CN107349912A - A kind of carbon composite gelatin sponge and preparation method thereof - Google Patents
A kind of carbon composite gelatin sponge and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of carbon composite gelatin sponge and preparation method thereof.Its technical scheme is：By solid-to-liquid ratio it is 2.5 ~ 80kg/m by gelatin and deionized water3Mixing, 20 ~ 40min is stirred under the conditions of 30 ~ 80 DEG C, obtains gelatin solution；According to gelatin solution: metal salt: the mass ratio of nano-carbon material is 100:（0.1~5）∶（0~30）, metal salt and nano-carbon material are added into gelatin solution, stirs, obtains mixed liquor.By mixed liquor: the volume ratio of formalin is 100:（0.3~3）, formalin is added into mixed liquor, 0.5 ~ 1h is stirred, obtains hydrogel；The hydrogel is freezed into 6 ~ 10h under the conditions of 40 ~ 2 DEG C, 42 ~ 52h is dried in freeze drier, that is, obtains carbon composite gelatin sponge.The present invention has the characteristics of synthesis technique is simple, cost is low, green, crosslinking time is short and easily controllable, and prepared carbon composite gelatin sponge even aperture distribution, hydrophobic oleophilic oil is good, intensity is high and the excellent adsorption to oil.
Description
Technical field
The invention belongs to gelfoam technical field.More particularly to a kind of carbon composite gelatin sponge and preparation method thereof.
Background technology
With the development of the modern industry, oily pollution event is taken place frequently, and particularly sudden water environment oily pollution event is repeatedly sent out
It is raw.Because oils is difficult to biodegradation in water body, difficulty is removed, thus there is stronger bioconcentration after entering environment,
Potential hidden danger is caused to the mankind and marine organisms.Therefore, it is quick, efficient to go oil pollutant in water removal significant.
Currently used water body oil contaminants sweep-out method has adsorption treatment, chemical method to carry out scattered and settlement treatment, micro-
Biodegradable and combustion in situ etc., these methods have respective limitation, as processing time is long, are also easy to produce secondary pollution etc..
Comparatively speaking, material absorption process has benefited from the absorption property of material itself quickly and efficiently, and can recycle, and does not produce two
Secondary pollution, it is widely used in oily pollution processing.The oil absorption material used earliest is mainly natural with loose and porous structure
Material, such as activated carbon, vermiculite, fluolite, bentonite and cotton fiber, though these material costs are relatively low, adsorbance and water oil
Selectivity is poor.
Polymer oil absorption material absorbability is strong and cost is low, and compared to inorganic material, its oil-water separation is more preferable, can
For petroleum hydrocarbons adsorption treatment, such as polyurethane foam, polypropylene fibre.However, traditional polymer oil suction material
Material there is poor biocompatibility, hydrophobicity is poor the shortcomings of.Gelatin is that a kind of natural biological being made up of several amino acids is high
Molecule, because of its characteristic such as cheap and easy to get, environment-friendly, it is widely used in food, medicine and chemical industry.Gelfoam is by bright
The polymer porous material that xanthan molecule is cross-linked to form, it is a kind of environmentally friendly green not only with strong absorbability but also environmentally friendly
Color sorbing material.But the gelfoam prepared at present there is crosslinking time length, low intensity, poor toughness and to water oil selectivity compared with
The defects of poor, constrain its application in terms of water body oil contaminants removing.Such as：" a kind of Aquatic product fish skin gelatin sponge and its system
Preparation Method "（CN103525097A）Gelfoam need be crosslinked 12h under the conditions of 4 DEG C；" a kind of PEI grafted gelatins sponge
Preparation and its application in heavy metal-polluted water process "（CN105754137A）Gelfoam need in 40 DEG C ~ 70 DEG C conditions
Lower crosslinking more than 20h.
The content of the invention
It is contemplated that overcome prior art defect, and it is an object of the present invention to provide a kind of technique is simple, cost is low, it is green,
The easily controllable and preparation method of the short carbon composite gelatin sponge of crosslinking time；The carbon composite gelatin sponge prepared with this method is dredged
Water lipophile is good, intensity is higher, even aperture distribution and to oil excellent adsorption.
To achieve the above object, the technical solution adopted by the present invention is：
Step 1: by solid-to-liquid ratio it is 2.5 ~ 80kg/m by gelatin and deionized water3Mixing, under the conditions of 30 ~ 80 DEG C stir 20 ~
40min, obtain gelatin solution.
