Fluorescent dry lubricant and preparation method thereof

Abstract

The invention relates to the technical field of lubricants, in particular to a fluorescent dry lubricant and a preparation method thereof.The fluorescent dry lubricant is prepared from, by mass, 0.001%-0.1% of a fluorescent agent, 2%-10% of fluorine oil, 0%-10% of polytetrafluoroethylene and the balance fluorine solvent; the fluorescent agent with a specific structure overcomes the problems that an OB fluorescent agent in the market is poor in solubility and low in fluorescent brightness in a fluorine solvent, so that the lubricant has good solubility and relatively high fluorescent brightness in the fluorine solvent, and an effective tracing effect can be achieved. Through the fluorescence detection equipment, the distribution position, leakage and other conditions of the lubricant can be rapidly and accurately positioned, the convenience of detection and maintenance is greatly improved, problems can be found in time, corresponding measures can be taken, and equipment faults caused by poor lubrication or leakage and other problems are avoided.

Description

Technical Field

[0001] The invention relates to the technical field of lubricants, and in particular to a fluorescent dry lubricant and a preparation method thereof. Background Art

[0002] Fluorescent whitening agent OB is a symmetrical structured dibenzoxazole type "2,5-thiophene derivative" fluorescent whitening agent. It has a bright yellow crystal appearance, a melting point of 198℃~202℃, is soluble in most organic solvents, has very low solubility in water, has a maximum absorption wavelength of 375 nm, and a fluorescence emission wavelength of 435 nm. Fluorescent whitening agent OB can be widely used in the whitening of plastics such as PVC, PS, ABS, PE, PP, and is also suitable for the whitening of polyester fibers, coatings, paints, inks and acrylic acid. Due to its superior fluorescent whitening effect, non-toxicity, good thermal stability, and low addition amount, it has become one of the fluorescent whitening agents commonly used in China. However, the OB fluorescent agent on the market has poor solubility in fluorine solvents, low fluorescence brightness, and no tracer effect. Summary of the invention

[0003] In order to overcome the above-mentioned shortcomings, the present invention aims to provide a technical solution that can solve the above-mentioned problems.

[0004] A fluorescent dry lubricant comprising the following components in mass fractions: Fluorescent agent 0.001%-0.1% Fluorine oil 2%-10% Polytetrafluoroethylene 0%-10% Fluorinated solvent balance.

[0005] Preferably, the structural formula of the fluorescent agent is: (I) In the formula, R1 and R2 are one or two of the following molecular structural formulas (II) to (VII): -CH2-(CH2)n-CH3 (Ⅱ); -CH2-O-(CH2)n-CH3 (III); -COO-(CH2)nCH3 (IV); -CF2C(CF2)nCF3(V); -CF2-O-(CF2)n-CF3(VI); (VII); Where n is a natural number from 1 to 5.

[0006] Preferably, the fluorine oil is perfluoropolyether oil, and the kinematic viscosity of the perfluoropolyether oil at a temperature of 40° C. ranges from 10 mm 2 / s to 3500 mm 2 / s.

[0007] Preferably, the molecular structure of the perfluoropolyether oil includes one or both of (VIII) and (IX), and (VIII) and (IX) are as follows: (VIII) (IX) In (VIII), the range of m+n is 8-45, and the range of the ratio of m to n is 20-1000; in (IX), the range of p+q is 40-180, and the range of the ratio of p to q is 0.5-2.

[0008] Preferably, the median particle size of the polytetrafluoroethylene is 0.1 micron to 100 microns.

[0009] Preferably, the fluorine solvent includes one or more of trifluorotrichloroethane, hydrofluoroether, perfluorobutyl cyclic ether, pentafluorobutane, hexafluoropropylene trimer, hexafluoropropylene dimer, perfluorocyclohexane, perfluorohexane, perfluoromethylhexane, ethoxy nonafluorobutyl ether, and methoxy nonafluorobutyl ether.

