CN115138335A - Modified molecular sieve and preparation method and application thereof - Google Patents
Modified molecular sieve and preparation method and application thereof Download PDFInfo
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- CN115138335A CN115138335A CN202210899626.5A CN202210899626A CN115138335A CN 115138335 A CN115138335 A CN 115138335A CN 202210899626 A CN202210899626 A CN 202210899626A CN 115138335 A CN115138335 A CN 115138335A
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- 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
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/0008—Working-up used lubricants to recover useful products ; Cleaning with the use of adsorbentia
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/0083—Lubricating greases
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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Abstract
The invention discloses a modified molecular sieve and a preparation method and application thereof, and belongs to wind power gear oil purification treatment. Dipping a 13X molecular sieve in nitric acid, then placing the dipped molecular sieve in a muffle furnace for calcination, and carrying out acid treatment and hole expansion; preparing an ethylene diamine tetraacetic acid solution as a complexing agent and a sodium alginate solution as a cross-linking agent; and (3) soaking the reamed 13X molecular sieve in a prepared ethylene diamine tetraacetic acid solution, adding a sodium alginate solution, fully stirring, carrying out hydrothermal reaction, and drying the obtained product to obtain the final modified 13X molecular sieve adsorbent. The adsorbent is applied to the removal of metal impurity elements in the gear oil of the wind driven generator, the whole synthesis process is simple and efficient, the operation is easy, the adsorbent is suitable for large-scale production, the difficulty that the combined metal impurity elements in the existing wind power gear oil cannot be effectively removed through a physical method is broken through, and the adsorbent can effectively remove iron elements in the wind power gear oil, so that the reliable and stable long-period operation of wind driven generator equipment is ensured.
Description
Technical Field
The invention belongs to the technical field of wind power gear oil purification treatment, and particularly relates to a modified molecular sieve and a preparation method and application thereof.
Background
With the continuous development and maturity of science and technology, wind power generation has become a hot spot of the world new energy industry as a power generation mode of clean renewable energy. As wind driven generator equipment is expensive in manufacturing cost and bad in working environment, main parts are inconvenient to disassemble and maintain on site, the lubricating performance of oil products is reduced along with the increase of the running time of a fan, the transmission of motion and power is completed in the interaction and relative motion of each pair of meshing tooth surfaces in a gear mechanism, friction is necessarily generated between the motion and the power, tiny metal abrasive particles are generated, and the stable structure of a gear is damaged, so that very strict requirements are provided for the performance of the gear oil which plays a role in lubricating in the running system of the wind driven generator. The gear oil used not only has excellent extreme pressure antiwear performance, cooling performance and cleaning performance, but also has good thermal oxidation stability, low temperature performance and long service life, and simultaneously has lower friction coefficient to reduce power loss in gear transmission so as to ensure reliable and stable long-period operation of equipment.
The recovery and regeneration of the waste oil are one of effective measures for saving resources, magnetic iron particles or iron oxides in the waste gear oil can be adsorbed by a magnetic filter, but iron elements existing in a non-magnetic combined state cannot be filtered by a physical mechanical method, which brings great difficulty to the recovery and reuse of the waste gear oil. Therefore, it is very important to develop a novel adsorbent for adsorbing and removing iron element from wind power gear oil.
Disclosure of Invention
In order to overcome the defect that the waste gear oil is difficult to recycle in the prior art, the invention aims to provide a modified molecular sieve, a preparation method and application thereof, which are used for solving the technical problem that combined metal impurity elements in the existing wind power gear oil cannot be effectively removed by physical methods such as mechanical filtration and magnetic filtration; the modified molecular sieve adsorbent provided by the invention realizes the removal of metallic iron element in gear oil through a complex reaction between the adsorbent and metallic ions.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention provides a preparation method of a modified molecular sieve adsorbent, which comprises the following steps:
s1: carrying out acid treatment, calcining and hole expanding on the 13X molecular sieve;
s2: soaking the reamed 13X molecular sieve in an ethylenediamine tetraacetic acid solution serving as a complexing agent, adding a sodium alginate solution serving as a crosslinking agent, fully stirring, and placing in a reaction kettle for hydrothermal reaction;
s3: and after the hydrothermal reaction is finished, cooling the reaction kettle to room temperature, and drying the obtained product to obtain the modified molecular sieve adsorbent.
