CN107552020A - The method of the polyvinyl alcohol of synthesizing blender carbon nanomaterial/sodium alginate gel ball adsorbent - Google Patents
The method of the polyvinyl alcohol of synthesizing blender carbon nanomaterial/sodium alginate gel ball adsorbent Download PDFInfo
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- CN107552020A CN107552020A CN201710841121.2A CN201710841121A CN107552020A CN 107552020 A CN107552020 A CN 107552020A CN 201710841121 A CN201710841121 A CN 201710841121A CN 107552020 A CN107552020 A CN 107552020A
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- polyvinyl alcohol
- carbon nanomaterial
- sodium alginate
- gel ball
- alginate gel
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Abstract
The invention belongs to the field of chemical synthesis, it is related to a kind of method of polyvinyl alcohol of synthesizing blender carbon nanomaterial/sodium alginate gel ball adsorbent, including carbon nanomaterial powder is added to the water into obtained carbon nanomaterial aqueous dispersion, sodium alginate and polyvinyl alcohol are added afterwards mixing water dispersion is made in aqueous dispersion, and with peristaltic pump the polyvinyl alcohol/sodium alginate gel ball adsorbent for adulterating carbon nanomaterial is made in its all instills dropwise in boric acid calcium chloride mixed solution.Raw material of the present invention is easy to get, and cost is relatively low, and biocompatibility is strong；Production method is simple and easy, can continuous operation, suitable for large-scale production；Product advantages of good adsorption effect, it is easy to collect recovery, it is environmentally safe.
Description
Technical field
The invention belongs to environmentally conscious materialses to synthesize field, and in particular to a kind of polyvinyl alcohol/sea of synthesizing blender carbon nanomaterial
The method of sodium alginate gel ball adsorbent.
Background technology
Water is Source of life, but with present industrial high speed development, the situation of water environment pollution is increasingly serious, therefore
Develop that efficient water technology is particularly important, among conventional water technology, adsorbent because its low cost, high efficiency,
Easily operated, selectively strong etc. advantage has obtained increasing concern.But conventional sorbent material such as activated carbon etc. pair
It is relatively low in pollutant adsorption efficiency, and it is difficult to separation and recovery regeneration.Therefore, efficient sorbent material is developed for inhaling
The development of attached technology is particularly critical.
Sodium alginate is a kind of linear polysaccharide extracted from natural seaweed, by beta-D-mannuronic acid and α-L- gulose
Aldehydic acid connection composition, it is nontoxic, there is good biocompatibility, and sodium alginate is easily formed gel, this is for absorption
The separation and recovery of agent has very big advantage.Polyvinyl alcohol is a kind of colourless nontoxic, biodegradable high molecular polymer,
Both of which can form gel ball by method physically or chemically, but sodium alginate gel ball is broken, bad mechanical property,
Polyvinyl alcohol then easy adhesion, and both absorption properties are weaker.
Carbon nanomaterial refers at least one-dimensional structural type carbon material less than 100nm of dispersed phase yardstick.It is main to include richness
Strangle alkene, CNT, graphene quantum dot, graphene, mesoporous nano carbon etc., carbon nanomaterial have stability is good, intensity is high,
The advantages such as specific surface area height, and carbon nanomaterial is easy to carry out modification oxidation, and it is for water pollutant (such as antibiotic, dye
Material, heavy metal) there is good absorption property, but harm of the bio-toxicity that has of carbon nanomaterial to environment is very big, by
It is difficult to reclaim in carbon nanomaterial more in powdered, during applied to adsorbent.
The content of the invention
A kind of it is an object of the present invention to overcome the deficiencies in the prior art, there is provided poly- second of synthesizing blender carbon nanomaterial
The method of enol/sodium alginate gel ball adsorbent.
In the present invention, carbon nanomaterial is dispersed in the mixing of sodium alginate and polyvinyl alcohol using the method for ultrasound
In aqueous dispersion, next instill in chemical cross-linking agent and form complex microsphere；It is simple and quick to be efficiently synthesized doped carbon nanometer
The polyvinyl alcohol of material/sodium alginate gel ball adsorbent.Carbon nanomaterial is entrained in gel ball system by the present invention, can be with
It is strong to improve absorption effect mechanical performance, and is advantageous to separate and recover.
