Lubricating grease composite composition and preparation process thereof

Abstract

The invention discloses a lubricating grease composite composition and a preparation process thereof. The lubricating grease composite composition is prepared from base oil, graphene, xylene, a coupling agent, an adhesive, triethylene glycol monomethyl ether, a blending agent and a dispersing agent. The invention discloses a metal-free lubricating oil which comprises the following components in parts by weight: 1000-1200 parts of base oil, 47-53 parts of graphene, 10-12 parts of xylene, 15-21 parts of a coupling agent, 6-10 parts of an adhesive, 2-4 parts of triethylene glycol monomethyl ether, 12-18 parts of a blending agent and 7-9 parts of a dispersant.The metal-free lubricating oil has the advantages that corrosion to the surface of metal is avoided by using a metal-free additive, the service life of equipment is prolonged, generation of toxic gas is avoided, and the service life of the equipment is prolonged. The pollution to the environment is reduced; the graphene is modified by using organic matters, so that the dispersity and the stability of the graphene are improved, the graphene is prevented from being separated out, and the lubricating property of the lubricating grease is guaranteed; the mixed oil is cooled and precipitated to remove the bottom slag in the oil liquid, so that the ground bottom slag is prevented from being doped in the lubricating grease to influence the product purity.

Description

Technical Field

[0001] The present invention relates to the technical field of lubricating grease, in particular to a lubricating grease composite composition and a preparation process thereof. Background Art

[0002] Grease is a thick, oily semisolid, used for the friction part of machinery to lubricate and seal, and also used for metal surfaces to fill gaps and prevent rust. It is mainly prepared from mineral oil (or synthetic lubricant) and a thickener, and has been widely used in the field of mechanical manufacturing. Most existing greases use additives containing metal elements as the raw materials of the grease. During long-term use, the metal elements in the grease will corrode the metal surface, reducing the working efficiency and service life of the equipment. At the same time, the metal elements in the grease under high temperature conditions will diffuse toxic gases to pollute the environment. In addition, the composition of existing grease is simple, and the dispersion and stability of graphene in the grease after preparation are poor. During use, graphene is easily precipitated from the grease, thereby affecting the lubrication properties of the grease. The existing grease lacks a treatment process for the oil before grinding, and the unreacted substances remaining in the oil will settle at the bottom of the oil. After grinding, they will be mixed in the grease, affecting the purity of the product. Therefore, it is very necessary to design a grease composite composition and its preparation process. Summary of the invention

[0003] The object of the present invention is to provide a grease composite composition and a preparation process thereof to solve the problems raised in the above background technology.

[0004] To achieve the above-mentioned purpose, the present invention provides the following technical scheme: a grease composite composition, the formula of which includes: base oil, graphene, xylene, coupling agent, adhesive, triethylene glycol monomethyl ether, formulation agent and dispersant; the weight proportions of each component are: 1000-1200 parts of base oil, 47-53 parts of graphene, 10-12 parts of xylene, 15-21 parts of coupling agent, 6-10 parts of adhesive, 2-4 parts of triethylene glycol monomethyl ether, 12-18 parts of formulation agent and 7-9 parts of dispersant.

[0005] Preferably, the formulation is a mixture of boric acid, cyclohexane and petroleum ether, and the mass ratio of boric acid, cyclohexane and petroleum ether is 4:1:2, wherein the cyclohexane used is pentylcyclohexane.

[0006] Preferably, the dispersant consists of T151, HY105, oleic acid and Span80, and the mass ratio of T151, HY105, oleic acid and Span80 is 1:1:3:1.

[0007] The preparation process of the grease composite composition comprises the following steps: step 1, weighing raw materials; step 2, preparing additives; step 3, modifying graphene; step 4, compounding and blending; step 5, high-temperature kneading; step 6, mixing and grinding;

[0008] In the above step 1, 1000-1200 parts of base oil, 47-53 parts of graphene, 10-12 parts of xylene, 15-21 parts of coupling agent, 6-10 parts of adhesive, 2-4 parts of triethylene glycol monomethyl ether, 12-18 parts of formulation agent and 7-9 parts of dispersant are weighed according to the weight of each component and set aside;

[0009] In the above step 2, the triethylene glycol monomethyl ether and the formulation prepared in the above step 1 are placed in a flask, and then a water-carrying agent is added to the flask, and then a separation device consisting of a water separator and a condenser is used to perform reaction separation, and the reaction is stopped when no water droplets are generated in the condenser, and then the flask is subjected to rotary distillation, and then a vacuum pump is used to extract unreacted materials to obtain a metal-free additive, and then the metal-free additive is placed in a vacuum box for storage for standby use;

[0010] In the above step 3, the graphene and xylene prepared in the above step 1 are placed in a flask, and then ultrasonic dispersion is performed using an ultrasonic disperser, a coupling agent is added after dispersion, and then high-speed dispersion is performed in an ultrasonic disperser, and then ultrasonic treatment is performed, and after treatment, the mixture is allowed to stand in the flask, and after standing, an adhesive is added to perform constant temperature stirring, and after constant temperature stirring, the modified graphene is obtained and set aside;

