CN108088792B - Intermediate scale sample and preparation method and application thereof - Google Patents
Intermediate scale sample and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 59
- 238000000576 coating method Methods 0.000 claims abstract description 40
- 238000005245 sintering Methods 0.000 claims abstract description 37
- 239000002002 slurry Substances 0.000 claims abstract description 36
- 239000011248 coating agent Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 239000011230 binding agent Substances 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 11
- 239000001110 calcium chloride Substances 0.000 claims abstract description 11
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 11
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 11
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 11
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 11
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 11
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 11
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000012216 screening Methods 0.000 claims abstract description 9
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical group [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims description 9
- 239000002689 soil Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 6
- 230000003373 anti-fouling effect Effects 0.000 claims description 4
- 230000003449 preventive effect Effects 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 238000004523 catalytic cracking Methods 0.000 abstract description 9
- 238000007670 refining Methods 0.000 abstract description 4
- 238000004381 surface treatment Methods 0.000 abstract description 2
- 239000010963 304 stainless steel Substances 0.000 description 10
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 10
- 239000000779 smoke Substances 0.000 description 9
- 239000012153 distilled water Substances 0.000 description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 6
- 239000003546 flue gas Substances 0.000 description 6
- 238000011049 filling Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 229910003470 tongbaite Inorganic materials 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001360 synchronised effect 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
- G01N19/00—Investigating materials by mechanical methods
- G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention belongs to the technical field of surface treatment of catalytic cracking devices in the oil refining industry, and particularly relates to an intermediate scale sample and a preparation method and application thereof. The intermediate scale sample comprises component basic powder and a binder; wherein the basic powder comprises the following components in parts by mass: 0.88 part of calcium chloride, 2.77 parts of ferrous sulfate, 2.81 parts of nickel sulfate and 93.54 parts of MMC-2 catalyst. Mixing calcium chloride, ferrous sulfate, nickel sulfate and an MMC-2 catalyst to obtain basic powder; mixing the basic powder with a binder to obtain blended powder, and then adding water to obtain blended slurry; and sintering the blended slurry at high temperature, and cooling to obtain an intermediate scale sample. The intermediate scale sample prepared by the method disclosed by the invention is easy to scale, has higher cohesive strength, and can be used for preliminary screening of an anti-scale coating.
Description
Technical Field
The invention belongs to the technical field of surface treatment of catalytic cracking devices in the oil refining industry, and particularly relates to an intermediate scale sample and a preparation method and application thereof.
Background
In the oil refining industry, a catalytic cracking flue gas turbine (a smoke machine for short) is a power device which converts the heat energy of high-temperature flue gas into mechanical energy, drives a main fan or a generator to work and realizes energy conversion, the recovery efficiency can reach more than 130%, and the catalytic cracking flue gas turbine has a remarkable energy-saving effect.
The third stage cyclone separator (triple cyclone for short) is one of the key devices of the energy recovery system of the flue gas outlet of the catalytic cracking unit, and the normal use of the smoke machine is directly influenced by the efficiency in the operation process. Abnormal shutdown caused by excessive vibration of a main shaft of a range hood in an industrial operation process is one of common problems, and the root cause is abrasion of blades of the range hood and scaling of a catalyst. In recent years, with the continuous improvement of catalytic cracking process, the scaling problem of the cyclone and the smoke machine caused by the problems of the use of novel catalyst and the quality of raw oil is increasingly prominent, and the long-period operation of an energy recovery system is seriously influenced.
The problem of scaling inside the range hood, particularly scaling on the surfaces of movable blades of the range hood, is more and more serious, the dynamic balance of a rotor is seriously damaged, the range hood is slightly vibrated and stops at an excessive level, and the movable blades collide with the outer edge and are broken. The smoke machine of some oil refineries often stops for several months to remove scale, and cannot be synchronous with the overhaul of the whole equipment, so that the recycling efficiency of high-temperature smoke is reduced due to frequent stoppage of faults, the energy consumption is increased, and sometimes even the unplanned shutdown of the whole device is caused, thereby seriously influencing the economic benefit of enterprises and causing huge economic loss. Therefore, the development of the anti-scaling method for the flue gas turbine is of great significance.
