CN1234826C - Graphite lubricating oil and its preparing method - Google Patents

Graphite lubricating oil and its preparing method Download PDF

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Publication number
CN1234826C
CN1234826C CN 03139216 CN03139216A CN1234826C CN 1234826 C CN1234826 C CN 1234826C CN 03139216 CN03139216 CN 03139216 CN 03139216 A CN03139216 A CN 03139216A CN 1234826 C CN1234826 C CN 1234826C
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graphite
agent
base oil
oil
lubricating oil
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CN1523089A (en
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张汝春
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Abstract

The present invention discloses a graphite lubricating oil and a preparation method thereof. The graphite lubricating oil comprises 0.1 to 0.4% of graphite powder, 0.04 to 0.3% of coupling agent, 1 to 3% of dispersing agent, 1 to 3% of detergent, 4 to 7% of viscosity index improver, 0.2 to 1% of pour point depressant, 4 to 9% of complexing agent, 1.7 to 2.3% of antioxygen preservative and base oil as the balance. The pour point depressant is firstly added to the base oil at the temperature of 65DEG C to 75DEG C, and then, the viscosity index improver is added; after the detergent, the complexing agent, the antioxygen preservative and a graphite addition agent are respectively added., stirred and dispersed evenly, a mixture of the base oil, the viscosity index improver, the detergent, the complexing agent, the antioxygen preservative and the graphite addition agent is sent to a high-pressure homogenization processing device under the pressure of 55 to 60Mpa for secondary high-pressure homogenization processing, and the graphite lubricating oil is obtained; finished products are evenly distributed, no coagula are accumulated, and no delamination occurs within six months.

