A fluorescent dry lubricant and a method of making the same

Abstract

The present application relates to the technical field of lubricant, in particular to a fluorescent dry lubricant and a preparation method thereof, comprising the following components by mass fraction: fluorescent agent 0.001%-0.1%, fluorine oil 2%-10%, polytetrafluoroethylene 0%-10%, and fluorine solvent in the rest; the fluorescent agent with a specific structure overcomes the poor solubility of OB fluorescent agent on the market in fluorine solvent and the low fluorescent brightness, so that the lubricant has good solubility in fluorine solvent and high fluorescent brightness, and can effectively play a tracking effect. Through the fluorescent detection equipment, the distribution position of the lubricant and leakage and the like can be quickly and accurately located, the convenience of detection and maintenance is greatly improved, problems can be found in time and corresponding measures can be taken, and equipment failure caused by poor lubrication or leakage and the like can be avoided.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of lubricant technology, in particular to a fluorescent dry lubricant and a preparation method thereof. BACKGROUND

[0002] The fluorescent whitening agent OB belongs to symmetrical structure double benzohumazol type "2, 5-thiophene derivative" fluorescent whitening agent, which is bright yellow crystal in appearance, has a melting point of 198-202℃, is soluble in most organic solvents, has very small solubility in water, has a maximum absorption wavelength of 375 nm, and has a fluorescent emission wavelength of 435 nm. The fluorescent whitening agent OB can be widely applied to the whitening of PVC, PS, ABS, PE, PP and other plastics, and is also suitable for the whitening of polyester fibers, coatings, paints, inks and acrylics. Since it has excellent fluorescent whitening effect, is non-toxic, has good thermal stability, and has a small amount of addition, etc., it has been one of the commonly used fluorescent whitening agents in China. However, the OB fluorescent agent on the market has very poor solubility in fluorine solvents, low fluorescent brightness, and cannot play a tracking effect. SUMMARY

[0003] The present application is aimed at providing a technical solution to solve the above problems.

[0004] A fluorescent dry lubricant, comprising the following components by mass fraction:

[0005] Fluorescent agent 0.001%-0.1%

[0006] Fluorine oil 2%-10%

[0007] Polytetrafluoroethylene 0%-10%

[0008] Fluorine solvent in the remaining amount.

[0009] Preferably, the structural formula of the fluorescent agent is:

[0010]

[0011] (I)

[0012] In the formula, R1 and R2 are one or both of the following molecular structural formula (II)~molecular structural formula (VII):

[0013] -CH2-(CH2)n-CH3 (II);

[0014] -CH2-O-(CH2)n-CH3 (III);

[0015] -COO-(CH2)nCH3 (IV);

[0016] -CF2C(CF2)nCF3 (V);

[0017] -CF2-O-(CF2)n-CF3(VI);

[0018] (VII);

[0019] wherein n is a natural number from 1 to 5.

[0020] Preferably, the fluorine oil is a perfluoropolyether oil, and the perfluoropolyether oil has a kinematic viscosity value ranging from 10 mm2 / s to 3500 mm2 / s at a temperature of 40°C.

[0021] Preferably, the molecular structure of the perfluoropolyether oil includes one or both of (VIII) and (IX) as follows:

[0022]

[0023] (VIII)

[0024]

[0025] (IX)

[0026] In (VIII), m+n ranges from 8 to 45, and the ratio of m to n ranges from 20 to 1000; in (IX), p+q ranges from 40 to 180, and the ratio of p to q ranges from 0.5 to 2.

[0027] Preferably, the polytetrafluoroethylene has a median particle size ranging from 0.1 μm to 100 μm.

[0028] 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.

[0029] A method for preparing a fluorescent dry lubricant, for preparing the fluorescent dry lubricant described above, includes the following steps:

[0030] Step 1: A four-necked flask is provided with a reflux condenser, a thermometer, a gas inlet tube, and a stirring rod. Phenyltrichloride, phenol, acid, and a catalyst are sequentially added to the flask. Toluene is then pumped into the flask. After stirring is started, 99.9% nitrogen is introduced into the flask to prevent oxidation of the materials. The materials are then heated to 140°C to 180°C, and condensation and dehydration reactions begin to occur. The reaction continues to dehydrate as the temperature is increased to 210°C to 250°C. As the materials are dehydrated, toluene is evaporated. When no water is produced from the reaction materials, the reaction is complete. The temperature is then decreased to 50°C to 60°C. Methanol (80 mL to 100 mL) is added, and the mixture is cooled to room temperature. The mixture is then filtered.