The coating protection is one of the methods for treating the scale of the blades of the three-rotation single tube and the smoke turbine, and the preparation of the scale sample is the research basis for the interaction between the coating and the scale sample. The scale formation of the catalyst on a three-rotation single tube and a flue gas turbine usually takes several months, and the scale shape is irregular. If the regular sample of the scale sample can be prepared, the compatibility research of the coating and the scale sample is facilitated, and the screening of the protective coating is facilitated.
In the aspect of scale sample preparation, static high-temperature sintering experiments are carried out in a high-temperature electric furnace, a heating furnace simulates the working environment in a smoke machine, an equivalent catalyst sample at the inlet of a catalytic device smoke machine is placed on a test piece which is made of the same material as movable blades of the smoke machine, and the sintering experiments are carried out to prepare the scale sample. Hurenbo et al (Hurenbo, white, Zhao jin 32704m. et al. catalytic cracking triple-rotation catalyst fine powder sintering and scaling mechanism [ J ]. Chinese university of Petroleum institute (Nature science edition), 37(4), 2013, 169 and 173. all.) also selected the triple-rotation fine powder of a typical catalytic cracking device as a research object, and carried out roasting experiments on the triple-rotation fine powder at different temperatures, wherein the main components of the catalyst fine powder are alumina and silica. Although the composition is close to that of industrial scale, the above sintering method has disadvantages in that the scale itself is not high in cohesive strength and does not adhere to the base metal.
Disclosure of Invention
In order to overcome the disadvantages and drawbacks of the prior art, it is a primary object of the present invention to provide an intermediate scale sample.
Another object of the present invention is to provide a method for preparing the above intermediate soil sample.
It is a further object of the present invention to provide the use of the above intermediate soil sample.
The purpose of the invention is realized by the following technical scheme:
an intermediate soil sample comprising a component base powder (JCF) and a binder;
the basic powder comprises the following components in parts by mass:
the binder is preferably aluminum dihydrogen phosphate (chemical formula Al (H)2PO4)3)；
The dosage of the aluminum dihydrogen phosphate is preferably 30-50% of the total mass of the binder and the base powder;
the preparation standard of the MMC-2 catalyst is preferably Q/SH 3610236-2015;
the preparation method of the intermediate scale sample comprises the following steps:
(1) mixing calcium chloride, ferrous sulfate, nickel sulfate and an MMC-2 catalyst to obtain basic powder (JCF);
(2) mixing the base powder (JCF) prepared in the step (1) with a binder to obtain a blended powder (GHF), and then adding water to obtain a blended slurry (GHLJ);
(3) sintering the blended slurry prepared in the step (2) at a high temperature, and cooling to obtain an intermediate scale sample;
the water in the step (2) is preferably distilled water;
the amount of water used in step (2) is preferably: the water adding amount of each 100g of the blended powder is 55-65 mL;
the sintering condition in the step (3) is preferably 680-750 ℃, and the temperature is kept for 2-4 h;
the intermediate scale sample is applied to the field of screening of anti-scale coatings;
a method of screening for antifouling coatings comprising the steps of:
(1) mixing calcium chloride, ferrous sulfate, nickel sulfate and an MMC-2 catalyst to obtain basic powder (JCF);
(2) mixing the base powder (JCF) prepared in the step (1) with a binder to obtain a blended powder (GHF), and then adding water to obtain a blended slurry (GHLJ);
