CN110452755B - Viscosity index improver and preparation method thereof - Google Patents
Viscosity index improver and preparation method thereof Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F8/34—Introducing sulfur atoms or sulfur-containing groups
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M149/00—Lubricating compositions characterised by the additive being a macromolecular compound containing nitrogen
- C10M149/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The invention provides a viscosity index improver and a preparation method thereof. The preparation method of the viscosity index improver comprises the following steps: s1, mixing a grafting initiator, maleic anhydride, an ethylene propylene rubber polymer and a solvent, and carrying out grafting reaction to obtain a first solution of an ethylene propylene copolymer grafted by maleic anhydride; and S2, mixing the first solution with an amine compound and carrying out amination reaction to obtain the viscosity index improver. The anhydride compound is easy to perform amidation reaction with organic amine, and the reaction temperature and pressure are low, so that the preparation process of the ethylene-propylene copolymer viscosity index improver can be performed at a low temperature, and experiments prove that the ethylene-propylene copolymer viscosity index improver prepared by the preparation method has low-temperature stability, high-temperature thickening capacity and shear stability reaching the level of the T615 viscosity index improver.
Description
Technical Field
The invention relates to the field of petrochemical industry, in particular to a viscosity index improver and a preparation method thereof.
Background
Viscosity index improvers, also known as tackifiers, are used primarily in internal combustion engine oils, hydraulic oils, automatic transmission fluids, and gear oils, and are used second to detergents and dispersants in the range of lubricating oil additives. The viscosity index improver is an oil-soluble chain-shaped high molecular compound, can be dissolved in hydrocarbon base oil used for a lubricant, and has small influence on the internal friction of the base oil due to the shrinkage of a high molecular coil of the viscosity index improver at low temperature, so that the viscosity of an oil product is relatively small; the high-molecular coil of the viscosity index improver swells and stretches at high temperature, the hydrodynamic volume and the surface area are increased, the internal friction of the base oil is obviously increased, the viscosity of the base oil is increased, the high-temperature lubricity of the base oil is improved, and the purpose of improving the viscosity performance of an oil product at different temperatures is achieved.
The viscosity index improver can thicken base oil, change the viscosity-temperature property of oil products, ensure that the oil products have good high-temperature lubricity and low-temperature fluidity, reduce the consumption of fuel and lubricating oil and realize the generalization of the oil products. In addition, the viscosity index improver is not only required to have no obvious harmful effect on the oxidation stability and detergency of the oil product, but also required to have moderate viscosity loss of the thickened oil under the action of mechanical shear. In practical application, a good viscosity index improver not only requires large thickening capacity and good shear stability, but also requires good low-temperature performance, thermal oxidation stability and good compatibility with other oil additives (such as pour point depressants). Therefore, in the development and production of lubricating oils, care must be taken to select viscosity index improvers.
The viscosity index improver commonly used is four main types of hydrogenated styrene diene (styrene-isoprene) polymer (HSD), Polyisobutylene (PIB), ethylene-propylene copolymer (OCP) and Polymethacrylate (PMA). The ethylene-propylene copolymer viscosity index improver (OCP) has the advantages of excellent comprehensive performance, low price and the like in the use of engines, so the ethylene-propylene copolymer viscosity index improver is widely applied and developed. The ethylene-propylene copolymer can be obtained through two ways, one is that ethylene-propylene rubber with higher molecular weight is degraded to certain molecular weight through thermal oxidation and machinery, so as to meet the use requirement; and the other is that the ethylene propylene rubber is directly polymerized to obtain a polymer with proper molecular weight or the ethylene propylene rubber with higher molecular weight is chemically degraded and then is subjected to functionalization treatment to obtain the ethylene propylene rubber.
The ethylene propylene rubber chemical degradation process is to dissolve a polymer in base oil, then carry out free radical chain scission, and finally introduce a functionalized substance, and has the main defects that: one is that the polymer has high dissolution temperature, and needs longer dissolution time and higher energy consumption; secondly, the viscosity of the base oil and the ethylene-propylene polymer is greatly changed along with the temperature, so that the free radical grafting process also needs to be carried out at a higher temperature; thirdly, the functionalized substances and the reaction residual substances must be removed under the conditions of high temperature and vacuum; and fourthly, the product contains base oil, and for different users, the adjustment of the using process is caused due to the difference of the source of the base oil.