[0031] Step 2, transfer the filter cake to a three-necked flask, add 80 mL~100 mL detergent, heat to 50℃~60℃, stir for 0.5 h, cool to room temperature, filter;

[0032] Step 3, repeat Step 2, dry the filter cake in an oven at 100℃~105℃ for 1~2 h;

[0033] Step 4, recrystallization, obtain the fluorescent agent as light green yellow solid;

[0034] Step 5, weigh polytetrafluoroethylene and fluorine oil in a ratio of 1:1~3, mix and stir uniformly, then pass through a three-roll mill twice for standby;

[0035] Step 6, weigh the prepared fluorescent agent and fluorine solvent in a ratio of 0.1~3:100 to prepare a fluorescent agent solution for standby;

[0036] Step 7, add the materials prepared in Step 5 and Step 6 to the container in proportion, and stir at high speed to disperse uniformly;

[0037] Step 8, filter and package the material after high-speed stirring and dispersion in Step 7 to obtain the finished product of the fluorescent dry lubricant.

[0038] Preferably, the acid in Step 1 is thiophene-2,5-dicarboxylic acid, and the phenol structure is one of the following (X) to (XIII):

[0039] 、 、 、

[0040] (X) (XI) (XII) (XIII)

[0041] R in (X) to (XIII) is the same as R1 or R2.

[0042] Preferably, the catalyst is boric acid, and the detergent includes one of dimethylformamide, methanol, petroleum ether, and ethanol.

[0043] Preferably, the molar ratio of the five substances of acid, phenol, boric acid, benzene trichloride, and toluene is 1:2.0~2.5:0.10~0.25:3.0~4.0:3.0~4.0.

[0044] Compared with the prior art, the present application has the following beneficial effects:

[0045] As one of the main components, fluorine oil itself has good lubricating performance, and polytetrafluoroethylene can also enhance the lubricating effect to a certain extent. The cooperation of the two can effectively reduce the friction loss and prolong the service life of the equipment in various use scenarios of devices and parts, and improve the efficiency and stability of the equipment operation.

[0046] The present application adds a fluorescent agent with a specific ratio and a specific molecular structure formula, wherein,

[0047] In terms of the influence on solubility, -CH2-(CH2) n-CH3 is an alkyl chain structure, has lipophilicity, and is compatible with oily components such as fluorine 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 makes it have a certain polarity, and can interact with the polar region of the fluorine solvent and the non-polar components such as fluorine oil, balancing the solubility; -COO-(CH2) nCH3 is an ester group structure, the ester group increases the molecular polarity, which can interact with the polar part of the fluorine solvent, and the long-chain alkyl group is compatible with the fluorine oil, balancing the solubility of the system; -CF2C (CF2) nCF3 is a fluorine-containing structure, which has strong hydrophobicity and compatibility with the fluorine solvent, ensuring uniform distribution of the fluorescent agent in the fluorine solvent and improving the solubility; -CF2-O-(CF2) n-CF3 is an ether bond and fluorine structure, the ether bond interacts with the polar region of the fluorine solvent, and the fluorine-containing part is compatible with the non-polar region, improving the solubility of the fluorescent agent in the fluorine solvent.

[0048] In terms of the influence on the fluorescence performance, -CH2-O-(CH2) n-CH3 can affect the molecular orbital and electron cloud distribution to a certain extent, adjust the fluorescence emission wavelength and intensity; -CF2-O-(CF2) n-CF3 affects the molecular energy level and electron transition, and can adjust the fluorescence characteristics to adapt to specific detection needs.

[0049] In terms of the influence on the lubrication performance, the alkyl chain structure of -CH2-(CH2) n-CH3 is relatively soft, which can form a film on the friction surface to assist lubrication and reduce the friction coefficient; the ester group of -COO-(CH2) nCH3 may react chemically on the friction surface to form a lubricating film, and the long-chain alkyl group also assists lubrication.