[0010] A method for preparing a fluorescent dry lubricant, used for preparing the fluorescent dry lubricant described above, comprises the following steps: Step 1, add trichlorobenzene, phenol, acid, and catalyst in a four-necked flask equipped with a reflux condenser, a thermometer, a vent pipe, and a stirring rod, and then pump toluene into the feeding kettle. After stirring evenly, introduce 99.9% nitrogen into the flask to prevent the material from being oxidized, and then heat the material to 140°C to 180°C, start condensation dehydration reaction for 3 to 4 hours, continue to heat the reaction and dehydration until the material is heated to 210°C to 250°C. During the dehydration process, toluene is evaporated. When no water is removed from the reaction material, the reaction is terminated; cool to 50°C to 60°C, add 80 to 100 mL of methanol, cool to room temperature, and filter; Step 2, transfer the filter cake into a three-necked flask, add 80 mL~100 mL of detergent, heat to 50℃~60℃, stir for 0.5 h, cool to room temperature, and filter; Step 3, repeat step 2, and dry the filter cake in an oven at 100°C to 105°C for 1 to 2 h; Step 4, recrystallization to obtain a light green-yellow solid fluorescent agent; Step 5, weigh polytetrafluoroethylene and fluorine oil in a ratio of 1:1-3, mix and stir evenly, and grind twice with three rollers for later use; Step 6, weighing the prepared fluorescent agent and the fluorine solvent and mixing them in a ratio of 0.1 to 3:100 to prepare a fluorescent agent solution for later use; Step 7, adding the materials prepared in step 5 and step 6 into the container in proportion, stirring at high speed to disperse evenly; Step 8, filtering and packaging the material that has been uniformly dispersed by high-speed stirring in step 7 to obtain a finished fluorescent dry lubricant.

[0011] Preferably, the acid in step 1 is thiophene-2,5-dicarboxylic acid, and the phenol structure is one of the following (X) to (XIII): , , , (X) (XI) (XII) (XIII) In (X) to (XIII), R is the same as R1 or R2.

[0012] Preferably, the catalyst is boric acid, and the detergent comprises one of dimethylformamide, methanol, petroleum ether, and ethanol.

[0013] Preferably, the molar ratio of the five substances, namely, acid, phenol, boric acid, trichlorobenzene and toluene, is 1:2.0-2.5:0.10-0.25:3.0-4.0:3.0-4.0.

[0014] Compared with the prior art, the present invention has the following beneficial effects: As one of the main ingredients, fluoro oil itself has good lubricating properties, and polytetrafluoroethylene can also enhance the lubrication effect to a certain extent. The cooperation between the two enables the lubricant to effectively reduce friction loss in the use scenarios of various equipment and components, extend the service life of the equipment, and improve the efficiency and stability of equipment operation.

[0015] The present invention adds a fluorescent agent with a specific ratio and a specific molecular structure, wherein: In terms of the influence on solubility, -CH2-(CH2)n-CH3 is an alkyl chain structure, which is lipophilic and has good compatibility with oily components such as fluorinated oil, which helps to improve the dispersibility and solubility of the fluorescent agent in the lubricant system; -CH2-O-(CH2)n-CH3 is an ether bond structure. The ether bond gives it a certain polarity, which can interact with the polar region of the fluorinated solvent and non-polar components such as fluorinated oil to balance the solubility; -COO-(CH2)nCH3 is an ester group structure. The ester group increases the molecular polarity and can interact with the polar part of the fluorinated solvent. The long-chain alkyl group is compatible with fluorinated oil and balances the solubility of the system; -CF2C (CF2)nCF3 is a fluorinated structure with strong hydrophobicity and compatibility with fluorinated solvents, which ensures that the fluorescent agent is evenly distributed in the fluorinated solvent and improves the solubility; -CF2-O-(CF2)n-CF3 is a structure containing ether bonds and fluorine. The ether bond interacts with the polar region of the fluorinated solvent, and the fluorinated part is compatible with the non-polar region, which improves the solubility of the fluorescent agent in the fluorinated solvent.

[0016] In terms of the influence on fluorescence properties, -CH2-O-(CH2) n-CH3 can affect the molecular orbital and electron cloud distribution to a certain extent, and adjust the fluorescence emission wavelength and intensity; -CF2-O-(CF2) n-CF3 affects the molecular energy level and electronic transition, and can adjust the fluorescence characteristics to meet specific detection needs.

