CN113150859B - Environment-friendly carbon-nitrogen-based water-based lubricant and preparation method thereof - Google Patents

Environment-friendly carbon-nitrogen-based water-based lubricant and preparation method thereof Download PDF

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CN113150859B
CN113150859B CN202110374596.1A CN202110374596A CN113150859B CN 113150859 B CN113150859 B CN 113150859B CN 202110374596 A CN202110374596 A CN 202110374596A CN 113150859 B CN113150859 B CN 113150859B
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lubricant
auxiliary agent
carbon
water
nitrogen
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CN113150859A (en
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蒋炜
贾璐菡
吴潘
刘长军
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Sichuan University
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Sichuan University
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M173/00Lubricating compositions containing more than 10% water
    • C10M173/02Lubricating compositions containing more than 10% water not containing mineral or fatty oils
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/061Carbides; Hydrides; Nitrides
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/062Oxides; Hydroxides; Carbonates or bicarbonates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08Inorganic acids or salts thereof
    • C10M2201/081Inorganic acids or salts thereof containing halogen

Abstract

The invention discloses an environment-friendly carbon-nitrogen-based water-based lubricant and a preparation method thereof, wherein the lubricant comprises water and carbonitride powder uniformly dispersed in the water, and the mass percent of the carbonitride in the lubricant is 0.01-8%; the carbonitride powder is obtained by washing a product formed by calcining a mixed material of a carbonitride precursor and an auxiliary agent I with water to remove free auxiliary agent I, wherein the content of the auxiliary agent I is 12-71% of the total mass of the carbonitride precursor and the auxiliary agent I. According to the environment-friendly carbon-nitrogen-based water-based lubricant, the carbonitride powder is used as the only component, so that the basic lubricant not only has excellent lubricating property (Pb value can reach 40 kg), high-stability dispersion, corrosion resistance, rust resistance, high temperature resistance and other properties, but also has properties of super-hydrophilicity, hygroscopicity, moisture retention, emulsification and other multifunctional applications; on the basis of the basic lubricant, the corresponding performance can be further improved by adding an auxiliary agent II, an auxiliary agent III or an auxiliary agent IV.

Description

Environment-friendly carbon-nitrogen-based water-based lubricant and preparation method thereof
Technical Field
The invention belongs to the technical field of liquid lubricants, and relates to a carbon-nitrogen-based water-based lubricant and a preparation method thereof.
Background
In the industrial field, lubricants play a crucial role in reducing friction, wear, mechanical damage of contact pairs and in improving energy efficiency and productivity. Currently, liquid lubricants in common use are largely classified into oil-based lubricants and water-based lubricants. Oil-based lubricants have good lubricating effects, but also have the following problems: (1) The oil-based lubricant has poor cooling effect in the using process, so that the service life of the die is influenced; (2) The oil-based lubricant is inflammable and easy to carbonize, and has potential storage safety hazards; (3) Oil-based lubricants are difficult to clean, resulting in high post-use treatment costs; (4) Oil-based lubricants are also prone to deterioration of the working environment, environmental pollution, and the like.
Therefore, with the development of economy, the environmental and energy problems become more serious, and the water-based lubricant is concerned about the advantages of energy conservation, environmental pollution reduction, oil stain and waste reduction, good water cooling performance, safety and the like; meanwhile, the water-based lubricant has the functions of cooling, lubricating, cleaning, corrosion resistance, film forming, rust prevention and the like, and is commonly used in metal cutting and processing processes, stamping processes, hydraulic systems and the like.
There are some current research reports on water-based lubricants, such as: (1) The patent CN110066357A discloses a fluorine-containing super-lubricating water-based acrylic resin, which is prepared by diluting grease and ester substances with water to obtain a mixed monomer, and then dropwise adding the mixed monomer and an initiator into tertiary carbonic acid glycidyl ester together for polymerization reaction; (2) Patent CN106047461a discloses an aqueous environment-friendly pollution-free high-temperature graphite lubricating coating, which is obtained by uniformly dispersing graphite with a lubricating effect, nano-silica powder, a surfactant and other auxiliaries. Although the existing water-based lubricant is improved more than an oil-based lubricant in terms of environmental protection and the like, a plurality of problems still exist: (1) The performances of dispersion stability, corrosion resistance and the like of the lubricant are improved by adding a plurality of auxiliary agents, so that the lubricant has complex components and high cost, the preparation difficulty is increased, the process steps are very complicated, and the popularization and the use are not facilitated; (2) The components such as ester, grease and graphite are easy to carbonize, the COD value is high, the treatment is difficult, and the direct discharge easily causes environmental pollution.
It is because of the aforementioned shortcomings that water-based lubricants have, which has restricted further development of water-based lubricants. Therefore, the research on the water-based lubricant which is environment-friendly and has high performance has important significance in the field of industrial manufacturing.
Disclosure of Invention
Aiming at the defects of the existing water-based lubricant and the preparation process thereof, the invention aims to provide the environment-friendly carbon-nitrogen-based water-based lubricant and the preparation method thereof.
The environment-friendly carbon-nitrogen-based water-based lubricant provided by the invention comprises water and carbonitride powder uniformly dispersed in the water, wherein the mass percent of the carbonitride in the lubricant is 0.01-8%; the carbonitride powder is obtained by washing a product formed by calcining a mixed material of a carbonitride precursor and an additive I with water to remove free additive I, wherein the content of the additive I is 12-71% of the total mass of the carbonitride precursor and the additive I, and the additive I is a metal halide or a mixed material of the metal halide and a nano oxide.
The water in the environment-friendly carbon-nitrogen-based water-based lubricant can be selected from tap water, deionized water or distilled water according to the use object.