Disclosure of Invention
The invention mainly aims to provide a viscosity index improver and a preparation method thereof, and aims to solve the problem of high energy consumption caused by high temperature in the existing preparation process of the ethylene-propylene copolymer viscosity index improver.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for preparing a viscosity index improver, comprising the steps of: s1, mixing a grafting initiator, maleic anhydride, an ethylene propylene rubber polymer and a solvent, and carrying out grafting reaction to obtain a first solution of an ethylene propylene copolymer grafted by maleic anhydride; and S2, mixing the first solution with an amine compound and carrying out amination reaction to obtain the viscosity index improver.
Further, the weight of the maleic anhydride is 1.5-3.0% of the weight of the ethylene propylene rubber polymer.
Further, the ethylene-propylene rubber polymer is a copolymer of ethylene and propylene, wherein the corresponding content of ethylene is 48-70%, the Mooney viscosity of the ethylene-propylene rubber polymer is preferably 5-60, and the weight of the ethylene-propylene rubber polymer is preferably 4-20% of the total weight of the ethylene-propylene rubber polymer and the solvent.
Further, the grafting initiator is peroxide, preferably the grafting initiator comprises benzoyl peroxide and/or dicumyl peroxide, and preferably the weight of the grafting initiator is 1.0-2.0% of that of the ethylene propylene rubber polymer.
Further, the solvent includes any one or more of aromatic hydrocarbons, naphthenic hydrocarbons, and linear alkanes including any one or more of hexane, heptane, and octane, and preferably the solvent is hexane.
Further, in step S1, the reaction temperature of the grafting reaction is 80-120 ℃, the reaction pressure is 0.1-0.2 MPa, and the reaction time is 1.0-4.0 h.
Further, the solid content of the first solution is 5-40%.
Further, the amine compound is H2N(CH2CH2NH)mH, wherein m is 1-6, preferably 2 or 3, and the weight of the amine compound is preferably 0.05-0.2% of the weight of the ethylene propylene rubber polymer.
Further, step S2 includes: s21, heating the first solution to a first temperature, preferably the first temperature is 80-120 ℃; and S22, dropwise adding an amine compound into the heated first solution under the stirring condition, so that the first solution and the amine compound are mixed and subjected to amination reaction to obtain a second solution containing the viscosity index improver, wherein the reaction pressure of the amination reaction is preferably 0.1-0.2 MPa, and the reaction time is 2-4 h.
Further, after step S22, step S2 further includes the step of separating the purified viscosity index improver from the second solution; preferably, the separation and purification step comprises: and subjecting the second solution to falling film evaporation to obtain the viscosity index improver.
According to another aspect of the present invention, there is provided a viscosity index improver comprising CH3-(CH2CH2) a-(CH2CH(CH3))b-CH(COOH)CH2(COHN(CH2CH2)mNH2) Wherein a is 500-1000, b is 500-1200, a: b is 0.9-1.5: 1, preferably 0.95-1.2; m is 1 to 6, preferably 3 or 4.
Further, a is 700-900; preferably, b is 700-1000; preferably, a: b is 0.95 to 1.2; preferably m is 3 or 4.
