JPS58162865A - Method and apparatus for estimating organic compound fluid - Google Patents

Abstract

PURPOSE:To estimate oxidation life of a sample accurately and rapidly, by compulsorily deteriorating the whole sample of a liquid org. compd. circulated in a thin film. CONSTITUTION:A circulation pump 21 is actuated to draw a sample 13 from a storage tank 10 through a tube 18 and feed it to a sample introduction part 5. The sample 13 is fed to the upper part of the conical large-diameter part 2A of a funnel 2, flows down along the external peripheral surface of the part 2A, gradually formed into a thinner film, and propagated to the inner cylinder surface 1A of a glass cylinder 1 in a cylindrical thin film 6 having uniform thickness. At that time, the film 6 is deteriorated by heating the sample 13 to a temp. higher than that of it in the tank 10 with a heater 11, and further degraded by bringing it into contact with the atmospheric gas injected from an injection nozzle 8B, and rising with replacing all the gas contained in the cylinder 1. The sample 13 flows down moreover accelerated toward deterioration by contact with a catalyst 30. Oxidation life of the org. liq. compd., etc. can be thus estimated exactly and rapidly.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an evaluation method and an evaluation apparatus for evaluating an organic compound fluid by forcibly degrading the organic compound fluid and measuring the deterioration straight pipe. Improvements in methods of degrading fluids and their 5j! Application device Kl
I do it.

Various methods for evaluating organic compound fluids have been proposed, including those by the Japanese Standards Institute (JIS) and the American Society for Testing and Materials (ASTM). Evaluation methods include the Indiana oxidation test (proposed by Standard Oil-Indiana), the rotary ribbon oxidation stability test (ASTM D 2272), and the Indiana Stirling oxidation test (JIS K 251).
4) Turbine oil oxidation stability test (JIS K 2
515 units) etc. are widely adopted. however,
All of these test methods uniformly heat the entire sample of lubricating oil to forcefully degrade it, and therefore, the samples are not heated above 200°C.

However, the situation with lubricating oil in practice is that it is heated to extremely high temperatures, sometimes reaching 800°C, in moving parts such as bearings and near the surfaces of gears.
The temperature in the storage tank i1 in the first part is relatively low, and the lubricating oil is circulated between the high temperature moving part and the low temperature O storage tank part. Therefore, each of the test methods described above, in which lubricating oil is forcibly degraded under conditions that are extremely different from the conditions in which lubricating oil is actually used, does not necessarily guarantee the proper oxidation life of lubricating oil. It had the disadvantage of not being able to be evaluated. Moreover, the turbine oil oxidation stability test required a test time of over 2,000 to 5,000 hours. Furthermore, in addition to the oxidation life of lubricating oil, there is a need for an evaluation method and apparatus that can appropriately and quickly evaluate organic compound fluids including oils and fats.

An object of the present invention is to provide an evaluation method and evaluation value *' for an organic compound fluid that can appropriately and quickly evaluate the organic compound fluid.

In the evaluation method according to the present invention, an organic compound fluid as a sample is made into a -Wt-thin film, and then introduced into a storage tank, and a part of the sample in the storage tank is taken out and the sample is made into a thin film again. The purpose is to approximate the situation and conditions of the sample actually used and achieve the above objective by accelerating the deterioration of mainly the thin film sample while circulating the sample, thereby forcibly degrading the entire sample.

Furthermore, the evaluation device according to the present invention includes a wall surface that is inclined or oriented in a vertical direction, through which the organic compound fluid as a sample flows down in the form of a thin film, and a thin film generation mechanism that is disposed on the lower side of the wall surface. A storage tank for accommodating one sample that has been washed down and a circulation pump that supplies the sample in the storage tank to the thin film generation mechanism is provided. In the generation mechanism, the above objective is achieved by making the sample into a thin film and accelerating the deterioration.

Embodiments of the present invention will be described below based on the drawings.

