Biodiesel for use in the cecl-109 method and methods of making
By preparing biodiesel with specific components and purity, the reproducibility problem of the standard biodiesel test in the CECL-109 method was solved, achieving antioxidant performance that meets the standards and is suitable for screening high-grade engine oil formulations.
Patent Information
- Application Number
- CN202210754399.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-06-29
- Publication Date
- 2026-01-23
- Estimated Expiration
- 2042-06-29
AI Technical Summary
The existing technology lacks standard test requirements for biodiesel that can meet the CECL-109 method, and biodiesel is easily oxidized and deteriorated during transportation, making it difficult to verify the reproducibility of the method.
A biodiesel composed of methyl palmitate, methyl erucic acid, methyl linoleate and methyl oleate was prepared with purities ranging from 97%, 90%, 98% and 70%, respectively. The mixture was stirred at 20℃ to 30℃ for 20 min to 40 min to form a biodiesel conforming to the CECL-109 method.
It provides standard biodiesel testing conforming to the CECL-109 method, meeting laboratory needs and can be used for screening high-grade engine oil formulations to ensure that antioxidant performance meets standards.
Smart Images

Figure GDA0003822875430000041 
Figure GDA0003822875430000051 
Figure GDA0003822875430000061
Abstract
Description
Technical Field
[0001] This invention belongs to the field of biodiesel technology, and relates to a biodiesel used in the CECL-109 method. This invention also relates to a method for preparing the above-mentioned biodiesel used in the CECL-109 method. Background Technology
[0002] With the increasing adoption of biodiesel, more and more commercial vehicles and ships are using it, and its impact on engine oil is gradually becoming apparent. This is mainly because biodiesel molecules contain a large number of unsaturated components, which are prone to thermal oxidation when entering the crankcase under high temperatures. This induces engine oil deterioration, leading to increased gum buildup, increased corrosiveness, and poor detergency and dispersibility. It can even cause problems such as gumming in the fuel system and clogging of filters and fuel injectors.
[0003] In 2014, Europe published the standard test method CECL-109 for evaluating the antioxidant properties of engine oils in the presence of biodiesel. In 2016, the CECL-109 method was included in the quality control indicators of the ACEA specifications. Currently, my country lacks a method for evaluating the antioxidant properties of engine oils containing biodiesel. Therefore, introducing the CECL-109 method to establish a laboratory-based method for assessing the antioxidant properties of biodiesel-containing engine oils is essential for oil developers and engine OEMs. However, introducing this method requires addressing its core issue: biodiesel. Imported biodiesel is prone to deterioration during transportation and storage due to oxidation, making method reproducibility difficult to verify. Therefore, if China were to implement the standard test method CECL-109 for engine oil antioxidant properties, it would be necessary to prepare biodiesel that meets the requirements of CECL-109. Summary of the Invention
[0004] The purpose of this invention is to provide a biodiesel for use in the CECL-109 method that enables the engine oil to undergo standard tests to meet the requirements for oil antioxidant properties.
[0005] Another object of the present invention is to provide a method for preparing biodiesel used in the CECL-109 method described above.
[0006] The first technical solution adopted in this invention is a biodiesel used in the CECL-109 method, which is composed of the following components by mass percentage: methyl palmitate 7% to 10%, methyl erucate 20% to 24%, methyl linoleate 33% to 36%, methyl oleate 33% to 37%, and the sum of the mass percentages of the above components is 100%.
[0007] The first technical solution of the present invention is further characterized in that,
[0008] The purity range of methyl palmitate is not less than 97%, the purity range of methyl erucate is not less than 90%, the purity range of methyl linoleate is not less than 98%, and the purity range of methyl oleate is not less than 70%.
[0009] Another technical solution adopted in this invention is a method for preparing biodiesel in the CECL-109 method, the specific steps of which are as follows:
[0010] Step 1: Weigh out 7%–10% methyl palmitate, 20%–24% methyl erucic acid, 33%–36% methyl linoleate, and 33%–37% methyl oleate by mass percentage, respectively, and the sum of the mass percentages of the above components is 100%.
[0011] Step 2: Add the components weighed in Step 1 to a beaker, place it on a thermostatic magnetic stirrer, adjust the temperature, and stir.
[0012] Another feature of the present invention is that,
[0013] Step 2: Adjust the temperature to 20℃~30℃.
