CN115746946A - Preparation method of cracked transformer reclaimed oil based on graphene column chromatography - Google Patents
Preparation method of cracked transformer reclaimed oil based on graphene column chromatography Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 34
- 238000004440 column chromatography Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002699 waste material Substances 0.000 claims abstract description 29
- 238000005336 cracking Methods 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 27
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 27
- 239000000741 silica gel Substances 0.000 claims description 27
- 229910002027 silica gel Inorganic materials 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 15
- 230000005526 G1 to G0 transition Effects 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 claims 3
- 230000008929 regeneration Effects 0.000 abstract description 8
- 238000011069 regeneration method Methods 0.000 abstract description 8
- 238000001179 sorption measurement Methods 0.000 abstract description 8
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 75
- 239000003463 adsorbent Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 238000004949 mass spectrometry Methods 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000005311 nuclear magnetism Effects 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 description 1
- GMQBTYDSNWTPBJ-UHFFFAOYSA-N 4-bicyclo[2.2.1]heptanylmethanesulfonic acid Chemical compound C1CC2CCC1(CS(=O)(=O)O)C2 GMQBTYDSNWTPBJ-UHFFFAOYSA-N 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- AFVFQIVMOAPDHO-UHFFFAOYSA-N methanesulfonic acid Substances CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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Abstract
The invention discloses a preparation method of regenerated oil of a cracking transformer based on graphene column chromatography. The invention can realize the high-efficiency adsorption and regeneration of the waste transformer oil, improve the resource utilization rate and avoid environmental pollution and resource waste.
Description
Technical Field
The invention relates to the technical field of transformers, in particular to a transformer oil recycling technology.
Background
The transformer oil is used as an important medium in power system power transmission and transformation equipment, is widely applied to oil-immersed insulation high-voltage power transmission and transformation equipment such as transformers, current transformers, circuit breakers, sleeves and the like, can play roles in improving electrical insulation strength, arc extinction, improving heat dissipation performance and the like, and ensures safe and reliable operation of the equipment. However, with the operation of the equipment, due to the high temperature generated by the electric appliance, the contact with oxygen in the air, the moisture entering the air and other factors or synergistic effects, the transformer oil can generate chemical reactions to generate compounds such as aldehyde, ketone, carboxylic acid, naphthenic acid and the like after absorbing dissolved oxygen, so that the inevitable phenomena of gradual oxidation degradation of oil such as increased acid value, oil sludge precipitation, reduced interfacial tension, unqualified breakdown voltage, dielectric loss factor, volume resistivity and the like can be caused, and if the transformer oil is not replaced in time, the transformer fault accident can be caused. So a large amount of deteriorated oil of the transformer needs to be replaced every year.
However, the waste transformer oil is not a completely useless waste, belongs to renewable and comprehensive utilization resources, the oxidation product of the waste transformer oil only accounts for a small part, generally accounts for 1% -25% of the total amount, and the main body of the waste transformer oil is still the base oil, so that the waste is caused by direct waste.
Disclosure of Invention
Aiming at the defects of the prior art, the technical problem to be solved by the invention is to provide a preparation method of the regenerated oil of the cracking transformer based on graphene column chromatography, so as to realize the regeneration of the waste transformer oil.
In order to solve the technical problem, the invention adopts the following technical scheme:
a method for preparing regenerated oil of a cracking transformer based on graphene column chromatography comprises the steps of taking waste transformer oil as a raw material, taking graphene and column chromatography silica gel powder as a stationary phase and n-hexane as a mobile phase, and adopting a column chromatography separation and purification method to obtain the regenerated transformer oil.
Preferably, the preparation method takes a glass chromatographic column as a preparation carrier, and normal hexane and column chromatography silica gel powder are filled into the column by a wet method; and then, laying a layer of graphene powder on the upper layer of a silica gel column, taking n-hexane as a mobile phase, carrying out column chromatography separation to obtain a product, and finally carrying out reduced pressure distillation to remove the n-hexane solution.
