WO2023000934A1 - Method for detecting acid value of synthetic lubricating oil - Google Patents
Method for detecting acid value of synthetic lubricating oil Download PDFInfo
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- WO2023000934A1 WO2023000934A1 PCT/CN2022/102048 CN2022102048W WO2023000934A1 WO 2023000934 A1 WO2023000934 A1 WO 2023000934A1 CN 2022102048 W CN2022102048 W CN 2022102048W WO 2023000934 A1 WO2023000934 A1 WO 2023000934A1
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- Prior art keywords
- acid value
- synthetic
- solution
- potassium hydroxide
- lubricating oil
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- 239000002253 acid Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000010689 synthetic lubricating oil Substances 0.000 title claims abstract description 22
- 239000003921 oil Substances 0.000 claims abstract description 60
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 56
- 239000002904 solvent Substances 0.000 claims abstract description 35
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 29
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 29
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 29
- 239000000243 solution Substances 0.000 claims abstract description 28
- 239000012086 standard solution Substances 0.000 claims abstract description 28
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011259 mixed solution Substances 0.000 claims abstract description 25
- ADYYRXNLCZOUSU-UHFFFAOYSA-M potassium;propan-2-ol;hydroxide Chemical compound [OH-].[K+].CC(C)O ADYYRXNLCZOUSU-UHFFFAOYSA-M 0.000 claims abstract description 20
- 239000012046 mixed solvent Substances 0.000 claims abstract description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 48
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 30
- 238000012360 testing method Methods 0.000 claims description 19
- 239000003208 petroleum Substances 0.000 claims description 15
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims description 9
- 238000001514 detection method Methods 0.000 claims description 9
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 claims description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical group CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 3
- KFNNIILCVOLYIR-UHFFFAOYSA-N Propyl formate Chemical compound CCCOC=O KFNNIILCVOLYIR-UHFFFAOYSA-N 0.000 claims description 3
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 3
- 229940017219 methyl propionate Drugs 0.000 claims description 3
- 238000004448 titration Methods 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract 3
- 238000013215 result calculation Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 15
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 15
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 15
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 15
- 239000005642 Oleic acid Substances 0.000 description 15
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 15
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 15
- 238000005259 measurement Methods 0.000 description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 238000010561 standard procedure Methods 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 229920013639 polyalphaolefin Polymers 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000002199 base oil Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003759 ester based solvent Substances 0.000 description 2
- 239000002798 polar solvent Substances 0.000 description 2
- 238000003918 potentiometric titration Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
Definitions
- the application belongs to the technical field of acid value testing of lubricating oil products, and relates to a method for testing the acid value of synthetic lubricating oil.
- Acid value is an index indicating the amount of acidic components contained in oil, and refers to the number of milligrams of potassium hydroxide required to titrate 1g of oil.
- the acid value represents the refining degree of the new oil and the aging degree of the operating oil, and is an important indicator for judging the quality of the oil.
- Oil acid value test is usually potentiometric titration and color indicator method.
- the acid value test method using potentiometric titration requires the use of expensive precision instruments and electrodes, and the cost of the instruments is high.
- There are two acid value test methods using color indicators one needs to use 95% ethanol to reflux, and the titration must be completed in a short time; the other needs to use the precursor chemical toluene, and the waste after the test The recovery of the liquid is difficult, the disposal cost is high, and the health of the test personnel is endangered during the test.
- Synthetic oil uses polyalphaolefin as the base oil, and obtains excellent oil performance by adding different additives to meet different service conditions. As the operating time of the equipment increases, various acidic deterioration substances are produced, which will corrode the metal parts of the equipment.
- the common acid value test method for synthetic oil is the color indicator method using toluene and isopropanol as solvents, which makes the existing acid value detection methods unable to detect the acid value of synthetic oil economically, environmentally friendly, efficiently and accurately.
- the purpose of this application is to provide a method for detecting the acid value of synthetic lubricating oil, which can detect the acid value of synthetic oil economically, environmentally friendly, efficiently and accurately.
- a method for detecting the acid value of synthetic lubricating oil which comprises placing a synthetic oil sample to be tested in a container, adding a mixed solvent of an ester solvent and a hydrocarbon solvent, vibrating to dissolve the synthetic oil sample to be tested, adding an indicator, and using Potassium hydroxide isopropanol standard solution is titrated until the solution color changes from orange to dark green, and the acid value of synthetic lubricating oil is calculated according to the volume of potassium hydroxide isopropanol standard solution added.
- ester solvent is methyl acetate, n-propyl formate, methyl propionate or ethyl acetate.
- hydrocarbon solvent is petroleum ether, n-pentane, n-hexane or n-heptane.
- a further improvement of the present application is that the ratio of the synthetic oil sample to be tested to the mixed solvent of the ester solvent and the hydrocarbon solvent is 1.0g-5.0g: 20mL-50mL.
- a further improvement of the present application is that the volume ratio of the ester solvent to the hydrocarbon solvent in the mixed solution is 2:1-5:1.
- the further improvement of the present application is that the indicator is a 5-15g/L p-naphtholbenzene solution.