Further, in the step S1, the acid treatment, calcination and hole expansion process comprises the steps of immersing the 13X molecular sieve in nitric acid and then calcining; the concentration of the nitric acid is 1% -2%, the dipping time is 1-3 h, and the dosage ratio of the 13X molecular sieve to the nitric acid is 1g: (10-30) mL.
Further to the invention, the calcination is carried out in a muffle furnace; the calcining temperature is 400-500 ℃, and the calcining time is 2-3 h.
Further, in the step S2, the preparation process of the ethylenediaminetetraacetic acid solution is as follows: dissolving ethylene diamine tetraacetic acid in deionized water, and uniformly stirring at room temperature until the solution is clear to prepare an ethylene diamine tetraacetic acid solution;
the concentration of the ethylene diamine tetraacetic acid solution is 10-30%.
Further, in the step S2, the preparation process of the sodium alginate solution is as follows: dissolving sodium alginate in deionized water, and stirring at room temperature to obtain sodium alginate solution;
the concentration of the sodium alginate solution is 1-2%.
Further, the reaction kettle in the S2 is a polytetrafluoroethylene reaction kettle.
Further, in the step S2, the stirring time is 1-3 hours; the temperature of the hydrothermal reaction is 140-160 ℃, and the time of the hydrothermal reaction is 2-4 h.
In the step S3, the drying temperature is 50-70 ℃, and the drying time is 8-12 h.
A modified molecular sieve adsorbent obtained by the preparation method of any one of the above.
The modified molecular sieve adsorbent obtained by any one of the preparation methods is applied to the purification treatment of wind power gear oil.
Compared with the prior art, the invention has the following beneficial effects:
the invention firstly adopts the 13X molecular sieve as the adsorbent, and the adsorbent has low price, better ion exchange performance and easy cation exchange modification. Compared with adsorbents such as silica gel and activated alumina, the 13X molecular sieve used for the adsorbent has the characteristics of higher specific surface area, abundant pore volume, large amount of compensation cations on the surface, ionic conductivity and the like, so that the 13X molecular sieve is superior to other adsorbents. Then, sodium alginate is added as a cross-linking agent, and the cross-linking agent has good solubility, low toxicity and biocompatibility, can firmly combine Ethylene Diamine Tetraacetic Acid (EDTA) with the 13X molecular sieve, enhances the adsorbability of the molecular sieve, and effectively improves the removal efficiency. And then, the 13X molecular sieve is modified by using Ethylene Diamine Tetraacetic Acid (EDTA), the EDTA has six coordination atoms, can generate a complexing reaction with metallic iron elements to generate iron-containing precipitates, has extremely strong complexing capability on the metallic ions, and can effectively remove the metallic iron elements in the oil. The method provided by the invention can be used for carrying out acid treatment, calcination and hole expansion on the 13X molecular sieve, so that the aperture is increased, the mass transfer diffusion capacity of the molecular sieve is enhanced, and the load of the 13X molecular sieve loaded with EDTA is improved, thereby effectively removing the metallic iron element in oil.
The modified molecular sieve prepared by the preparation method solves the difficulty that the bound metal impurity elements in the existing wind power gear oil can not be effectively removed by physical methods such as mechanical filtration, magnetic filtration and the like, and realizes the removal of metal iron elements in the gear oil by the complexation reaction between the adsorbent and metal ions.
The modified molecular sieve adsorbent is applied to removing metal impurity elements in the gear oil of the wind driven generator, the whole preparation process is simple and efficient, the operation is easy, and the modified molecular sieve adsorbent is suitable for large-scale production, and can effectively remove iron elements in the gear oil of the wind driven generator, so that the reliable and stable long-period operation of equipment of the wind driven generator set is ensured.
Detailed Description
To make the features and effects of the present invention comprehensible to those skilled in the art, general description and definitions are made below with reference to terms and expressions mentioned in the specification and claims. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The theory or mechanism described and disclosed herein, whether correct or incorrect, should not limit the scope of the present invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features defined herein as numerical ranges or percentage ranges, such as values, amounts, levels and concentrations, are for brevity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to cover and specifically disclose all possible subranges and individual numerical values (including integers and fractions) within the range.
