CN108088792A - Dirty sample and preparation method and application among a kind of - Google Patents
Dirty sample and preparation method and application among a kind of Download PDFInfo
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- CN108088792A CN108088792A CN201711205178.XA CN201711205178A CN108088792A CN 108088792 A CN108088792 A CN 108088792A CN 201711205178 A CN201711205178 A CN 201711205178A CN 108088792 A CN108088792 A CN 108088792A
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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
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- 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
Abstract
The invention belongs to oil refining industry catalytic cracking unit technical field of surface, and in particular to dirty sample and preparation method and application among a kind of.Dirty sample includes component basis powder and binding agent among described；Wherein, basic powder includes following component in parts by mass：0.88 part of calcium chloride, 2.77 parts of ferrous sulfate, 2.81 parts of nickel sulfate, 93.54 parts of 2 catalyst of MMC.The present invention mixes calcium chloride, ferrous sulfate, nickel sulfate and 2 catalyst of MMC, obtains basic powder；Basic powder is mixed with binding agent, is obtained blending powder, is then added in water, obtains blending slurry；Slurry high temperature sintering is blended, cooling obtains intermediate dirty sample.The easy fouling of dirty sample among produced by the present invention, dirty sample cohesive strength is larger, the preliminary screening available for scale prevention coating.
Description
Technical field
The invention belongs to oil refining industry catalytic cracking unit technical field of surface, and in particular among a kind of dirty sample and
Its preparation method and application.
Background technology
In oil refining industry, catalytic cracking flue gas turbine (abbreviation smoke machine) is that the thermal energy of high-temperature flue gas is converted into machinery
Can, and main air blower or generator operation are driven, realize the power-equipment of energy conversion, organic efficiency has up to more than 130%
Significant energy-saving effect.
Third-stage cyclone separator (referred to as three revolve) is the key that catalytic cracking unit exhanst gas outlet energy-recuperation system is set
One of standby, the height of efficiency directly affects the normal use of smoke machine in operational process.The smoke machine main shaft during industry park plan
It is one of FAQs that vibration exceeding the standard, which causes non-normal stop, and basic reason is that smoke machine blade wear and fouling of catalyst are made
Into.In recent years, the problem of continuously improving with catalytic cracking process, the use of new catalyst and raw material oil quality, is drawn
Three rotations risen and smoke machine scale problems become increasingly conspicuous, and have seriously affected the long-term operation of energy-recuperation system.
Smoke machine internal incrustation particularly smoke machine movable vane surface scale problem is increasingly severe, serious to destroy the dynamic flat of rotor
Weighing apparatus gently then causes smoke machine vibration exceeding the standard to shut down, heavy then cause the collision of movable vane and outer rim, and fracture blade.The smoke machine of some oil plants
Scale removal will be shut down by often having run some months, can not be synchronous with the overhaul of whole equipment, because failure frequent shutdown reduces pair
The recycling efficiency of high-temperature flue gas, energy consumption rise, and even cause the unplanned shutdown of whole device sometimes, this is seriously affected
The economic benefit of enterprise causes huge economic loss.Therefore, the exploitation of flue gas turbine expander good antiscale property method has important meaning
Justice.
Coating protection is one of method for carrying out three rotation single tubes and turbine blade fouling improvement, and the preparation of dirty sample is
Carry out the Research foundation to interact between coating and dirty sample.The fouling of catalyst will often be undergone on three rotation single tubes, flue gas turbine expander
Some months could be formed, and dirty sample is in irregular shape.If the regular sample of dirty sample can be prepared, be conducive to coating and dirty sample
Study on Compatibility facilitates the screening of protective coating.
Wang Yu et al. (Wang Yu, Xing Shaowei, in Wang Jianjun catalytic cracking flue gas turbines the experiment of fouling of catalyst mechanism grind
Study carefully [J] China powder technology, 22 (1), 2016,92-96.) in terms of dirty sample preparation, it is static high using being carried out in high-temperature electric resistance furnace
Warm sintering experiment, heating furnace simulate the working environment in smoke machine, with placing equivalent on the test specimen of smoke machine movable vane phase same material
Catalytic unit flue gas turbine inlet catalyst sample is sintered experiment to prepare dirty sample.Hu Renbo et al. (Hu Renbo, Bai Rui, Zhao Jin
Chong, wait catalytic cracking three revolve catalyst fines sintering and mechanism of scaling [J] China University Of Petroleum Beijing's journals (natural science edition), 37
(4), it is also 2013,169-173.) that we selected typical catalytic cracking unit three revolves fine powder for research object, at different temperatures to three
Rotation fine powder carries out roasting experiment, and catalyst fines main component is aluminium oxide and silica.Although ingredient is approached with industrial dirty sample,
But above-mentioned sintering method has the drawback that itself cohesive strength of dirty sample is not high and not be bonded with parent metal.
The content of the invention
For overcome the deficiencies in the prior art and shortcoming, primary and foremost purpose of the invention is to provide dirty sample among a kind of.
Another object of the present invention is to provide the preparation method of dirty sample among above-mentioned.
It is still another object of the present invention to provide the applications of above-mentioned intermediate dirty sample.
