CN106520283A - Preparation method of rolling bearing grease - Google Patents

Abstract

The invention discloses a preparation method of rolling bearing grease, and belongs to the technical field of the bearing grease. The method comprises the following steps: taking filtered biogas slurry and powdered rice hull, sealing and fermenting, suction filtering, drying and calcining at high temperature, ultrasonically treating with petroleum ether and hexadecyl trimethyl ammonium bromide, adding organobentonite and others, ball-milling for later use; taking glacial acetic acid, hydrogen peroxide and concentrated sulfuric acid mixed solution to react with soybean oil, and regulating the pH by use of sodium hydroxide, stirring an obtained organic layer with lithium hydroxide and reserved ball-milling mixture at constant temperature, rotary-evaporating and concentrating to obtain the rolling bearing grease. The instance proves that the obtained bearing grease is stable in operation property under high temperature state, can resist high temperature and has good antioxidant performance; a lubricant film can be formed on the surface of a rolling bearing so as to greatly reduce the friction force and guarantee the normal use of the rolling bearing; the rolling bearing grease has good colloid stability so as to maintain appropriate thickness under an operating condition, and the application prospect is relatively extensive.

Description

A kind of preparation method of antifriction-bearing grease

Technical field

The invention discloses a kind of preparation method of antifriction-bearing grease, belongs to bearing grease technical field.

Background technology

In operation process, contact surface is subject to high temperature, high pressure, the working condition of high speed to bearing, and surface is inevitably There is wear phenomenon.Wherein common wear form has abrasive wear, adhesive wear, fatigue wear, corrosive wear and fine motion Abrasion.Generally, fretting wear can be related to adhere, aoxidize, abrasive particle and fatigue wear form, failure rolling bearing existed simultaneously Several wear forms, reduce abrasion, can effectively extend the service life of bearing.With the upgrading of rolling bearing product, roll Dynamic bearing develops towards lightweight, integrated direction, therefore, for the greasy property of rolling bearing requires also more and more higher, and Antifriction-bearing grease on the market lacks enough resistances to elevated temperatures and extreme pressure, abrasion resistance now, it is therefore necessary to study High-temperature behavior and the extreme pressure and antiwear behavior of grease is improved, to adapt to market demand.Main profit of the grease as rolling bearing One of lubrication prescription, is referred to as the The Fifth Element of rolling bearing, all plays important in terms of the safe and environment-friendly of bearing products, energy-conservation Effect.Antifriction-bearing grease is to be thickened semi-synthetic lubricating oil with compound soap, and added with structural improvement agent and antioxidant additive Make.Grease is applied to the lubrication of various bearings, gear, chain and other gearing parts under high and low temperature；Or it is suitable For the lubrication of the plant equipment such as the engineering machinery of cold district outwork, automobile, motor, drive mechanism.

The content of the invention

Present invention mainly solves technical problem：Easily oxidation point is deposited at high temperature for conventional rolling bearing grease Solution, viscosity change, and generate peroxide and organic acid, make the corrosion of matched bearings so as to accelerate bearing failure, or even serious shadow The defect to vehicle safety is rung, the present invention takes biogas slurry and powdered rice hulls sealed fermenting after filter, and sucking filtration, drying high temperature are forged Add the ball millings such as organobentonite standby after burning, with petroleum ether, cetyl trimethylammonium bromide supersound process, then take ice vinegar Acid, hydrogen peroxide and concentrated sulphuric acid mixed liquor and soybean oil reaction, and pH is adjusted with sodium hydroxide, by gained organic layer and hydroxide Simultaneously concentrated by rotary evaporation obtains final product antifriction-bearing grease to the stirring of the constant temperature such as lithium, standby ball mill mixing, and Jing examples are proved, present invention gained axle Operation property is stable at high operating temperatures to hold grease, high temperature resistant and can have good antioxygenic property, can roll Bearing surface forms lubricating oil film, greatly reducing frictional force, it is ensured that the normal use of rolling bearing, and possesses good Colloid stability, in operating conditions, grease can keep appropriate denseness, with wide application prospect.

