CN109364845A - Application and a kind of anti-corrosion reaction kettle of the molybdenum disulfide on equipment anticorrosion - Google Patents

Application and a kind of anti-corrosion reaction kettle of the molybdenum disulfide on equipment anticorrosion Download PDF

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Publication number
CN109364845A
CN109364845A CN201811316608.XA CN201811316608A CN109364845A CN 109364845 A CN109364845 A CN 109364845A CN 201811316608 A CN201811316608 A CN 201811316608A CN 109364845 A CN109364845 A CN 109364845A
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China
Prior art keywords
reaction kettle
molybdenum disulfide
wall
time
autoclave body
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CN201811316608.XA
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Chinese (zh)
Inventor
成兰兴
丁为公
赵腾飞
赵增兵
王柏楠
师传兴
赵怡丽
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Luoyang Shen Mo Molybdenum Industry Co Ltd
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Luoyang Shen Mo Molybdenum Industry Co Ltd
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Priority to CN201811316608.XA priority Critical patent/CN109364845A/en
Publication of CN109364845A publication Critical patent/CN109364845A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/02Apparatus characterised by being constructed of material selected for its chemically-resistant properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • B01J19/0066Stirrers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/02Apparatus characterised by their chemically-resistant properties
    • B01J2219/0204Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components
    • B01J2219/0236Metal based

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Accessories For Mixers (AREA)

Abstract

The invention belongs to molybdenum disulfide application and preparation technical fields, and in particular to a kind of application of molybdenum disulfide and molybdenum disulfide remove silicon anti-corrosion type reaction kettle.A kind of anti-corrosion type reaction kettle, including autoclave body and agitating device, the agitating device are vertically arranged in the autoclave body, and anti-corrosion coat is provided on the inner wall of the agitating device and autoclave body, and the anti-corrosion coat is layer of molybdenum-disulfide.The production of the reaction kettle prepared using molybdenum disulfide as inside coating is simple, and manufacturing cost is low, and reaction kettle is wear-resisting, high temperature resistant, hydrofluoric acid corrosion resistance, has good greasy property, and thermal coefficient is high, and heat-transfer effect is good, and low energy consumption, and cleaning is easy, and can be used for a long time.

