A method for evaluating phosphorus retention in gasoline engine oil high temperature performance testing

Abstract

The present invention discloses a method for evaluating the phosphorus retention of gasoline engine oil during a high-temperature performance test. The method comprises the following steps: 1. blending gasoline engine oil with a catalyst to obtain a gasoline engine oil containing the catalyst; 2. conducting a test to evaluate the phosphorus retention of the gasoline engine oil; 3. measuring 10 mL of the test oil and 10 mL of new gasoline engine oil without the catalyst from a reactor after 96 hours and 140 hours of testing, respectively, and determining the calcium and phosphorus contents in the test oils according to the method of GB / T17476; and 4. calculating the phosphorus retention rate based on the calcium and phosphorus contents in the test oils. The present invention provides a method for evaluating the phosphorus retention of gasoline engine oil during a high-temperature performance test, solving the problems of the long measurement cycle and high cost of the GB method for evaluating the performance of automotive engine oils in the prior art.

Description

Technical Field

[0001] The invention belongs to the technical field of high-temperature oxidation performance evaluation methods for gasoline engine oil, and relates to a method for evaluating phosphorus retention in a high-temperature performance test of gasoline engine oil. Background Art

[0002] With the development of engine oil specifications, starting with GF-5, gasoline engine oils are required to have good phosphorus retention and pass the ШGB method for evaluating automotive engine oil performance. However, the ШGB method is a bench test, which has the disadvantages of long testing cycles and high costs. Therefore, it is necessary to develop a simulation test method for evaluating the phosphorus retention of gasoline engine oils during high-temperature performance testing. Summary of the Invention

[0003] The purpose of the present invention is to provide a method for evaluating the phosphorus retention in the high-temperature performance test of gasoline engine oil, which solves the problem of long measurement cycle and huge cost in the prior art of using the ШGB method for evaluating the performance of automobile engine oil.

[0004] The technical solution adopted by the present invention is a method for evaluating the phosphorus retention in the high-temperature performance test of gasoline engine oil, which is specifically implemented according to the following steps:

[0005] Step 1: blending gasoline engine oil and a catalyst to obtain gasoline engine oil containing the catalyst;

[0006] Step 2: Conduct a test to evaluate the phosphorus retention performance of gasoline engine oil, specifically:

[0007] The gasoline engine oil containing catalyst prepared in step 1 was injected into the reactor of the engine oil high temperature oxidation ROBO test machine, and the speed of the stirrer connected to the reactor was controlled at rpm, the oil temperature of the gasoline engine oil containing the catalyst is controlled between 160 and 180°C, the flow rate of dry air introduced into the reactor is controlled between 10 and 15 L / h, and the test time is 40 to 160 h;

[0008] Step 3: After 96 hours and 140 hours of testing, 10 mL of the test oil and 10 mL of new gasoline engine oil without the addition of a catalyst were measured from the reactor, and the calcium and phosphorus contents of the test oils were determined according to the method of GB / T 17476.

[0009] Step 4: Calculate the phosphorus retention rate based on the obtained calcium and phosphorus contents in the test oil.

[0010] The present invention is also characterized in that

[0011] Step 3 also includes measuring the kinematic viscosity at 100 degrees of the new gasoline engine oil containing the catalyst and the gasoline engine oil containing the catalyst after the test according to the method of GB / T256.

[0012] In step 1, gasoline engine oil and catalyst are blended according to the following steps:

[0013] Step 1.1, mix 3 g to 7 g of ferrocene solution and 190 g to 210 g of gasoline engine oil;

[0014] Step 1.2, measure Add the iron acetylacetonate solution to the mixed solution of gasoline engine oil and ferrocene solution prepared in step 1.1;

[0015] In step 1.3, the gasoline engine oil mixed with the catalysts ferrocene and ferric acetylacetonate obtained in step 1.2 is placed on a constant temperature magnetic stirrer, a magnetic bar is placed in the stirrer, the stirrer is adjusted to a suitable speed, the temperature is adjusted to 40°C ± 5°C, and the stirrer is stirred for 50 min ± 10 min to obtain a gasoline engine oil containing the catalyst.

[0016] The appropriate speed in step 1.3 is based on the fact that the gasoline engine oil used for the test does not splash out.