Step 2: according to institute's gelatine solution: metal salt: the mass ratio of nano-carbon material is 100:（0.1~5）∶（0~
30）, metal salt and nano-carbon material are added into institute's gelatine solution, stirs, obtains mixed liquor.
Step 3: press the mixed liquor: the volume ratio of formalin is 100:（0.3~3）, added into the mixed liquor
Formalin, 0.5 ~ 1h is stirred, obtains hydrogel.
Step 4: the hydrogel is freezed into 6 ~ 10h under the conditions of -40 ~ -2 DEG C, 42 are then dried in freeze drier
~ 52h, that is, obtain carbon composite gelatin sponge.
The metal salt be ferric acetate, cobalt acetate, nickel acetate, iron chloride, cobalt chloride, nickel chloride, aluminium chloride, manganese chloride,
One in copper chloride, zinc chloride, ferric nitrate, ferric nitrate, cobalt nitrate, nickel nitrate, aluminum nitrate, manganese nitrate, copper nitrate and zinc nitrate
Kind.
The nano-carbon material is one kind in CNT, graphene, fullerene and carbosphere；The nano-carbon material
Particle diameter be 50 ~ 500nm.
Due to there is following good effect compared with prior art using above-mentioned technical proposal, the present invention：
1st, the metal salt that the present invention uses, metal cation therein can not only pass through interionic with the anion in gelatin group
Active force forms double-spiral structure, and can also promote different double-stranded combinations.Addition metal salt not only shortens solidifying
The glue time, the absorption property of carbon composite gelatin sponge can be also significantly improved simultaneously
2nd, the nano-carbon material that the present invention uses, the intensity and toughness of carbon composite gelatin sponge can be improved, while it is hydrophobic to improve its
Lipophile.
3rd, carbon composite gelatin sponge prepared by the present invention can reclaim the waste oil of absorption, be reused, green,
It has preferable sorption cycle performance simultaneously.
4th, the present invention only needs the raw material being successively mixed to prepare hydrogel in proportion under the conditions of 30 ~ 80 DEG C, and freezing is dry
It is dry that gelfoam is made, there is the advantages of synthesis technique is simple, crosslinking time is short and easily controllable.
5th, raw materials used wide material sources of the present invention, cheap low with production cost, have industrialization prospect.
Therefore, the present invention has the spy that synthesis technique is simple, cost is low, green, crosslinking time is short and easily controllable
Point, prepared carbon composite gelatin sponge even aperture distribution, hydrophobic oleophilic oil is good, intensity is high, to oily excellent adsorption and production
Industry prospect is big.
Brief description of the drawings
Fig. 1 is a kind of SEM figures of carbon composite gelatin sponge of the present invention；
Fig. 2 is absorption schematic diagram of the sponge of carbon composite gelatin shown in Fig. 1 to different waste oil.
Embodiment
The present invention will be further described with reference to the accompanying drawings and detailed description, not to the limit of its protection domain
System.
The particle diameter of nano-carbon material described in present embodiment is 50 ~ 500nm, is repeated no more in embodiment.
Embodiment 1
A kind of carbon composite gelatin sponge and preparation method thereof.Preparation method described in the present embodiment comprises the concrete steps that：
Step 1: by solid-to-liquid ratio it is 2.5 ~ 20kg/m by gelatin and deionized water3Mixing, under the conditions of 30 ~ 60 DEG C stir 20 ~
40min, obtain gelatin solution.
Step 2: according to institute's gelatine solution: metal salt: the mass ratio of nano-carbon material is 100:（0.1~1）∶（10~
20）, metal salt and nano-carbon material are added into institute's gelatine solution, stirs, obtains mixed liquor.
Step 3: press the mixed liquor: the volume ratio of formalin is 100:（0.3~1）, added into the mixed liquor
Formalin, 0.5 ~ 1h is stirred, obtains hydrogel.
Step 4: the hydrogel is freezed into 6 ~ 10h under the conditions of -40 ~ -20 DEG C, then dried in freeze drier
42 ~ 52h, that is, obtain carbon composite gelatin sponge.
This implementation metal salt is ferric acetate.
This implementation nano-carbon material is CNT.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Embodiment 2
A kind of carbon composite gelatin sponge and preparation method thereof.The present embodiment is in addition to metal salt and nano-carbon material, and remaining is the same as implementation
Example 1.
This implementation metal salt is cobalt acetate.
This implementation nano-carbon material is graphene.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Embodiment 3
A kind of carbon composite gelatin sponge and preparation method thereof.The present embodiment is in addition to metal salt and nano-carbon material, and remaining is the same as implementation
Example 1.
