CN108744606A - The preparation method of graphene sponge for water-oil separating - Google Patents
The preparation method of graphene sponge for water-oil separating Download PDFInfo
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- CN108744606A CN108744606A CN201810767983.XA CN201810767983A CN108744606A CN 108744606 A CN108744606 A CN 108744606A CN 201810767983 A CN201810767983 A CN 201810767983A CN 108744606 A CN108744606 A CN 108744606A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28042—Shaped bodies; Monolithic structures
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Abstract
The present invention relates to a kind of preparation methods of the graphene sponge for water-oil separating, sponge is immersed successively in chitosan and graphene oxide solution, obtain chitosan, graphene oxide cladding sponge material, then it is reducing agent leniently redox graphene under hydrothermal conditions to utilize sodium borohydride, it is then immersed in trishydroxymethylaminomethane hexane solution and obtains graphene sponge material, there is excellent oil absorbency, oil-water separation is good, and sponge high mechanical strength.
Description
Technical field
The invention belongs to water treatment fields, and in particular to a kind of preparation method of graphene sponge for water-oil separating.
Background technology
Oil absorption material generally can be divided into traditional oil absorption material and high oil-absorbent material, and the oil absorption material used in China is main at present
It is traditional oil absorption material, such as maize straw, non-woven fleece, bombax cotton, vermiculite, expanded graphite, zeolite etc..However tradition is inhaled
Light wood material relies primarily on physisorption and oil is adsorbed in material surface or internal capillaries, and oil absorbing effect is simultaneously paid no attention to
Think, shows as：1, the little oil suction multiplying power of oil absorption is smaller；2, oil-water selectivity is not high, often also absorbs water while oil suction；3, it inhales
Oil keeping is poor after oil, and slightly pressure will oil leak again.This undoubtedly limits its application in oil mixing with water system.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of the graphene sponge for water-oil separating.
The technical solution adopted by the present invention to solve the technical problems is：The preparation of graphene sponge for water-oil separating
Method, steps are as follows：
1）It takes chitosan to be dissolved in the acetic acid solution that mass concentration is 2%, it is molten to be configured to the chitosan acetic acid that mass concentration is 3-5%
Liquid；
2）Sponge ethyl alcohol and deionized water are washed three times, it is dry to constant weight, it is then dipped in chitosan acetic acid solution, fully
Drying is taken out after being impregnated with；
3）It takes graphene oxide to be added in deionized water and is ultrasonically treated 2-3h, graphene oxide water solution is obtained, by step 2）Middle baking
Dry sponge is immersed in graphene oxide water solution, and drying is taken out after full penetration；
4）By step 3）The sponge of middle drying is immersed in sodium borohydride solution, is restored under water bath condition, takes out sea after reaction
Silk floss drying；
5）It takes trishydroxymethylaminomethane to be added drop-wise in n-hexane, is configured to the trishydroxymethylaminomethane that volume fraction is 1-2%
Hexane solution, by step 4）The sponge of middle drying is immersed in trishydroxymethylaminomethane hexane solution, and it is small to be sufficiently impregnated 2-3
When, drying is taken out to get the graphene sponge for water-oil separating.
Specifically, the step 1）The weight average molecular weight of middle chitosan is 30-50 ten thousand.
Specifically, the sponge is melamine sponge or polyurethane sponge.
Specifically, the step 3）The mass concentration of middle graphene oxide water solution is 0.5-5%.
Specifically, the step 4）A concentration of 1-2mol/L of middle sodium borohydride solution, bath temperature are 60-90 DEG C.
Specifically, the step 2）Step 5）Middle drying temperature is 70-80 DEG C.
The invention has the advantages that：The present invention immerses sponge in chitosan and graphene oxide solution successively,
Obtain chitosan, graphene oxide cladding sponge material, then utilize sodium borohydride be reducing agent under hydrothermal conditions leniently
Redox graphene is then immersed in trishydroxymethylaminomethane hexane solution and obtains graphene sponge material, has excellent
Oil absorbency, oil-water separation is good, and sponge high mechanical strength.
Specific implementation mode
The following is specific embodiments of the present invention, is described further to technical scheme of the present invention, but the present invention
Protection domain is not limited to these examples.It is every to be included in the present invention without departing substantially from the change of present inventive concept or equivalent substitute
Protection domain within.
