CN105542906A - Preparation method of metal anti-wear agent - Google Patents

Abstract

The invention discloses a preparation method of a metal anti-wear agent, and belongs to the technical field of anti-wear agent. The preparation method comprises the following steps: carrying out oxidation reactions among graphite, which is obtained from the pencil core, potassium permanganate, and concentrated sulfuric acid; then placing the reaction system in an ice bath, whose base liquid is composed of ammonia water and formaldehyde; then dropwise adding a silver nitrate solution during the process of ice bathing to generate silver-containing graphene precipitate, and adding aluminum powder to carry out gasification so as to obtain the metal anti-wear agent. The practices show that the produced metal anti-wear agent has the advantages of easily available raw material, low cost, and strong high temperature resistant performance, the machine cannot be corroded easily, the lubricating performance of lubricant can be obviously improved, the surface friction and wear of mechanical movement are reduced largely, and the energy loss is reduced by 35 to 38%.

Description

A kind of preparation method of metal antiwear agent

Technical field

The invention discloses a kind of preparation method of metal antiwear agent, belong to anti-wear agent technical field.

Background technology

Anti-wear agent is a kind of high-tech machine oil (lubricating oil) additive, various technique means is utilized to process, engine scuffing can be reduced, increase engine power, so be also called engine curing agent or strong repairing agent, the work-ing life of machine oil can be extended, save fuel oil, promote power.

According to internal authority mechanism statistics, Material Wear, corrosion and fatigue three lossy account for 30% of gross industrial output value, and frictional wear is ubiquitous spontaneous phenomenon.The frictionloss primary energy source in the world about 1/3rd, wearing and tearing are one of three kinds of topmost forms causing material and damage of facilities and inefficacy, and lubrication is then the most effective technology reducing friction, reduce or avoid wearing and tearing.Development has good wear resistance, high bearing capacity, wear surface is had to the wearing technic of certain repairing effect, environmentally safe or less contamination, is chemistry and one of important topic of Materials science and tribology in the present age.

Easily sharp wear is produced due to the effect between multiple friction pair in engine.For this reason, on the basis of lubricating oil, anti-wear agent must be added to slow down component wear, with extending engine work-ing life.At present, wear preventive additive product faces variety of problems, mainly comprises molybdenumdisulphide class first-generation product, tetrafluoroethylene s-generation product and the third generation product that can generate rapidly chemical conversion film.Wherein the affine adhesion property of first-generation product is poor, can not use under high temperature height speed conditions.S-generation product then must rely on suspension agent, otherwise easily in oil circuit wall built-up deposition result in blockage, and make gelatinize in engine, therefore its use in side effect harm larger.Third generation product Problems existing does not possess repairing effect, and action period is short, lacks broad spectrum nature.Therefore, it is very important for preparing a kind of anti-wear agent that can meet more and more higher intermetallic composite coating level and green manufacturing demand.

Summary of the invention

The technical problem that the present invention mainly solves: easily produce violent wearing and tearing for metal current material in friction process, cause the loss of the energy, and the conventional wear preventive additive of tradition in use still to there is affine adhesion property poor, repairing effect is weak and high thermal resistance is poor, the problem of easy corrosion machine, provide one and utilize graphite in pencil-lead, potassium permanganate and the vitriol oil at high temperature carry out oxidizing reaction, recycling ammoniacal liquor, formaldehyde carries out ice bath as liquid at the bottom of ice-water bath to it, and drip silver nitrate solution generation argentiferous Graphene throw out in ice bath process after, add aluminium powder again to gasify, finally obtain a kind of method of metal antiwear agent.The metal antiwear agent that the present invention obtains not only raw material is easy to get, and cost is lower, and high thermal resistance is strong, not easily corrodes machine, significantly can improve the lubricity of lubricant, significantly reduces the friction and wear on mechanical movement surface, decreases the loss of the energy.

In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:

(1) 15 ~ 20 long 10 ~ 15cm are got, diameter is that container put into by the pencil of 0.7 ~ 0.9cm, backward being equipped with in the container of pencil pour clear water into, until the complete submergence pencil of clear water, after 20 ~ 30h, take out the pencil after soaking, use the openning of pencil-knife dark 0.2 ~ 0.3cm in standardized road from pencil top to bottom immediately, slowly pencil crust is peeled off, obtain complete pencil graphite core;

