CN114628143A - Preparation method of low-volatility high-temperature-resistant magnetic fluid - Google Patents
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- CN114628143A CN114628143A CN202210358370.7A CN202210358370A CN114628143A CN 114628143 A CN114628143 A CN 114628143A CN 202210358370 A CN202210358370 A CN 202210358370A CN 114628143 A CN114628143 A CN 114628143A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16J—PISTONS; CYLINDERS; SEALINGS
- F16J15/00—Sealings
- F16J15/16—Sealings between relatively-moving surfaces
- F16J15/40—Sealings between relatively-moving surfaces by means of fluid
- F16J15/43—Sealings between relatively-moving surfaces by means of fluid kept in sealing position by magnetic force
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/44—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
- H01F1/445—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids the magnetic component being a compound, e.g. Fe3O4
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Abstract
A preparation method of low-volatility high-temperature-resistant magnetic fluid belongs to the technical field of magnetic fluid preparation. The method comprises the following steps: adding iron acetylacetonate and manganese acetylacetonate into an oleic acid solution, stirring and heating to obtain a reaction solution I; adding an ester solvent into the reaction solution I, stirring and heating to obtain a reaction solution II; putting the reaction solution II into a three-mouth bottle, introducing inert gas, stirring, heating and cooling to room temperature to obtain a reaction solution III; and adding high-temperature-resistant carrier liquid into the reaction solution III, introducing inert gas, stirring, heating, completely evaporating ester solvents, and cooling to room temperature to obtain the low-volatility high-temperature-resistant magnetic fluid. The magnetic powder in the magnetic fluid is MnFe2O4The particle size is 5 to 50nm, and the magnetic saturation intensity is 50 to 500 GS. The magnetic saturation intensity is controlled by the content of magnetic powder, and the magnetic fluid is inThe volatilization loss is less than 1 percent at 250 ℃ for 60 min.
Description
Technical Field
The invention belongs to the technical field of magnetic fluid preparation, and particularly relates to a preparation method of a low-volatility high-temperature-resistant magnetic fluid.
Background
The magnetic fluid sealing element is composed of magnetic conductive stainless steel, permanent magnet, magnetic fluid, bearing and other main components. Compared with the traditional O-shaped ring seal, the O-shaped ring seal has the advantages of small torque, difficulty in abrasion, long replacement period and the like, and is widely applied to numerous high-end equipment. The longer the replacement cycle of the magnetic fluid sealing component is, the more beneficial the application, wherein the magnetic conductive stainless steel, the permanent magnet and the bearing have longer service life than the magnetic fluid, the main factor influencing the service life of the magnetic fluid is the volatilization rate, and the replacement cycle of the sealing component is prolonged in order to reduce the volatilization rate of the magnetic fluid. If the low-volatility high-temperature-resistant magnetic fluid can be prepared, inconvenience caused by water circulation is avoided, and meanwhile, the replacement frequency of a common magnetic fluid sealing element can be prolonged, so that the application field is widened, and the preparation of the low-volatility magnetic fluid becomes a research hotspot.
The earliest magnetic fluids were kerosene, oleic acid and Fe3O4Composed of a magnetic material and a magnetic material, and is successfully applied to a dynamic sealing part, and Chinese patent application No. 201710017819.2 discloses a preparation method of kerosene-based magnetic liquid and an oleic acid coated nano Fe3O4The kerosene-based magnetic fluid is prepared by dispersing the kerosene-based magnetic fluid in the preparation method of the kerosene-based magnetic fluid (application No. 201410290825.1), and the magnetic fluid with good dispersibility can be prepared by a simple method due to the low specific gravity, good compatibility and the like of the kerosene. But the kerosene is difficult to popularize and apply due to the low flash point, the high volatilization rate and the like of the kerosene.
In order to improve the high temperature resistance of magnetic fluid, high flash point and low evaporation rate carrier liquid is used, Chinese patent ' preparation method of turbine oil-based magnetic fluid ' (application number: 201610160151.2) and Shuoshi's article ' preparation of engine oil-based magnetic fluid and thermo-magnetic property research ' (Jinhaoning, Shenyang industrial university, 2015) use turbine oil and engine oil as carrier liquid to prepare magnetic fluid, the volatility of which is higher than that of kerosene, but the requirements of long service life cannot be met due to the low flow point, poor oxidation resistance and the like of mineral oil, so that suitable carrier liquid is searched from synthetic oil to prepare magnetic fluid.
