CN114276857A - OCP viscosity index improver and preparation method thereof - Google Patents
OCP viscosity index improver and preparation method thereof Download PDFInfo
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- CN114276857A CN114276857A CN202111651435.9A CN202111651435A CN114276857A CN 114276857 A CN114276857 A CN 114276857A CN 202111651435 A CN202111651435 A CN 202111651435A CN 114276857 A CN114276857 A CN 114276857A
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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, fully re-polymerizes the OCP polymer into the modified OCP viscosity index improver which has good shear stability and good thickening capability through high-temperature cracking and catalysis of oxygen, and effectively improves the planning capability and the shear stability of the OCP viscosity index improver through cracking and recombination.
Description
Technical Field
The invention relates to the technical field of lubricating oil additives, in particular to an OCP viscosity index improver and a preparation method thereof.
Background
Viscosity Index Improvers (VII) are generally oil-soluble, polymeric compounds that are generally rubbery or solid at room temperature. Viscosity index improvers are based on having different morphologies at different temperatures and having different effects on viscosity to increase oil viscosity and improve viscosity temperature performance. The viscosity index improver is added into the lubricating oil, so that the multi-grade oil with good low-temperature starting performance and proper viscosity at high temperature can be obtained, 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. Compared with single-stage oil with the same viscosity, the multi-stage oil added with the viscosity index improver has higher viscosity index and smooth viscosity-temperature curve, can simultaneously meet the requirement of multi-viscosity grade, and the consumption of lubricating oil can be reduced by 27 percent while the consumption of fuel oil can be reduced by 3 to 5 percent.
The most used adhesives in recent years are Polymethyl Methacrylate (PMA), Polyisobutylene (PIB), ethylene-propylene copolymer (OCP), hydrogenated styrene diene copolymer (HSD), and the like. PIB is less effective at low temperatures, and PMA is less effective at internal combustion engine oils due to its higher cost. The OCP has the characteristics of easy availability of raw materials, low price, good tackifying capability and shear stability, good high-temperature performance, good field use performance and the like, is a variety which is used more in the world at present, and has very wide market prospect. However, the existing OCP is not very good in thickening capability and shear stability, the SSI index is good, the price is high due to the manufacturing process, and the thickening capability and the shear stability are difficult to be considered simultaneously. Therefore, in order to meet the current market demand and the current production situation, the production process of the OCP type viscosity index improver needs to be reasonably optimized and adjusted.
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 purpose, the invention provides a preparation method of an OCP viscosity index improver, which comprises the following steps:
step one, heating base oil: pumping a certain amount of 150N base oil into the 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 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 hours;
step four, 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 volume of the OCP gel strip in the second step is 1.5X 10cm3。
Further preferably, the speed of adding the OCP rubber strip in the second step is 4 cm/s.
More preferably, the air flow introduced in the third step is 0.3-2.0m3/100kg·h。
Further preferably, the reaction temperature in the third step is 147-163 ℃, and the reaction time is 3 hours.
The invention also provides an OCP viscosity index improver.
Further preferably, the OCP viscosity index improver has a shear stability index at 100 ℃ of less than 20.
Further preferably, the thickening power of the OCP viscosity index improver is not less than 6.5mm2/s。
Further preferably, the kinematic viscosity of the OCP viscosity index improver at 100 ℃ is not less than 1900mm2/s。
Further preferably, the OCP viscosity index improver comprises the following components in a mass ratio of 7-9: 1-3 of base oil and OCP.
The invention has the beneficial effects that: 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 re-polymerizes the OCP polymer into the modified OCP viscosity index improver with good shear stability and good thickening capability through pyrolysis and catalysis of oxygen at high temperature, and effectively improves the planning capability and the shear stability of the OCP viscosity index improver through pyrolysis and recombination. The modified OCP viscosity index improver can ensure that the high-temperature high-shear of engine lubricating oil is superior to that of unmodified OCP under the same condition, can effectively maintain the thickness of a lubricating oil and an oil film in the using 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 the tendency of the viscosifying ability of the OCP viscosity index improver over time;
FIG. 3 is a graph of the shear stability index of the OCP viscosity index improver as a function of time.
Detailed Description
The embodiments described below are only a part of the embodiments of the present invention, and not all of them. 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.