[0050] In terms of the influence on stability, -CH2-(CH2) n-CH3 has relatively stable chemical properties and is not prone to reaction with other components, ensuring long-term stability of the lubricant; -CF2C (CF2) nCF3 has a large number of carbon-fluorine bonds, which makes it have extremely high thermal stability and chemical stability, and remains stable under high temperature and harsh chemical environments.

[0051] In terms of compatibility, -CH2-O-(CH2) n-CH3 can better compatible with substances of different chemical properties when used with other additives or materials, and the ether bond acts as a bridge; -CF2-O-(CF2) n-CF3 has good compatibility with fluorine oil, polytetrafluoroethylene and other materials, and the fluorine-containing part enhances the overall performance of the lubricant.

[0052] Therefore, the fluorescent agent with the specific structure overcomes the problems of poor solubility in fluorine solvents and low fluorescence brightness of the OB fluorescent agent on the market, so that the lubricant has good solubility and high fluorescence brightness in the fluorine solvent, and can effectively play a tracking effect. Through the fluorescence detection equipment, the distribution position of the lubricant and the leakage and the like can be quickly and accurately located, the convenience of detection and maintenance is greatly improved, and timely problems can be found and corresponding measures can be taken to avoid equipment failure caused by poor lubrication or leakage and the like.

[0053] In addition, the components synergize with each other to ensure good lubricating performance while imparting the fluorescent tracking function. This combination not only meets the demand for efficient lubrication of equipment in the field of industrial production and the like, but also provides a new means for detection and maintenance of the equipment, and helps to improve the safety and reliability of the entire production process and reduce the risk of shutdown and maintenance cost caused by equipment failure, poor lubrication and the like.

[0054] Additional aspects and advantages of the application will be set forth in part in the description which follows, and in part will become apparent to those skilled in the art upon examination of the following description and drawings. BRIEF DESCRIPTION OF DRAWINGS

[0055] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiment or prior art description. Obviously, the drawings in the following description are only some embodiments of the present application, and those skilled in the art can also obtain other drawings according to these drawings without creative labor.

[0056] Figure 1 is the molecular reaction formula structure diagram of the fluorescent agent of the embodiment 1 of the present application;

[0057] Figure 2 is the molecular reaction formula structure diagram of the fluorescent agent of the embodiment 2 of the present application;

[0058] Figure 3 is the molecular reaction formula structure diagram of the fluorescent agent of the embodiment 3 of the present application;

[0059] Figure 4 is the molecular reaction formula structure diagram of the fluorescent agent of the embodiment 4 of the present application;

[0060] Figure 5 is the molecular reaction formula structure diagram of the fluorescent agent of the embodiment 5 of the present application;

[0061] Figure 6 is the molecular reaction formula structure diagram of the fluorescent agent of the embodiment 6 of the present application. DETAILED DESCRIPTION

[0062] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0063] During the preparation process, the molar ratios of each raw material, as well as the specific reaction temperature and time ranges, were clearly defined, ensuring a high degree of controllability throughout the entire reaction process. This helps ensure that the fluorescent dry lubricant prepared each time has stable performance and reliable quality. By precisely controlling the reaction conditions, such as carrying out the condensation and dehydration reaction within a specific temperature range, the reaction can be effectively promoted, reaction efficiency can be improved, and side reactions can be avoided, thus ensuring the purity of the product.

[0064] Through multiple steps of filtration, drying, and recrystallization, impurities are effectively removed, improving the purity of the fluorescent agent. High-purity fluorescent agents can better exert their fluorescent properties in lubricants, enhancing fluorescence brightness and tracer effects. The preparation of the base grease utilizes specific mixing ratios and grinding processes, ensuring uniform dispersion of polytetrafluoroethylene (PTFE) in the fluorinated oil, forming a stable base grease. This contributes to improving the lubricating performance and stability of the lubricant. Nitrogen gas is introduced during the reaction to prevent material oxidation, reducing byproducts and harmful substances generated by oxidation reactions and improving product safety. Simultaneously, it reduces environmental pollution. The resulting fluorescent dry lubricant combines the excellent lubrication properties of fluorinated oil, the enhanced lubrication effect of PTFE, and the tracer function of the fluorescent agent. The synergistic effect of the components allows the lubricant to meet various needs in practical applications, improving equipment operating efficiency and reliability. The precise preparation method ensures product quality stability, enabling the fluorescent dry lubricant to exhibit excellent performance under different working environments, reducing the risks associated with product quality fluctuations. Specifically, please refer to the following examples:

