CN109880682B - Method for preparing composite lithium-calcium grease by using waste lithium-based lubricating grease as raw material - Google Patents
Method for preparing composite lithium-calcium grease by using waste lithium-based lubricating grease as raw material Download PDFInfo
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Abstract
The invention belongs to the technical field of recycling or processing of waste materials containing carboxylic ester, and particularly relates to a method for preparing composite lithium-calcium grease by taking waste lithium-based lubricating grease as a raw material. The method comprises the following steps: A. diluting the recovered waste lithium-based lubricating grease with mineral oil to a cone penetration of 420-480, removing mechanical impurities, adding 12-hydroxystearic acid and stearic acid, heating to 80 ℃, adding a calcium hydroxide aqueous solution, stirring and reacting at 80-100 ℃ for 4-6h, heating to 160 ℃, dehydrating until the mass content of water is less than or equal to 0.05%, and cooling to less than or equal to 60 ℃; B. and C, adding the antioxidant preservative, the extreme pressure antiwear agent, the benzotriazole and the benzotriazole derivative into the mixture obtained in the step A, stirring, homogenizing and degassing to obtain the lubricant. The composite lithium-calcium-based grease prepared by the method has excellent high temperature resistance, excellent compression resistance and excellent water leaching loss resistance.
Description
Technical Field
The invention belongs to the technical field of recycling or processing of waste materials containing carboxylic ester, and particularly relates to a method for preparing composite lithium-calcium grease by taking waste lithium-based lubricating grease as a raw material.
Background
The lubrication of various industries such as industry, agriculture, communication, metallurgy, textile and the like cannot be kept. The lubricating grease occupies an important part thereof and can play a lubricating role which cannot be solved by lubricating oil. The lubricating grease is a solid lubricant produced by thickening a soap-based or non-soap-based thickening agent by using mineral oil (or synthetic oil) and adding various additives such as antioxidant, antiwear, anticorrosive, extreme pressure and the like (the relation between the current state of the domestic lubricating grease and energy consumption, huaping, Chinese energy, 31 st volume 1 in 2009, pages 43-44, and 2009, 04/15 th day).
With the continuous improvement of industrialization degree, the application field of the lubricating grease is also inThe development of industrial machinery, agricultural machinery, transportation industry, electronic information industry and various military equipment are almost covered (the development and the technical situation of lubricating grease, Zhangjie and the like, chemical management, 31 st 2017, pages 64-65, published 2017, 11 th and 21 st). In recent years, chinese grease production and consumption have been rapidly increasing, and the proportion of the grease production and consumption has been increasing year by year in the world ("analysis of grease production status and development situation in recent years", yaohuandan et al, petroleum commerce, 2011, volume 29, pages 6, 12-15, published 2011, 12 months 31 days). In 2016, the total yield of the Chinese grease reaches 8.996X 108b (1b 453.6g) about 4.081X 108kg, about 35% of the total global grease yield ("a 1.4% increase in the same ratio of global grease yield in 2016", huanglimin, petroleum refining and chemical, vol.48, No. 9 in 2017, page 68, published day 2017, 12 months and 31 days).
At present, a large amount of grease products are consumed in China each year ("national grease products and advanced brief description of application technology thereof", yanhaining et al, vol 28, No. 3, page 18-25, published day 2010, 09 months and 15 days). After a certain period of use on mechanical equipment, grease is affected by its own properties and the type of friction site, operating conditions (such as temperature, speed, load), ambient environmental factors (such as steam, moisture, impurities, chemicals, etc.), and eventually fails due to continuous deterioration in quality. The failure mechanism of the lubricating grease in the use process is quite complex, has chemical reasons and physical reasons, and is the result of the comprehensive action of a plurality of factors such as environment, working conditions and the like (analysis of decay characteristics of the lubricating grease in the use process and discussion of scrapping indexes thereof, dynasty and the like, petroleum commerce and technology, 29 rd volume 3, 54 th to 57 th pages in 2011, 12 th and 31 th days in 2011). These heavily spent greases become waste greases, which have poor biodegradability ("preparation of environmentally friendly greases and study of tribological and biodegradable properties", chenoden, doctrine on doctrine, university of academy of sciences, 22014 years, abstract, published 2014 12 and 31 days), and which, if discarded into the environment at will, cause great harm to the environment.