In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is：

（1）1～2L of methane liquid is measured, filtering residue is filtered to remove, filtrate is collected, and filtrate is proceeded in fermentation tank, add 2000 ～3500g powdered rice hulls, in temperature be 30～32 DEG C, rotating speed be 180～200r/min under the conditions of, 48～72h of constant-temperature enclosed fermentation, Sucking filtration, removes filtrate, is washed with deionized filter cake 3～5 times, subsequently filter cake is placed in baking oven, in 105～110 DEG C of conditions Lower drying is to constant weight, then dried filter cake is proceeded in Muffle furnace, in air atmosphere, calcines 30 with 680～700 DEG C of conditions ～45min, cools to room temperature with the furnace, obtains porous rice hull ash；

（2）The above-mentioned gained porous rice hull ash of 30～50g is weighed successively, is poured in the beaker for filling 100～120mL petroleum ether, then 0.6～0.8g cetyl trimethylammonium bromide is added, beaker is placed in into sonic oscillation instrument subsequently, it is super with 200～250W power 30～45min of sonication, sucking filtration, remove filtrate, gained filter cake is placed in vacuum drying oven, in temperature be 60～65 DEG C of conditions 3～5h of lower drying, obtains surface modified porous rice hull ash；

（3）Count by weight, sequentially add 20～30 parts of above-mentioned gained surface modified porous rice hull ash in ball mill, 30～ 40 parts of organobentonites, 100～120 parts of liquid paraffin are 30 by ratio of grinding media to material：1～45：1 adds zirconium oxide ball milling pearl, in rotating speed Under the conditions of 500～600r/min, 2～4h of ball-milling treatment, discharging obtain ball milling mixing material, standby；

（4）Measure 60～80mL glacial acetic acid successively, 45～70mL mass fractions are 15～20% hydrogen peroxide, 15～20mL mass point Number in adding Dropping funnel after mixing, then Dropping funnel is installed on fills three mouthfuls of 20～30mL soybean oils for 98% concentrated sulphuric acid On flask, subsequently there-necked flask is placed on water-bath magnetic stirring apparatuss, is heated to 65～70 DEG C, start agitator, setting To 450～500r/min, under constant temperature stirring condition, in control Dropping funnel, mixed solution is dripped off in 60～80min rotating speed, Completion of dropping is treated, is continued 3～5h of reaction, then material in there-necked flask is proceeded in separatory funnel, Deca mass fraction is 2～4% Sodium hydroxide solution, adjusts pH to 5.0～5.2, stands, and layering removes water phase, obtains organic layer；

（5）Count by weight, sequentially add 80～100 parts of above-mentioned gained organic layers, 20～30 parts of hydroxides in fat kettle processed Lithium, 15～20 parts of steps（3）Standby ball milling compound, 60～80 parts of deionized waters are 118～120 DEG C in temperature, and rotating speed is 80 Under the conditions of～100r/min, constant temperature 2～4h of stirring reaction, question response terminate, and material in fat kettle processed is proceeded to Rotary Evaporators, in Under the conditions of temperature is 95～100 DEG C, 20～30min of concentrated by rotary evaporation, discharging, after naturally cool to room temperature, by the material after cooling Proceed in triple-roller mill, grind 60～90min, discharging, encapsulation obtain final product antifriction-bearing grease.

The present invention application process be：Antifriction-bearing grease obtained in taking 80～100g present invention is evenly applied to bearing Inner side, controls thickness for 2～3mm, under 220～250 DEG C of high temperature operating conditions, using 4～5 months after, after testing, steaming It is 2～3% to send out loss amount, and work cone penetration does not occur significant change, and extreme pressure property remains 178～200N, and pressure is reduced to 0.05 ～0.17Mpa, illustrates its good mechanical stability, and thixotropy is good, can improve the service life of rolling bearing 8～10 months.

The invention has the beneficial effects as follows：

（1）The antifriction-bearing grease of gained of the invention has good colloid stability, can keep certain during use Point oil mass, it is not thinning in usage cycles, do not dry up, it is stable in properties；

（2）Grease has good greasy property, can reduce bearing friction abrasion, makes bearing service life improve 8～10 Month, it is adapted to large-scale production and application.