In this document, unless otherwise specified, "comprising," including, "" containing, "" having, "or the like, means" consisting of … … "and" consisting essentially of … …, "e.g.," a comprises a "means" a comprises a and the other "and" a comprises a only.
In this context, for the sake of brevity, not all possible combinations of features in the various embodiments or examples are described. Therefore, the respective features in the respective embodiments or examples may be arbitrarily combined as long as there is no contradiction between the combinations of the features, and all the possible combinations should be considered as the scope of the present specification.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Instrumentation conventional in the art is used in the following examples. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out under conventional conditions or conditions recommended by the manufacturers. The various starting materials used in the examples which follow, unless otherwise indicated, are conventional commercial products having specifications which are conventional in the art. In the description of the present invention and the following examples, "%" represents weight percent, "parts" represents parts by weight, and proportions represent weight ratios, unless otherwise specified.
The preparation method of the modified molecular sieve adsorbent comprises the following steps:
s1: dipping a 13X molecular sieve in nitric acid, then placing the dipped molecular sieve in a muffle furnace for calcination, and performing acid treatment, calcination and hole expansion;
the concentration of nitric acid is 1-2%, the dipping time is 1-3h, and the dosage ratio of 13X molecular sieve to nitric acid is 1g: (10-30) mL; the calcining treatment is carried out in a muffle furnace for calcining, the calcining temperature is 400-500 ℃, and the calcining time is 2-3 h.
The invention adopts the 13X molecular sieve as the adsorbent, has higher specific surface area, abundant pore volume, a large amount of compensation cations on the surface, ionic conductivity and the like, and has excellent adsorption performance.
S2: weighing ethylene diamine tetraacetic acid EDTA, dissolving the ethylene diamine tetraacetic acid EDTA in deionized water, uniformly stirring the mixture at room temperature until the mixture is clear, and preparing an ethylene diamine tetraacetic acid EDTA solution as a complexing agent;
the concentration of the prepared EDTA solution is 10-30%.
The 13X molecular sieve is modified by using the EDTA, the EDTA can generate a complexing reaction with the iron element to generate an iron-containing precipitate, the complexing agent has strong complexing ability on metal ions, and the metal iron element in the oil can be effectively removed.
S3: weighing sodium alginate, dissolving in deionized water, stirring at room temperature, and preparing sodium alginate solution as crosslinking agent.
The concentration of the prepared sodium alginate solution is 1 to 2 percent.
According to the invention, sodium alginate is selected as a cross-linking agent, so that EDTA and the 13X molecular sieve can be firmly combined, the adsorbability of the modified molecular sieve is enhanced, and the removal efficiency is effectively improved.
According to the invention, the 13X molecular sieve is subjected to pore-expanding treatment by acid treatment and calcination, so that the mass transfer diffusion capacity of the molecular sieve is enhanced, and the load capacity of the molecular sieve loaded with an EDTA complexing agent is improved, thereby effectively removing metallic iron element in oil.
S4: and (3) soaking the reamed 13X molecular sieve in a prepared Ethylene Diamine Tetraacetic Acid (EDTA) solution, adding a sodium alginate solution, fully stirring, and placing in a polytetrafluoroethylene reaction kettle for hydrothermal reaction.
The stirring time is 1-3 h, the temperature of the hydrothermal reaction is 140-160 ℃, and the reaction time is 2-4 h.
S5: and after the hydrothermal reaction is finished, cooling the reaction kettle to room temperature, and drying the obtained product to obtain the final treatment modified 13X molecular sieve adsorbent.
The drying temperature is 50-70 ℃ after the hydrothermal reaction is finished, and the drying time is 8-12 h.
The prepared modified 13X molecular sieve adsorbent is applied to the removal of metallic iron elements in wind power gear oil.
The technical solution of the present invention is further described in detail by the following specific examples.