(2) pencil graphite core obtained above is put into ball mill and carry out ball milling, with the rotating speed of 1400 ~ 1500rpm, ball milling 25 ~ 40min, obtain graphite core powder, the vitriol oil that 150 ~ 250mL mass concentration is 72% is added afterwards in the graphite core powder obtained, mix, temperature is regulated to be 150 ~ 300 DEG C, stirring reaction 1 ~ 2h, question response is complete, add the potassium permanganate of graphite core powder quality 30 ~ 35% more wherein, after mixing, promote temperature to 500 ~ 800 DEG C, and stir with the rotating speed of 800 ~ 1200r/min, oxidizing reaction 2 ~ 3h,

(3) reaction to be oxidized terminates, pour the graphite oxidation product obtained into chromatography bag, again chromatography bag is placed in 4 ~ 6 DEG C of ice-water bath reaction 45 ~ 55min, wherein liquid at the bottom of ice-water bath by 500 ~ 600mL mass concentration be 17% ammonia soln and 150 ~ 250mL mass concentration be 25% formaldehyde solution dissolve obtain completely by stirring, after question response is steady, stir with glass stick again, add with dropping form the silver nitrate solution that 3 ~ 4mL mass concentration is 35% in the process stirred, control rate of addition to be added dropwise to complete in 2 ~ 3min, and continue reaction 35 ~ 55min,

(4) after above-mentioned ice bath completes, take out article in chromatography bag and be placed in drying machine, drying treatment 40 ~ 50min at 100 ~ 110 DEG C, obtain argentiferous Graphene throw out;

(5) in mass ratio 3: 2, crucible is put into after being mixed with alumina powder by argentiferous Graphene throw out obtained above, afterwards crucible is put into high-temperature heater, and high-temperature heater is evacuated to vacuum state, then nitrogen is filled with, be be incubated 2 ~ 3h under the condition of 1200 ~ 1300 DEG C in temperature, Heating temperature to 1250 ~ 1350 DEG C are promoted after insulation, and continue constantly to pass into nitrogen in heat-processed, flow is 100mL/min, stop after 20 ~ 35min passing into nitrogen, be slowly cooled to room temperature, take out powder in process furnace;

(6) powder in the process furnace of above-mentioned taking-up is put into clean crucible, and heat in atmosphere, regulate temperature to be 800 ~ 900 DEG C, after heating 20 ~ 25min, stop heating, allow it naturally cool to room temperature, a kind of metal antiwear agent can be obtained.

The metal antiwear agent color that the present invention obtains is filbert, and lubricity is 50 ~ 70 times of common lubricant, and wherein silver content is 0.1 ~ 0.5%, and aluminium content is 1 ~ 2%, and Graphene content is 96 ~ 98%.

Application method of the present invention is: during operation, first start water pump machine, make its preheating 20 ~ 25min, when its temperature rises to 40 ~ 50 DEG C, water pump machine is allowed to keep idling mode, getting the metal antiwear agent that 10 ~ 12g the present invention obtains afterwards slowly joins in the water pump in running, after to be added.Not only significantly can reduce the friction and wear on mechanical movement surface, decrease the energy loss of 35 ~ 38%, and resistance to elevated temperatures is strong, not easily corrodes machine, improves the work-ing life of water pump machine.

The invention has the beneficial effects as follows:

(1) metal antiwear agent that the present invention obtains has the performances such as good resistance to abrasion, high thermal resistance, non-corrosibility, and green, environmental protection, has huge application prospect;

(2) metal antiwear agent that obtains of the present invention not only raw material be easy to get, cost is lower, environmentally safe, and significantly reduces the friction and wear on mechanical movement surface, decreases the loss of the energy.