Description

Graphite lubricating oil (GLO) and preparation method thereof
Technical field the present invention relates to a kind of lubricating oil composition, specifically a kind of lubricating oil composition that contains graphite, comprise Vehicular internal combustion engine oil, internal combustion marine engine oil, automobile-used gear oil, industrial gear oil, industrial hydraulic efficiency oil, vehicle hydraulic efficiency oil, thermal oil and slide rail oil, kelmet wet goods, and its preparation method.
Background technology is because graphite has the stratiform hexagonal crystallographic texture, and in laminate structure inside, adjacent carbon atom is with the covalent linkage mortise, and is survivable; And the distance between layer and the layer is far away, by the more weak Van der Waals force combination of bonding force, therefore when being subjected to shear action, is easy to slide between layer and the layer, plays lubrication.Therefore in lubricating oil, add a certain amount of graphitic composition, can effectively reduce frictional coefficient, increase the anti-extreme pressure energy of lubricating oil, improve lubricating quality.
In fact, because graphite and greasy proportion differ bigger, adopt traditional technology, be about to be incorporated in the lubricating oil after graphite is ground to certain particle size, it is mixed, the graphite lubricating oil (GLO) of making is easy to produce the precipitation of graphite and greasy layering and graphite in storing transportation and use.Not only be difficult to play good lubrication, can produce detrimentally affect to the device that uses this class lubricating oil on the contrary.
The many certain amount of dispersant, the additive of coupling agent and other kinds of in preparation process, adding of comparatively advanced in the market graphite lubricating oil (GLO).This way has alleviated the separation problem of graphite and lubricating oil to a certain extent, played certain improving effect, but, because manufacturing process and component are selected the deficiency on the compatibility, this class graphite lubrication oil-proofness still can not be satisfactory, when particularly depositing in the long period, layering and precipitation still appear to some extent.
Summary of the invention the object of the present invention is to provide a kind of graphite lubricating oil (GLO) and preparation method thereof, in order to overcome the defective of above-mentioned prior art and product, thoroughly solves the Solid-Liquid Separation problem, makes the stability of graphite lubricating oil (GLO) better.
To achieve these goals, graphite lubricating oil (GLO) of the present invention is composed of the following components,
Graphite Powder 99 0.1-0.4% (weight percent, down together), coupling agent 0.04-0.3%,
Dispersion agent 1-3%, purification agent 1-3%, viscosity index improver 4-7%,
Pour point depressant 0.2-1%, recombiner 4-9%, antioxidant preservative 1.7-2.3%,
Surplus is a base oil;
Wherein the particle diameter of Graphite Powder 99 requires: the Graphite Powder 99 particle diameter more than 99.5% is less than 6 microns, and all the other are all less than 9 microns;
Coupling agent is three (dioctyl-phosphorus acyloxy) isopropyl titanate, any in monoalkoxy phosphate type titanic acid ester and the two fatty acyl group metatitanic acid second diester;
Dispersion agent is the two succimides of polyisobutene, any in the two succimides of boronation polyisobutene;
Purification agent is the low alkali value calcium sulphonate, middle base number calcium alkylbenzenesulfonate, polyisobutene sulfation barium salt, any in the alkyl sodium salicylate;
Viscosity index improver is poly-second third glue;
Pour point depressant is a polymethyl acrylate;
Recombiner is the I. C. engine oil recombiner, any in the gear oil compounding agent;
Antioxidant preservative is a sulfuric acid fourth octyl group zinc salt, any in the two octyl group basic zinc salt of sulfuric acid;
Base oil is 150SN, 400SN, any one or more among the 150BS.
The preparation method of graphite lubricating oil (GLO) of the present invention is:
1), in having the reactor of agitator, fully contact moistening Graphite Powder 99 with base oil;
2), with behind the base oil dilution coupling agent, drop in the above-mentioned Graphite Powder 99, carry out surface-active-treatment, extruding was stirred 60--100 minute, obtained surface-active-treatment liquid;
3), dilute dispersion agent, the dispersion agent of dilution is joined in the surface-active-treatment liquid, continue to stir 60--100 minute, carry out the dispersoid processing, obtain dispersoid solution with base oil;
4), add base oil in dispersoid solution, the high-pressure homogeneous treatment unit of sending into 55-60Mpa carries out high pressure homogenizing to be handled, and obtains high pressure homogenizing solution, i.e. the graphite auxiliary agent;
