CN107638867A - A kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil - Google Patents
A kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil Download PDFInfo
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- CN107638867A CN107638867A CN201711001838.2A CN201711001838A CN107638867A CN 107638867 A CN107638867 A CN 107638867A CN 201711001838 A CN201711001838 A CN 201711001838A CN 107638867 A CN107638867 A CN 107638867A
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- insulating oil
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- molecular sieve
- benzyldithio toluene
- sorbent preparation
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Abstract
A kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil, the present invention relates to sorbent preparation method field.The invention solves because corrosion of the active sulfur in insulating oil based on benzyldithio toluene to Transformer Winding copper cash, caused transformer fault frequently occur, the safety belt to power network carrys out the technical problem of high risks at present.The inventive method：First, lanthanum modified molecular screen is prepared；2nd, copper-loaded lanthanum modified molecular screen is prepared；3rd, compound, drying and roasting is carried out to copper-loaded lanthanum modified molecular screen using nickel nitrate solution.Adsorbent of the present invention has very strong selective absorption effect to benzyldithio toluene in insulating oil, and clearance is high, and can effectively improve insulation oil quality.Adsorbent prepared by the present invention is used to remove active sulfur compound in product oil.
Description
Technical field
The present invention relates to sorbent preparation method field.
Background technology
In recent years, transformer fault frequently occurs caused by active sulfur in insulating oil both at home and abroad, the safety to power network
High risks are brought, and cause larger economic loss and social influence.By to 540 220kV and above
Transformer carries out sulfur corrosion experiment, finds to contain benzyldithio toluene (DBDS), content in the strong insulating oil of sulfur corrosion
In the range of 35mg/kg~115mg/kg, and the insulating oil for not containing benzyldithio toluene does not have sulfur corrosion, therefore dibenzyl
Disulfide is most important copper corrosion performance material.During transformer station high-voltage side bus, benzyldithio toluene meeting and transformation in insulating oil
The copper conductor of device is reacted, and corrodes metallic copper, and cuprous sulfide is produced on its surface and is separated out, and the higher reaction speed of temperature
It is faster, when the cuprous sulfide amount of generation is more, it can penetrate into insulating paper, destroy the insulating properties of insulating paper, led when serious
Mutagens depressor breakdown between adjacent turns, make winding scaling loss.New insulation oil standard (IEC 60296) requirement that IEC is formulated is in product oil
The content of benzyldithio toluene (DBDS) is not higher than 5mg/kg.Therefore, containing for benzyldithio toluene in insulating oil should strictly be controlled
Amount, and should take measures to remove it for the insulating oil containing benzyldithio toluene.
In terms of active sulfur compound in removing product oil, people have done more work, are mainly entered using adsorbent
Row absorption.The CuHY molecular sieves, CuMCM41 adsorbents, mesoporous composite molecular sieve ZSM-5/MCM- of lanthanum modification are reported in document
41st, the preparation method and its desulfurization performance of Cu/Ce-MCM-41 molecular sieves and copper-loaded 5A molecular sieves；The A of patent CN 106693888
It is using activated carbon as matrix, by soda acid processing and copper-loaded processing, prepares desulfuration adsorbent；The A of patent CN 103240053 are to use
Zeolite molecular sieve, nickel nitrate, water conventional ion exchange to obtain adsorbent, filter adsorbent, are calcined siliceous, aluminium zeolite molecules
Sieve, then to adsorbent drying process, obtain powder insulating oil active sulfur scavenger, by powder insulating oil active sulfur scavenger with
Kaolin, waterglass, sodium pyrophosphate and water mixing, forming processes obtain finished product；The A of patent CN 103566867 are more than with aperture
3nm molecular sieve, 0.5mol/L copper nitrate solution is added, soak and be stirred at room temperature 24 hours, take out the molecule of immersion
Sieve, with distilled water washing and filtering repeatedly, much filtrate is dried 2 hours at 105 DEG C, dried object is loaded and is communicated with helium input
In the activator of pipeline, under helium protection, cooled down after 450 DEG C reduce 3 hours；Dried object is pressed 30：1 ratio adds dilute
Native cerium, grinding stir, and both obtain product.