- a further improvement of the present application is that the ratio of the synthetic oil sample to be tested to the indicator is (1.0g-5.0g): (0.1-1.0mL).
- the further improvement of the present application is that the standard solution containing potassium hydroxide is potassium hydroxide isopropanol standard solution.
- Synthetic oils have different components due to different manufacturers and different aging degrees. It is necessary to adjust the ratio of ester solvents to hydrocarbon solvents according to different working conditions to achieve the ideal dissolution effect.
- the method for detecting the acid value of the synthetic oil described in this application is to dissolve the synthetic oil sample to be tested in sequence, titrate at room temperature, and calculate the results in order to obtain the acid value of the synthetic oil sample to be tested, which has the advantages of simple operation and economical operation. The characteristics of environmental protection, high efficiency and accuracy are worthy of popularization and application.
- Synthetic oil uses polyalphaolefin as the base oil, and the refined oil is obtained by adding different additives.
- the choice of solvent for the determination of its acid value must meet two conditions: one is good miscibility with synthetic oil; Solubility. After several tests, it was found that synthetic oil has better solubility in hydrocarbon solvents, but the solubility of hydrocarbon solvents to potassium hydroxide is small, which cannot meet the test requirements.
- ester solvent As a good polar solvent, ester solvent not only has a certain dissolving ability for potassium hydroxide, but also has a certain dissolving ability for synthetic oil, and the ester solvent and hydrocarbon solvent have better mutual solubility.
- the mixed solvent of ester solvent and hydrocarbon solvent was selected as the solvent for the determination of the acid value of synthetic oil.
- Synthetic oils have different components due to different manufacturers and different aging degrees. It is necessary to adjust the ratio of ester solvents to hydrocarbon solvents according to different working conditions to achieve the ideal dissolution effect.
- the detection method of synthetic oleic acid value described in the application adopts the mixed solution of ester solvent and hydrocarbon solvent as synthetic oil solvent, uses potassium hydroxide isopropanol solution as standard titration solution, specifically comprises the following steps:
- the value of synthetic oleic acid was calculated according to the concentration and volume of potassium hydroxide standard solution. Accompanied by a reagent blank test.
- the synthetic oleic acid value (mgKOH/g) was calculated by the following formula according to the concentration and volume of the potassium hydroxide solution.
- V 1 the amount of potassium hydroxide isopropanol standard solution consumed for titration of the sample, mL;
- V 0 the amount of potassium hydroxide isopropanol standard solution consumed for titrating the blank, mL;
- the detection method of synthetic oleic acid value described in the application comprises the following steps:
- the detection method of synthetic oleic acid value described in the application comprises the following steps:
- the detection method of synthetic oleic acid value described in the application comprises the following steps:
- the detection method of synthetic oleic acid value described in the application comprises the following steps:
- Example 2 The difference from Example 1 is that the hydrocarbon solvent is n-pentane.
- Example 2 The difference from Example 1 is that the hydrocarbon solvent is n-hexane.
- Example 2 The difference from Example 1 is that the hydrocarbon solvent is n-heptane.
- Example 2 The difference from Example 1 is that the ester solvent is methyl acetate.
- Example 2 The difference from Example 1 is that the ester solvent is n-propyl formate.
- Example 2 The difference from Example 1 is that the ester solvent is methyl propionate.
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- Physics & Mathematics (AREA)
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- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
A method for detecting the acid value of a synthetic lubricating oil, which method comprises: weighing a synthetic oil sample to be detected into a conical flask, adding a mixed solvent of an ester solvent and a hydrocarbon solvent, and fully oscillating same to completely dissolve the oil sample; adding a p-naphthol benzene indicator to a uniformly mixed solution of the synthetic oil, the ester solvent and the hydrocarbon solvent, titrating same with a potassium hydroxide isopropanol standard solution having a known concentration at room temperature until the color of the solution is changed from orange to dark green, recording the volume of the potassium hydroxide solution added, and calculating the acid value of the synthetic oil. When the method for detecting the acid value of a synthetic oil is specifically operated, the synthetic oil sample to be detected is sequentially subjected to dissolution, room-temperature titration and result calculation to obtain the acid value of the synthetic oil sample to be detected. The method has the characteristics of simplicity in terms of operation, being economical and environmentally friendly, having high efficiency and accuracy, and being worthy of popularization and use.
Description
相关申请的交叉引用Cross References to Related Applications
本申请要求在2021年7月19日提交中国专利局、申请号为202110815654.X、发明名称为“一种合成润滑油酸值检测方法”的中国专利申请的优先权，其全部内容通过引用的方式并入本文中。This application claims the priority of the Chinese patent application with the application number 202110815654.X and the title of the invention "A method for detecting the acid value of synthetic lubricating oil" submitted to the China Patent Office on July 19, 2021, the entire contents of which are incorporated by reference way incorporated into this article.
本申请属于润滑油油品酸值测试技术领域，涉及一种合成润滑油酸值检测方法。The application belongs to the technical field of acid value testing of lubricating oil products, and relates to a method for testing the acid value of synthetic lubricating oil.