The environment-friendly carbon-based aqueous lubricant has multifunctional properties such as lubrication wear resistance, corrosion resistance, temperature resistance, rust resistance, super-hydrophilicity, hygroscopicity, moisture retention and emulsibility. Other functional additives can be added into the environment-friendly carbon-based water-based lubricant to further improve the application characteristics of the lubricant such as lubricating wear resistance, corrosion resistance, temperature resistance and the like. The functional auxiliary agent is an auxiliary agent II for promoting wear resistance and corrosion resistance, an auxiliary agent III for promoting rust resistance or/and an auxiliary agent IV with water-soluble color characteristic. The volume percentage of the auxiliary agent II in the lubricant is 0.03-30%, and the preferred volume percentage is 0.06-3%; the mass percentage of the auxiliary agent III in the lubricant is 1-20%; the mass percentage of the auxiliary agent IV in the lubricant is 0.05-2.5%. The auxiliary agent II is at least one of waterborne polyurethane, waterborne fluorocarbon, waterborne soap solution, triethyl phosphate and polyacrylamide; the wear resistance and corrosion resistance of the lubricant can be further improved by the aid of the auxiliary agent II. The auxiliary agent III is at least one of sodium dodecyl sulfate, sodium citrate, sodium tungstate, sodium sulfite and sodium nitrite; the rust resistance can be enhanced by adding the aid III. The auxiliary agent IV is a water-soluble color material, and the water-soluble color material is not particularly limited and can be water-soluble color materials which are conventionally used in the field, such as methylene blue, rhodamine B, congo red and the like; the addition of the water-soluble color material can obtain the color lubricant, thereby having better color adaptability and wider application environment.
In the above environment-friendly aqueous carbonitride-based lubricant, the carbonitride precursor may be a precursor for preparing a carbonitride, and may be at least one of analytically pure or industrial grade urea, melamine, dicyandiamide, cyanamide, cyanuric acid, thiourea, and biuret. The metal halide of the aid I is preferably single salt or double salt of more than two of potassium bromide, sodium chloride, potassium iodide, potassium chloride, sodium bromide, lithium chloride and the like. The nano oxide is at least one of silicon dioxide, titanium dioxide, magnesium oxide, tin dioxide, copper oxide, zirconium oxide, bismuth oxide and aluminum oxide.
The invention also provides a preparation method of the environment-friendly carbon-nitrogen-based water-based lubricant, which comprises the following steps:
(1) Uniformly mixing a carbon nitride precursor and an auxiliary agent I according to the set proportion to form a mixed material, and calcining the mixed material at 400-600 ℃ for 0.5-6 h to obtain a calcined product containing carbon nitride powder;
(2) Washing a calcined product containing carbonitride powder with water until the mass percentage of the carbonitride in the washing liquid is 0.08-1%, wherein the obtained washing liquid is a first-level carbon-nitrogen-based aqueous lubricant;
(3) And drying the solid phase material obtained by cleaning, and then uniformly dispersing the dried powdery solid phase material into water according to the mass percent of carbon nitride in the lubricant being 0.01-8%, thus obtaining the secondary carbon nitrogen-based water-based lubricant with the mass percent of carbon nitride being 0.01-8%.
In the preparation method of the environment-friendly carbon-nitrogen-based aqueous lubricant, in the step (2), the cleaning mode can be suction filtration, sedimentation, ultrasonic, centrifugation and the like. The cleaning aims to remove free auxiliary agent I so as to recover and clean the auxiliary agent I in the obtained filtrate, reduce the pollution to the environment, improve the utilization rate of raw materials and reduce the production cost. The water used for cleaning is not particularly required, and may be tap water, distilled water or deionized water.
In the step (3), the water used is not particularly required, and may be tap water, distilled water or deionized water.
The research shows that the primary carbon-based water-based lubricant and the secondary carbon nitrogen-based water-based lubricant have excellent wear resistance, corrosion resistance and the like, have low COD value and have good environmental protection property besides the stability superior to the traditional water-based lubricant.
In the step (3), the drying may be performed by a conventional drying method in the art, and preferably, the drying method is freeze drying or oven drying, and the drying time is 8 to 24 hours.
The obtained first-stage or second-stage aqueous lubricant also has properties of super-hydrophilicity, hygroscopicity, moisture retention, emulsification and other multifunctional applications. And other functional additives can be further added into the first-stage carbon-based water-based lubricant or the second-stage carbon nitrogen-based water-based lubricant, so that the application characteristics of the lubricants such as wear resistance, lubricity, corrosion resistance, temperature resistance and the like are further improved.
When the lubricant further comprises an auxiliary agent II, the preparation method of the environment-friendly carbon-nitrogen-based water-based lubricant further comprises the following steps:
(4) Uniformly dispersing the auxiliary agent II in the carbon-nitrogen-based lubricant obtained in the step (2) and the step (3) to obtain the carbon-nitrogen-based lubricant added with the auxiliary agent II; the volume percentage of the auxiliary agent II in the lubricant is 0.03-30%;
when the lubricant further comprises an auxiliary agent III, the following steps are further included:
(5) Uniformly dispersing the aid III in the carbon-nitrogen-based lubricant obtained in the step (2), the step (3) and the step (4) to obtain the carbon-nitrogen-based lubricant added with the aid III; the mass percentage of the auxiliary agent III in the lubricant is 1-20%;
when the lubricant further comprises an auxiliary agent IV, the method further comprises the following steps:
(6) Uniformly dispersing the aid IV into the carbon-nitrogen-based lubricant obtained in the steps (2), (3), (4) and (5) to obtain the carbon-nitrogen-based lubricant added with the aid IV; the mass percentage of the auxiliary agent IV in the lubricant is 0.05-2.5%.