The technical scheme of the invention is applied to provide a preparation method of a viscosity index improver, and the preparation method comprises the steps of firstly mixing raw materials comprising a grafting initiator, maleic anhydride, an ethylene-propylene rubber polymer and a solvent, carrying out grafting reaction to obtain a first solution of the ethylene-propylene copolymer grafted by the maleic anhydride, and then mixing the first solution with an amine compound, and carrying out amination reaction to obtain the viscosity index improver. The anhydride compound is easy to perform amidation reaction with organic amine, and the reaction temperature and pressure are low, so that the preparation process of the ethylene-propylene copolymer viscosity index improver can be performed at a low temperature, and experiments prove that the ethylene-propylene copolymer viscosity index improver prepared by the preparation method has low-temperature stability, high-temperature thickening capacity and shear stability reaching the level of the T615 viscosity index improver.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that the terms first, second and the like in the description and in the claims of the present invention are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged under appropriate circumstances in order to facilitate the description of the embodiments of the invention herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
As can be seen from the background art, there is a need in the prior art to provide an ethylene-propylene rubber lubricating oil viscosity index improver with high thickening capability and low shear stability index. The inventors of the present invention have studied in view of the above problems and provide a method for producing a viscosity index improver, comprising the steps of: s1, mixing a grafting initiator, maleic anhydride, an ethylene propylene rubber polymer and a solvent, and carrying out grafting reaction to obtain a first solution of an ethylene propylene copolymer grafted by maleic anhydride; s2, mixing the first solution with an amine compound and carrying out amination reaction to obtain the viscosity index improver.
The product of the ethylene-propylene copolymer viscosity index improver obtained by the preparation method has the advantages that the kinematic viscosity, the high-temperature thickening capacity and the shear stability can reach the level of the T615 viscosity index improver; the preparation method can be directly reconstructed on the existing production device, the added grafting reaction and amination reaction equipment belongs to common chemical equipment, the operation conditions are not harsh, the original processes of high-temperature flash evaporation concentration and extrusion granulation of glue solution are omitted, and the actual operation difficulty is greatly simplified; the preparation method can use the transition materials generated in the grade switching process of the ethylene propylene rubber, not only can fully utilize raw material resources, but also can greatly improve the added value of the part of materials and greatly improve the efficacy creating capability of the device; in addition, a certain amount of waste liquid containing maleic anhydride and polyene polyamine can be generated by the amination process, organic impurities in the waste liquid can be removed by an acid-base neutralization process, and the waste liquid can meet the production requirements after being recycled.
An exemplary embodiment of a method for preparing a viscosity index improver provided according to the present invention will be described in more detail below. These exemplary embodiments may, however, be embodied in many different forms and should not be construed as limited to only the embodiments set forth herein. It should be understood that these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of these exemplary embodiments to those skilled in the art.
First, step S1 is executed: and mixing a grafting initiator, maleic anhydride, an ethylene-propylene rubber polymer and a solvent, and carrying out grafting reaction to obtain a first solution of an ethylene-propylene copolymer grafted by maleic anhydride. The solvent may include any one or more of aromatic hydrocarbons, naphthenic hydrocarbons and straight-chain alkanes including any one or more of hexane, heptane and octane, and those skilled in the art can reasonably select the kind of the solvent according to the prior art. Preferably, the solvent is hexane, the ethylene propylene rubber polymer hexane solution is used as a raw material, the characteristics of full extension of the polymer in the hexane solution and low system viscosity are fully utilized, the reaction can be carried out at low reaction temperature and pressure, and the high-temperature operation condition is avoided.
In the step S1, the weight of the maleic anhydride is preferably 1.5 to 3.0% of the weight of the ethylene propylene rubber polymer. By limiting the weight of the maleic anhydride to the preferable range, a proper amount of maleic anhydride can be grafted, so that the viscosity index improver with low-temperature stability, high-temperature thickening capability and shear stability reaching the T-615 level can be obtained after amination reaction of the ethylene-propylene copolymer grafted with the maleic anhydride.
In the step S1, the ethylene-propylene rubber polymer is an ethylene-propylene copolymer, preferably, the ethylene content in the ethylene-propylene rubber polymer is 48 to 70%; more preferably, the Mooney viscosity ML of the ethylene-propylene rubber polymer1+4 100℃5-60 percent, wherein the weight of the polymer is 4-20 percent of the total weight of the ethylene propylene rubber polymer and the solvent. By limiting the ethylene content, the Mooney viscosity and the polymer content in the preferable ranges, a proper amount of maleic anhydride can be grafted on the ethylene-propylene copolymer, and the viscosity index improver obtained after the amination reaction of the ethylene-propylene copolymer grafted with the maleic anhydride has excellent performance.