[0017] In terms of the influence on lubrication performance, the alkyl chain structure of -CH2-(CH2)n-CH3 is relatively soft and can form a film on the friction surface to assist lubrication and reduce the friction coefficient. The ester group of -COO-(CH2)nCH3 may undergo a chemical reaction on the friction surface to form a lubricating film, and the long-chain alkyl group also assists lubrication.

[0018] In terms of the impact on stability, -CH2-(CH2)n-CH3 has relatively stable chemical properties and is not easy to react with other components, ensuring the long-term stability of the lubricant; the large number of carbon-fluorine bonds in -CF2C (CF2)nCF3 gives it extremely high thermal and chemical stability, and it remains stable under high temperature and harsh chemical environments.

[0019] In terms of compatibility, -CH2-O-(CH2) n-CH3 is better compatible with substances of different chemical properties when used in combination with other additives or materials, and the ether bond acts as a bridge; -CF2-O-(CF2) n-CF3 has good compatibility with materials such as fluorinated oil and polytetrafluoroethylene, and the fluorinated part enhances the overall performance of the lubricant.

[0020] Therefore, the fluorescent agent with a specific structure overcomes the problem of poor solubility and low fluorescence brightness of the OB fluorescent agent on the market in fluorine solvents, making the lubricant have good solubility and high fluorescence brightness in fluorine solvents, and can play an effective tracing effect. Through the fluorescence detection equipment, the distribution position of the lubricant and leakage can be quickly and accurately located, which greatly improves the convenience of detection and maintenance, helps to find problems in time and take corresponding measures to avoid equipment failures due to poor lubrication or leakage.

[0021] In addition, the components work together to ensure good lubrication performance while providing fluorescent tracing function. This combination not only meets the needs of industrial production and other fields for efficient equipment lubrication, but also provides a new means for equipment detection and maintenance, which helps to improve the safety and reliability of the entire production process and reduce the risk of downtime and maintenance costs caused by equipment failure, poor lubrication and other problems.

[0022] Additional aspects and advantages of the present invention will be given in part in the following description and in part will be obvious from the following description, or will be learned through practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0024] Figure 1 is a molecular reaction structure diagram of the fluorescent agent of Example 1 of the present invention; Figure 2 is a molecular reaction structure diagram of the fluorescent agent of Example 2 of the present invention; Figure 3 is a molecular reaction structure diagram of the fluorescent agent of Example 3 of the present invention; Figure 4 is a molecular reaction structure diagram of the fluorescent agent of Example 4 of the present invention; Figure 5 is a molecular reaction structure diagram of the fluorescent agent of Example 5 of the present invention; Figure 6 It is a molecular reaction structure diagram of the fluorescent agent of Example 6 of the present invention. DETAILED DESCRIPTION

[0025] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0026] During the preparation process, the molar ratio of each raw material and the specific reaction temperature and time range are clearly defined, making the entire reaction process highly controllable. This helps to ensure that the fluorescent dry lubricant prepared each time has stable performance and reliable quality; by precisely controlling the reaction conditions, such as conducting the condensation dehydration reaction within a specific temperature range, the reaction can be effectively promoted, the reaction efficiency can be improved, and the occurrence of side reactions can be avoided, ensuring the purity of the product.