Unlike waste lubricating oil, waste grease is difficult to recycle. At present, no mature process is available for recycling waste lubricating grease. At present, flying grease is generally treated by incineration, however, the incineration process itself causes environmental pollution. If the waste lubricating grease can be recycled, the environmental pollution can be reduced, and meanwhile, the product added value of the waste lubricating grease can be improved, so that the method has strong practical significance in the aspects of reducing the production cost, improving the product utilization rate and saving resources.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for preparing a composite lithium-calcium based grease from waste lithium-based grease as a raw material, which has important social significance in resource recycling, cost saving and environmental pollution reduction, and the prepared composite lithium-calcium based grease has excellent anti-leaching loss performance, shear stability and extreme pressure property.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the preparation method of the composite lithium-calcium-based grease comprises the following steps:
A. diluting the recovered waste lithium-based lubricating grease with mineral oil to a cone penetration of 420-480, removing mechanical impurities, adding 12-hydroxystearic acid and stearic acid, heating to 80 ℃, adding a calcium hydroxide aqueous solution, stirring and reacting for 4-6h at 80-100 ℃, heating to 160 ℃, dehydrating until the mass content of water is less than or equal to 0.05%, and cooling to less than or equal to 60 ℃;
B. and C, adding the antioxidant preservative, the extreme pressure antiwear agent, the benzotriazole and the benzotriazole derivative into the mixture obtained in the step A, stirring, homogenizing and degassing to obtain the lubricant.
Further, the cone penetration of the recovered waste lithium-based lubricating grease is less than or equal to 400.
Further, the kinematic viscosity of the mineral oil at 40 ℃ is 20-300mm2·s-1。
Further, the mass ratio of the 12-hydroxystearic acid to the mixture after the mechanical impurities are removed is 4: 100-8:100, and the mass ratio of the 12-hydroxystearic acid to the stearic acid is 4:1-8: 1.
Further, the mass fraction of the calcium hydroxide in the calcium hydroxide aqueous solution is 10-30 wt%
Further, the amount of the aqueous calcium hydroxide solution was such that the ratio of the amount of the substance of hydroxide ion contained in the aqueous calcium hydroxide solution to the amount of the sum of the substances of carboxylate ion contained in 12-hydroxystearic acid and stearic acid was 1: 1.
Further, the antioxidant preservative is zinc primary and secondary alcohol-based sulfur and phosphorus salt.
Furthermore, the mass ratio of the antioxidant preservative to the mixture without the mechanical impurities is 0.5:100-2.0: 100.
Further, the extreme pressure antiwear agent is 1-3 of thiophosphoric acid amine salt, sulfurized isobutylene and diisobutyl phosphite.
Further, the mass ratio of the dosage of the extreme pressure antiwear agent to the mixture after the mechanical impurities are removed is 0.5:100-2.0: 100.
Furthermore, the mass ratio of the benzotriazole to the mixture without the mechanical impurities is 0.2:100-0.5: 100.
Further, the mass ratio of the benzotriazole derivative to the mixture after removal of mechanical impurities is 0.02: 100-0.1:100.