[0014] The stirring time in step 2 is 20 to 40 minutes.
[0015] The beneficial effects of this invention are:
[0016] (1) In the CECL-109 method of the present invention, biodiesel can play a core role in the localization of the CECL-109 test standard, which helps to meet the laboratory's needs for the test method.
[0017] (2) In the CECL-109 method of the present invention, biodiesel can be used as a basic experimental means for screening high-grade engine oil formulations. Detailed Implementation
[0018] The present invention will now be described in detail with reference to specific embodiments.
[0019] The biodiesel used in the CECL-109 process of this invention is composed of the following components by mass percentage: methyl palmitate 7%–10%, methyl erucate 20%–24%, methyl linoleate 33%–36%, and methyl oleate 33%–37%, with the sum of the mass percentages of the above components being 100%.
[0020] The specific requirements for the four components used in the CECL-109 method to prepare biodiesel are shown in Table 1.
[0021] type purity Cas Methyl palmitate Not less than 97% 112-39-0 Methyl erucic acid Not less than 90% 1120-34-9 Methyl linoleate Not less than 98% 112-63-0 Methyl oleate Not less than 70% 112-62-9
[0022] Table 1
[0023] Methyl palmitate CAS number 112-39-0 with a purity range of not less than 97%, methyl erucate CAS number 1120-34-9 with a purity range of not less than 90%, methyl linoleate CAS number 112-63-0 with a purity range of not less than 98%, and methyl oleate CAS number 112-62-9 with a purity range of not less than 70%.
[0024] The present invention relates to a method for preparing biodiesel using the CECL-109 process, the specific steps of which are as follows:
[0025] Step 1: Weigh out 7%–10% methyl palmitate, 20%–24% methyl erucic acid, 33%–36% methyl linoleate, and 33%–37% methyl oleate by mass percentage, respectively, and the sum of the mass percentages of the above components is 100%.
[0026] Step 2: Add the components weighed in Step 1 to a beaker, place it on a thermostatic magnetic stirrer, adjust the speed to a suitable level so that the biodiesel does not splash out, adjust the temperature to 20℃~30℃, and stir for 20min~40min.
[0027] By using existing qualified engine oils RL257 and RL258 as reference oils, a standard test on antioxidant performance was conducted to determine whether the biodiesel prepared in this invention could meet the experimental requirements of the standard test on antioxidant performance.
[0028] Example 1
[0029] Step 1: Weigh out 10% methyl palmitate, 24% methyl erucic acid, 33% methyl linoleate, and 33% methyl oleate by mass percentage, with the sum of the mass percentages of the above components being 100%.
[0030] Step 2: Add the components weighed in Step 1 to a beaker, place it on a thermostatic magnetic stirrer, adjust the speed to a suitable level so that the biodiesel does not splash out, adjust the temperature to 20°C, and stir for 20 minutes.
[0031] The biodiesel prepared in Example 1 was subjected to standard tests on antioxidant properties with RL257 and RL258, respectively. The viscosity growth rate and oxidation value of RL257 and RL258 were detected. The experimental data are shown in Table 2.
[0032]
[0033]
[0034] Table 2
[0035] Note: A represents the control range required by the reference oil standard CECL-109.
[0036] As shown in Table 2, when the biodiesel prepared in Example 1 was used as a standard reagent to conduct standard tests on the antioxidant properties of RL257 and RL258, the viscosity growth rate and oxidation value values obtained were within the control range specified in the standard requirements for engine oil antioxidant performance tests. This indicates that the biodiesel prepared in Example 1 meets the requirements of the standard reagents in engine oil antioxidant performance tests.
[0037] Example 2
[0038] Step 1: Weigh out 9% methyl palmitate, 22% methyl erucic acid, 34% methyl linoleate, and 35% methyl oleate by mass percentage, with the sum of the mass percentages of the above components being 100%.
[0039] Step 2: Add the components weighed in Step 1 to a beaker, place it on a thermostatic magnetic stirrer, adjust the speed to a suitable level so that the biodiesel does not splash out, adjust the temperature to 30°C, and stir for 30 minutes.
[0040] The biodiesel prepared in Example 2 was subjected to standard tests on antioxidant properties with RL257 and RL258, respectively. The viscosity growth rate and oxidation value of RL257 and RL258 were detected. The experimental data are shown in Table 3.