Without for most important sulfur corrosion material benzyldithio toluene in insulating oil in these documents and patent
Removal is studied, and adsorbent is to the removal effect of active sulfur and imprecise.
The content of the invention
The invention solves at present because the active sulfur in insulating oil based on benzyldithio toluene is to Transformer Winding copper
The corrosion of line, caused transformer fault frequently occur, and the safety belt to power network carrys out the technical problem of high risks, and provides one
Kind is used for the sorbent preparation method for removing benzyldithio toluene in insulating oil.
A kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil, is carried out according to the following steps：
First, the quality NaY types molecular sieve such as general and demineralized water mix, and keep 2~2.5h, draining, add lanthanum nitrate hexahydrate, stir
Mix uniformly, soak 36~40h, leach molecular sieve, dry, it is 450~455 DEG C that temperature is controlled in nitrogen atmosphere, by molecular sieve
2~2.5h is calcined, then controls temperature to be cooled to room temperature for 550~555 DEG C of 2~2.5h of roasting, lanthanum modified molecular screen is made；
Wherein the Si/Al mol ratios of molecular sieve are 3.2~3.5, and spherical, particle diameter is 1.0~1.5mm；
2nd, by etc. the obtained lanthanum modified molecular screen of quality step one and demineralized water mix, keep 2~2.5h, draining, add
Copper ammonium chloride solution, stirs, soak 48~50h, leach molecular sieve, dry, control in nitrogen atmosphere temperature be 550~
555 DEG C, molecular sieve is calcined 2~2.5h, is cooled to room temperature, copper-loaded lanthanum modified molecular screen is made；
3rd, by etc. quality step two obtained copper-loaded lanthanum modified molecular screen and nickel nitrate solution stir, immersion 36~
40h, leach molecular sieve, clean 3 times with demineralized water, molecular sieve is leached, dry, controlled in nitrogen atmosphere temperature be 500~
505 DEG C, molecular sieve is calcined 2~2.5h, is cooled to room temperature, obtains the compound copper-loaded lanthanum modified molecular screen of nickel, completed one kind and be used for
Remove the sorbent preparation method of benzyldithio toluene in insulating oil.
The beneficial effects of the invention are as follows：
By the experimental study of project team, this patent proposes benzyldithio toluene in a kind of insulating oil dedicated for removal
Sorbent preparation method, obtained adsorbent is good to the selectivity of benzyldithio toluene, and adsorption efficiency is high, low cost, is suitable to
Popularization and application.After the adsorbent adsorption treatment prepared through the present invention, the oil of insulating oil is also greatly improved, oily medium damage
Consumption factor is reduced to 0.0031 by the 0.0079 of before processing；Acid number is reduced to 0.017mgKOH/g by the 0.069mg KOH/g of before processing.
Illustrate that adsorbent of the present invention has very strong selective absorption effect to benzyldithio toluene in insulating oil, clearance is high, exceedes
92%, and insulation oil quality can be effectively improved.
Adsorbent prepared by the present invention is used to remove active sulfur compound in product oil.
Brief description of the drawings
Fig. 1 is the sulfur corrosion copper sheet photo of the sorbent treatment prepared without embodiment one；
Fig. 2 is the sulfur corrosion copper sheet photo of the sorbent treatment prepared through embodiment one.
Embodiment
Technical solution of the present invention is not limited to the embodiment of act set forth below, in addition to each embodiment it
Between any combination.
