CN106380544A - Preparation method of graphene oxide doped environment-friendly super absorbent resin - Google Patents
Preparation method of graphene oxide doped environment-friendly super absorbent resin Download PDFInfo
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- CN106380544A CN106380544A CN201610812513.1A CN201610812513A CN106380544A CN 106380544 A CN106380544 A CN 106380544A CN 201610812513 A CN201610812513 A CN 201610812513A CN 106380544 A CN106380544 A CN 106380544A
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- 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
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
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Abstract
The invention belongs to a preparation method of graphene oxide doped environment-friendly super absorbent resin. The preparation method comprises: (1) adding 0.04g to 0.05g of graphene oxide into 25mL to 35mL of de-ionized water, and carrying out ultrasonic dispersion for 35 minutes to 45 minutes to obtain a uniformly dispersed graphene oxide solution; adding 0.7g to 0.75g of carboxymethyl cellulose into the graphene oxide solution, and uniformly stirring to obtain a transparent viscous solution; under the protection of nitrogen gas, heating the solution to 58 DEG C to 62 DEG C; keeping nitrogen gas bubbling for 25 minutes to 35 minutes; (2) adding 0.004g to 0.005g of N,N'-methylene-bisacrylamide into 7g to 8g of acrylic acid with the neutralization degree of 40 percent to 90 percent; carrying out the ultrasonic dispersion for 20 minutes to 50 minutes to obtain a homogeneous phase solution; (3) adding the solution obtained by the step (2) into the solution obtained by the step (1); stirring and raising the temperature to 68 DEG C to 72 DEG C under the protection of the nitrogen gas, and reacting for 2.5 hours to 3.5 hours; washing and drying.
Description
Technical field
The invention belongs to the preparation field of High hydrophilous resin and in particular to a kind of graphene oxide doped environmentally friendly
The preparation method of High hydrophilous resin.
Background technology
High hydrophilous resin is a kind of new polymerss hydrogel with appropriately crosslinked network structure, and it can be in very short time
The interior water absorbing hundreds of or even thousands of times of own wt, even if also can keep the long period under liter high-temperature and certain pressure
This solvent swelling state.Just because of these excellent performances, High hydrophilous resin is many in agricultural, health care, wastewater treatment etc.
Field is widely used.It is currently used in and prepare the raw material of High hydrophilous resin and be mainly derived from petrochemicals, such as third
Olefin(e) acid, acrylamide, acrylonitrile and polyvinyl alcohol etc..Use because High hydrophilous resin is generally used as disposable product,
Therefore high cost and difficult degradation become the major issue of the High hydrophilous resin of petrochemical materials preparation.Therefore, developing low-cost,
Environmentally friendly High hydrophilous resin is just particularly important.
At present, using natural polysaccharide, such as starch, cellulose, shitosan etc. is proved to hydrophilic high polymer monomer copolymerization
It is a kind of effective ways preparing inexpensive, environmentally friendly High hydrophilous resin.But merely by these natural Product formation
High hydrophilous resin, its combination property, such as gel strength, heat resistance, water absorption rate and water holding capacity etc. are difficult to produce with petrochemical industry
Condition ratio, therefore receives certain restriction in actual applications.
Content of the invention
It is an object of the invention to provide a kind of environment friend of graphene oxide doped with high water absorbing capacity and water holding capacity
The preparation method of good type High hydrophilous resin.