[0065]

Example 1

[0066] like Figure 1 As shown, this embodiment prepares a fluorescent dry lubricant and its preparation method. The raw material components and their mass fractions for preparing the lubricant in this embodiment are as follows:

[0067] Fluorescent agent 0.01%;

[0068] Perfluoropolyether oil (Y-type fluorinated oil) 5%;

[0069] 1% polytetrafluoroethylene;

[0070] 20% trifluorochloroethane;

[0071] Balance of hydrofluoroether;

[0072] The preparation method comprises the following steps:

[0073] Step 1, prepare the acid, phenol, boric acid, trichlorobenzene, toluene in a molar ratio of 1:2.1:0.10:3.0:3.0, wherein the boric acid is used as a catalyst; sequentially add the phenol, acid and catalyst into a four-necked flask provided with a reflux condenser, a thermometer, an air inlet pipe and a stirring rod, then pump toluene into the feeding kettle, open the stirring to be uniform, then introduce 99.9% nitrogen into the flask to prevent the material from being oxidized, then heat the material to 140-160 DEG C, and start the condensation dehydration reaction for 3 hours, continue to heat and react to dehydrate until the material is heated to 210-220 DEG C, during the dehydration, toluene is evaporated, and when no water is dehydrated from the reaction material, the reaction is completed; cool to 60 DEG C, add 80 mL of methanol, cool to room temperature, and filter;

[0074] Step 2, transfer the filter cake into a three-necked flask, add 100 mL of methanol, heat to 60 DEG C, stir for 0.5 h, cool to room temperature, and filter;

[0075] Step 3, repeat step 2, and dry the filter cake in an oven at 105 DEG C for 1 h;

[0076] Step 4, recrystallize to obtain the fluorescent agent solid, and the reaction formula is as shown in Figure 1 .

[0077] Step 5, weigh the Y type fluorine oil with a viscosity of 15 mm2 / s at 40 DEG C, uniformly mix the Y type fluorine oil with polytetrafluoroethylene with a median particle size of 1 microns at a ratio of 3:7, and then grind for two times by a three-roll mill to obtain a base fat for standby; wherein the molecular structural formula of the Y type fluorine oil is formula (VIII);

[0078] Step 6, add the fluorescent agent, the base fat, the remaining fluorine oil and the fluorescent agent into a container in proportion, and disperse at a high speed for 3-10 minutes;

[0079] Step 7, filter through a 300 mesh screen, and package to obtain a fluorescent dry lubricant product.

[0080]

Example 2

[0081] The example prepares a fluorescent dry lubricant and a preparation method thereof, and the preparation raw material components and mass fractions of the lubricant of the example are as follows:

[0082] Fluorescent agent 0.02%;

[0083] Perfluoropolyether oil (Y type fluorine oil) 5%;

[0084] Polytetrafluoroethylene 1%;

[0085] Trifluorotrichloroethane 20%;

[0086] Hexafluoropropylene dimer the balance;

[0087] The preparation method comprises the following steps:

[0088] Step 1, prepare the acid, phenol, boric acid, trichlorobenzene and toluene in a molar ratio of 1:2.1:0.10:3.0:3.0, wherein the boric acid is used as a catalyst; sequentially add the phenol, acid and catalyst into a four-necked flask provided with a reflux condenser, a thermometer, an air inlet pipe and a stirring rod, then pump the toluene into the feeding kettle, open the stirring to be uniform, then introduce 99.9% nitrogen into the flask to prevent the material from being oxidized, then heat the material to 140-160 DEG C, and start the condensation dehydration reaction for 3 hours, continue to heat the reaction to dehydrate, until the material is heated to 210-220 DEG C, during the dehydration, the toluene is evaporated, when there is no water in the reaction material, the reaction is completed; cool to 60 DEG C, add 80 mL of methanol, cool to room temperature, and filter;

[0089] Step 2, transfer the filter cake into a three-necked flask, add 100 mL of methanol, heat to 60 DEG C, stir for 0.5 h, cool to room temperature, and filter;

[0090] Step 3, repeat step 2, and dry the filter cake in an oven at 105 DEG C for 1 h;

[0091] Step 4, recrystallize to obtain the fluorescent agent solid, and the reaction formula is as shown in Figure 2 .