Example 1
The preparation method of the lithium ion battery negative electrode material comprises the following steps:
the method comprises the following steps: dipping 10g 13X molecular sieve in 100mL 1% nitric acid for 1h, then placing the molecular sieve in a muffle furnace, calcining at 400 ℃ for 3h, and carrying out acid treatment and hole expansion;
step two: weighing EDTA, dissolving in deionized water, stirring at room temperature to clarify, and making into 10% EDTA solution as complexing agent;
step three: weighing sodium alginate, dissolving the sodium alginate in deionized water, stirring the solution uniformly at room temperature, and preparing a 1% sodium alginate solution as a cross-linking agent;
step four: soaking the reamed 13X molecular sieve in a prepared ethylene diamine tetraacetic acid solution, adding a sodium alginate solution, stirring for 1h, and placing the mixture in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at 140 ℃ for 4h;
step five: and after the hydrothermal reaction is finished, cooling the reaction kettle to room temperature, and drying the obtained product in an oven at 50 ℃ for 12 hours to obtain the final treatment modified 13X molecular sieve adsorbent.
Example 2
The method comprises the following steps: dipping 10g 13X molecular sieve in 100mL 2% nitric acid for 1h, then placing the molecular sieve in a muffle furnace, calcining at 400 ℃ for 3h, and carrying out acid treatment and hole expansion;
step two: weighing EDTA, dissolving in deionized water, stirring at room temperature to clarify, and preparing 30% EDTA solution as complexing agent;
step three: weighing sodium alginate, dissolving the sodium alginate in deionized water, uniformly stirring at room temperature, and preparing a 2% sodium alginate solution as a cross-linking agent;
step four: soaking the reamed 13X molecular sieve in a prepared ethylene diamine tetraacetic acid solution, adding a sodium alginate solution, stirring for 1h, and placing the mixture in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at 140 ℃ for 4h;
step five: and after the hydrothermal reaction is finished, cooling the reaction kettle to room temperature, and drying the obtained product in an oven at 50 ℃ for 12 hours to obtain the finally treated and modified 13X molecular sieve adsorbent.
Example 3
The method comprises the following steps: dipping 10g 13X molecular sieve in 100mL 1% nitric acid for 1h, then placing the molecular sieve in a muffle furnace, calcining for 2h at 500 ℃, and carrying out acid treatment and hole expansion;
step two: weighing EDTA, dissolving in deionized water, stirring at room temperature to clarify, and preparing 10% EDTA solution as complexing agent;
step three: weighing sodium alginate, dissolving the sodium alginate in deionized water, stirring the solution uniformly at room temperature, and preparing a 1% sodium alginate solution as a cross-linking agent;
step four: soaking the reamed 13X molecular sieve in a prepared ethylene diamine tetraacetic acid solution, adding a sodium alginate solution, stirring for 1h, and placing in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at 160 ℃ for 2h;
step five: and after the hydrothermal reaction is finished, cooling the reaction kettle to room temperature, and drying the obtained product in an oven at 70 ℃ for 8 hours to obtain the finally treated and modified 13X molecular sieve adsorbent.
Example 4
The method comprises the following steps: dipping 10g 13X molecular sieve in 100mL 1% nitric acid for 2h, then placing the molecular sieve in a muffle furnace, calcining for 2.5h at 450 ℃, and carrying out acid treatment and hole expansion;
step two: weighing EDTA, dissolving in deionized water, stirring at room temperature to clarify, and preparing 20% EDTA solution as complexing agent;
step three: weighing sodium alginate, dissolving the sodium alginate in deionized water, stirring the solution uniformly at room temperature, and preparing a 1% sodium alginate solution as a cross-linking agent;
step four: soaking the reamed 13X molecular sieve in a prepared ethylene diamine tetraacetic acid solution, adding a sodium alginate solution, stirring for 2 hours, and placing the mixture in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at 150 ℃ for 3 hours;
step five: and after the hydrothermal reaction is finished, cooling the reaction kettle to room temperature, and drying the obtained product in an oven at 60 ℃ for 10 hours to obtain the final treatment modified 13X molecular sieve adsorbent.