[0017] Ferrocene solution was prepared as follows:

[0018] Ferrocene with a purity of not less than 98% and API No. 100 Group II base oil are mixed to obtain a ferrocene solution, and the mass ratio of ferrocene to API No. 100 Group II base oil is: 0.1±0.001g:99.9±0.1g.

[0019] Ferric acetylacetonate solution was prepared as follows:

[0020] Ferric acetylacetonate with a purity of 100 mg / kg was dissolved in chloroform and mixed to obtain a ferric acetylacetonate solution. The mass volume ratio of ferric acetylacetonate to chloroform was

[0021] After the test in step 3 is completed and the reactor temperature is cooled to 60°C ± 10°C, 10 mL of the gasoline engine oil containing the catalyst for the test is taken and the calcium and phosphorus contents in the oil are determined according to the method of GB / T17476.

[0022] The phosphorus retention rate in step 4 is calculated as follows:

[0023] Phosphorus retention rate = (calcium content in new gasoline engine oil / calcium content in test oil after oxidation) * (phosphorus content in test oil after oxidation / phosphorus content in new gasoline engine oil) * 100, where test oil after oxidation refers to oil samples taken 96 hours, 140 hours and after the end of the test.

[0024] During the operation test, record and adjust the air flow rate every 4 hours to ensure it is 10-15L / h.

[0025] The beneficial effects of the present invention are:

[0026] (1) The method of the present invention for evaluating phosphorus retention in a high-temperature performance test of gasoline engine oil has the advantages of low test cost (no consumables, and a small amount of test oil) and convenient operation (can be completed by one person). In contrast, the III GB bench test is more expensive (consumables are engine parts, and a large amount of test oil is used) and complex to operate (at least four people are required to complete). The method can be used as a basic simulation test method for the development of high-end gasoline engine oil formulation screening.

[0027] (2) The method of the present invention for evaluating phosphorus retention in a high-temperature performance test of gasoline engine oil can be used as a simulation test for the ШGB method bench test for evaluating the performance of automobile engine oil, and as a basis for screening oil formulations before bench testing. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 The present invention is a schematic structural diagram of an engine oil high-temperature oxidation ROBO tester in a method for evaluating phosphorus retention in a gasoline engine oil high-temperature performance test.

[0029] In the figure, 1. Heating jacket, 2. Air duct, 3. Reactor, 4. Air flow meter, 5. Agitator. DETAILED DESCRIPTION

[0030] The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.

[0031] The present invention provides a method for evaluating phosphorus retention in a gasoline engine oil high-temperature performance test, which is specifically implemented according to the following steps:

[0032] Step 1, blending gasoline engine oil and catalyst to obtain gasoline engine oil containing catalyst, is specifically carried out according to the following steps:

[0033] In step 1.1, 3 g to 7 g of ferrocene solution and 190 g to 210 g of gasoline engine oil are mixed.

[0034] Wherein, the ferrocene solution is prepared as follows:

[0035] Ferrocene with a purity of not less than 98% and API No. 100 Group II base oil are mixed to obtain a ferrocene solution, wherein the mass ratio of ferrocene to API No. 100 Group II base oil is: 0.1±0.001g:99.9±0.1g;

[0036] Step 1.2, measure The ferric acetylacetonate solution was added to the mixed solution of gasoline engine oil and ferrocene solution prepared in step 1.1.

[0037] Wherein, ferric acetylacetonate solution is prepared as follows:

[0038] Ferric acetylacetonate with a purity of 100 mg / kg was dissolved in chloroform and mixed to obtain a ferric acetylacetonate solution. The mass volume ratio of ferric acetylacetonate to chloroform was

[0039] As shown in Table 1, the preparation requirements of the catalyst are:

[0040]

[0041]

[0042] In step 1.3, the gasoline engine oil mixed in step 1.2 and containing the catalysts ferrocene and ferric acetylacetonate is placed on a constant temperature magnetic stirrer, a magnetic rod is placed in the stirrer, and the stirrer is adjusted to an appropriate speed so that the gasoline engine oil used for the test does not splash. The temperature is adjusted to 40°C ± 5°C and stirred for 50 min ± 10 min to obtain the catalyst-containing gasoline engine oil.