FIG. 1 shows the overall configuration of an embodiment of an organic compound fluid evaluation apparatus according to the present invention. In this diagram,
The d-las cylinder/1 made of thick Pyrex glass (trade name) is arranged along the vertical direction and placed at a predetermined position near the upper end of the glass cylinder 1, with the conical large diameter part 2^ side facing vertically downward. A thin film generating mechanism 3 is constituted by the funnel 2 and the funnel 2 which are arranged upside down.

The thin tube part 2B of the funnel 2 is connected to the upper end opening 1 of the glass cylinder 1.
The cap 11 is press-fitted into the center of a column-shaped cap 4 made of Teflon (trade name: Litetrafluoroethylene) resin or the like so as to close this opening, and is held through the center of the cap 4. The cat f4PclI is fixedly supported so that it is not in close contact with the inner circumferential surface of the linear cylinder 1, but is very close to it.

Next, a sample introduction part 5 is bored in the character 7'''4. part 5A and a vertical part 5B that opens at the center of the lower surface of the cap 4, communicates with the front horizontal part 5A, and surrounds the narrow tube part 2B' of the funnel 2 with a predetermined gap. The sample introduced from the horizontal part 5A flows down to the upper end side of the large diameter part 2^ of the funnel 2 through the vertical part 5Btl-, and the next sample after flowing down flows into the conical part of the large diameter part 2A. The sample is flowed down while being made into a thin film, and the sample is transferred in a thin film form to the inner peripheral surface 1A of the glass cylinder 1, which serves as the wall surface on which it flows down, and then a thin film portion is formed along the inner periphery WJIAK 6 and flow down.The inner peripheral surface IAK is provided with a coiled catalyst 30 made of copper, iron, etc., in contact with the inner peripheral surface 1A, and the thin film portion 6 flows down while contacting the catalyst 30.

A heating mechanism T is surrounded by a predetermined range on the outer periphery of the glass cylinder 1 along the longitudinal direction of the glass cylinder 1 . This heating mechanism 7 has a nichrome wire 7A wrapped around the outer periphery and an asbestos ribbon (not shown) covering the nichrome M7A, and the heating mechanism 7 also has a thermocouple (not shown). The temperature of the heating mechanism T is controlled by this thermocouple.

An Fi funnel-shaped connector 8 is attached to the lower end opening of the glass cylinder 1.
is installed. The upper end edge of this connector 8 is brought into close contact with the lower end edge of the glass cylinder 1 via a sliding part 9 to prevent gas leakage, and the connector 8
The narrow tube part 8A is inserted downward through the center of a lid part 11 made of rubber or the like fitted into the opening of a storage tank 10 shaped like a wide-mouthed bottle, and is connected to the inside of the glass cylinder 1 by the p1 connector 8. It is in communication with the inside of the storage tank 10. In addition, the thin tube portion 8A is provided with a side tube 8B, and the side tube 8B is used to store a gas cylinder, and the gas cylinder 12 is provided with an atmosphere containing any gas such as air, oxygen, nitrogen, ammonia, freon, etc. For example, if the sample is actually used in air, air is used, and even if the sample is actually used in air, the oxygen in the air may Oxygen is used when deterioration is a problem, or ammonia or Freon is used when the sample is actually used in an atmosphere of K11l refrigerant. The zero exhaled gas contained in the gas cylinder 12 is introduced into the glass 7 cylinder 1 through the side pipe 8B, and then is discharged to the outside of the glass cylinder 1 through the narrow tube portion 28 of the funnel 2. Note that the atmospheric gas introduced through the side pipe 8B is blown out downward through the downward outlet 8C, and the sample mist is passed through the side pipe 8B.
It is designed to prevent it from getting inside.

A predetermined amount of a sample 13, which is an organic compound fluid such as lubricating oil or fats and oils, is contained in the second type 10, and
The storage tank 10 has a double wall structure with a double wall 15t through which a constant temperature fluid 14 such as cooling water flows, and the sample 13 in the storage tank 10 is maintained at a predetermined temperature by the constant temperature fluid 14. It's K.