[0027] After multiple steps of filtration, drying and recrystallization, impurities can be effectively removed and the purity of the fluorescent agent can be improved. High-purity fluorescent agents can better exert their fluorescent properties in lubricants, improve fluorescent brightness and tracing effects; a specific mixing ratio and grinding process are used in the preparation of base grease, so that polytetrafluoroethylene is evenly dispersed in fluorine oil to form a stable base grease; this helps to improve the lubrication performance and stability of the lubricant. During the reaction, nitrogen is introduced to prevent the material from being oxidized, which reduces the by-products and harmful substances produced by the oxidation reaction and improves the safety of the product; at the same time, it also reduces the pollution to the environment. The prepared fluorescent dry lubricant combines the good lubrication performance of fluorine oil, the enhanced lubrication effect of polytetrafluoroethylene and the tracing function of the fluorescent agent. The components work together to enable the lubricant to meet a variety of needs in practical applications and improve the operating efficiency and reliability of the equipment. The precise preparation method ensures the quality stability of the product, so that the fluorescent dry lubricant can exert excellent performance in different working environments and reduce the risks caused by product quality fluctuations. Specifically, please refer to the following examples: [Example 1] like Figure 1 As shown, this embodiment prepares a fluorescent dry lubricant and a preparation method thereof. The raw material components and their mass fractions of the lubricant in this embodiment are: Fluorescent agent 0.01%; Perfluoropolyether oil (Y-type fluoro oil) 5%; Polytetrafluoroethylene 1%; Trichlorotrifluoroethane 20%; Hydrofluoroether residual; The preparation method thereof comprises the following steps: Step 1, prepare acid, phenol, boric acid, trichlorobenzene, and toluene in a molar ratio of 1:2.1:0.10:3.0:3.0, wherein boric acid is used as a catalyst; add phenol, acid, and catalyst in a four-necked flask equipped with a reflux condenser, a thermometer, a vent pipe, and a stirring rod in sequence, and then pump toluene into the feeding kettle, start stirring evenly, and introduce 99.9% nitrogen into the flask to prevent the material from being oxidized, and then heat the material to 140°C to 160°C, start condensation dehydration reaction for 3 hours, continue to heat the reaction and dehydrate until the material is heated to 210°C to 220°C, and toluene is evaporated during the dehydration process. When no water is removed from the reaction material, the reaction is terminated; cool to 60°C, add 80 mL of methanol, cool to room temperature, and filter; Step 2, transfer the filter cake into a three-necked flask, add 100 mL of methanol, heat to 60°C, stir for 0.5 h, cool to room temperature, and filter; Step 3, repeat step 2, and dry the filter cake in an oven at 105°C for 1 hour; Step 4, recrystallization, to obtain a fluorescent solid, the reaction formula of which is as follows: Figure 1 As shown; Step 5, weighing Y-type fluorine oil with a viscosity of 15 mm2 / s at 40°C, and mixing it with polytetrafluoroethylene with a median particle size of 1 micron at a ratio of 3:7, and then grinding it twice with three rollers to prepare it as a base grease; wherein the molecular structure of the Y-type fluorine oil is formula (VIII); Step 6, weigh the fluorine solvent, base grease, remaining fluorine oil and fluorescent agent in proportion, add them into the container, and disperse them at high speed for 3-10 minutes; Step 7, after 300 mesh filtering, it is packaged as a finished fluorescent dry lubricant.

[0028] [Example 2] This embodiment prepares a fluorescent dry lubricant and a preparation method thereof. The raw material components and their mass fractions of the lubricant in this embodiment are: Fluorescent agent 0.02%; Perfluoropolyether oil (Y-type fluoro oil) 5%; Polytetrafluoroethylene 1%; Trichlorotrifluoroethane 20%; Hexafluoropropylene dimer balance; The preparation method thereof comprises the following steps: Step 1, prepare acid, phenol, boric acid, trichlorobenzene, and toluene in a molar ratio of 1:2.1:0.10:3.0:3.0, wherein boric acid is used as a catalyst; add phenol, acid, and catalyst in a four-necked flask equipped with a reflux condenser, a thermometer, a vent pipe, and a stirring rod in sequence, and then pump toluene into the feeding kettle, start stirring evenly, and introduce 99.9% nitrogen into the flask to prevent the material from being oxidized, and then heat the material to 140°C to 160°C, start condensation dehydration reaction for 3 hours, continue to heat the reaction and dehydrate until the material is heated to 210°C to 220°C, and toluene is evaporated during the dehydration process. When no water is removed from the reaction material, the reaction is terminated; cool to 60°C, add 80 mL of methanol, cool to room temperature, and filter; Step 2, transfer the filter cake into a three-necked flask, add 100 mL of methanol, heat to 60°C, stir for 0.5 h, cool to room temperature, and filter; Step 3, repeat step 2, and dry the filter cake in an oven at 105°C for 1 hour; Step 4, recrystallization, to obtain a fluorescent solid, the reaction formula of which is as follows: Figure 2 As shown; Step 5, weighing Y-type fluorine oil with a viscosity of 30 mm2 / s at 40°C, and mixing it with polytetrafluoroethylene with a median particle size of 1 micron at a ratio of 3:7, and then grinding it twice with three rollers to prepare it as a base grease; wherein the molecular structure of the Y-type fluorine oil is formula (VIII); Step 6, weigh the fluorine solvent, base grease, remaining fluorine oil and fluorescent agent in proportion, add them into the container, and disperse them at high speed for 3-10 minutes; Step 7, after 300 mesh filtering, it is packaged as a finished fluorescent dry lubricant.