Embodiment

First 15 ~ 20 long 10 ~ 15cm are got, diameter is that container put into by the pencil of 0.7 ~ 0.9cm, backward being equipped with in the container of pencil pour clear water into, until the complete submergence pencil of clear water, after 20 ~ 30h, take out the pencil after soaking, use the openning of pencil-knife dark 0.2 ~ 0.3cm in standardized road from pencil top to bottom immediately, slowly pencil crust is peeled off, obtain complete pencil graphite core, then pencil graphite core obtained above is put into ball mill and carry out ball milling, with the rotating speed of 1400 ~ 1500rpm, ball milling 25 ~ 40min, obtain graphite core powder, the vitriol oil that 150 ~ 250mL mass concentration is 72% is added afterwards in the graphite core powder obtained, mix, temperature is regulated to be 150 ~ 300 DEG C, stirring reaction 1 ~ 2h, question response is complete, add the potassium permanganate of graphite core powder quality 30 ~ 35% more wherein, after mixing, promote temperature to 500 ~ 800 DEG C, and stir with the rotating speed of 800 ~ 1200r/min, oxidizing reaction 2 ~ 3h, reaction to be oxidized terminates, pour the graphite oxidation product obtained into chromatography bag, again chromatography bag is placed in 4 ~ 6 DEG C of ice-water bath reaction 45 ~ 55min, wherein liquid at the bottom of ice-water bath by 500 ~ 600mL mass concentration be 17% ammonia soln and 150 ~ 250mL mass concentration be 25% formaldehyde solution dissolve obtain completely by stirring, after question response is steady, stir with glass stick again, add with dropping form the silver nitrate solution that 3 ~ 4mL mass concentration is 35% in the process stirred, control rate of addition to be added dropwise to complete in 2 ~ 3min, and continue reaction 35 ~ 55min, after above-mentioned ice bath completes, take out article in chromatography bag and be placed in drying machine, drying treatment 40 ~ 50min at 100 ~ 110 DEG C, obtain argentiferous Graphene throw out, next in mass ratio 3: 2, crucible is put into after being mixed with alumina powder by argentiferous Graphene throw out obtained above, afterwards crucible is put into high-temperature heater, and high-temperature heater is evacuated to vacuum state, then nitrogen is filled with, be be incubated 2 ~ 3h under the condition of 1200 ~ 1300 DEG C in temperature, Heating temperature to 1250 ~ 1350 DEG C are promoted after insulation, and continue constantly to pass into nitrogen in heat-processed, flow is 100mL/min, stop after 20 ~ 35min passing into nitrogen, be slowly cooled to room temperature, take out powder in process furnace, finally powder in the process furnace of above-mentioned taking-up is put into clean crucible, and heat in atmosphere, regulate temperature to be 800 ~ 900 DEG C, after heating 20 ~ 25min, stop heating, allow it naturally cool to room temperature, a kind of metal antiwear agent can be obtained.

Example 1

First 15 long 10cm are got, diameter is that container put into by the pencil of 0.7cm, backward being equipped with in the container of pencil pour clear water into, until the complete submergence pencil of clear water, after 20h, take out the pencil after soaking, use the openning of pencil-knife dark 0.2cm in standardized road from pencil top to bottom immediately, slowly pencil crust is peeled off, obtain complete pencil graphite core; Then pencil graphite core obtained above is put into ball mill and carry out ball milling, with the rotating speed of 1400rpm, ball milling 25min, obtain graphite core powder, in the graphite core powder obtained, add the vitriol oil that 150mL mass concentration is 72% afterwards, mix, temperature is regulated to be 150 DEG C, stirring reaction 1h, question response is complete, then adds the potassium permanganate of graphite core powder quality 30% wherein, after mixing, promote temperature to 500 DEG C, and stir with the rotating speed of 800r/min, oxidizing reaction 2h; Reaction to be oxidized terminates, pour the graphite oxidation product obtained into chromatography bag, again chromatography bag is placed in 4 DEG C of ice-water baths and reacts 45min, wherein liquid at the bottom of ice-water bath by 500mL mass concentration be 17% ammonia soln and 150mL mass concentration be 25% formaldehyde solution dissolve obtain completely by stirring, after question response is steady, stir with glass stick again, add with dropping form the silver nitrate solution that 3mL mass concentration is 35% in the process stirred, control rate of addition to be added dropwise to complete in 2min, and continue reaction 35min; After above-mentioned ice bath completes, take out article in chromatography bag and be placed in drying machine, drying treatment 40min at 100 DEG C, obtain argentiferous Graphene throw out; Next in mass ratio 3: 2, crucible is put into after being mixed with alumina powder by argentiferous Graphene throw out obtained above, afterwards crucible is put into high-temperature heater, and high-temperature heater is evacuated to vacuum state, then nitrogen is filled with, be be incubated 2h under the condition of 1200 DEG C in temperature, Heating temperature to 1250 DEG C is promoted after insulation, and continue constantly to pass into nitrogen in heat-processed, flow is 100mL/min, stop after 20min passing into nitrogen, be slowly cooled to room temperature, take out powder in process furnace; Finally powder in the process furnace of above-mentioned taking-up is put into clean crucible, and heat in atmosphere, regulate temperature to be 800 DEG C, after heating 20min, stop heating, allow it naturally cool to room temperature, a kind of metal antiwear agent can be obtained.

This example operation is simple, during operation, first starts water pump machine, make its preheating 20min, when its temperature rises to 40 DEG C, allow water pump machine keep idling mode, getting the metal antiwear agent that 10g the present invention obtains afterwards slowly joins in the water pump in running, after to be added.Not only significantly can reduce the friction and wear on mechanical movement surface, decrease the energy loss of 35%, and resistance to elevated temperatures is strong, not easily corrodes machine, improves the work-ing life of water pump machine.