[0092] Step 5, weigh the Y type fluorine oil with a viscosity of 30 mm2 / s at 40 DEG C, uniformly mix the Y type fluorine oil with polytetrafluoroethylene with a median particle size of 1 microns at a ratio of 3:7, then grind the mixture by three-roller grinding for two times, and use the mixture as a base fat;

[0093] Step 6, sequentially weigh the fluorine solvent, the base fat, the remaining fluorine oil and the fluorescent agent according to the proportion, and add the materials into a container, and disperse at a high speed for 3-10 minutes;

[0094] Step 7, filter through a 300 mesh screen, and package to obtain a fluorescent dry lubricant product.

[0095]

Example 3

[0096] The example prepares a fluorescent dry lubricant and a preparation method thereof, and the preparation raw material components and mass fractions of the lubricant of the example are as follows:

[0097] Fluorescent agent 0.02%;

[0098] Perfluoropolyether oil (Y type fluorine oil) 5%;

[0099] Polytetrafluoroethylene 1%;

[0100] Trifluorotrichloroethane 20%;

[0101] Fluorine solvent residual amount

[0102] The preparation method comprises the following steps:

[0103] Step 1, prepare the acid, phenol, boric acid, trichlorobenzene, toluene in a molar ratio of 1:2.1:0.10:3.0:3.0, wherein the boric acid is used as a catalyst; sequentially add the phenol, acid, and catalyst into a four-necked flask provided with a reflux condenser, a thermometer, an air inlet pipe, and a stirring rod, then pump toluene into the feeding kettle, open the stirring, uniformly mix, then introduce 99.9% nitrogen into the flask to prevent the material from being oxidized, then heat the material to 140-160 DEG C, start the condensation dehydration reaction for 3 hours, continue to heat and react to dehydrate until the material is heated to 210-220 DEG C, during the dehydration, toluene is evaporated, and when no water is dehydrated from the reaction material, the reaction is completed; cool to 60 DEG C, add 80 mL of methanol, cool to room temperature, and filter;

[0104] Step 2, transfer the filter cake into a three-necked flask, add 100 mL of methanol, heat to 60 DEG C, stir for 0.5 h, cool to room temperature, and filter;

[0105] Step 3, repeat step 2, and dry the filter cake in an oven at 105 DEG C for 1 h;

[0106] Step 4, recrystallize to obtain the fluorescent agent solid, and the reaction formula is as shown in Figure 3 ;

[0107] Step 5, weigh the Y-type fluorine oil with a viscosity of 1000 mm2 / s at 40 DEG C, uniformly mix with polytetrafluoroethylene with a median particle size of 1 microns at a ratio of 3:7, then pass through three-roller grinding for two times, and use as the base fat; wherein the molecular structural formula of the Y-type fluorine oil is formula (VIII);

[0108] Step 6, sequentially weigh the fluorine solvent, the base fat, the remaining fluorine oil, and the fluorescent agent in a container according to the proportion, and high-speed disperse for 3-10 minutes;

[0109] Step 7, filter through a 300 mesh screen, and package as the fluorescent dry lubricant finished product.

[0110]

Example 4

[0111] The example prepares a fluorescent dry lubricant and a preparation method thereof, and the preparation raw material components and mass fractions of the lubricant of the example are as follows:

[0112] Fluorescent agent 0.02%;

[0113] Perfluoropolyether oil (M-type fluorine oil) 5%;

[0114] Trifluorotrichloroethane 20%;

[0115] Methoxy nonafluorobutyl ether residual amount;

[0116] The preparation method comprises the following steps:

[0117] Step 1, prepare the acid, phenol, boric acid, trichlorobenzene and toluene in a molar ratio of 1:2.1:0.10:3.0:3.0, wherein the boric acid is used as a catalyst; sequentially add the phenol, acid and catalyst into a four-necked flask provided with a reflux condenser, a thermometer, an air inlet pipe and a stirring rod, then pump the toluene into the feeding kettle, open the stirring to be uniform, then introduce 99.9% nitrogen into the flask to prevent the material from being oxidized, then heat the material to 140-160 DEG C, and start the condensation dehydration reaction for 3 hours, continue to heat the reaction to dehydrate, until the material is heated to 210-220 DEG C, during the dehydration, the toluene is evaporated, when there is no water in the reaction material, the reaction is completed; cool to 60 DEG C, add 80 mL of methanol, cool to room temperature, and filter;

[0118] Step 2, transfer the filter cake into a three-necked flask, add 100 mL of methanol, heat to 60 DEG C, stir for 0.5 h, cool to room temperature, and filter;

[0119] Step 3, repeat step 2, and dry the filter cake in an oven at 105 DEG C for 1 h;

[0120] Step 4, recrystallize to obtain the fluorescent agent solid; the reaction formula is shown in Figure 4 .

