CN114276857B - OCP viscosity index improver - Google Patents
OCP viscosity index improver Download PDFInfo
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- CN114276857B CN114276857B CN202111651435.9A CN202111651435A CN114276857B CN 114276857 B CN114276857 B CN 114276857B CN 202111651435 A CN202111651435 A CN 202111651435A CN 114276857 B CN114276857 B CN 114276857B
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Abstract
The invention provides a preparation method of an OCP viscosity index improver, which takes thermal degradation, oxidative degradation and thermal reaction recombination as main process routes, optimizes the preparation process and conditions of the OCP viscosity index improver, dissolves an OCP polymer in oil at a certain temperature, and fully and repolymerizes the OCP polymer into a modified OCP viscosity index improver with good shear stability and good thickening capacity through high-temperature catalysis with oxygen, and effectively improves the planning capacity and the shear stability of the OCP viscosity index improver through pyrolysis and recombination.
Description
Technical Field
The invention relates to the technical field of lubricating oil additives, in particular to an OCP viscosity index improver.
Background
The viscosity index improver (viscosity index improver, VII) is typically an oil-soluble polymer compound, which is typically rubbery or solid at room temperature. Viscosity index improvers are based on having different morphologies at different temperatures and have different effects on viscosity to increase oil viscosity and improve visco-thermal properties. The viscosity index improver is added into the lubricating oil to obtain multistage oil with good low-temperature starting performance and proper viscosity at high temperature, so that the performance of the lubricating oil is improved, the grade of the lubricating oil is improved, the service life of the lubricating oil is prolonged, and the lubricating oil can be used in four seasons. The multi-stage oil added with the viscosity index improver has higher viscosity index and smooth viscosity-temperature curve compared with single-stage oil with the same viscosity, can simultaneously meet the requirement of multiple viscosity grades, and the lubricating oil consumption is reported to be reduced by 27 percent, and the fuel oil consumption is reduced by 3 to 5 percent.
The most used adhesion agents in recent years are Polymethyl Methacrylate (PMA), polyisobutylene (PIB), ethylene propylene copolymer (OCP), hydrogenated styrene diene copolymer (HSD), and the like. PIB is poor in low-temperature performance, and PMA is low in cost and is used for internal combustion engine oil. OCP is a variety which is widely used in the world at present because the OCP has the characteristics of easily available raw materials, low price, better tackifying capability and shearing stability, good high-temperature performance, good field use performance and the like. However, the existing OCP is not good in thickening ability and shear stability, and SSI indexes are good, so that the price is high due to the manufacturing process, and the thickening ability and the shear stability are difficult to be simultaneously considered. Therefore, in order to meet the current market demand and current state of production, it is necessary to reasonably optimize and adjust the production process of the OCP-type viscosity index improver.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an OCP viscosity index improver with excellent performance and a preparation method of the OCP viscosity index improver.
In order to achieve the above object, the present invention provides a method for preparing an OCP viscosity index improver, comprising the steps of:
step one, heating base oil: pumping a certain amount of 150N base oil into a reaction kettle, stirring and heating to 90-130 ℃, and keeping the temperature stable;
step two, sol: adding an OCP adhesive tape into the reaction kettle at a constant speed;
step three, oxidative degradation: after the material feeding is finished, continuously heating, keeping the reaction temperature at 140-170 ℃, opening an air inlet valve, introducing air into the reaction kettle, and reacting for 3-6.5 h;
fourth, discharging: after the reaction is finished, the air inlet valve is closed, the jacket is filled with water and cooled to 80+/-5 ℃, and the product is discharged and barreled.
Further preferably, the OCP strip in step two has a volume of 1.5X1.5X10 cm 3 。
It is further preferred that the OCP tape is added in step two at a rate of 4cm/s.
Further preferably, the air flow rate in the third step is 0.3-2.0m 3 /100kg·h。
It is further preferable that the reaction temperature in the third step is 147 to 163 ℃ and the reaction time is 3 hours.
The invention also provides an OCP viscosity index improver.
Further preferred, the OCP viscosity index improver has a shear stability index at 100 ℃ of less than 20.
Further preferably, the OCP viscosity index improver has a thickening power of not less than 6.5mm 2 /s。
Further preferably, the OCP viscosity index improver has a kinematic viscosity at 100 ℃ of not less than 1900mm 2 /s。
Further preferably, the OCP viscosity index improver comprises the following components in mass ratio of 7-9: 1-3, and OCP.