Embodiment one：It is prepared by a kind of adsorbent for being used to remove benzyldithio toluene in insulating oil of present embodiment
Method, specifically carry out according to the following steps：
First, the quality NaY types molecular sieve such as general and demineralized water mix, and keep 2~2.5h, draining, add lanthanum nitrate hexahydrate, stir
Mix uniformly, soak 36~40h, leach molecular sieve, dry, it is 450~455 DEG C that temperature is controlled in nitrogen atmosphere, by molecular sieve
2~2.5h is calcined, then controls temperature to be cooled to room temperature for 550~555 DEG C of 2~2.5h of roasting, lanthanum modified molecular screen is made；
Wherein the Si/Al mol ratios of molecular sieve are 3.2~3.5, and spherical, particle diameter is 1.0~1.5mm；
2nd, by etc. the obtained lanthanum modified molecular screen of quality step one and demineralized water mix, keep 2~2.5h, draining, add
Copper ammonium chloride solution, stirs, soak 48~50h, leach molecular sieve, dry, control in nitrogen atmosphere temperature be 550~
555 DEG C, molecular sieve is calcined 2~2.5h, is cooled to room temperature, copper-loaded lanthanum modified molecular screen is made；
3rd, by etc. quality step two obtained copper-loaded lanthanum modified molecular screen and nickel nitrate solution stir, immersion 36~
40h, leach molecular sieve, clean 3 times with demineralized water, molecular sieve is leached, dry, controlled in nitrogen atmosphere temperature be 500~
505 DEG C, molecular sieve is calcined 2~2.5h, is cooled to room temperature, obtains the compound copper-loaded lanthanum modified molecular screen of nickel, completed one kind and be used for
Remove the sorbent preparation method of benzyldithio toluene in insulating oil.
Embodiment two：Present embodiment is unlike embodiment one：Lanthanum nitrate hexahydrate in step 1
Using the pure La of analysis3(NO3)3·6H2O is prepared, concentration 0.12mol/L.It is other identical with embodiment one.
Embodiment three：Present embodiment is unlike embodiment one or two：NaY types point in step 1
Son sieve active porosity is 4nm~6nm.It is other identical with embodiment one or two.
Embodiment four：Unlike one of present embodiment and embodiment one to three：Done in step 1
Dry temperature is 100 DEG C, drying time 6h.It is other identical with one of embodiment one to three.
Embodiment five：Unlike one of present embodiment and embodiment one to four：Chlorine in step 2
Change cuoxam using the pure (NH of analysis4)2CuCl2·2H2O is prepared, concentration 0.20mol/L.Other and embodiment one
It is identical to one of four.
Embodiment six：Unlike one of present embodiment and embodiment one to five：Done in step 2
Dry temperature is 120 DEG C, drying time 6h.It is other identical with one of embodiment one to five.
Embodiment seven：Unlike one of present embodiment and embodiment one to six：Nitre in step 3
Sour nickel solution is using the pure Ni NO of analysis3·6H2O is prepared, concentration 0.15mol/L.It is other with embodiment one to six it
One is identical.
Embodiment eight：Unlike one of present embodiment and embodiment one to seven：Done in step 3
Dry temperature is 100 DEG C, drying time 8h.It is other identical with one of embodiment one to seven.
Embodiment nine：Unlike one of present embodiment and embodiment one to eight：Used in step 3
When demineralized water cleans, demineralized water is cleaned in three times, the total dosage of demineralized water is 3 times of molecular sieve quality.Other and specific reality
It is identical to apply one of mode one to eight.
Embodiment ten：Unlike one of present embodiment and embodiment one to nine：NaY in step 1
The mass ratio of copper ammonium chloride solution is 1: 1: 1 in type molecular sieve, lanthanum nitrate hexahydrate and step 2.Other and embodiment one
It is identical to one of nine.