Example 2

First 18 long 13cm are got, diameter is that container put into by the pencil of 0.8cm, backward being equipped with in the container of pencil pour clear water into, until the complete submergence pencil of clear water, after 25h, take out the pencil after soaking, use the openning of pencil-knife dark 0.25cm in standardized road from pencil top to bottom immediately, slowly pencil crust is peeled off, obtain complete pencil graphite core; Then pencil graphite core obtained above is put into ball mill and carry out ball milling, with the rotating speed of 1450rpm, ball milling 35min, obtain graphite core powder, the vitriol oil that 200mL mass concentration is 72% is added afterwards in the graphite core powder obtained, mix, temperature is regulated to be 250 DEG C, stirring reaction 1.5h, question response is complete, then adds the potassium permanganate of graphite core powder quality 33% wherein, after mixing, promote temperature to 650 DEG C, and stir with the rotating speed of 1000r/min, oxidizing reaction 2.5h; Reaction to be oxidized terminates, pour the graphite oxidation product obtained into chromatography bag, again chromatography bag is placed in 5 DEG C of ice-water baths and reacts 50min, wherein liquid at the bottom of ice-water bath by 550mL mass concentration be 17% ammonia soln and 200mL mass concentration be 25% formaldehyde solution dissolve obtain completely by stirring, after question response is steady, stir with glass stick again, add with dropping form the silver nitrate solution that 3.5mL mass concentration is 35% in the process stirred, control rate of addition to be added dropwise to complete in 2 ~ 3min, and continue reaction 45min; After above-mentioned ice bath completes, take out article in chromatography bag and be placed in drying machine, drying treatment 45min at 105 DEG C, obtain argentiferous Graphene throw out; Next in mass ratio 3: 2, crucible is put into after being mixed with alumina powder by argentiferous Graphene throw out obtained above, afterwards crucible is put into high-temperature heater, and high-temperature heater is evacuated to vacuum state, then nitrogen is filled with, be be incubated 2.5h under the condition of 1250 DEG C in temperature, Heating temperature to 1300 DEG C is promoted after insulation, and continue constantly to pass into nitrogen in heat-processed, flow is 100mL/min, stop after 30min passing into nitrogen, be slowly cooled to room temperature, take out powder in process furnace; Finally powder in the process furnace of above-mentioned taking-up is put into clean crucible, and heat in atmosphere, regulate temperature to be 850 DEG C, after heating 23min, stop heating, allow it naturally cool to room temperature, a kind of metal antiwear agent can be obtained.

This example operation is simple, during operation, first starts water pump machine, make its preheating 23min, when its temperature rises to 45 DEG C, allow water pump machine keep idling mode, getting the metal antiwear agent that 11g the present invention obtains afterwards slowly joins in the water pump in running, after to be added.Not only significantly can reduce the friction and wear on mechanical movement surface, decrease the energy loss of 37%, and resistance to elevated temperatures is strong, not easily corrodes machine, improves the work-ing life of water pump machine.

Example 3

First 20 long 15cm are got, diameter is that container put into by the pencil of 0.9cm, backward being equipped with in the container of pencil pour clear water into, until the complete submergence pencil of clear water, after 30h, take out the pencil after soaking, use the openning of pencil-knife dark 0.3cm in standardized road from pencil top to bottom immediately, slowly pencil crust is peeled off, obtain complete pencil graphite core; Then pencil graphite core obtained above is put into ball mill and carry out ball milling, with the rotating speed of 1500rpm, ball milling 40min, obtain graphite core powder, in the graphite core powder obtained, add the vitriol oil that 250mL mass concentration is 72% afterwards, mix, temperature is regulated to be 300 DEG C, stirring reaction 2h, question response is complete, then adds the potassium permanganate of graphite core powder quality 35% wherein, after mixing, promote temperature to 800 DEG C, and stir with the rotating speed of 1200r/min, oxidizing reaction 3h; Reaction to be oxidized terminates, pour the graphite oxidation product obtained into chromatography bag, again chromatography bag is placed in 6 DEG C of ice-water baths and reacts 55min, wherein liquid at the bottom of ice-water bath by 600mL mass concentration be 17% ammonia soln and 250mL mass concentration be 25% formaldehyde solution dissolve obtain completely by stirring, after question response is steady, stir with glass stick again, add with dropping form the silver nitrate solution that 4mL mass concentration is 35% in the process stirred, control rate of addition to be added dropwise to complete in 3min, and continue reaction 55min; After above-mentioned ice bath completes, take out article in chromatography bag and be placed in drying machine, drying treatment 50min at 110 DEG C, obtain argentiferous Graphene throw out; Next in mass ratio 3: 2, crucible is put into after being mixed with alumina powder by argentiferous Graphene throw out obtained above, afterwards crucible is put into high-temperature heater, and high-temperature heater is evacuated to vacuum state, then nitrogen is filled with, be be incubated 3h under the condition of 1300 DEG C in temperature, Heating temperature to 1350 DEG C is promoted after insulation, and continue constantly to pass into nitrogen in heat-processed, flow is 100mL/min, stop after 35min passing into nitrogen, be slowly cooled to room temperature, take out powder in process furnace; Finally powder in the process furnace of above-mentioned taking-up is put into clean crucible, and heat in atmosphere, regulate temperature to be 900 DEG C, after heating 25min, stop heating, allow it naturally cool to room temperature, a kind of metal antiwear agent can be obtained.