酸值是表明油品中含有酸性组分量的指标,指滴定1g油品所需的氢氧化钾毫克数。酸值的大小表征了新油的精制程度及运行油的油质老化程度，是判断油品质量的重要指标。Acid value is an index indicating the amount of acidic components contained in oil, and refers to the number of milligrams of potassium hydroxide required to titrate 1g of oil. The acid value represents the refining degree of the new oil and the aging degree of the operating oil, and is an important indicator for judging the quality of the oil.
油品酸值测试通常为电位滴定法和颜色指示剂法。采用电位滴定的酸值测试方法需使用价格昂贵的精密仪器及电极，仪器成本高。采用颜色指示剂的酸值测试方法有两种，一种需使用95％乙醇加热回流，且必须在较短时间内完成滴定；另一种需使用易制毒化学品甲苯，且测试后的废液回收难度大、处置费用高、测试过程中危害试验人员身体健康。Oil acid value test is usually potentiometric titration and color indicator method. The acid value test method using potentiometric titration requires the use of expensive precision instruments and electrodes, and the cost of the instruments is high. There are two acid value test methods using color indicators, one needs to use 95% ethanol to reflux, and the titration must be completed in a short time; the other needs to use the precursor chemical toluene, and the waste after the test The recovery of the liquid is difficult, the disposal cost is high, and the health of the test personnel is endangered during the test.
合成油以聚α烯烃为基础油，通过添加不同的添加剂获得极佳的油品性能，以满足不同的使用条件。随着设备运行时间的增加，产生各种酸性劣化物质，这些酸性劣化物质会腐蚀设备的金属部件。目前，合成油通用的酸值测试方法是以甲苯和异丙醇为溶剂的颜色指示剂法，使得现有的酸值检测方法均无法经济环保、高效准确检测合成油的酸值。Synthetic oil uses polyalphaolefin as the base oil, and obtains excellent oil performance by adding different additives to meet different service conditions. As the operating time of the equipment increases, various acidic deterioration substances are produced, which will corrode the metal parts of the equipment. At present, the common acid value test method for synthetic oil is the color indicator method using toluene and isopropanol as solvents, which makes the existing acid value detection methods unable to detect the acid value of synthetic oil economically, environmentally friendly, efficiently and accurately.
发明内容Contents of the invention
为克服现有技术中的问题，本申请的目的在于提供一种合成润滑油酸值 检测方法，该方法能够经济环保、高效准确的对合成油酸值进行检测。In order to overcome the problems in the prior art, the purpose of this application is to provide a method for detecting the acid value of synthetic lubricating oil, which can detect the acid value of synthetic oil economically, environmentally friendly, efficiently and accurately.
为达到上述目的，本申请采用的技术方案如下：In order to achieve the above object, the technical scheme adopted by the application is as follows:
一种合成润滑油酸值检测方法，将待测合成油油样置于容器中，然后加入酯类溶剂与烃类溶剂的混合溶剂，震荡使待测合成油油样溶解后加入指示剂，用氢氧化钾异丙醇标准溶液滴定至溶液颜色由橙色变为深绿色，根据加入氢氧化钾异丙醇标准溶液的体积，计算合成润滑油酸值。A method for detecting the acid value of synthetic lubricating oil, which comprises placing a synthetic oil sample to be tested in a container, adding a mixed solvent of an ester solvent and a hydrocarbon solvent, vibrating to dissolve the synthetic oil sample to be tested, adding an indicator, and using Potassium hydroxide isopropanol standard solution is titrated until the solution color changes from orange to dark green, and the acid value of synthetic lubricating oil is calculated according to the volume of potassium hydroxide isopropanol standard solution added.
本申请进一步的改进在于，具体包括以下步骤：The further improvement of the present application lies in that it specifically includes the following steps:
1)将待测合成油油样于三角烧瓶中，加入酯类溶剂与烃类溶剂的混合溶剂，震荡至混匀；1) Put the synthetic oil sample to be tested in an Erlenmeyer flask, add a mixed solvent of ester solvent and hydrocarbon solvent, shake until mixed;
2)向混匀后的溶液中加入指示剂；2) adding an indicator to the mixed solution;
3)在室温下采用含氢氧化钾的标准溶液滴定至溶液颜色由橙色变为深绿色，记录加入氢氧化钾异丙醇标准溶液的体积；3) At room temperature, titrate with a standard solution containing potassium hydroxide until the color of the solution changes from orange to dark green, and record the volume of the potassium hydroxide isopropanol standard solution added;
4)试剂空白试验；4) Reagent blank test;
5)根据氢氧化钾异丙醇标准溶液浓度和体积计算合成润滑油酸值。5) Calculate the acid value of synthetic lubricating oil according to the concentration and volume of potassium hydroxide isopropanol standard solution.
本申请进一步的改进在于，酯类溶剂为乙酸甲酯、甲酸正丙酯、丙酸甲酯或乙酸乙酯。A further improvement of the present application is that the ester solvent is methyl acetate, n-propyl formate, methyl propionate or ethyl acetate.
本申请进一步的改进在于，烃类溶剂为石油醚、正戊烷、正己烷或正庚烷。A further improvement of the present application is that the hydrocarbon solvent is petroleum ether, n-pentane, n-hexane or n-heptane.