(3) coating the blend slurry prepared in the step (2) on a coating sample, sintering at high temperature, and cooling to obtain an intermediate scale sample, wherein if the intermediate scale sample is not bonded with the coating sample, the coating sample has an anti-scaling effect; if the intermediate scale sample is bonded with the coating sample, the coating sample does not have the scale prevention effect;
the water in the step (2) is preferably distilled water;
the amount of water used in step (2) is preferably: the water adding amount of each 100g of the blended powder is 55-65 mL;
the sintering condition in the step (3) is preferably 680-750 ℃, and the temperature is kept for 2-4 h;
the principle of the invention is as follows:
the method comprises the steps of firstly preparing basic powder (JCF for short), enabling the powder to be basically the same as industrial scale sample components after high-temperature sintering, preparing blended powder (GHF for short) by adopting a mode of blending the basic powder (JCF) and aluminum dihydrogen phosphate, adding a proper amount of water to form blended slurry (GHLJ for short), and sintering the blended slurry GHLJ to form an intermediate scale sample. For the coating, if a certain coating is not adhered to an intermediate scale sample with higher viscosity before sintering and higher strength after sintering, the coating can be inferred to be not adhered to industrial scale, namely, the coating has the anti-scaling effect under industrial conditions, and the coating can be further screened by industrial tests at a later stage. The intermediate scale sample can indirectly realize the primary screening of the catalytic cracking unit surface coating material in the oil refining industry under simple sintering conditions.
Compared with the prior art, the invention has the following advantages and effects:
(1) the blended slurry prepared by the invention is easy to form block dirty samples after being sintered, is difficult to break by hands, has high cohesive strength, and improves the condition that basic powder (JCF) is sintered and then is lightly twisted to form powder.
(2) The JCF is not scaled, so that the anti-scaling capability of the coating cannot be judged by the JCF; if a coating X prevents the adhesion of the intermediate scale to its surface, the adhesion of the JCF to the coating is prevented with great probability. And the preliminary screening of the coating can be realized by adopting a middle dirt sample mode.
Drawings
FIG. 1 is a graph showing the appearance and morphology of an intermediate soil sample prepared in example 1.
FIG. 2 is a graph showing the appearance and morphology of an intermediate soil sample prepared in example 2.
FIG. 3 is a graph showing the appearance and appearance of an intermediate soil sample obtained in example 3.
FIG. 4 is a graph showing the appearance and morphology of the scale sample prepared in comparative example 1.
FIG. 5 is a graph showing the appearance and morphology of the scale sample prepared in comparative example 2.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
(1) 0.88g of calcium chloride, 2.77g of ferrous sulfate, 2.81g of nickel sulfate and 93.54g of MMC-2 catalyst (powder preparation standard Q/SH 3610236-2015) are mixed to obtain basic powder (JCF);
(2) mixing 14g of the base powder (JCF) prepared in the step (1) with 6g of binder aluminum dihydrogen phosphate to obtain blended powder (GHF), and then adding 12ml of distilled water to obtain blended slurry (GHLJ-1);
(3) preparing a 304 stainless steel sample with a specification of 50mm multiplied by 50mm, and placing a 304 stainless steel square frame (the outer dimension is 50mm multiplied by 5mm, the inner dimension is 45mm multiplied by 5mm) on the surface of the sample; coating the blending slurry (GHLJ-1) prepared in the step (2) on the surface of a sample, filling the slurry into a square frame, sintering the sample coated with the slurry in a sintering furnace at the sintering temperature of 700 ℃, and preserving heat for 2 hours; and then closing the heat preservation program, and cooling the sample along with the furnace to room temperature to obtain an intermediate scale sample.
As shown in FIG. 1, the intermediate-scale-like product is hard to be broken by an adult and has high strength by itself.