Description

Application and a kind of anti-corrosion reaction kettle of the molybdenum disulfide on equipment anticorrosion
Technical field
The invention belongs to molybdenum disulfide application and preparation technical fields, and in particular to a kind of application of molybdenum disulfide and two sulphur Change molybdenum and removes silicon anti-corrosion type reaction kettle.
Background technique
Molybdenum disulfide is a kind of black powder with metallic luster, belongs to hexagonal crystal system, it has diamagnetism and half The property of conductor, wherein Mo-S faceted pebble is more, large specific surface area, is covalent bond in layer, is then Van der Waals force between layers, layer with It is easily separated between layer, shows very low coefficient of friction.And because sulphur has very strong adhesive capacity to metal, it can make Molybdenum disulfide is attached to metal surface well, plays lubricating function always, especially under conditions of high temperature, high vacuum, still It can be widely used in as good solid lubricant solid with lower coefficient of friction due to its property Body lubricant industry.
In traditional molybdenum disulfide silicon removing process, general method is added into corrosion resistant ptfe autoclave Enter 50% hydrofluoric acid and molybdenum concentrate, the inner cavity of reaction kettle is made to keep certain temperature by heating reacting kettle jacketing, it is agitated and anti- Siliceous satisfactory molybdenum disulfide powder should be prepared by the process of filtering, washing, drying, crushing after a certain period of time.But There is following points for current traditional handicraft: 1, the heat-transfer effect of corrosion resistant ptfe autoclave is poor, reaction heating Need the time long to certain temperature, energy consumption is high;2, ptfe autoclave intensity is small, and softening point is low, reaction temperature by Certain restrictions, manufacturing cost are high.
Reaction kettle is made of autoclave body, stirring, collet, transmission etc., and traditional reaction kettle has stainless steel cauldron, enamel anti- Kettle is answered, these reaction kettles have certain corrosion resistance, but all bad to the corrosion resistance of hydrofluoric acid, and especially enamel is anti- The operating condition for answering kettle to cannot be used for fluoride ion uses.CN1718562A discloses a kind of anti-for air entrained concrete with protective layer Kettle is answered, is that compound aluminized coating is coated using steel bomb autoclave body inner surface, air entrained concrete reaction is only limitted to and uses; CN101274261 discloses a kind of nanocomposite ceramic reactor, is using steel bomb autoclave body inner surface supersonic flame One layer of nanocomposite ceramic material is sprayed, as high temperature resistant, anti-oxidant, corrosion resistant reaction kettle for petrochemical industry, biology doctor The reactor in the fields such as medicine, but since ceramic material contains silica composition, corrosiveness of the hydrofluoric acid to silica Obviously, it is impossible to be used in the medium of fluoride ion ingredient.How a kind of hydrofluoric acid corrosion resistance, intensity height, high temperature resistant, thermally conductive system are manufactured The reaction kettle that number is big, manufacturing cost is low, is the problem to be solved in the present invention.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of anti-corrosion type reaction kettle, it being capable of effective hydrofluoric acid corrosion resistance.
The technical scheme adopted by the invention is as follows:
Application of the molybdenum disulfide on equipment anticorrosion, molybdenum disulfide are coated on the face of equipment being in contact with corrosive liquid.
A kind of anti-corrosion type reaction kettle, including autoclave body and agitating device, the agitating device are vertically arranged in the autoclave body, And anti-corrosion coat is provided on the inner wall of the agitating device and autoclave body, the anti-corrosion coat is layer of molybdenum-disulfide.
The coat with a thickness of 12-15 microns.
The agitating device is made of agitating shaft with the agitating paddle for being set to the agitating shaft lower end, on agitating shaft and agitating paddle Equipped with anti-corrosion coat.
The preparation method of anti-corrosion type reaction kettle, comprising the following steps: 1) by reaction kettle inner wall of kettle, agitating shaft and agitating paddle Outer wall carries out derusting by sandblasting processing, and reaction kettle inner wall of kettle and agitating paddle outer wall is made to keep cleaning;
2) first time spraying is then carried out, for the first time the process of spraying are as follows: molybdenum disulfide slurry is sprayed into reaction kettle autoclave body It on wall, agitating shaft and agitating paddle outer wall, 4-5 microns of coating layer thickness, dries, reusable heat air dries 10-20h;
3) it then carries out spraying for the second time and third time sprays, the process and first time of spraying for the second time and third time spraying spray Process it is identical, third time spray after complete.
The group of the molybdenum disulfide slurry becomes ultra-fine molybdenum disulfide, adhesive, deionized water, and ultra-fine molybdenum disulfide glues Mixture, deionized water mass ratio be 1:0.2-0.8:1-5.
The granularity of the ultra-fine molybdenum disulfide is 0.8-5 microns, and described adhesive is the polymerization of perfluoro capryl methyl acrylate Object, perfluoro capryl X 4460 or perfluoro capryl sodium acrylate polymer.
The material of the reaction kettle autoclave body is steel.
Drying temperature is 105-150 DEG C in the step 2.
Anti-corrosion type reaction kettle is further preferred:
The autoclave body is fixed on horizontal plane by support, and is set with collet on autoclave body outer wall.
The collet top is provided with water inlet pipe, and collet bottom end side is provided with outlet pipe, described in the collet inner close fitting Autoclave body outer wall is provided with infrared ray heating tube.
The autoclave body top is provided with kettle cover, and a manhole, two mirror mouths and more are circumferentially distributed on the kettle cover A feed opening, described two mirror mouths are symmetrical arranged, and temperature-measuring port, setting in temperature-measuring port are provided on the position at kettle cover edge There is thermometer, which is vertically arranged and protrudes into the autoclave body middle and lower part.
