CN109056118B - Graphene fiber and preparation method thereof - Google Patents
Graphene fiber and preparation method thereof Download PDFInfo
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- CN109056118B CN109056118B CN201810833034.7A CN201810833034A CN109056118B CN 109056118 B CN109056118 B CN 109056118B CN 201810833034 A CN201810833034 A CN 201810833034A CN 109056118 B CN109056118 B CN 109056118B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 108
- 239000000835 fiber Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 29
- -1 amino modified ferroferric oxide Chemical class 0.000 claims abstract description 16
- 238000002166 wet spinning Methods 0.000 claims abstract description 15
- 230000009471 action Effects 0.000 claims abstract description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 24
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical class O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 238000005576 amination reaction Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000004132 cross linking Methods 0.000 claims description 8
- 230000009467 reduction Effects 0.000 claims description 7
- 239000007822 coupling agent Substances 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims description 5
- 230000003197 catalytic effect Effects 0.000 claims description 5
- 230000006698 induction Effects 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 3
- 229940071870 hydroiodic acid Drugs 0.000 claims description 3
- 239000000047 product Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 238000003828 vacuum filtration Methods 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 244000207740 Lemna minor Species 0.000 description 1
- 235000006439 Lemna minor Nutrition 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 241001343083 Tonna Species 0.000 description 1
- NJSVDVPGINTNGX-UHFFFAOYSA-N [dimethoxy(propyl)silyl]oxymethanamine Chemical compound CCC[Si](OC)(OC)OCN NJSVDVPGINTNGX-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- QKSIFUGZHOUETI-UHFFFAOYSA-N copper;azane Chemical compound N.N.N.N.[Cu+2] QKSIFUGZHOUETI-UHFFFAOYSA-N 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001891 gel spinning Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Fibers (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a preparation method of graphene fiber, which is characterized in that amino modified ferroferric oxide is used for modifying graphene oxide, wet spinning is carried out under the action of a magnetic field, the elongation of the graphene fiber prepared by the method can reach 50%, and is obviously higher than that of the existing graphene fiber (the elongation is about 10%), and the graphene fiber obtained by the method has high strength, high conductivity and excellent mechanical and electrical properties.
Description
Technical Field
The invention relates to the technical field of graphene fiber materials, in particular to a preparation method of graphene fibers.
Background
The one-dimensional reduced graphene oxide fiber has higher flexibility and excellent electrical performance compared with the traditional semiconductor, and the flexibility and the resistance stability of the fiber can be improved after the fiber is functionalized. Therefore, the one-dimensional reduced graphene oxide fiber has attracted a wide range of attention, and has a potential role in the fields of wearable electronic devices, stretch sensors, smart actuators, supercapacitors, smart clothing, and the like.
At present, methods such as dry-wet spinning, chemical assembly reduction, electrophoretic assembly, dry film rolling and the like have been applied to synthesis of graphene oxide-based fibers. The method mainly comprises the steps of utilizing pure graphene oxide spinning or introducing a third substance (such as metal ions, high polymers and the like) in the graphene oxide spinning process, and reducing the graphene oxide fibers by using strong acid or strong base, so that the finally obtained graphene fibers have excellent mechanical, electrical or electro-mechanical properties.
However, although these studies have reached a significant achievement at present, the elongation of the graphene fiber spun by introducing metal ions and high polymer into the graphene oxide solution is about 10%, because the introduction of metal ions and high polymer has insufficient influence on the stacking rule of the graphene oxide during the graphene oxide spinning process, and the stacking of graphene sheets cannot be well regulated, so that the flexibility of the prepared fiber cannot reach the expected value of researchers, and the prepared fiber product has poor elasticity and poor electrical stability during the twisting and stretching processes.
Disclosure of Invention
The invention aims to provide a preparation method of graphene fibers, which is used for improving the elongation of the graphene fibers, enhancing the flexibility of the graphene fibers and further improving the electrical stability of the graphene fibers.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of graphene fibers, which comprises the following steps:
carrying out a crosslinking reaction on graphene oxide and amino modified ferroferric oxide under the catalytic action of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to obtain magnetic graphene oxide;
carrying out wet spinning on the magnetic graphene oxide under the action of a magnetic field to obtain graphene oxide fibers;
and reducing the graphene oxide fibers to obtain the graphene fibers.
