CN113430044A - Method for removing metal impurity elements in wind power gear oil - Google Patents

Method for removing metal impurity elements in wind power gear oil Download PDF

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Publication number
CN113430044A
CN113430044A CN202110838011.7A CN202110838011A CN113430044A CN 113430044 A CN113430044 A CN 113430044A CN 202110838011 A CN202110838011 A CN 202110838011A CN 113430044 A CN113430044 A CN 113430044A
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China
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gear oil
metal impurity
wind power
impurity elements
alcohol
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CN202110838011.7A
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Chinese (zh)
Inventor
谢佳林
刘永洛
王腾
封强锁
唐金伟
付龙飞
常治军
严涛
王笑微
王娟
冯丽苹
李光明
刘晓莹
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Xian Thermal Power Research Institute Co Ltd
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Xian Thermal Power Research Institute Co Ltd
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Priority to CN202110838011.7A priority Critical patent/CN113430044A/en
Publication of CN113430044A publication Critical patent/CN113430044A/en
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M175/00Working-up used lubricants to recover useful products ; Cleaning
    • C10M175/0016Working-up used lubricants to recover useful products ; Cleaning with the use of chemical agents

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

A method for removing metallic impurity elements from gear oil of wind driven generator includes such steps as mixing metallic impurity remover, alcohol-water cosolvent and reaction-removing promoter to obtain mixed solvent, adding it to the waste gear oil to be treated, reacting at 60-100 deg.C for 30-120 min to obtain oleophobic product, depositing the oleophobic product by silica gel particles, and filtering. The metal impurity remover, the alcohol-water cosolvent and the removal reaction promoter used in the method have the advantages of low consumption, low cost and convenient transportation and storage; the removing method is simple and reliable, is easy to operate, can efficiently remove metal impurity elements such as iron element, copper element and the like in the wind power gear oil, has no influence on other indexes of oil products, and can effectively improve the safety and stability of the operation of the wind generating set.