The agitating device is made of agitating shaft with the agitating paddle for being set to the agitating shaft lower end, and the agitating shaft top is worn Out the kettle cover and connect on the drive means.
The driving device includes driving motor, and the driving motor is arranged in the kettle cover top by sealing sleeve pipe The heart, and driving motor output end is arranged downward and is fixedly connected by shaft coupling with the agitating shaft.
In the above-mentioned technical solutions, the autoclave body bottom center is provided with discharge gate.
Compared with prior art, the method have the benefit that:
1, thinking of the invention is ingenious, has changed the thinking that molybdenum disulfide is commonly used to lubricant, attempt using molybdenum disulfide as A kind of anti-corrosion material, using special process molybdenum disulfide is firmly attached to by suitable adhesive compounding needs On the inner wall for wanting corrosion-resistant consersion unit, the inner wall of such consersion unit can high temperature resistant, acid corrosion-resistant, also being capable of hydrogen resistant fluorine The corrosion of acid, while the consersion unit thermal coefficient is high, saves the energy, the service life is long, and manufacturing cost is low.
2, simultaneously as molybdenum disulfide is also good solid lubricant, the inner wall surface of molybdenum disulfide coating simultaneously It is very smooth, it is not easy to the surface attachment reaction material as traditional reaction kettle.
3, molybdenum disulfide has good heating conduction, and heating conduction is similar to graphite, and the material of reaction kettle autoclave body can To use steel, therefore the drawbacks of do not influence the heating speed of consersion unit material, overcome polytetrafluoroethylene material poor heat transfer.
4, using molybdenum disulfide as corrosion-inhibiting coating, when production need adhesive by molybdenum disulfide and special ratios and Special technique is made, and manufacturing process is simple, and manufacturing cost is low, be suitble to promote and apply, selected adhesive be it is aqueous, It is pollution-free, environmental protection.
5, the molybdenum disulfide utilized high stability in a solution of hydrofluoric acid and silica or silicate are soluble in hydrogen fluorine The characteristic of acid, reaction kettle of the invention is highly suitable for remove to molybdenum disulfide the reaction environment of silicon using hydrofluoric acid, at this In reaction kettle, molybdenum disulfide does not dissolve in hydrofluoric acid, and free silica or silicate dissolution remove.In addition to being suitable for curing Molybdenum removes pasc reaction, and the consersion unit with molybdenum disulfide coating applies also for the reaction environments such as other various sours, high temperature, applies Range is wide.
6, the production of the reaction kettle prepared using molybdenum disulfide as inside coating is simple, and manufacturing cost is low, and reaction kettle is resistance to Mill, hydrofluoric acid corrosion resistance, has good greasy property at high temperature resistant, and thermal coefficient is high, and heat-transfer effect is good, and low energy consumption, and cleaning is held Easily, it can be used for a long time.
Detailed description of the invention
Fig. 1 is that the molybdenum disulfide in the present invention removes silicon anti-corrosion type reaction kettle;
Fig. 2 is kettle cover structural schematic diagram of the present invention.
Specific embodiment
Illustrate a specific embodiment of the invention below with reference to embodiment, but following embodiment is used only to be described in detail The present invention does not limit the scope of the invention in any way.
Embodiment 1: a kind of molybdenum disulfide removes silicon anti-corrosion type reaction kettle, as depicted in figs. 1 and 2, including reaction kettle autoclave body And mixing plant, including autoclave body 4 and agitating device 7, agitating device 7 be vertically arranged in autoclave body 4, to be carried out to reaction mass It stirs, is provided with anti-corrosion coat 12 on the inner wall and agitating device 7 of autoclave body 4, which is layer of molybdenum-disulfide And with a thickness of 12-15 microns, autoclave body 4 is stainless steel material.
Embodiment 2: molybdenum disulfide removes the preparation method of silicon anti-corrosion type reaction kettle in embodiment 1, comprising the following steps:
1) steel reactor inner wall of kettle and agitating paddle outer wall are subjected to derusting by sandblasting processing, make reaction kettle inner wall of kettle and stirring Paddle outer wall keeps cleaning;
2) molybdenum disulfide slurry is prepared, by ultra-fine molybdenum disulfide (0.8 micron), the adhesive (perfluoro capryl of mass ratio 1:0.2:1 Sodium acrylate polymer), deionized water be uniformly mixed so as to obtain molybdenum disulfide slurry;
3) first time spraying is then carried out, for the first time the process of spraying are as follows: be sprayed into molybdenum disulfide slurry instead with high-pressure spray gun It answers on kettle inner wall of kettle and agitating paddle outer wall, 4 microns of coating layer thickness, naturally dry, then dries 20h with 105 DEG C of hot-airs;
4) it then carries out spraying for the second time and third time sprays, the process and first time of spraying for the second time and third time spraying spray Process it is identical, third time spray after complete.
Embodiment 3: molybdenum disulfide removes the preparation method of silicon anti-corrosion type reaction kettle in embodiment 1, comprising the following steps:
1) steel reactor inner wall of kettle and agitating paddle outer wall are subjected to derusting by sandblasting processing, make reaction kettle inner wall of kettle and stirring Paddle outer wall keeps cleaning;
2) molybdenum disulfide slurry is prepared, by ultra-fine molybdenum disulfide (2 microns), the adhesive (perfluoro capryl third of mass ratio 1:0.8:5 E pioic acid methyl ester polymer), deionized water be uniformly mixed so as to obtain molybdenum disulfide slurry;
3) first time spraying is then carried out, for the first time the process of spraying are as follows: be sprayed into molybdenum disulfide slurry instead with high-pressure spray gun It answers on kettle inner wall of kettle and agitating paddle outer wall, 5 microns of coating layer thickness, naturally dry, then dries 10h with 150 DEG C of hot-airs;