Example 5
The method comprises the following steps: soaking a 20g 13X molecular sieve in 200mL of 1% nitric acid for 3 hours, then placing the molecular sieve in a muffle furnace, calcining for 3 hours at the temperature of 400 ℃, and performing acid treatment and hole expansion;
step two: weighing EDTA, dissolving in deionized water, stirring at room temperature to clarify, and concocting with 20% EDTA solution as complexing agent;
step three: weighing sodium alginate, dissolving the sodium alginate in deionized water, stirring the solution uniformly at room temperature, and preparing a 1% sodium alginate solution as a cross-linking agent;
step four: soaking the reamed 13X molecular sieve in a prepared ethylene diamine tetraacetic acid solution, adding a sodium alginate solution, stirring for 2 hours, and placing in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at 150 ℃ for 3 hours;
step five: and after the hydrothermal reaction is finished, cooling the reaction kettle to room temperature, and drying the obtained product in an oven at 60 ℃ for 10 hours to obtain the final treatment modified 13X molecular sieve adsorbent.
Example 6
The method comprises the following steps: dipping 10g 13X molecular sieve in 300mL of 2% nitric acid for 1h, then placing the molecular sieve in a muffle furnace, calcining for 2h at 500 ℃, and carrying out acid treatment and hole expansion;
step two: weighing EDTA, dissolving in deionized water, stirring at room temperature to clarify, and preparing 20% EDTA solution as complexing agent;
step three: weighing sodium alginate, dissolving the sodium alginate in deionized water, uniformly stirring at room temperature, and preparing a 1% sodium alginate solution as a cross-linking agent;
step four: soaking the reamed 13X molecular sieve in a prepared ethylene diamine tetraacetic acid solution, adding a sodium alginate solution, stirring for 2 hours, and placing the mixture in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at 160 ℃ for 2 hours;
step five: and after the hydrothermal reaction is finished, cooling the reaction kettle to room temperature, and drying the obtained product in an oven at 50 ℃ for 12 hours to obtain the final treatment modified 13X molecular sieve adsorbent.
Example 7
The method comprises the following steps: dipping a 10g 13X molecular sieve in 200mL of 2% nitric acid for 1h, then placing the molecular sieve in a muffle furnace, calcining for 2h at 500 ℃, and carrying out acid treatment and hole expansion;
step two: weighing EDTA, dissolving in deionized water, stirring at room temperature to clarify, and preparing 20% EDTA solution as complexing agent;
step three: weighing sodium alginate, dissolving the sodium alginate in deionized water, stirring the solution uniformly at room temperature, and preparing a 1% sodium alginate solution as a cross-linking agent;
step four: soaking the reamed 13X molecular sieve in a prepared ethylene diamine tetraacetic acid solution, adding a sodium alginate solution, stirring for 2 hours, and placing the mixture in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at 160 ℃ for 3 hours;
step five: and after the hydrothermal reaction is finished, cooling the reaction kettle to room temperature, and drying the obtained product in an oven at 50 ℃ for 12 hours to obtain the final treatment modified 13X molecular sieve adsorbent.
Example 8
The method comprises the following steps: dipping 10g 13X molecular sieve in 250mL 1.5% nitric acid for 1h, then placing the molecular sieve in a muffle furnace, calcining for 2h at 500 ℃, and carrying out acid treatment and hole expansion;
step two: weighing EDTA, dissolving in deionized water, stirring at room temperature to clarify, and preparing 20% EDTA solution as complexing agent;
step three: weighing sodium alginate, dissolving the sodium alginate in deionized water, uniformly stirring at room temperature, and preparing a 1% sodium alginate solution as a cross-linking agent;
step four: soaking the reamed 13X molecular sieve in a prepared ethylene diamine tetraacetic acid solution, adding a sodium alginate solution, stirring for 3 hours, and placing in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at 155 ℃ for 4 hours;
step five: and after the hydrothermal reaction is finished, cooling the reaction kettle to room temperature, and drying the obtained product in an oven at 50 ℃ for 12 hours to obtain the final treatment modified 13X molecular sieve adsorbent.