This example operation is simple, during operation, first starts water pump machine, make its preheating 25min, when its temperature rises to 50 DEG C, allow water pump machine keep idling mode, getting the metal antiwear agent that 12g the present invention obtains afterwards slowly joins in the water pump in running, after to be added.Not only significantly can reduce the friction and wear on mechanical movement surface, decrease the energy loss of 38%, and resistance to elevated temperatures is strong, not easily corrodes machine, improves the work-ing life of water pump machine.

Claims (1)

1. a preparation method for metal antiwear agent, is characterized in that concrete operation step is:

(1) 15 ~ 20 long 10 ~ 15cm are got, diameter is that container put into by the pencil of 0.7 ~ 0.9cm, backward being equipped with in the container of pencil pour clear water into, until the complete submergence pencil of clear water, after 20 ~ 30h, take out the pencil after soaking, use the openning of pencil-knife dark 0.2 ~ 0.3cm in standardized road from pencil top to bottom immediately, slowly pencil crust is peeled off, obtain complete pencil graphite core;

(2) pencil graphite core obtained above is put into ball mill and carry out ball milling, with the rotating speed of 1400 ~ 1500rpm, ball milling 25 ~ 40min, obtain graphite core powder, the vitriol oil that 150 ~ 250mL mass concentration is 72% is added afterwards in the graphite core powder obtained, mix, temperature is regulated to be 150 ~ 300 DEG C, stirring reaction 1 ~ 2h, question response is complete, add the potassium permanganate of graphite core powder quality 30 ~ 35% more wherein, after mixing, promote temperature to 500 ~ 800 DEG C, and stir with the rotating speed of 800 ~ 1200r/min, oxidizing reaction 2 ~ 3h,

(3) reaction to be oxidized terminates, pour the graphite oxidation product obtained into chromatography bag, again chromatography bag is placed in 4 ~ 6 DEG C of ice-water bath reaction 45 ~ 55min, wherein liquid at the bottom of ice-water bath by 500 ~ 600mL mass concentration be 17% ammonia soln and 150 ~ 250mL mass concentration be 25% formaldehyde solution dissolve obtain completely by stirring, after question response is steady, stir with glass stick again, add with dropping form the silver nitrate solution that 3 ~ 4mL mass concentration is 35% in the process stirred, control rate of addition to be added dropwise to complete in 2 ~ 3min, and continue reaction 35 ~ 55min,

(4) after above-mentioned ice bath completes, take out article in chromatography bag and be placed in drying machine, drying treatment 40 ~ 50min at 100 ~ 110 DEG C, obtain argentiferous Graphene throw out;

(5) in mass ratio 3: 2, crucible is put into after being mixed with alumina powder by argentiferous Graphene throw out obtained above, afterwards crucible is put into high-temperature heater, and high-temperature heater is evacuated to vacuum state, then nitrogen is filled with, be be incubated 2 ~ 3h under the condition of 1200 ~ 1300 DEG C in temperature, Heating temperature to 1250 ~ 1350 DEG C are promoted after insulation, and continue constantly to pass into nitrogen in heat-processed, flow is 100mL/min, stop after 20 ~ 35min passing into nitrogen, be slowly cooled to room temperature, take out powder in process furnace;

(6) powder in the process furnace of above-mentioned taking-up is put into clean crucible, and heat in atmosphere, regulate temperature to be 800 ~ 900 DEG C, after heating 20 ~ 25min, stop heating, allow it naturally cool to room temperature, a kind of metal antiwear agent can be obtained.