Specific embodiment

1～2L of methane liquid is measured first, filtering residue is filtered to remove, and collects filtrate, and filtrate is proceeded in fermentation tank, add 2000～3500g powdered rice hulls, in temperature be 30～32 DEG C, rotating speed be 180～200r/min under the conditions of, it is constant-temperature enclosed fermentation 48～ 72h, sucking filtration remove filtrate, are washed with deionized filter cake 3～5 times, subsequently filter cake are placed in baking oven, in 105～110 DEG C Under the conditions of be dried to constant weight, then dried filter cake is proceeded in Muffle furnace, in air atmosphere, is forged with 680～700 DEG C of conditions 30～45min is burnt, room temperature is cooled to the furnace, is obtained porous rice hull ash；The above-mentioned gained porous rice hull ash of 30～50g is weighed successively, Enter to fill in the beaker of 100～120mL petroleum ether, add 0.6～0.8g cetyl trimethylammonium bromide, subsequently by beaker Sonic oscillation instrument is placed in, 30～45min is processed with 200～250W power ultrasonics, sucking filtration removes filtrate, gained filter cake is placed in In vacuum drying oven, 3～5h is dried under the conditions of temperature is for 60～65 DEG C, obtains surface modified porous rice hull ash；By weight Meter, sequentially adds 20～30 parts of above-mentioned gained surface modified porous rice hull ash in ball mill, 30～40 parts of organobentonites, 100～120 parts of liquid paraffin, are 30 by ratio of grinding media to material：1～45：1 add zirconium oxide ball milling pearl, in rotating speed be 500～600r/min Under the conditions of, 2～4h of ball-milling treatment, discharging obtain ball milling mixing material, standby；60～80mL glacial acetic acid, 45～70mL matter is measured successively Amount fraction is 15～20% hydrogen peroxide, and 15～20mL mass fractions are 98% concentrated sulphuric acid, in adding Dropping funnel after mixing, then will drop Liquid funnel is installed on the there-necked flask for filling 20～30mL soybean oils, and there-necked flask is placed in water-bath magnetic stirring apparatuss subsequently On, 65～70 DEG C being heated to, starts agitator, setting speed to 450～500r/min, under constant temperature stirring condition, is controlled In Dropping funnel processed, mixed solution is dripped off in 60～80min, treats completion of dropping, continues 3～5h of reaction, then by there-necked flask Material is proceeded in separatory funnel, and Deca mass fraction is 2～4% sodium hydroxide solutions, adjusts pH to 5.0～5.2, is stood, point Layer, removes water phase, obtains organic layer；Count by weight, sequentially add 80～100 parts of above-mentioned gained organic layers in fat kettle processed, 20～30 parts of Lithium hydrates, 15～20 parts of standby ball milling compounds, 60～80 parts of deionized waters, in temperature be 118～120 DEG C, Under the conditions of rotating speed is 80～100r/min, constant temperature 2～4h of stirring reaction, question response terminate, and material in fat kettle processed is proceeded to rotation Evaporimeter, under the conditions of temperature is 95～100 DEG C, 20～30min of concentrated by rotary evaporation, discharging, after naturally cool to room temperature, will cooling Material afterwards is proceeded in triple-roller mill, grinds 60～90min, and discharging, encapsulation obtain final product antifriction-bearing grease.