[0029] [Example 3] This embodiment prepares a fluorescent dry lubricant and a preparation method thereof. The raw material components and their mass fractions of the lubricant in this embodiment are: Fluorescent agent 0.02%; Perfluoropolyether oil (Y-type fluoro oil) 5%; Polytetrafluoroethylene 1%; Trichlorotrifluoroethane 20%; Fluorinated solvent residue; The preparation method thereof comprises the following steps: Step 1, prepare acid, phenol, boric acid, trichlorobenzene, and toluene in a molar ratio of 1:2.1:0.10:3.0:3.0, wherein boric acid is used as a catalyst; add phenol, acid, and catalyst in a four-necked flask equipped with a reflux condenser, a thermometer, a vent pipe, and a stirring rod in sequence, and then pump toluene into the feeding kettle, start stirring evenly, and introduce 99.9% nitrogen into the flask to prevent the material from being oxidized, and then heat the material to 140°C to 160°C, start condensation dehydration reaction for 3 hours, continue to heat the reaction and dehydrate until the material is heated to 210°C to 220°C, and toluene is evaporated during the dehydration process. When no water is removed from the reaction material, the reaction is terminated; cool to 60°C, add 80 mL of methanol, cool to room temperature, and filter; Step 2, transfer the filter cake into a three-necked flask, add 100 mL of methanol, heat to 60°C, stir for 0.5 h, cool to room temperature, and filter; Step 3, repeat step 2, and dry the filter cake in an oven at 105°C for 1 hour; Step 4, recrystallization, to obtain a fluorescent solid, the reaction formula of which is as follows: Figure 3 As shown; Step 5, weighing Y-type fluorine oil with a viscosity of 1000 mm2 / s at 40°C, and mixing it with polytetrafluoroethylene with a median particle size of 1 micron at a ratio of 3:7, and then grinding it twice with three rollers to prepare it as a base grease; wherein the molecular structure of the Y-type fluorine oil is formula (VIII); Step 6, weigh the fluorine solvent, base grease, remaining fluorine oil and fluorescent agent in proportion, add them into the container, and disperse them at high speed for 3-10 minutes; Step 7, after 300 mesh filtering, it is packaged as a finished fluorescent dry lubricant.

[0030] [Example 4] This embodiment prepares a fluorescent dry lubricant and a preparation method thereof. The raw material components and their mass fractions of the lubricant in this embodiment are: Fluorescent agent 0.02%; Perfluoropolyether oil (M-type fluoro oil) 5%; Trichlorotrifluoroethane 20%; Methoxy nonafluorobutyl ether balance; The preparation method thereof comprises the following steps: Step 1, prepare acid, phenol, boric acid, trichlorobenzene, and toluene in a molar ratio of 1:2.1:0.10:3.0:3.0, wherein boric acid is used as a catalyst; add phenol, acid, and catalyst in a four-necked flask equipped with a reflux condenser, a thermometer, a vent pipe, and a stirring rod in sequence, and then pump toluene into the feeding kettle, start stirring evenly, and introduce 99.9% nitrogen into the flask to prevent the material from being oxidized, and then heat the material to 140°C to 160°C, start condensation dehydration reaction for 3 hours, continue to heat the reaction and dehydrate until the material is heated to 210°C to 220°C, and toluene is evaporated during the dehydration process. When no water is removed from the reaction material, the reaction is terminated; cool to 60°C, add 80 mL of methanol, cool to room temperature, and filter; Step 2, transfer the filter cake into a three-necked flask, add 100 mL of methanol, heat to 60°C, stir for 0.5 h, cool to room temperature, and filter; Step 3, repeat step 2, and dry the filter cake in an oven at 105°C for 1 hour; Step 4, recrystallization, to obtain a fluorescent agent solid; its reaction formula is as follows Figure 4 As shown; Step 5, weighing M-type fluorine oil with a viscosity of 30 mm2 / s at 40°C, and mixing it with polytetrafluoroethylene with a median particle size of 1 micron at a ratio of 3:7, and then grinding it twice with three rollers to prepare it as a base grease; wherein the molecular structure of the M-type fluorine oil is formula (IX); Step 6, weighing the fluorine solvent, M-type fluorine oil and fluorescent agent in proportion, adding them into a container, and dispersing at high speed for 3-10 minutes; Step 7, after 300 mesh filtering, it is packaged as a finished fluorescent dry lubricant.