For achieving the above object, the technical solution used in the present invention is, a kind of graphene oxide doped environmentally friendly
The preparation method of High hydrophilous resin, comprises the following steps：1. by the graphite oxide of 0.04 ~ 0.05 g be added to 25 ~ 35 mL go from
In sub- water, ultrasonic disperse 35 ~ 45 minutes, obtain homodisperse graphene oxide（GO）Solution；Then molten in graphene oxide
The carboxymethyl cellulose of 0.7 ~ 0.75 g is added in liquid（CMC）, it is uniformly mixing to obtain transparent viscosity solution, nitrogen protection is lower will
Solution is heated to 58 ~ 62 DEG C, and keeps nitrogen bubble 25 ~ 35 minutes；2. add in the acrylic acid of 7 ~ 8g degree of neutralization 40-90%
The N of 0.004 ~ 0.005g, N '-methylene-bisacrylamide（MBA）, ultrasonic disperse 20 ~ 50 minutes, obtain homogeneous phase solution；3. will
2. step obtains solution and adds in the solution that 1. step obtains, and is warming up to 68 ~ 72 DEG C under stirring, nitrogen protection, and at 68 ~ 72 DEG C
Lower reaction 2.5 ~ 3.5 hours, washs, is dried, obtain the environmentally friendly High hydrophilous resin of graphene oxide doped.
Described step 3. in drying be at 70 DEG C be dried to constant weight.
Described graphite oxide can buy existing graphite oxide；Preferably, prepared using following methods：The burning of 250 mL
In bottle, add the analytically pure graphite powder of 2g, flask is placed in ice salt bath, add 50 mL concentrated sulphuric acids so that graphite powder is disperseed, then
It is slowly added to 1g sodium nitrate and 7g potassium permanganate under conditions of stirring, react 2 hours；Reaction flask is removed ice salt bath, puts
Enter to be gradually heated in oil bath 80 DEG C continue reaction 6h, stop heating, after being cooled to room temperature, add 30% hydrogen peroxide until
Do not have gas to release, product filtered, use hydrochloric acid solution, the deionized water wash of 0.1M respectively, deionized water disperses, centrifugation,
Graphite oxide is obtained after lyophilization.
There is the two-dimensional graphene of single atomic thickness and its oxide with its unique structure and excellent physico
Learn performance, surface of graphene oxide contains the oxy radicals such as abundant hydroxyl, carboxyl, epoxy, ketone, carbonyl, and these groups make
Graphene oxide has good hydrophilic, can be well dispersed in water being formed stable dispersion liquid.Therefore it is especially suitable for
For preparing hydrophilic nano composite material.Oxy radical one side using graphite oxide surface can increase super absorbent resin
The hydrophilic group quantity of fat, the oxy radical on another aspect surface can form hydrogen with the hydrophilic group in polymer mesh structure
Key, thus playing the effect of physical crosslinking, both effects, for increasing water absorption rate and water holding capacity, improve combination property and have
Important meaning.
The beneficial effect comprise that：The present invention adopts a kind of method of graft copolymerization, in cellulose base high water absorption
It has been successfully introduced into the graphene oxide of nano-lamellar structure in resin, be prepared for a kind of ring with high water absorbing capacity and water holding capacity
Border friendly High hydrophilous resin.Test result indicate that, the introducing of graphene oxide does not affect the formation mechenism of water-absorbing resin and interior
In structure, but very big impact is caused to its configuration of surface, the high water absorption of this graphene oxide doped of what is more important
Resin has more excellent water suction and water holding capacity, and hot property also has greatly improved simultaneously.
Brief description
Fig. 1 is the water-absorbent resin surfaces SEM figure of reference examples 1 preparation；
Fig. 2 is the water-absorbent resin surfaces SEM figure of embodiment 1 preparation；
Fig. 3 is embodiment 1 and the water-absorbing resin water absorbing capacity test result of reference examples 1 preparation；
Fig. 4 is embodiment 1 and the water holding capacity test result at 100 DEG C for the water-absorbing resin of reference examples 1 preparation；
Fig. 5 ties in the water holding capacity test under 4000rpm high speed centrifugation for the water-absorbing resin of embodiment 1 and reference examples 1 preparation
Really；
Fig. 6 is the building-up process schematic diagram of the environmentally friendly High hydrophilous resin of graphene oxide doped of the present invention.
Specific embodiment
Below in conjunction with embodiment, embodiment of the present invention is described in detail, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and be not construed as limiting the scope of the present invention.Unreceipted concrete in embodiment
Condition person, the condition according to normal condition or manufacturer's suggestion is carried out.Agents useful for same or the unreceipted production firm person of instrument, are
Can be by the commercially available conventional products bought and obtain.