The invention provides an OCP viscosity index improver, and a preparation method thereof 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 ℃, and 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 feeding is finished, the temperature is continuously increased, the reaction temperature is kept at 140-170 ℃, an air inlet valve is opened, air is introduced into the reaction kettle, and the air flow is 0.3-2.0m3Reaction for 3-6.5 h at 147-163 ℃ under 100 kg/h;
step four, 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 content of the OCP adhesive tape is less than or equal to 1.2 percent, the test method is GB/T6737 (oven method), the ash content is less than or equal to 0.1 percent, and the test method is GB/T4498 (method A); the ethylene content is 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 8-13, and the test method is GB/T1232.
The base oil is HVIH 5.
Example 1
The embodiment provides an OCP viscosity index improver, which comprises the following components in a mass ratio of 8: 2 and OCP, prepared as follows:
step one, heating base oil: pumping 150N base oil with the formula amount into the reaction kettle, stirring and heating to 90 ℃, and keeping the temperature stable;
step two, sol: adding OCP rubber strips with formula amount of 1.5 × 1.5 × 10cm in volume into the reaction kettle at constant speed3Adding OCP adhesive tape at a speed of 4cm/s, keeping the temperature at 149 +/-2 ℃, and dissolving for 3 h;
step three, oxidative degradation: after the feeding is finished, the temperature is continuously increased, the reaction temperature is kept at 145 +/-2 ℃, an air inlet valve is opened, air is introduced into the reaction kettle, and the air flow is 0.3m3Reaction for 3 hours at the temperature of 149 +/-2 ℃ under the conditions of 100kg per hour;
step four, 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 a mass ratio of 7.5: 2.5 base oil and OCP, prepared 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 OCP rubber strips with formula amount of 1.5 × 1.5 × 10cm in volume into the reaction kettle at constant speed3Adding OCP adhesive tape at a speed of 4cm/s, keeping the temperature at 152 +/-2 ℃, and dissolving the sol for 3.5 h;
step three, oxidative degradation: after the feeding is finished, the temperature is continuously increased, the reaction temperature is kept at 150 +/-2 ℃, an air inlet valve is opened, air is introduced into the reaction kettle, and the air flow is 0.7m3Reaction for 3.5h at the temperature of 152 +/-2 ℃ under the condition of 100kg per hour;
step four, 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 a mass ratio of 7: 3 and OCP, which is prepared by the following process:
step one, heating base oil: pumping 150N base oil with the formula amount into the reaction kettle, stirring and heating to 110 ℃, and keeping the temperature stable;
step two, sol: adding OCP rubber strips with formula amount of 1.5 × 1.5 × 10cm in volume into the reaction kettle at constant speed3Adding OCP adhesive tape at a speed of 4cm/s, keeping the temperature at 155 +/-2 ℃, and dissolving for 4.5 h;
step three, oxidative degradation: after the feeding is finished, the temperature is continuously increased, the reaction temperature is kept at 155 +/-2 ℃, an air inlet valve is opened, air is introduced into the reaction kettle, and the air flow is 1.1m3Reaction for 4.5h at the temperature of 155 +/-2 ℃ under the condition of 100kg per h;
step four, 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 a mass ratio of 8.5: 1.5 base oil and OCP prepared as follows:
step one, heating base oil: pumping 150N base oil with the formula amount into the reaction kettle, stirring and heating to 120 ℃, and keeping the temperature stable;
step two, sol: adding OCP rubber strips with formula amount of 1.5 × 1.5 × 10cm in volume into the reaction kettle at constant speed3Adding OCP adhesive tape at 4cm/s, maintaining the temperature at 158 + -2 deg.C, and dissolving for 5.5 h;
step three, oxidative degradation: after the feeding is finished, the temperature is continuously increased, the reaction temperature is kept at 158 +/-2 ℃, an air inlet valve is opened, air is introduced into the reaction kettle, and the air flow is 1.5m3Reaction for 5.5h at the temperature of 158 +/-2 ℃ under the condition of 100kg per h;
step four, 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 a mass ratio of 9: 1 and OCP prepared as follows:
step one, heating base oil: pumping 150N base oil with the formula amount into the reaction kettle, stirring and heating to 130 ℃, and keeping the temperature stable;
step two, sol: adding OCP rubber strips with formula amount of 1.5 × 1.5 × 10cm in volume into the reaction kettle at constant speed3Adding OCP adhesive tape at a speed of 4cm/s, keeping the temperature at 161 +/-2 ℃, and dissolving for 6.5 h;
step three, oxidative degradation: after the feeding is finished, the temperature is continuously increased, the reaction temperature is kept at 161 +/-2 ℃, an air inlet valve is opened, air is introduced into the reaction kettle, and the air flow is 2m3Reaction for 6.5h at the temperature of 161 +/-2 ℃ under the condition of 100kg per hour;
step four, 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 prepared by a method different from that of example 1 in that the volume of the OCP strip in step 2 was 2X 10cm3。
Comparative example 2
This comparative example provides an OCP viscosity index improver, which was prepared in a manner different from that of example 1 in that the OCP rubber strip was entirely charged at one time in step 2.