In the above step S1, in order to improve the grafting efficiency of maleic anhydride on the ethylene-propylene rubber polymer, preferably, the grafting initiator is peroxide; more preferably, the grafting initiator comprises benzoyl peroxide and/or dicumyl peroxide. In order to avoid waste caused by excessive weight of the grafting initiator, the weight of the grafting initiator is preferably 1.0-2.0% of the weight of the ethylene propylene rubber polymer.
In a preferred embodiment, in step S1, the reaction temperature of the graft polymerization reaction is 80-120 ℃, the reaction pressure is 0.1-0.2 MPa, and the reaction time is 1.0-4.0 h. Specifically, the grafting initiator and the maleic anhydride are added into a solution containing an ethylene propylene rubber polymer, grafting reaction is carried out at the reaction temperature of 80-120 ℃ and the reaction pressure of 0.1-0.2 MPa for 1.0-4.0 h, and after the reaction is finished, a first solution containing an intermediate product of the ethylene propylene copolymer grafted by the maleic anhydride is obtained.
In the preferred embodiment, after the reaction is completed, the first solution may be obtained by flash evaporation, and in order to improve the process efficiency of the subsequent amination reaction, the first solution with a solid content of 5 to 40% is preferably obtained by a flash evaporation process. The process conditions of the above flash evaporation can be reasonably set by those skilled in the art according to the prior art, and are not described herein again.
After the step S1 is performed, a step S2 is performed: and mixing the first solution containing the ethylene-propylene copolymer grafted by maleic anhydride with an amine compound, and carrying out amination reaction to obtain the viscosity index improver. The kind of the above amine compound can be reasonably selected by those skilled in the art according to the prior art, and in order to improve the low temperature stability, high temperature thickening ability and shear stability of the viscosity index improver obtained after amination reaction, the above amine compound is preferably H2N(CH2)mNH2Wherein m is 1-6, preferably 3 or 4; more preferably, the weight of the amine compound is 0.05 to 0.2% of the weight of the ethylene-propylene rubber polymer.
The step S2 may include: s21, heating the first solution to a first temperature; and S22, dropwise adding an amine compound into the heated first solution under the stirring condition, so that the first solution and the amine compound are mixed and subjected to amination reaction to obtain a second solution containing the viscosity index improver. In order to fully perform amination reaction on the maleic anhydride grafted ethylene-propylene copolymer in the first solution and improve the efficiency of the amination reaction, in a preferred embodiment, the first solution containing the maleic anhydride grafted ethylene-propylene copolymer is heated to 80-120 ℃, then the amine compound is dropwise added under the stirring condition, and the reaction is performed for 2-4 hours under the reaction pressure of 0.1-0.2 MPa.
After the step S22, the step S2 may further include a step of separating and purifying the viscosity index improver from the second solution; in order to improve the efficiency of the separation and purification, preferably, the separation and purification step includes: and subjecting the second solution to falling film evaporation to obtain the viscosity index improver.
According to another aspect of the invention, the viscosity index improver is CH3- (CH2CH2)a-(CH2CH(CH3))b-CH(COOH)CH2(COHN(CH2CH2)mNH2) Wherein a is 500-1000, preferably 700-900; b is 500 to 1200, preferably 700 to 1000; a: b is 0.9-1.5, preferably 0.95-1.2; m is 1 to 6, preferably 3 or 4.
The low-temperature stability, high-temperature thickening capability and shear stability of the ethylene-propylene copolymer viscosity index improver can reach the level of a T615 viscosity index improver.
The method for producing the viscosity index improver according to the present invention will be further described with reference to examples and comparative examples.
The following examples were all carried out in a laboratory 1.0L autoclave, which employed an electric heating method, a jacket heat transfer medium was heat transfer oil, and an ethylene-propylene polymer hexane solution was taken from an ethylene-propylene rubber production apparatus.
Example 1
Hexane solution of ethylene propylene Polymer in this exampleThe initial temperature of (A) is 50-65 ℃ (60 ℃), the solid content is 4.7%, the ethylene content is 49.5%, and the Mooney viscosity (ML) of the polymer1+4 1006.8 ℃ C.), a polymer number average molecular weight of 7.7 ten thousand, a weight average molecular weight of 15.3 ten thousand and a relative molecular mass distribution of 1.98.