A drain 1T with a cock 16 is installed at the bottom of the storage tank 10.
is provided, and serves as a trap so that the sample 13 can be sampled from this drain 17 as appropriate.

Further, a suction pipe 18 is inserted into the sample 13 in the storage tank 10, and the suction pipe 18 is supported by a first branch pipe 19 of the storage tank 10 via a Demu plug 20.

The suction pipe 18 is a circulation bong 7'' located outside the storage tank 10.
21, and the sample 13 in the storage tank 10 is connected to the circulation pump 2.
After being sucked in from the suction pipe 18 by the action of 1, it is branched through the circulation pump 21, and one side is drawn into the storage tank 10 again through the return pipe 23 inserted and held in the lid part 11 via the first regulating valve 22. and the other is sent to the sample introduction section 5 via the second regulating valve 24. moreover,
A stirring rod 27 is introduced into the storage tank 10 through the second branch pipe 25 of the storage tank 10 and the seal portion 26, and the stirring rod 27 is rotated by a motor (not shown) to stir the sample 13 in the storage tank 10.
At the same time, a measuring device 28 is introduced into the sample 13 in the storage tank 10 through the lid part 11 via a stopper 29.

Measuring equipment 2B is an automatic transmittance measuring meter, an automatic absorbance measuring meter, an automatic refractive index measuring needle, and an automatic viscosity measuring meter, each of which is selected as appropriate and is used to measure various properties of the sample 130. can be measured accordingly.

Next, a case will be described in which an organic compound fluid such as lubricating oil is evaluated using the above embodiment of the evaluation apparatus according to the present invention.

A predetermined amount of the sample 13 contained in the storage tank 10 is placed in the double wall 1
A constant temperature fluid 14 such as cooling water is flowed into the chamber 5 at a predetermined temperature, for example, when lubricating oil is used as the sample 13, the temperature is maintained at a predetermined temperature within the range of 30°C to 100°C, using a stirring rod 27. The sample 13 in the storage tank 10 is stirred inside the storage tank 10.
equalize.

Next, the circulation pump 7'21 is activated, and the regulating valve 22 is activated.
．． 24 and transfer the sample 13 in the storage tank 10 to the suction pipe 18.
The sample 13 is circulated at a predetermined circulation speed so that a certain amount of the sample 13 with a predetermined value is supplied to the sample introduction section 5 and the remaining sample 13 is returned into the storage tank 10 through the return pipe 23. Circulate.

The sample 13Fi supplied to the sample introduction part 5 flows down to the upper part of the conical large diameter part 2A of the funnel 20, and after that, the large diameter part 2^
It flows down while becoming a thin film along the outer circumferential surface of the glass cylinder 1, and is transmitted to the inner circumferential surface 1A of the glass cylinder 1 in the form of a thin film having a uniform thickness.

The sample 13 flowing down along the inner circumferential surface 1A becomes a cylindrical thin film [6] with a uniform thickness, and flows down almost the entire length of the inner circumferential surface 1^ in the longitudinal direction. At this time, the thin film portion 6 is heated to a predetermined temperature by a heater 11, for example, if the sample 13 is lubricating oil, the predetermined temperature is within 60°C to 800°C, which is higher than the temperature of the sample 13 in the storage tank 10. While being heated to a high temperature and deteriorating, it is also brought into contact with the atmospheric gas that is blown out from the air outlet and rises while filling the inside of the glass cylinder 1, and is also brought into contact with the catalyst 30, so that these atmospheric gases and the catalyst 30 are It flows down the river, showing its deteriorated condition.