[0121] Step 5, weigh the M-type fluorine oil with a viscosity of 30 mm2 / s at 40 DEG C, uniformly mix the M-type fluorine oil with polytetrafluoroethylene with a median particle size of 1 microns at a ratio of 3:7, then grind the mixture by three-roller grinding for two times, and use the mixture as a base fat;

[0122] Step 6, sequentially weigh the fluorine solvent, M-type fluorine oil and fluorescent agent according to the proportion, and add the fluorine solvent, M-type fluorine oil and fluorescent agent into a container and disperse at a high speed for 3-10 minutes;

[0123] Step 7, filter through a 300 mesh screen, and package to obtain a fluorescent dry lubricant product.

[0124]

Example 5

[0125] The example prepares a fluorescent dry lubricant and a preparation method thereof, and the preparation raw material components and mass fractions of the lubricant of the example are as follows:

[0126] Fluorescent agent 0.02%;

[0127] Perfluoropolyether oil (M-type fluorine oil) 5%;

[0128] Pentafluorobutane 10%;

[0129] Methoxy nonafluorobutyl ether in an amount;

[0130] The preparation method comprises the following steps:

[0131] Step 1, prepare the acid, phenol, boric acid, trichlorobenzene, toluene in a molar ratio of 1:2.1:0.10:3.0:3.0, wherein the boric acid is used as a catalyst; add the phenol, acid, and catalyst into a four-necked flask in sequence, which is equipped with a reflux condenser, a thermometer, a gas inlet tube, and a stirring rod, then pump toluene into the feeding kettle, start stirring, and then pass 99.9% nitrogen into the flask to prevent the material from being oxidized, then heat the material to 140-160°C, and start the condensation dehydration reaction for 3 hours, continue to heat and react to dehydrate until the material is heated to 210-220°C, during the dehydration process, toluene is evaporated, and when there is no water in the reaction material, the reaction is completed; cool to 60°C, add 80 mL of methanol, cool to room temperature, and filter;

[0132] 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;

[0133] Step 3, repeat Step 2, and dry the filter cake in an oven at 105°C for 1 h;

[0134] Step 4, recrystallize to obtain the solid fluorescent agent; the reaction formula is as shown in Figure 5 ;

[0135] Step 5, weigh M-type fluorine oil with a viscosity of 30 mm2 / s at 40°C, mix evenly with polytetrafluoroethylene with a median particle size of 1 micrometer at a ratio of 3:7, pass through a three-roll mill for two passes, and use as a base fat; wherein the molecular structure of the M-type fluorine oil is formula (IX);

[0136] Step 6, weigh the fluorine solvent, the base fat, the remaining fluorine oil, and the fluorescent agent in a container in proportion, and disperse at high speed for 3-10 minutes;

[0137] Step 7, filter through a 300-mesh sieve, and package as a fluorescent dry lubricant finished product.

[0138]

Example 6

[0139] A fluorescent dry lubricant and a preparation method thereof are prepared in this example, and the preparation raw material components and mass fractions of the lubricant of this example are as follows:

[0140] Fluorescent agent 0.02%;

[0141] Perfluoropolyether oil (M-type fluorine oil) 5%;

[0142] Ethoxy nonafluorobutyl ether in an amount;

[0143] The preparation method comprises the following steps:

[0144] Step 1, prepare the acid, phenol, boric acid, trichlorobenzene, toluene in a molar ratio of 1:2.1:0.10:3.0:3.0, wherein the boric acid is used as a catalyst; add the phenol, acid, and catalyst into a four-necked flask in sequence, which is equipped with a reflux condenser, a thermometer, a gas inlet tube, and a stirring rod, then pump toluene into the feeding kettle, start stirring, and then pass 99.9% nitrogen into the flask to prevent the material from being oxidized, then heat the material to 140-160°C, and start the condensation dehydration reaction for 3 hours, continue to heat and react to dehydrate until the material is heated to 210-220°C, and toluene is evaporated during the dehydration, and the reaction is completed when no water is generated in the reaction material; cool to 60°C, add 80 mL of methanol, cool to room temperature, and filter;