本申请进一步的改进在于，待测合成油油样和酯类溶剂与烃类溶剂的混合溶剂的比为1.0g-5.0g：20mL-50mL。A further improvement of the present application is that the ratio of the synthetic oil sample to be tested to the mixed solvent of the ester solvent and the hydrocarbon solvent is 1.0g-5.0g: 20mL-50mL.
本申请进一步的改进在于，混合溶液中酯类溶剂与烃类溶剂的体积比为2：1-5：1。A further improvement of the present application is that the volume ratio of the ester solvent to the hydrocarbon solvent in the mixed solution is 2:1-5:1.
本申请进一步的改进在于，指示剂为5-15g/L的对-萘酚苯溶液。The further improvement of the present application is that the indicator is a 5-15g/L p-naphtholbenzene solution.
本申请进一步的改进在于，待测合成油油样与指示剂的比为(1.0g-5.0g)：(0.1-1.0mL)。A further improvement of the present application is that the ratio of the synthetic oil sample to be tested to the indicator is (1.0g-5.0g): (0.1-1.0mL).
本申请进一步的改进在于，含氢氧化钾的标准溶液为氢氧化钾异丙醇标准溶液。The further improvement of the present application is that the standard solution containing potassium hydroxide is potassium hydroxide isopropanol standard solution.
本申请进一步的改进在于，具体包括以下步骤：The further improvement of the present application lies in that it specifically includes the following steps:
1)将待测合成油油样1.0g-5.0g于容器中，加入乙酸乙酯与石油醚的混合溶液20mL-50mL，震荡至混匀；1) Put 1.0g-5.0g of the synthetic oil sample to be tested in a container, add 20mL-50mL of a mixed solution of ethyl acetate and petroleum ether, shake until well mixed;
2)向混匀后的溶液中加入0.1-1.0mL对-萘酚苯溶液；2) Add 0.1-1.0mL p-naphtholbenzene solution to the mixed solution;
3)在室温下滴定至溶液颜色由橙色变为深绿色，记录加入氢氧化钾异丙醇标准溶液的体积；3) Titrate at room temperature until the solution color changes from orange to dark green, and record the volume of potassium hydroxide isopropanol standard solution added;
4)试剂空白试验；4) Reagent blank test;
5)根据氢氧化钾异丙醇标准溶液浓度和体积，计算合成润滑油酸值。5) According to potassium hydroxide isopropanol standard solution concentration and volume, calculate synthetic lubricating oil acid value.
与现有技术相比，本申请具有以下有益效果：Compared with the prior art, the present application has the following beneficial effects:
由于成品油通过想以聚α烯烃为基础油的合成油中添加不同的添加剂得到，成品油酸值测定时溶剂的选择必须满足两个条件：一是与合成油互溶性良好；二是对氢氧化钾有一定溶解度。合成油在烃类溶剂中溶解性较好，但烃类溶剂对氢氧化钾的溶解度较小，不能满足试验需求。而酯类溶剂作为一种良好的极性溶剂，不但对氢氧化钾有一定的溶解能力，并对合成油有一定的溶解能力，且酯类溶剂与烃类溶剂互溶性较好。所以本申请选择了酯类溶剂与烃类溶剂的混合溶剂作为合成油酸值测定的溶剂。合成油因其生产厂家不同、老化程度不同而出现不同油品间组分的差异，需根据不同工况调整酯类溶剂与烃类溶剂的比例，以达到理想的溶解效果。本申请所述的合成油酸值的检测方法在具体操作时，将待测合成油油样依次进行溶解、室温滴定、结果计算，得待测合成油油样的酸值，具有操作简单、经济环保、高效准确的特点，值得推广应用。Since refined oil is obtained by adding different additives to synthetic oil based on polyalphaolefin, the choice of solvent for acid value determination of refined oil must meet two conditions: one is good miscibility with synthetic oil; Potassium oxide has a certain solubility. Synthetic oil has good solubility in hydrocarbon solvents, but the solubility of potassium hydroxide in hydrocarbon solvents is small, which cannot meet the test requirements. As a good polar solvent, ester solvent not only has a certain dissolving ability for potassium hydroxide, but also has a certain dissolving ability for synthetic oil, and the ester solvent and hydrocarbon solvent have better mutual solubility. Therefore, this application chooses the mixed solvent of ester solvent and hydrocarbon solvent as the solvent for the determination of the acid value of synthetic oil. Synthetic oils have different components due to different manufacturers and different aging degrees. It is necessary to adjust the ratio of ester solvents to hydrocarbon solvents according to different working conditions to achieve the ideal dissolution effect. The method for detecting the acid value of the synthetic oil described in this application is to dissolve the synthetic oil sample to be tested in sequence, titrate at room temperature, and calculate the results in order to obtain the acid value of the synthetic oil sample to be tested, which has the advantages of simple operation and economical operation. The characteristics of environmental protection, high efficiency and accuracy are worthy of popularization and application.
下面结合实施例对本申请做进一步详细描述。The present application will be further described in detail below in conjunction with the embodiments.