[0011] In the above step 4, the base oil prepared in the above step 1 is evenly divided into two parts, and the base oil is respectively contained in a No. 1 container and a No. 2 container, then the base oil in the No. 1 container is poured into the reactor, and then the modified graphene prepared in step 3 and the dispersant prepared in step 1 are added to the reactor, and then magnetic stirring is performed in a magnetic stirrer, and ultrasonic dispersion is performed using an ultrasonic disperser after magnetic stirring, and a composite oil liquid is obtained after ultrasonic dispersion, which is set aside;

[0012] In the above step 5, the composite oil prepared in the above step 4 is placed in a mixing tower, and then the metal-free additive prepared in step 2 is added, and then the temperature of the mixing tower is increased for high-temperature mixing, and after high-temperature mixing, the mixed oil is taken out and set aside;

[0013] In the above step six, the mixed oil obtained in the above step five is poured into a cooling sedimentation tank for cooling and sedimentation. After cooling and sedimentation, it is filtered and poured into a blender, and then poured into the base oil contained in the No. 2 container barrel in step four, followed by stirring in the blender, and then grinding to obtain a grease composite composition.

[0014] Preferably, in step 2, the amount of the water-carrying agent added is 200% to 500% of the weight of the solids in the flask, the temperature in the separation device during reaction separation is 130 to 135°C, the rotation speed of the flask during rotary distillation is 30 to 60 r / min, and the temperature in the flask during rotary distillation is 85 to 90°C, and the vacuum degree of the vacuum pump is 0.8 to 1.2 Pa when the vacuum pump is evacuated.

[0015] Preferably, in the step three, the operating frequency of the ultrasonic disperser during ultrasonic dispersion is 5 to 13 kHz, the dispersion time is 3 to 7 min, the operating frequency of the ultrasonic disperser during high-speed dispersion is 25 to 28 Hz, the dispersion time is 25 to 30 min, the standing time in the flask is 120 to 150 min, the stirring speed of the constant temperature stirring is 30 to 60 r / min, the temperature during constant temperature stirring is 45 to 48° C., and the constant temperature stirring time is 50 to 60 min.

[0016] Preferably, in step 4, during magnetic stirring, the temperature in the magnetic stirrer is 85-90°C, the stirring speed of the magnetic stirrer is 15-18 r / min, the magnetic stirring time is 120-150 min, and the operating frequency of the ultrasonic disperser during ultrasonic dispersion is 18-25 Hz, and the dispersion time is 25-30 min.

[0017] Preferably, in step five, the heating rate of the mixing tower before high-temperature mixing is 6 to 8°C / min, and the temperature of the mixing tower is increased to 150 to 180°C. During high-temperature mixing, the stirring speed of the stirring frame in the mixing tower is 18 to 25 r / min, and the high-temperature mixing time is 60 to 80 min.

[0018] Preferably, in step six, the temperature in the cooling sedimentation tank is 15-18° C., and the cooling sedimentation time is 100-120 min. During the stirring process, the stirring speed of the stirrer is 30-32 r / min, and the stirring process time is 200-240 min.

[0019] Compared with the prior art, the beneficial effects of the present invention are as follows: the grease composite composition and its preparation process use triethylene glycol monomethyl ether as the main raw material to prepare a metal-free additive that does not contain metal elements, thereby avoiding corrosion of the metal surface caused by long-term use of lubricating grease and extending the service life of the equipment. At the same time, no toxic gas is generated in a high-temperature environment, reducing pollution to the environment; organic matter is used to modify graphene before mixing, thereby improving the dispersibility and stability of graphene, avoiding the precipitation of graphene from the grease during use, thereby ensuring the lubricating properties of the grease; before grinding to prepare the grease, the mixed oil is cooled and precipitated to remove the bottom residue in the oil, thereby avoiding the bottom residue after grinding being mixed in the grease to affect the purity of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a process flow chart of the present invention. DETAILED DESCRIPTION

[0021] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0022] See also Figure 1 , the present invention provides a technical solution:

[0023] Embodiment 1:

[0024] A grease composite composition, the formula of which includes: base oil, graphene, xylene, coupling agent, adhesive, triethylene glycol monomethyl ether, a formulation agent and a dispersant; the weight proportions of the components are: 1200 parts of base oil, 53 parts of graphene, 12 parts of xylene, 21 parts of coupling agent, 10 parts of adhesive, 4 parts of triethylene glycol monomethyl ether, 18 parts of formulation agent and 9 parts of dispersant, the formulation agent is a mixture of boric acid, cyclohexane and petroleum ether, and the mass ratio of boric acid, cyclohexane and petroleum ether is 4:1:2, wherein the cyclohexane used is pentylcyclohexane with a CAS number of 38792-89-1, the dispersant is composed of T151, HY105, oleic acid and Span80, and the mass ratio of T151, HY105, oleic acid and Span80 is 1:1:3:1; wherein the CAS number of triethylene glycol monomethyl ether is 112-35-6.