[0145] 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;

[0146] Step 3, repeat Step 2, and dry the filter cake in an oven at 105°C for 1 h;

[0147] Step 4, recrystallize to obtain the fluorescent agent solid; the reaction formula is shown in Figure 6 ;

[0148] Step 5, weigh the M-type fluorine oil with a viscosity of 30 mm2 / s at 40°C, and then weigh the fluorine solvent in proportion, and then add the fluorine oil and the fluorescent agent into a container and disperse at a high speed for 3-10 minutes; wherein the molecular structural formula of the M-type fluorine oil is formula (IX);

[0149] Step 6, filter through a 300-mesh sieve, and package as a fluorescent dry lubricant product.

[0150]

Comparative Example 1

[0151] A fluorescent dry lubricant and a preparation method thereof are prepared in this example, and the preparation raw material components and mass fractions of the lubricant of this example are as follows:

[0152] OP fluorescent agent 0.01%;

[0153] Perfluoropolyether oil (M-type fluorine oil) 5%;

[0154] Ethoxy nonafluorobutyl ether in an amount;

[0155] The preparation method comprises the following steps:

[0156] Step 5, weigh the M-type fluorine oil with a viscosity of 30 mm2 / s at 40°C, and then weigh the fluorine solvent in proportion, and then add the fluorine oil and the fluorescent agent into a container and disperse at a high speed for 3-10 minutes; wherein the molecular structural formula of the M-type fluorine oil is formula (IX);

[0157] Step 2, filter through a 300-mesh sieve, and package as a fluorescent dry lubricant product.

[0158] Example 2

[0159] A fluorescent dry lubricant and its preparation method are prepared in this example. The raw material components and their mass fractions of the lubricant prepared in this example are as follows:

[0160] 0.01% of OP fluorescent agent;

[0161] 5% of perfluoropolyether oil (Y type fluorine oil);

[0162] 1% of polytetrafluoroethylene

[0163] the balance of ethoxy nonafluorobutyl ether;

[0164] The preparation method comprises the following steps:

[0165] Step 1, Y type fluorine oil with a viscosity of 1000 mm2 / s at 40℃ is mixed with polytetrafluoroethylene with a median particle size of 1 micron at a ratio of 3:7, and then ground by three rollers for two times to obtain a base fat for standby; wherein the molecular structural formula of the Y type fluorine oil is formula (VIII);

[0166] Step 2, the fluorine solvent, the base fat, the remaining fluorine oil and the fluorescent agent are weighed according to the proportion and added into a container, and then dispersed at a high speed for 3-10 minutes;

[0167] Step 3, after 300 mesh filtration, the product is packaged as a fluorescent dry lubricant.

[0168] Example 3

[0169] A fluorescent dry lubricant and its preparation method are prepared in this example. The raw material components and their mass fractions of the lubricant prepared in this example are as follows:

[0170] 5% of perfluoropolyether oil (M type fluorine oil);

[0171] the balance of ethoxy nonafluorobutyl ether;

[0172] The preparation method comprises the following steps:

[0173] M type fluorine oil with a viscosity of 30 mm2 / s at 40℃ is weighed, and then the fluorine solvent and the fluorine oil are weighed according to the proportion and added into a container, and then dispersed at a high speed for 3-10 minutes; wherein the molecular structural formula of the M type fluorine oil is formula (IX);

[0174] Step 6, after 300 mesh filtration, the product is packaged as a fluorescent dry lubricant.

[0175] Example 4

[0176] A fluorescent dry lubricant and its preparation method are prepared in this example. The raw material components and their mass fractions of the lubricant prepared in this example are as follows:

[0177] Perfluoropolyether oil (Y type fluorine oil) 5%;

[0178] Polytetrafluoroethylene 1%

[0179] Ethoxy nonafluorobutyl ether balance;

[0180] The preparation method comprises the following steps:

[0181] Step 1, Y type fluorine oil with viscosity of 1000 mm2 / s at 40 DEG C is weighed, mixed with polytetrafluoroethylene with median particle size of 1 microns at 3:7, uniformly mixed, and then ground by three rollers for two times to serve as base grease; wherein, the molecular structural formula of the Y type fluorine oil is formula (VIII);

[0182] Step 2, fluorine solvent, base grease and residual fluorine oil are weighed according to the proportion, added into a container, and dispersed at high speed for 3-10 minutes;

[0183] Step 3, after 300 mesh filtration, the product is packaged as fluorescent dry lubricant.