Preferably, after the wet column packing, air in the silica gel column is discharged by using a pressure pump so as to reduce the micropore structure in the silica gel particles of the column chromatography.
Preferably, the column chromatography silica gel powder is 300-400 meshes.
Preferably, the thickness of the graphene powder is 1cm.
The method takes the waste transformer oil as a raw material, takes graphene and column chromatography silica gel powder as a stationary phase and n-hexane as a mobile phase, and adopts a column chromatography separation and purification method to obtain the regenerated transformer oil.
The analysis results of the physical and chemical properties of the transformer oil before and after adsorption and the combination of nuclear magnetism, infrared and gas chromatography show that: after the waste transformer oil is adsorbed and treated by the graphene composite adsorbent, the oxidation product of the obtained regenerated transformer oil is obviously reduced or disappears, the functional group of the regenerated transformer oil is formed, the overall composition of the regenerated transformer oil is basically consistent with that of the new transformer oil, the physical and chemical properties of the regenerated transformer oil are obviously improved, and the indexes such as volume resistivity, interfacial tension, dielectric loss factors, breakdown voltage, acid value and the like completely meet the national standard.
Therefore, the method can realize the efficient adsorption and regeneration of the waste transformer oil, improve the resource utilization rate, avoid the environmental pollution and the resource waste and develop the application of the graphene in the field of adsorption and refining of the waste transformer oil.
The following detailed description and the accompanying drawings are included to provide a further understanding of the invention.
Drawings
The invention is further described with reference to the accompanying drawings and the detailed description below:
FIG. 1 is a flow chart of purification and refining of waste transformer oil according to the present invention;
FIG. 2 is a nuclear magnetic resonance spectrum of three transformer oils;
FIG. 3 is an infrared spectrum of waste transformer oil and regenerated transformer oil.
Detailed Description
The technical solutions of the embodiments of the present invention are explained and illustrated below with reference to the drawings of the embodiments of the present invention, but the following embodiments are only preferred embodiments of the present invention, and not all embodiments. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative effort belong to the protection scope of the present invention.
It will be appreciated by those skilled in the art that features from the examples and embodiments described below may be combined with each other without conflict.
According to the invention, the graphene and silica gel with staggered laminated structures are used as the composite adsorbent, so that the adsorption regeneration application research on the waste transformer oil is carried out, and the physical and chemical structures of the graphene are correspondingly characterized.
A method for preparing regenerated oil of a cracking transformer based on graphene column chromatography comprises the steps of taking waste transformer oil to be replaced as an object, taking graphene and column chromatography silica gel powder (300-400 meshes) as a stationary phase and n-hexane as a mobile phase, and separating and purifying by using column chromatography to obtain the recyclable regenerated transformer oil (n-hexane, rf = 0.9).
As shown in fig. 1, the specific steps are as follows:
1. taking a dry and clean glass chromatographic column;
2. filling the column with n-hexane and column chromatography silica gel powder by a wet method, and discharging air in the silica gel column by a pressure pump to reduce a micropore structure inside column chromatography silica gel particles;
3. laying a layer of graphene powder on the upper layer of the treated silica gel column, wherein the thickness of the graphene powder is about 1 cm;
4. using n-hexane as a mobile phase, and performing column chromatography separation to obtain a refined product (Rf = 0.9);
5. and (4) distilling under reduced pressure to remove the n-hexane solution, and preparing the regenerated transformer oil.
Furthermore, nuclear magnetism and infrared characterization are carried out on the prepared regenerative transformer oil.
And (3) carrying out verification:
in order to verify the effectiveness and practicability of the method provided by the invention, the following 4 types of methods are used for verification.