[0025] The preparation process of the grease composite composition comprises the following steps: step 1, weighing raw materials; step 2, preparing additives; step 3, modifying graphene; step 4, compounding and blending; step 5, high-temperature kneading; step 6, mixing and grinding;

[0026] In the above step 1, 1200 parts of base oil, 53 parts of graphene, 12 parts of xylene, 21 parts of coupling agent, 10 parts of adhesive, 4 parts of triethylene glycol monomethyl ether, 18 parts of formulation agent and 9 parts of dispersant are weighed according to the weight of each component and set aside;

[0027] Wherein in the above step 2, the triethylene glycol monomethyl ether and the formulation prepared in the above step 1 are put into a flask, and then a water-carrying agent is added to the flask, and the amount of the water-carrying agent added is 500% of the weight of the solid in the flask, and then a separation device composed of a water separator and a condenser is used for reaction separation, and the temperature in the separation device is 135°C during reaction separation, and the reaction is stopped when no water droplets are produced in the condenser, and then the flask is subjected to rotary distillation, and the rotation speed of the flask during rotary distillation is 60r / min, and the temperature in the flask during rotary distillation is 90°C, and then a vacuum pump is used to extract the unreacted material to obtain a metal-free additive, and the vacuum degree of the vacuum pump is 1.2Pa when the vacuum pump is extracted, and then the metal-free additive is placed in a vacuum box for storage for standby;

[0028] Wherein in the above step three, the graphene and xylene prepared in the above step one are put into a flask, and then an ultrasonic disperser is used for ultrasonic dispersion, the operating frequency of the ultrasonic disperser during ultrasonic dispersion is 13kHz, and the dispersion time is 7min. After dispersion, a coupling agent is added, and then high-speed dispersion is performed in the ultrasonic disperser. During the high-speed dispersion process, the operating frequency of the ultrasonic disperser is 28Hz, and the dispersion time is 30min. Then, ultrasonic treatment is performed, and the flask is allowed to stand for 150min after treatment. After standing, an adhesive is added for constant temperature stirring, the stirring speed of the constant temperature stirring is 60r / min, the temperature during constant temperature stirring is 48°C, and the constant temperature stirring time is 60min. After constant temperature stirring, modified graphene is obtained for standby use;

[0029] In the above step 4, the base oil prepared in the above step 1 is evenly divided into two parts, and the base oil is respectively contained in a No. 1 container and a No. 2 container, then the base oil in the No. 1 container is poured into the reactor, and then the modified graphene prepared in step 3 and the dispersant prepared in step 1 are added to the reactor, and then magnetic stirring is performed in a magnetic stirrer. During the magnetic stirring, the temperature in the magnetic stirrer is 90° C., and the stirring speed of the magnetic stirrer is 18 r / min. The magnetic stirring time is 150 min. After the magnetic stirring, an ultrasonic disperser is used for ultrasonic dispersion. During the ultrasonic dispersion, the working frequency of the ultrasonic disperser is 25 Hz, and the dispersion time is 30 min. After ultrasonic dispersion, a composite oil liquid is obtained for standby use;

[0030] In the above step 5, the composite oil prepared in the above step 4 is placed in a mixing tower, and then the metal-free additive prepared in step 2 is added, and then the temperature of the mixing tower is increased to perform high-temperature mixing. Before high-temperature mixing, the heating rate of the mixing tower is 8°C / min, and the temperature of the mixing tower is increased to 180°C. During high-temperature mixing, the stirring speed of the stirring frame in the mixing tower is 25r / min, and the high-temperature mixing time is 80min. After high-temperature mixing, the mixed oil is taken out to be used for standby;

[0031] In the above step six, the mixed oil obtained in the above step five is poured into a cooling sedimentation tank for cooling sedimentation. The temperature in the cooling sedimentation tank is 18°C, and the cooling sedimentation time is 120 minutes. After cooling sedimentation, it is filtered and poured into a blender, and then poured into the base oil contained in the No. 2 container barrel in step four. Then, it is stirred in the blender. The stirring speed of the blender during the stirring treatment is 32r / min, and the stirring treatment time is 240 minutes. After the stirring treatment, it is ground to obtain a grease composite composition.

[0032] Embodiment 2:

[0033] A grease composite composition, the formula of which includes: base oil, graphene, xylene, coupling agent, adhesive, triethylene glycol monomethyl ether, a formulation agent and a dispersant; the weight proportions of the components are: 1000 parts of base oil, 47 parts of graphene, 10 parts of xylene, 15 parts of coupling agent, 6 parts of adhesive, 2 parts of triethylene glycol monomethyl ether, 12 parts of formulation agent and 7 parts of dispersant, the formulation agent is a mixture of boric acid, cyclohexane and petroleum ether, and the mass ratio of boric acid, cyclohexane and petroleum ether is 4:1:2, wherein the cyclohexane used is pentylcyclohexane with a CAS number of 38792-89-1, the dispersant is composed of T151, HY105, oleic acid and Span80, and the mass ratio of T151, HY105, oleic acid and Span80 is 1:1:3:1; wherein the CAS number of triethylene glycol monomethyl ether is 112-35-6.