To realize object above, the invention provides following technical scheme：
A kind of method for the polyvinyl alcohol/sodium alginate gel ball adsorbent for adulterating carbon nanomaterial, comprises the following steps：
(1) the carbon nanomaterial powder of certain mass is added in deionized water, after stirring, is placed in ultrasonic instrument and carries out
Ultrasonic disperse, carbon nanomaterial aqueous dispersion is made；
(2) appropriate polyvinyl alcohol is added in a small amount of deionized water, is placed in being heated in hot bath, interval is certain
Time is stirred with glass bar, is taken out after polyvinyl alcohol is completely dissolved, and is stood and is extremely recovered to normal temperature；
(3) polyvinyl alcohol dissolved in appropriate sodium alginate powder and step (2) is added to step (1) preparation
In carbon nanomaterial aqueous dispersion, mixed dispersion is obtained, is made by the way of mechanical agitation or magnetic agitation described mixed
Dispersion is closed to stir；
(4) appropriate boric acid and calcium chloride are dissolved in water, and adjusts pH to neutrality, prepare boric acid-calcium chloride mixing
Solution；
(5) mixed dispersion obtained by step (3) is added dropwise to boric acid-calcium chloride mixed solution using peristaltic pump
In, gel ball is formed immediately, and the gel ball is continued to be placed in boric acid-calcium chloride mixed solution of step (4) preparation to standing 4
Hour, obtain polyvinyl alcohol/sodium alginate gel ball adsorbent of doping carbon nanomaterial.
Further, the carbon nanomaterial be graphene oxide, oxide/carbon nanometer tube, one kind in graphene quantum dot or
It is a variety of.
In the present invention, the addition of used carbon nanomaterial can be depending on the species of carbon nanomaterial.With reference to
Standard is:With the increase of carbon nanomaterial addition, its mechanical performance is fallen after rising, and its absorption property is continuously increased.With oxygen
Exemplified by graphite alkene, when the mass ratio of graphene oxide and sodium alginate is 1:5, the mechanical performance and adsorption effect of its balling-up are equal
Preferably.
Further, the carbon nanomaterial is graphene oxide, and the addition quality of the graphene oxide is no more than marine alga
0.5 times of sour sodium addition quality.
Further, the addition quality of the graphene oxide is that sodium alginate adds 0.5 times of quality.
In the present invention, the solubility and ratio of used polyvinyl alcohol and sodium alginate are also adjustable.Normative reference is：
When the content increase of polyvinyl alcohol, the caking property increase of gel ball, but balling-up is easily trailed；When the content of sodium alginate increases
Added-time, balling-up effect is good, but gel ball matter is crisp；By taking the polyvinyl alcohol/sodium alginate gel ball for adulterating graphene oxide as an example,
When the mass ratio of polyvinyl alcohol and sodium alginate is 2：When 5, when total concentration is 4%, the mechanical performance and adsorption effect of its balling-up
It is preferable.
Further, the addition quality of the polyvinyl alcohol is that sodium alginate adds 0.4 times of quality.
Further, the temperature of the polyvinyl alcohol hot bath in step (2) is 50 DEG C -90 DEG C.
Further, the concentration of the boric acid in step (4) was 3% -5% (in mass), the concentration of calcium chloride for 1% -
5% (in mass).
Further, the flow of peristaltic pump is 20-50mL/min in step (5).
The beneficial effects of the present invention are：
1. the present invention forms gel using polyvinyl alcohol and sodium alginate, both possesses preferable biocompatibility, sea
Mosanom has excellent gel-forming property, and polyvinyl alcohol then improves the mechanical performance of gel, for adsorbent efficiently separate and
Recovery provides facility.
2. for this method using calcium chloride and boric acid as crosslinking agent, calcium chloride makes sodium alginate be chemically crosslinked to form gel net
Network, boric acid make polyvinyl alcohol be chemically crosslinked to form gel network, are chemically crosslinked Stability Analysis of Structures, and dual network mutually runs through, and makes gel
Mechanical performance lifting.
3. this method using carbon nanomaterial as graphene oxide, oxide/carbon nanometer tube, graphene quantum dot or it is several
Mixture etc., different materials have stronger adsorption effect for pollutants such as antibiotic, dyestuff, heavy metals.
4. present invention process is simple and easy, the stable plural gel ball of size homogeneous structural, product are formed using drip
Filler etc. is can be easily made, is easy to large-scale application；Equipment is simple, can be with continuous operation, suitable for large-scale production.
Brief description of the drawings
The outward appearance shape of polyvinyl alcohol/sodium alginate gel ball adsorbent of Fig. 1 doping graphene oxides provided by the invention
Looks.
Embodiment
The following examples are the further explanations to the present invention, rather than limit the scope of the present invention.