The invention provides an environment-friendly carbon-nitrogen-based water-based lubricant and a preparation method thereof, and the innovation points are as follows: by adding metal halide or a mixed material of metal halide and nano oxide into a carbonitride precursor, the regulation and control of the surface charge strength and the particle size of the carbonitride powder obtained by calcination can be realized, and polar groups are enhanced, so that the prepared basic lubricant (namely the lubricant which is prepared by only water and carbonitride powder uniformly dispersed in water without adding auxiliary agents II, III or IV) shows excellent lubricant application characteristics such as wear resistance, corrosion resistance, temperature resistance and the like, and other multifunctional application properties such as super-hydrophilicity, hygroscopicity, moisture retention, emulsification and the like. And an auxiliary agent II, an auxiliary agent III or an auxiliary agent IV is added on the basis of the basic lubricant, so that the anti-rust or colored lubricant with more excellent wear resistance and corrosion resistance can be further obtained. The lubricant has environmental protection property with extremely low COD value, and can basically reach 0 mg.L through simple treatment -1 The high environmental protection standard of COD value discharge can be used for the lubrication of synthetic cutting fluid, rolling bearings and sliding bearings of various mechanical equipment and other friction parts, and can also be used for corresponding coatings with other multifunctional properties.
Compared with the prior art, the environment-friendly carbon-nitrogen-based water-based lubricant and the preparation method thereof provided by the invention have the following beneficial effects that:
(1) In the invention, the basic lubricant obtained by dispersing the carbonitride powder as the only component in water not only has excellent lubricity (Pb value can reach 40 kg), corrosion resistance, rust resistance, high temperature resistance and other performances, but also has other performances of multifunctional application such as super-hydrophilicity, hygroscopicity, moisture retention, emulsification and the like, and has very strong practical value; on the basis of the basic lubricant, the corresponding performance can be improved again by adding the auxiliary agent II, the auxiliary agent III or the auxiliary agent IV, and the regulation and control are applied to different environments and conditions with different deviation requirements, so that the lubricant has strong environmental applicability.
(2) The environment-friendly carbon-nitrogen-based water-based lubricant disclosed by the invention is simple in composition, small in component particle size and very excellent in dispersion stability (the zeta potential absolute value can reach 6)5 mV), thus ensuring good performance stability; the carbon-nitrogen-based solid component has high thermal stability and chemical stability, and the high temperature resistance and the environmental applicability of the lubricant can be improved; the lubricant has COD value at least 250 times lower than that of many commercial water-base lubricant products in the current market, and basically reaches 0 mg.L except the lubricant added with the auxiliary agent II through simple flocculation treatment -1 High environmental protection standard of COD value discharge.
(3) The carbonitride powder prepared by the environment-friendly carbon-nitrogen-based aqueous lubricant disclosed by the invention is beneficial to regulation and control of different concentration contents, and in addition, carbonitride precursors such as urea, melamine and the like and several auxiliaries are stable in chemical properties, wide in source, low in price and easy to obtain, so that the production cost is low.
(4) The preparation method of the environment-friendly carbon-nitrogen-based water-based lubricant has a simple formula, and the lubricant can be obtained only through operations such as calcination, mixing and the like, so that the preparation process is simple, the used equipment is conventional equipment, the energy consumption is low, the production period is short, and large-scale batch production is easy to realize.
Drawings
FIG. 1 is a graph of ZETA potential and particle size of base lubricant I prepared in example 1 of the present invention and a lubricant prepared in a comparative example.
FIG. 2 is a thermogram of a powdery solid phase material of a secondary product of the preparation of base lubricant I according to example 1 of the present invention.
FIG. 3 is an IR spectrum obtained by drying the solid-phase material washed in example 1 of the present invention and the solid-phase material washed in comparative example and then performing IR characterization.
FIG. 4 is a PB plot of base lubricant I and lubricant II prepared in example 1 of the present invention.
FIG. 5 is a graph showing the results of stability tests on base lubricants I and II prepared in example 1 of the present invention.
FIG. 6 is a graph of the corrosion resistance effect of base lubricant I and DI water prepared in example 1 of the present invention.
FIG. 7 is a graph showing the rust inhibitive effect of the secondary product of base lubricant I, the secondary product of lubricant III, and deionized water prepared in example 1 of the present invention.
FIG. 8 is a graph showing the results of the super-affinity and optical filtering tests on the surface of the first-class base lubricant I and the first-class lubricant IV prepared in example 1.
FIG. 9 is a graph showing the effect of emulsifying solid phase material in powder form after drying the solid phase material washed in example 1 of the present invention.
Fig. 10 is a graph showing moisturizing effects of the base lubricant i and deionized water prepared in example 1 of the present invention.
Detailed Description
So that the technical solutions of the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings, it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, belong to the present invention.
The raw materials used in the following examples, such as urea, melamine, dicyandiamide, sodium chloride, potassium bromide, and nanosilica, were all commercially available.