1. Nuclear magnetic comparison results
The composition of the transformer oil was examined using a Bruker Avance 400MHz NMR spectrometer from Bruker, inc. of Bruker, switzerland. The detection system is kept at 298K, TMS is used as an internal standard, each spectrogram is scanned for 32 times, the spectral width is 11.5ppm, the sampling time is 2s, and the pulse interval d1 is 5s. Data processing is carried out through Topspin2.0 software carried by nuclear magnetism.
As shown in FIG. 2 (processing with silica gel), in the column chromatography purification system using silica gel as the stationary phase, the integral of 2.5ppm of chemical shift is 1.00, and the integral of 6.9ppm of chemical shift is 0.45, compared with the waste oil, the impurity contents of the two parts are obviously reduced, the impurity content of 2.5ppm is slightly higher than that of the new oil, and the impurity content of 6.9ppm is almost twice as high as that of the new oil, which indicates that the waste oil treated by the column chromatography method has better purification effect. It is worth noting that when silica gel and Graphene are used as a fixed phase (processing with Graphene and silica gel), the impurity content in the processed sample is the lowest and better than that of the new oil, the integral of the chemical shift of 2.5ppm is 0.98, the integral of the chemical shift of 6.9ppm is 0.26, the result is almost the same as the nuclear magnetic integral result of the new oil, and the signal peak intensity at 1.5ppm is obviously reduced, which indicates that the functional group composition of the regenerated oil obtained by processing the waste transformer oil by using the Graphene composite silica gel adsorbent is basically consistent with that of the new transformer oil.
2. Oil quality analysis and comparison of transformer oil
The testing method adopts the latest national standard or electric power industry standard for measurement, and the physical properties of the test comprise appearance (GB/T511), water-soluble acid (pH value) (GB/T7598), acid value (GB/T264), closed flash point (GB/T261), moisture (GB/T7600), interfacial tension (GB/T6541), dielectric loss factor (GB/T5654), breakdown voltage (DL/T507), volume resistivity (DL/T421), oil sludge and precipitate (mass fraction) (GB/T511) and corrosive sulfur (SH/T0804).
And selecting the regenerated transformer oil with better regeneration effect and obtained by adopting the graphene and silica gel composite adsorbent, and comparing the regenerated transformer oil with the new and waste transformer oils for oil quality analysis. The performance tests are compared in table 1. The index electrical performance index of the regenerated oil subjected to graphene regeneration treatment is basically equivalent to that of the new oil.
Table 1: analysis results of main indexes of three transformer oils
3. Infrared comparison result
The transformer oil was examined using a Nexus Fourier transform infrared spectrometer (FT-IR) of the Nexus type.
Fig. 3 is an infrared spectrum of the waste transformer oil and the regenerated transformer oil subjected to composite adsorption of graphene and silica gel. From the figure, the methyl (-CH) group can be seen 3 ) The antisymmetric telescopic vibration absorption is 2952cm -1 Symmetric telescopic vibration absorption is 2858cm -1 Methylene (-CH) 2 -) antisymmetric telescopic vibration absorption at 2918cm -1 Symmetric telescopic vibration absorption of 1375cm -1 And 1458cm -1 Then respectively correspond to methyl (-CH) 3 ) And methylene (-CH) 2 -in-plane bending vibration absorption of the transformer oil, these polar functional groups, indicate oxidation products resulting from gradual aging of the transformer oil during use: ketones, aldehydes or alcohols, consistent with nuclear magnetic results, and eventually will be further oxidatively converted to carboxylic acids. The infrared spectrogram shows that the regenerated transformer oil obtained after the adsorption treatment of the waste transformer oil has methyl (-CH) 3 ) And methylene (-CH) 2 Decrease in the intensity of the infrared peak indicating an improvement in its performance, which also corresponds to the nuclear magnetic characterization results.