Further, the preparation method of the composite lithium-calcium-based grease comprises the following steps:
A. diluting the recovered waste lithium-based lubricating grease with mineral oil to a cone penetration degree of 420-480, removing mechanical impurities, putting the waste lithium-based lubricating grease into a reaction kettle, adding 12-hydroxystearic acid and stearic acid into the reaction kettle, heating to 80 ℃, adding a calcium hydroxide aqueous solution, stirring and reacting for 4-6 hours at the temperature of 80-100 ℃ under normal pressure, heating to 160 ℃, dehydrating until the mass content of water is less than or equal to 0.05%, and cooling to below 60 ℃;
the mass ratio of the used amount of the 12-hydroxystearic acid to the mixture after the mechanical impurities are removed is 4: 100-8:100, and the mass ratio of the 12-hydroxystearic acid to the stearic acid is 4:1-8: 1; the mass fraction of calcium hydroxide in the calcium hydroxide aqueous solution is 10-30 wt%, and the ratio of the amount of hydroxide ion substances in the calcium hydroxide aqueous solution to the sum of carboxylate ion substances in 12-hydroxystearic acid and stearic acid is 1: 1;
the antioxidant preservative is zinc primary and secondary sulfur and phosphorus alcohol-based salt, and the mass ratio of the antioxidant preservative to the mixture after the mechanical impurities are removed is 0.5:100-2.0: 100;
B. adding an antioxidant preservative, an extreme pressure antiwear agent, benzotriazole and a benzotriazole derivative into a reaction kettle, stirring, homogenizing and degassing to obtain the final product;
the extreme pressure antiwear agent is 1-3 of thiophosphoric acid amine salt, sulfurized isobutylene and diisobutylphosphite, the mass ratio of the dosage of the extreme pressure antiwear agent to the mixture after the mechanical impurities are removed is 0.5:100-2.0:100, the mass ratio of the dosage of benzotriazole to the mixture after the mechanical impurities are removed is 0.2:100-0.5:100, the mass ratio of the dosage of benzotriazole derivatives to the mixture after the mechanical impurities are removed is 0.02: 100-0.1:100.
The invention has the beneficial effects that:
the method of the invention has important social significance in the aspects of resource recycling, cost saving and environmental pollution reduction.
The composite lithium-calcium-based grease prepared by the method has high hardness and wide application range, and the cone penetration degree is 226-272.
The composite lithium-calcium-based grease prepared by the method has excellent high temperature resistance, and the dropping point is 170-182 ℃.
The composite lithium-calcium-based grease prepared by the method has excellent corrosion resistance, and the copper sheet corrosion test result shows that the picture is green or black.
The composite lithium-calcium-based grease prepared by the method has excellent extreme pressure resistance, and the sintering load P of the composite lithium-calcium-based greaseD2450 and 4089N.
The lithium-calcium complex grease prepared by the method has excellent water leaching loss resistance, and the water leaching loss rate (38 ℃ and 1 hour) is less than or equal to 0.01 percent.
Detailed Description
The examples are provided for better illustration of the present invention, but the present invention is not limited to the examples. Therefore, those skilled in the art should make insubstantial modifications and adaptations to the embodiments of the present invention in light of the above teachings and remain within the scope of the invention.
The cone penetration is detected according to GB/T269 & 1991 lubricating grease and petroleum ester cone penetration determination method;
the following kinematic viscosity (40 ℃) was measured in accordance with GB/T265-1998 petroleum products kinematic viscosity determination method;
the following dropping points were detected according to GB/T4929-1985 lubricating grease dropping point assay;
the following copper sheet corrosion test is carried out according to GB/T7326 lubricating grease copper sheet corrosion test method;
the following sintering loads were measured according to "SH/T0202-;
the water spray loss rate (38 ℃, 1h) is detected according to the SH/T0109-2004 lubricating grease water spray resistance performance determination method;
the water content was measured according to GB/T512-1965 grease moisture test method.