[0031] [Example 5] This embodiment prepares a fluorescent dry lubricant and a preparation method thereof. The raw material components and their mass fractions of the lubricant in this embodiment are: Fluorescent agent 0.02%; Perfluoropolyether oil (M-type fluoro oil) 5%; Pentafluorobutane 10%; Methoxy nonafluorobutyl ether balance; The preparation method thereof comprises the following steps: Step 1, prepare acid, phenol, boric acid, trichlorobenzene, and toluene in a molar ratio of 1:2.1:0.10:3.0:3.0, wherein boric acid is used as a catalyst; add phenol, acid, and catalyst in a four-necked flask equipped with a reflux condenser, a thermometer, a vent pipe, and a stirring rod in sequence, and then pump toluene into the feeding kettle, start stirring evenly, and introduce 99.9% nitrogen into the flask to prevent the material from being oxidized, and then heat the material to 140°C to 160°C, start condensation dehydration reaction for 3 hours, continue to heat the reaction and dehydrate until the material is heated to 210°C to 220°C, and toluene is evaporated during the dehydration process. When no water is removed from the reaction material, the reaction is terminated; cool to 60°C, add 80 mL of methanol, cool to room temperature, and filter; Step 2, transfer the filter cake into a three-necked flask, add 100 mL of methanol, heat to 60°C, stir for 0.5 h, cool to room temperature, and filter; Step 3, repeat step 2, and dry the filter cake in an oven at 105°C for 1 hour; Step 4, recrystallization, to obtain a fluorescent agent solid; its reaction formula is as follows Figure 5 As shown; Step 5, weighing M-type fluorine oil with a viscosity of 30 mm2 / s at 40°C, and mixing it with polytetrafluoroethylene with a median particle size of 1 micron at a ratio of 3:7, and then grinding it twice with three rollers to prepare it as a base grease; wherein the molecular structure of the M-type fluorine oil is formula (IX); Step 6, weigh the fluorine solvent, base grease, remaining fluorine oil and fluorescent agent in proportion, add them into the container, and disperse them at high speed for 3-10 minutes; Step 7, after 300 mesh filtering, it is packaged as a finished fluorescent dry lubricant.

[0032] [Example 6] This embodiment prepares a fluorescent dry lubricant and a preparation method thereof. The raw material components and their mass fractions of the lubricant in this embodiment are: Fluorescent agent 0.02%; Perfluoropolyether oil (M-type fluoro oil) 5%; Ethoxy nonafluorobutyl ether balance; The preparation method thereof comprises the following steps: Step 1, prepare acid, phenol, boric acid, trichlorobenzene, and toluene in a molar ratio of 1:2.1:0.10:3.0:3.0, wherein boric acid is used as a catalyst; add phenol, acid, and catalyst in a four-necked flask equipped with a reflux condenser, a thermometer, a vent pipe, and a stirring rod in sequence, and then pump toluene into the feeding kettle, start stirring evenly, and introduce 99.9% nitrogen into the flask to prevent the material from being oxidized, and then heat the material to 140°C to 160°C, start condensation dehydration reaction for 3 hours, continue to heat the reaction and dehydrate until the material is heated to 210°C to 220°C, and toluene is evaporated during the dehydration process. When no water is removed from the reaction material, the reaction is terminated; cool to 60°C, add 80 mL of methanol, cool to room temperature, and filter; Step 2, transfer the filter cake into a three-necked flask, add 100 mL of methanol, heat to 60°C, stir for 0.5 h, cool to room temperature, and filter; Step 3, repeat step 2, and dry the filter cake in an oven at 105°C for 1 hour; Step 4, recrystallization, to obtain a fluorescent agent solid; its reaction formula is as follows Figure 6 As shown; Step 5, weighing M-type fluorine oil with a viscosity of 30 mm2 / s at 40°C, weighing fluorine solvent, fluorine oil and fluorescent agent in proportion, adding them into a container, and dispersing at high speed for 3-10 minutes; wherein the molecular structure of M-type fluorine oil is formula (IX); Step 6, after 300 mesh filtering, it is packaged as a finished fluorescent dry lubricant.

