CN112691637A - Adsorbent for transformer oil and preparation method thereof - Google Patents
Adsorbent for transformer oil and preparation method thereof Download PDFInfo
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- CN112691637A CN112691637A CN202011528357.9A CN202011528357A CN112691637A CN 112691637 A CN112691637 A CN 112691637A CN 202011528357 A CN202011528357 A CN 202011528357A CN 112691637 A CN112691637 A CN 112691637A
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- adsorbent
- transformer oil
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- metal impurities
- acid solution
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000002253 acid Substances 0.000 claims abstract description 22
- 239000004927 clay Substances 0.000 claims abstract description 15
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 11
- 150000007524 organic acids Chemical class 0.000 claims description 11
- 239000003929 acidic solution Substances 0.000 claims description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 9
- 229960000892 attapulgite Drugs 0.000 claims description 9
- 229910052625 palygorskite Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 229910052902 vermiculite Inorganic materials 0.000 claims description 6
- 239000010455 vermiculite Substances 0.000 claims description 6
- 235000019354 vermiculite Nutrition 0.000 claims description 6
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 4
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 45
- 239000002184 metal Substances 0.000 abstract description 45
- 239000012535 impurity Substances 0.000 abstract description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 27
- 238000001179 sorption measurement Methods 0.000 abstract description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052802 copper Inorganic materials 0.000 abstract description 13
- 239000010949 copper Substances 0.000 abstract description 13
- 229910052742 iron Inorganic materials 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 7
- 238000000746 purification Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000000047 product Substances 0.000 description 11
- 239000010913 used oil Substances 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 4
- 125000003396 thiol group Chemical group [H]S* 0.000 description 4
- 239000010410 layer Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
Classifications
-
- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
-
- 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
- B01J20/28002—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 physical properties
Abstract
The application belongs to the technical field of oil purification for transformers. The application provides an adsorbent for transformer oil and a preparation method thereof, wherein a natural clay adsorbent is used as a raw material, and after the natural clay adsorbent is sequentially treated by an acid solution and a thioglycollic acid solution, the prepared adsorbent for transformer oil has a larger specific surface area, and the adsorption effect on metal impurities is enhanced. The preparation method disclosed by the application has the advantages that on one hand, the phenomenon that the performance of the transformer oil is affected by metal impurities dissolved out of an adsorption system is avoided, on the other hand, the technical problem that in the prior art, the adsorption capacity of the adsorbent for the transformer oil to the metal impurities is weak is solved, and the preparation method has the advantages of easiness in obtaining raw materials and simplicity in preparation process. The adsorbent for transformer oil prepared by the preparation method has no metal impurities dissolved out among layers, has a removal rate of iron, copper and other metal impurities close to 100%, and has a great application prospect in the field of purification of metal impurities in transformer oil.
Description
Technical Field
The application belongs to the technical field of oil purification for transformers, and particularly relates to an adsorbent for transformer oil and a preparation method thereof.
Background
The transformer oil has the characteristics of strong insulativity and good cooling property, and can play the roles of insulation, heat dissipation and arc extinction in the transformer. But along with transformer oil's ageing and pollution, can produce products such as acid and corrosive sulfur for metal components such as iron core and copper parts suffer the corruption in the transformer, and metallic impurity gets into transformer oil with the free state, thereby influences transformer oil's insulating nature and cooling nature, and transformer oil quality's reduction has undoubtedly buried great potential safety hazard to transformer and even whole power system's safe operation. Therefore, the treatment of metal impurities in transformer oil is not very gentle.
At present, the method for removing the metal impurities in the transformer oil is mainly an adsorption method, and the adsorption method generally has the advantages of low cost, high efficiency, easy industrialization and the like, and is suitable for the field of removing and purifying the metal impurities in the transformer oil. However, the existing adsorbing materials, such as activated clay, silica-alumina polymer, etc., are very easy to introduce other metal impurities during the removing process, such as a small amount of Na between activated clay layers+、Mg2+The oil is dissolved in the transformer oil during purification, and has negative influence on the transformer oil. In addition, in transformer oil, metal copper is widely used due to good conductivity, and metals such as iron and aluminum in the transformer are common metal materials in the transformer, and are partially dissolved in the transformer oil after multiple operations, so that the performance of the transformer oil is seriously affected.
Disclosure of Invention
In view of this, the application provides an adsorbent for transformer oil and a preparation method thereof, which can realize simultaneous and efficient adsorption of various metal impurities.