The sample 13 that has flown down from the lower part of the glass cylinder 10 St is dropped into the storage tank 10 through the connection part 8, and the sample 13 returned to the storage tank 10 is cooled to a predetermined temperature and then stirred and homogenized.
be converted into

While the sample 13 is kept agitating so that such a process is constantly repeated, changes in the properties of the sample 13 in the storage tank 10 are measured by the measuring device 28, or alternatively, all sampling is performed from the over-current drain 17. Sample 13 is evaluated by conducting tests such as total wI value, neutralization value, various spectra such as infrared absorption spectrum, and gas analysis.

This embodiment has the following effects.

Sample 13, which is an organic compound fluid such as lubricating oil, is forcibly degraded under FC conditions that approximate the conditions in which it is actually used, and then it becomes possible to properly evaluate sample 13t.

For example, Table 1 listed below shows the evaluation results and rotary ribbon oxidation stability test according to this example using two types of lubricating oils A and B (both containing ZnDTP as an antioxidant) as samples. The evaluation results are shown in comparison with the actual lifespan of an actual machine. Here, the time adopted as the evaluation result in this example is the time until the total acid value of each sample reaches its minimum, and this time is defined as the life of the sample added as an antioxidant. Focusing on the fact that ZnDTP decomposes as it is oxidized, and once it is completely decomposed, the oxidation prevention ability is lost and the total acid value begins to rise, the lifespan of the lubricant should be defined as the time in the trench where ZnDTP is completely decomposed. That's why. In addition, for lubricating oils that do not contain antioxidants, the total acid value increases immediately after measurement, and in this case, the time until the total acid value reaches a constant value (for example, 0.5) can be defined as the life span. .

1st table 1111'j! Machine life span "'pe 7bonp (V-10
It can be used almost continuously in a hydraulic system using 4C111) under lubricated conditions with an oil temperature of 65℃.

12 Examples゛°・Total amount of lubricating oil as sample: 300'
- Circulation rate: 1.1wLV min Heating temperature: 300℃ Storage tank temperature: 140℃ Atmosphere is 1 air (flt amount 5L), catalyst is small, overall length is 3, diameter is 1.6mm Copper coil *30 - Talibump oxidation stable Degree test: Based on ASTM D 2272.

As is clear from Table 1, it is impossible to estimate the life of the lubricating oil in the actual machine using the rotary ribbon oxidation stability test, but according to this example, the life of the lubricating oil in the machine can be estimated. It is possible to estimate it very accurately.

Further, according to this embodiment, the sample 13 is heated in the form of a thin film and brought into contact with the atmosphere and the catalyst 30, so that the forced deterioration progresses in a short period of time. It becomes possible to quickly evaluate sample 13 gold.

For example, Table 2 below lists three types of lubricating oils C, D, and E (all containing Zn D as an antioxidant) as samples.
Contains TP. ) The evaluation results according to this example and the evaluation results according to the Indiana oxidation test are shown for comparison. Here, the time adopted as the evaluation result is the time until the total acid value of each sample reaches its minimum.

Table 2 Hata 4 This example: The heating temperature was 280°C in total, and the conditions were the same as those in Table JIII above, except for 9. *5 Indiana oxidation test: The reaction temperature was 140 t.
: According to the method proposed by Standard Oil-Indiana Company.

As is clear from Table 2, according to this example, there is a correlation with the Indiana oxidation test, and the time required is only about a minute.

In addition, in the above-mentioned embodiment, the glass cylinder 1 and the storage tank 10
Although it is assumed that they are configured separately from each other, they may be configured integrally or continuously.

In addition, the wall surface on which the sample N13 flows down in a thin film form is
Although the inner circumferential surface 1A of the glass cylinder 1 is arranged vertically, as in the other embodiment shown in FIG.
A, and the upper end surface 51A may be inclined at a predetermined angle. That is, in the other embodiment shown in FIG. 2, the heating gray 1-51Fi is a substantially rectangular rectangular parallelepiped that is inclined at a predetermined angle and is flattened in the vertical direction in the figure. It consists of a lower side wall, and a heating mechanism T is attached to the side wall. Further, an atmospheric gas is introduced into the glass chamber 52 through a gas inlet 53, and after the atmospheric gas fills the glass chamber 52, it is led out through a gas outlet 54.