Embodiment 1
(1) 200mg graphite oxide powder is placed in 100mL deionized waters, after stirring, solution is placed in ultrasound
Ultrasonic 3h in instrument, it is graphene oxide aqueous dispersion to peel off graphite oxide；
(2) 1g polyvinylalcohol solids are dissolved in the 50 DEG C of hot baths of 10mL deionized waters, interval 10min is entered with glass bar
Row stirring, takes out after polyvinyl alcohol is completely dissolved, and stands to recovery normal temperature；
(3) polyvinyl alcohol that step (2) has dissolved is added into 100mL mixing carbon nanomaterials together with 2.0g sodium alginates
In dispersion, for mechanical agitation to being mixed thoroughly, placement 2h makes the bubble collapse in mixed solution；
(4) boric acid and calcium chloride are dissolved in water, and adjusts pH to neutrality, prepare the mixing of the calcium chloride of 3% boric acid -5%
Solution；
(5) mixed solution is instilled in boric acid-calcium chloride mixed solution dropwise with peristaltic pump and forms microballoon, stand solidification
4h, polyvinyl alcohol/sodium alginate gel ball adsorbent of doping graphene oxide is made.
Embodiment 2
(1) multi-walled carbon nanotube of 500mg graphite oxide and 500mg is placed in 100mL distilled water, stirred
Afterwards, solution is placed in ultrasonic 5h in ultrasonic instrument, prepares mixing carbon nanomaterial dispersion；
(2) 0.5g polyvinylalcohol solids are dissolved in 70 DEG C of hot baths in 10mL deionized waters, is spaced 10min glass
Rod is stirred, and is taken out after polyvinyl alcohol is completely dissolved, and is stood to recovery normal temperature；
(3) polyvinyl alcohol that step (2) has dissolved is added into 100mL mixing carbon nanomaterial point together with 2g sodium alginates
In granular media system, for mechanical agitation to being mixed thoroughly, placement 2h makes the bubble collapse in mixed solution；
(4) boric acid and calcium chloride are dissolved in water, and adjusts pH to neutrality, prepare the mixing of the calcium chloride of 5% boric acid -1%
Solution；
(5) mixed solution is instilled dropwise with peristaltic pump in the mixed solution of boric acid-calcium chloride mixed solution and forms microballoon,
Solidification 4h is stood, polyvinyl alcohol/sodium alginate gel ball adsorbent of doping graphene oxide and CNT is made.
Embodiment 3
(1) graphene quantum dot of 200mg graphite oxide and 100mg is placed in 100mL distilled water, stirred
Afterwards, solution is placed in ultrasonic 5h in ultrasonic instrument, prepares mixing carbon nanomaterial dispersion；
(2) 2g polyvinylalcohol solids are dissolved in 70 DEG C of hot baths in 10mL deionized waters, is spaced 10min glass bars
It is stirred, is taken out after polyvinyl alcohol is completely dissolved, is stood to recovery normal temperature；
(3) polyvinyl alcohol that step (2) has dissolved is added into 100mL mixing carbon nanomaterial point together with 5g sodium alginates
In granular media system, for mechanical agitation to being mixed thoroughly, placement 2h makes the bubble collapse in mixed solution.
(4) boric acid and calcium chloride are dissolved in water, and adjusts pH to neutrality, prepare the mixing of the calcium chloride of 3% boric acid -5%
Solution.
(5) mixed solution is instilled dropwise with peristaltic pump in the mixed solution of boric acid-calcium chloride mixed solution and forms microballoon,
Solidification 4h is stood, polyvinyl alcohol/sodium alginate gel ball adsorbent of doping graphene oxide and CNT is made.
Embodiment 4
(1) 200mg graphite oxide is placed in 100mL distilled water, after stirring, solution is placed in ultrasonic instrument
Ultrasonic 3h, it is graphene oxide aqueous dispersion to peel off graphite oxide；
(2) 2g polyvinylalcohol solids are dissolved in 70 DEG C of hot baths in 10mL deionized waters, is spaced 10min glass bars
It is stirred, is taken out after polyvinyl alcohol is completely dissolved, is stood to recovery normal temperature；
(3) polyvinyl alcohol that step (2) has dissolved is added into 100mL mixing carbon nanomaterial point together with 5g sodium alginates
In granular media system, for mechanical agitation to being mixed thoroughly, placement 2h makes the bubble collapse in mixed solution.
(4) boric acid and calcium chloride are dissolved in water, and adjusts pH to neutrality, prepare the mixing of the calcium chloride of 4% boric acid -3%
Solution.
(5) mixed solution is instilled dropwise with peristaltic pump in the mixed solution of boric acid-calcium chloride mixed solution and forms microballoon,
Solidification 4h is stood, polyvinyl alcohol/sodium alginate gel ball adsorbent of doping graphene oxide and CNT is made.
In the present invention, using sodium alginate and polyvinyl alcohol processing machinery plural gel ball of good performance, and will absorption
The carbon nanomaterial of function admirable is entrained in plural gel ball, can both ensure the good absorption property of adsorbent, while again
It is easily isolated and recycled, avoids the secondary pollution to environment；It is green and the preparation technology of the present invention is simple, it is easy to expand
Big production, has preferable commercial application prospect.