Preferably, the mass ratio of the amino modified ferroferric oxide to the graphene oxide is 2.5: 97.5-30: 70.
Preferably, the time of the crosslinking reaction is 15-180 min.
Preferably, during wet spinning, the induction direction of the magnetic field and the filamentation direction form an included angle of 0-180 degrees.
Preferably, the magnetic field strength of the magnetic field is 25-500 mT.
Preferably, the speed of the wet spinning is 1-50 mL/h, and the time is 1-180 s.
Preferably, the reduction temperature is 10-100 ℃ and the time is 1-20 h.
Preferably, the preparation method of the amino modified ferroferric oxide comprises the following steps:
mixing Fe3O4Mixing the particles, a coupling agent and an organic solvent, and then carrying out an amination reaction to obtain amino modified ferroferric oxide; the above-mentionedThe coupling agent is aminopropyl triethoxysilane.
Preferably, the organic solvent is a mixture of methanol and toluene, and the volume ratio of the methanol to the toluene is 1: 1.
Preferably, the temperature of the amination reaction is 100-120 ℃, and the time is 5-20 h.
The invention provides a preparation method of graphene fibers, which comprises the steps of modifying graphene oxide by amino modified ferroferric oxide to obtain magnetic graphene oxide; and then carrying out wet spinning on the magnetic graphene oxide under the action of a fixed magnetic field, and changing the stacking structure of the internal lamellar layers of the fiber by regulating and controlling the induction direction of the magnetic field, thereby improving the mechanical, electrical and electro-mechanical properties of the graphene fiber.
The elongation of the graphene fiber prepared by the method can reach 50%, which is obviously higher than that of the existing graphene fiber (the elongation is about 10%), and meanwhile, the graphene fiber product obtained by the method has excellent elasticity and excellent electrical stability in the twisting and stretching processes.
The method has the advantages of wide applicability, simple operation, flexible process adjustment, lower production cost and high efficiency, and is easy for industrialized production.
Detailed Description
The invention provides a preparation method of graphene fibers, which comprises the following steps:
carrying out a crosslinking reaction on graphene oxide and amino modified ferroferric oxide under the catalytic action of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to obtain magnetic graphene oxide;
carrying out wet spinning on the magnetic graphene oxide under the action of a magnetic field to obtain graphene oxide fibers;
and reducing the graphene oxide fibers to obtain the graphene fibers.
According to the invention, graphene oxide and amino modified ferroferric oxide are subjected to a crosslinking reaction under the catalytic action of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, so as to obtain the magnetic graphene oxide. In the invention, the mass ratio of the amino-modified ferroferric oxide to the graphene oxide is preferably 2.5: 97.5-30: 70, and more preferably 5: 95-15: 85. In the present invention, the time for the crosslinking reaction is preferably 15min to 180min, more preferably 50min to 150min, and most preferably 80min to 120 min. In the embodiment of the invention, the graphene oxide is prepared by an improved Hummer method according to a method of literature (Chengchen, tonna, Lemna minor, and the like, electrical properties of graphene layer group copper ammonia fibers [ J ] printing and dyeing, 2017(20): 7-10.).
In the invention, the preparation method of the amino-modified ferroferric oxide preferably comprises the following steps:
mixing Fe3O4Mixing the particles, a coupling agent and an organic solvent, and then carrying out an amination reaction to obtain amino modified ferroferric oxide; the coupling agent is aminopropyl triethoxysilane.
In the present invention, the organic solvent is preferably a mixture of methanol and toluene, and the volume ratio of methanol to toluene is preferably 1: 1. The mixing method is not particularly limited, and the mixing method can be selected from methods well known to those skilled in the art. In the invention, the temperature of the amination reaction is preferably 100-120 ℃, more preferably 110-118 ℃, and the time is preferably 5-20 hours, more preferably 10-15 hours. The present invention preferably performs the amination reaction under oil bath and reflux conditions. After the amination reaction is completed, methanol is preferably adopted to wash the amination reaction product for 2-3 times, then the washed product is subjected to vacuum filtration, and then the product obtained by the vacuum filtration is placed in a vacuum drying oven to be dried and is crushed to obtain the amino modified ferroferric oxide. The source of the ferroferric oxide particles is not particularly limited, and the ferroferric oxide particles can be prepared by a preparation method well known by a person skilled in the art, such as a coprecipitation method, a thermal decomposition method, a hydrothermal method, a solvothermal method, a microemulsion method and an air oxidation method.