Description

Method for removing metal impurity elements in wind power gear oil
Technical Field
The invention belongs to the technical field of wind power gear oil purification treatment, and particularly relates to a method for removing metal impurity elements in wind power gear oil.
Background
In the long-time running process of the wind driven generator, the gear of the gearbox can not be abraded inevitably, and the abrasion is mainly caused by the movement of materials between sliding tooth surfaces. Along with the increase of the running time of the fan, the lubricating performance of an oil product is reduced, when the pressure born by the oil film thickness of gear oil is smaller than the occlusion pressure of the gears, metal parts between the gears can be in direct contact to generate tiny metal abrasive particles, and meanwhile, the stable structure of the gears can be damaged; in addition, various mechanical impurity particles can be mixed into the gear oil during long-term operation of the fan. The bearing capacity of the gear oil can be greatly reduced by the tiny metal abrasive particles and the mechanical impurity particles generated by gear friction, meanwhile, the bearing capacity is also used as an abrasive material, the abrasion of the gear is accelerated, if the abrasion lasts all the time, the structural strength of metal parts can be influenced, even the faults of tooth clamping and tooth breaking occur, and the safe and stable operation of the wind turbine generator is seriously influenced.
The main components of the main gearbox of the wind power generation equipment are iron and copper elements, so that the contents of the iron element and the copper element are typical representative elements for judging the internal wear condition of the gearbox. Magnetic metal impurities such as tiny metal particles in the gearbox gear oil, iron particles and the like can be removed through the magnetic filter, but the magnetic filter has no removal effect on nonmagnetic metal particles, such as ferric oxide, ferrous oxide and the like. In addition, because wind driven generators are often installed in areas with harsh environmental conditions, the gear oil is easily deteriorated and deteriorated due to large temperature change of the working environment of the gear box, large coastal humidity, large torsional load and instability of the load, and aging products such as oxides, aldehydes, acids, hydroxy acids and the like are generated. Various aging products easily generate stable compounds with metal impurities in oil in the presence of oil micro water and in a high-temperature environment when tooth surfaces are abraded, and the compounds can be gradually crosslinked to generate oil sludge along with the prolonging of time, so that the lubricating and heat conducting properties of the gear oil are seriously reduced, the color of the gear oil is deepened, and the service life of the oil product is influenced.
In recent years, China vigorously develops new energy, wherein the wind power generation proportion is high, and therefore the reserve of wind power generation gear oil is quite large. With the increase of the running time of the fan, the quantity of the waste gear oil in China is rapidly increased. The recovery and regeneration of waste oil are one of measures for effectively saving resources, and are also effective ways for preventing environmental pollution, but metal impurity elements existing in a combined state in wind power gear oil cannot be filtered by a physical mechanical method, and cannot be adsorbed by a magnetic filter, which brings great difficulty to the recovery and utilization of the waste gear oil, so that a new method for removing the metal impurity elements of the waste gear oil is urgently needed.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a method for removing metal impurity elements in wind power gear oil.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for removing metallic impurity elements from gear oil of wind driven generator includes such steps as mixing metallic impurity remover, alcohol-water cosolvent and reaction-removing promoter to obtain mixed solvent, adding it to the waste gear oil to be treated, reacting at 60-100 deg.C for 30-120 min to obtain oleophobic product, depositing the oleophobic product by silica gel particles, and filtering.
The invention further improves the following steps: the metal impurity remover is disodium ethylene diamine tetraacetate.
The invention further improves the following steps: the dosage of the metal impurity remover is 0.1-4% of the mass of the waste gear oil.
The invention further improves the following steps: the alcohol-water cosolvent is a mixture of alcohol with 2-5 carbon atoms and water, wherein the volume concentration of the alcohol is 5% -100%.
The invention further improves the following steps: the dosage of the alcohol-water cosolvent is 3-5 times of the mass of the metal impurity remover.
The invention further improves the following steps: the removal reaction promoter is heptanoic acid.
The invention further improves the following steps: the dosage of the removal reaction accelerant is 0.05 to 2 percent of the mass of the waste gear oil.
The invention further improves the following steps: the dosage of the silica gel particles is 1 to 10 percent of the mass of the waste gear oil, and the diameter of the silica gel particles is 50 to 100 mu m.
The invention further improves the following steps: the settling time is 2-5 hours.
The invention further improves the following steps: the filtration is carried out by adopting pressure-resistant filter cloth with the aperture size of 5um-25 um.
Compared with the prior art, the invention has the following beneficial effects:
the method breaks through the difficulty that bound metal impurity elements in the wind power gear oil cannot be effectively removed by physical methods such as mechanical filtration, magnetic filtration and the like, and realizes the removal of the metal impurity elements in the wind power gear oil by the extremely strong chelating capacity of the metal impurity remover on metal ions. The metal impurity remover, the alcohol-water cosolvent and the removal reaction promoter used in the method have the advantages of low consumption, low cost and convenient transportation and storage; the removing method is simple and reliable, is easy to operate, can efficiently remove metal impurity elements such as iron element, copper element and the like in the wind power gear oil, has no influence on other indexes of oil products, and can effectively improve the safety and stability of the operation of the wind generating set.
Furthermore, the metal chelating agent, namely the disodium ethylene diamine tetraacetate, is applied to the field of gear oil treatment for the first time. The disodium ethylene diamine tetraacetate has six coordination atoms and extremely strong chelating capacity for metal ions, can generate an oleophobic reaction product under the synergistic action of the alcohol-water cosolvent and the heptanoic acid, and can effectively remove metal impurity elements such as iron, copper and the like in oil.