The modified molecular sieve adsorbent prepared by the preparation method is applied to the removal of metallic iron elements in wind power gear oil, solves the difficulty that combined metallic impurity elements in the wind power gear oil cannot be effectively removed by physical methods such as mechanical filtration and magnetic filtration at present, and realizes the removal of the metallic iron elements in the gear oil by the complexation reaction between the adsorbent and the metallic ions.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. The preparation method of the modified molecular sieve adsorbent is characterized by comprising the following steps:
s1: carrying out acid treatment on the 13X molecular sieve, calcining and reaming;
s2: soaking the reamed 13X molecular sieve in an ethylenediamine tetraacetic acid solution serving as a complexing agent, adding a sodium alginate solution serving as a crosslinking agent, fully stirring, and placing in a reaction kettle for hydrothermal reaction;
s3: and after the hydrothermal reaction is finished, cooling the reaction kettle to room temperature, and drying the obtained product to obtain the modified molecular sieve adsorbent.
2. The preparation method according to claim 1, wherein in S1, the acid treatment calcination pore expansion process comprises immersing a 13X molecular sieve in nitric acid and then calcining; the concentration of the nitric acid is 1% -2%, the dipping time is 1-3 h, and the dosage ratio of the 13X molecular sieve to the nitric acid is 1g: (10-30) mL.
3. The method according to claim 2, wherein the calcination is performed in a muffle furnace; the calcining temperature is 400-500 ℃, and the calcining time is 2-3 h.
4. The method according to claim 1, wherein in the step S2, the edta solution is prepared by: dissolving ethylenediamine tetraacetic acid in deionized water, and stirring at room temperature to be clear to prepare an ethylenediamine tetraacetic acid solution;
the concentration of the ethylene diamine tetraacetic acid solution is 10-30%.
5. The preparation method of claim 1, wherein in the step S2, the sodium alginate solution is prepared by: dissolving sodium alginate in deionized water, and stirring at room temperature to obtain sodium alginate solution;
the concentration of the sodium alginate solution is 1-2%.
6. The method according to claim 1, wherein the reaction vessel in S2 is a polytetrafluoroethylene reaction vessel.
7. The preparation method according to claim 1, wherein in the step S2, the stirring time is 1 to 3 hours; the temperature of the hydrothermal reaction is 140-160 ℃, and the time of the hydrothermal reaction is 2-4 h.
8. The method according to claim 1, wherein the drying temperature in S3 is 50 to 70 ℃ and the drying time is 8 to 12 hours.
9. A modified molecular sieve adsorbent obtained by the production method according to any one of claims 1 to 8.
10. Use of a modified molecular sieve adsorbent obtained by the preparation method of any one of claims 1 to 8 in the purification treatment of wind power gear oil.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006272144A (en) * | 2005-03-29 | 2006-10-12 | Sumitomo Osaka Cement Co Ltd | Heavy metal insolubilizing material and method of treating heavy metal |
| CN101890337A (en) * | 2010-08-02 | 2010-11-24 | 长春理工大学 | Metal ion nanoadsorbent |
| CN103769033A (en) * | 2014-01-27 | 2014-05-07 | 北京工业大学 | Preparation method and application of modified zeolite permeable reactive wall filling carrying zero-valent iron powder |
| WO2016187796A1 (en) * | 2015-05-21 | 2016-12-01 | 江南大学 | Preparation method and use of heavy metal ion adsorbent |
| CN113430044A (en) * | 2021-07-23 | 2021-09-24 | 西安热工研究院有限公司 | Method for removing metal impurity elements in wind power gear oil |
-
2022
- 2022-07-28 CN CN202210899626.5A patent/CN115138335A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006272144A (en) * | 2005-03-29 | 2006-10-12 | Sumitomo Osaka Cement Co Ltd | Heavy metal insolubilizing material and method of treating heavy metal |
| CN101890337A (en) * | 2010-08-02 | 2010-11-24 | 长春理工大学 | Metal ion nanoadsorbent |
| CN103769033A (en) * | 2014-01-27 | 2014-05-07 | 北京工业大学 | Preparation method and application of modified zeolite permeable reactive wall filling carrying zero-valent iron powder |
| WO2016187796A1 (en) * | 2015-05-21 | 2016-12-01 | 江南大学 | Preparation method and use of heavy metal ion adsorbent |
| CN113430044A (en) * | 2021-07-23 | 2021-09-24 | 西安热工研究院有限公司 | Method for removing metal impurity elements in wind power gear oil |
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