Example 1

Methane liquid 1L is measured first, filtering residue is filtered to remove, and collects filtrate, and filtrate is proceeded in fermentation tank, add 2000g rice Shell powder, is 30 DEG C in temperature, and under the conditions of rotating speed is 180r/min, constant-temperature enclosed fermentation 48h, sucking filtration remove filtrate, use deionization Water washing filter cake 3 times, is subsequently placed in filter cake in baking oven, is dried to constant weight under the conditions of 105 DEG C, then dried filter cake is turned Enter in Muffle furnace, in air atmosphere, 30min is calcined with 680 DEG C of conditions, cool to room temperature with the furnace, obtain porous rice hull ash；Successively The above-mentioned gained porous rice hull ash of 30g is weighed, is poured in the beaker for filling 100mL petroleum ether, add 0.6g cetyl front threes Beaker is subsequently placed in sonic oscillation instrument by base ammonium bromide, processes 30min with 200W power ultrasonics, and sucking filtration removes filtrate, by institute Obtain filter cake to be placed in vacuum drying oven, 3h is dried under the conditions of temperature is for 60 DEG C, obtains surface modified porous rice hull ash；By weight Number meter, sequentially adds 20 parts of above-mentioned gained surface modified porous rice hull ash, 30 parts of organobentonites, 100 parts of liquid in ball mill Body paraffin, is 30 by ratio of grinding media to material：1 adds zirconium oxide ball milling pearl, under the conditions of rotating speed is 500r/min, ball-milling treatment 2h, and discharging, Ball milling mixing material is obtained, it is standby；Measure 60mL glacial acetic acid successively, 45mL mass fractions are 15% hydrogen peroxide, 15mL mass fractions are 98% concentrated sulphuric acid, in adding Dropping funnel, then Dropping funnel is installed on the there-necked flask for filling 20mL soybean oils after mixing, Subsequently there-necked flask is placed on water-bath magnetic stirring apparatuss, 65 DEG C are heated to, starts agitator, setting speed to 450r/ Min, under constant temperature stirring condition, in control Dropping funnel, mixed solution is dripped off in 60min, treats completion of dropping, continues reaction 3h, then material in there-necked flask is proceeded in separatory funnel, Deca mass fraction is 2% sodium hydroxide solution, adjusts pH to 5.0, Stand, layering removes water phase, obtains organic layer；Count by weight, sequentially add 80 parts of above-mentioned gained in fat kettle processed organic Layer, 20 parts of Lithium hydrates, 15 parts of standby ball milling compounds, 60 parts of deionized waters are 118 DEG C in temperature, and rotating speed is 80r/min bars Under part, constant temperature stirring reaction 2h, question response terminate, and material in fat kettle processed is proceeded to Rotary Evaporators, in temperature be 95 DEG C of conditions Under, concentrated by rotary evaporation 20min, discharging, after naturally cool to room temperature, the material after cooling are proceeded in triple-roller mill, grind 60min, Discharging, encapsulation, obtains final product antifriction-bearing grease.

The present invention application process be：Antifriction-bearing grease obtained in taking the 80g present invention is evenly applied on the inside of bearing, Thickness is controlled for 2mm, under 220 DEG C of high temperature operating conditions, using 4 months after, after testing, evaporation loss is 2%, work Make cone penetration and significant change do not occur, extreme pressure property remains 178N, and pressure is reduced to 0.05Mpa, illustrates its good mechanical stability, Thixotropy is good, can improve the service life of rolling bearing 8 months.

Example 2

Methane liquid 2L is measured first, filtering residue is filtered to remove, and collects filtrate, and filtrate is proceeded in fermentation tank, add 3500g rice Shell powder, is 32 DEG C in temperature, and under the conditions of rotating speed is 200r/min, constant-temperature enclosed fermentation 72h, sucking filtration remove filtrate, use deionization Water washing filter cake 5 times, is subsequently placed in filter cake in baking oven, is dried to constant weight under the conditions of 110 DEG C, then dried filter cake is turned Enter in Muffle furnace, in air atmosphere, 45min is calcined with 700 DEG C of conditions, cool to room temperature with the furnace, obtain porous rice hull ash；Successively The above-mentioned gained porous rice hull ash of 50g is weighed, is poured in the beaker for filling 120mL petroleum ether, add 0.8g cetyl front threes Beaker is subsequently placed in sonic oscillation instrument by base ammonium bromide, processes 45min with 250W power ultrasonics, and sucking filtration removes filtrate, by institute Obtain filter cake to be placed in vacuum drying oven, 5h is dried under the conditions of temperature is for 65 DEG C, obtains surface modified porous rice hull ash；By weight Number meter, sequentially adds 30 parts of above-mentioned gained surface modified porous rice hull ash, 40 parts of organobentonites, 120 parts of liquid in ball mill Body paraffin, is 45 by ratio of grinding media to material：1 adds zirconium oxide ball milling pearl, under the conditions of rotating speed is 600r/min, ball-milling treatment 4h, and discharging, Ball milling mixing material is obtained, it is standby；Measure 80mL glacial acetic acid successively, 70mL mass fractions are 20% hydrogen peroxide, 20mL mass fractions are 98% concentrated sulphuric acid, in adding Dropping funnel, then Dropping funnel is installed on the there-necked flask for filling 30mL soybean oils after mixing, Subsequently there-necked flask is placed on water-bath magnetic stirring apparatuss, 70 DEG C are heated to, starts agitator, setting speed to 500r/ Min, under constant temperature stirring condition, in control Dropping funnel, mixed solution is dripped off in 80min, treats completion of dropping, continues reaction 5h, then material in there-necked flask is proceeded in separatory funnel, Deca mass fraction is 4% sodium hydroxide solution, adjusts pH to 5.2, Stand, layering removes water phase, obtains organic layer；Count by weight, sequentially add 100 parts of above-mentioned gained in fat kettle processed organic Layer, 30 parts of Lithium hydrates, 20 parts of standby ball milling compounds, 80 parts of deionized waters are 120 DEG C in temperature, and rotating speed is 100r/min Under the conditions of, constant temperature stirring reaction 4h, question response terminate, and material in fat kettle processed is proceeded to Rotary Evaporators, in temperature be 100 DEG C of bars Under part, concentrated by rotary evaporation 30min, discharging, after naturally cool to room temperature, the material after cooling are proceeded in triple-roller mill, are ground 90min, discharging, encapsulation obtain final product antifriction-bearing grease.