Furthermore, the silica gel precipitation aid selected in the invention has the advantages of high porosity, large specific surface area, strong adsorption capacity and the like, can accelerate the precipitation of the oleophobic chelate generated by the metal removal reaction, and powerfully improves the removal efficiency.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
The invention relates to a method for removing metal impurity elements in wind power gear oil, which comprises the following steps:
weighing the waste gear oil to be treated, and then placing the weighed waste gear oil in a constant temperature environment with the required reaction temperature. Weighing the required metal impurity removing agent, alcohol-water cosolvent and reaction removing promoter, mixing the three additives under the condition of normal temperature and closed mouth, and stirring for at least 30 minutes until the three additives are uniformly mixed. Adding the mixed solvent into the waste gear oil to be treated, keeping the constant temperature state and fully stirring, so that the removal reaction can be completely carried out. And (3) carrying out assisted precipitation by using a certain amount of silica gel particles, and then filtering the silica gel particles by using pressure-resistant filter cloth so as to completely separate metal impurity elements from oil.
The metal impurity remover is disodium ethylene diamine tetraacetate.
The addition amount of the metal impurity remover is 0.1-4% of the mass of the waste gear oil liquid.
The removal reaction promoter is heptanoic acid.
The addition amount of the removal reaction accelerant is 0.05-2% of the mass of the waste gear oil liquid.
The alcohol-water cosolvent is a mixture of alcohol with 2-5 carbon atoms and water, wherein the volume percentage concentration of the alcohol is 5-100% vol.
The addition amount of the alcohol-water cosolvent is 3-5 times of the addition amount of the metal impurity remover.
The environmental temperature required in the removing reaction process is 60-100 ℃, and the reaction time is 30-120 minutes.
The settling agent of the reaction product is silica gel particles, the dosage of the settling agent is 1-10% of the mass of the waste gear oil liquid, the diameter of the particles is 50-100 mu m, and the settling time is 2-5 hours.
The aperture of the pressure-proof filter cloth is 5um-25 um.
Example 1
The gear lubricating oil for the wind driven generator is treated, wherein the content of iron element in the gear lubricating oil for the wind driven generator is 205mg/kg, and the content of copper element in the gear lubricating oil for the wind driven generator is 20 mg/kg.
The specific operation process flow is as follows:
5kg of waste gear oil to be treated was weighed and then placed in a constant temperature environment of 80 ℃. Weighing disodium ethylene diamine tetraacetate accounting for 1% of the mass of the waste gear oil, 50% vol ethanol accounting for 5% of the mass of the waste gear oil and heptanoic acid accounting for 1% of the mass of the waste gear oil, mixing the three additives under a normal-temperature closed condition, and stirring for 40 minutes to uniformly mix the three additives to obtain a mixed solvent. Adding the mixed solvent into waste gear oil with the temperature of 80 ℃, keeping the constant temperature state and stirring for 60 minutes. And (3) assisting the oil liquid after the reaction to sink for 2 hours by using silica gel particles with the aperture of 75um and the mass of the waste gear oil, and filtering the oil liquid by using pressure-resistant filter cloth with the aperture of 10um to thoroughly separate metal impurity elements from the gear oil.
The final treatment effect of this embodiment is: the iron element is reduced to 39mg/kg, and the copper element is reduced to 7 mg/kg.
Example 2
The gear lubricating oil for the wind driven generator is treated, wherein the content of iron elements in the gear lubricating oil for the wind driven generator is 951mg/kg, and the content of copper elements in the gear lubricating oil for the wind driven generator is 48 mg/kg.
The specific operation process flow is as follows:
5kg of waste gear oil to be treated was weighed and then placed in a constant temperature environment of 100 ℃. Weighing disodium ethylene diamine tetraacetate accounting for 3% of the mass of the waste gear oil, 30% vol ethanol accounting for 10% of the mass of the waste gear oil and heptanoic acid accounting for 2% of the mass of the waste gear oil, mixing the three additives under a normal-temperature closed condition, and stirring for 60 minutes to uniformly mix the three additives to obtain a mixed solvent. Adding the mixed solvent into waste gear oil at the temperature of 100 ℃, keeping the constant temperature state and stirring for 100 minutes. And (3) assisting the oil liquid after the reaction to sink for 5 hours by using silica gel particles with 7% of the mass of the waste gear oil and 75um of pore diameter, and filtering the oil liquid by using pressure-resistant filter cloth with 5um of pore diameter to thoroughly separate metal impurity elements from the gear oil.
The final treatment effect of this embodiment is: the iron element is reduced to 145mg/kg, and the copper element is reduced to 20 mg/kg.
Example 3
Weighing the waste gear oil to be treated, and then placing the weighed waste gear oil in a constant temperature environment with the required reaction temperature. Weighing the required metal impurity removing agent, alcohol-water cosolvent and reaction removing promoter, mixing the three additives under the condition of normal temperature and closed mouth, and stirring for at least 30 minutes until the three additives are uniformly mixed. Adding the mixed solvent into the waste gear oil to be treated, keeping the constant temperature state and fully stirring, so that the removal reaction can be completely carried out. And (3) carrying out assisted precipitation by using a certain amount of silica gel particles, and then filtering the silica gel particles by using pressure-resistant filter cloth so as to completely separate metal impurity elements from oil.
The metal impurity remover is disodium ethylene diamine tetraacetate.
The addition amount of the metal impurity remover is 0.1 percent of the mass of the waste gear oil liquid.
The removal reaction promoter is heptanoic acid.
The addition amount of the removal reaction accelerant is 0.05 percent of the mass of the waste gear oil liquid.
The alcohol-water cosolvent is a mixture of alcohol with 2 carbon atoms and water, wherein the volume percentage concentration of the alcohol is 100% vol.