合成油以聚α烯烃为基础油，通过添加不同的添加剂得到成品油，其酸值测定时溶剂的选择必须满足两个条件：一是与合成油互溶性良好；二是对氢氧化钾有一定溶解度。经多次试验发现，合成油在烃类溶剂中溶解性较好，但烃类溶剂对氢氧化钾的溶解度较小，不能满足试验需求。而酯类溶剂作为一种良好的极性溶剂，不但对氢氧化钾有一定的溶解能力，并对合成油有一定的溶解能力，且酯类溶剂与烃类溶剂互溶性较好。基于上述试验现象，选择了酯类溶剂与烃类溶剂的混合溶剂作为合成油酸值测定的溶剂。合成油因其生产厂家不同、老化程度不同而出现不同油品间组分的差异，需根据不同工况调整酯类溶剂与烃类溶剂的比例，以达到理想的溶解效果。Synthetic oil uses polyalphaolefin as the base oil, and the refined oil is obtained by adding different additives. The choice of solvent for the determination of its acid value must meet two conditions: one is good miscibility with synthetic oil; Solubility. After several tests, it was found that synthetic oil has better solubility in hydrocarbon solvents, but the solubility of hydrocarbon solvents to potassium hydroxide is small, which cannot meet the test requirements. As a good polar solvent, ester solvent not only has a certain dissolving ability for potassium hydroxide, but also has a certain dissolving ability for synthetic oil, and the ester solvent and hydrocarbon solvent have better mutual solubility. Based on the above test phenomena, the mixed solvent of ester solvent and hydrocarbon solvent was selected as the solvent for the determination of the acid value of synthetic oil. Synthetic oils have different components due to different manufacturers and different aging degrees. It is necessary to adjust the ratio of ester solvents to hydrocarbon solvents according to different working conditions to achieve the ideal dissolution effect.
本申请所述的合成油酸值的检测方法采用酯类溶剂与烃类溶剂混合溶液作为合成油溶剂，使用氢氧化钾异丙醇溶液作为标准滴定溶液，具体包括以下步骤：The detection method of synthetic oleic acid value described in the application adopts the mixed solution of ester solvent and hydrocarbon solvent as synthetic oil solvent, uses potassium hydroxide isopropanol solution as standard titration solution, specifically comprises the following steps:
称取待测合成油油样1.0g-5.0g于250mL三角烧瓶中，加入酯类溶剂与烃类溶剂的混合溶液20mL-50mL，其中混合溶液中酯类溶剂与烃类溶剂的体积比为2：1-5：1，充分震荡使溶液完全混匀。向混合均匀的合成油、酯类溶剂与烃类溶剂的溶液中加入0.1-1.0mL的5-15g/L的对-萘酚苯溶液。在室温下用已知浓度的氢氧化钾异丙醇标准溶液滴定至溶液颜色由橙色变为深绿色，记录加入氢氧化钾溶液的体积。根据氢氧化钾标准溶液浓度和体积计算合成油酸值。随同做试剂空白试验。根据氢氧化钾溶液浓度和体积通过下式计算合成油酸值(mgKOH/g)。Weigh 1.0g-5.0g of the synthetic oil sample to be tested into a 250mL Erlenmeyer flask, add 20mL-50mL of the mixed solution of ester solvent and hydrocarbon solvent, wherein the volume ratio of ester solvent and hydrocarbon solvent in the mixed solution is 2 :1-5:1, fully shake to make the solution completely mixed. Add 0.1-1.0mL of 5-15g/L p-naphtholbenzene solution to the uniformly mixed solution of synthetic oil, ester solvent and hydrocarbon solvent. Titrate with a standard solution of potassium hydroxide isopropanol at room temperature until the color of the solution changes from orange to dark green, and record the volume of potassium hydroxide solution added. The value of synthetic oleic acid was calculated according to the concentration and volume of potassium hydroxide standard solution. Accompanied by a reagent blank test. The synthetic oleic acid value (mgKOH/g) was calculated by the following formula according to the concentration and volume of the potassium hydroxide solution.
酸值＝[(V
1-V
0)M×56.1]/W
Acid value = [(V 1 -V 0 )M×56.1]/W
式中：V
1—滴定试样所消耗氢氧化钾异丙醇标准溶液的量，mL；
In the formula: V 1 - the amount of potassium hydroxide isopropanol standard solution consumed for titration of the sample, mL;
V
0—滴定空白所消耗氢氧化钾异丙醇标准溶液的量，mL；
V 0 —the amount of potassium hydroxide isopropanol standard solution consumed for titrating the blank, mL;
M—氢氧化钾异丙醇标准溶液的浓度，mol/L；M—concentration of potassium hydroxide isopropanol standard solution, mol/L;
W—试样量，g；W—sample weight, g;
56.1—氢氧化钾的摩尔质量，g/mol。56.1—the molar mass of potassium hydroxide, g/mol.