Embodiment 1
A kind of preparation method of the environmentally friendly High hydrophilous resin of graphene oxide doped, comprises the following steps：1. by 0.045
The graphite oxide of g is added in 30 mL deionized waters, and ultrasonic disperse 40 minutes obtains homodisperse graphene oxide solution；
Then add the carboxymethyl cellulose of 0.72 g in graphene oxide solution, be uniformly mixing to obtain transparent viscosity solution, nitrogen
Under gas shielded, solution is heated to 60 DEG C, and keeps nitrogen bubble 30 minutes；2. add in the acrylic acid of 7.2g degree of neutralization 80%
The N of 0.0045g, N '-methylene-bisacrylamide, ultrasonic disperse 30 minutes, obtain homogeneous phase solution；3. 2. step is obtained molten
Liquid adds in the solution that 1. step obtains, and is warming up to 70 DEG C, and reacts 3 hours at 70 DEG C under stirring, nitrogen protection, washing,
It is dried, be dried at 70 DEG C to constant weight and obtain the environmentally friendly High hydrophilous resin of graphene oxide doped.The present embodiment oxygen
The building-up process schematic diagram of the environmentally friendly High hydrophilous resin of graphite alkene doping is as shown in Figure 1.
Described graphite oxide adopts following methods to prepare：In the flask of 250 mL, add the analytically pure graphite powder of 2g, will burn
Bottle is placed in ice salt bath, adds 50 mL concentrated sulphuric acids so that graphite powder is disperseed, is then slowly added to 1g sodium nitrate under conditions of stirring
With 7g potassium permanganate, react 2 hours；Reaction flask is removed ice salt bath, puts into and in oil bath, be gradually heated to 80 DEG C of continuation reactions
6h, stops heating, after being cooled to room temperature, adding 30% hydrogen peroxide until not having gas to release, product being filtered, uses respectively
The hydrochloric acid solution of 0.1M, deionized water wash, deionized water disperses, centrifugation, obtains graphite oxide after lyophilization.
Reference examples 1
A kind of preparation method of water-absorbing resin, comprises the following steps the carboxymethyl 1. adding 0.72 g in 30 mL deionized waters
Cellulose, is uniformly mixing to obtain transparent viscosity solution, under nitrogen protection, solution is heated to 60 DEG C, and keeps nitrogen bubble 30
Minute；2. the N of 0.0045g, N '-methylene-bisacrylamide, ultrasonic disperse are added in the acrylic acid of 7.2g degree of neutralization 80%
30 minutes, obtain homogeneous phase solution；3. 2. step is obtained solution and add in the solution that 1. step obtains, under stirring, nitrogen protection
It is warming up to 70 DEG C, and reacts 3 hours at 70 DEG C, wash, be dried, be dried at 70 DEG C and obtain water-absorbing resin to constant weight.
Embodiment 2
A kind of preparation method of the environmentally friendly High hydrophilous resin of graphene oxide doped, comprises the following steps：1. by 0.04
The graphite oxide of g is added in 25 mL deionized waters, and ultrasonic disperse 35 minutes obtains homodisperse graphene oxide solution；
Then add the carboxymethyl cellulose of 0.7 g in graphene oxide solution, be uniformly mixing to obtain transparent viscosity solution, nitrogen
Under protection, solution is heated to 58 DEG C, and keeps nitrogen bubble 25 minutes；2. add in the acrylic acid of 7g degree of neutralization 40%
The N of 0.004g, N '-methylene-bisacrylamide, ultrasonic disperse 20 minutes, obtain homogeneous phase solution；3. 2. step is obtained solution
Add in the solution that 1. step obtains, be warming up to 68 DEG C under stirring, nitrogen protection, and react 2.5 hours at 68 DEG C, washing,
It is dried at 70 DEG C to constant weight and obtain the environmentally friendly High hydrophilous resin of graphene oxide doped.