The beneficial effects of the invention are as follows: the preparation method of the OCP viscosity index improver provided by the invention takes thermal degradation, oxidative degradation and thermal reaction recombination as main process routes, optimizes the preparation process and conditions of the OCP viscosity index improver, dissolves an OCP polymer in oil at a certain temperature, fully and repolymerizes the OCP polymer into a modified OCP viscosity index improver with good shear stability and good thickening capacity through high-temperature pyrolysis and catalysis of oxygen, and effectively improves the planning capacity and the shear stability of the OCP viscosity index improver through pyrolysis and recombination. Under the same condition, the modified OCP viscosity index improver can ensure that the high-temperature high-shear of the engine lubricating oil is superior to that of the unmodified OCP, can effectively maintain the lubricating oil and the oil film thickness in the use process, and improves the oil pressure of the engine oil.
The preparation method of the OCP viscosity index improver provided by the invention has the advantages of stable and reliable process, good repeatability, simple method and low production cost.
Drawings
FIG. 1 is a graph of the kinematic viscosity of the OCP viscosity index improver as a function of time;
FIG. 2 is a graph of thickening power versus time for the OCP viscosity index improver;
FIG. 3 is a graph showing the trend of the shear stability index of the OCP viscosity index improver over time.
Detailed Description
The embodiments described below are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides an OCP viscosity index improver, which comprises the following steps:
step one, heating base oil: pumping 70-90 parts by mass of 150N base oil into a reaction kettle, stirring and heating to 90-130 ℃ while keeping the temperature stable;
step two, sol: adding 10-30 parts by mass of OCP adhesive tape into the reaction kettle at a constant speed;
step three, oxidative degradation: after the material feeding is finished, continuously heating, keeping the reaction temperature at 140-170 ℃, opening an air inlet valve, and introducing air into the reaction kettle, wherein the air flow is 0.3-2.0m 3 100 kg.h, reacting for 3-6.5 h, wherein the reaction temperature is 147-163 ℃;
fourth, discharging: after the reaction is finished, the air inlet valve is closed, the jacket is filled with water and cooled to 80+/-5 ℃, and the product is discharged and barreled.
The volatile component of the OCP adhesive tape is less than or equal to 1.2%, the test method is GB/T6737 (oven method), the ash content is less than or equal to 0.1%, and the test method is GB/T4498 (method A); ethylene content of 48.1-53.1%, and the test method is Q/SY JH F104001; the vanadium content is less than or equal to 10mg/kg, and the test method is Q/SY JH F104004; the Mooney viscosity (100 ℃) is 8 to 13, and the test method is GB/T1232.
The base oil is HVIH5.
Example 1
The embodiment provides an OCP viscosity index improver, which comprises the following components in percentage by mass: 2 and OCP, the preparation method thereof is as follows:
step one, heating base oil: pumping 150N base oil with the formula amount into a reaction kettle, stirring and heating to 90 ℃, and keeping the temperature stable;
step two, sol: adding the formula amount of OCP adhesive tape into a reaction kettle at constant speed, wherein the volume of the OCP adhesive tape is 1.5X1.5X10 cm 3 The adding speed of the OCP adhesive tape is 4cm/s, the temperature is kept at 149+/-2 ℃, and the sol is carried out for 3 hours;
step three, oxidative degradation: after the material feeding is finished, continuously heating, keeping the reaction temperature at 145+/-2 ℃, opening an air inlet valve, and introducing air into the reaction kettle, wherein the air flow is 0.3m 3 100 kg.h, reacting for 3h at 149+/-2 ℃;
fourth, discharging: after the reaction is finished, the air inlet valve is closed, the jacket is filled with water and cooled to 80+/-5 ℃, and the product is discharged and barreled.
Example 2
The embodiment provides an OCP viscosity index improver, which comprises the following components in percentage by mass of 7.5:2.5 and OCP, the preparation method is as follows:
step one, heating base oil: pumping 150N base oil with the formula amount into a reaction kettle, stirring and heating to 100 ℃, and keeping the temperature stable;
step two, sol: adding the formula amount of OCP adhesive tape into a reaction kettle at constant speed, wherein the volume of the OCP adhesive tape is 1.5X1.5X10 cm 3 The adding speed of the OCP adhesive tape is 4cm/s, the temperature is kept at 152+/-2 ℃, and the sol is dissolved for 3.5 hours;
step three, oxidative degradation: after the material feeding is finished, continuously heating, keeping the reaction temperature at 150+/-2 ℃, opening an air inlet valve, and introducing air into the reaction kettle, wherein the air flow is 0.7m 3 100 kg.h, reacting for 3.5h at 152+/-2 ℃;
fourth, discharging: after the reaction is finished, the air inlet valve is closed, the jacket is filled with water and cooled to 80+/-5 ℃, and the product is discharged and barreled.