Example 2
(1) 0.88g of calcium chloride, 2.77g of ferrous sulfate, 2.81g of nickel sulfate and 93.54g of MMC-2 catalyst (powder preparation standard Q/SH 3610236-2015) are mixed to obtain basic powder (JCF);
(2) mixing 12g of the base powder (JCF) prepared in the step (1) with 8g of binder aluminum dihydrogen phosphate to obtain blended powder (GHF), and then adding 11ml of distilled water to obtain blended slurry (GHLJ-2);
(3) preparing a 304 stainless steel sample with the specification of 50 multiplied by 5mm, placing a 304 stainless steel square frame (the outer dimension is 50 multiplied by 50mm multiplied by 5mm, the inner dimension is 45 multiplied by 45mm multiplied by 5mm) on the surface of the sample, coating the blended slurry (GHLJ-2) prepared in the step (2) on the surface of the sample, filling the square frame with the slurry, placing the sample coated with the slurry in a sintering furnace for sintering, wherein the sintering temperature is 750 ℃, and preserving heat for 4 hours; then closing the heat preservation program, and cooling the sample to room temperature along with the furnace to obtain an intermediate scale sample;
as shown in FIG. 2, the blended slurry forms a lump-like intermediate scale after sintering, which is difficult to be broken by both hands of an adult and has high strength.
Example 3
(1) 0.88g of calcium chloride, 2.77g of ferrous sulfate, 2.81g of nickel sulfate and 93.54g of MMC-2 catalyst (powder preparation standard Q/SH 3610236-2015) are mixed to obtain basic powder (JCF);
(2) mixing 10g of the base powder (JCF) prepared in the step (1) with 10g of binder aluminum dihydrogen phosphate to obtain blended powder (GHF), and then adding 13ml of distilled water to obtain blended slurry (GHLJ-3);
(3) preparing a 304 stainless steel sample with a specification of 50 x 5mm, the surface of which is sprayed with a NiCr-Cr3C2 coating, placing a 304 stainless steel square box (the outer dimension of which is 50mm x 5mm, the inner dimension of which is 45mm x 5mm) on the surface of the coating sample, coating the mixed slurry (GHLJ-3) prepared in the step (2) on the surface of the NiCr-Cr3C2 coating sample, filling the square box with the slurry, placing the coating sample coated with the slurry in a sintering furnace for sintering, wherein the sintering temperature is 680 ℃, and keeping the temperature for 3 h; then closing the heat preservation program, and cooling the sample to room temperature along with the furnace to obtain an intermediate scale sample;
as shown in fig. 3, the blended slurry forms a lump-like intermediate scale sample after sintering, the scale sample is firmly adhered to the metal frame and is difficult to remove, and the scale sample is difficult to be broken off by hands of adults and has high strength. After testing, the intermediate scale sample was found to adhere to the NiCr-Cr3C2 coating, indicating that the NiCr-Cr3C2 coating was not scale inhibiting, which is consistent with the situation in an industrial range hood.
Comparative example 1
(1) 0.88g of calcium chloride, 2.77g of ferrous sulfate, 2.81g of nickel sulfate and 93.54g of MMC-2 catalyst (powder preparation standard Q/SH 3610236-2015) are mixed to obtain basic powder (JCF);
(2) adding 12ml of distilled water into 20g of the base powder (JCF) prepared in the step (1) to form slurry (LJ-0);
(3) preparing a 304 stainless steel sample with the specification of 50 multiplied by 5mm, placing a 304 stainless steel square frame (the outer dimension is 50 multiplied by 50mm multiplied by 5mm, the inner dimension is 45 multiplied by 45mm multiplied by 5mm) on the surface of the sample, coating the slurry (LJ-0) prepared in the step (2) on the surface of the sample, filling the square frame with the slurry, placing the sample coated with the slurry in a sintering furnace for sintering, wherein the sintering temperature is 700 ℃, and preserving heat for 4 hours; and then closing the heat preservation program, and cooling the sample to room temperature along with the furnace.
As shown in FIG. 4, the slurry was sintered to a loose powder, not to a scale-like mass, having a powder composition as shown in Table 1, similar to the composition of a scale sample from the cigarette-making industry (see Table 2).