Beneficial effects of the present invention are verified using following examples and contrast experiment：
Embodiment one：
A kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil of the present embodiment, specifically by following step
It is rapid to carry out：
First, 1000gNaY types molecular sieve and 1000g demineralized waters are mixed, keeps 2h, draining, adding 1000g concentration is
0.12mol/L lanthanum nitrate hexahydrates, stir, and soak 36h, leach molecular sieve, and drying temperature is 100 DEG C, 6h is dried, in nitrogen
It is 450 DEG C that temperature is controlled in atmosphere, and molecular sieve is calcined into 2h, then controls temperature to be cooled to room temperature for 550 DEG C of roasting 2h, make
Obtain lanthanum modified molecular screen；Wherein the Si/Al mol ratios of molecular sieve are 3.2, and spherical, particle diameter is 1.0~1.5mm；NaY type molecular sieves
Active porosity is 4nm~6nm；
2nd, lanthanum modified molecular screen and 1000g the demineralized waters mixing obtained step 1, keeps 2h, draining, adds 1000g
Concentration is 0.20mol/L copper ammonium chloride solution, is stirred, and soaks 48h, leaches molecular sieve, and drying temperature is 120 DEG C, is dried
6h, it is 550 DEG C that temperature is controlled in nitrogen atmosphere, and molecular sieve is calcined into 2h, is cooled to room temperature, and copper-loaded lanthanum modified molecules are made
Sieve；
3rd, the copper-loaded lanthanum modified molecular screen and 1000g concentration obtained step 2 stirs for 0.15mol/L nickel nitrate solutions
Uniformly, 36h is soaked, leaches molecular sieve, with 3 cleanings of 3000g desalinations moisture, molecular sieve is leached, dried, in nitrogen atmosphere
It is 500 DEG C to control temperature, and molecular sieve is calcined into 2h, is cooled to room temperature, obtains the compound copper-loaded lanthanum modified molecular screen of nickel, is completed a kind of
For removing the sorbent preparation method of benzyldithio toluene in insulating oil.
One 500kV transformer is Ukraine's production, is put into operation within 1998, dibenzyl in the insulating oil in transformer
Disulfide content is 108.5mg/kg, and very strong sulfur corrosion is presented.It is modified using the compound copper-loaded lanthanum of nickel manufactured in the present embodiment
Molecular sieve carries out adsorption treatment to the insulation oil samples, and the mass ratio of molecular sieve and insulating oil is 1:10；Using static agitation
During adsorption treatment mode, benzyl disulfide ether content drops to 3.1mg/kg, clearance 97.1% in insulating oil after 24h；Using
During oil filter circular treatment mode, under conditions of controlling oil flow rate to be 0.5m/h, benzyldithio toluene in insulating oil after 24h
Content drops to 8.6mg/kg, clearance 92.1%.
Sulfur corrosion copper sheet photo without the present embodiment sorbent treatment is as shown in Figure 1；At the present embodiment adsorbent
The sulfur corrosion copper sheet photo of reason is as shown in Figure 2.
After adsorption treatment, the sulfur corrosion of the insulating oil disappears (as depicted in figs. 1 and 2)；Meanwhile the oil of insulating oil
Also it is greatly improved, oily dielectric dissipation factor is reduced to 0.0031 by the 0.0079 of before processing；Acid number is by before processing
0.069mgKOH/g is reduced to 0.017mgKOH/g.Illustrate that adsorbent of the present invention has very strong choosing to benzyldithio toluene in insulating oil
The suction-operated of selecting property, clearance is high, more than 92%, and can effectively improve insulation oil quality.
Claims (10)
1. a kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil, it is characterised in that this method is specifically pressed
Following steps are carried out：
First, will etc. quality NaY types molecular sieve and demineralized water mix, keep 2~2.5h, draining adds lanthanum nitrate hexahydrate, and stirring is equal
It is even, 36~40h is soaked, leaches molecular sieve, is dried, it is 450~455 DEG C that temperature is controlled in nitrogen atmosphere, and molecular sieve is calcined into 2
~2.5h, temperature is then controlled to be cooled to room temperature for 550~555 DEG C of 2~2.5h of roasting, lanthanum modified molecular screen is made；Wherein divide
The Si/Al mol ratios of son sieve are 3.2~3.5, and spherical, particle diameter is 1.0~1.5mm；
2nd, by etc. the obtained lanthanum modified molecular screen of quality step one and demineralized water mix, keep 2~2.5h, draining, add chlorination
Cuoxam, stir, soak 48~50h, leach molecular sieve, dry, it is 550~555 that temperature is controlled in nitrogen atmosphere
DEG C, molecular sieve is calcined 2~2.5h, is cooled to room temperature, copper-loaded lanthanum modified molecular screen is made；
3rd, by etc. quality step two obtained copper-loaded lanthanum modified molecular screen and nickel nitrate solution stir, soak 36~40h,
Molecular sieve is leached, is cleaned 3 times with demineralized water, molecular sieve is leached, is dried, it is 500~505 that temperature is controlled in nitrogen atmosphere
DEG C, molecular sieve is calcined 2~2.5h, is cooled to room temperature, obtains the compound copper-loaded lanthanum modified molecular screen of nickel, is completed a kind of for removing
The sorbent preparation method of benzyldithio toluene in insulating oil.
