixed liquid B；
Step 3 seals obtained mixed liquid B in transfer ultrasonic cleaner, and ultrasonic reaction, reaction are completed under constant temperature conditions
Product is taken out afterwards and is shredded, and is handled with soaked in absolute ethyl alcohol；
Step 4 dries the product placement after immersion treatment in a vacuum drying oven, and pulverization process obtains final product propylene
Acidic group composite hydrogel, is placed in drier and saves；
In the step 1, when preparing mixed liquor A, the concentration of used sodium hydroxide solution is 9.8mmol/L, used
The concentration of acrylic acid solution is 14.57mol/L；The volume ratio of used acrylic acid solution and sodium hydroxide solution is 1:1, institute
The reaction time stated is 10min.
2. a kind of preparation method of acrylic composite hydrogel according to claim 1, which is characterized in that in step 2,
When preparing mixed liquid B, used lignosulfonates, glucan, initiator, crosslinking agent and mixed liquor A amount ratio be
0.05~0.2g:0.1~0.4g:0.06~0.12g:0.0085~0.017g:10mL.
3. a kind of preparation method of acrylic composite hydrogel according to claim 1, which is characterized in that step 2
In, when preparing mixed liquid B, used lignosulfonates are sodium lignin sulfonate, and used initiator is ammonium persulfate,
Used crosslinking agent is N,N methylene bis acrylamide.
4. a kind of preparation method of acrylic composite hydrogel according to claim 1, which is characterized in that in step 3,
The constant temperature is 60~70 DEG C, and ultrasonic time 2h is 12h with the time of soaked in absolute ethyl alcohol.
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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 |
| CN111261878B (en) * | 2020-01-23 | 2022-06-14 | 同济大学 | Catalyst slurry containing aqueous gel, catalyst layer and fuel cell electrode produced therefrom |
| 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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| 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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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
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| "Dextran-based hydrogels as stimuli-sensitive carriers for zidovudine delivery";Thakur, Shiwali等;《Trends in Carbohydrate Research 》;20141231;第6卷(第2期);第7-16页 |
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