According to the invention, amino modified ferroferric oxide is covalently crosslinked on a graphene oxide sheet under the catalysis, the graphene oxide sheet is driven to rotate through the induction of a magnetic field, graphene oxide fibers with regular structures can be obtained, and then the graphene oxide fibers are obtained through reduction.
After the magnetic graphene oxide is obtained, wet spinning is carried out on the magnetic graphene oxide under the action of a magnetic field, so as to obtain the graphene oxide fiber. According to the invention, the solution of the magnetic graphene oxide is preferably filled into a plastic injector, injected into an acetic acid bath at a speed of 10mL/h by using an injection pump, and subjected to wet spinning under the action of a magnetic field. In the invention, during wet spinning, the inducing direction of the magnetic field preferably forms an included angle of 0-180 degrees with the filamentation direction of the fiber, and more preferably forms an included angle of 0-90 degrees; the wet spinning speed is preferably 1-50 mL/h, more preferably 10-30 mL/h, and the time is preferably 1-180 s, more preferably 50-150 s; the magnetic field strength of the magnetic field is preferably 25-500mT, more preferably 50-300 mT. According to the invention, the stacking structure of the internal lamella of the fiber can be changed through magnetic field induction, the flexibility of the graphene fiber can be enhanced, the elongation of the graphene fiber can be improved, and the electrical and electro-mechanical properties of the graphene fiber can be improved.
After the graphene oxide fiber is obtained, the graphene oxide fiber is reduced to obtain the graphene fiber. In the invention, the reduction temperature is preferably 10-100 ℃, more preferably 30-70 ℃, and the time is preferably 1-20 hours, more preferably 5-15 hours. The reduction mode is not particularly limited, and graphene can be obtained by selecting a mode for reducing graphene oxide into graphene, which is well known to those skilled in the art. In the embodiment of the invention, the graphene oxide fiber is specifically reduced by soaking in hydroiodic acid.
The following will explain the preparation method of the graphene fiber provided by the present invention in detail with reference to the examples, but they should not be construed as limiting the scope of the present invention.
Example 1
230mL of H2SO4、5g NaNO3Adding 10g of graphite powder and 30g of potassium permanganate into a beaker, uniformly mixing, stirring and reacting for 1h to obtain the graphite insertA layer composite; heating to 45 ℃ and continuing to react for 30min, adding 460mL of deionized water, and continuing to react for 30 min; adding 1400mL of deionized water and 50mL of hydrogen peroxide with the mass concentration of 30% in sequence, changing the solution from brick red to yellow, continuously reacting for 15min, washing with dilute hydrochloric acid with the mass concentration of 3% for three times, then centrifuging and washing with deionized water for multiple times to obtain graphite oxide, and performing ultrasonic dispersion on the graphite oxide for 4 hours to obtain graphene oxide;
mixing 1g of Fe3O4Dispersing the nanoparticles in 5.4g of silane coupling agent KH-540(APTMS), mixing the mixture into a solvent with the volume ratio of methanol to toluene being 1:1 (50 mL of each of methanol and toluene), putting the mixture into a 500mL three-neck flask, performing oil bath and refluxing for 10 hours at 110 ℃, after the reaction is finished, cleaning the refluxing product for 2-3 times by using methanol, and repeatedly performing vacuum filtration on the cleaning product. After the suction filtration is finished, placing the suction filtration product in a vacuum drying oven for drying, and grinding the dried product into powder to obtain amino modified ferroferric oxide;
mixing 5g of amino modified ferroferric oxide, 95g of graphene oxide and water, mixing and stirring for 90min under the catalytic action of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, carrying out a crosslinking reaction to obtain a magnetic graphene oxide solution, and drying to obtain magnetic graphene oxide powder;
preparing the magnetic graphene oxide powder into a solution with the mass concentration of 2%, filling the solution into a plastic injector, injecting the solution into an acetic acid bath at the speed of 10mL/h by using an injection pump, and performing wet spinning under the action of a magnetic field (the magnetic field intensity is 500mT) to obtain graphene oxide fibers; and soaking the graphene oxide fiber in hydroiodic acid, and reducing for 8 hours at 95 ℃ to obtain the graphene fiber.
Example 2
Graphene fibers were prepared according to the method described in example 1, except that the weight ratio of amino-modified ferroferric oxide to graphene oxide was 7.5:92.5 in this example.