实施例1Example 1
本申请所述的合成油酸值的检测方法包括以下步骤：The detection method of synthetic oleic acid value described in the application comprises the following steps:
1)称取待测合成油油样1.0g于250mL三角烧瓶中，加入乙酸乙酯与石油醚的混合溶液50mL，其中混合溶液中乙酸乙酯与石油醚的体积比为5：1，充分震荡使溶液完全混匀。1) Weigh 1.0 g of the synthetic oil sample to be tested into a 250 mL Erlenmeyer flask, add 50 mL of a mixed solution of ethyl acetate and petroleum ether, where the volume ratio of ethyl acetate to petroleum ether in the mixed solution is 5:1, shake well Mix the solution thoroughly.
2)向混合均匀的合成油、乙酸乙酯和石油醚的溶液中加入浓度为15g/L的对-萘酚苯溶液0.1mL。2) Add 0.1 mL of p-naphtholbenzene solution with a concentration of 15 g/L to the homogeneously mixed solution of synthetic oil, ethyl acetate and petroleum ether.
3)在室温下用已知浓度的氢氧化钾异丙醇标准溶液滴定至溶液颜色由橙色变为深绿色，记录加入氢氧化钾溶液的体积。3) At room temperature, titrate with a standard potassium hydroxide solution of known concentration in isopropanol until the color of the solution changes from orange to dark green, and record the volume of potassium hydroxide solution added.
4)随同做试剂空白试验。4) Do reagent blank test along with it.
5)根据氢氧化钾标准溶液浓度和体积计算合成油酸值，参见表1。5) Calculate the synthetic oleic acid value according to the potassium hydroxide standard solution concentration and volume, see Table 1.
表1合成油酸值Table 1 Synthetic oleic acid value
| 方法method | 酸值mgKOH/gAcid value mgKOH/g |
| GB/T4945测定结果GB/T4945 measurement results | 0.7710.771 |
| 本方法测定结果The result of this method | 0.7550.755 |
从表1可以看出，本申请的测定结果与国标法测定结果比较接近，说明本申请的计算比较准确。As can be seen from Table 1, the measurement result of the present application is closer to the measurement result of the national standard method, indicating that the calculation of the present application is more accurate.
实施例2Example 2
本申请所述的合成油酸值的检测方法包括以下步骤：The detection method of synthetic oleic acid value described in the application comprises the following steps:
1)称取待测合成油油样2.0g于250mL三角烧瓶中，加入乙酸乙酯与石油醚的混合溶液20mL，其中混合溶液中乙酸乙酯与石油醚的体积比为2：1，充分震荡使溶液完全混匀。1) Weigh 2.0g of the synthetic oil sample to be tested into a 250mL Erlenmeyer flask, add 20mL of a mixed solution of ethyl acetate and petroleum ether, where the volume ratio of ethyl acetate and petroleum ether in the mixed solution is 2:1, shake well Mix the solution thoroughly.
2)向混合均匀的合成油、乙酸乙酯和石油醚的溶液中加入浓度为10g/L的对-萘酚苯溶液0.5mL。2) Add 0.5 mL of p-naphtholbenzene solution with a concentration of 10 g/L to the homogeneously mixed solution of synthetic oil, ethyl acetate and petroleum ether.
3)在室温下用已知浓度的氢氧化钾异丙醇标准溶液滴定至溶液颜色由橙色变为深绿色，记录加入氢氧化钾溶液的体积。3) At room temperature, titrate with a standard potassium hydroxide solution of known concentration in isopropanol until the color of the solution changes from orange to dark green, and record the volume of potassium hydroxide solution added.
4)随同做试剂空白试验。4) Do reagent blank test along with it.
5)根据氢氧化钾标准溶液浓度和体积计算合成油酸值，参见表2。5) Calculate the synthetic oleic acid value according to the potassium hydroxide standard solution concentration and volume, see Table 2.
表2合成油酸值Table 2 Synthetic oleic acid value
| 方法method | 酸值mgKOH/gAcid value mgKOH/g |
| GB/T4945测定结果GB/T4945 measurement results | 0.7070.707 |
| 本方法测定结果The result of this method | 0.7140.714 |
从表2可以看出，本申请的测定结果与国标法测定结果比较接近，说明本申请的计算比较准确。As can be seen from Table 2, the measurement result of the present application is closer to the measurement result of the national standard method, indicating that the calculation of the present application is more accurate.
实施例3Example 3
本申请所述的合成油酸值的检测方法包括以下步骤：The detection method of synthetic oleic acid value described in the application comprises the following steps:
1)称取待测合成油油样3.0g于250mL三角烧瓶中，加入乙酸乙酯与石油醚的混合溶液30mL，其中混合溶液中乙酸乙酯与石油醚的体积比为3：1，充分震荡使溶液完全混匀。1) Weigh 3.0g of the synthetic oil sample to be tested into a 250mL Erlenmeyer flask, add 30mL of a mixed solution of ethyl acetate and petroleum ether, where the volume ratio of ethyl acetate and petroleum ether in the mixed solution is 3:1, shake well Mix the solution thoroughly.
2)向混合均匀的合成油、乙酸乙酯和石油醚的溶液中加入浓度为5g/L 的对-萘酚苯溶液1.0mL。2) Add 1.0 mL of p-naphtholbenzene solution with a concentration of 5 g/L to the homogeneously mixed solution of synthetic oil, ethyl acetate and petroleum ether.