Example 1
The preparation method of the composite lithium-calcium-based grease comprises the following steps:
A. the recovered waste lithium grease (cone penetration 242) was treated with 26# technical white oil (kinematic viscosity 25mm at 40 ℃ C.)2·s-1) Diluting to a cone penetration degree of 430, performing high-speed centrifugation, filtering to remove mechanical impurities, weighing 400.0g, putting into a reaction kettle, sequentially adding 24.0g of 12-hydroxystearic acid and 6.0g of stearic acid into the reaction kettle, heating to 80 ℃ under normal pressure, adding 37.7g of calcium hydroxide aqueous solution with the mass fraction of 20.0%, stirring and reacting for 4 hours at 90 ℃, gradually heating to 160 ℃, stirring for 1.6 hours, dehydrating to a water mass content of 0.02%, and cooling to 60 ℃;
B. adding 2.2g of zinc primary and secondary sulfur and phosphorus alcohol-based salt, 4.0g of sulfurized isobutylene, 1.0g of benzotriazole and 10.2 g of benzotriazole derivative into a reaction kettle, fully stirring, homogenizing by a homogenizer, and degassing to obtain the product.
Example 2
The preparation method of the composite lithium-calcium-based grease comprises the following steps:
A. the recovered waste lithium grease (cone penetration of 235) was treated with 100# technical white oil (kinematic viscosity of 100mm at 40 ℃ C.)2·s-1) Diluting to cone penetration 460, performing high-speed centrifugation, filtering to remove mechanical impurities, weighing 400.0g, putting into a reaction kettle, sequentially adding 32.0g of 12-hydroxystearic acid and 8.0g of stearic acid into the reaction kettle, heating to 80 ℃ under normal pressure, adding 100.0g of calcium hydroxide aqueous solution with the mass fraction of 10.0%, stirring and reacting for 4 hours at 90 ℃, gradually heating to 160 ℃, stirring for 2 hours, dehydrating until the mass content of water is 0.03%, and cooling to below 58 ℃;
B. adding 3.0g of zinc primary and secondary sulfur and phosphorus alcohol-based salt, 8.0g of sulfurized isobutylene, 1.2g of benzotriazole and 10.4 g of benzotriazole derivative T5510, fully stirring, homogenizing by a homogenizer, and degassing to obtain the product.
Example 3
The preparation method of the composite lithium-calcium-based grease comprises the following steps:
A. the recovered waste lithium grease (cone penetration of 235) was used with SN150# base oil (kinematic viscosity of 30mm at 40 ℃)2·s-1) Diluting to a cone penetration degree of 430, performing high-speed centrifugation, filtering to remove mechanical impurities, weighing 400.0g, putting into a reaction kettle, sequentially adding 16.0g of 12-hydroxystearic acid and 4.0g of stearic acid into the reaction kettle, heating to 80 ℃ under normal pressure, adding 16.7g of calcium hydroxide aqueous solution with the mass fraction of 30.0%, stirring and reacting for 4 hours at 90 ℃, gradually heating to 160 ℃, stirring for 2 hours, dehydrating to the mass content of 0.02% of water, and cooling to 40 ℃;
B. adding 2.5g of zinc primary and secondary sulfur and phosphorus alcohol base salt, 6.0g of sulfurized isobutylene, 1.0g of benzotriazole and 1.3 g of benzotriazole derivative T5510.3 g into a reaction kettle, fully stirring, homogenizing by a homogenizer, and degassing to obtain the product.
Example 4
The preparation method of the composite lithium-calcium-based grease comprises the following steps:
A. the recovered waste lithium-based lubricating grease (penetration 358) is treated with mineral base oil (40℃)Kinematic viscosity of 300mm2·s-1) Diluting to a cone penetration of 480, performing high-speed centrifugation, filtering to remove mechanical impurities, weighing 400.0g, putting into a reaction kettle, sequentially adding 20.0g of 12-hydroxystearic acid and 5.0g of stearic acid into the reaction kettle, heating to 80 ℃ under normal pressure, adding 24.8g of calcium hydroxide aqueous solution with the mass fraction of 25.0%, stirring and reacting for 4 hours at 90 ℃, gradually heating to 160 ℃, stirring for 2 hours, dehydrating to the mass content of 0.02% of water, and cooling to 58 ℃;
B. 6.0g of zinc primary and secondary sulfur and phosphorus alcohol base salt, 8.0g of sulfurized isobutylene, 2.0g of benzotriazole and 2.3 g of benzotriazole derivative T5510.3 g are added into a reaction kettle, and the mixture is fully stirred, homogenized by a homogenizer and degassed again to obtain the product.