[0034] The preparation process of the grease composite composition comprises the following steps: step 1, weighing raw materials; step 2, preparing additives; step 3, modifying graphene; step 4, compounding and blending; step 5, high-temperature kneading; step 6, mixing and grinding;

[0035] In the above step 1, 1000 parts of base oil, 47 parts of graphene, 10 parts of xylene, 15 parts of coupling agent, 6 parts of adhesive, 2 parts of triethylene glycol monomethyl ether, 12 parts of formulation agent and 7 parts of dispersant are weighed according to the weight of each component and set aside;

[0036] Wherein in the above step 2, the triethylene glycol monomethyl ether and the formulation prepared in the above step 1 are put into a flask, and then a water-carrying agent is added to the flask, and the amount of the water-carrying agent added is 200% of the weight of the solid in the flask, and then a separation device composed of a water separator and a condenser is used for reaction separation, and the temperature in the separation device is 130°C during reaction separation, and the reaction is stopped when no water droplets are produced in the condenser, and then the flask is subjected to rotary distillation, and the rotation speed of the flask during rotary distillation is 30r / min, and the temperature in the flask during rotary distillation is 85°C, and then a vacuum pump is used to extract the unreacted material to obtain a metal-free additive, and the vacuum degree of the vacuum pump is 0.8Pa when the vacuum pump is extracted, and then the metal-free additive is placed in a vacuum box for storage for standby;

[0037] Wherein in the above step three, the graphene and xylene prepared in the above step one are put into a flask, and then an ultrasonic disperser is used for ultrasonic dispersion, the operating frequency of the ultrasonic disperser during ultrasonic dispersion is 5kHz, and the dispersion time is 3min. After dispersion, a coupling agent is added, and then high-speed dispersion is performed in the ultrasonic disperser. During the high-speed dispersion process, the operating frequency of the ultrasonic disperser is 25Hz, and the dispersion time is 25min. Then, ultrasonic treatment is performed, and the flask is allowed to stand for 120min after treatment. After standing, an adhesive is added for constant temperature stirring, the stirring speed of the constant temperature stirring is 30r / min, the temperature during constant temperature stirring is 45°C, and the constant temperature stirring time is 50min. After constant temperature stirring, modified graphene is obtained for standby use;

[0038] In the above step 4, the base oil prepared in the above step 1 is evenly divided into two parts, and the base oil is respectively contained in a No. 1 container and a No. 2 container, then the base oil in the No. 1 container is poured into a reactor, and then the modified graphene prepared in step 3 and the dispersant prepared in step 1 are added to the reactor, and then magnetic stirring is performed in a magnetic stirrer. During the magnetic stirring, the temperature in the magnetic stirrer is 85° C., and the stirring speed of the magnetic stirrer is 15 r / min. The magnetic stirring time is 120 min. After the magnetic stirring, an ultrasonic disperser is used for ultrasonic dispersion. During the ultrasonic dispersion, the working frequency of the ultrasonic disperser is 18 Hz, and the dispersion time is 25 min. After ultrasonic dispersion, a composite oil liquid is obtained for standby use;

[0039] In the above step 5, the composite oil prepared in the above step 4 is placed in a mixing tower, and then the metal-free additive prepared in step 2 is added, and then the temperature of the mixing tower is increased to perform high-temperature mixing. Before high-temperature mixing, the heating rate of the mixing tower is 6°C / min, and the temperature of the mixing tower is increased to 150°C. During high-temperature mixing, the stirring speed of the stirring frame in the mixing tower is 18r / min, and the high-temperature mixing time is 60min. After high-temperature mixing, the mixed oil is taken out to be used for standby;

[0040] In the above step six, the mixed oil obtained in the above step five is poured into a cooling sedimentation tank for cooling sedimentation. The temperature in the cooling sedimentation tank is 15°C, and the cooling sedimentation time is 100 minutes. After cooling sedimentation, it is filtered and poured into a blender, and then poured into the base oil contained in the second container in step four. Then, it is stirred in the blender. The stirring speed of the blender during the stirring treatment is 30r / min, and the stirring treatment time is 200 minutes. After the stirring treatment, it is ground to obtain a grease composite composition.

[0041] Embodiment 3:

[0042] A grease composite composition, the formula of which includes: base oil, graphene, xylene, coupling agent, adhesive, triethylene glycol monomethyl ether, a formulation agent and a dispersant; the weight proportions of the components are: 1200 parts of base oil, 47 parts of graphene, 12 parts of xylene, 15 parts of coupling agent, 10 parts of adhesive, 2 parts of triethylene glycol monomethyl ether, 18 parts of formulation agent and 7 parts of dispersant, the formulation agent is a mixture of boric acid, cyclohexane and petroleum ether, and the mass ratio of boric acid, cyclohexane and petroleum ether is 4:1:2, wherein the cyclohexane used is pentylcyclohexane with a CAS number of 38792-89-1, the dispersant is composed of T151, HY105, oleic acid and Span80, and the mass ratio of T151, HY105, oleic acid and Span80 is 1:1:3:1; wherein the CAS number of triethylene glycol monomethyl ether is 112-35-6.

[0043] The preparation process of the grease composite composition comprises the following steps: step 1, weighing raw materials; step 2, preparing additives; step 3, modifying graphene; step 4, compounding and blending; step 5, high-temperature kneading; step 6, mixing and grinding;

[0044] In the above step 1, 1200 parts of base oil, 47 parts of graphene, 12 parts of xylene, 15 parts of coupling agent, 10 parts of adhesive, 2 parts of triethylene glycol monomethyl ether, 18 parts of formulation agent and 7 parts of dispersant are weighed according to the weight of each component and set aside;