The magnetic fluid prepared by taking ester-based lubricating oil as carrier fluid is a main product in the current dynamic sealing application because of good high-low temperature performance and longer service life than mineral oil-based magnetic fluid. Articles "preparation and performance analysis of ester-based magnetic fluid" (chemical engineer, 2008, 8), "influence of preparation and heating time of diester-based magnetic fluid on magnetic fluid performance" (chemical engineer, 2014(6)), and Master thesis "diester-based nano Fe3O4The preparation and performance research of the magnetofluid (Zhangwei, university of inner Mongolia science and technology, 2013) successfully prepares the ester-based magnetic fluid, particularly prepares the tetra-ester-based magnetic fluid with the flash point of 265 ℃, and greatly prolongs the service life. But also can not reach the strict requirement of ultra-high service life in the application of high-temperature non-circulating cooling environment.
In order to further improve the service life of the magnetic liquid, a high polymer material is used as a carrier liquid of the magnetic liquid, a polyalkyl-based magnetic fluid is prepared in an article "preparation of hydrocarbon-based magnetic fluid" (proceedings of university of great ligature, 2008 and 6), a high polymer chain silicone oil-based magnetic fluid is prepared in an article "preparation of silicone oil-based magnetic fluid" (proceedings of xu zhou architecture occupational technology academy, 2003 and 6), and a magnetic fluid is prepared by using polyfluoroether oil as the carrier liquid in a Chinese patent "a fluorine-containing oil-based magnetic fluid and a preparation method thereof" (application number: 201410257749.4) and a U.S. Pat. No. 3, 5,785,882, and the evaporation rate of the high polymer material is greatly reduced along with the increase of molecular weight. However, the polymer material has a high viscosity with an increase in molecular weight, and therefore, not only is it difficult to disperse the magnetic powder, but also the polymer material is liable to undergo chain scission at high temperature to cause aging and cracking, and particularly the high activity of the nano magnetic powder accelerates the aging of the polymer material, and the evaporation rate is low but the life is short.
In summary, in the field of high-temperature dynamic sealing without water circulation cooling, such as single crystal furnaces, low-volatility high-temperature-resistant magnetic fluid is required to ensure the service life of the high-temperature-resistant magnetic fluid.
Disclosure of Invention
The invention aims to solve the problem of preparation of low-volatility high-temperature-resistant magnetic fluid, and provides a preparation method of low-volatility high-temperature-resistant magnetic fluid for dynamic seal, which utilizes MnFe prepared by a thermal decomposition method2O4The magnetic fluid is dispersed in a carrier liquid with the flash point higher than 280 ℃ to obtain the low-volatility high-temperature-resistant magnetic fluid, thereby meeting the application problem of the high-temperature field of the dynamic seal of the magnetic fluid.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a low-volatility high-temperature-resistant magnetic fluid comprises the following steps:
adding iron acetylacetonate and manganese acetylacetonate into an oleic acid solution, stirring and heating to obtain a reaction solution I;
adding an ester solvent into the reaction solution I, stirring and heating to obtain a reaction solution II;
step three, putting the reaction solution II into a three-mouth bottle, introducing inert gas, stirring, heating and cooling to room temperature to obtain a reaction solution III;
and step four, adding high-temperature-resistant carrier liquid into the reaction solution III, introducing inert gas, stirring, heating, completely evaporating ester solvents, and cooling to room temperature to obtain the low-volatility high-temperature-resistant magnetic fluid.
The magnetic powder in the magnetic fluid is MnFe2O4The particle size is 5 to 50nm, and the magnetic saturation intensity is 50 to 500 GS. The magnetic saturation intensity is controlled by the content of magnetic powder, and the volatilization loss of the magnetic fluid is less than 1 percent at 250 ℃ for 60 min.
Further, in the first step, the molar ratio of the iron acetylacetonate to the manganese acetylacetonate is 2: 1; the weight ratio of the mixture of ferric acetylacetonate and manganese acetylacetonate to oleic acid is 1: 5-10; the concentration of the oleic acid solution was 85 vol.%.
Further, in the first step, the stirring speed is 50 r/min-500 r/min; the heating temperature is 100-150 ℃, and the time is 10-100 min.
Further, in the second step, the ester solvent is one or more of ethyl oleate, butyl oleate, isooctyl oleate, lauryl oleate and butyl laurate; the volume ratio of the reaction solution I to the ester solvent is 1:1 to 20.