[0184] Performance detection result:

[0185]

[0186] It is apparent to those skilled in the art that the present application is not limited to the details of the foregoing exemplary embodiments, but can be implemented in other concrete forms without departing from the spirit or essential characteristics of the present application. Therefore, the embodiments should be considered in all respects as illustrative and not restrictive, the scope of the present application being defined by the appended claims rather than the foregoing description, and it is intended that all changes falling within the meaning and range of equivalency of the claims be embraced therein.

Claims

1. A fluorescent dry lubricant, characterized by, The composition comprises the following components by mass fraction: 0.001%-0.1% fluorescent agent 2%-10% fluorine oil 0%-10% polytetrafluoroethylene the rest is fluorine solvent. The structural formula of the fluorescent agent is: （Ⅰ） In the formula, R1 and R2 are one or both of the following molecular structural formula (II)~molecular structural formula (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）； In the formula, n is a natural number ranging from 1 to 5.

2. A fluorescent dry lubricant according to claim 1, characterised in that, The fluorine oil is a perfluoropolyether oil, and the kinematic viscosity of the perfluoropolyether oil at a temperature of 40°C ranges from 10 mm2 / s to 3500 mm2 / s.

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

4. The fluorescent dry lubricant of claim 1, wherein, The median particle size of the polytetrafluoroethylene ranges from 0.1 microns to 100 microns.

5. The fluorescent dry lubricant of claim 1, wherein, 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.

6. A process for the preparation of a fluorescent dry lubricant for the preparation of a fluorescent dry lubricant according to any one of claims 1 to 5, characterized in that, The method comprises the following steps: Step 1: A four-necked flask is provided with a reflux condenser, a thermometer, an air inlet pipe, and a stirring rod. Phenyltrichloride, phenol, acid, and a catalyst are sequentially added to the flask, and then toluene is pumped into the flask. After stirring, 99.9% nitrogen is introduced into the flask to prevent oxidation of the materials. The materials are then heated to 140-180°C, and condensation and dehydration reactions begin to occur. The temperature is continuously increased until the materials reach 210-250°C, and toluene is evaporated. When no water is produced, the reaction is complete. The temperature is then reduced to 50-60°C, and 80-100 mL of methanol is added. After cooling to room temperature, the mixture is filtered. Step 2: The filter cake is transferred to a three-necked flask, 80-100 mL of detergent is added, and the temperature is increased to 50-60°C. After stirring for 0.5 h, the mixture is cooled to room temperature and filtered. Step 3: Step 2 is repeated, and the filter cake is dried in an oven at 100-105°C for 1-2 h. Step 4: The filter cake is recrystallized to obtain a light green-yellow solid fluorescent agent. Step 5: Polytetrafluoroethylene and fluorine oil are weighed and mixed in a ratio of 1:1-3. After stirring, the mixture is passed through a three-roll mill twice and is ready for use. Step 6: The fluorescent agent prepared in Step 4 and fluorine solvent are mixed in a ratio of 0.1-3:100 to prepare a fluorescent agent solution, which is ready for use. Step 7: The materials prepared in Steps 5 and 6 are added to a container in a certain proportion, and are stirred at high speed to disperse uniformly. Step 8: The material obtained in Step 7 is filtered and packaged to obtain a fluorescent dry lubricant.

7. A process for the preparation of a fluorescent dry lubricant according to claim 6, 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.

8. A process for the preparation of a fluorescent dry lubricant as claimed in claim 6, wherein, The catalyst is boric acid, and the washing agent includes one of dimethylformamide, methanol, petroleum ether, and ethanol.

9. A process for the preparation of a fluorescent dry lubricant according to claim 8, characterized in that, The molar ratio of the five substances, acid, phenol, boric acid, benzene trichloride, and methylbenzene, is 1:2.0-2.5:0.10-0.25:3.0-4.0:3.0-4.0.

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