Described graphite oxide can buy existing graphite oxide；In the flask of 250 mL, add the analytically pure graphite of 2g
Powder, flask is placed in ice salt bath, adds 50 mL concentrated sulphuric acids so that graphite powder is disperseed, is then slowly added under conditions of stirring
1g sodium nitrate and 7g potassium permanganate, react 2 hours；Reaction flask is removed ice salt bath, puts into and in oil bath, be gradually heated to 80 DEG C
Continuing reaction 6h, stop heating, after being cooled to room temperature, adding 30% hydrogen peroxide until not having gas to release, by product mistake
Filter, uses hydrochloric acid solution, the deionized water wash of 0.1M respectively, and deionized water disperses, centrifugation, obtains aoxidizing stone after lyophilization
Ink.
Embodiment 3
A kind of preparation method of the environmentally friendly High hydrophilous resin of graphene oxide doped, comprises the following steps：1. by 0.05
The graphite oxide of g is added in 35 mL deionized waters, and ultrasonic disperse 45 minutes obtains homodisperse graphene oxide solution；
Then add the carboxymethyl cellulose of 0.75 g in graphene oxide solution, be uniformly mixing to obtain transparent viscosity solution, nitrogen
Under gas shielded, solution is heated to 62 DEG C, and keeps nitrogen bubble 35 minutes；2. add in the acrylic acid of 8g degree of neutralization 90%
The N of 0.005g, N '-methylene-bisacrylamide, ultrasonic disperse 50 minutes, obtain homogeneous phase solution；3. 2. step is obtained solution
Add in the solution that 1. step obtains, be warming up to 72 DEG C under stirring, nitrogen protection, and react 3.5 hours at 72 DEG C, washing,
It is dried at 70 DEG C to constant weight and obtain the environmentally friendly High hydrophilous resin of graphene oxide doped.
Described graphite oxide can buy existing graphite oxide；In the flask of 250 mL, add the analytically pure graphite of 2g
Powder, flask is placed in ice salt bath, adds 50 mL concentrated sulphuric acids so that graphite powder is disperseed, is then slowly added under conditions of stirring
1g sodium nitrate and 7g potassium permanganate, react 2 hours；Reaction flask is removed ice salt bath, puts into and in oil bath, be gradually heated to 80 DEG C
Continuing reaction 6h, stop heating, after being cooled to room temperature, adding 30% hydrogen peroxide until not having gas to release, by product mistake
Filter, uses hydrochloric acid solution, the deionized water wash of 0.1M respectively, and deionized water disperses, centrifugation, obtains aoxidizing stone after lyophilization
Ink.
Interpretation of result
Fig. 1 is the water-absorbent resin surfaces SEM figure of reference examples 1 preparation；Fig. 2 is the water-absorbent resin surfaces SEM of embodiment 1 preparation；By
Fig. 1-2 can be seen that the High hydrophilous resin not having graphene oxide doped, and surface smooths, compacts, and through graphene oxide
The High hydrophilous resin of doping, surface porosity, coarse, with the presence of obvious micropore, the change of this surface texture and form, to mixing
The water suction of miscellaneous tree fat and water holding capacity cause large effect.
The water-absorbing resin water absorbing capacity test result of embodiment 1 and reference examples 1 preparation is as shown in figure 3, can from Fig. 3
Go out, unadulterated resin water absorption rate is 500g/g, and the water-absorbing resin equilibrium water absorption after graphene oxide doped up to
700 g/g about, water absorbing capacity significantly improves.
Fig. 4 is embodiment 1 and the water holding capacity test result at 100 DEG C for the water-absorbing resin of reference examples 1 preparation；Fig. 5 is
The water-absorbing resin of embodiment 1 and reference examples 1 preparation is in the water holding capacity test result under 4000rpm high speed centrifugation；From Fig. 4-
As can be seen that either heating test or centrifugation test in 5, the High hydrophilous resin of graphene oxide doped is compared unadulterated
High hydrophilous resin all shows more excellent water holding capacity.
Although illustrate and describing the present invention with specific embodiment, but it will be appreciated that without departing substantially from the present invention's
Many other changes can be made in the case of spirit and scope and change.It is, therefore, intended that in the following claims
Including all such changes and modifications belonging in the scope of the invention.