A downstream nozzle 55 is attached to the upper side of the crow chamber 52, and the losing side of the downstream nozzle 55 is flattened to have a narrow slit outlet 55A, as shown in FIG. 9. The sample 13 that is flown down onto the upper end surface 51A from the flow nozzle 55 is formed into a thin film on the upper end surface 51A. In addition, a thin tube-shaped dripping portion 56 is integrally formed at the bottom 11111 of the glass chamber 52, and the sample 13 that has flown down as a thin film portion 6 on the upper end surface 51A is transferred to the dripping portion. 561- and into the storage tank 10. In addition, the heating mentioned above! The rate 51 and the downstream nozzle 55 constitute a thin film generating mechanism 57.

According to the second embodiment shown in the figure, even when the sample 13 has an extremely low viscosity, it can be kept in a thin film form for a relatively long period of time.

Furthermore, the sample 13 flows down in the form of a thin film.
The IWJ may have an outer peripheral surface shape such as a cylinder or a cone.

Furthermore, although the sample 13, which is in the form of a thin film, is supposed to be brought into contact with the atmospheric gas and the catalyst 30, for the purpose of evaluation, one or both of these may not be brought into contact. .

Further, the atmosphere is assumed to be continuously flowed, and an atmospheric gas at a predetermined pressure may be sealed in the glass cylinder 1 or the glass cylinder 52, and in this case, the pressure of the sealed atmospheric gas will drop. The life of the sample 13 may be evaluated by measuring.

As described above, according to the present invention, it is possible to provide an organic compound fluid evaluation method and an evaluation apparatus that can appropriately and quickly evaluate an organic compound fluid.

[Brief explanation of the drawing]

FIG. 1 is a sectional view showing the overall configuration of one embodiment of the organic compound fluid evaluation device according to the present invention, FIG. 2 is a sectional view showing the main parts of another embodiment, and FIG. 3 is similar to FIG. FIG. 2 is an enlarged perspective view showing the shape of a downstream nozzle in one example of the towing embodiment shown in FIG. 1°...Glass cylinder, IA, 51.A...9 inner peripheral surface as a wall surface on which the organic compound fluid flows down, upper end surface,
2... Funnel, 3,57... Thin film generation mechanism, 6...
Thin film part, 7... Heating mechanism, 10... Storage tank, 13°.
- Sample that is an organic compound fluid, 14... Constant temperature fluid, 12... Gas cylinder, 21... Circulation pump, 51
... Heating plate, 55... Downstream nozzle. Agent Patent Attorney Minoru Kinoshita

Claims (1)

[Claims] (1) In an organic compound fluid evaluation method for evaluating an organic compound fluid by forcibly degrading the organic compound fluid as a sample and measuring the degree of deterioration, a part of the sample is After making it into a thin film, it is first introduced into the storage tank, and then a part of the sample in the storage tank is taken out and made into a thin film.While the sample is being circulated, the amount of sample is mainly accelerated, which accelerates the deterioration of the thin film sample. A method for evaluating organic compound fluids characterized by forced deterioration of the body. (2) A method for evaluating an organic compound fluid according to claim S, characterized in that the sample formed into a thin film is heated and the heated sample is cooled in one storage tank. (Conclusion) A method for evaluating an organic compound 'IIR compound according to claim 1 or 2, characterized in that the thin film sample is brought into contact with an atmospheric gas. (4) An organic compound as a sample a thin film generation mechanism having an inclined or vertically oriented wall surface through which the compound fluid flows down in the form of a thin film; a storage tank disposed below the wall surface for accommodating the sample that has flown down; and a circulation pump for supplying the sample to the thin film generation mechanism'f:
Evaluation device for organic compound fluids based on % characteristics.