[0043] Step 2: Conduct a test to evaluate the phosphorus retention performance of gasoline engine oil, specifically:

[0044] The gasoline engine oil containing catalyst prepared in step 1 was injected into the reactor of the engine oil high temperature oxidation ROBO test machine, and the speed of the stirrer connected to the reactor was controlled at rpm, the oil temperature of the gasoline engine oil containing the catalyst is controlled between 160 and 180°C, the flow rate of dry air introduced into the reactor is controlled between 10 and 15 L / h, and the test time is 40 to 160 h;

[0045] Step 3. After 96 hours and 140 hours of the test, 10 mL of the test oil and 10 mL of new gasoline engine oil without catalyst were measured from the reactor, and the calcium and phosphorus contents in the test oils were determined according to the method of GB / T 17476. If necessary, the kinematic viscosity at 100 degrees of the new gasoline engine oil with catalyst and the gasoline engine oil containing catalyst after the test can also be determined according to the method of GB / T 256. After the test, when the reactor temperature has cooled to 60°C ± 10°C, 10 mL of the gasoline engine oil containing catalyst for the test was taken and the calcium and phosphorus contents in the oil were determined according to the method of GB / T 17476.

[0046] Step 4: Calculate the phosphorus retention rate based on the calcium and phosphorus contents in the test oil, as follows:

[0047] Phosphorus retention rate = (calcium content in new gasoline engine oil / calcium content in test oil after oxidation) * (phosphorus content in test oil after oxidation / phosphorus content in new gasoline engine oil) * 100, where test oil after oxidation refers to oil sampled at 96 hours, 140 hours and after the end of the test.

[0048] Example 1:

[0049] 5W-30GF-5 engine oils A, B, C, D, and E were selected as reference oils. The five oils were blended according to the blending method of the test sample of the present invention (3 g of ferrocene solution was dissolved in 190 g of gasoline engine oil and 10 mL of ferric acetylacetonate solution was added, wherein the blending ratio of the ferric acetylacetonate solution was: 1.50 g of ferric acetylacetonate was dissolved in 100 mL of chloroform.) and tested under the following test conditions: temperature 160°C, air flow rate 10 L / h, stirring speed 180 rpm, and test time 40 h. The tests were conducted separately, and the test results are shown in Table 2.

[0050] The results in Table 2 show that this experiment can effectively distinguish five oils with different phosphorus retention rates in high-temperature performance tests.

[0051] Table 2 Simulation test results of reference oils A and B

[0052]

[0053] Example 2:

[0054] 5W-30GF-5 engine oils A, B, C, D, and E were selected as reference oils. The five oils were blended according to the blending method of the test sample of the present invention (7 g of ferrocene solution was dissolved in 190 g of gasoline engine oil and 5 mL of ferric acetylacetonate solution was added, wherein the blending ratio of the ferric acetylacetonate solution was: 1.0 g of ferric acetylacetonate was dissolved in 50 mL of chloroform.) and then tested. The test conditions were: temperature 170°C, air flow rate 15 L / h, stirring speed 180 rpm, and test time 96 h. The tests were conducted separately, and the test results are shown in Table 3.

[0055] The results in Table 3 show that this experiment can well distinguish five oils with different phosphorus retention rates in high-temperature performance tests.

[0056] Table 3 Simulation test results of reference oils A and B

[0057]

[0058] Example 3:

[0059] 5W-30GF-5 engine oils A, B, C, D, and E were selected as reference oils. The five oils were blended according to the blending method of the test sample of the present invention (5 g of ferrocene solution was dissolved in 210 g of gasoline engine oil and 20 mL of ferric acetylacetonate solution was added, wherein the blending ratio of the ferric acetylacetonate solution was: 2.0 g of ferric acetylacetonate was dissolved in 50 mL of chloroform.) and tested. The test conditions were: temperature 170°C, air flow rate 15 L / h, stirring speed 230 rpm, and test time 140 h. The tests were conducted separately, and the test results are shown in Table 4.

[0060] The results in Table 4 show that this experiment can well distinguish five oils with different phosphorus retention rates in high-temperature performance tests.

[0061] Table 4 Simulation test results of reference oils A and B

[0062]

[0063] Example 4:

[0064] 5W-30GF-5 engine oils A, B, C, D, and E were selected as reference oils. The five oils were blended according to the blending method of the test sample of the present invention (7 g of ferrocene solution was dissolved in 210 g of gasoline engine oil and 20 mL of ferric acetylacetonate solution was added, wherein the blending ratio of the ferric acetylacetonate solution was: 1.66 g of ferric acetylacetonate was dissolved in 100 mL of chloroform.) and tested under the following test conditions: temperature 180°C, air flow rate 15 L / h, stirring speed 200 rpm, and test time 160 h. The tests were conducted separately, and the test results are shown in Table 5.