Adding 0.6L of the polymer hexane solution into a reaction kettle, adding benzoyl peroxide and maleic anhydride, wherein the weight of the maleic anhydride is 2.0% of the weight of the ethylene propylene rubber polymer, the weight of the benzoyl oxide is 1.5% of the weight of the ethylene propylene rubber polymer, the stirring revolution is 125r/min, the internal temperature of the reaction kettle is 80-82 ℃, the pressure of the reaction kettle is 0.115-0.120 MPa, stopping stirring after 4 hours of reaction, slowly opening a gas phase outlet valve to perform flash evaporation operation, condensing discharged gas phase materials through a condenser, and stopping the flash evaporation operation and heating when the recycled condensate is close to 200 mL. And (5) after the pressure of the reaction kettle is recovered to normal pressure. At this point, the solids content of the gum was 6.9% and the temperature was 66 ℃.
Heating 400mL of the hexane solution to 80-82 ℃, dropwise adding propylene diamine into the hexane solution by using a feeder under the stirring condition, wherein the weight of the propylene diamine is 0.10% of the weight of the ethylene propylene rubber polymer, the stirring rotation number is 125r/min, reacting for 4 hours under the reaction pressure of 0.115-0.120 MPa, stopping stirring, slowly opening a gas phase outlet valve to perform flash evaporation operation, condensing discharged gas phase materials by a condenser, and stopping the flash evaporation operation when the recovered condensate is close to 50 mL. Opening a vacuum valve at the rear part of the condenser, carrying out vacuum desolventizing operation, removing low molecules in vacuum for 10 minutes after no condensate exists, closing the vacuum valve and electrically heating, recovering the pressure of the reaction kettle, continuously injecting nitrogen to 0.15MPa, and discharging materials when the temperature of the reaction kettle is reduced to below 50 ℃.
Example 2
This example differs from example 1 in that:
the solid content of the ethylene-propylene polymer hexane solution was 5.1%, and the solid content of the flash-evaporated gum solution was 7.4%.
Example 3
This example differs from example 1 in that:
the solid content of the ethylene-propylene polymer hexane solution was 15.2%, and the solid content of the flash-evaporated gum solution was 22.2%.
Example 4
This example differs from example 2 in that:
the ethylene-propylene rubber polymer has an ethylene content of 51% and a Mooney viscosity of 55.
Example 5
This example differs from example 2 in that:
the ethylene-propylene rubber polymer had an ethylene content of 68% and a Mooney viscosity of 9.5.
Example 6
This example differs from example 4 in that:
the weight of the maleic anhydride was 1.5% of the weight of the ethylene-propylene rubber polymer.
Example 7
This example differs from example 4 in that:
the weight of the maleic anhydride was 3.0% of the weight of the ethylene-propylene rubber polymer.
Example 8
This example differs from example 6 in that:
the weight of the grafting initiator is 1.0 percent of the weight of the ethylene propylene rubber polymer.
Example 9
This example differs from example 6 in that:
the weight of the grafting initiator is 2.0 percent of the weight of the ethylene propylene rubber polymer.
Example 10
This example differs from example 8 in that:
the internal temperature of the reaction kettle is 90-92 ℃, the pressure of the reaction kettle is 0.145-0.150 MPa, and the reaction lasts for 4 hours.
Example 11
This example differs from example 8 in that:
the internal temperature of the reaction kettle is 118-120 ℃, the pressure of the reaction kettle is 0.185-0.190 MPa, and the reaction lasts for 1 hour.
Example 12
The present embodiment differs from embodiment 10 in that:
the weight of the propylene diamine was 0.05% of the weight of the ethylene propylene rubber polymer.
Example 13
The present embodiment differs from embodiment 10 in that:
the weight of the propylene diamine is 0.20 percent of the weight of the ethylene propylene rubber polymer.