The specific technical scheme of the application is as follows:
the application provides a preparation method of an adsorbent for transformer oil, which comprises the following steps:
s1: washing and filtering a natural clay adsorbent in an acid solution;
s2: and stirring, filtering and drying the adsorbent obtained in the step S1 in an organic acid solution to obtain the adsorbent for the transformer oil.
In this application, adopt natural clay adsorbent as the raw materials, after acid solution and organic acid solution are handled in proper order, the adsorbent for transformer oil that the preparation obtained has bigger specific surface area, the reinforcing is to metallic impurity's adsorption. The preparation method disclosed by the application has the advantages that on one hand, the phenomenon that the performance of the transformer oil is affected by metal impurities dissolved out of an adsorption system is avoided, on the other hand, the technical problem that in the prior art, the adsorption capacity of the adsorbent for the transformer oil to the metal impurities is weak is solved, and the preparation method has the advantages of easiness in obtaining raw materials and simplicity in preparation process. The carboxyl in the organic acid solution and the hydroxyl in the adsorbent modified by the acidic solution are used for esterification bonding, so that the affinity effect of the adsorbent on metal ions and the adsorption effect of the pore structure on the metal ions are greatly enhanced.
Preferably, the acidic solution comprises one or more of hydrochloric acid, sulfuric acid and phosphoric acid;
the organic acid solution is a thioglycollic acid solution.
Preferably, the concentration of the solute in the acidic solution is 0.1-2 mol/L, and more preferably 0.5 mol/L;
the concentration of solute in the organic acid solution is 0.1-2 mol/L, and more preferably 1 mol/L.
Preferably, in the acidic solution, the molar ratio of the hydrochloric acid to the sulfuric acid is 1 (1-5), and the molar ratio of the hydrochloric acid to the phosphoric acid is 1 (1-6). More preferably, the molar ratio of hydrochloric acid to sulfuric acid is 1:3 and the molar ratio of hydrochloric acid to phosphoric acid is 1: 4.
Preferably, the dosage ratio of the natural clay adsorbent to the acidic solution in S1 is 1 g: (20-100) ml, more preferably 1 g: 50 ml;
the dosage ratio of the natural clay adsorbent to the organic acid solution in the S2 is 1 g: (30-100) ml, more preferably 1 g: 50 ml.
Preferably, the natural clay adsorbent is selected from at least one of attapulgite, vermiculite and montmorillonite. More preferably, the natural clay adsorbent is attapulgite.
Preferably, the washing in S1 is performed in an ultrasonic environment;
the time of the ultrasonic treatment is 1-4 h, more preferably 2h, and the frequency is 20-100 kHz, more preferably 50 kHz.
In the application, the adsorbent is ultrasonically washed in an acid solution, the specific surface area of the adsorbent can be increased, the adsorption effect of metal impurities among the adsorbents is effectively promoted, and compared with the existing acid leaching heating method, the metal impurity residue in the transformer oil is reduced.
Preferably, the stirring temperature in S2 is room temperature, the rotation speed is 60-200 r/min, more preferably 100r/min, and the time is 3-6 h, more preferably 4 h.
Preferably, the drying temperature in S2 is 80-120 ℃, more preferably 100 ℃, and the time is 6-12 h, more preferably 8 h.
The application also provides an adsorbent for transformer oil, which is prepared by the preparation method.
In the application, the adsorbent for transformer oil prepared by the preparation method has no metal impurities dissolved out from the interlayer, the removal rate of the metal impurities such as iron and copper is close to 100%, and the adsorbent has a great application prospect in the field of purification of the metal impurities in the transformer oil.
In summary, the application provides an adsorbent for transformer oil and a preparation method thereof. The natural clay adsorbent is used as a raw material and is sequentially treated by an acid solution and an organic acid solution, so that the prepared adsorbent for the transformer oil has a larger specific surface area, and the adsorption effect on metal impurities is enhanced. The preparation method disclosed by the application has the advantages that on one hand, the phenomenon that the performance of the transformer oil is affected by metal impurities dissolved out of an adsorption system is avoided, on the other hand, the technical problem that in the prior art, the adsorption capacity of the adsorbent for the transformer oil to the metal impurities is weak is solved, and the preparation method has the advantages of easiness in obtaining raw materials and simplicity in preparation process. The adsorbent for transformer oil prepared by the preparation method has no metal impurities dissolved out among layers, has a removal rate of iron, copper and other metal impurities close to 100%, and has a great application prospect in the field of purification of metal impurities in transformer oil.