Foregoing description is only the description to present pre-ferred embodiments, is not any restriction to the scope of the invention.Appoint
Any change or modification what those skilled in the art makes according to the technology contents of the disclosure above should regard
For equivalent effective embodiment, the scope that technical solution of the present invention is protected is belonged to.
Claims (7)
- A kind of 1. method of polyvinyl alcohol of synthesizing blender carbon nanomaterial/sodium alginate gel ball adsorbent, it is characterised in that Comprise the following steps：(1) the carbon nanomaterial powder of certain mass is added in deionized water, after stirring, is placed in ultrasonic instrument and carries out ultrasound It is scattered, carbon nanomaterial aqueous dispersion is made；(2) appropriate polyvinyl alcohol is added in a small amount of deionized water, is placed in being heated in hot bath, separated in time It is stirred with glass bar, is taken out after polyvinyl alcohol is completely dissolved, is stood and extremely recover to normal temperature；(3) carbon that the polyvinyl alcohol dissolved in appropriate sodium alginate powder and step (2) is added to step (1) preparation is received In rice material aqueous dispersion, mixed dispersion is obtained, the mixing point is made by the way of mechanical agitation or magnetic agitation Granular media system stirs；(4) appropriate boric acid and calcium chloride are dissolved in water, and adjusts pH to neutrality, prepare boric acid-calcium chloride mixed solution；(5) mixed dispersion obtained by step (3) is added dropwise in boric acid-calcium chloride mixed solution using peristaltic pump, Immediately gel ball is formed, it is small to continue to be placed in standing 4 in boric acid-calcium chloride mixed solution of step (4) preparation by the gel ball When, obtain polyvinyl alcohol/sodium alginate gel ball adsorbent of doping carbon nanomaterial.
- 2. the polyvinyl alcohol of synthesizing blender carbon nanomaterial according to claim 1/sodium alginate gel ball adsorbent Method, it is characterised in that：The carbon nanomaterial is one kind in graphene oxide, oxide/carbon nanometer tube, graphene quantum dot It is or a variety of.
- 3. the polyvinyl alcohol of synthesizing blender carbon nanomaterial according to claim 2/sodium alginate gel ball adsorbent Method, it is characterised in that：The carbon nanomaterial is graphene oxide, and the addition quality of the graphene oxide is no more than marine alga 0.5 times of sour sodium addition quality.
- 4. the polyvinyl alcohol of synthesizing blender carbon nanomaterial according to claim 3/sodium alginate gel ball adsorbent Method, it is characterised in that：The addition quality of the graphene oxide is 0.5 times that sodium alginate adds quality.
- 5. the polyvinyl alcohol of synthesizing blender carbon nanomaterial according to claim 3/sodium alginate gel ball adsorbent Method, it is characterised in that：The addition quality of the polyvinyl alcohol is 0.4 times that sodium alginate adds quality.
- 6. the polyvinyl alcohol of synthesizing blender carbon nanomaterial according to claim 1/sodium alginate gel ball adsorbent Method, it is characterised in that：The temperature of polyvinyl alcohol hot bath in step (2) is 50 DEG C -90 DEG C.
- 7. the polyvinyl alcohol of synthesizing blender carbon nanomaterial according to claim 1/sodium alginate gel ball adsorbent Method, it is characterised in that：The concentration of boric acid in step (4) was 3% -5% (in mass), the concentration of calcium chloride for 1% - 5% (in mass).
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| CN109126747A (en) * | 2018-08-30 | 2019-01-04 | 上海应用技术大学 | A kind of preparation method of high resiliency GO-SA-PVA plural gel adsorbent material |
| CN109277080A (en) * | 2018-09-21 | 2019-01-29 | 曲阜师范大学 | It is a kind of to include graphene oxide quantum dot/magnetism chitosan oligosaccharide plural gel ball and its preparation method and application |
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| CN110280192B (en) * | 2019-07-10 | 2022-05-20 | 南京理工大学 | Preparation method of carbon nano tube-polyvinyl alcohol gel microspheres |
| CN110496607B (en) * | 2019-07-31 | 2020-10-27 | 西安交通大学 | Preparation method of phosphorus removal adsorbent PVA (polyvinyl alcohol) immobilized powder calcium silicate CSH (calcium silicate chloride) gel beads |
| CN110496607A (en) * | 2019-07-31 | 2019-11-26 | 西安交通大学 | A kind of preparation method of the immobilized powders calcium silicate CSH gel beads of dephosphorization adsorbent PVA |
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Application publication date: 20180109 |