Example 3
The embodiment provides an OCP viscosity index improver, which comprises the following components in percentage by mass: 3 and OCP, the preparation method thereof is as follows:
step one, heating base oil: pumping 150N base oil with the formula amount into a reaction kettle, stirring and heating to 110 ℃, and keeping the temperature stable;
step two, sol: adding the formula amount of OCP adhesive tape into a reaction kettle at constant speed, wherein the volume of the OCP adhesive tape is 1.5X1.5X10 cm 3 The adding speed of the OCP adhesive tape is 4cm/s, the temperature is kept at 155+/-2 ℃, and the sol is dissolved for 4.5 hours;
step three, oxidative degradation: after the material feeding is finished, continuously heating, keeping the reaction temperature at 155+/-2 ℃, opening an air inlet valve, and introducing air into the reaction kettle, wherein the air flow is 1.1m 3 100 kg.h, and reacting for 4.5h at 155+/-2 ℃;
fourth, discharging: after the reaction is finished, the air inlet valve is closed, the jacket is filled with water and cooled to 80+/-5 ℃, and the product is discharged and barreled.
Example 4
The embodiment provides an OCP viscosity index improver, which comprises the following components in percentage by mass of 8.5:1.5 and OCP, the preparation method is as follows:
step one, heating base oil: pumping 150N base oil with the formula amount into a reaction kettle, stirring and heating to 120 ℃, and keeping the temperature stable;
step two, sol: adding the formula amount of OCP adhesive tape into a reaction kettle at constant speed, wherein the volume of the OCP adhesive tape is 1.5X1.5X10 cm 3 The adding speed of the OCP adhesive tape is 4cm/s, the temperature is kept at 158+/-2 ℃, and the sol is dissolved for 5.5 hours;
step three, oxidative degradation: after the material feeding is finished, continuously heating, keeping the reaction temperature at 158+/-2 ℃, opening an air inlet valve, and introducing air into the reaction kettle, wherein the air flow is 1.5m 3 100 kg.h, reacting for 5.5h at 158+/-2 ℃;
fourth, discharging: after the reaction is finished, the air inlet valve is closed, the jacket is filled with water and cooled to 80+/-5 ℃, and the product is discharged and barreled.
Example 5
The embodiment provides an OCP viscosity index improver, which comprises the following components in percentage by mass: 1 and OCP, the preparation method thereof is as follows:
step one, heating base oil: pumping 150N base oil with the formula amount into a reaction kettle, stirring and heating to 130 ℃, and keeping the temperature stable;
step two, sol: adding the formula amount of OCP adhesive tape into a reaction kettle at constant speed, wherein the volume of the OCP adhesive tape is 1.5X1.5X10 cm 3 The adding speed of the OCP adhesive tape is 4cm/s, the temperature is kept at 161+/-2 ℃, and the sol is dissolved for 6.5 hours;
step three, oxidative degradation: after the material feeding is finished, continuously heating, keeping the reaction temperature at 161+/-2 ℃, opening an air inlet valve, and introducing air into the reaction kettle, wherein the air flow is 2m 3 100 kg.h, reacting for 6.5h at 161+/-2 ℃;
fourth, discharging: after the reaction is finished, the air inlet valve is closed, the jacket is filled with water and cooled to 80+/-5 ℃, and the product is discharged and barreled.
Comparative example 1
This comparative example provides an OCP viscosity index improver which is prepared by a method different from example 1 in that the OCP gel strip volume in step 2 is 2X 10cm 3 。
Comparative example 2
This comparative example provides an OCP viscosity index improver which is prepared by a process different from that of example 1 in that the OCP tape is fed in one portion at a time.
The parameter indexes of the OCP viscosity index improvers obtained in examples 1 to 5 are shown in Table 1 below.
TABLE 1 parameter index of OCP viscosity index improver obtained in examples 1 to 5
The OCP tape in comparative example 1 was excessively large in volume, resulting in prolonged hot melt adhesive time, and the OCP tape in comparative example 2 was completely put in at one time, resulting in adhesive bonding of the tape in the base oil.