4. Comparison of gas chromatography and mass spectrometry
In the gas-fixation chromatography, an adsorbent with large surface area and certain activity is used as a stationary phase. Due to the different adsorption forces of the adsorbent on each component, the components are run at different speeds in the column. Mass spectrometry is an analytical method for measuring the charge-to-mass ratio (charge-to-mass ratio) of ions. In a mass analyzer, the mass is determined by dispersing the occurring opposite velocities using an electric field and a magnetic field, and focusing them to obtain mass spectra, respectively. The gas chromatograph-mass spectrometer was manufactured by 6890N/5975MSD from Agilent, USA, and the sensitivity: 1, 1pgOFN, m/z272, S/N: 175.
Quantitative analysis of two oxidation products, classified as butylhydroxytoluene and bicyclo [2.2.1] heptane-1-methanesulfonic acid, at 9.50min and 12.76min, respectively, was performed by careful comparison of the mass spectral components of the three transformer oils, see table 2.
Table 2: analysis result table for oil-gas-mass spectrometry of three transformer oils
Wherein the content of the butyl hydroxy toluene in the waste oil is 10.223%, the content of the butyl hydroxy toluene in the new oil is only 4.194%, and the content of the transformer oil regenerated by the graphene is 5.999%; bicyclo [2.2.1] heptane-1-methane sulfonic acid accounts for 10.251% of the waste oil, only 2.229% of the new oil, and 5.369% of the transformer oil after graphene regeneration. It can be seen that the content of alkane oxide in the regenerated oil is obviously reduced and is close to the content of the new oil, which indicates that the waste transformer oil refined by adopting the graphene and silica gel composite adsorbent is a simple, easy and highly efficient regeneration treatment process.
While the invention has been described with reference to specific embodiments, it will be understood by those skilled in the art that the present invention may be practiced without limitation to such specific embodiments. Any modification which does not depart from the functional and structural principles of the present invention is intended to be included within the scope of the claims.
Claims (5)
1. The preparation method of the regenerated oil of the cracking transformer based on the graphene column chromatography is characterized in that the regenerated transformer oil is obtained by adopting a column chromatography separation and purification method by taking waste transformer oil as a raw material, taking graphene and column chromatography silica gel powder as a stationary phase and n-hexane as a mobile phase.
2. The method for preparing the regenerated oil of the cracking transformer based on the graphene column chromatography is characterized by comprising the following steps of: the preparation method comprises the steps of taking a glass chromatographic column as a preparation carrier, and filling the glass chromatographic column with n-hexane and column chromatography silica gel powder by a wet method; and then, laying a layer of graphene powder on the upper layer of a silica gel column, taking n-hexane as a mobile phase, carrying out column chromatography separation to obtain a product, and finally carrying out reduced pressure distillation to remove the n-hexane solution.
3. The preparation method of the regenerated oil for the pyrolysis transformer based on the graphene column chromatography as claimed in claim 2, characterized by comprising the following steps: and after the column is packed by the wet method, discharging the air in the silica gel column by using a pressure pump so as to reduce the microporous structure in the silica gel particles for column chromatography.
4. The preparation method of the regenerated oil for the pyrolysis transformer based on the graphene column chromatography as claimed in claim 2, characterized by comprising the following steps: the column chromatography silica gel powder is 300-400 meshes.
5. The preparation method of the regenerated oil for the pyrolysis transformer based on the graphene column chromatography as claimed in claim 2, characterized by comprising the following steps: the thickness of the graphene powder is 1cm.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102899069A (en) * | 2012-10-30 | 2013-01-30 | 复旦大学 | Separating and upgrading method of bio-oil by column chromatography |
| CN111450573A (en) * | 2019-01-22 | 2020-07-28 | 福州奥尼多生物科技有限公司 | Graphene mixed filler, preparation method thereof, graphene mixed filler chromatographic column and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102899069A (en) * | 2012-10-30 | 2013-01-30 | 复旦大学 | Separating and upgrading method of bio-oil by column chromatography |
| CN111450573A (en) * | 2019-01-22 | 2020-07-28 | 福州奥尼多生物科技有限公司 | Graphene mixed filler, preparation method thereof, graphene mixed filler chromatographic column and application thereof |
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