CN114487359A - Device and method for testing hydrolysis performance of lubricating oil and refrigerant in mixed state - Google Patents
Device and method for testing hydrolysis performance of lubricating oil and refrigerant in mixed state Download PDFInfo
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- CN114487359A CN114487359A CN202011262739.1A CN202011262739A CN114487359A CN 114487359 A CN114487359 A CN 114487359A CN 202011262739 A CN202011262739 A CN 202011262739A CN 114487359 A CN114487359 A CN 114487359A
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- 238000012360 testing method Methods 0.000 title claims abstract description 116
- 239000003507 refrigerant Substances 0.000 title claims abstract description 88
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 32
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 18
- 239000003921 oil Substances 0.000 claims abstract description 76
- 239000000463 material Substances 0.000 claims abstract description 41
- 239000002184 metal Substances 0.000 claims abstract description 33
- 229910052751 metal Inorganic materials 0.000 claims abstract description 33
- 239000000523 sample Substances 0.000 claims description 54
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 24
- 229910000831 Steel Inorganic materials 0.000 claims description 23
- 239000010959 steel Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 230000008859 change Effects 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 8
- 230000007797 corrosion Effects 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 239000000314 lubricant Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 235000019198 oils Nutrition 0.000 description 53
- 150000002148 esters Chemical class 0.000 description 16
- 239000004744 fabric Substances 0.000 description 9
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 8
- 229910010271 silicon carbide Inorganic materials 0.000 description 8
- 239000002199 base oil Substances 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 230000003301 hydrolyzing effect Effects 0.000 description 4
- 239000008139 complexing agent Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005057 refrigeration Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 230000009970 fire resistant effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241001572350 Lycaena mariposa Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000013538 functional additive Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000010721 machine oil Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 235000019476 oil-water mixture Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/26—Oils; Viscous liquids; Paints; Inks
- G01N33/28—Oils, i.e. hydrocarbon liquids
- G01N33/2888—Lubricating oil characteristics, e.g. deterioration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- Immunology (AREA)
- General Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Food Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
The invention provides a device and a method for testing hydrolysis performance of lubricating oil and refrigerant in a mixed state, wherein the device comprises: the device comprises an autoclave body, a temperature controller, a constant temperature sleeve, a refrigerating device, a vacuumizing device and a pressure measuring device, wherein the autoclave body is used for placing a test oil sample, a metal test material and a refrigerant; the temperature controller is connected with the high-pressure kettle body and is used for measuring the temperature of the high-pressure kettle body; the constant temperature sleeve is sleeved on the outer surface of the high-pressure kettle body and is used for maintaining the high-pressure kettle body within a constant temperature; the refrigerating device is connected with the high-pressure kettle body and used for providing the refrigerant; the vacuumizing device is connected with the high-pressure kettle body and is used for vacuumizing the high-pressure kettle body; and the pressure measuring device is connected with the high-pressure kettle body and used for measuring the pressure in the high-pressure kettle body.
Description
Technical Field
The invention relates to a method and a device for testing hydrolysis performance of synthetic ester refrigerator oil under the coexistence of refrigerants, belonging to the technical field of refrigerator oil research.
Background
Synthetic ester (POE) has reliable lubricity, excellent thermal stability, chemical stability, material compatibility and good safety and environmental protection performance, and is the first choice base oil of synthetic refrigerator oil due to good intersolubility with chlorine-free hydrocarbon refrigerants (such as R134a, R410a, R407c, R290 and the like) at present when chlorine-containing refrigerants are gradually eliminated.
The hydrolytic stability of the synthetic ester is one of the important performance properties, and is used for representing the stability of oil products under the action of water and metal. A test method for measuring the hydrolysis stability of the synthetic ester mainly comprises SH/T0301 hydraulic fluid hydrolysis stability measurement method (glass bottle method), wherein an oil sample, water and a copper sheet are sealed in a pressure-resistant glass tube, then the pressure-resistant glass tube is placed in an oil product hydrolysis stability test box at the temperature of 93 +/-0.5 ℃, after the pressure-resistant glass tube rotates for 48 hours in a head-tail reversal mode, an oil-water mixture is filtered, insoluble substances are measured, oil and water are separated, and the viscosity, the acid value, the total acidity of a water layer and the quality change of the copper sheet of the oil are respectively measured; in addition, there is also a method for measuring hydrolytic stability of DL/T1420 phosphate fire-resistant oil, which comprises mixing oil sample and water at a mass ratio of 3:1, refluxing at 85 deg.C for 96h to hydrolyze the sample, and measuring the acid values of the sample and water before and after the reaction. SH/T0301 can effectively represent the hydrolysis performance condition of the synthetic ester in the presence of water, but is limited by equipment and a method, and the method cannot evaluate the performance decay condition of the synthetic ester when a refrigerant coexists; DL/T1420 is not only unable to characterize the hydrolysis state of the synthetic ester in the presence of refrigerant, but also the method is only suitable for measuring the hydrolysis stability of the phosphate fire-resistant oil, so that both methods are not suitable for measuring the hydrolysis stability of the synthetic ester in the presence of refrigerant.