[0033] [Comparative Example 1] This embodiment prepares a fluorescent dry lubricant and a preparation method thereof. The raw material components and their mass fractions of the lubricant in this embodiment are: OP fluorescent agent 0.01%; Perfluoropolyether oil (M-type fluoro oil) 5%; Ethoxy nonafluorobutyl ether balance; The preparation method thereof comprises the following steps: Step 5, weighing M-type fluorine oil with a viscosity of 30 mm2 / s at 40°C, weighing fluorine solvent, fluorine oil and fluorescent agent in proportion, adding them into a container, and dispersing at high speed for 3-10 minutes; wherein the molecular structure of M-type fluorine oil is formula (IX); Step 2, after 300 mesh filtering, it is packaged as a finished fluorescent dry lubricant.

[0034] [Comparative Example 2] This embodiment prepares a fluorescent dry lubricant and a preparation method thereof. The raw material components and their mass fractions of the lubricant in this embodiment are: OP fluorescent agent 0.01%; Perfluoropolyether oil (Y-type fluoro oil) 5%; Polytetrafluoroethylene 1% Ethoxy nonafluorobutyl ether balance; The preparation method thereof comprises the following steps: Step 1, weighing Y-type fluorine oil with a viscosity of 1000 mm2 / s at 40°C, and mixing it with polytetrafluoroethylene with a median particle size of 1 micron at a ratio of 3:7, and then grinding it twice with three rollers to prepare it as a base grease; wherein the molecular structure of the Y-type fluorine oil is formula (VIII); Step 2, weigh the fluorine solvent, base grease, remaining fluorine oil and fluorescent agent in proportion, add them into a container, and disperse them at high speed for 3-10 minutes; Step 3, after 300 mesh filtering, it is packaged as a finished fluorescent dry lubricant.

[0035] [Comparative Example 3] This embodiment prepares a fluorescent dry lubricant and a preparation method thereof. The raw material components and their mass fractions of the lubricant in this embodiment are: Perfluoropolyether oil (M-type fluoro oil) 5%; Ethoxy nonafluorobutyl ether balance; The preparation method thereof comprises the following steps: Weigh M-type fluorine oil with a viscosity of 30 mm2 / s at 40°C, weigh fluorine solvents in proportion, add the fluorine oil into a container, and disperse at high speed for 3-10 minutes; wherein the molecular structure of the M-type fluorine oil is formula (IX); Step 6, after 300 mesh filtering, it is packaged as a finished fluorescent dry lubricant.

[0036] [Comparative Example 4] This embodiment prepares a fluorescent dry lubricant and a preparation method thereof. The raw material components and their mass fractions of the lubricant in this embodiment are: Perfluoropolyether oil (Y-type fluoro oil) 5%; Polytetrafluoroethylene 1% Ethoxy nonafluorobutyl ether balance; The preparation method thereof comprises the following steps: Step 1, weighing Y-type fluorine oil with a viscosity of 1000 mm2 / s at 40°C, and mixing it with polytetrafluoroethylene with a median particle size of 1 micron at a ratio of 3:7, and then grinding it twice with three rollers to prepare it as a base grease; wherein the molecular structure of the Y-type fluorine oil is formula (VIII); Step 2, weigh the fluorine solvent, base grease and remaining fluorine oil in proportion, add them into a container, and disperse them at high speed for 3-10 minutes; Step 3, after 300 mesh filtering, it is packaged as a finished fluorescent dry lubricant.

[0037] Performance test results: It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be considered exemplary and non-restrictive in all respects, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention.

Claims

1. A fluorescent dry lubricant, characterized in that: The following components are included in mass fraction: Fluorescent agent 0.001%-0.1% Fluorine oil 2%-10% Polytetrafluoroethylene 0%-10% Fluorinated solvent balance.

2. A fluorescent dry lubricant according to claim 1, characterized in that: The structural formula of the fluorescent agent is: （Ⅰ） In the formula, R1 and R2 are one or two of the following molecular structural formulas (II) to (VII): -CH2-(CH2)n-CH3 (Ⅱ); -CH2-O-(CH2)n-CH3 (III); -COO-(CH2)nCH3 (IV); -CF2C(CF2)nCF3(V); -CF2-O-(CF2)n-CF3(VI); （Ⅶ）； Where n is a natural number ranging from 1 to 5.