[0045] Wherein in the above step 2, the triethylene glycol monomethyl ether and the formulation prepared in the above step 1 are put into a flask, and then a water-carrying agent is added to the flask, and the amount of the water-carrying agent added is 500% of the weight of the solid in the flask, and then a separation device composed of a water separator and a condenser is used for reaction separation, and the temperature in the separation device is 130°C during reaction separation, and the reaction is stopped when no water droplets are produced in the condenser, and then the flask is subjected to rotary distillation, and the rotation speed of the flask during rotary distillation is 60r / min, and the temperature in the flask during rotary distillation is 85°C, and then a vacuum pump is used to extract the unreacted material to obtain a metal-free additive, and the vacuum degree of the vacuum pump is 1.2Pa when the vacuum pump is extracted, and then the metal-free additive is placed in a vacuum box for storage for standby;

[0046] Wherein in the above step three, the graphene and xylene prepared in the above step one are put into a flask, and then an ultrasonic disperser is used for ultrasonic dispersion, the operating frequency of the ultrasonic disperser during ultrasonic dispersion is 5kHz, and the dispersion time is 7min. After dispersion, a coupling agent is added, and then high-speed dispersion is performed in the ultrasonic disperser. During the high-speed dispersion process, the operating frequency of the ultrasonic disperser is 28Hz, and the dispersion time is 25min. Then, ultrasonic treatment is performed, and the flask is allowed to stand for 150min after treatment. After standing, an adhesive is added for constant temperature stirring, the stirring speed of the constant temperature stirring is 30r / min, the temperature during constant temperature stirring is 48°C, and the constant temperature stirring time is 50min. After constant temperature stirring, modified graphene is obtained for standby use;

[0047] In the above step 4, the base oil prepared in the above step 1 is evenly divided into two parts, and the base oil is respectively contained in a No. 1 container and a No. 2 container, then the base oil in the No. 1 container is poured into a reactor, and then the modified graphene prepared in step 3 and the dispersant prepared in step 1 are added to the reactor, and then magnetic stirring is performed in a magnetic stirrer, during which the temperature in the magnetic stirrer is 90° C., and the stirring speed of the magnetic stirrer is 15 r / min, and the magnetic stirring time is 150 min. After the magnetic stirring, an ultrasonic disperser is used for ultrasonic dispersion, and the working frequency of the ultrasonic disperser during ultrasonic dispersion is 18 Hz, and the dispersion time is 30 min. After ultrasonic dispersion, a composite oil liquid is obtained for standby use;

[0048] In the above step 5, the composite oil prepared in the above step 4 is placed in a mixing tower, and then the metal-free additive prepared in step 2 is added, and then the temperature of the mixing tower is increased to perform high-temperature mixing. Before high-temperature mixing, the heating rate of the mixing tower is 8°C / min, and the temperature of the mixing tower is increased to 150°C. During high-temperature mixing, the stirring speed of the stirring frame in the mixing tower is 25r / min, and the high-temperature mixing time is 60min. After high-temperature mixing, the mixed oil is taken out to be used for standby;

[0049] In the above step six, the mixed oil obtained in the above step five is poured into a cooling sedimentation tank for cooling sedimentation. The temperature in the cooling sedimentation tank is 18°C, and the cooling sedimentation time is 100 minutes. After cooling sedimentation, it is filtered and poured into a blender, and then poured into the base oil contained in the No. 2 container barrel in step four. Then, it is stirred in the blender. The stirring speed of the blender during the stirring treatment is 32r / min, and the stirring treatment time is 200 minutes. After the stirring treatment, it is ground to obtain a grease composite composition.

[0050] Embodiment 4:

[0051] A grease composite composition, the formula of which includes: base oil, graphene, xylene, coupling agent, adhesive, triethylene glycol monomethyl ether, a formulation agent and a dispersant; the weight proportions of the components are: 1200 parts of base oil, 53 parts of graphene, 12 parts of xylene, 15 parts of coupling agent, 6 parts of adhesive, 2 parts of triethylene glycol monomethyl ether, 18 parts of formulation agent and 9 parts of dispersant, the formulation agent is a mixture of boric acid, cyclohexane and petroleum ether, and the mass ratio of boric acid, cyclohexane and petroleum ether is 4:1:2, wherein the cyclohexane used is pentylcyclohexane with a CAS number of 38792-89-1, the dispersant is composed of T151, HY105, oleic acid and Span80, and the mass ratio of T151, HY105, oleic acid and Span80 is 1:1:3:1; wherein the CAS number of triethylene glycol monomethyl ether is 112-35-6.

[0052] The preparation process of the grease composite composition comprises the following steps: step 1, weighing raw materials; step 2, preparing additives; step 3, modifying graphene; step 4, compounding and blending; step 5, high-temperature kneading; step 6, mixing and grinding;

[0053] In the above step 1, 1200 parts of base oil, 53 parts of graphene, 12 parts of xylene, 15 parts of coupling agent, 6 parts of adhesive, 2 parts of triethylene glycol monomethyl ether, 18 parts of formulation agent and 9 parts of dispersant are weighed according to the weight of each component and set aside;

[0054] Wherein in the above step 2, the triethylene glycol monomethyl ether and the formulation prepared in the above step 1 are put into a flask, and then a water-carrying agent is added to the flask, and the amount of the water-carrying agent added is 500% of the weight of the solid in the flask, and then a separation device composed of a water separator and a condenser is used for reaction separation, and the temperature in the separation device is 135°C during reaction separation, and the reaction is stopped when no water droplets are produced in the condenser, and then the flask is subjected to rotary distillation, and the rotation speed of the flask during rotary distillation is 60r / min, and the temperature in the flask during rotary distillation is 85°C, and then a vacuum pump is used to extract the unreacted material to obtain a metal-free additive, and the vacuum degree of the vacuum pump is 0.8Pa when the vacuum pump is extracted, and then the metal-free additive is placed in a vacuum box for storage for standby;