[0065] The results in Table 5 show that this experiment can well distinguish five oils with different phosphorus retention rates in high-temperature performance tests.

[0066] Table 5 Simulation test results of reference oils A and B

[0067]

[0068]

Claims

1. A method for evaluating the phosphorus retention in a gasoline engine oil high temperature performance test, characterized in that: The specific implementation steps are as follows: Step 1: blending gasoline engine oil and catalyst to obtain gasoline engine oil containing catalyst, specifically: In step 1.1, 3 g to 7 g of ferrocene solution and 190 g to 210 g of gasoline engine oil are mixed; wherein the ferrocene solution is prepared as follows: Ferrocene with a purity of not less than 98% and API No. 100 Group II base oil are mixed to obtain a ferrocene solution, wherein the mass ratio of the ferrocene to the API No. 100 Group II base oil is: 0.1±0.001g:99.9±0.1g; Step 1.2: Measure 5 mL to 20 mL of ferric acetylacetonate solution and add it to the mixed solution of gasoline engine oil and ferrocene solution prepared in step 1.1; wherein the ferric acetylacetonate solution is prepared as follows: Ferric acetylacetonate with a purity of 100 mg / kg is dissolved in chloroform and mixed to obtain a ferric acetylacetonate solution, wherein the mass volume ratio of the ferric acetylacetonate to chloroform is (1.0∽2.0) g: (50∽150) mL; In step 1.3, the gasoline engine oil mixed with the catalysts ferrocene and ferric acetylacetonate obtained in step 1.2 is placed on a constant temperature magnetic stirrer, a magnetic bar is placed in the stirrer, the stirrer is adjusted to an appropriate speed, the temperature is adjusted to 40°C ± 5°C, and the mixture is stirred for 50 min ± 10 min to obtain the catalyst-containing gasoline engine oil; Step 2: Conduct a test to evaluate the phosphorus retention performance of gasoline engine oil, specifically: The catalyst-containing gasoline engine oil prepared in step 1 is injected into the reactor of the engine oil high-temperature oxidation ROBO tester, the speed of the stirrer connected to the reactor is controlled at 180-230 rpm, the oil temperature of the catalyst-containing gasoline engine oil is controlled between 160-180°C, the flow rate of dry air introduced into the reactor is controlled between 10-15 L / h, and the test time is 96-160 hours; Step 3: After 96 hours and 140 hours of testing, 10 mL of the test oil and 10 mL of new gasoline engine oil without the addition of a catalyst were measured from the reactor, and the calcium and phosphorus contents of the test oils were determined according to the method of GB / T 17476. Step 4: Calculate the phosphorus retention rate based on the obtained calcium and phosphorus contents in the test oil. The phosphorus retention rate is calculated as follows: Phosphorus retention rate = (calcium content in new gasoline engine oil / calcium content in test oil after oxidation) * (phosphorus content in test oil after oxidation / phosphorus content in new gasoline engine oil) * 100, where test oil after oxidation refers to oil samples taken after 96 hours, 140 hours and the end of the test.

2. The method for evaluating phosphorus retention in a gasoline engine oil high temperature performance test according to claim 1, characterized in that: The step 3 further includes measuring the kinematic viscosity at 100 degrees of the new gasoline engine oil containing the catalyst and the gasoline engine oil containing the catalyst after the test according to the method of GB / T265.

3. The method for evaluating phosphorus retention in a gasoline engine oil high temperature performance test according to claim 1, characterized in that: The appropriate rotation speed in step 1.3 is determined so that the gasoline engine oil used in the test does not splash out.

4. A method for evaluating phosphorus retention in a gasoline engine oil high temperature performance test according to claim 1 or 2, characterized in that: After the test in step 3 is completed and the reactor temperature is cooled to 60° C.±10° C., 10 ml of gasoline engine oil containing the catalyst for the test is taken and the contents of calcium and phosphorus in the oil are determined according to the method of GB / T17476.

5. A method for evaluating phosphorus retention in a gasoline engine oil high temperature performance test according to claim 1 or 2, characterized in that: During the test in step 2, record and adjust the air flow rate every 4 hours to ensure it is 10~15L / h.

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