[0041]
[0042] Table 3
[0043] Note: A represents the control range required by the reference oil standard CEC L-109.
[0044] As shown in Table 3, when the biodiesel prepared in Example 2 was used as a standard reagent to conduct standard tests on the antioxidant properties of RL257 and RL258, the viscosity growth rate and oxidation value values obtained were within the control range specified in the standard requirements for engine oil antioxidant performance tests. This indicates that the biodiesel prepared in Example 2 meets the requirements of the standard reagents in engine oil antioxidant performance tests.
[0045] Example 3
[0046] Step 1: Weigh out 7% methyl palmitate, 20% methyl erucic acid, 36% methyl linoleate, and 37% methyl oleate by mass percentage, with the sum of the mass percentages of the above components being 100%.
[0047] Step 2: Add the components weighed in Step 1 to a beaker, place it on a thermostatic magnetic stirrer, adjust the speed to a suitable level so that the biodiesel does not splash out, adjust the temperature to 40°C, and stir for 40 minutes.
[0048] The biodiesel prepared in Example 3 was subjected to standard tests on antioxidant properties with RL257 and RL258, respectively. The viscosity growth rate and oxidation value of RL257 and RL258 were detected. The experimental data are shown in Table 4.
[0049]
[0050]
[0051] Table 4
[0052] As shown in Table 4, when the biodiesel prepared in Example 3 was used as a standard reagent to conduct standard tests on the antioxidant properties of RL257 and RL258, the viscosity growth rate and oxidation value values obtained were within the control range specified in the standard requirements for engine oil antioxidant performance tests. This indicates that the biodiesel prepared in Example 3 meets the requirements of the standard reagents in engine oil antioxidant performance tests.
[0053] This application also purchased commonly used biodiesel on the market and conducted a comparative experiment with the biodiesel prepared in this application to further demonstrate that the biodiesel prepared in this application can perform standard tests on the antioxidant properties of engine oil.
[0054] Commercially available palm oil biodiesel, waste cooking oil biodiesel, and the biodiesel prepared in this application were added to RL257 and RL258 at a ratio of 7% respectively for antioxidant performance testing. The test results are shown in Table 5.
[0055]
[0056]
[0057] Table 5
[0058] As shown in Table 5, the antioxidant performance test data of palm oil biodiesel and waste cooking oil biodiesel did not reach the specified control range. However, the RL257 and RL258 used in the test were qualified engine oils. Therefore, it can be concluded that palm oil biodiesel and waste cooking oil biodiesel cannot be used to test the antioxidant performance of engine oils. In contrast, the biodiesel prepared in this application, as shown in Table 5, has antioxidant performance test data for reference oils RL257 and RL258 that are all within the specified control range. In summary, the four sets of tests show that the components and their contents described in this application can obtain biodiesel that meets the ACEA specification for engine oil antioxidant performance testing, and the measured viscosity growth rate and oxidation value are all within the specified range. Therefore, the scheme provided in this application can ideally prepare biodiesel for use in the CECL-109 method.
[0059] The biodiesel used in the CECL-109 method of this invention can serve as the core of the localization of the CECL-109 testing standard, which helps to meet the laboratory's needs for this testing method and can also serve as a basic experimental means for screening high-grade engine oil formulations.
Claims
1. An application of biodiesel, characterized in that, In the CECL-109 method, the following components are used by mass percentage: methyl palmitate 7%~10%, methyl erucate 20%~24%, methyl linoleate 33%~36%, methyl oleate 33%~37%, and the sum of the mass percentages of the above components is 100%. The purity of the methyl palmitate is not less than 97%, the purity of the methyl erucate is not less than 90%, the purity of the methyl linoleate is not less than 98%, and the purity of the methyl oleate is not less than 70%. The specific steps are as follows: Step 1: Weigh out 7%~10% methyl palmitate, 20%~24% methyl erucic acid, 33%~36% methyl linoleate, and 33%~37% methyl oleate by mass percentage, with the sum of the mass percentages of the above components being 100%. Step 2: Add the components weighed in Step 1 to a beaker, place it on a thermostatic magnetic stirrer, adjust the temperature, and stir. The temperature in step 2 is adjusted to 20℃~30℃; The stirring time in step 2 is 20 min to 40 min.
Citation Information
Patent Citations
Biodiesel having enhanced pour point
KR1020090076234A
Palm diesel with low pour point for cold climate countries
US20040231236A1