The metal salt is nickel acetate.
The nano-carbon material is fullerene.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Embodiment 4
A kind of carbon composite gelatin sponge and preparation method thereof.Preparation method described in the present embodiment comprises the concrete steps that：
Step 1: by solid-to-liquid ratio it is 10 ~ 30kg/m by gelatin and deionized water3Mixing, under the conditions of 30 ~ 60 DEG C stir 20 ~
40min, obtain gelatin solution.
Step 2: according to institute's gelatine solution: metal salt: the mass ratio of nano-carbon material is 100:（1~2）∶（20~30）,
Metal salt and nano-carbon material are added into institute's gelatine solution, stirs, obtains mixed liquor.
Step 3: press the mixed liquor: the volume ratio of formalin is 100:（0.3~1）, added into the mixed liquor
Formalin, 0.5 ~ 1h is stirred, obtains hydrogel.
Step 4: the hydrogel is freezed into 6 ~ 10h under the conditions of -30 ~ -10 DEG C, then dried in freeze drier
42 ~ 52h, that is, obtain carbon composite gelatin sponge.
This implementation metal salt is iron chloride.
This implementation nano-carbon material is carbosphere.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Embodiment 5
A kind of carbon composite gelatin sponge and preparation method thereof.The present embodiment is in addition to metal salt and nano-carbon material, and remaining is the same as implementation
Example 4.
This implementation metal salt is cobalt chloride.
This implementation nano-carbon material is CNT.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Embodiment 6
A kind of carbon composite gelatin sponge and preparation method thereof.The present embodiment is in addition to metal salt and nano-carbon material, and remaining is the same as implementation
Example 4.
This implementation metal salt is nickel chloride.
This implementation nano-carbon material is graphene.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Embodiment 7
A kind of carbon composite gelatin sponge and preparation method thereof.Preparation method described in the present embodiment comprises the concrete steps that：
Step 1: by solid-to-liquid ratio it is 20 ~ 40kg/m by gelatin and deionized water3Mixing, under the conditions of 30 ~ 60 DEG C stir 20 ~
40min, obtain gelatin solution.
Step 2: according to institute's gelatine solution: metal salt: the mass ratio of nano-carbon material is 100:（2~3）∶（20~30）,
Metal salt and nano-carbon material are added into institute's gelatine solution, stirs, obtains mixed liquor.
Step 3: press the mixed liquor: the volume ratio of formalin is 100:（0.3~1）, added into the mixed liquor
Formalin, 0.5 ~ 1h is stirred, obtains hydrogel.
Step 4: the hydrogel is freezed into 6 ~ 10h under the conditions of -20 ~ -2 DEG C, 42 are then dried in freeze drier
~ 52h, that is, obtain carbon composite gelatin sponge.
This implementation metal salt is aluminium chloride.
This implementation nano-carbon material is fullerene.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Embodiment 8
A kind of carbon composite gelatin sponge and preparation method thereof.The present embodiment is in addition to metal salt and nano-carbon material, and remaining is the same as implementation
Example 7.
This implementation metal salt is manganese chloride.
This implementation nano-carbon material is carbosphere.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Embodiment 9
A kind of carbon composite gelatin sponge and preparation method thereof.The present embodiment is in addition to metal salt and nano-carbon material, and remaining is the same as implementation
Example 7.
This implementation metal salt is copper chloride.
This implementation nano-carbon material is CNT.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Embodiment 10
A kind of carbon composite gelatin sponge and preparation method thereof.Preparation method described in the present embodiment comprises the concrete steps that：
Step 1: by solid-to-liquid ratio it is 30 ~ 50kg/m by gelatin and deionized water3Mixing, under the conditions of 40 ~ 70 DEG C stir 20 ~
40min, obtain gelatin solution.
Step 2: according to institute's gelatine solution: metal salt: the mass ratio of nano-carbon material is 100:（3~4）∶（10~20）,
Metal salt and nano-carbon material are added into institute's gelatine solution, stirs, obtains mixed liquor.
Step 3: press the mixed liquor: the volume ratio of formalin is 100:（1~2）, first is added into the mixed liquor
Aldehyde solution, 0.5 ~ 1h is stirred, obtains hydrogel.
Step 4: the hydrogel is freezed into 6 ~ 10h under the conditions of -40 ~ -20 DEG C, then dried in freeze drier
42 ~ 52h, that is, obtain carbon composite gelatin sponge.
The metal salt is zinc chloride.
The nano-carbon material is graphene.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Embodiment 11
A kind of carbon composite gelatin sponge and preparation method thereof.The present embodiment is in addition to metal salt and nano-carbon material, and remaining is the same as implementation
Example 11.