When the hydrolysis performance of the synthetic ester type refrigerating machine oil in the presence of the refrigerant is measured, due to the presence of the refrigerant, the testing equipment is required to resist high temperature and bear ultrahigh pressure generated when the refrigerant is heated, and the pressure is influenced by the type and the temperature of the refrigerant and ranges from several megapascals to dozens of megapascals; the high pressure of the refrigerant has very strict requirements on the material of the test equipment, and the common glass material can resist high temperature but cannot bear the high pressure, so that the test equipment, namely an autoclave and stainless steel material is introduced into the method, so that the high temperature resistance is realized, the pressure of dozens of megapascals can be borne, and the requirement of the test on the hydrolysis performance of the synthetic ester can be completely met.
The method is a trend of technical research on synthetic refrigerator oil.
Disclosure of Invention
In order to solve the above technical problem, the present invention provides a device for testing hydrolysis performance of a lubricant in a mixed state with a refrigerant, the device comprising:
the high-pressure kettle body is used for placing a test oil sample, a metal test material and a refrigerant;
the temperature controller is connected with the high-pressure kettle body and used for measuring the temperature of the high-pressure kettle body;
the constant temperature sleeve is sleeved on the outer surface of the high-pressure kettle body and is used for maintaining the high-pressure kettle body within a constant temperature;
the refrigerating device is connected with the high-pressure kettle body and used for providing the refrigerant;
the vacuumizing device is connected with the high-pressure kettle body and is used for vacuumizing the high-pressure kettle body;
and the pressure measuring device is connected with the high-pressure kettle body and used for measuring the pressure in the high-pressure kettle body.
In one embodiment, the refrigeration device is a refrigerant tank with high pressure, and the refrigeration device is connected with the autoclave body through a refrigerant conveying pipeline provided with a refrigerant valve.
In one embodiment, the pressure measuring device includes a pressure gauge and a pressure sensor connected to the pressure gauge, and the pressure sensor is connected to the autoclave body.
In one embodiment, the temperature controller is further provided with a thermistor temperature measuring probe, and the thermistor temperature measuring probe is connected with the autoclave body.
In an embodiment, the vacuum pumping device includes a vacuum pump and a vacuum valve, and the vacuum pump is connected to the autoclave body through a vacuum pipeline provided with the vacuum valve.
In one embodiment, the vacuum pipeline and the refrigerant conveying pipeline are combined into a main pipeline close to the autoclave body, the main pipeline is provided with the pressure gauge, the pressure sensor, the pressure safety valve, the blow-down valve and the stop valve, and the main pipeline is communicated with the autoclave body.
In one embodiment, the metal test material is a steel sheet and/or a copper wire.
The invention also provides a method for testing the hydrolysis performance of the lubricating oil and the refrigerant in a mixed state, which is characterized by comprising the following steps of:
step S1, grinding the surface of the metal test material and removing free particles on the surface;
step S2, putting the metal test material, the test oil sample and the water processed in the step S1 into an autoclave body to enable the water-oil ratio to reach a preset water-oil ratio, and covering a kettle cover;
step S3, vacuumizing the autoclave body, closing the vacuum pump when the vacuum degree in the autoclave body reaches a preset value, and injecting a refrigerant into the autoclave body while recording the weight of the refrigerant injected into the autoclave body;
step S4, heating the autoclave body to enable the temperature in the autoclave body to reach a preset temperature value and enable the system pressure in the autoclave body to reach a preset pressure value by adjusting an emptying valve on the autoclave body;
step S5, maintaining the metal test material in the autoclave body for a test time under the preset temperature value, the preset pressure value and the preset water-oil ratio;
step S6, after the pressure in the high-pressure autoclave is reduced to normal pressure and the temperature is reduced to room temperature, emptying the refrigerant and taking out the metal test material and the test oil sample;
step S7, processing the metal test material and the test oil sample;
removing oil stains on the surface of a metal test material, and observing the appearance and the corrosion condition of the metal test material;
and removing the refrigerant in the tested oil sample before testing the tested oil sample, filtering the tested oil sample, testing the viscosity and the acid value of the tested oil sample, and calculating the viscosity change rate of the sample.