Further, in the second step, the stirring speed is 50 r/min-500 r/min; the heating temperature is 50-80 ℃, and the time is 10-100 min.
Further, in the third step, the inert gas is nitrogen or argon; the flow rate of the inert gas is 0.1-10L/min.
Further, in the third step, the stirring speed is 50r/min to 1000 r/min; the heating temperature is 180-400 ℃, the time is 10-100 min, and the heating rate is 1-20 ℃/min.
Further, in the fourth step, the high-temperature resistant carrier liquid is one or more of glycerol trioleate, trimellitate and dipentaerythritol tetraoleate; the volume ratio of the reaction solution III to the high-temperature-resistant carrier liquid is 1: 0.1-20.
Further, in the fourth step, the inert gas used in the reaction solution III is argon or nitrogen; the flow rate of the inert gas is 0.1-10L/min.
Further, in the fourth step, the stirring speed is 100r/min to 1000 r/min; the heating temperature is 150-400 ℃, the time is 10-100 min, and the heating rate is 1-20 ℃/min.
The invention prepares ester solvent MnFe2O4Dispersing MnFe by transferring2O4The magnetic fluid with low volatility is obtained by dispersing the magnetic fluid into high-temperature resistant ester carrier liquid, and can be used in sealing devices under high temperature and no cooling conditions. The magnetic fluid has the following characteristics:
(1) the invention uses manganese element to replace all ferrous iron in the spar structure, obtains nanometer magnetic powder with better oxidation resistance and more easily controlled size, and has the advantages of MnFe2O4High-temperature stability is good, and the reaction is easy to control.
(2) The invention uses ester solvent as reaction liquid and ester lubricating oil as magnetic fluid carrier liquid, and prepares MnFe in organic ester solution by decomposition method2O4The surface of the nano-particles is provided with ester surfactant load, and the nano-particles have good dispersion stability and no precipitation in high-temperature resistant ester carrier liquid.
(3) The magnetic fluid is prepared by a high-temperature reflux method, and the method has the advantages that low-volatility substances are removed by distillation, and the low volatility of a final product of the magnetic fluid is powerfully guaranteed.
(4) The method transfers the uniformly dispersed magnetic powder from the low-volatility solvent to the high-temperature-resistant carrier liquid by a dispersion transfer method, and has the advantage of avoiding the phenomena of nonuniform dispersion, agglomeration and the like caused by factors such as viscosity, surface tension and the like when the magnetic powder is directly dispersed to the high-temperature-resistant carrier liquid.
(5) MnFe by production2O4The dispersion liquid is added into the carrier liquid to prepare the magnetic fluid, the generation and growth processes of the prepared magnetic powder crystal nucleus directly occur in the ester solvent, and the generated magnetic powder can be directly dispersed in the liquid.
(6) All the raw materials for preparation are organic matters or organic metals, and the method has the advantage of avoiding the defect of poor magnetic powder dispersibility caused by rejection caused by trace immiscible elements.
Drawings
FIG. 1 is a XRD diffractogram of magnetic powder prepared in example 1;
FIG. 2 shows MnFe prepared in example 12O4A magnetic powder TEM diffraction pattern;
FIG. 3 is a graph showing the specific saturation magnetization of the magnetic powder prepared in example 1;
FIG. 4 is a graph of the evaporation loss rate of the magnetic fluid prepared in example 1 for 60min at different temperatures.
Detailed Description
The technical solution of the present invention is further described below with reference to the embodiments and the drawings, but the present invention is not limited thereto, and any modification or equivalent replacement of the technical solution of the present invention without departing from the spirit of the technical solution of the present invention shall be covered within the protection scope of the present invention.
Example 1:
a preparation method of 400GS high saturation magnetization magnetic fluid for dynamic sealing is completed according to the following steps:
firstly, adding iron acetylacetonate and manganese acetylacetonate into an oleic acid solution according to a certain molar ratio, and stirring and heating for a certain time to obtain a reaction solution I;
the molar ratio of the ferric acetylacetonate to the manganese acetylacetonate is 2: 1; the weight ratio of the mixture of the ferric acetylacetonate and the manganese acetylacetonate to the oleic acid is 1: 5; the stirring speed is 200 r/min; the heating temperature is 110 ℃; the heating time is 45 min;
secondly, adding a certain amount of ester solvent into the reaction solution I, and stirring and heating for a certain time to obtain a reaction solution II.