[0055] Wherein in the above step three, the graphene and xylene prepared in the above step one are put into a flask, and then an ultrasonic disperser is used for ultrasonic dispersion, the operating frequency of the ultrasonic disperser during ultrasonic dispersion is 5kHz, and the dispersion time is 7min. After dispersion, a coupling agent is added, and then high-speed dispersion is performed in the ultrasonic disperser. During the high-speed dispersion process, the operating frequency of the ultrasonic disperser is 28Hz, and the dispersion time is 30min. Then, ultrasonic treatment is performed, and the flask is allowed to stand for 120min after treatment. After standing, an adhesive is added for constant temperature stirring, the stirring speed of the constant temperature stirring is 30r / min, the temperature during constant temperature stirring is 45°C, and the constant temperature stirring time is 60min. After constant temperature stirring, modified graphene is obtained for standby use;

[0056] In the above step 4, the base oil prepared in the above step 1 is evenly divided into two parts, and the base oil is respectively contained in a No. 1 container and a No. 2 container, then the base oil in the No. 1 container is poured into the reactor, and then the modified graphene prepared in step 3 and the dispersant prepared in step 1 are added to the reactor, and then magnetic stirring is performed in a magnetic stirrer. During the magnetic stirring, the temperature in the magnetic stirrer is 90° C., and the stirring speed of the magnetic stirrer is 18 r / min. The magnetic stirring time is 120 min. After the magnetic stirring, an ultrasonic disperser is used for ultrasonic dispersion. During the ultrasonic dispersion, the working frequency of the ultrasonic disperser is 18 Hz, and the dispersion time is 25 min. After ultrasonic dispersion, a composite oil liquid is obtained for standby use;

[0057] In the above step 5, the composite oil prepared in the above step 4 is placed in a mixing tower, and then the metal-free additive prepared in step 2 is added, and then the temperature of the mixing tower is increased to perform high-temperature mixing. Before high-temperature mixing, the heating rate of the mixing tower is 8°C / min, and the temperature of the mixing tower is increased to 180°C. During high-temperature mixing, the stirring speed of the stirring frame in the mixing tower is 25r / min, and the high-temperature mixing time is 60min. After high-temperature mixing, the mixed oil is taken out to be used for standby;

[0058] In the above step six, the mixed oil obtained in the above step five is poured into a cooling sedimentation tank for cooling sedimentation. The temperature in the cooling sedimentation tank is 18°C, and the cooling sedimentation time is 120 minutes. After cooling sedimentation, it is filtered and poured into a blender, and then poured into the base oil contained in the No. 2 container barrel in step four. Then, it is stirred in the blender. The stirring speed of the blender during the stirring treatment is 32r / min, and the stirring treatment time is 200 minutes. After the stirring treatment, it is ground to obtain a grease composite composition.

[0059] Embodiment 5:

[0060] A grease composite composition, the formula of which includes: base oil, graphene, xylene, coupling agent, adhesive, triethylene glycol monomethyl ether, a formulation agent and a dispersant; the weight proportions of the components are: 1100 parts of base oil, 50 parts of graphene, 11 parts of xylene, 18 parts of coupling agent, 9 parts of adhesive, 3 parts of triethylene glycol monomethyl ether, 15 parts of formulation agent and 8 parts of dispersant, the formulation agent is a mixture of boric acid, cyclohexane and petroleum ether, and the mass ratio of boric acid, cyclohexane and petroleum ether is 4:1:2, wherein the cyclohexane used is pentylcyclohexane with a CAS number of 38792-89-1, the dispersant is composed of T151, HY105, oleic acid and Span80, and the mass ratio of T151, HY105, oleic acid and Span80 is 1:1:3:1; wherein the CAS number of triethylene glycol monomethyl ether is 112-35-6.

[0061] The preparation process of the grease composite composition comprises the following steps: step 1, weighing raw materials; step 2, preparing additives; step 3, modifying graphene; step 4, compounding and blending; step 5, high-temperature kneading; step 6, mixing and grinding;

[0062] In the above step 1, 1100 parts of base oil, 50 parts of graphene, 11 parts of xylene, 18 parts of coupling agent, 9 parts of adhesive, 3 parts of triethylene glycol monomethyl ether, 15 parts of formulation agent and 8 parts of dispersant are weighed according to the weight of each component and set aside;

[0063] Wherein in the above step 2, the triethylene glycol monomethyl ether and the formulation prepared in the above step 1 are put into a flask, and then a water-carrying agent is added to the flask, and the amount of the water-carrying agent added is 400% of the weight of the solid in the flask, and then a separation device composed of a water separator and a condenser is used for reaction separation, and the temperature in the separation device is 133°C during reaction separation, and the reaction is stopped when no water droplets are produced in the condenser, and then the flask is subjected to rotary distillation, and the rotation speed of the flask during rotary distillation is 50r / min, and the temperature in the flask during rotary distillation is 87°C, and then a vacuum pump is used to extract the unreacted material to obtain a metal-free additive, and the vacuum degree of the vacuum pump is 1.1Pa when the vacuum pump is extracted, and then the metal-free additive is placed in a vacuum box for storage for standby;