5), under 65--75 ℃ temperature, in base oil, at first add pour point depressant, add viscosity index improver then, and add purification agent respectively, recombiner, antioxidant preservative and graphite auxiliary agent, the high-pressure homogeneous treatment unit that dispersed with stirring is sent into 55-60Mpa after evenly carries out the secondary high-pressure processing that homogenizes, and obtains graphite lubricating oil (GLO).
In the technical program, all components and consumption thereof all obtain by the several times experiment, it is key of the present invention, wherein the big consumption of the adding of purification agent and dispersion agent is a focus technology of the present invention, the function of purification agent mainly is the suspension effect that swims, and in order to disperse to swim graphite particle, makes solid materials (particle) not adhere to or be deposited on wall or bottom, by introducing the dispersion agent of purification agent and capacity, make the stability of finished product obviously improve.
The setting pressure that twice high pressure homogenizing handled is an another gordian technique of the present invention, only experiment showed, just to prepare solid-liquid phase stably dispersing in this pressure range, is difficult for the graphite lubricating oil (GLO) of layering and precipitating.
Dilute dispersion agent with base oil, the dispersion agent that dilutes is joined in the surface-active-treatment liquid, continue to stir 60--100 minute, extruding churning time herein is enough abundant.This time range is one of gordian technique of the present invention, only reaches this time, can guarantee graphite particulate effectively by coupling agent wrap up more evenly, slick and sly.
The present invention compared with the prior art owing to added the purification agent and the dispersion agent of capacity, and has done whole prescription to improve significantly, and prescription and preparation technology's design more become perfect.Graphite lubricating oil (GLO) of the present invention and the graphite lubricating oil (GLO) that does not add (or only having on a small quantity) purification agent and adding paucidisperse agent (about 0.5%) are compared discovery, the former obviously reduces than latter throw out, the former did not see layering in 6 months, and the latter found tangible layering in the time of 30 days.Microscopic examination particles dispersed degree shows, the former uniform distribution, and no grumeleuse is assembled, and the latter is precipitated obviously, and tangible cohesion block is arranged.
Embodiment specifies the present invention below in conjunction with preparation embodiment.
Embodiment one
1), in having the reactor of agitator, fully contact moistening 0.1 kilogram of Graphite Powder 99 with 0.1 kilogram of base oil (150SN), the particle diameter of Graphite Powder 99 requires: the Graphite Powder 99 particle diameter more than 99.5% is less than 6 microns, and all the other are all less than 9 microns;
2), with behind 0.04 kilogram of three (dioctyl-phosphorus acyloxy) isopropyl titanate of 0.04 kilogram of base oil (150SN) dilution, drop in the above-mentioned Graphite Powder 99, carry out surface-active-treatment, extruding was stirred 60--100 minute, obtained surface-active-treatment liquid;
3), with the two succimides of 1 kilogram of polyisobutene of 1 kilogram of base oil (150SN) dilution, the two succimides of the polyisobutene of dilution are joined in the surface-active-treatment liquid, continue to stir 60--100 minute, carry out the dispersoid processing, obtain dispersoid solution;
4), in dispersoid solution, add 7.72 kilograms of base oils (150SN), the high-pressure homogeneous treatment unit of sending into 55-60Mpa carries out high pressure homogenizing to be handled, and obtains high pressure homogenizing solution, i.e. the graphite auxiliary agent;
5), in 79.1 kilograms of base oils (150SN), at first adding 0.2 kg polypropylene acid methyl esters (T132) under 65--75 ℃ the temperature, add 4 kilograms of OCPA (poly-second third glue) then, and add 1 kilogram of low alkali value calcium sulphonate respectively, 4 kilograms of I. C. engine oil recombiners (T1288), 1.7 kilo sulfuric acid fourth octyl group zinc salt, with 10 kilograms of graphite auxiliary agents, the high-pressure homogeneous treatment unit that dispersed with stirring is sent into 55-60Mpa after evenly carries out the secondary high-pressure processing that homogenizes, and obtains the double centner graphite lubricating oil (GLO).
Embodiment two
1), in having the reactor of agitator, fully contact moistening 0.2 kilogram of Graphite Powder 99 with 0.2 kilogram of base oil (400SN), the particle diameter of Graphite Powder 99 requires: the Graphite Powder 99 particle diameter more than 99.5% is less than 6 microns, and all the other are all less than 9 microns;
2), with after 0.1 kilogram of monoalkoxy phosphate type titanic acid ester of 0.1 kilogram of base oil (400SN) dilution, drop in the above-mentioned Graphite Powder 99, carry out surface-active-treatment, extruding was stirred 60-100 minute, obtained surface-active-treatment liquid;