4) it then carries out spraying for the second time and third time sprays, the process and first time of spraying for the second time and third time spraying spray Process it is identical, third time spray after complete.
Embodiment 4: molybdenum disulfide removes the preparation method of silicon anti-corrosion type reaction kettle in embodiment 1, comprising the following steps:
1) steel reactor inner wall of kettle and agitating paddle outer wall are subjected to derusting by sandblasting processing, make reaction kettle inner wall of kettle and stirring Paddle outer wall keeps cleaning;
2) molybdenum disulfide slurry is prepared, by ultra-fine molybdenum disulfide (4 microns), the adhesive (perfluoro capryl third of mass ratio 1:0.5:3 Olefin(e) acid polymerizable methacrylate object), deionized water be uniformly mixed so as to obtain molybdenum disulfide slurry;
3) first time spraying is then carried out, for the first time the process of spraying are as follows: be sprayed into molybdenum disulfide slurry instead with high-pressure spray gun It answers on kettle inner wall of kettle and agitating paddle outer wall, 5 microns of coating layer thickness, naturally dry, then dries 15h with 120 DEG C of hot-airs;
4) it then carries out spraying for the second time and third time sprays, the process and first time of spraying for the second time and third time spraying spray Process it is identical, third time spray after complete.
Particular condition in use of the invention is as follows: the 3000L reaction kettle made according to 2-4 embodiment of the present invention is added 50% Hydrofluoric acid 2000L, stirs lower 72 hours releasings materials of soak at room temperature, observation molybdenum disulfide coat layer surface without fall off, immaculate, Inner wall smooth is without attachment.
50% hydrofluoric acid 2000L is added according to the 3000L reaction kettle of 2-4 of embodiment of the present invention production, is warming up under stirring 48 hours releasing materials of 70-90 DEG C of holding, coating layer surface without fall off, immaculate, inner wall smooth are without attachment.
50% hydrofluoric acid 1000L is added according to the 3000L reaction kettle of 2-4 of embodiment of the present invention production, contains silica 2.13% molybdenum disulfide 1000kg, is warming up to 48 hours releasing materials of 70-90 DEG C of holding under stirring, coating layer surface without fall off, Immaculate, inner wall smooth are without attachment.
Embodiment 5: being provided with the reaction kettle of corrosion-inhibiting coating, advanced optimize on the basis of embodiment 1,
As depicted in figs. 1 and 2, autoclave body 4 is fixed on horizontal plane by support 13, is kept autoclave body 4 fixed, is guaranteed the connection of reaction kettle Firm and stable operation;Collet 6 is set on the outer wall of the autoclave body 4, autoclave body 4 is heated and be cooled down, collet 6 Top is provided with water inlet pipe 14, and the bottom end side of collet 6 is provided with outlet pipe 9, through water inlet pipe 14 and can go out after completion of the reaction Water pipe 9, which is passed through recirculated cooling water into collet 6, keeps 4 fast cooling of autoclave body cooling, discharges as early as possible, reduces the waiting time, is conducive to Improve the production efficiency of molybdenum disulfide;The outer wall of 6 inner close fitting autoclave body 4 of collet is provided with infrared ray heating tube 5, by infrared ray plus Heat pipe 5 can provide required reaction temperature for reaction kettle, and 5 heating speed of infrared ray heating tube is fast, be conducive to improve heating efficiency, Save the time.
5 top of autoclave body is provided with kettle cover 3, and to seal autoclave body 4, a manhole 15, two views are circumferentially distributed with thereon Mirror mouth 19 and multiple feed openings 16, manhole 15 are convenient for installation, maintenance and the safety inspection of reaction kettle, play safety in reaction and answer The effect suddenly ventilated.Two mirror mouths 19 are symmetrical arranged, and are monitored at any time to inner case of the staff to reaction kettle, Guarantee going on smoothly for reaction;Multiple feed openings 16 are matched with the discharge gate 8 for being set to 4 bottom center of autoclave body, to react When reaction raw materials feeding and after reaction react gains discharge;Survey is additionally provided on the position at 3 edge of kettle cover Thermometer 18 is arranged inside in warm mouth 17, and the thermometer 18 is vertically arranged and protrudes into 4 middle and lower part of autoclave body, to monitor autoclave body 4 Interior real time temperature timely regulates and controls in order to make, and guarantees preferable reaction temperature to improve the quality of reaction gains.
Agitating device 7 is made of agitating shaft 10 with the agitating paddle 11 for being set to 10 lower end of agitating shaft, to reaction mass It is stirred, agitating paddle 11 uses frame type agitating blade, and stabilized structure stirs the amount of material greatly and is conducive to conduct heat, can accelerate The progress of reaction;10 top of agitating shaft is pierced by kettle cover 3 and is connected in driving device 1, and driving device 1 includes driving motor, should The top center of kettle cover 3 is arranged in by sealing sleeve pipe 2 for driving motor, guarantees the leakproofness of reaction kettle entirety, output end court Lower setting is simultaneously fixedly connected by shaft coupling with agitating shaft 10, is stirred to provide power realization for agitating shaft 10 and agitating paddle 11 It mixes.
Hydrofluoric acid and molybdenum concentrate are sent into autoclave body 4 in use, first passing through feed opening 16, then starts driving motor and drives Agitating shaft 10 and agitating paddle 11 start to be stirred, while heat the energization of infrared ray heating tube 5 to autoclave body 4, work as temperature The temperature that meter 18 measures powers off infrared ray heating tube 5 after reaching reaction required temperature.Pass through water inlet after to material reaction Pipe 14 and outlet pipe 9, which are passed through recirculated cooling water into collet 6, keeps 4 fast cooling of autoclave body cooling, is finally discharged and reacts from discharge gate 8 Gains.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, this field is common Other modifications or equivalent replacement that technical staff makes technical solution of the present invention, without departing from technical solution of the present invention Spirit and scope, be intended to be within the scope of the claims of the invention.