The parameters of the OCP viscosity index improver obtained in examples 1-5 are shown in Table 1 below.
TABLE 1 parameter index of OCP viscosity index improver obtained in examples 1 to 5
OCP adhesive tape volume is too big in the comparative example 1, leads to the hot melt adhesive time extension, and OCP adhesive tape once only drops into totally in the comparative example 2, leads to the adhesive tape to bond in the base oil.
Testing the performance rule of the OCP viscosity index improver: test groups 1-5 are set, and OCP viscosity index improvers 1-5 are prepared, wherein the preparation method is the same as that in example 3 except that the oxidative degradation reaction time is 3, 4, 5, 6 and 6.5 hours respectively. The parameter indexes of 1-5 of the OCP viscosity index improver prepared by the test groups 1-5 are shown in the following table 2.
Table 2 parameter indexes of OCP viscosity index improvers obtained from test groups 1-5
As shown in figures 1-3, the OCP viscosity index improver has a tendency that the kinematic viscosity (100 ℃) is increased and then decreased within 3-6.5 h of oxidative degradation reaction time, and the thickening capacity is 6.5-7mm2The shear stability index is increased after being smoothed due to the fluctuation between/s, but the shear stability index meets the index requirement of national energy 615, and the shear stability index has better operability and test reproducibility. The optimum reaction under the process conditions of the present invention recommends an oxidative degradation reaction for 3h under the process conditions of example 3, considering the practical use requirements of maximizing thickening power, minimizing SSI, and production efficiency.
The OCP viscosity index improver with SSI less than 20 can be obtained by cracking and recombining OCP with SSI of 24, has good shear stability and good thickening capability, and has simple preparation method and low production cost.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention.
Claims (10)
1. A preparation method of an OCP viscosity index improver is characterized by comprising the following steps:
step one, heating base oil: pumping a certain amount of 150N base oil into the 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 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 hours;
step four, 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.
2. The method of claim 1, wherein the volume of the OCP gel strip in step two is 1.5 x 10cm3。
3. The method of claim 2, wherein in step two the speed of addition of the OCP gel strip is 4 cm/s.
4. The method of claim 1, wherein the flow rate of air introduced in step three is 0.3 to 2.0m3/100kg·h。
5. The preparation method of the OCP viscosity index improver according to claim 1, wherein the reaction temperature in the third step is 147-163 ℃ and the reaction time is 3 h.
6. An OCP viscosity index improver prepared by the preparation method of the OCP viscosity index improver as set forth in any one of claims 1 to 5.
7. The OCP viscosity index improver of claim 6, wherein the OCP viscosity index improver has a shear stability index at 100 ℃ of less than 20.
8. The OCP viscosity index improver of claim 6, wherein the OCP viscosity index improver has a viscosifying capacity of not less than 6.5mm2/s。
9. The OCP viscosity index improver of claim 6, wherein the kinematic viscosity of the OCP viscosity index improver at 100 ℃ is not less than 1900mm2/s。
10. The OCP viscosity index improver of claim 6, wherein the OCP viscosity index improver comprises a blend of, by mass, 7-9: 1-3 of base oil and OCP.
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| US3923919A (en) * | 1972-07-07 | 1975-12-02 | Sun Ventures Inc | Ethylene-propylene copolymer oil |
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