Embodiment 1
The preparation method of graphene sponge for water-oil separating, steps are as follows：
1）The chitosan for taking weight average molecular weight to be 400,000 is dissolved in the acetic acid solution that mass concentration is 2%, is configured to mass concentration and is
4% chitosan acetic acid solution；
2）Melamine sponge ethyl alcohol and deionized water are washed three times, it is dry to be then dipped in chitosan acetic acid solution to constant weight,
Drying is taken out after full penetration；
3）It takes graphene oxide to be added in deionized water and is ultrasonically treated 2h, obtain the graphene oxide water solution that mass concentration is 2%,
By step 2）The sponge of middle drying is immersed in graphene oxide water solution, and drying is taken out after full penetration；
4）By step 3）The sponge of middle drying is immersed in the sodium borohydride solution of a concentration of 2mol/L, under 70 DEG C of water bath conditions also
Original takes out sponge drying after reaction；
5）It takes trishydroxymethylaminomethane to be added drop-wise in n-hexane, is being configured to the trishydroxymethylaminomethane that volume fraction is 1% just
Hexane solution, by step 4）The sponge of middle drying is immersed in trishydroxymethylaminomethane hexane solution, is sufficiently impregnated 3 hours,
Drying is taken out to get the graphene sponge for water-oil separating.
Step 2）Step 5）Middle drying temperature is 70 DEG C.
Embodiment 2
The preparation method of graphene sponge for water-oil separating, steps are as follows：
1）The chitosan for taking weight average molecular weight to be 300,000 is dissolved in the acetic acid solution that mass concentration is 2%, is configured to mass concentration and is
3% chitosan acetic acid solution；
2）Polyurethane sponge ethyl alcohol and deionized water are washed three times, it is dry to constant weight, then it is dipped in chitosan acetic acid solution
In, drying is taken out after full penetration；
3）It takes graphene oxide to be added in deionized water and is ultrasonically treated 3h, obtain the graphene oxide water solution that mass concentration is 3%,
By step 2）The sponge of middle drying is immersed in graphene oxide water solution, and drying is taken out after full penetration；
4）By step 3）The sponge of middle drying is immersed in the sodium borohydride solution of a concentration of 1mol/L, under 80 DEG C of water bath conditions also
Original takes out sponge drying after reaction；
5）It takes trishydroxymethylaminomethane to be added drop-wise in n-hexane, is being configured to the trishydroxymethylaminomethane that volume fraction is 2% just
Hexane solution, by step 4）The sponge of middle drying is immersed in trishydroxymethylaminomethane hexane solution, is sufficiently impregnated 2 hours,
Drying is taken out to get the graphene sponge for water-oil separating.
Step 2）Step 5）Middle drying temperature is 75 DEG C.
Embodiment 3
The preparation method of graphene sponge for water-oil separating, steps are as follows：
1）The chitosan for taking weight average molecular weight to be 500,000 is dissolved in the acetic acid solution that mass concentration is 2%, is configured to mass concentration and is
5% chitosan acetic acid solution；
2）Polyurethane sponge ethyl alcohol and deionized water are washed three times, it is dry to constant weight, then it is dipped in chitosan acetic acid solution
In, drying is taken out after full penetration；
3）It takes graphene oxide to be added in deionized water and is ultrasonically treated 2h, obtain the graphene oxide water solution that mass concentration is 5%,
By step 2）The sponge of middle drying is immersed in graphene oxide water solution, and drying is taken out after full penetration；
4）By step 3）The sponge of middle drying is immersed in the sodium borohydride solution of a concentration of 2mol/L, under 90 DEG C of water bath conditions also
Original takes out sponge drying after reaction；
5）It takes trishydroxymethylaminomethane to be added drop-wise in n-hexane, is being configured to the trishydroxymethylaminomethane that volume fraction is 1% just
Hexane solution, by step 4）The sponge of middle drying is immersed in trishydroxymethylaminomethane hexane solution, is sufficiently impregnated 2 hours,
Drying is taken out to get the graphene sponge for water-oil separating.
Step 2）Step 5）Middle drying temperature is 80 DEG C.
Embodiment 4
The preparation method of graphene sponge for water-oil separating, steps are as follows：
1）The chitosan for taking weight average molecular weight to be 500,000 is dissolved in the acetic acid solution that mass concentration is 2%, is configured to mass concentration and is
3% chitosan acetic acid solution；
2）Melamine sponge ethyl alcohol and deionized water are washed three times, it is dry to be then dipped in chitosan acetic acid solution to constant weight,
Drying is taken out after full penetration；
3）It takes graphene oxide to be added in deionized water and is ultrasonically treated 3h, it is water-soluble to obtain the graphene oxide that mass concentration is 0.5%
Liquid, by step 2）The sponge of middle drying is immersed in graphene oxide water solution, and drying is taken out after full penetration；
4）By step 3）The sponge of middle drying is immersed in the sodium borohydride solution of a concentration of 1mol/L, under 60 DEG C of water bath conditions also
Original takes out sponge drying after reaction；
5）It takes trishydroxymethylaminomethane to be added drop-wise in n-hexane, is being configured to the trishydroxymethylaminomethane that volume fraction is 2% just
Hexane solution, by step 4）The sponge of middle drying is immersed in trishydroxymethylaminomethane hexane solution, is sufficiently impregnated 3 hours,
Drying is taken out to get the graphene sponge for water-oil separating.