[0064] Wherein in the above step three, the graphene and xylene prepared in the above step one are put into a flask, and then an ultrasonic disperser is used for ultrasonic dispersion, the operating frequency of the ultrasonic disperser during ultrasonic dispersion is 8kHz, and the dispersion time is 5min. After dispersion, a coupling agent is added, and then high-speed dispersion is performed in the ultrasonic disperser. During the high-speed dispersion process, the operating frequency of the ultrasonic disperser is 26Hz, and the dispersion time is 28min. Thereafter, ultrasonic treatment is performed, and after treatment, the mixture is allowed to stand in the flask for 140min, and after standing, an adhesive is added for constant temperature stirring. The stirring speed of the constant temperature stirring is 45r / min, the temperature during constant temperature stirring is 47°C, and the constant temperature stirring time is 55min. After constant temperature stirring, modified graphene is obtained for standby use;

[0065] In the above step 4, the base oil prepared in the above step 1 is evenly divided into two parts, and the base oil is respectively contained in a No. 1 container and a No. 2 container, then the base oil in the No. 1 container is poured into the reactor, and then the modified graphene prepared in step 3 and the dispersant prepared in step 1 are added to the reactor, and then magnetic stirring is performed in a magnetic stirrer. During the magnetic stirring, the temperature in the magnetic stirrer is 88° C., and the stirring speed of the magnetic stirrer is 17 r / min. The magnetic stirring time is 135 min. After the magnetic stirring, an ultrasonic disperser is used for ultrasonic dispersion. During the ultrasonic dispersion, the working frequency of the ultrasonic disperser is 20 Hz, and the dispersion time is 28 min. After ultrasonic dispersion, a composite oil liquid is obtained for standby use;

[0066] In the above step 5, the composite oil prepared in the above step 4 is placed in a mixing tower, and then the metal-free additive prepared in step 2 is added, and then the temperature of the mixing tower is increased to perform high-temperature mixing. Before high-temperature mixing, the heating rate of the mixing tower is 7°C / min, and the temperature of the mixing tower is increased to 170°C. During high-temperature mixing, the stirring speed of the stirring frame in the mixing tower is 20r / min, and the high-temperature mixing time is 70min. After high-temperature mixing, the mixed oil is taken out to be used for standby;

[0067] In the above step six, the mixed oil obtained in the above step five is poured into a cooling sedimentation tank for cooling sedimentation. The temperature in the cooling sedimentation tank is 16°C, and the cooling sedimentation time is 115 minutes. After cooling sedimentation, it is filtered and poured into a blender, and then poured into the base oil contained in the No. 2 container barrel in step four. Then, it is stirred in the blender. The stirring speed of the blender during the stirring treatment is 30r / min, and the stirring treatment time is 220 minutes. After the stirring treatment, it is ground to obtain a grease composite composition.

[0068] The lubricating grease composite compositions obtained in the above examples were tested for performance and compared with common lubricating greases on the market. The results are shown in the following table:

[0069] Doping rate Four ball test ZMZ / N Wear spot area Friction coefficient Example 1 0.14％ 518 <![CDATA[0.634mm 2 ]]> 0.072 Example 2 0.08％ 536 <![CDATA[0.628mm 2 ]]> 0.077 Example 3 0.03％ 523 <![CDATA[0.640mm 2 ]]> 0.075 Example 4 0.11％ 513 <![CDATA[0.612mm 2 ]]> 0.070 Example 5 0.09％ 533 <![CDATA[0.635mm 2 ]]> 0.077 Comparative Example 2.35％ 834 <![CDATA[0.739mm 2 ]]> 0.108

[0070] Based on the above, the advantages of the present invention are that, when used, the present invention uses triethylene glycol monomethyl ether as the main raw material to prepare a metal-free additive that does not contain metal elements, thereby avoiding corrosion of the metal surface caused by long-term use of lubricating grease, improving the working efficiency of the equipment, and extending the service life. At the same time, no toxic gas is generated in a high temperature environment, reducing pollution to the environment; before mixing, the graphene is modified with organic matter to improve the dispersibility and stability of the graphene, and the precipitation of graphene from the grease during use is avoided, thereby ensuring the lubricating properties of the grease; before grinding to prepare the grease, the mixed oil is cooled and precipitated to remove the bottom residue in the oil, so as to avoid the bottom residue after grinding being mixed in the grease to affect the purity of the product.

[0071] It will be apparent to those skilled in the art that the invention is not limited to the details of the exemplary embodiments described above and that the invention can be implemented in other specific forms without departing from the spirit or essential features of the invention. Therefore, the embodiments should be considered exemplary and non-limiting in all respects, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations falling within the meaning and scope of the equivalent elements of the claims be included in the invention. Any reference numeral in a claim should not be considered as limiting the claim to which it relates.

Claims

1. A lubricating grease composite composition, the formula comprising: Base oil, graphene, xylene, coupling agent, adhesive, triethylene glycol monomethyl ether, blending agent and dispersant; characterized in that the weight proportions of the components are: 1000-1200 parts of base oil, 47-53 parts of graphene, 10-12 parts of xylene, 15-21 parts of coupling agent, 6-10 parts of adhesive, 2-4 parts of triethylene glycol monomethyl ether, 12-18 parts of blending agent and 7-9 parts of dispersant.