In one embodiment, the pair of metal test materials is a steel sheet and/or a copper wire.
In one embodiment, the temperature is 175 degrees, the pressure is 2.5MPa, the test time is 336 hours, and the water-oil ratio is 1: 1000.
Has the advantages that:
the method has the advantages of overcoming the defect that the prior art can not evaluate the hydrolysis performance of the synthetic ester under the condition of coexisting refrigerants, filling the blank in the country in the aspect, effectively developing an evaluation method of the actual hydrolysis performance of the synthetic ester refrigerator oil under the contact state of four of lubricating oil, water, refrigerants and workpieces in the actual operation process, greatly shortening the research and development test period and improving the working efficiency.
Drawings
Fig. 1 is a device for testing hydrolysis performance of a lubricating oil and a refrigerant in a mixed state.
Wherein the reference numerals are:
an autoclave body 10;
a main pipe 101;
a pressure relief valve 102;
a blow-down valve 103;
a shut-off valve 104;
a temperature controller 20;
a thermistor temperature probe 201;
a constant temperature jacket 30;
a refrigeration device 40;
A refrigerant valve 403;
a vacuum-pumping device 50;
a vacuum pump 501;
a vacuum valve 502;
a pressure measuring device 60;
a pressure gauge 601;
a pressure sensor 602.
Detailed Description
The detailed description and technical contents of the invention are described as follows with the accompanying drawings: the invention is further described with reference to the following figures and examples: the following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Referring to fig. 1, the invention provides a device for testing hydrolysis performance of lubricating oil and refrigerant in a mixed state, which comprises an autoclave body 10, a temperature controller 20, a constant temperature sleeve 30, a refrigerating device 40, a vacuumizing device 50 and a pressure measuring device, wherein the autoclave body 10 is used for placing a test oil sample, a metal test material and a refrigerant; in this embodiment, the metal test material is steel sheet, copper wire, temperature controller 20, with the autoclave body 10 is connected, temperature controller 20 still is equipped with a thermistor temperature probe 201, thermistor temperature probe 201 with the autoclave body 10 is connected for measure the temperature of the autoclave body 10. The constant temperature sleeve 30 is sleeved on the outer surface of the autoclave body 10 and is used for maintaining the autoclave body 10 at a constant temperature;
the refrigerating device 40 is connected with the autoclave body 10 and used for providing the refrigerant, the refrigerating device 40 is a refrigerant tank 401 with high pressure, and the refrigerating device 40 is connected with the autoclave body 10 through a refrigerant conveying pipeline 402 with a refrigerant valve; the refrigerant conveying pipe 402 is a high pressure resistant pipe, and the refrigerant conveying pipe 402 is wrapped with an insulating layer.
An evacuating device 50, with the autoclave body 10 is connected, it is right to be used for evacuation in the autoclave body 10, evacuating device 50 includes a vacuum pump 501 and a vacuum valve 502, vacuum pump 501 is equipped with through one the vacuum line of vacuum valve 502 with the autoclave body 10 is connected.
The pressure measuring device is connected with the autoclave body 10 and used for measuring the pressure in the autoclave body 10, the pressure measuring device comprises a pressure gauge 601 and a pressure sensor 602 connected with the pressure gauge 601, and the pressure sensor 602 is connected with the autoclave body 10.
The vacuum pipeline and the refrigerant conveying pipeline 402 are combined into a main pipeline 101 at a position close to the autoclave body 10, the main pipeline 101 is provided with the pressure gauge 601, the pressure sensor 602, the pressure safety valve 102, the blow-down valve 103 and the stop valve 104, and the main pipeline 101 is communicated with the autoclave body 10.