This implementation metal salt is ferric nitrate.
This implementation nano-carbon material is fullerene.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Embodiment 12
A kind of carbon composite gelatin sponge and preparation method thereof.The present embodiment is in addition to metal salt and nano-carbon material, and remaining is the same as implementation
Example 11.
This implementation metal salt is cobalt nitrate.
This implementation nano-carbon material is carbosphere.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Embodiment 13
A kind of carbon composite gelatin sponge and preparation method thereof.Preparation method described in the present embodiment comprises the concrete steps that：
Step 1: by solid-to-liquid ratio it is 40 ~ 60kg/m by gelatin and deionized water3Mixing, under the conditions of 40 ~ 70 DEG C stir 20 ~
40min, obtain gelatin solution.
Step 2: according to institute's gelatine solution: the mass ratio of metal salt is 100:（4~5）, add into institute's gelatine solution
Enter metal salt, stir, obtain mixed liquor.
Step 3: press the mixed liquor: the volume ratio of formalin is 100:（2~3）, first is added into the mixed liquor
Aldehyde solution, 0.5 ~ 1h is stirred, obtains hydrogel.
Step 4: the hydrogel is freezed into 6 ~ 10h under the conditions of -30 ~ -10 DEG C, then dried in freeze drier
42 ~ 52h, that is, obtain carbon composite gelatin sponge.
This implementation metal salt is nickel nitrate.
This implementation nano-carbon material is CNT.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment.
Embodiment 14
A kind of carbon composite gelatin sponge and preparation method thereof.Preparation method described in the present embodiment comprises the concrete steps that：
Step 1: by solid-to-liquid ratio it is 50 ~ 70kg/m by gelatin and deionized water3Mixing, under the conditions of 50 ~ 80 DEG C stir 20 ~
40min, obtain gelatin solution.
Step 2: according to institute's gelatine solution: metal salt: the mass ratio of nano-carbon material is 100:（3.5~4.5）∶
（0.01~1.00）, metal salt and nano-carbon material are added into institute's gelatine solution, stirs, obtains mixed liquor.
Step 3: press the mixed liquor: the volume ratio of formalin is 100:（2~3）, first is added into the mixed liquor
Aldehyde solution, 0.5 ~ 1h is stirred, obtains hydrogel.
Step 4: the hydrogel is freezed into 6 ~ 10h under the conditions of -20 ~ -2 DEG C, 42 are then dried in freeze drier
~ 52h, that is, obtain carbon composite gelatin sponge.
This implementation metal salt is aluminum nitrate.
This implementation nano-carbon material is graphene.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Embodiment 15
A kind of carbon composite gelatin sponge and preparation method thereof.The present embodiment is in addition to metal salt and nano-carbon material, and remaining is the same as implementation
Example 14.
This implementation metal salt is manganese nitrate.
This implementation nano-carbon material is fullerene.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to height
With the excellent adsorption to oil.
Embodiment 16
A kind of carbon composite gelatin sponge and preparation method thereof.Preparation method described in the present embodiment comprises the concrete steps that：
Step 1: by solid-to-liquid ratio it is 60 ~ 80kg/m by gelatin and deionized water3Mixing, under the conditions of 50 ~ 80 DEG C stir 20 ~
40min, obtain gelatin solution.
Step 2: according to institute's gelatine solution: metal salt: the mass ratio of nano-carbon material is 100:（2.5~3.5）∶（1~
10）, metal salt and nano-carbon material are added into institute's gelatine solution, stirs, obtains mixed liquor.
Step 3: press the mixed liquor: the volume ratio of formalin is 100:（1~2）, first is added into the mixed liquor
Aldehyde solution, 0.5 ~ 1h is stirred, obtains hydrogel.
Step 4: the hydrogel is freezed into 6 ~ 10h under the conditions of -40 ~ -20 DEG C, then dried in freeze drier
42 ~ 52h, that is, obtain carbon composite gelatin sponge.
This implementation metal salt is zinc nitrate.
This implementation nano-carbon material is carbosphere.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Embodiment 17
A kind of carbon composite gelatin sponge and preparation method thereof.The present embodiment is in addition to metal salt and nano-carbon material, and remaining is the same as implementation
Example 16.
This implementation metal salt is copper nitrate.
This implementation nano-carbon material is CNT.
Carbon composite gelatin sponge even aperture distribution prepared by the present embodiment, hydrophobic oleophilic oil is good, intensity is high and to oil
Excellent adsorption.