The present invention application process be：Antifriction-bearing grease obtained in taking the 100g present invention is evenly applied in bearing Side, controls thickness for 3mm, under 250 DEG C of high temperature operating conditions, using 5 months after, after testing, evaporation loss is 3%, There is no significant change in work cone penetration, extreme pressure property remains 200N, and pressure is reduced to 0.17Mpa, illustrates its mechanical stability Good, thixotropy is good, can improve the service life of rolling bearing 9 months.

Example 3

Methane liquid 1.5L is measured first, filtering residue is filtered to remove, and collects filtrate, and filtrate is proceeded in fermentation tank, add 2800g Powdered rice hulls, in temperature be 31 DEG C, rotating speed be 190r/min under the conditions of, constant-temperature enclosed fermentation 60h, sucking filtration, remove filtrate, spend from Sub- water washing filter cake 4 times, is subsequently placed in filter cake in baking oven, is dried to constant weight under the conditions of 107 DEG C, then by dried filter cake Proceed in Muffle furnace, in air atmosphere, 38min is calcined with 690 DEG C of conditions, cool to room temperature with the furnace, obtain porous rice hull ash；According to It is secondary to weigh the above-mentioned gained porous rice hull ash of 40g, pour in the beaker for filling 110mL petroleum ether, add 0.7g cetyls three Beaker is subsequently placed in sonic oscillation instrument by methyl bromide ammonium, processes 38min with 230W power ultrasonics, and sucking filtration removes filtrate, will Gained filter cake is placed in vacuum drying oven, is dried 4h, obtains surface modified porous rice hull ash under the conditions of temperature is for 63 DEG C；By weight Number meter, sequentially adds 25 parts of above-mentioned gained surface modified porous rice hull ash in ball mill, 35 parts of organobentonites, 110 parts Liquid paraffin, is 38 by ratio of grinding media to material：1 adds zirconium oxide ball milling pearl, and under the conditions of rotating speed is 550r/min, ball-milling treatment 3h goes out Material, obtains ball milling mixing material, standby；Measure 70mL glacial acetic acid successively, 60mL mass fractions are 17% hydrogen peroxide, 17mL mass fractions For 98% concentrated sulphuric acid, in Dropping funnel being added after mixing, then Dropping funnel is installed on the there-necked flask for filling 25mL soybean oils On, subsequently there-necked flask being placed on water-bath magnetic stirring apparatuss, 67 DEG C are heated to, starts agitator, setting speed is extremely 470r/min, under constant temperature stirring condition, in control Dropping funnel, mixed solution is dripped off in 70min, treats completion of dropping, is continued Reaction 4h, then material in there-necked flask is proceeded in separatory funnel, and Deca mass fraction is 3% sodium hydroxide solution, adjust pH to 5.1, stand, layering removes water phase, obtains organic layer；Count by weight, sequentially adding 90 parts of above-mentioned gained in fat kettle processed has Machine layer, 25 parts of Lithium hydrates, 17 parts of standby ball milling compounds, 70 parts of deionized waters are 119 DEG C in temperature, and rotating speed is 90r/min Under the conditions of, constant temperature stirring reaction 3h, question response terminate, and material in fat kettle processed is proceeded to Rotary Evaporators, in temperature be 97 DEG C of bars Under part, concentrated by rotary evaporation 25min, discharging, after naturally cool to room temperature, the material after cooling are proceeded in triple-roller mill, are ground 75min, discharging, encapsulation obtain final product antifriction-bearing grease.