The application also provides a method for testing the hydrolysis performance of lubricating oil and a refrigerant in a mixed state, which is characterized by comprising the following steps of:
step S1, grinding the surface of the metal test material and removing free particles on the surface;
step S2, putting the metal test material, the test oil sample and the water processed in the step S1 into the autoclave body 10 to enable the water-oil ratio to reach a preset water-oil ratio, and covering a kettle cover;
step S3, vacuumizing the autoclave body 10, turning off the vacuum pump 501 when the vacuum degree in the autoclave body 10 reaches a preset value, and injecting a refrigerant into the autoclave body 10 while recording the weight of the refrigerant injected into the autoclave body 10;
step S4, heating the autoclave body 10 by using a constant temperature sleeve 30 to enable the temperature in the autoclave body 10 to reach a preset temperature value and enabling the system pressure in the autoclave body 10 to reach a preset pressure value by adjusting an emptying valve 103 on the autoclave body 10;
step S5, maintaining the metal test material in the autoclave body 10 for a test time under the preset temperature value, the preset pressure value and the preset water-oil ratio;
step S6, after the pressure in the autoclave body 10 is reduced to normal pressure and the temperature is reduced to room temperature, emptying the refrigerant and taking out the metal test material and the test oil sample;
step S7, processing the metal test material and the test oil sample;
removing oil stains on the surface of a metal test material, and observing the appearance and the corrosion condition of the metal test material;
and removing the refrigerant in the tested oil sample before testing the tested oil sample, filtering the tested oil sample, testing the viscosity and the acid value of the tested oil sample, and calculating the viscosity change rate of the sample.
The pair of metal test materials are steel sheets and/or copper wires. The temperature preset value is 175 degrees, the pressure preset value is 2.5MPa, the test time is 336 hours, and the preset water-oil ratio is 1: 1000.
The following is a specific application scenario, and further details the method for testing the hydrolysis performance of the lubricating oil and the refrigerant in a mixed state.
And selecting the base oil A of the synthetic ester refrigerator oil as a test oil sample, performing a test, comparing the test result with the test oil sample B added with the composite functional additive, and investigating the influence of the change of the additive scheme and the test conditions on the hydrolytic stability performance of the synthetic ester refrigerator oil.
The physicochemical properties of the base oil are shown in Table 2.
TABLE 2 physical and chemical Properties of base oils for synthetic ester refrigerator oils
Step 1, preparation of test materials: steel sheet: meets the requirement of GB/T699, the size is 75.3mm plus or minus 0.1mm plus or minus 8.9mm plus or minus 0.1mm plus or minus 0.3mm plus or minus 0.02mm, and the surface roughness Ra is 0.63-1.25 mu m. Copper wire: the purity of the copper which meets the requirement of T2 in GB/T5231 is more than 99.9%. Diameter 1.6mm, length 75 mm. The treatment process is as follows: firstly, grinding the prepared steel sheet once by using No. 240 silicon carbide abrasive paper or abrasive cloth, then grinding once by using No. 600 silicon carbide abrasive paper or abrasive cloth, and finally grinding once by using No. 240 silicon carbide abrasive paper or abrasive cloth and No. 600 silicon carbide abrasive paper or abrasive cloth respectively; in the same steel sheet treatment process, firstly grinding the prepared copper wire once by using No. 240 silicon carbide abrasive paper or abrasive cloth, then grinding once by using No. 600 silicon carbide abrasive paper or abrasive cloth, finally grinding once by using No. 240 silicon carbide abrasive paper or abrasive cloth and then grinding once by using No. 600 silicon carbide abrasive paper or abrasive cloth, and finally cutting the copper wire into segments with the thickness of 75 mm; and wiping the polished steel sheet and copper wire with absorbent cotton or cotton paper dipped with gasoline, removing free particles on the surfaces of the steel sheet and the copper wire, and finally putting the steel sheet and the copper wire into a ground bottle filled with acetone for later use.
And 2, putting the treated metal test materials (one steel sheet and one copper wire) into a 0.5L autoclave body 10, adding 200g of test oil sample, injecting a certain proportion of water, closing the autoclave cover, tightening a screw cap, and closing all valves.