In the following examples, in order to distinguish lubricants prepared by adding different additives, a lubricant prepared from water and carbonitride powder uniformly dispersed in water (without adding additives II, III or IV) was referred to as a base lubricant I, in which a lubricant formed from a cleaning liquid was referred to as a primary product of the base lubricant I and a lubricant formed from a dried powdery solid-phase material dispersed in water was referred to as a secondary product of the base lubricant I; the lubricant added with the auxiliary agent II in the base lubricant I is called lubricant II, wherein the lubricant added with the auxiliary agent II in the primary product of the base lubricant I is called the primary product of the lubricant II, and the lubricant added with the auxiliary agent II in the secondary product of the base lubricant I is called the secondary product of the lubricant II; the lubricant added with the auxiliary agent III in the base lubricant I is called a lubricant III, wherein the lubricant added with the auxiliary agent III in the primary product of the base lubricant I is called a primary product of the lubricant III, and the lubricant added with the auxiliary agent III in the secondary product of the base lubricant I is called a secondary product of the lubricant III; the lubricant added with the auxiliary agent IV in the base lubricant I is called a lubricant IV, wherein the lubricant added with the auxiliary agent IV in the first-stage product of the base lubricant I is called a first-stage product of the lubricant IV, and the lubricant added with the auxiliary agent IV in the second-stage product of the base lubricant I is called a second-stage product of the lubricant IV; the lubricant added with at least two of the auxiliary agent II, the auxiliary agent III and the auxiliary agent IV in the basic lubricant I is called a multi-auxiliary agent lubricant, wherein the lubricant added with at least two of the auxiliary agent II, the auxiliary agent III and the auxiliary agent IV in the primary product of the basic lubricant I is called a primary product of the multi-auxiliary agent lubricant, and the lubricant added with at least two of the auxiliary agent II, the auxiliary agent III and the auxiliary agent IV in the secondary product of the basic lubricant I is called a secondary product of the multi-auxiliary agent lubricant.
Example 1
The base lubricant I, lubricant II, lubricant III, and lubricant IV provided in this example were prepared by the following steps:
(1) Uniformly mixing urea and potassium chloride to form a mixed material, wherein the content of potassium chloride is 37% of the total mass of the urea and the potassium chloride, and then carrying out heat preservation and calcination on the mixed material at 520 ℃ for 4h to obtain a calcined product containing carbonitride powder;
(2) Ultrasonically cleaning a calcined product containing carbonitride powder by using deionized water, wherein the usage amount of the deionized water is 15mL/g (15 mL of the deionized water is used for each g of the calcined product) during each cleaning, and obtaining 6 th cleaning liquid to obtain a first-grade product of a basic lubricant I with the mass percent of carbonitride of about 0.08%;
(3) Drying the solid phase material obtained by cleaning at 80 ℃ for 12h, and uniformly dispersing the dried powdery solid phase material in deionized water according to the proportion of 0.4g/L (0.4 g of powdery solid phase material is dispersed in each 1L of deionized water), thus obtaining a secondary product of the basic lubricant I with the mass percent of carbonitride of about 0.04%;
(4) Respectively and uniformly dispersing waterborne polyurethane into the primary product of the basic lubricant I and the secondary product of the basic lubricant I obtained in the steps (2) and (3) to obtain a primary product of the lubricant II and a secondary product of the lubricant II; the volume percentage of the aqueous polyurethane in the first-stage product of the lubricant II and the second-stage product of the lubricant II is about 0.3 percent;
(5) Uniformly dispersing sodium citrate into the primary product of the base lubricant I and the secondary product of the base lubricant I obtained in the steps (2) and (3) respectively to obtain a primary product of a lubricant III and a secondary product of a lubricant III; the mass percent of the sodium citrate in the first-stage product of the lubricant III and the second-stage product of the lubricant III is about 3 percent;
(6) Uniformly dispersing methylene blue into the primary product of the basic lubricant I and the secondary product of the basic lubricant I obtained in the steps (2) and (3) respectively to obtain a first primary product of a lubricant IV and a first secondary product of the lubricant IV; the mass percent of methylene blue in the first stage product of lubricant IV and the first second stage product of lubricant IV is about 0.1%;
(7) Uniformly dispersing Congo red into the primary product of the base lubricant I and the secondary product of the base lubricant I obtained in the steps (2) and (3) respectively to obtain a second primary product of the lubricant IV and a second secondary product of the lubricant IV; the Congo Red is about 0.1% by mass of the second primary product of lubricant IV and the second secondary product of lubricant IV;
(8) Uniformly dispersing rhodamine B into the primary product of the basic lubricant I and the secondary product of the basic lubricant I obtained in the steps (2) and (3) respectively to obtain a third primary product of the lubricant IV and a third secondary product of the lubricant IV; the percentage by mass of rhodamine B in the third primary product of lubricant iv and the third secondary product of lubricant iv is about 0.1%.
Example 2
This example provides a base lubricant I, lubricant II, lubricant III, and lubricant IV prepared by the following steps:
(1) Uniformly mixing melamine with sodium chloride and potassium chloride double salt to form a mixed material, wherein the content of the sodium chloride and the potassium chloride is 12% of the total mass of the melamine, the sodium chloride and the potassium chloride (the mass ratio of the sodium chloride to the potassium chloride is 1.91), and then, carrying out heat preservation calcination on the mixed material at 600 ℃ for 0.5h to obtain a calcined product containing carbonitride powder;
(2) Performing suction filtration and cleaning on a calcined product containing carbonitride powder by using deionized water, wherein the usage amount of the deionized water is 10mL/g (10 mL of the deionized water is used for each g of the calcined product) during each cleaning, and obtaining a 5 th cleaning solution to obtain a primary product of a basic lubricant I with the mass percent of carbonitride of about 0.1%;
(3) Drying the solid phase material obtained by cleaning at 80 ℃ for 8h, and uniformly dispersing the dried powdery solid phase material in deionized water according to the proportion of 0.2g/L (0.2 g of powdery solid phase material is dispersed in every 1L of deionized water), thus obtaining a secondary product of the basic lubricant I with the mass percent of carbonitride of about 0.02%;
(4) Uniformly dispersing water-based fluorocarbon into the primary product of the basic lubricant I and the secondary product of the basic lubricant I obtained in the steps (2) and (3) respectively to obtain a primary product of the lubricant II and a secondary product of the lubricant II; the volume percent of the water fluorocarbon in the first-stage product of the lubricant II and the second-stage product of the lubricant II is about 0.03 percent;
(5) Uniformly dispersing sodium tungstate into the primary product of the base lubricant I and the secondary product of the base lubricant I obtained in the steps (2) and (3) respectively to obtain a primary product of the lubricant III and a secondary product of the lubricant III; the mass percent of sodium tungstate in the first-grade product of the lubricant III and the second-grade product of the lubricant III is about 10 percent;
(6) Uniformly dispersing Congo red into the primary product of the basic lubricant I and the secondary product of the basic lubricant I obtained in the steps (2) and (3) respectively to obtain a primary product of a lubricant IV and a secondary product of the lubricant IV; the percentage by mass of Congo red in the first-class product of lubricant IV and the second-class product of lubricant IV is about 0.05%.