The ester solvent is butyl oleate; the volume ratio of the reaction solution I to the ester solvent is 1: 8; the stirring speed is 400 r/min; the heating temperature is 65 ℃; the heating time is 40 min;
and thirdly, putting the reaction solution II into a three-mouth bottle, introducing inert gas, stirring, heating for a certain time, and cooling to room temperature to obtain a reaction solution III.
The inert gas used in the reaction solution II is nitrogen; the flow rate of the inert gas is 0.4L/min; the stirring speed is 600 r/min; the heating temperature is 240 ℃; the heating rate is 10 ℃/min; the heating time is 30 min;
and fourthly, adding high-temperature-resistant carrier liquid into the reaction solution III, introducing inert gas, stirring, heating for a certain time, completely evaporating ester solvents, and then cooling to room temperature to obtain the high-temperature-resistant magnetic fluid.
The high-temperature resistant carrier liquid is dipentaerythritol tetraoleate. The volume ratio of the reaction solution III to the high-temperature-resistant carrier liquid is 1: 0.15; the inert gas used in the reaction solution II is argon; the flow rate of the inert gas is 0.5L/min; the stirring speed is 700 r/min; the above-mentionedThe heating temperature is 280 ℃; the heating rate is 10 ℃/min; the heating time is 120 min; the magnetic powder in the magnetic fluid is MnFe2O4The particle size is 10 nm; the magnetic saturation intensity in the magnetic fluid was 400 GS.
As can be seen from fig. 1, the magnetic powder has diffraction peaks at 30.3 °, 35.5 °, 43.2 °, 57.1 °, and 62.8 °, corresponding to the crystal planes (220), (311), (400), (511), and 440) of the spinel-type ferrite, respectively, and the product was confirmed to be manganese ferrite. As can be seen from FIG. 2, the magnetic powder is spheroidal, the size is about 20nm, the size is relatively uniform, and the crystallinity is good. Consistent with the XRD analysis structure. As can be seen from fig. 3, the magnetic powder prepared in example 1 has a saturation magnetization of 64emu/g under 20000Oe magnetic field, and has zero coercive force and remanence, and exhibits superparamagnetism, which is advantageous for preparing magnetic fluid and is not magnetized under magnetic field conditions for a long period of time. It can be seen from fig. 4 that the evaporation loss becomes larger as the temperature rises. But tend to be smaller values, with evaporation losses of only 0.015% at 100 ℃ for 60min and 0.9% at 250 ℃. This is because the evaporation loss of the carrier liquid itself is small and it is prepared by stirring at a high temperature under the protection of an inert gas, and therefore the low-volatility impurities are all removed, and therefore this small evaporation loss can ensure a long life even under the anhydrous circulation cooling condition.
Example 2:
a preparation method of a 350GS high saturation magnetization magnetic fluid for dynamic sealing is completed according to the following steps:
firstly, adding iron acetylacetonate and manganese acetylacetonate into an oleic acid solution according to a certain molar ratio, and stirring and heating for a certain time to obtain a reaction solution I.
The molar ratio of the ferric acetylacetonate to the manganese acetylacetonate is 2: 1; the weight ratio of the mixture of the ferric acetylacetonate and the manganese acetylacetonate to the oleic acid is 1: 8; the stirring speed is 300 r/min; the heating temperature is 105 ℃; the heating time is 40 min;
secondly, adding a certain amount of ester solvent into the reaction solution I, and stirring and heating for a certain time to obtain a reaction solution II.
The ester solvent is ethyl oleate; the volume ratio of the reaction solution I to the ester solvent is as follows: 1: 10; the stirring speed is 300 r/min; the heating temperature is 60 ℃; the heating time is 30 min;
and thirdly, putting the reaction solution II into a three-mouth bottle, introducing inert gas, stirring, heating for a certain time, and cooling to room temperature to obtain a reaction solution III.
The inert gas used in the reaction solution II is nitrogen; the flow rate of the inert gas is 0.3L/min; the stirring speed is 600 r/min; the heating temperature is 220 ℃; the heating rate is 10 ℃/min;
and fourthly, adding a high-temperature-resistant carrier liquid into the reaction solution III, introducing inert gas, stirring, heating for a certain time, completely evaporating ester solvents, and cooling to room temperature to obtain the high-temperature-resistant magnetic fluid.