Claims (9)

1. application of the molybdenum disulfide on equipment anticorrosion, which is characterized in that molybdenum disulfide is coated in connecting with corrosive liquid for equipment On the face of touching.
2. a kind of anti-corrosion type reaction kettle, including autoclave body and agitating device, which is characterized in that the agitating device is vertically arranged at institute It states in autoclave body, and is provided with anti-corrosion coat on the inner wall and agitating device of the autoclave body, the anti-corrosion coat is curing Molybdenum layer.
3. anti-corrosion type reaction kettle according to claim 2, it is characterised in that: the coat with a thickness of 12-15 microns.
4. anti-corrosion type reaction kettle according to claim 2, it is characterised in that: the agitating device is by agitating shaft and is set to The agitating paddle of the agitating shaft lower end forms, and agitating shaft and agitating paddle are equipped with anti-corrosion coat.
5. the preparation method of anti-corrosion type reaction kettle according to claim 2, which comprises the following steps: 1) will Reaction kettle inner wall of kettle, agitating shaft and agitating paddle outer wall carry out derusting by sandblasting processing, make outside reaction kettle inner wall of kettle and agitating paddle Wall keeps cleaning;
2) first time spraying is then carried out, for the first time the process of spraying are as follows: molybdenum disulfide slurry is sprayed into reaction kettle autoclave body It on wall, agitating shaft and agitating paddle outer wall, 4-5 microns of coating layer thickness, dries, reusable heat air dries 10-20h;
3) it then carries out spraying for the second time and third time sprays, the process and first time of spraying for the second time and third time spraying spray Process it is identical, third time spray after complete.
6. preparation method according to claim 5, it is characterised in that: the group of the molybdenum disulfide slurry becomes ultra-fine two sulphur Change molybdenum, adhesive, deionized water, ultra-fine molybdenum disulfide, adhesive, deionized water mass ratio be 1:0.2-0.8:1-5.
7. preparation method according to claim 5, it is characterised in that: the granularity of the ultra-fine molybdenum disulfide is that 0.8-5 is micro- Rice, described adhesive are perfluoro capryl methyl acrylate polymer, perfluoro capryl X 4460 or perfluoro capryl third Olefin(e) acid sodium polymer.
8. preparation method according to claim 5, it is characterised in that: the material of the reaction kettle autoclave body is steel.
9. preparation method according to claim 5, it is characterised in that: drying temperature is 105-150 DEG C in the step 2.
CN201811316608.XA 2018-11-07 2018-11-07 Application and a kind of anti-corrosion reaction kettle of the molybdenum disulfide on equipment anticorrosion Pending CN109364845A (en)

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