Example 14
This example differs from example 12 in that:
heating the hexane solution to 80-82 ℃, dropwise adding propane diamine into the hexane solution by using a feeder under the stirring condition, and reacting for 2 hours under the reaction pressure of 0.145-0.150 MPa.
Example 15
This example differs from example 12 in that:
heating the hexane solution to 118-120 ℃, dropwise adding propane diamine into the hexane solution by using a feeder under the stirring condition, and reacting for 4 hours under the reaction pressure of 0.185-0.195 MPa.
The viscosity index improvers were rated as shown in table 1, and the kinematic viscosity, thickening ability and shear stability of the viscosity index improvers prepared in examples 1 to 15 were measured by GB/T265-88 "kinematic viscosity measurement and calculation of kinematic viscosity of petroleum products", SH/T0566-93 "measurement of thickening ability of viscosity index improvers of lubricating oils", and SH/T0103-2007 "measurement of shear stability with polymers (diesel injector method)", and the results of the measurements are shown in table 2.
TABLE 1 lubricating oil viscosity index improver grading Standard Table
Table 2 examples test data table
From the above test results, it can be seen that the viscosity index improvers prepared in examples 1 to 15 of the present application all achieved T-615 levels in the viscosity index improver grade standard.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
1. the ethylene-propylene copolymer viscosity index improver product obtained by the invention has low-temperature stability, high-temperature thickening capability and shear stability reaching the level of T-615;
2. the method takes the ethylene propylene rubber polymer hexane solution as a raw material, fully utilizes the characteristics of full extension of the polymer in the hexane solution and low system viscosity, can carry out reaction at low reaction temperature and pressure, and avoids high-temperature operation conditions;
3. the preparation method of the viscosity index improver can be directly reconstructed on the existing production device, the added grafting reaction and amination reaction equipment belongs to common chemical equipment, the operation conditions are not harsh, the original high-temperature flash evaporation concentration and extrusion granulation processes of glue solution are omitted, and the actual operation difficulty is greatly simplified;
4. the preparation method of the viscosity index improver can use transition materials generated in the grade switching process of the ethylene propylene rubber, not only can fully utilize raw material resources, but also can greatly improve the additional value of the part of materials and greatly improve the efficacy creating capability of the device;
5. the grafting reaction and amination reaction process can generate a certain amount of waste liquid containing maleic anhydride and polyene polyamine, organic impurities in the waste liquid can be removed through an acid-base neutralization process, and the waste liquid can be recycled to meet production requirements.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (21)
1. A preparation method of a viscosity index improver is characterized by comprising the following steps:
s1, mixing a grafting initiator, maleic anhydride, an ethylene propylene rubber polymer and a solvent, and carrying out a grafting reaction to obtain a first solution of an ethylene propylene copolymer grafted by maleic anhydride, wherein in the step S1, the reaction temperature of the grafting reaction is 80-120 ℃, the reaction pressure is 0.1-0.2 MPa, and the reaction time is 1.0-4.0 h;
s2, mixing the first solution with an amine compound and carrying out amination reaction to obtain the viscosity index improver,
the step S2 includes: s21, heating the first solution to a first temperature, wherein the first temperature is 80-120 ℃; the reaction pressure of the amination reaction is 0.1-0.2 MPa, and the reaction time is 2-4 h.
2. The preparation method according to claim 1, wherein the weight of the maleic anhydride is 1.5-3.0% of the weight of the ethylene-propylene rubber polymer.
3. The preparation method according to claim 1 or 2, wherein the ethylene-propylene rubber polymer is an ethylene-propylene copolymer, wherein the corresponding content of ethylene is 48-70%.
4. The method according to claim 3, wherein the ethylene-propylene rubber polymer has a Mooney viscosity of 5 to 60.
5. The preparation method according to claim 3, wherein the weight of the ethylene-propylene rubber polymer is 4-20% of the total weight of the ethylene-propylene rubber polymer and the solvent.
6. The method according to claim 3, wherein the grafting initiator is a peroxide.
7. The method according to claim 6, wherein the grafting initiator comprises benzoyl peroxide and/or dicumyl peroxide.
8. The preparation method according to claim 6, wherein the weight of the grafting initiator is 1.0-2.0% of the weight of the ethylene propylene rubber polymer.