Present embodiment has following good effect compared with prior art：
1st, the metal salt that present embodiment uses, metal cation therein can not only lead to the anion in gelatin group
Cross ion intermolecular forces and form double-spiral structure, and different double-stranded combinations can also be promoted.Add metal salt not only
Gel time is shortened, can also improve the absorption property of carbon composite gelatin sponge simultaneously
2nd, the nano-carbon material that present embodiment uses, can improve the intensity and toughness of carbon composite gelatin sponge, carry simultaneously
Its high hydrophobic oleophilic oil.
3rd, Fig. 1 is a kind of SEM figures of carbon composite gelatin sponge prepared by embodiment 4 in present embodiment, and Fig. 2 is figure
Absorption schematic diagram of the sponge of carbon composite gelatin shown in 1 to different waste oil.It can be seen that from Fig. 1 and Fig. 2：Prepared carbon is compound bright
Gelatin sponge even aperture distribution, absorption waste oil performance are good；It can also be reused simultaneously, it is green, have and preferably inhale
Attached cycle performance.
4th, present embodiment only needs the raw material being successively mixed to prepare water-setting in proportion under the conditions of 30 ~ 80 DEG C
Gelfoam is made in glue, freeze-drying, has the advantages of synthesis technique is simple, crosslinking time is short and easily controllable.
5th, raw materials used wide material sources of present embodiment, cheap low with production cost, have industrialization prospect.
Therefore, present embodiment has that synthesis technique is simple, cost is low, green, crosslinking time is short and is easy to
The characteristics of control, prepared carbon composite gelatin sponge even aperture distribution, hydrophobic oleophilic oil is good, intensity is high and the absorption to oil
Property good and industrialization prospect it is big.
Claims (4)
1. a kind of preparation method of carbon composite gelatin sponge, it is characterised in that be the step of the preparation method：
Step 1: by solid-to-liquid ratio it is 2.5 ~ 80kg/m by gelatin and deionized water3Mixing, under the conditions of 30 ~ 80 DEG C stir 20 ~
40min, obtain gelatin solution；
Step 2: according to institute's gelatine solution: metal salt: the mass ratio of nano-carbon material is 100:（0.1~5）∶（0~30）, to
Metal salt and nano-carbon material are added in institute's gelatine solution, stirs, obtains mixed liquor；
Step 3: press the mixed liquor: the volume ratio of formalin is 100:（0.3~3）, formaldehyde is added into the mixed liquor
Solution, 0.5 ~ 1h is stirred, obtains hydrogel；
Step 4: the hydrogel is freezed into 6 ~ 10h under the conditions of -40 ~ -2 DEG C, then dry 42 in freeze drier ~
52h, that is, obtain carbon composite gelatin sponge.
2. the preparation method of carbon composite gelatin sponge according to claim 1, it is characterised in that the metal salt is acetic acid
Iron, cobalt acetate, nickel acetate, iron chloride, cobalt chloride, nickel chloride, aluminium chloride, manganese chloride, copper chloride, zinc chloride, ferric nitrate, nitric acid
One kind in iron, cobalt nitrate, nickel nitrate, aluminum nitrate, manganese nitrate, copper nitrate and zinc nitrate.
3. the preparation method of carbon composite gelatin sponge according to claim 1, it is characterised in that the nano-carbon material is
One kind in CNT, graphene, fullerene and carbosphere；The particle diameter of the nano-carbon material is 50 ~ 500nm.
4. a kind of carbon composite gelatin sponge, it is characterised in that the carbon composite gelatin sponge is appointed according in claim 1 ~ 3
Carbon composite gelatin sponge prepared by the preparation method of one carbon composite gelatin sponge.
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| CN108114311A (en) * | 2017-12-20 | 2018-06-05 | 江苏省健尔康医用敷料有限公司 | The preparation method of iodoform gelatin sponge |
| CN109078616A (en) * | 2018-09-14 | 2018-12-25 | 河南科技大学 | A kind of tannic acid modified graphene/gelatin porous composite material and preparation method, application |
| CN109920918A (en) * | 2019-03-25 | 2019-06-21 | 电子科技大学 | Perovskite photodetector and preparation method thereof based on composite electron transport layer |
| CN110040713A (en) * | 2019-04-25 | 2019-07-23 | 太原理工大学 | A kind of preparation method of carbon aerogels |
| CN110511402A (en) * | 2019-09-12 | 2019-11-29 | 东华大学 | A kind of cobalt cross-linked hydrogel and preparation method thereof with high cross-link intensity |
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