The present invention application process be：Antifriction-bearing grease obtained in taking the 90g present invention is evenly applied on the inside of bearing, Thickness is controlled for 2.5mm, under 230 DEG C of high temperature operating conditions, using 4.5 months after, after testing, evaporation loss is 2.5%, there is no significant change in work cone penetration, extreme pressure property remains 190N, and pressure is reduced to 0.12Mpa, illustrate that its machinery is steady Qualitative good, thixotropy is good, can improve the service life of rolling bearing 10 months.

Claims (1)

1. a kind of preparation method of antifriction-bearing grease, it is characterised in that concrete preparation process is：

（1）1～2L of methane liquid is measured, filtering residue is filtered to remove, filtrate is collected, and filtrate is proceeded in fermentation tank, add 2000 ～3500g powdered rice hulls, in temperature be 30～32 DEG C, rotating speed be 180～200r/min under the conditions of, 48～72h of constant-temperature enclosed fermentation, Sucking filtration, removes filtrate, is washed with deionized filter cake 3～5 times, subsequently filter cake is placed in baking oven, in 105～110 DEG C of conditions Lower drying is to constant weight, then dried filter cake is proceeded in Muffle furnace, in air atmosphere, calcines 30 with 680～700 DEG C of conditions ～45min, cools to room temperature with the furnace, obtains porous rice hull ash；

（2）The above-mentioned gained porous rice hull ash of 30～50g is weighed successively, is poured in the beaker for filling 100～120mL petroleum ether, then 0.6～0.8g cetyl trimethylammonium bromide is added, beaker is placed in into sonic oscillation instrument subsequently, it is super with 200～250W power 30～45min of sonication, sucking filtration, remove filtrate, gained filter cake is placed in vacuum drying oven, in temperature be 60～65 DEG C of conditions 3～5h of lower drying, obtains surface modified porous rice hull ash；

（3）Count by weight, sequentially add 20～30 parts of above-mentioned gained surface modified porous rice hull ash in ball mill, 30～ 40 parts of organobentonites, 100～120 parts of liquid paraffin are 30 by ratio of grinding media to material：1～45：1 adds zirconium oxide ball milling pearl, in rotating speed Under the conditions of 500～600r/min, 2～4h of ball-milling treatment, discharging obtain ball milling mixing material, standby；

（4）Measure 60～80mL glacial acetic acid successively, 45～70mL mass fractions are 15～20% hydrogen peroxide, 15～20mL mass point Number in adding Dropping funnel after mixing, then Dropping funnel is installed on fills three mouthfuls of 20～30mL soybean oils for 98% concentrated sulphuric acid On flask, subsequently there-necked flask is placed on water-bath magnetic stirring apparatuss, is heated to 65～70 DEG C, start agitator, setting To 450～500r/min, under constant temperature stirring condition, in control Dropping funnel, mixed solution is dripped off in 60～80min rotating speed, Completion of dropping is treated, is continued 3～5h of reaction, then material in there-necked flask is proceeded in separatory funnel, Deca mass fraction is 2～4% Sodium hydroxide solution, adjusts pH to 5.0～5.2, stands, and layering removes water phase, obtains organic layer；

（5）Count by weight, sequentially add 80～100 parts of above-mentioned gained organic layers, 20～30 parts of hydroxides in fat kettle processed Lithium, 15～20 parts of steps（3）Standby ball milling compound, 60～80 parts of deionized waters are 118～120 DEG C in temperature, and rotating speed is 80 Under the conditions of～100r/min, constant temperature 2～4h of stirring reaction, question response terminate, and material in fat kettle processed is proceeded to Rotary Evaporators, in Under the conditions of temperature is 95～100 DEG C, 20～30min of concentrated by rotary evaporation, discharging, after naturally cool to room temperature, by the material after cooling Proceed in triple-roller mill, grind 60～90min, discharging, encapsulation obtain final product antifriction-bearing grease.