Example 3
The base lubricant I, lubricant II, lubricant III, and lubricant IV provided in this example were prepared by the following steps:
(1) The preparation method comprises the following steps of uniformly mixing dicyandiamide, sodium chloride, potassium bromide and nano-silica double salt to form a mixed material, wherein the contents of the sodium chloride, the potassium bromide and the nano-silica are 71% of the total mass of the dicyandiamide, the sodium chloride, the potassium bromide and the nano-silica (the mass ratio of the sodium chloride to the potassium bromide to the nano-silica is 23.4;
(2) Centrifugally cleaning the calcined product containing the carbonitride powder by using tap water, wherein the using amount of the tap water is 3mL/g (3 mL of tap water is used for each g of calcined product) during each cleaning, and obtaining a 3 rd cleaning solution to obtain a first-grade product of a basic lubricant I with the carbonitride mass percentage of about 0.8%;
(3) Drying the solid phase material obtained by cleaning at 80 ℃ for 24h, and uniformly dispersing the dried powdery solid phase material in tap water according to the proportion of 40g/L (40 g of the powdery solid phase material is dispersed in every 1L of tap water), thus obtaining a secondary product of the basic lubricant I with the mass percent of carbonitride of about 3.8%;
(4) Respectively and uniformly dispersing waterborne polyurethane into the primary product of the basic lubricant I and the secondary product of the basic lubricant I obtained in the steps (2) and (3) to obtain a primary product of the lubricant II and a secondary product of the lubricant II; the volume percentage of the aqueous polyurethane in the first-stage product of the lubricant II and the second-stage product of the lubricant II is about 30 percent;
(5) Uniformly dispersing sodium dodecyl sulfate in the primary product of the basic lubricant I and the secondary product of the basic lubricant I obtained in the steps (2) and (3) respectively to obtain a primary product of a lubricant III and a secondary product of a lubricant III; the mass percent of the sodium dodecyl sulfate in the first-grade product of the lubricant III and the second-grade product of the lubricant III is about 15 percent;
(6) Uniformly dispersing rhodamine B into the primary product of the basic lubricant I and the secondary product of the basic lubricant I obtained in the steps (2) and (3) respectively to obtain a primary product of a lubricant IV and a secondary product of the lubricant IV; the mass percent of rhodamine B in the first-grade product of the lubricant IV and the second-grade product of the lubricant IV is about 2 percent.
Example 4
This example provides a base lubricant I, lubricant II, lubricant III, and lubricant IV prepared by the following steps:
(1) The preparation method comprises the following steps of uniformly mixing dicyandiamide, sodium chloride, potassium bromide and nano-silica double salt to form a mixed material, wherein the contents of the sodium chloride, the potassium bromide and the nano-silica are 71% of the total mass of the dicyandiamide, the sodium chloride, the potassium bromide and the nano-silica (the mass ratio of the sodium chloride to the potassium bromide to the nano-silica is 14;
(2) Naturally settling and cleaning a calcined product containing carbonitride powder by using tap water, wherein the using amount of the tap water is 20mL/g (20 mL of the tap water is used for each g of the calcined product) during each cleaning, and obtaining a 5 th cleaning solution to obtain a primary product of a basic lubricant I with the carbonitride mass percentage of about 0.5%;
(3) Drying the solid phase material obtained by cleaning at 80 ℃ for 20h, and uniformly dispersing the dried powdery solid phase material in tap water according to the proportion of 80g/L (80 g of the powdery solid phase material is dispersed in every 1L of tap water), thus obtaining a secondary product of the basic lubricant I with the mass percent of carbonitride of about 7.4%;
(4) Respectively and uniformly dispersing waterborne polyurethane into the primary product of the basic lubricant I and the secondary product of the basic lubricant I obtained in the steps (2) and (3) to obtain a primary product of the lubricant II and a secondary product of the lubricant II; the volume percentage of the aqueous polyurethane in the first-stage product of the lubricant II and the second-stage product of the lubricant II is about 0.06 percent;
(5) Uniformly dispersing sodium dodecyl sulfate in the primary product of the basic lubricant I and the secondary product of the basic lubricant I obtained in the steps (2) and (3) respectively to obtain a primary product of a lubricant III and a secondary product of a lubricant III; the mass percent of the sodium dodecyl sulfate in the first-grade product of the lubricant III and the second-grade product of the lubricant III is about 10 percent;
(6) Uniformly dispersing rhodamine B into the primary product of the basic lubricant I and the secondary product of the basic lubricant I obtained in the steps (2) and (3) respectively to obtain a primary product of a lubricant IV and a secondary product of the lubricant IV; the mass percent of rhodamine B in the first-grade product of the lubricant IV and the second-grade product of the lubricant IV is about 1 percent.