The performance laws of the OCP viscosity index improver were tested: test groups 1 to 5 were used to prepare OCP viscosity index improvers 1 to 5, and the preparation method was the same as in example 3 except that the oxidative degradation reaction time was 3, 4, 5, 6, and 6.5 hours, respectively. The OCP viscosity index improvers 1 to 5 prepared in test groups 1 to 5 were indexed as shown in Table 2 below.
Table 2 parameter index of OCP viscosity index improver obtained in test groups 1 to 5
As shown in figures 1-3, the OCP viscosity index improver has the tendency that the kinematic viscosity (100 ℃) is firstly increased and then decreased within the oxidative degradation reaction time of 3-6.5 hours, and the thickening capacity is 6.5-7mm 2 The shear stability index is smooth and then increases, but meets the national energy 615 index requirement, and has better operability and better test reproducibility. In view of the practical use requirements of maximizing thickening power, minimizing SSI, and production efficiency, the optimal reaction under the process conditions of the present invention recommends the oxidative degradation reaction for 3 hours under the process conditions of example 3.
According to the invention, the OCP with SSI of 24 can be obtained into the OCP viscosity index improver with SSI of less than 20 through cracking and recombination, and the OCP viscosity index improver has good shear stability, good thickening capacity, simple preparation method and low production cost.
The foregoing disclosure is only illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the scope of the invention, which is defined by the appended claims.
Claims (2)
1. An OCP viscosity index improver comprising a mass ratio of 7:3 and OCP, the method of making comprising the steps of:
step one, heating base oil: pumping 150N base oil with the formula amount into a reaction kettle, stirring and heating to 110 ℃, and keeping the temperature stable;
step two, sol: adding an OCP adhesive tape into a reaction kettle at a constant speed, wherein the volume of the OCP adhesive tape is 1.5X1.5X10 cm 3 The adding speed of the OCP adhesive tape is 4cm/s, the temperature is kept at 155+/-2 ℃, and the sol is dissolved for 4.5 hours;
step three, oxidative degradation: after the material feeding is finished, continuously heating, keeping the reaction temperature at 155+/-2 ℃, opening an air inlet valve, and introducing air into the reaction kettle, wherein the air flow is 1.1m 3 100 kg.h, reacting for 3h;
fourth, discharging: after the reaction is finished, closing an air inlet valve, cooling the jacket to 80+/-5 ℃ by introducing water, and discharging products and barreling; the OCP viscosity index improver has a shear stability index at 100deg.C of less than 20, and a thickening power of not less than 6.5mm 2 /s。
2. The OCP viscosity index improver of claim 1 having a kinematic viscosity at 100 ℃ of not less than 1900mm 2 /s。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3923919A (en) * | 1972-07-07 | 1975-12-02 | Sun Ventures Inc | Ethylene-propylene copolymer oil |
| US6362286B1 (en) * | 1999-12-13 | 2002-03-26 | Exxon Chemical Patents Inc. | Molecular weight reduction of olefin copolymers using low-sulfur oils |
| CN102776054A (en) * | 2011-05-13 | 2012-11-14 | 中国石油天然气股份有限公司 | Preparation method of viscosity index improver with high shear resistance |
| CN105132081A (en) * | 2015-08-19 | 2015-12-09 | 西京学院 | Preparation method for ethylene-propylene copolymer viscosity index improver |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030013623A1 (en) * | 2001-05-01 | 2003-01-16 | Kwok-Leung Tse | Olefin copolymer viscocity index improvers |
| CN101392208B (en) * | 2008-10-13 | 2011-07-06 | 深圳海润德石化技术有限公司 | Method for producing lubricating oil viscosity index improver |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3923919A (en) * | 1972-07-07 | 1975-12-02 | Sun Ventures Inc | Ethylene-propylene copolymer oil |
| US6362286B1 (en) * | 1999-12-13 | 2002-03-26 | Exxon Chemical Patents Inc. | Molecular weight reduction of olefin copolymers using low-sulfur oils |
| CN102776054A (en) * | 2011-05-13 | 2012-11-14 | 中国石油天然气股份有限公司 | Preparation method of viscosity index improver with high shear resistance |
| CN105132081A (en) * | 2015-08-19 | 2015-12-09 | 西京学院 | Preparation method for ethylene-propylene copolymer viscosity index improver |
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