Example 5
The preparation method of the composite lithium-calcium-based grease comprises the following steps:
A. the recovered waste lithium-based grease (cone penetration of 235) was treated with mineral base oil (kinematic viscosity at 40 ℃ C. of 20 mm)2·s-1) Diluting to a cone penetration degree of 420, performing high-speed centrifugation, filtering to remove mechanical impurities, weighing 400.0g, putting into a reaction kettle, sequentially adding 33.5g of 12-hydroxystearic acid and 8.0g of stearic acid into the reaction kettle, heating to 80 ℃ under normal pressure, adding 24.8g of calcium hydroxide aqueous solution with the mass fraction of 30.0%, stirring and reacting for 4 hours at 90 ℃, gradually heating to 160 ℃, stirring for 2 hours, dehydrating to the mass content of 0.03% of water, and cooling to 55 ℃;
B. adding 9.0g of zinc primary and secondary sulfur and phosphorus alcohol-based zinc salt, 9.0g of sulfurized isobutylene, 2.2g of benzotriazole and 10.4 g of benzotriazole derivative T5510.4g into a reaction kettle, fully stirring, homogenizing by a homogenizer, and degassing to obtain the product.
Example 6
The preparation method of the composite lithium-calcium-based grease comprises the following steps:
A. the recycled waste lithium-based lubricating grease (with cone penetration of 235) is mixed with mineral base oil SN150 (with kinematic viscosity of 28mm at 40℃)2·s-1) Diluting to cone penetration 430, centrifuging at high speed, filtering to remove mechanical impurities, weighing 400.0g, placing into a reaction kettle, sequentially adding 16.0g of 12-hydroxystearic acid and 4.0g of stearic acid into the reaction kettleHeating to 80 ℃ under normal pressure, adding 16.7g of calcium hydroxide aqueous solution with the mass fraction of 30.0%, stirring and reacting for 4 hours at 90 ℃, gradually heating to 160 ℃, stirring for 2 hours, dehydrating until the mass content of water is 0.02%, and cooling to 40 ℃;
B. adding 2.5g of zinc primary and secondary thiophosphoryl alcohol salt, T3078.0 g of ammonium thiophosphate salt, 1.0g of benzotriazole and T5510.3 g of benzotriazole derivative into a reaction kettle, fully stirring, homogenizing by a homogenizer, and degassing to obtain the product.
Example 7
The preparation method of the composite lithium-calcium-based grease comprises the following steps:
A. the recovered waste lithium-based grease (cone penetration of 235) was used at 40 ℃ with a kinematic viscosity of 20mm2·s-1Diluting the mineral base oil to a cone penetration degree of 420, performing high-speed centrifugation, filtering to remove mechanical impurities, weighing 400.0g, putting into a reaction kettle, sequentially adding 32.0g of 12-hydroxystearic acid and 84.0g of stearin into the reaction kettle, heating to 80 ℃ under normal pressure, adding 33.5g of calcium hydroxide aqueous solution with the mass fraction of 30.0%, stirring and reacting for 4 hours at 90 ℃, gradually heating to 160 ℃, stirring for 2 hours, dehydrating to the mass content of 0.02% of water, and cooling to 60 ℃;
B. adding 2.5g of zinc primary and secondary thiophosphoryl alcohol base, 9.0g of diisobutylphosphite, 2.2g of benzotriazole and 10.4 g of benzotriazole derivative T5510, stirring fully, homogenizing by a homogenizer, and degassing to obtain the product.