3)在室温下用已知浓度的氢氧化钾异丙醇标准溶液滴定至溶液颜色由橙色变为深绿色，记录加入氢氧化钾溶液的体积。3) At room temperature, titrate with a standard potassium hydroxide solution of known concentration in isopropanol until the color of the solution changes from orange to dark green, and record the volume of potassium hydroxide solution added.
4)随同做试剂空白试验。4) Do reagent blank test along with it.
5)根据氢氧化钾标准溶液浓度和体积计算合成油酸值，参见表3。5) Calculate the synthetic oleic acid value according to the potassium hydroxide standard solution concentration and volume, see Table 3.
表3合成油酸值Table 3 Synthetic oleic acid value
| 方法method | 酸值mgKOH/gAcid value mgKOH/g |
| GB/T4945测定结果GB/T4945 measurement results | 0.3250.325 |
| 本方法测定结果The result of this method | 0.3410.341 |
从表3可以看出，本申请的测定结果与国标法测定结果比较接近，说明本申请的计算比较准确。As can be seen from Table 3, the measurement result of the present application is closer to the measurement result of the national standard method, indicating that the calculation of the present application is more accurate.
实施例4Example 4
本申请所述的合成油酸值的检测方法包括以下步骤：The detection method of synthetic oleic acid value described in the application comprises the following steps:
1)称取待测合成油油样5.0g于250mL三角烧瓶中，加入乙酸乙酯与石油醚的混合溶液40mL，其中混合溶液中乙酸乙酯与石油醚的体积比为4：1，充分震荡使溶液完全混匀。1) Weigh 5.0g of the synthetic oil sample to be tested into a 250mL Erlenmeyer flask, add 40mL of a mixed solution of ethyl acetate and petroleum ether, wherein the volume ratio of ethyl acetate and petroleum ether in the mixed solution is 4:1, shake well Mix the solution thoroughly.
2)向混合均匀的合成油、乙酸乙酯和石油醚的溶液中加入浓度为8g/L的对-萘酚苯溶液0.6mL。2) Add 0.6mL of p-naphtholbenzene solution with a concentration of 8g/L to the homogeneously mixed solution of synthetic oil, ethyl acetate and petroleum ether.
3)在室温下用已知浓度的氢氧化钾异丙醇标准溶液滴定至溶液颜色由橙色变为深绿色，记录加入氢氧化钾溶液的体积。3) At room temperature, titrate with a standard potassium hydroxide solution of known concentration in isopropanol until the color of the solution changes from orange to dark green, and record the volume of potassium hydroxide solution added.
4)随同做试剂空白试验。4) Do reagent blank test along with it.
5)根据氢氧化钾标准溶液浓度和体积计算合成油酸值，参见表4。5) Calculate the synthetic oleic acid value according to the potassium hydroxide standard solution concentration and volume, see Table 4.
表4合成油酸值Table 4 Synthetic oleic acid value
| 方法method | 酸值mgKOH/gAcid value mgKOH/g |
| GB/T4945测定结果GB/T4945 measurement results | 1.2381.238 |
| 本方法测定结果The result of this method | 1.2361.236 |
从表4可以看出，本申请的测定结果与国标法测定结果比较接近，说明本申请的计算比较准确。As can be seen from Table 4, the measurement result of the present application is closer to the measurement result of the national standard method, indicating that the calculation of the present application is more accurate.
实施例5Example 5
与实施例1不同在于，烃类溶剂为正戊烷。The difference from Example 1 is that the hydrocarbon solvent is n-pentane.
实施例6Example 6
与实施例1不同在于，烃类溶剂为正己烷。The difference from Example 1 is that the hydrocarbon solvent is n-hexane.
实施例7Example 7
与实施例1不同在于，烃类溶剂为正庚烷。The difference from Example 1 is that the hydrocarbon solvent is n-heptane.
实施例8Example 8
与实施例1不同在于，酯类溶剂为乙酸甲酯。The difference from Example 1 is that the ester solvent is methyl acetate.
实施例9Example 9
与实施例1不同在于，酯类溶剂为甲酸正丙酯。The difference from Example 1 is that the ester solvent is n-propyl formate.
实施例10Example 10
与实施例1不同在于，酯类溶剂为丙酸甲酯。The difference from Example 1 is that the ester solvent is methyl propionate.
Claims (10)
- 一种合成润滑油酸值检测方法，其特征在于，将待测合成油油样置于容器中，然后加入酯类溶剂与烃类溶剂的混合溶剂，震荡使待测合成油油样溶解后加入指示剂，用氢氧化钾异丙醇标准溶液滴定至溶液颜色由橙色变为深绿色，根据加入氢氧化钾异丙醇标准溶液的体积，计算合成润滑油酸值。A method for detecting the acid value of synthetic lubricating oil, which is characterized in that the synthetic oil sample to be tested is placed in a container, and then a mixed solvent of an ester solvent and a hydrocarbon solvent is added, oscillated to dissolve the synthetic oil sample to be tested, and then added As an indicator, titrate with potassium hydroxide isopropanol standard solution until the color of the solution changes from orange to dark green, and calculate the acid value of synthetic lubricating oil according to the volume of potassium hydroxide isopropanol standard solution added.