Example 5
(1) Uniformly mixing dicyandiamide, sodium chloride and nano-silica double salt to form a mixed material, wherein the content of sodium chloride and nano-silica is 50% of the total mass of dicyandiamide, sodium chloride and nano-silica (the mass ratio of sodium chloride to nano-silica is 16: 1)), and then carrying out heat preservation calcination on the mixed material at 550 ℃ for 1h to obtain a calcination product containing carbonitride powder;
(2) Ultrasonically cleaning a calcined product containing carbonitride powder by using deionized water, wherein the usage amount of the deionized water is 10mL/g (10 mL of the deionized water is used for each g of the calcined product) during each cleaning, and obtaining a 3 rd cleaning solution to obtain a first-grade product of a basic lubricant I with the mass percent of carbonitride of about 0.25%;
(3) Drying the solid phase material obtained by cleaning at 80 ℃ for 24h, and uniformly dispersing the dried powdery solid phase material in deionized water according to the proportion of 40g/L (40 g of the powdery solid phase material is dispersed in every 1L of the deionized water), thus obtaining a secondary product of the basic lubricant I with the mass percent of carbonitride of about 3.8%;
(4) Uniformly dispersing triethyl phosphate, sodium nitrite and methylene blue into the primary product of the basic lubricant I and the secondary product of the basic lubricant I obtained in the steps (2) and (3) respectively to obtain the primary product and the secondary product of the multi-additive lubricant; in the first-stage product of the multi-additive lubricant and the second-stage product of the multi-additive lubricant, the volume percentage of the triethyl phosphate is about 0.1 percent, the mass percentage of the sodium nitrite is about 8 percent, and the mass percentage of the methylene blue is about 2 percent.
Comparative example
This comparative example was prepared identically to base lubricant I provided in example 1, except that: in the comparative example, the preparation method comprises the following specific steps of:
(1) Calcining urea at 520 ℃ for 4h to obtain carbonitride powder;
(2) Ultrasonically cleaning carbonitride powder by using deionized water, wherein the usage amount of the deionized water is 15mL/g (15 mL of the deionized water is used for each g of the carbonitride powder) during each cleaning, and obtaining 6 th cleaning solution to obtain a first-grade product of a contrast lubricant with the mass percent of the carbonitride of about 0.05%;
(3) And (3) drying the solid phase material obtained by cleaning at 80 ℃ for 12h, uniformly dispersing the dried powdery solid phase material in deionized water according to the proportion of 0.4g/L (0.4 g of powdery solid phase material is dispersed in every 1L of deionized water), and thus obtaining a secondary product of the comparative lubricant with the mass percent of carbonitride of about 0.04%.
The properties of the base lubricant i, the lubricant ii, the lubricant iii and the lubricant iv prepared in example 1 were analyzed with reference to the drawings to further demonstrate the advantages of the aqueous carbon nitrogen-based lubricant provided by the present invention. The water used during the analysis was deionized water.
(1) Stability analysis
The first-stage product and the second-stage product of the base lubricant I prepared in example 1 and the first-stage product and the second-stage product of the comparative lubricant prepared in the comparative example were subjected to Zeta potential and particle size tests, and thermogravimetric analysis was performed on the solid-phase material from which the second-stage product of the base lubricant I was prepared in example 1, the thermogravimetric analysis operation steps being: respectively taking 20mg samples of the lubricant product into crucibles, and respectively heating the samples from 30 ℃ to 1000 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere to perform testing; the results are shown in FIGS. 1-2. As can be seen from FIG. 1, the comparative lubricants prepared in the comparative examples all had a Zeta potential of less than 30mV in absolute value, were very unstable, and the carbonitride had an average particle size of greater than 2 μm and tended to agglomerate and settle. The Zeta absolute value of the base lubricant I obtained in example 1 is greatly improved, and the average grain size of carbonitride is less than 500nm, so that the system dispersion is more stable. The auxiliary agent I is proved to have good adjusting effect on the Zeta potential and the grain diameter of the carbonitride. In fig. 2, the weight loss of the product components is started at about 600 ℃, which shows that the product components have excellent thermal stability, and the carbon-nitrogen-based water-based lubricant provided by the invention can be applied under high-temperature operating conditions such as metal cutting, punching lubrication cooling and the like.
The solid phase material obtained by cleaning in comparative example 1 was dried and then subjected to infrared characterization, and the solid phase material obtained by cleaning in example 1 was dried and then subjected to infrared characterization, and the results are shown in fig. 3. As can be seen from FIG. 3, the solid phase material of example 1 was 3200cm in length relative to the solid phase material described in the comparative example without the addition of auxiliary I -1 And 1425cm -1 The left and right positions showed peak position shift and some peak shape change, still at 2150cm -1 And 980cm -1 A new peak appears. The results in connection with FIG. 1 show that the auxiliary I has a regulating effect on the properties and properties of the carbonitrides.
(2) Wear lubrication analysis
The first-grade product and the second-grade product of the base lubricant I and the lubricant II prepared in example 1 were subjected to a PB value test, and the test results are shown in FIGS. 4 to 5. The PB (maximum non-seizure load) value is an important index of extreme pressure anti-wear performance of the lubricant, and refers to the maximum non-seizure load for preventing the test steel balls from seizure under test conditions. The PB value is also an important performance index of the water-based lubricant in the applications of synthetic cutting fluid, stamping and the like, and the larger the PB value is, the better the extreme pressure anti-wear performance of the material is. If the extreme pressure antiwear performance of the lubricant is not good, the equipment can be seriously abraded. As can be seen from FIG. 4, the base lubricant I prepared in example 1 already has a PB value of more than 20kg, and the lubricant II with the addition of the auxiliary II has a higher PB value, up to 40kg. As can be seen from FIG. 5, the PB value test is performed on the lubricant after the lubricant is placed for a long time, and the result shows that the lubricant has stable lubricating performance in the placement for 90 days, so that the requirements of practical application can be met.