TABLE 1X-ray spectral composition of basic powder (JCF) after sintering at 700 deg.C
TABLE 2X-ray spectral composition of industrial scale samples
Comparative example 2
(1) 0.88g of calcium chloride, 2.77g of ferrous sulfate, 2.81g of nickel sulfate and 93.54g of MMC-2 catalyst (powder preparation standard Q/SH 3610236-2015) are mixed to obtain basic powder (JCF);
(2) blending 18g of the base powder (JCF) prepared in the step (1) with 2g of binder aluminum dihydrogen phosphate to prepare blended powder (GHF), and then adding 12ml of distilled water to obtain blended slurry (GHLJ-4);
(3) preparing a 304 stainless steel sample with a specification of 50mm multiplied by 5mm, placing a 304 stainless steel square frame (the outer dimension is 50mm multiplied by 5mm, the inner dimension is 45mm multiplied by 5mm) on the surface of the sample, coating the prepared blended slurry (GHLJ-4) on the surface of the sample, and filling the square frame with the slurry; placing the sample coated with the slurry into a sintering furnace for sintering, wherein the sintering temperature is 720 ℃, and preserving heat for 4 hours; and then closing the heat preservation program, and cooling the sample to room temperature along with the furnace.
As shown in fig. 5, the blended slurry was a loose powder after sintering, not a scale-like mass.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. An intermediate scale sample is characterized by being prepared from raw material components of basic powder and a binder;
the basic powder comprises the following components in parts by mass:
the binder is aluminum dihydrogen phosphate;
the using amount of the aluminum dihydrogen phosphate is 30-50% of the total mass of the binder and the base powder.
2. An intermediate scale sample as defined in claim 1, wherein:
the preparation standard of the MMC-2 catalyst is Q/SH 3610236-2015.
3. The method for preparing an intermediate scale sample according to any one of claims 1 to 2, comprising the steps of:
(1) mixing calcium chloride, ferrous sulfate, nickel sulfate and an MMC-2 catalyst to obtain basic powder;
(2) mixing the base powder prepared in the step (1) with a binder to obtain blended powder, and then adding water to obtain blended slurry;
(3) and (3) sintering the blended slurry prepared in the step (2) at a high temperature, and cooling to obtain an intermediate scale sample.
4. A method for preparing an intermediate soil sample according to claim 3, wherein:
the water consumption in the step (2) is as follows: the water adding amount of each 100g of the blended powder is 55-65 mL.
5. A method for preparing an intermediate soil sample according to claim 3, wherein:
and (4) sintering at 680-750 ℃ for 2-4 h.
6. Use of an intermediate scale sample according to any one of claims 1 to 2 in the field of screening of anti-fouling coatings.
7. A method of screening for anti-fouling coatings, characterized by comprising the steps of:
(1) mixing calcium chloride, ferrous sulfate, nickel sulfate and an MMC-2 catalyst to obtain basic powder;
(2) mixing the base powder prepared in the step (1) with a binder to obtain blended powder, and then adding water to obtain blended slurry;
(3) coating the blend slurry prepared in the step (2) on a coating sample, sintering at high temperature, and cooling to obtain an intermediate scale sample, wherein if the intermediate scale sample is not bonded with the coating sample, the coating sample has an anti-scaling effect; if the intermediate scale sample is adhered to the coated sample, it indicates that the coated sample has no scale preventive effect.
8. A method of screening for anti-fouling coatings according to claim 7, characterized in that:
and (4) sintering at 680-750 ℃ for 2-4 h.
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| JP6760019B2 (en) * | 2015-12-17 | 2020-09-23 | 住友金属鉱山株式会社 | Sample preparation method for X-ray fluorescence analysis |
| CN106906437B (en) * | 2017-02-24 | 2019-06-28 | 中国船舶重工集团公司第七二五研究所 | A kind of turbine blade high corrosion resistant scale prevention coating and its preparation process |
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