The addition amount of the alcohol-water cosolvent is 3 times of that of the metal impurity remover.
The ambient temperature required for the removal reaction was 70 ℃ and the reaction time was 50 minutes.
The settling agent of the reaction product is silica gel particles, the dosage of the settling agent is 5 percent of the mass of the waste gear oil liquid, the diameter of the particles is 50 mu m, and the settling time is 2 hours.
The aperture size of the pressure-proof filter cloth is 5 um.
Example 4
Weighing the waste gear oil to be treated, and then placing the weighed waste gear oil in a constant temperature environment with the required reaction temperature. Weighing the required metal impurity removing agent, alcohol-water cosolvent and reaction removing promoter, mixing the three additives under the condition of normal temperature and closed mouth, and stirring for at least 30 minutes until the three additives are uniformly mixed. Adding the mixed solvent into the waste gear oil to be treated, keeping the constant temperature state and fully stirring, so that the removal reaction can be completely carried out. And (3) carrying out assisted precipitation by using a certain amount of silica gel particles, and then filtering the silica gel particles by using pressure-resistant filter cloth so as to completely separate metal impurity elements from oil.
The metal impurity remover is disodium ethylene diamine tetraacetate.
The addition amount of the metal impurity remover is 2 percent of the mass of the waste gear oil liquid.
The removal reaction promoter is heptanoic acid.
The addition amount of the removal reaction accelerant is 1 percent of the mass of the waste gear oil liquid.
The alcohol-water cosolvent is a mixture of alcohol with 4 carbon atoms and water, wherein the volume percentage concentration of the alcohol is 25% vol.
The addition amount of the alcohol-water cosolvent is 4 times of that of the metal impurity remover.
The ambient temperature required for the removal reaction was 90 ℃ and the reaction time was 100 minutes.
The settling agent of the reaction product is silica gel particles, the dosage of the settling agent is 7 percent of the mass of the waste gear oil liquid, the diameter of the particles is 70 mu m, and the settling time is 3 hours.
The aperture size of the pressure-proof filter cloth is 15 um.
Example 5
Weighing the waste gear oil to be treated, and then placing the weighed waste gear oil in a constant temperature environment with the required reaction temperature. Weighing the required metal impurity removing agent, alcohol-water cosolvent and reaction removing promoter, mixing the three additives under the condition of normal temperature and closed mouth, and stirring for at least 30 minutes until the three additives are uniformly mixed. Adding the mixed solvent into the waste gear oil to be treated, keeping the constant temperature state and fully stirring, so that the removal reaction can be completely carried out. And (3) carrying out assisted precipitation by using a certain amount of silica gel particles, and then filtering the silica gel particles by using pressure-resistant filter cloth so as to completely separate metal impurity elements from oil.
The metal impurity remover is disodium ethylene diamine tetraacetate.
The addition amount of the metal impurity remover is 4 percent of the mass of the waste gear oil liquid.
The removal reaction promoter is heptanoic acid.
The addition amount of the removal reaction accelerant is 2 percent of the mass of the waste gear oil liquid.
The alcohol-water cosolvent is a mixture of alcohol with 3 carbon atoms and water, wherein the volume percentage concentration of the alcohol is 50% vol.
The addition amount of the alcohol-water cosolvent is 5 times of that of the metal impurity remover.
The ambient temperature required for the removal reaction was 100 ℃ and the reaction time was 30 minutes.
The settling agent of the reaction product is silica gel particles, the dosage of the settling agent is 1 percent of the mass of the waste gear oil liquid, the diameter of the particles is 100 mu m, and the settling time is 5 hours.
The aperture size of the pressure-proof filter cloth is 20 um.
Example 6
Weighing the waste gear oil to be treated, and then placing the weighed waste gear oil in a constant temperature environment with the required reaction temperature. Weighing the required metal impurity removing agent, alcohol-water cosolvent and reaction removing promoter, mixing the three additives under the condition of normal temperature and closed mouth, and stirring for at least 30 minutes until the three additives are uniformly mixed. Adding the mixed solvent into the waste gear oil to be treated, keeping the constant temperature state and fully stirring, so that the removal reaction can be completely carried out. And (3) carrying out assisted precipitation by using a certain amount of silica gel particles, and then filtering the silica gel particles by using pressure-resistant filter cloth so as to completely separate metal impurity elements from oil.
The metal impurity remover is disodium ethylene diamine tetraacetate.
The addition amount of the metal impurity remover is 2 percent of the mass of the waste gear oil liquid.
The removal reaction promoter is heptanoic acid.
The addition amount of the removal reaction accelerant is 2 percent of the mass of the waste gear oil liquid.
The alcohol-water cosolvent is a mixture of alcohol with 2 carbon atoms and water, wherein the volume percentage concentration of the alcohol is 5% vol.
The addition amount of the alcohol-water cosolvent is 4 times of that of the metal impurity remover.
The ambient temperature required for the removal reaction was 60 ℃ and the reaction time was 120 minutes.
The settling agent of the reaction product is silica gel particles, the dosage of the settling agent is 10 percent of the mass of the waste gear oil liquid, the diameter of the particles is 75 mu m, and the settling time is 4 hours.
The aperture size of the pressure-proof filter cloth is 25 um.
The invention is used for removing metal impurity elements such as iron element, copper element and the like in the gear lubricating oil of the wind driven generator; the metal impurity remover used in the method is disodium ethylene diamine tetraacetate, the alcohol-water cosolvent is a mixture of alcohol and water, and the removal reaction promoter is heptanoic acid; the metal impurity remover, the alcohol-water cosolvent and the removal reaction promoter used in the method have the advantages of low consumption, low cost and convenient transportation and storage; the removing method is simple and reliable, is easy to operate, can efficiently remove metal impurity elements such as iron element, copper element and the like in the wind power gear oil, has no influence on other indexes of oil products, and can effectively improve the safety and stability of the operation of the wind generating set.