Detailed Description
In order to make the objects, features and advantages of the present application more obvious and understandable, the technical solutions in the embodiments of the present application are clearly and completely described, and it is obvious that the embodiments described below are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The reagents and starting materials used in the examples of the present application are commercially available.
Example 1
(1) Carrying out ultrasonic washing on 1g of attapulgite in 50ml of a mixed solution of 0.0625mol/L hydrochloric acid, 0.1875mol/L sulfuric acid and 0.25mol/L phosphoric acid, wherein the ultrasonic frequency is 50kHz, the ultrasonic time is 2 hours, and filtering to obtain an acid modified adsorbent;
(2) adding the acid modified adsorbent into 50ml of 1mol/L thioglycollic acid solution, and stirring at the stirring speed of 100r/min at normal temperature for reacting for 4 hours to obtain the sulfhydryl modified adsorbent;
(3) filtering the sulfydryl modified adsorbent, and drying at 100 ℃ for 8 hours to obtain a finished product.
Respectively adding 1g of attapulgite, 1g of acid modified adsorbent and 1g of finished product into a wide-mouth bottle filled with 50ml of old oil containing metal impurities such as iron, copper and the like, carrying out oil bath at a constant temperature of 60 ℃, stirring for 2 hours, filtering and collecting filtrate, and carrying out metal content test, dielectric loss factor test and volume resistivity test.
Example 2
(1) Carrying out ultrasonic washing on 0.5g of attapulgite and 0.5g of montmorillonite in 70ml of a mixed solution of 0.0625mol/L hydrochloric acid, 0.2mol/L sulfuric acid and 0.25mol/L phosphoric acid, wherein the ultrasonic frequency is 60kHz, and the ultrasonic time is 1.5h, and filtering to obtain an acid modified adsorbent;
(2) adding the acid modified adsorbent into 60ml of 0.2mol/L thioglycollic acid solution, and stirring at the stirring speed of 150r/min at normal temperature for reaction for 3 hours to obtain the sulfhydryl modified adsorbent;
(3) filtering the sulfydryl modified adsorbent, and drying at 110 ℃ for 9 hours to obtain a finished product.
Respectively adding 0.5g of attapulgite, 0.5g of montmorillonite, 1g of acid modified adsorbent and 1g of finished product into a wide-mouth bottle filled with 50ml of old oil containing metal impurities such as iron, copper and the like, carrying out oil bath at a constant temperature of 60 ℃, stirring for 2h, filtering and collecting filtrate, and carrying out metal content test, medium loss factor test and volume resistivity test.
Example 3
(1) Carrying out ultrasonic washing on 1g of vermiculite in 60ml of a mixed solution of 0.1mol/L hydrochloric acid, 0.3mol/L sulfuric acid and 0.4mol/L phosphoric acid, wherein the ultrasonic frequency is 60kHz, the ultrasonic time is 1h, and filtering to obtain an acid modified adsorbent;
(2) adding the acid modified adsorbent into 50ml of 2mol/L thioglycollic acid solution, and stirring at the stirring speed of 120r/min at normal temperature for 5 hours to obtain the sulfhydryl modified adsorbent;
(3) filtering the sulfydryl modified adsorbent, and drying at 100 ℃ for 9 hours to obtain a finished product.
Respectively adding 1g of vermiculite, 1g of acid modified adsorbent and 1g of finished product into a wide-mouth bottle filled with 50ml of old oil containing metal impurities such as iron, copper and the like, carrying out oil bath at a constant temperature of 60 ℃, stirring for 2 hours, filtering and collecting filtrate, and carrying out metal content test, dielectric loss factor test and volume resistivity test.
Example 4
(1) Ultrasonic washing 0.8g of attapulgite and 0.2g of vermiculite in 60ml of 0.1mol/L hydrochloric acid, 0.3mol/L sulfuric acid and 0.2mol/L phosphoric acid solution, wherein the ultrasonic frequency is 90kHz, and the ultrasonic time is 2 hours, and filtering to obtain an acid modified adsorbent;
(2) adding the acid modified adsorbent into 40ml of 0.5mol/L thioglycollic acid solution, and stirring at the stirring speed of 130r/min at normal temperature for 5 hours to obtain the sulfhydryl modified adsorbent;
(3) filtering the sulfydryl modified adsorbent, and drying at 120 ℃ for 8 hours to obtain a finished product.