Example 8
The preparation method of the composite lithium-calcium-based grease comprises the following steps:
A. the recovered waste lithium-based grease (cone penetration of 235) was used at 40 ℃ with a kinematic viscosity of 120mm2·s-1Diluting the mineral base oil to a cone penetration degree of 420, performing high-speed centrifugation, filtering to remove mechanical impurities, weighing 400.0g, putting into a reaction kettle, sequentially adding 32.0g of 12-hydroxystearic acid and 8.0g of stearic acid into the reaction kettle, heating to 80 ℃ under normal pressure, adding 33.5g of calcium hydroxide aqueous solution with the mass fraction of 30.0%, stirring and reacting for 4 hours at 90 ℃, gradually heating to 160 ℃, stirring for 2 hours, dehydrating to the mass content of 0.02% of water, and coolingTo 60 ℃;
B. adding 2.5g of zinc primary and secondary sulfur-phosphorus alcohol-based zinc salt, 4.0g of sulfurized isobutylene, T3074.0 g of thiophosphoric acid amine salt, 1.0g of diisobutyl phosphite, 2.2g of benzotriazole and 10.4 g of benzotriazole derivative into a reaction kettle, fully stirring, homogenizing by a homogenizer, and degassing to obtain the product.
Performance detection
The lithium-calcium complex greases obtained in examples 1 to 8 were subjected to penetration test, dropping point test, copper sheet corrosion test and sintering load PDAnd the water leaching loss rate (38 ℃, 1h) and the like, and the results are shown in tables 1 and 2.
Table 1 results of performance testing
Table 2 results of performance testing
As is apparent from tables 1 and 2, the penetration of the composite lithium-calcium based grease prepared in examples 1-8 was 226-272. Therefore, the composite lithium-calcium-based grease prepared by the method has high hardness and wide application range.
As is apparent from tables 1 and 2, the dropping point of the complex lithium-calcium based grease prepared in examples 1-8 was 170-182 ℃. Therefore, the composite lithium-calcium-based grease prepared by the method has excellent high-temperature resistance.
As is apparent from tables 1 and 2, the corrosion test results of the copper sheets of the lithium-calcium based composite greases prepared in examples 1 to 8 were in the form of green or black discoloration. Therefore, the composite lithium-calcium-based grease prepared by the method has excellent corrosion resistance.
As is clear from tables 1 and 2, the sintering loads P of the composite lithium-calcium based greases obtained in examples 1 to 8D2450 and 4089N. Therefore, the compression resistance of the composite lithium-calcium-based grease prepared by the method is excellent.
As is clear from tables 1 and 2, the lithium-calcium complex greases obtained in examples 1 to 8 showed a water leaching loss rate (38 ℃ C., 1 hour) of 0.01% or less. Therefore, the composite lithium-calcium base grease prepared by the method has excellent water leaching loss resistance.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (23)
1. The preparation method of the composite lithium-calcium-based grease is characterized by comprising the following steps:
A. diluting the recovered waste lithium-based lubricating grease with mineral oil to a cone penetration of 420-480, removing mechanical impurities, adding 12-hydroxystearic acid and stearic acid, heating to 80 ℃, adding a calcium hydroxide aqueous solution, stirring and reacting at 80-100 ℃ for 4-6h, heating to 160 ℃, dehydrating until the mass content of water is less than or equal to 0.05%, and cooling to less than or equal to 60 ℃;
B. adding zinc primary and secondary sulfur-phosphorus alcohol-based salt, an extreme pressure antiwear agent, benzotriazole and a benzotriazole derivative into the mixture obtained in the step A, stirring, homogenizing and degassing to obtain the product; the extreme pressure antiwear agent is 1-3 of thiophosphoric acid amine salt, sulfurized isobutylene and diisobutyl phosphite.
2. The method of claim 1, wherein the recycled used lithium-based grease has a penetration of 400 or less.
3. The method according to claim 1 or 2, wherein the mineral oil has a kinematic viscosity at 40 ℃ of 20 to 300mm2·s -1 。
4. The method according to claim 1 or 2, wherein the 12-hydroxystearic acid is used in an amount such that the mass ratio of the 12-hydroxystearic acid to the mixture after removal of the mechanical impurities is 4: 100-8:100, and the mass ratio of the 12-hydroxystearic acid to the stearic acid is 4:1-8: 1.