Claims (10)

1. A method for removing metal impurity elements in wind power gear oil is characterized by comprising the following steps: mixing a metal impurity remover, an alcohol-water cosolvent and a removal reaction promoter to obtain a mixed solvent, adding the mixed solvent into waste gear oil to be treated, reacting at 60-100 ℃ for 30-120 minutes to obtain an oleophobic product, and carrying out assisted precipitation and filtration on silica gel particles passing through the oleophobic product.
2. The method for removing the metal impurity elements in the wind power gear oil according to claim 1, wherein the method comprises the following steps: the metal impurity remover is disodium ethylene diamine tetraacetate.
3. The method for removing the metal impurity elements in the wind power gear oil according to claim 1, wherein the method comprises the following steps: the dosage of the metal impurity remover is 0.1-4% of the mass of the waste gear oil.
4. The method for removing the metal impurity elements in the wind power gear oil according to claim 1, wherein the method comprises the following steps: the alcohol-water cosolvent is a mixture of alcohol with 2-5 carbon atoms and water, wherein the volume concentration of the alcohol is 5% -100%.
5. The method for removing the metal impurity elements in the wind power gear oil according to claim 1, wherein the method comprises the following steps: the dosage of the alcohol-water cosolvent is 3-5 times of the mass of the metal impurity remover.
6. The method for removing the metal impurity elements in the wind power gear oil according to claim 1, wherein the method comprises the following steps: the removal reaction promoter is heptanoic acid.
7. The method for removing the metal impurity elements in the wind power gear oil according to claim 1, wherein the method comprises the following steps: the dosage of the removal reaction accelerant is 0.05 to 2 percent of the mass of the waste gear oil.
8. The method for removing the metal impurity elements in the wind power gear oil according to claim 1, wherein the method comprises the following steps: the dosage of the silica gel particles is 1 to 10 percent of the mass of the waste gear oil, and the diameter of the silica gel particles is 50 to 100 mu m.
9. The method for removing the metal impurity elements in the wind power gear oil according to claim 1, wherein the method comprises the following steps: the settling time is 2-5 hours.
10. The method for removing the metal impurity elements in the wind power gear oil according to claim 1, wherein the method comprises the following steps: the filtration is carried out by adopting pressure-resistant filter cloth with the aperture size of 5um-25 um.
CN202110838011.7A 2021-07-23 2021-07-23 Method for removing metal impurity elements in wind power gear oil Withdrawn CN113430044A (en)

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