Respectively adding 0.8g of attapulgite, 0.2g of vermiculite, 1g of acid modified adsorbent and 1g of finished product into a wide-mouth bottle filled with 50ml of old oil containing metal impurities such as iron, copper and the like, carrying out oil bath at a constant temperature of 60 ℃, stirring for 2h, filtering and collecting filtrate, and carrying out metal content test, medium loss factor test and volume resistivity test.
The transformer oil contains more metal impurities, and the copper content and the iron content in the transformer oil are detected by using a spectrophotometry, taking the metal copper with the largest content and the metal iron which is difficult to remove as examples. The metal content test results of examples 1-4 are shown in tables 1-4 below, wherein the used oil is obtained from the used transformer oil in the same batch.
The test results in tables 1-4 show that the removal rate of the natural adsorbent to metal impurities such as iron and copper is lower than 40%, and part of the metal impurities are dissolved out. The removal rate of the acid modified adsorbent to metal impurities such as iron, copper and the like is close to 70 percent. The removal rate of the finished product prepared by esterifying and bonding carboxyl in thioglycolic acid and hydroxyl in the acid modified adsorbent to metal impurities such as iron and copper is close to 100%, which shows that the adsorbent for transformer oil obtained by the preparation method has stronger adsorption effect on the metal impurities, and other metal impurities cannot be introduced between the adsorbent layers.
Table 1 example 1 test results of adsorbent treatment of used oil
Table 2 example 2 test results of adsorbent treatment of used oil
Table 3 example 3 test results of adsorbent treatment of used oil
Table 4 example 4 test results of adsorbent treatment of used oil
The dielectric loss factor and volume resistivity test results of the old transformer oil before and after the old transformer oil is treated by the finished product adsorbent in examples 1-4 are shown in table 5 below, wherein the old transformer oil is obtained from the old transformer oil used in the same batch. The presence of metallic impurities in transformer oil causes an increase in dielectric loss factors and a decrease in volume resistivity in the transformer oil. The test results in table 5 show that the adsorbent prepared by the preparation method of the application has excellent adsorption effect, the dielectric loss factor is remarkably reduced after the old oil of the transformer is purified, the volume resistivity is remarkably increased, and the purification purpose is achieved.
TABLE 5 dielectric loss factor and volume resistivity test results for old transformer oil before and after treatment with the finished adsorbents of examples 1-4
The above embodiments are only used for illustrating the technical solutions of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions in the embodiments of the present application.
Claims (10)
1. The preparation method of the adsorbent for the transformer oil is characterized by comprising the following steps of:
s1: ultrasonically washing and filtering a natural clay adsorbent in an acid solution;
s2: and stirring, filtering and drying the adsorbent obtained in the step S1 in an organic acid solution to obtain the adsorbent for the transformer oil.
2. The method of claim 1, wherein the acidic solution comprises one or more of hydrochloric acid, sulfuric acid, and phosphoric acid;
the organic acid solution is a thioglycollic acid solution.
3. The preparation method according to claim 1, wherein the concentration of the solute in the acidic solution is 0.1 to 2 mol/L;
the concentration of solute in the organic acid solution is 0.1-2 mol/L.
4. The method according to claim 2, wherein the acidic solution contains hydrochloric acid and sulfuric acid at a molar ratio of 1 (1-5) and phosphoric acid at a molar ratio of 1 (1-6).
5. The method according to claim 1, wherein the amount ratio of the natural clay adsorbent to the acidic solution in S1 is 1 g: (20-100) ml;
the dosage ratio of the natural clay adsorbent to the organic acid solution in the S2 is 1 g: (30-100) ml.
6. The method of claim 1, wherein the natural clay adsorbent is selected from at least one of attapulgite, vermiculite and montmorillonite.
7. The method according to claim 1, wherein the washing in S1 is performed in an ultrasonic environment;
the ultrasonic time is 1-4 h, and the frequency is 20-100 kHz.
8. The preparation method according to claim 1, wherein the stirring in S2 is performed at room temperature and at a rotation speed of 60-200 r/min for 3-6 h.
9. The method according to claim 1, wherein the drying in S2 is carried out at 80-120 ℃ for 6-12 h.
10. An adsorbent for transformer oil, characterized by being prepared by the preparation method of any one of claims 1 to 9.
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Application publication date: 20210423 |