The high-temperature resistant carrier liquid is glycerol trioleate; the volume ratio of the reaction solution III to the high-temperature-resistant carrier liquid is 1: 0.25; the inert gas used in the reaction solution II is argon; the flow rate of the inert gas is 0.3L/min; the stirring speed is 1000 r/min; the heating temperature is 300 ℃; the heating rate is 12 ℃/min; the heating time is 60 min; the magnetic powder in the magnetic fluid is MnFe2O4The particle size is 10 nm; the magnetic saturation intensity in the magnetic fluid is 350 GS. The evaporation loss at 100 ℃ for 60min is only 0.017% and at 250 ℃ 0.95%. This is because the evaporation loss of the carrier liquid itself is small and it is prepared by stirring at a high temperature under the protection of an inert gas, and therefore the low-volatility impurities are all removed, and therefore this small evaporation loss can ensure a long life even under the cooling condition without water circulation.
Claims (10)
1. A preparation method of low-volatility high-temperature-resistant magnetic fluid is characterized by comprising the following steps: the method comprises the following steps:
adding iron acetylacetonate and manganese acetylacetonate into an oleic acid solution, stirring and heating to obtain a reaction solution I;
adding an ester solvent into the reaction solution I, stirring and heating to obtain a reaction solution II;
step three, putting the reaction solution II into a three-mouth bottle, introducing inert gas, stirring, heating and cooling to room temperature to obtain a reaction solution III;
and step four, adding high-temperature-resistant carrier liquid into the reaction solution III, introducing inert gas, stirring, heating, completely evaporating ester solvents, and cooling to room temperature to obtain the low-volatility high-temperature-resistant magnetic fluid.
2. The method for preparing a low-volatility high-temperature-resistant magnetic fluid according to claim 1, wherein the method comprises the following steps: in the first step, the molar ratio of the iron acetylacetonate to the manganese acetylacetonate is 2: 1; the weight ratio of the mixture of ferric acetylacetonate and manganese acetylacetonate to oleic acid is 1: 5-10; the concentration of the oleic acid solution was 85 vol.%.
3. A method for preparing a low-volatility high-temperature-resistant magnetic fluid according to claim 1 or 2, wherein the method comprises the following steps: in the first step, the stirring speed is 50 r/min-500 r/min; the heating temperature is 100-150 ℃, and the time is 10-100 min.
4. The method for preparing a low-volatility high-temperature-resistant magnetic fluid according to claim 1, wherein the method comprises the following steps: in the second step, the ester solvent is one or more of ethyl oleate, butyl oleate, isooctyl oleate, lauryl oleate and butyl laurate; the volume ratio of the reaction solution I to the ester solvent is 1:1 to 20.
5. The method for preparing a low-volatility high-temperature-resistant magnetic fluid according to claim 1 or 4, wherein the method comprises the following steps: in the second step, the stirring speed is 50 r/min-500 r/min; the heating temperature is 50-80 ℃, and the time is 10-100 min.
6. The method for preparing a low-volatility high-temperature-resistant magnetic fluid according to claim 1, wherein the method comprises the following steps: in the third step, the inert gas is nitrogen or argon; the flow rate of the inert gas is 0.1-10L/min.
7. The method for preparing a low-volatility high-temperature-resistant magnetic fluid according to claim 1 or 6, wherein the method comprises the following steps: in the third step, the stirring speed is 50r/min to 1000 r/min; the heating temperature is 180-400 ℃, the time is 10-100 min, and the heating rate is 1-20 ℃/min.
8. The method for preparing a low-volatility high-temperature-resistant magnetic fluid according to claim 1, wherein the method comprises the following steps: in the fourth step, the high-temperature resistant carrier liquid is one or more of glycerol trioleate, trimellitate and dipentaerythritol tetraoleate; the volume ratio of the reaction solution III to the high-temperature-resistant carrier liquid is 1: 0.1-20.
9. The method for preparing a low-volatility high-temperature-resistant magnetic fluid according to claim 1, wherein the method comprises the following steps: in the fourth step, the inert gas used in the reaction solution III is argon or nitrogen; the flow rate of the inert gas is 0.1-10L/min.
10. The method for preparing a low-volatility high-temperature-resistant magnetic fluid according to claim 1, wherein the method comprises the following steps: in the fourth step, the stirring speed is 100r/min to 1000 r/min; the heating temperature is 150-400 ℃, the time is 10-100 min, and the heating rate is 1-20 ℃/min.
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