Step 3, switching in and starting the vacuum pump 501, opening the vacuum valve 502 of the vacuum pump 501 to enable the vacuum degree in the autoclave body 10 to reach 50Pa, keeping the vacuum degree for 30min, then closing the vacuum valve 502, stopping the vacuum pump 501, and detaching the connecting pipe of the vacuum pump 501; placing a refrigerant tank 401 on an electronic platform scale, connecting a refrigerant valve 403 of the refrigerant tank 401 with a stop valve 104 of the autoclave body 10, but not tightening, slowly opening the refrigerant tank valve 403, and tightening after a refrigerant is sprayed out from an interface to fill a connecting pipe with the refrigerant; the electronic platform scale is reset to zero, an inlet valve of the high-pressure kettle body 10 is opened, the refrigerant is filled into the high-pressure kettle body 10, a stop valve 104 of the high-pressure kettle body 10 is closed after the refrigerant is filled to a certain pressure, the refrigerant connecting pipe is loosened slowly, the refrigerant in the pipe is discharged (protective gloves are arranged during operation to prevent the refrigerant from being frozen), and the connecting pipe is detached. When the pressure of the refrigerant tank 401 is insufficient, a metal Dewar bottle filled with liquid nitrogen (or absolute ethyl alcohol at the temperature lower than-50 ℃) can be placed below the autoclave body 10, so that the liquid nitrogen (or absolute ethyl alcohol at the temperature lower than-50 ℃) is immersed into the bottom 2/3 of the autoclave body 10, the temperature is kept for 15min, and then the refrigerant is filled according to the steps. Note that after the refrigerant is filled, the autoclave body 10 is wiped dry with a dry cloth.
Step 4, sleeving an electric heating sleeve at the bottom of the autoclave body 10, opening the autoclave body for heating, wherein in the heating process, a refrigerant in the autoclave body 10 is heated and expanded, so that the pressure in the system continuously rises, and at the moment, an air release valve 103 above the autoclave body 10 is timely opened to ensure that the pressure in the autoclave body does not exceed the pressure value in the table 1 all the time; the timer was started when the temperature and pressure reached the test conditions of table 1 simultaneously.
TABLE 1 autoclave body test conditions
| Item | Test conditions |
| Test temperature/. degree.C | 175 |
| Test time/h | 336 |
| Test pressure/MPa | 2.5 |
| Water/oil (m/m) | 1:1000 |
Step 5, the test was carried out under the test conditions specified in table 1.
And 6, removing the heating sleeve after the test is finished, naturally cooling the high-pressure kettle body 10, slowly opening the emptying valve 103 after the temperature is reduced to the room temperature, slowly discharging the refrigerant, and opening the high-pressure kettle body 10 after the pressure in the kettle is reduced to the normal pressure.
And 7, taking out the test material and the test oil sample from the autoclave body 10.
Step 8, processing of test materials and test oil samples:
steel sheet: the steel sheets after the test were degreased on the steel sheet surface with petroleum ether, the appearance was observed and the steel sheets were weighed with an analytical balance.
Copper wire: and removing oil stains on the surface of the copper wire by using petroleum ether for the tested copper wire, and observing the appearance and the corrosion condition of the copper wire.
Oil sample: before the tested oil sample is measured, the refrigerant in the sample is removed, then the oil sample is filtered by medium-speed filter paper, the viscosity and the acid value of the oil sample after filtering are measured, and the viscosity change rate of the sample is calculated.
The test results are shown in Table 4.
As can be seen from Table 4, after the complexing agent is added, the viscosity change rate of the tested oil sample B is greatly reduced, the acid value of the oil sample B is reduced, the weight loss of the steel sheet is reduced, and the corrosion of the steel sheet and the copper wire is lightened.
From the color of the test specimens and test pieces, test oil A was brown in color after the test, and the steel and copper wires were black in color after corrosion. The test oil sample B after the complexing agent is added is slightly yellowish, the steel sheet is slightly yellow, the copper wire is bright yellow and slightly corroded, which indicates that the hydrolytic stability of the base oil is greatly improved after the complexing agent is added, and also indicates that the method has very good distinctiveness.
TABLE 4 test results
The test materials (one steel sheet and one copper wire) are put into the autoclave body 10, a proper amount of tested oil sample and a certain proportion of water are added, and the refrigerant is filled after sealing and vacuum. The sealed autoclave was heated to a test temperature and kept under a constant pressure, and the test was carried out for a predetermined time. After the test, the change of the test material and the change of the oil sample are observed, and the change of the steel sheet after the test and the acid value of the oil sample are measured to evaluate the hydrolysis stability of the synthetic ester refrigerator oil under the condition of coexisting refrigerant.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications may be made without departing from the invention, and such modifications are intended to be included within the scope of the invention.