5. The method according to claim 3, wherein the 12-hydroxystearic acid is used in an amount such that the mass ratio of the 12-hydroxystearic acid to the mixture after removal of the mechanical impurities is 4: 100-8:100, and the mass ratio of the 12-hydroxystearic acid to the stearic acid is 4:1-8: 1.
6. The preparation method according to claim 1, 2 or 5, characterized in that the zinc primary and secondary thiophosphoryl salts are used in a mass ratio of 0.5:100-2.0: 100.
7. the preparation method according to claim 3, characterized in that the zinc primary and secondary thiophosphoryl salt is used in a mass ratio of 0.5:100-2.0: 100.
8. the preparation method according to claim 4, characterized in that the zinc primary and secondary thiophosphoryl salt is used in a mass ratio of 0.5:100-2.0: 100.
9. the preparation method of claim 1, 2, 5, 7 or 8, wherein the weight ratio of the extreme pressure antiwear agent to the mixture after removing the mechanical impurities is 0.5:100-2.0: 100.
10. the preparation method of claim 3, wherein the weight ratio of the extreme pressure antiwear agent to the mixture after the mechanical impurities are removed is 0.5:100-2.0: 100.
11. the preparation method of claim 4, wherein the weight ratio of the extreme pressure antiwear agent to the mixture after the mechanical impurities are removed is 0.5:100-2.0: 100.
12. the preparation method of claim 6, wherein the weight ratio of the extreme pressure antiwear agent to the mixture after the mechanical impurities are removed is 0.5:100-2.0: 100.
13. the preparation method according to claim 1, 2, 5, 7, 8, 10, 11 or 12, characterized in that the mass ratio of the benzotriazole to the mixture after removal of mechanical impurities is 0.2: 100-0.5:100.
14. The preparation method according to claim 3, characterized in that the mass ratio of the benzotriazole to the mixture after mechanical impurities are removed is 0.2: 100-0.5:100.
15. The preparation method according to claim 4, characterized in that the mass ratio of the benzotriazole to the mixture after mechanical impurities are removed is 0.2: 100-0.5:100.
16. The preparation method according to claim 6, characterized in that the mass ratio of the benzotriazole to the mixture after the mechanical impurities are removed is 0.2: 100-0.5:100.
17. The preparation method according to claim 9, characterized in that the mass ratio of the benzotriazole to the mixture after mechanical impurities are removed is 0.2: 100-0.5:100.
18. The production method according to claim 1, 2, 5, 7, 8, 10, 11, 12, 14, 15, 16 or 17, wherein the benzotriazole derivative is used in an amount such that the mass ratio to the mixture after removal of mechanical impurities is 0.02: 100-0.1: 100.
19. the production method according to claim 3, wherein the benzotriazole derivative is used in an amount such that the mass ratio of the benzotriazole derivative to the mixture after removal of mechanical impurities is 0.02: 100-0.1: 100.
20. the production method according to claim 4, wherein the amount of the benzotriazole derivative is such that the mass ratio of the mixture after removal of mechanical impurities is 0.02: 100-0.1: 100.
21. the production method according to claim 6, wherein the amount of the benzotriazole derivative is such that the mass ratio of the mixture after removal of mechanical impurities is 0.02: 100-0.1: 100.
22. the production method according to claim 9, wherein the benzotriazole derivative is used in an amount such that the mass ratio of the benzotriazole derivative to the mixture after removal of mechanical impurities is 0.02: 100-0.1: 100.
23. the production method according to claim 13, wherein the benzotriazole derivative is used in an amount such that the mass ratio of the benzotriazole derivative to the mixture after removal of mechanical impurities is 0.02: 100-0.1: 100.
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