3), with the two succimides of 2 kilograms of boronation polyisobutene of 2 kilograms of base oils (400SN) dilution, the two succimides of the boronation polyisobutene of dilution are joined in the surface-active-treatment liquid, continue to stir 60--100 minute, carry out the dispersoid processing, obtain dispersoid solution;
4), in dispersoid solution, add 15.4 kilograms of base oils (400SN), the high-pressure homogeneous treatment unit of sending into 55-60Mpa carries out high pressure homogenizing to be handled, and obtains high pressure homogenizing solution, i.e. the graphite auxiliary agent;
5), in 64.4 kilograms of base oils (400SN), at first adding 0.6 kg polypropylene acid methyl esters (T132) under 65--75 ℃ the temperature, add 5 kilograms of OCPA (poly-second third glue) then, and add base number calcium alkylbenzenesulfonate in 2 kilograms respectively, 6 kilograms of gear oil compounding agents (H343), 2.0 the two octyl group basic zinc salt of kilo sulfuric acid, with 20 kilograms of graphite auxiliary agents, the high-pressure homogeneous treatment unit that dispersed with stirring is sent into 55-60Mpa after evenly carries out the secondary high-pressure processing that homogenizes, and obtains the double centner graphite lubricating oil (GLO).
Embodiment three
1), in having the reactor of agitator, fully contact moistening 0.4 kilogram of Graphite Powder 99 with 0.4 kilogram of base oil (150BS), the particle diameter of Graphite Powder 99 requires: the Graphite Powder 99 particle diameter more than 99.5% is less than 6 microns, and all the other are all less than 9 microns;
2), with behind 0.30 kilogram of two fatty acyl group metatitanic acid second diester of 0.30 kilogram of base oil (150BS) dilution, drop in the above-mentioned Graphite Powder 99, carry out surface-active-treatment, extruding was stirred 60--100 minute, obtained surface-active-treatment liquid;
3), with the two succimides of 3 kilograms of polyisobutene of 3 kilograms of base oils (150BS) dilution, the two succimides of the polyisobutene of dilution are joined in the surface-active-treatment liquid, continue to stir 60--100 minute, carry out the dispersoid processing, obtain dispersoid solution;
4), in dispersoid solution, add 32.6 kilograms of base oils (150BS), the high-pressure homogeneous treatment unit of sending into 55-60Mpa carries out high pressure homogenizing to be handled, and obtains high pressure homogenizing solution, i.e. the graphite auxiliary agent;
5), in 37.7 kilograms of base oils (150BS), at first adding 1.0 kg polypropylene acid methyl esters (T132) under 65--75 ℃ the temperature, add 7 kilograms of OCPA (poly-second third glue) then, and add 3 kilograms of alkyl sodium salicylates respectively, 9 kilograms of I. C. engine oil recombiners (T1216), 2.3 kilo sulfuric acid fourth octyl group zinc salt, with 40 kilograms of graphite auxiliary agents, the high-pressure homogeneous treatment unit that dispersed with stirring is sent into 55-60Mpa after evenly carries out the secondary high-pressure processing that homogenizes, and obtains the double centner graphite lubricating oil (GLO).
Embodiment four
1), in having the reactor of agitator, fully contact moistening 0.2 kilogram of Graphite Powder 99 with 0.2 kilogram of base oil (500SN), the particle diameter of Graphite Powder 99 requires: the Graphite Powder 99 particle diameter more than 99.5% is less than 6 microns, and all the other are all less than 9 microns;
2), with after 0.1 kilogram of monoalkoxy phosphate type titanic acid ester of 0.1 kilogram of base oil (500SN) dilution, drop in the above-mentioned Graphite Powder 99, carry out surface-active-treatment, extruding was stirred 60--100 minute, obtained surface-active-treatment liquid;
3), with the two succimides of 2 kilograms of boronation polyisobutene of 2 kilograms of base oils (500SN) dilution, the two succimides of the boronation polyisobutene of dilution are joined in the surface-active-treatment liquid, continue to stir 60--100 minute, carry out the dispersoid processing, obtain dispersoid solution;
4), in dispersoid solution, add 15.4 kilograms of base oils (500SN), the high-pressure homogeneous treatment unit of sending into 55-60Mpa carries out high pressure homogenizing to be handled, and obtains high pressure homogenizing solution, i.e. the graphite auxiliary agent;
5), in 64.4 kilograms of base oils (500SN), at first adding 0.6 kg polypropylene acid methyl esters (T132) under 65--75 ℃ the temperature, add 5 kilograms of OCPA (poly-second third glue) then, and add 2 kilograms of polyisobutene sulfation barium salts respectively, 6 kilograms of gear oil compounding agents, 2.0 the two octyl group basic zinc salt of kilo sulfuric acid, 100ppm methyl-silicone oil (defoamer) and 20 kilograms of graphite auxiliary agents, the high-pressure homogeneous treatment unit that dispersed with stirring is sent into 55-60Mpa after evenly carries out the secondary high-pressure processing that homogenizes, and obtains the double centner graphite lubricating oil (GLO).