Step 2）Step 5）Middle drying temperature is 80 DEG C.
Claims (6)
1. the preparation method of the graphene sponge for water-oil separating, which is characterized in that steps are as follows：
1) it takes chitosan to be dissolved in the acetic acid solution that mass concentration is 2%, is configured to the chitosan acetic acid that mass concentration is 3-5%
Solution；
2) sponge ethyl alcohol and deionized water are washed three times, it is dry to constant weight, it is then dipped in chitosan acetic acid solution, fully
Drying is taken out after being impregnated with；
3) it takes graphene oxide to be added in deionized water and is ultrasonically treated 2-3h, obtain graphene oxide water solution, will be dried in step 2)
Dry sponge is immersed in graphene oxide water solution, and drying is taken out after full penetration；
4) sponge dried in step 3) is immersed in sodium borohydride solution, is restored under water bath condition, take out sea after reaction
Silk floss drying；
5) it takes trishydroxymethylaminomethane to be added drop-wise in n-hexane, is configured to the trihydroxy methyl amino first that volume fraction is 1-2%
The sponge dried in step 4) is immersed in trishydroxymethylaminomethane hexane solution, is sufficiently impregnated 2-3 by alkane hexane solution
Hour, drying is taken out to get the graphene sponge for water-oil separating.
2. the preparation method for the graphene sponge of water-oil separating as described in claim 1, which is characterized in that the step
1) weight average molecular weight of chitosan is 30-50 ten thousand in.
3. the preparation method for the graphene sponge of water-oil separating as described in claim 1, which is characterized in that the sponge
For melamine sponge or polyurethane sponge.
4. the preparation method for the graphene sponge of water-oil separating as described in claim 1, which is characterized in that the step
3) mass concentration of graphene oxide water solution is 0.5-5% in.
5. the preparation method for the graphene sponge of water-oil separating as described in claim 1, which is characterized in that the step
4) a concentration of 1-2mol/L of sodium borohydride solution in, bath temperature are 60-90 DEG C.
6. the preparation method for the graphene sponge of water-oil separating as described in claim 1, which is characterized in that the step
2) drying temperature is 70-80 DEG C in-step 5).
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| CN201810767983.XA CN108744606A (en) | 2018-07-13 | 2018-07-13 | The preparation method of graphene sponge for water-oil separating |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110394162A (en) * | 2019-07-10 | 2019-11-01 | 浙江海洋大学 | A kind of preparation method of environmentally friendly magnetic Nano compound oil absorption material |
| CN114345306A (en) * | 2021-12-10 | 2022-04-15 | 吉林省电力科学研究院有限公司 | Preparation method of hydrophilic positively charged emulsion separation material |
Citations (4)
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| CN102961893A (en) * | 2012-11-07 | 2013-03-13 | 清华大学 | Super-hydrophobic and super-oleophylic oil-water separating mesh membrane and preparation method thereof |
| CN103736400A (en) * | 2014-01-06 | 2014-04-23 | 中国海洋大学 | Preparation method of graphene oxide composite nano filter membrane |
| CN106310978A (en) * | 2016-10-17 | 2017-01-11 | 江苏新风环保科技有限公司 | Compound air filter membrane based on chitosan and graphene oxide and preparation method of compound air filter membrane |
| CN106693444A (en) * | 2016-12-27 | 2017-05-24 | 西南石油大学 | Preparing method of reproducible super-hydrophobic graphite alkenyl oil absorption sponge |
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2018
- 2018-07-13 CN CN201810767983.XA patent/CN108744606A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102961893A (en) * | 2012-11-07 | 2013-03-13 | 清华大学 | Super-hydrophobic and super-oleophylic oil-water separating mesh membrane and preparation method thereof |
| CN103736400A (en) * | 2014-01-06 | 2014-04-23 | 中国海洋大学 | Preparation method of graphene oxide composite nano filter membrane |
| CN106310978A (en) * | 2016-10-17 | 2017-01-11 | 江苏新风环保科技有限公司 | Compound air filter membrane based on chitosan and graphene oxide and preparation method of compound air filter membrane |
| CN106693444A (en) * | 2016-12-27 | 2017-05-24 | 西南石油大学 | Preparing method of reproducible super-hydrophobic graphite alkenyl oil absorption sponge |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110394162A (en) * | 2019-07-10 | 2019-11-01 | 浙江海洋大学 | A kind of preparation method of environmentally friendly magnetic Nano compound oil absorption material |
| CN114345306A (en) * | 2021-12-10 | 2022-04-15 | 吉林省电力科学研究院有限公司 | Preparation method of hydrophilic positively charged emulsion separation material |
| CN114345306B (en) * | 2021-12-10 | 2023-08-08 | 吉林省电力科学研究院有限公司 | Preparation method of hydrophilic positively charged emulsion separation material |
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