Therefore, the lubricant prepared by the invention has excellent wear-resistant and antifriction effects, can obtain multiple quality types of products, and has good regulation and control performance.
(3) Analysis of Corrosion resistance and Rust resistance
The base lubricant I prepared in example 1 was subjected to an anti-corrosion test in accordance with GB _ T5096-2017, and the results are shown in FIGS. 6 to 7. As can be seen from FIG. 6, compared with the standard color card, the degree of corrosion of deionized water is 3a and 3b, the level of corrosion of the first-grade base lubricant is 1b, and the level of corrosion of the second-grade base lubricant is 2a, which shows that the prepared water-based lubricant has good corrosion resistance without adding an additional antirust agent. Fig. 7 shows the results of rust inhibition tests performed on the third day after iron sheets are immersed in deionized water and the base lubricant i secondary product and the lubricant iii secondary product prepared in example 1, and the experimental results show that the corrosion resistance and rust inhibition of the base lubricant i secondary product and the lubricant iii secondary product prepared in example 1 are enhanced, and the corrosion resistance and rust inhibition of the lubricant iii secondary product are superior to those of the base lubricant i secondary product, and no obvious rust stains appear, compared with deionized water.
The results show that the lubricant provided by the invention has good corrosion resistance and rust resistance, and can meet the performance requirements of the water-based lubricant in the typical application field.
(4) Material surface treatment application analysis
Experiments show that the lubricant prepared in example 1 can be adsorbed on the surface of the material to form a film layer after the material is lubricated and washed, and the film layer has super-hydrophilic properties. As can be seen from fig. 8, the Contact Angle (CA) of the film formed by the primary base lubricant i was 3.2 °. A color film layer can be formed after an auxiliary agent IV (comprising methylene blue, congo red and rhodamine B) is added into a primary product of a basic lubricant I, the primary product of the basic lubricant I prepared in example 1 is used as a dye-free contrast sample, a Uv-Vis (ultraviolet-visible absorption spectrum) photometer is used for carrying out absorbance analysis on a first primary product, a second primary product and a third primary product of the lubricant IV prepared in example 1, and an analysis result is shown in figure 8.
(5) Emulsion application analysis
A powdery solid-phase material obtained by drying the solid-phase material obtained by cleaning in the step (3) in example 1 was added to a coal oil in a volume ratio of water to kerosene of 1: 0.005g, 0.01g and 0.015g were added to 10mL of the mixture of 1, respectively, and the mixture was shaken and mixed for 2 hours to form samples 1, 2 and 3, and as can be seen from FIG. 9, the thickness of the formed emulsion layer increased with the increase in the amount of the powdery solid-phase material, and the thickness was 10mm, 15mm and 24mm, respectively. Therefore, the lubricant provided by the invention has an emulsifying effect, and the practical value is increased.
(6) Application analysis of moisture retention and moisture absorption
The primary product of the base lubricant i, the secondary product of the base lubricant i, and deionized water prepared in example 1 were subjected to a water loss test for 10min at 80 ℃ using a rapid moisture meter, and the results are shown in fig. 10. As can be seen from the respective data fitting linear equations in fig. 10, the rate of water loss for the base lubricant i primary product, the base lubricant i secondary product was lower than the rate of water loss for deionized water.
The hygroscopicity of the filter paper sample materials of the same size (2 cm x 10 cm) of the spray base lubricant class I secondary product and the non-spray base lubricant class I secondary product was tested one sample at a time with the time of soaking the same distance of 5cm as a comparison parameter, and the results are shown in table 1.
TABLE 1 moisture and oil absorption Effect of the base Lubricant I
Figure BDA0003010678220000111
Figure BDA0003010678220000121
As can be seen from Table 1, the wetting time of the paper sample sprayed with the second-grade product of the base lubricant I to deionized water and oil is shortened by 1 time. The carbon-nitrogen-based water-based lubricant disclosed by the invention has a very excellent moisture absorption effect.
(7) Characterization of high environmental protection
The first grade base lubricant I, the second grade base lubricant I, the first grade lubricant II, the first grade lubricant III, the commercial water-based lubricant product SX-2 and the commercial water-based lubricant product SX-5 prepared in this example 1 were subjected to COD testing by the following steps:
(1) LH-D-500 reagent formulations
Adding a whole bottle of powder with the brand number of LH-D-500 into a beaker, then adding 348mL of deionized water, stirring, adding 22mL of concentrated sulfuric acid in the stirring process until the mixture is completely and uniformly mixed, and pouring the mixture into a special reagent bottle for later use, and marking the mixture as a reagent D.
(2) LH-E-500 reagent configuration
And pouring a whole bottle of LH-E-500 reagent and 2500mL of concentrated sulfuric acid into a beaker in sequence, continuously stirring in the pouring process until the reagent and the concentrated sulfuric acid are completely dissolved and uniformly mixed, and pouring the mixture into a special reagent bottle for later use, wherein the reagent bottle is marked as an E reagent.
(3) Sample preparation and processing
Preparation of sample A
(i) Non-flocculated treated sample: taking each product given in the table 2 as a target sample (sample numbers 1-6), and directly taking 10mL of liquid as each target sample of the non-flocculation treatment sample;
(ii) Flocculation treatment of the sample: using each of the products shown in Table 2 as a target sample (sample No. 1-6), 10mL of each sample was taken, and then 0.1g of sodium sulfate was added to each 10mL of each sample liquid, followed by mixing and standing for 6 hours to obtain each target sample subjected to flocculation treatment.