2. The grease composite composition according to claim 1, characterized in that: The formulation is prepared by mixing boric acid, cyclohexane and petroleum ether, and the mass ratio of boric acid, cyclohexane and petroleum ether is 4:1:2, wherein the cyclohexane used is pentylcyclohexane.

3. The grease composite composition according to claim 1, characterized in that: The dispersant consists of T151, HY105, oleic acid and Span80, and the mass ratio of T151, HY105, oleic acid and Span80 is 1:1:3:

1.

4. A process for preparing a grease composite composition, comprising the following steps: Step 1, weighing raw materials; step 2, preparing additives; step 3, modifying graphene; step 4, compounding and blending; step 5, high-temperature kneading; step 6, mixed grinding; it is characterized in that: In the above step 1, 1000-1200 parts of base oil, 47-53 parts of graphene, 10-12 parts of xylene, 15-21 parts of coupling agent, 6-10 parts of adhesive, 2-4 parts of triethylene glycol monomethyl ether, 12-18 parts of formulation agent and 7-9 parts of dispersant are weighed according to the weight of each component and set aside; In the above step 2, the triethylene glycol monomethyl ether and the formulation prepared in the above step 1 are placed in a flask, and then a water-carrying agent is added to the flask, and then a separation device consisting of a water separator and a condenser is used to perform reaction separation, and the reaction is stopped when no water droplets are generated in the condenser, and then the flask is subjected to rotary distillation, and then a vacuum pump is used to extract unreacted materials to obtain a metal-free additive, and then the metal-free additive is placed in a vacuum box for storage for standby use; In the above step 3, the graphene and xylene prepared in the above step 1 are placed in a flask, and then ultrasonic dispersion is performed using an ultrasonic disperser, a coupling agent is added after dispersion, and then high-speed dispersion is performed in an ultrasonic disperser, and then ultrasonic treatment is performed, and after treatment, the mixture is allowed to stand in the flask, and after standing, an adhesive is added to perform constant temperature stirring, and after constant temperature stirring, the modified graphene is obtained and set aside; In the above step 4, the base oil prepared in the above step 1 is evenly divided into two parts, and the base oil is respectively contained in a No. 1 container and a No. 2 container, then the base oil in the No. 1 container is poured into the reactor, and then the modified graphene prepared in step 3 and the dispersant prepared in step 1 are added to the reactor, and then magnetic stirring is performed in a magnetic stirrer, and ultrasonic dispersion is performed using an ultrasonic disperser after magnetic stirring, and a composite oil liquid is obtained after ultrasonic dispersion, which is set aside; In the above step 5, the composite oil prepared in the above step 4 is placed in a mixing tower, and then the metal-free additive prepared in step 2 is added, and then the temperature of the mixing tower is increased for high-temperature mixing, and after high-temperature mixing, the mixed oil is taken out and set aside; In the above step six, the mixed oil obtained in the above step five is poured into a cooling sedimentation tank for cooling and sedimentation. After cooling and sedimentation, it is filtered and poured into a blender, and then poured into the base oil contained in the No. 2 container barrel in step four, followed by stirring in the blender, and then grinding to obtain a grease composite composition.

5. The process for preparing the grease composite composition according to claim 4, characterized in that: In the step 2, the amount of the water-containing agent added is 200% to 500% of the weight of the solid in the flask, the temperature in the separation device is 130 to 135°C during reaction separation, the rotation speed of the flask is 30 to 60 r / min during rotary distillation, and the temperature in the flask is 85 to 90°C during rotary distillation, and the vacuum degree of the vacuum pump is 0.8 to 1.2 Pa when the vacuum pump is evacuated.

6. The process for preparing the grease composite composition according to claim 4, characterized in that: In the step three, the operating frequency of the ultrasonic disperser during ultrasonic dispersion is 5 to 13 kHz, and the dispersion time is 3 to 7 minutes. The operating frequency of the ultrasonic disperser during high-speed dispersion is 25 to 28 Hz, and the dispersion time is 25 to 30 minutes. The standing time in the flask is 120 to 150 minutes. The stirring speed of the constant temperature stirring is 30 to 60 r / min, the temperature during constant temperature stirring is 45 to 48° C., and the constant temperature stirring time is 50 to 60 minutes.

7. The process for preparing the grease composite composition according to claim 4, characterized in that: In the step 4, during magnetic stirring, the temperature in the magnetic stirrer is 85-90°C, the stirring speed of the magnetic stirrer is 15-18 r / min, the magnetic stirring time is 120-150 min, and the working frequency of the ultrasonic disperser during ultrasonic dispersion is 18-25 Hz, and the dispersion time is 25-30 min.

8. The process for preparing the grease composite composition according to claim 4, characterized in that: In the step 5, the heating rate of the mixing tower before high-temperature mixing is 6-8°C / min, and the temperature of the mixing tower is increased to 150-180°C. During high-temperature mixing, the stirring speed of the stirring frame in the mixing tower is 18-25r / min, and the high-temperature mixing time is 60-80min.

9. The process for preparing the grease composite composition according to claim 4, characterized in that: In the step six, the temperature in the cooling sedimentation tank is 15-18° C., and the cooling sedimentation time is 100-120 min. During the stirring process, the stirring speed of the stirrer is 30-32 r / min, and the stirring process time is 200-240 min.

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