9. The production method according to claim 1, wherein the solvent includes any one or more of aromatic hydrocarbons, naphthenic hydrocarbons, and linear alkanes including any one or more of hexane, heptane, and octane.
10. The method according to claim 1 or 2, wherein in the step S1, the reaction temperature of the grafting reaction is 80-120 ℃, the reaction pressure is 0.1-0.2 MPa, and the reaction time is 1.0-4.0 h.
11. The method according to claim 4, wherein the first solution has a solid content of 5 to 40%.
12. The process according to claim 1, wherein the amine compound is H2N(CH2CH2NH)mH, wherein m is 1-6.
13. The method according to claim 12, wherein the amine compound is H2N(CH2CH2NH)mH, wherein m is 2 or 3.
14. The preparation method of claim 12, wherein the weight of the amine compound is 0.05-0.2% of the weight of the ethylene-propylene rubber polymer.
15. The production method according to claim 1 or 12, wherein the step S2 further includes:
s22, dropwise adding the amine compound into the heated first solution under stirring conditions, so that the first solution and the amine compound are mixed and subjected to amination reaction, and a second solution containing the viscosity index improver is obtained.
16. The method as claimed in claim 15, wherein the step S2 further includes a step of separating and purifying the viscosity index improver from the second solution after the step S22.
17. The method of claim 16, wherein the step of separating and purifying comprises: subjecting the second solution to falling film evaporation to obtain the viscosity index improver.
18. A viscosity index improver made according to the method of any one of claims 1 to 17, wherein the viscosity index improver is CH3-(CH2CH2)a-(CH2CH(CH3))b-CH(COOH)CH2(COHN(CH2CH2)mNH2) Wherein a is 500-1000, b is 500-1200, a: b is 0.9-1.5: 1.
19. the viscosity index improver according to claim 18, wherein a: b is 0.95 to 1.2; m is 3 or 4.
20. The viscosity index improver according to claim 18, wherein a is 700 to 900.
21. The viscosity index improver according to claim 18, wherein b is 700 to 1000.
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| CN101376860B (en) * | 2007-08-27 | 2011-02-09 | 中国石油化工股份有限公司 | Lubricating oil viscosity index improver, preparation thereof and lubricant oil |
| CN102653696A (en) * | 2011-03-03 | 2012-09-05 | 中国石油天然气股份有限公司 | Viscosity index improver and preparation method thereof |
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| DE3279533D1 (en) * | 1981-05-06 | 1989-04-20 | Exxon Research Engineering Co | Preparation of ethylene copolymer viscosity index improver - dispersant additive useful in oil compositions |
| US4735736A (en) * | 1985-07-08 | 1988-04-05 | Exxon Chemical Patents Inc. | Viscosity index improver-dispersant additive |
| CN1115351C (en) * | 1999-08-31 | 2003-07-23 | 中国石油化工集团公司 | Process for preparing graft copolymerization type non-ash disperser |
| CN1390234A (en) * | 1999-10-19 | 2003-01-08 | 埃克森化学专利公司 | Amine-containing graft polymers, a method for making same, and their use |
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| CN101117363A (en) * | 2006-08-04 | 2008-02-06 | 中国石油天然气股份有限公司大连润滑油研究开发中心 | Process for producing high-nitrogen dispersion type ethylene-propylene copolymer viscosity index improver |
| CN100549148C (en) * | 2007-05-19 | 2009-10-14 | 中国石油兰州石油化工公司 | A kind of ethylene-propylene copolymer viscosity index improver and preparation thereof and application |
| CN101376860B (en) * | 2007-08-27 | 2011-02-09 | 中国石油化工股份有限公司 | Lubricating oil viscosity index improver, preparation thereof and lubricant oil |
| CN102653696A (en) * | 2011-03-03 | 2012-09-05 | 中国石油天然气股份有限公司 | Viscosity index improver and preparation method thereof |
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| CN110452755A (en) | 2019-11-15 |
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