Claims (10)
1. A device for testing hydrolysis performance of lubricating oil in a mixed state with a refrigerant is characterized by comprising:
the high-pressure kettle body is used for placing a test oil sample, a metal test material and a refrigerant;
the temperature controller is connected with the high-pressure kettle body and used for measuring the temperature of the high-pressure kettle body;
the constant temperature sleeve is sleeved on the outer surface of the high-pressure kettle body and is used for maintaining the high-pressure kettle body within a constant temperature;
the refrigerating device is connected with the high-pressure kettle body and is used for providing the refrigerant;
the vacuumizing device is connected with the high-pressure kettle body and is used for vacuumizing the high-pressure kettle body;
and the pressure measuring device is connected with the high-pressure kettle body and used for measuring the pressure in the high-pressure kettle body.
2. The apparatus for testing hydrolysis performance of lubricating oil in a mixed state with refrigerant according to claim 1, wherein the refrigerating apparatus is a refrigerant tank having a high pressure, and the refrigerating apparatus is connected to the autoclave body through a refrigerant delivery line provided with a refrigerant valve.
3. The device for testing the hydrolysis performance of the lubricating oil in the mixed state with the refrigerant according to claim 1, wherein the pressure measuring device comprises a pressure gauge and a pressure sensor connected with the pressure gauge, and the pressure sensor is connected with the autoclave body.
4. The apparatus for testing hydrolysis performance of lubricating oil and refrigerant in a mixed state as claimed in claim 1, wherein said temperature controller is further provided with a thermistor temperature probe, said thermistor temperature probe being connected to said autoclave body.
5. The apparatus for testing hydrolysis performance of lubricating oil in a mixed state with refrigerant according to claim 1, wherein the evacuation means includes a vacuum pump and a vacuum valve, and the vacuum pump is connected to the autoclave body through a vacuum line provided with the vacuum valve.
6. The apparatus for testing hydrolysis performance of a mixture of lubricant oil and refrigerant according to claim 2, wherein the vacuum line and the refrigerant delivery line are combined into a main line near the autoclave body, the main line is provided with the pressure gauge, the pressure sensor, the pressure safety valve, the blow-down valve and the stop valve, and the main line is communicated with the autoclave body.
7. The apparatus for testing hydrolysis performance in a state where lubricating oil is mixed with a refrigerant according to claim 2, wherein the metallic test material is a steel sheet and/or a copper wire.
8. A method for testing hydrolysis performance of lubricating oil and refrigerant in a mixed state is characterized by comprising the following steps:
step S1, grinding the surface of the metal test material and removing free particles on the surface;
step S2, putting the metal test material, the test oil sample and the water processed in the step S1 into an autoclave body to enable the water-oil ratio to reach a preset water-oil ratio, and covering a kettle cover;
step S3, vacuumizing the autoclave body, closing the vacuum pump when the vacuum degree in the autoclave body reaches a preset value, and injecting a refrigerant into the autoclave body while recording the weight of the refrigerant injected into the autoclave body;
step S4, heating the autoclave body to enable the temperature in the autoclave body to reach a preset temperature value and enable the system pressure in the autoclave body to reach a preset pressure value by adjusting an emptying valve 103 on the autoclave body;
step S5, maintaining the metal test material in the autoclave body for a test time under the preset temperature value, the preset pressure value and the preset water-oil ratio;
step S6, after the pressure in the autoclave body is reduced to normal pressure and the temperature is reduced to room temperature, emptying the refrigerant and taking out the metal test material and the test oil sample;
step S7, processing the metal test material and the test oil sample;
removing oil stains on the surface of a metal test material, and observing the appearance and the corrosion condition of the metal test material;
and removing the refrigerant in the tested oil sample before testing the tested oil sample, filtering the tested oil sample, testing the viscosity and the acid value of the tested oil sample, and calculating the viscosity change rate of the sample.
9. The method for testing hydrolysis performance of lubricating oil mixed with refrigerant according to claim 1, wherein the test material for metal is steel sheet and/or copper wire.
10. The method for testing the hydrolysis performance of the lubricating oil mixed with the refrigerant as claimed in claim 1, wherein the temperature is preset at 175 degrees, the pressure is preset at 2.5MPa, the test time is 336 hours, and the preset water-oil ratio is 1: 1000.
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| CN117368409A (en) * | 2023-09-21 | 2024-01-09 | 广州海关技术中心 | Method and equipment for detecting reliability of sensor of combustible refrigerant |
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