Claims (2)

1, a kind of graphite lubricating oil (GLO) is characterized in that: composed of the following components,
Graphite Powder 99 0.1-0.4% (weight percent, down together)
Coupling agent 0.04-0.3%
Dispersion agent 1-3%
Purification agent 1-3%
Viscosity index improver 4-7%
Pour point depressant 0.2-1%
Recombiner 4-9%
Antioxidant preservative 1.7-2.3%
Surplus is a base oil;
Wherein the particle diameter of Graphite Powder 99 requires: the Graphite Powder 99 particle diameter more than 99.5% is less than 6 microns, and all the other are all less than 9 microns;
Coupling agent is three (dioctyl-phosphorus acyloxy) isopropyl titanate, any in monoalkoxy phosphate type titanic acid ester and the two fatty acyl group metatitanic acid second diester;
Dispersion agent is the two succimides of polyisobutene, any in the two succimides of boronation polyisobutene;
Purification agent is the low alkali value calcium sulphonate, middle base number calcium alkylbenzenesulfonate, polyisobutene sulfation barium salt, any in the alkyl sodium salicylate;
Viscosity index improver is poly-second third glue;
Pour point depressant is a polymethyl acrylate;
Recombiner is the I. C. engine oil recombiner, any in the gear oil compounding agent;
Antioxidant preservative is a sulfuric acid fourth octyl group zinc salt, any in the two octyl group basic zinc salt of sulfuric acid;
Base oil is 150SN, 400SN, any one or more among the 150BS.
2, the preparation method of graphite lubricating oil (GLO) as claimed in claim 1 is characterized in that: realize by following steps:
1), in having the reactor of agitator, fully contact moistening Graphite Powder 99 with base oil;
2), with behind the base oil dilution coupling agent, drop in the above-mentioned Graphite Powder 99, carry out surface-active-treatment, extruding was stirred 60-100 minute, obtained surface-active-treatment liquid;
3), dilute dispersion agent, the dispersion agent of dilution is joined in the surface-active-treatment liquid, continue to stir 60-100 minute, carry out the dispersoid processing, obtain dispersoid solution with base oil;
4), add base oil in dispersoid solution, the high-pressure homogeneous treatment unit of sending into 55-60Mpa carries out high pressure homogenizing to be handled, and obtains high pressure homogenizing solution, i.e. the graphite auxiliary agent;
5), under 65-75 ℃ temperature, in base oil, at first add pour point depressant, add viscosity index improver then, and add purification agent respectively, recombiner, antioxidant preservative and graphite auxiliary agent, the high-pressure homogeneous treatment unit that dispersed with stirring is sent into 55-60Mpa after evenly carries out the secondary high-pressure processing that homogenizes, and obtains graphite lubricating oil (GLO).
CN 03139216 2003-09-08 2003-09-08 Graphite lubricating oil and its preparing method Expired - Fee Related CN1234826C (en)

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CN101338242B (en) * 2008-08-14 2011-10-05 济南润中润科技发展有限公司 Gear oil potentiator special for pumping unit
CN101338238B (en) * 2008-08-14 2010-06-09 济南润中润科技发展有限公司 Internal combustion engine oil potentiator special for shipping
CN101880577B (en) * 2010-07-01 2013-04-17 邹鸣 Solid-liquid phase composite internal combustion engine oil
CN101967419A (en) * 2010-11-02 2011-02-09 天津东方舜能润滑材料有限公司 Ceramic alloy lubricating oil special for dredging workboat engine and preparation method thereof
CN102154053A (en) * 2011-03-28 2011-08-17 陈强 Nanographite additive for water-based cutting fluid and preparation method thereof
CN104312701A (en) * 2014-11-14 2015-01-28 柳州聚龙科技有限公司 Lubrication oil
CN106802239A (en) * 2015-11-25 2017-06-06 青岛征和工业股份有限公司 Lubricating oil and engine timing chain test method when simulated engine works
CN106085561A (en) * 2016-06-07 2016-11-09 江苏金迪润滑油有限公司 A kind of low temperature resistant high wearproof lubricant of mineral oil base
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CN106085554A (en) * 2016-06-07 2016-11-09 江苏金迪润滑油有限公司 A kind of low temperature resistant lubricating oil
CN106147939A (en) * 2016-06-28 2016-11-23 陈小刚 A kind of additive for wear resistance of lubricating oil based on few layer graphene microplate and preparation method thereof

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