B. Sample processing
(i) Respectively taking 2.5mL and 2.5mL of deionized water from the prepared target samples, respectively transferring the deionized water into reaction tubes, taking the water sample as a zero-number comparison sample (namely a zero-number sample), respectively transferring 0.7mL of D reagent and 4.8mL of E reagent into each reaction tube, and vibrating the reaction tubes to fully and uniformly mix the two samples.
(ii) And (2) lightly putting each reaction tube into a digestion device preheated to 165 ℃ for 10min, taking out each reaction tube after the reaction is finished, putting the reaction tube into a cooling tank filled with cold water, adding 2.5mL of deionized water into each reaction tube after the reaction tube is cooled to normal temperature, and fully mixing.
(4) COD test
Firstly, pouring a zero sample into a cuvette, setting the sample as a blank sample, and then, zeroing the COD value of the zero sample, namely, deducting the background influence of the hydrosolvent so as to eliminate the COD value influence generated by taking water in the lubricant as the solvent; testing the target sample again, and recording after each reading is stable; the data read directly is the actual COD value of the lubricant composition after subtracting the effect of the sample No. zero.
The results of the COD tests of the non-flocculated sample and the flocculated sample are shown in table 2.
TABLE 2 COD results for base lubricant I, lubricant II, lubricant III and commercial lubricant
Serial number Sample(s) COD before flocculation (mg/L) COD after flocculation (mg/L)
1 First grade base lubricant I 82.77 3.01
2 Secondary products of base lubricant I 25.58 0
3 First grade base lubricant II 1478 1396
4 First grade base lubricant III 79.76 0
5 Comparative commercial water-based lubricant product SX-2 355150 226400
6 Comparative commercial water-based lubricant product SX-5 392800 229000
As can be seen from Table 2, compared with the current commercial water-based lubricant products, the COD values of the carbon nitrogen-based water-based lubricant of the invention are very low, and the COD values of the secondary product of the basic lubricant I and the primary product of the basic lubricant III after flocculation treatment reach 0mg/L. Therefore, the carbon-nitrogen-based water-based lubricant provided by the invention has good environmental protection property and good ecological benefit, can effectively reduce the post-treatment cost, and conforms to the green sustainable development strategy.
It will be appreciated by those of ordinary skill in the art that the embodiments described herein are intended to assist the reader in understanding the principles of the invention and are to be construed as being without limitation to such specifically recited embodiments and examples. Those skilled in the art can make various other specific changes and combinations based on the teachings of the present invention without departing from the spirit of the invention, and these changes and combinations are within the scope of the invention.

Claims (3)

1. The preparation method of the environment-friendly carbon-nitrogen-based water-based lubricant is characterized by comprising the following steps of:
(1) Uniformly mixing a carbon nitride precursor and an auxiliary agent I according to a set proportion to form a mixed material, and calcining the mixed material at 400-600 ℃ for 0.5-6 h to obtain a calcined product containing carbon nitride; the content of the auxiliary agent I is 12-71% of the total mass of the carbon-nitrogen compound precursor and the auxiliary agent I, and the auxiliary agent I is a mixed material of metal halide and nano oxide; the carbon-nitrogen compound precursor is at least one of urea, melamine, dicyandiamide, cyanamide, cyanuric acid, thiourea and biuret;
(2) Cleaning a calcined product containing carbonitride until the mass percentage of the carbonitride in a cleaning solution is 0.08-1%, wherein the cleaning solution is a primary carbon-nitrogen-based aqueous lubricant;
(3) And drying the solid phase material obtained by cleaning, and then uniformly dispersing the dried powdery solid phase material into water according to the mass percent of the carbon nitride in the lubricant being 0.01-8%, so as to obtain the secondary carbon nitrogen-based water-based lubricant with the mass percent of the carbon nitride being 0.01-8%.
2. The method for preparing the environmentally friendly aqueous carbonitride based lubricant according to claim 1,
when the lubricant further comprises an auxiliary agent II, the method further comprises the following steps:
(4) Uniformly dispersing an auxiliary agent II into the carbon-nitrogen-based lubricant obtained in the step (2) and the step (3) respectively to obtain the carbon-nitrogen-based lubricant added with the auxiliary agent II; the auxiliary agent II is at least one of waterborne polyurethane, waterborne fluorocarbon, waterborne soap solution, triethyl phosphate and polyacrylamide; the volume percentage of the auxiliary agent II in the lubricant is 0.03-30%;
when the lubricant further comprises an auxiliary agent III, the following steps are further included:
(5) Uniformly dispersing the aid III in the carbon-nitrogen-based lubricant obtained in the step (2), the step (3) and the step (4) respectively to obtain the carbon-nitrogen-based lubricant added with the aid III; the auxiliary agent III is at least one of sodium dodecyl sulfate, sodium citrate, sodium tungstate, sodium sulfite and sodium nitrite; the mass percent of the auxiliary agent III in the lubricant is 1% -20%;
when the lubricant further comprises an auxiliary agent IV, the method further comprises the following steps:
(6) Uniformly dispersing the aid IV into the carbon-nitrogen-based lubricant obtained in the steps (2), (3), (4) and (5) to obtain the carbon-nitrogen-based lubricant added with the aid IV; the auxiliary agent IV is a water-soluble color material; the mass percentage of the auxiliary agent IV in the lubricant is 0.05-2.5%.
3. The method for preparing the environmentally friendly aqueous carbonitride-based lubricant according to claim 1 or 2, wherein the metal halide is at least one of potassium bromide, sodium chloride, potassium iodide, potassium chloride, sodium bromide and lithium chloride; the nano oxide is at least one of silicon dioxide, titanium dioxide, magnesium oxide, tin dioxide, copper oxide, zirconium oxide, bismuth oxide and aluminum oxide.
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