2. a kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil according to claim 1, its
It is characterised by that lanthanum nitrate hexahydrate is using the pure La of analysis in step 13(NO3)3·6H2O is prepared, concentration 0.12mol/L.
3. a kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil according to claim 1, its
It is characterised by step 1 that NaY types molecular sieve active porosity is 4nm~6nm.
4. a kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil according to claim 1, its
It is characterised by step 1 that drying temperature is 100 DEG C, drying time 6h.
5. a kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil according to claim 1, its
It is characterised by that copper ammonium chloride solution is using the pure (NH of analysis in step 24)2CuCl2·2H2O is prepared, concentration 0.20mol/L.
6. a kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil according to claim 1, its
It is characterised by step 2 that drying temperature is 120 DEG C, drying time 6h.
7. a kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil according to claim 1, its
It is characterised by that nickel nitrate solution is using the pure Ni NO of analysis in step 33·6H2O is prepared, concentration 0.15mol/L.
8. a kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil according to claim 1, its
It is characterised by step 3 that drying temperature is 100 DEG C, drying time 8h.
9. a kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil according to claim 1, its
When being characterised by being cleaned with demineralized water in step 3, demineralized water is cleaned in three times, the total dosage of demineralized water is molecular sieve quality
3 times.
10. a kind of sorbent preparation method for being used to remove benzyldithio toluene in insulating oil according to claim 1, its
The mass ratio for being characterised by copper ammonium chloride solution in NaY types molecular sieve, lanthanum nitrate hexahydrate and step 2 in step 1 is 1: 1: 1.
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| CN110157470A (en) * | 2019-05-29 | 2019-08-23 | 广东卓原新材料科技有限公司 | The removal methods of active sulfur in a kind of natural esters insulating oil |
| CN111662741A (en) * | 2020-06-18 | 2020-09-15 | 刘云 | Transformer capable of reducing sulfur corrosion |
| CN111760547A (en) * | 2020-07-08 | 2020-10-13 | 山东西奥生物科技有限公司 | Deep treatment process for natural ester insulating oil, super-hydrophilic adsorbent, preparation method and application thereof |
| CN113083226A (en) * | 2021-03-16 | 2021-07-09 | 湖北工程学院 | Preparation method of nano copper-loaded active molecular sieve and treatment method of transformer oil |
| CN115779845A (en) * | 2022-11-16 | 2023-03-14 | 贵州电网有限责任公司 | Composite modified adsorbent and preparation method and application thereof |
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| CN111662741A (en) * | 2020-06-18 | 2020-09-15 | 刘云 | Transformer capable of reducing sulfur corrosion |
| CN111662741B (en) * | 2020-06-18 | 2022-01-25 | 刘云 | Transformer capable of reducing sulfur corrosion |
| CN111760547A (en) * | 2020-07-08 | 2020-10-13 | 山东西奥生物科技有限公司 | Deep treatment process for natural ester insulating oil, super-hydrophilic adsorbent, preparation method and application thereof |
| CN111760547B (en) * | 2020-07-08 | 2023-05-09 | 山东西奥生物科技有限公司 | Deep treatment process of natural ester insulating oil, super-hydrophilic adsorbent, and preparation method and application thereof |
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