3. A fluorescent dry lubricant according to claim 1, characterized in that: The fluorine oil is a perfluoropolyether oil. Under the condition of a temperature of 40°C, the kinematic viscosity of the perfluoropolyether oil ranges from 10 square millimeters per second to 3500 square millimeters per second.

4. A fluorescent dry lubricant according to claim 3, characterized in that: The molecular structure of perfluoropolyether oil includes one or both of Y-type fluorine oil and M-type fluorine oil. The Y-type fluorine oil and M-type fluorine oil are as follows: （Ⅷ） （Ⅸ） In (VIII), the range of m+n is 8-45, and the range of the ratio of m to n is 20-1000; in (IX), the range of p+q is 40-180, and the range of the ratio of p to q is 0.5-2.

5. The fluorescent dry lubricant according to claim 1, characterized in that: The median particle size of polytetrafluoroethylene is 0.1 micron ~ 100 microns.

6. The fluorescent dry lubricant according to claim 1, characterized in that: The fluorine solvent includes one or more of trifluorotrichloroethane, hydrofluoroether, perfluorobutyl cyclic ether, pentafluorobutane, hexafluoropropylene trimer, hexafluoropropylene dimer, perfluorocyclohexane, perfluorohexane, perfluoromethylhexane, ethoxy nonafluorobutyl ether, and methoxy nonafluorobutyl ether.

7. A method for preparing a fluorescent dry lubricant, used for preparing a fluorescent dry lubricant according to any one of claims 1 to 6, characterized in that: The following steps are included: Step 1, add trichlorobenzene, phenol, acid, and catalyst in a four-necked flask equipped with a reflux condenser, a thermometer, a vent pipe, and a stirring rod, and then pump toluene into the feeding kettle. After stirring evenly, introduce 99.9% nitrogen into the flask to prevent the material from being oxidized, and then heat the material to 140°C to 180°C, start condensation dehydration reaction for 3 to 4 hours, continue to heat the reaction and dehydration until the material is heated to 210°C to 250°C. During the dehydration process, toluene is evaporated. When no water is removed from the reaction material, the reaction is terminated; cool to 50°C to 60°C, add 80 to 100 mL of methanol, cool to room temperature, and filter; Step 2, transfer the filter cake into a three-necked flask, add 80 mL~100 mL of detergent, heat to 50°C~60°C, stir for 0.5 h, cool to room temperature, and filter; Step 3, repeat step 2, and dry the filter cake in an oven at 100°C to 105°C for 1 to 2 h; Step 4, recrystallization to obtain a light green-yellow solid fluorescent agent; Step 5, weigh polytetrafluoroethylene and fluorine oil in a ratio of 1:1-3, mix and stir evenly, and grind twice with three rollers for later use; Step 6, weighing the prepared fluorescent agent and the fluorine solvent and mixing them in a ratio of 0.1 to 3:100 to prepare a fluorescent agent solution for later use; Step 7, adding the materials prepared in step 5 and step 6 into the container in proportion, stirring at high speed to disperse evenly; Step 8, filtering and packaging the material dispersed evenly by high-speed stirring in step 7 to obtain a finished fluorescent dry lubricant.

8. The method for preparing a fluorescent dry lubricant according to claim 7, characterized in that: The acid in step 1 is thiophene-2,5-dicarboxylic acid, and the phenol structure is one of the following (X) to (XIII): 、 、 、 （Ⅹ） （Ⅺ） （Ⅻ） （ⅩⅢ） In (X) to (XIII), R is the same as R1 or R2.

9. The method for preparing a fluorescent dry lubricant according to claim 7, characterized in that: The catalyst is boric acid, and the detergent comprises one of dimethylformamide, methanol, petroleum ether, and ethanol.

10. The method for preparing a fluorescent dry lubricant according to claim 9, characterized in that: The molar ratio of the five substances, namely, acid, phenol, boric acid, trichlorobenzene and toluene, is 1:2.0-2.5:0.10-0.25:3.0-4.0:3.0-4.0.

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