Claims (3)
1. a kind of preparation method of the environmentally friendly High hydrophilous resin of graphene oxide doped is it is characterised in that include following walking
Suddenly：1. the graphite oxide of 0.04 ~ 0.05 g is added in 25 ~ 35 mL deionized waters, ultrasonic disperse 35 ~ 45 minutes, obtains all
Even scattered graphene oxide solution；Then add the carboxymethyl cellulose of 0.7 ~ 0.75 g in graphene oxide solution, stir
Mix and uniformly obtain transparent viscosity solution, under nitrogen protection, viscosity solution is heated to 58 ~ 62 DEG C, and keep nitrogen bubble 25 ~
35 minutes；2. the N, N '-methylene bisacrylamide acyl of 0.004 ~ 0.005g are added in the acrylic acid of 7 ~ 8g degree of neutralization 40-90%
Amine, ultrasonic disperse 20 ~ 50 minutes, obtain homogeneous phase solution；3. 2. step is obtained the solution that homogeneous phase solution adds step 1. to obtain
In, it is warming up to 68 ~ 72 DEG C under stirring, nitrogen protection, and reacts 2.5 ~ 3.5 hours at 68 ~ 72 DEG C, wash, be dried, obtain oxygen
The environmentally friendly High hydrophilous resin of graphite alkene doping.
2. the preparation method of the environmentally friendly High hydrophilous resin of graphene oxide doped as claimed in claim 2, its feature exists
In, described step 3. in drying be to be dried to constant weight at 70 DEG C.
3. the preparation method of the environmentally friendly High hydrophilous resin of graphene oxide doped as claimed in claim 1, its feature exists
In the preparation method of described graphite oxide is as follows：In the flask of 250 mL, add the analytically pure graphite powder of 2g, flask is placed in
In ice salt bath, add 50 mL concentrated sulphuric acids so that graphite powder is disperseed, under conditions of stirring, then add 1g sodium nitrate and 7g permanganic acid
Potassium, reacts 2 hours；Reaction flask is removed ice salt bath, puts into and in oil bath, be gradually heated to 80 DEG C of continuation reaction 6h, stop adding
Heat, after being cooled to room temperature, adding 30% hydrogen peroxide until not having gas to release, product being filtered, uses the salt of 0.1M respectively
Acid, deionized water wash, deionized water disperses, centrifugation, obtains graphite oxide after lyophilization.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286553A (en) * | 2017-06-12 | 2017-10-24 | 安徽省颍上县正泰电器有限责任公司 | A kind of preparation method of the plain cross-linked material of water-retaining type graphene nano fiber |
| CN110627956A (en) * | 2019-09-29 | 2019-12-31 | 中国石油大学(华东) | Preparation method of antibacterial super absorbent resin |
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| CN101941694A (en) * | 2010-09-07 | 2011-01-12 | 湘潭大学 | Preparation method of high-dispersivity graphene |
| CN104530293A (en) * | 2014-12-11 | 2015-04-22 | 青岛佰众化工技术有限公司 | Preparation method of polyacrylate-graphene oxide composites |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101941694A (en) * | 2010-09-07 | 2011-01-12 | 湘潭大学 | Preparation method of high-dispersivity graphene |
| CN104530293A (en) * | 2014-12-11 | 2015-04-22 | 青岛佰众化工技术有限公司 | Preparation method of polyacrylate-graphene oxide composites |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286553A (en) * | 2017-06-12 | 2017-10-24 | 安徽省颍上县正泰电器有限责任公司 | A kind of preparation method of the plain cross-linked material of water-retaining type graphene nano fiber |
| CN110627956A (en) * | 2019-09-29 | 2019-12-31 | 中国石油大学(华东) | Preparation method of antibacterial super absorbent resin |
| CN110627956B (en) * | 2019-09-29 | 2022-04-19 | 中国石油大学(华东) | Preparation method of antibacterial super absorbent resin |
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Application publication date: 20170208 |