- 根据权利要求1所述的合成润滑油酸值检测方法，其特征在于，具体包括以下步骤：synthetic lubricating oil acid value detection method according to claim 1, is characterized in that, specifically comprises the following steps:1)将待测合成油油样于三角烧瓶中，加入酯类溶剂与烃类溶剂的混合溶剂，震荡至混匀；1) Put the synthetic oil sample to be tested in an Erlenmeyer flask, add a mixed solvent of ester solvent and hydrocarbon solvent, shake until mixed;2)向混匀后的溶液中加入指示剂；2) adding an indicator to the mixed solution;3)在室温下采用含氢氧化钾的标准溶液滴定至溶液颜色由橙色变为深绿色，记录加入氢氧化钾异丙醇标准溶液的体积；3) At room temperature, titrate with a standard solution containing potassium hydroxide until the color of the solution changes from orange to dark green, and record the volume of the potassium hydroxide isopropanol standard solution added;4)试剂空白试验；4) Reagent blank test;5)根据氢氧化钾异丙醇标准溶液浓度和体积计算合成润滑油酸值。5) Calculate the acid value of synthetic lubricating oil according to the concentration and volume of potassium hydroxide isopropanol standard solution.
- 根据权利要求1或2所述的合成润滑油酸值检测方法，其特征在于，酯类溶剂为乙酸甲酯、甲酸正丙酯、丙酸甲酯或乙酸乙酯。The method for detecting the acid value of synthetic lubricating oil according to claim 1 or 2, wherein the ester solvent is methyl acetate, n-propyl formate, methyl propionate or ethyl acetate.
- 根据权利要求2所述的合成润滑油酸值检测方法，其特征在于，烃类溶剂为石油醚、正戊烷、正己烷或正庚烷。The method for detecting the acid value of synthetic lubricating oil according to claim 2, wherein the hydrocarbon solvent is sherwood oil, n-pentane, n-hexane or n-heptane.
- 根据权利要求2所述的合成润滑油酸值检测方法，其特征在于，待测合成油油样和酯类溶剂与烃类溶剂的混合溶剂的比为1.0g-5.0g：20mL-50mL。The method for detecting the acid value of synthetic lubricating oil according to claim 2, wherein the ratio of the synthetic oil sample to be tested to the mixed solvent of the ester solvent and the hydrocarbon solvent is 1.0g-5.0g: 20mL-50mL.
- 根据权利要求2所述的合成润滑油酸值检测方法，其特征在于，混合溶液中酯类溶剂与烃类溶剂的体积比为2：1-5：1。The method for detecting the acid value of synthetic lubricating oil according to claim 2, characterized in that the volume ratio of the ester solvent to the hydrocarbon solvent in the mixed solution is 2:1-5:1.
- 根据权利要求2所述的合成润滑油酸值检测方法，其特征在于，指示剂为5-15g/L的对-萘酚苯溶液。The synthetic lubricating oil acid value detection method according to claim 2, is characterized in that, indicator is the p-naphtholbenzene solution of 5-15g/L.
- 根据权利要求2所述的合成润滑油酸值检测方法，其特征在于，待测合成油油样与指示剂的比为(1.0g-5.0g)：(0.1-1.0mL)。The method for detecting the acid value of synthetic lubricating oil according to claim 2, wherein the ratio of the synthetic oil sample to be tested to the indicator is (1.0g-5.0g): (0.1-1.0mL).
- 根据权利要求2所述的合成润滑油酸值检测方法，其特征在于，含氢氧化钾的标准溶液为氢氧化钾异丙醇标准溶液。The method for detecting acid value of synthetic lubricating oil according to claim 2, characterized in that the standard solution containing potassium hydroxide is potassium hydroxide isopropanol standard solution.
- 根据权利要求2所述的合成润滑油酸值检测方法，其特征在于，具体包括以下步骤：synthetic lubricating oil acid value detection method according to claim 2, is characterized in that, specifically comprises the following steps:1)将待测合成油油样1.0g-5.0g于容器中，加入乙酸乙酯与石油醚的混合溶液20mL-50mL，震荡至混匀；1) Put 1.0g-5.0g of the synthetic oil sample to be tested in a container, add 20mL-50mL of a mixed solution of ethyl acetate and petroleum ether, shake until well mixed;2)向混匀后的溶液中加入0.1-1.0mL对-萘酚苯溶液；2) Add 0.1-1.0mL p-naphtholbenzene solution to the mixed solution;3)在室温下滴定至溶液颜色由橙色变为深绿色，记录加入氢氧化钾异丙醇标准溶液的体积；3) Titrate at room temperature until the solution color changes from orange to dark green, and record the volume of potassium hydroxide isopropanol standard solution added;4)试剂空白试验；4) Reagent blank test;5)根据氢氧化钾异丙醇标准溶液浓度和体积，计算合成润滑油酸值。5) According to potassium hydroxide isopropanol standard solution concentration and volume, calculate synthetic lubricating oil acid value.
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