Example 3
Graphene fibers were prepared according to the method described in example 1, except that the weight ratio of amino-modified ferroferric oxide to graphene oxide was 10:90 in this example.
Example 4
Graphene fibers were prepared according to the method described in example 1, except that the weight ratio of amino-modified ferroferric oxide to graphene oxide was 12.5:87.5 in this example.
Example 5
Graphene fibers were prepared according to the method described in example 1, except that the weight ratio of amino-modified ferroferric oxide to graphene oxide was 15:85 in this example.
The graphene fibers prepared in examples 1 to 5 were subjected to performance tests under magnetic field and non-magnetic field conditions, and the specific results are shown in tables 1 and 2.
Table 1 shows mechanical property data of the graphene fibers prepared in examples 1 to 5 under the condition of no magnetic field, and it can be seen from table 1 that the elongation of the graphene fibers prepared by the method of the present invention can reach 50%, and compared with the existing graphene fibers (the elongation is about 10%), the elongation of the graphene fibers is significantly improved, the flexibility of the fibers is improved, and the graphene fibers have excellent mechanical properties.
Table 1 mechanical property data of graphene fibers prepared in the presence of no magnetic field
Table 2 resistance data of graphene fibers prepared in the presence of no magnetic field
| Case(s) | With magnetic field (omega cm) | Non-magnetic field (omega cm) |
| Example 1 | 17.32 | 42.41 |
| Example 2 | 8.85 | 49.71 |
| Example 3 | 7.11 | 83.79 |
| Example 4 | 5.52 | 31.30 |
| Example 5 | 8.94 | 63.37 |
Table 2 shows resistance data of the graphene fibers prepared in examples 1 to 5 in the presence of a magnetic field, and it can be seen that the graphene fibers prepared by the method of the present invention have excellent electrical stability.
According to the embodiment, the graphene oxide is modified by amino-modified ferroferric oxide and then is subjected to wet spinning under the action of a magnetic field, so that the elongation of the graphene fiber prepared by the method can reach 50%, which is obviously higher than that of the existing graphene fiber (the elongation is about 10%), and the graphene fiber obtained by the method has high strength, high conductivity and excellent mechanical and electrical properties.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A preparation method of graphene fibers comprises the following steps:
carrying out a crosslinking reaction on graphene oxide and amino modified ferroferric oxide under the catalytic action of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to obtain magnetic graphene oxide;
carrying out wet spinning on the magnetic graphene oxide under the action of a magnetic field to obtain graphene oxide fibers;
reducing the graphene oxide fibers to obtain graphene fibers;
the mass ratio of the amino modified ferroferric oxide to the graphene oxide is 2.5: 97.5-30: 70;
the magnetic field intensity of the magnetic field is 25-500 mT;
the reduction was carried out in hydroiodic acid.
2. The method according to claim 1, wherein the time for the crosslinking reaction is 15 to 180 min.
3. The preparation method according to claim 1, wherein the angle between the induction direction of the magnetic field and the filament forming direction is 0-180 ° in the wet spinning.
4. The method according to claim 1 or 3, wherein the wet spinning speed is 1-50 mL/h and the time is 1-180 s.
5. The preparation method according to claim 1, wherein the reduction is carried out at a temperature of 10 to 100 ℃ for 1 to 20 hours.
6. The preparation method according to claim 1, wherein the preparation method of the amino-modified ferroferric oxide comprises the following steps:
mixing Fe3O4Mixing the particles, a coupling agent and an organic solvent, and then carrying out an amination reaction to obtain amino modified ferroferric oxide; the coupling agent is aminopropyl triethoxysilane.
7. The method according to claim 6, wherein the organic solvent is a mixture of methanol and toluene, and the volume ratio of methanol to toluene is 1: 1.
8. The preparation method according to claim 6, wherein the temperature of the amination reaction is 100 to 120 ℃ and the time is 5 to 20 hours.
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| CN114542990A (en) * | 2020-11-25 | 2022-05-27 | 中国石油化工股份有限公司 | Electro-spinning magnetic nanofiber demulsifier for low-temperature gathering and transportation of crude oil and preparation method thereof |
| CN114394679B (en) * | 2022-01-19 | 2023-05-23 | 江苏利然环保科技有限公司 | Microbial adsorbent for industrial wastewater and preparation method thereof |
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