The purpose of the present invention is achieved through the following technical solutions：
Dirty sample, includes component basis powder (JCF) and binding agent among a kind of；
The basic powder, includes component as follows in parts by mass：
The binding agent is preferably aluminium dihydrogen phosphate (chemical formula Al (H2PO4)3)；
The dosage of the aluminium dihydrogen phosphate is preferably the 30~50% of binding agent and basic powder gross mass；
The preparation standard of the MMC-2 catalyst is preferably 361 0236-2015 of Q/SH；
The preparation method of dirty sample, comprises the following steps among described：
(1) calcium chloride, ferrous sulfate, nickel sulfate and MMC-2 catalyst are mixed, obtains basic powder (JCF)；
(2) basic powder (JCF) made from step (1) with binding agent is mixed, obtains blending powder (GHF), Ran Houjia
Enter water, obtain blending slurry (GHLJ)；
(3) by step (2) blending slurry high temperature sintering obtained, cooling obtains intermediate dirty sample；
The preferred distilled water of water described in step (2)；
The dosage of water described in step (2) is preferably：Per 100g, the amount of water of blending powder is 55~65mL；
The condition of sintering described in step (3) is preferably 680~750 DEG C, keeps the temperature 2~4h；
Application of the dirty sample in scale prevention coating screening field among described；
A kind of method for screening scale prevention coating, comprises the following steps：
(1) calcium chloride, ferrous sulfate, nickel sulfate and MMC-2 catalyst are mixed, obtains basic powder (JCF)；
(2) basic powder (JCF) made from step (1) with binding agent is mixed, obtains blending powder (GHF), Ran Houjia
Enter water, obtain blending slurry (GHLJ)；
(3) by step (2) blending slurry obtained coated on coating sample, high temperature sintering, cooling obtains intermediate dirty sample
While, if intermediate dirt sample is not bonded with coating sample, illustrate that coating sample has antiscaling effect；If intermediate dirt sample is with applying
Layer sample bonds, and illustrates that coating sample does not have antiscaling effect；
Water described in step (2) is preferably distilled water；
The dosage of water described in step (2) is preferably：Per 100g, the amount of water of blending powder is 55~65mL；
The condition of sintering described in step (3) is preferably 680~750 DEG C, keeps the temperature 2~4h；
The principle of the present invention：
The method comprises the steps of firstly, preparing basic powder (abbreviation JCF) is gone out, make the powder after high temperature sintering with industrial scale sample ingredient
It is essentially identical, by the way of basic powder (JCF) and aluminium dihydrogen phosphate blending, blending powder (abbreviation GHF) is made, is added in
After suitable quantity of water, blending slurry (abbreviation GHLJ) is formed, then blending slurry GHLJ is sintered, forms intermediate dirty sample.For applying
For layer, if certain coating is not bonded with the higher intermediate dirty sample of intensity after viscosity bigger, sintering before sintering, the deducibility coating
It is not bonded with industrial dirt, i.e., has antiscaling effect in industrial conditions, the later stage can further be screened by commerical test.Pass through
Centre dirt sample, can realize oil refining industry catalytic cracking unit coating material indirectly under simple sintering condition
Preliminary screening.
The present invention is had the following advantages compared with the prior art and effect：
(1) block dirt sample is easily formed after blending fused slurry produced by the present invention, both hands are difficult to be broken disconnected, cohesion
Intensity is larger, improve basic powder (JCF) sintering after gently twist with the fingers powder situation.
(2) because of JCF non-scalings, the enhanced fouling resistance of coating can not be judged with JCF；If certain coating X can prevent intermediate dirty sample
Its surface is bonded in, then the bondings of JCF on the coating layer can be prevented in very big possibility.It, can by the way of intermediate dirty sample
Realize the preliminary screening of coating.
Description of the drawings
Fig. 1 is the exterior appearance figure of dirty sample among obtained in embodiment 1.
Fig. 2 is the exterior appearance figure of dirty sample among obtained in embodiment 2.
Fig. 3 is the exterior appearance figure of dirty sample among obtained in embodiment 3.
Fig. 4 is the exterior appearance figure of dirt sample obtained in comparative example 1.
Fig. 5 is the exterior appearance figure of dirt sample obtained in comparative example 2.
Specific embodiment
With reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) by 0.88g calcium chloride, 2.77g ferrous sulfate, 2.81g nickel sulfates and 93.54g MMC-2 catalyst (powder systems
Standby standard is 361 0236-2015 of Q/SH) mixing, obtain basic powder (JCF)；
(2) basic powder (JCF) made from 14g steps (1) with 6g binding agent aluminium dihydrogen phosphates is mixed, obtains blending powder
Body (GHF) then adds in 12ml distilled water, obtains blending slurry (GHLJ-1)；
(3) 304 stainless steel curved beams of 50 × 50 × 5mm specifications are got out, by 304 stainless steel boxes (outside dimension 50mm ×
50mm × 5mm, inside dimension 45mm × 45mm × 5mm) it is placed in specimen surface；By step (2) blending slurry (GHLJ-1) obtained
Coated on specimen surface, make slurry that the sample for coating slurry is placed in sintering furnace and is sintered, sintering temperature is full of box
700 DEG C, keep the temperature 2h；Heat preservation program is then shut off, sample furnace cooling room temperature obtains intermediate dirty sample.
It is broken into two with one's hands as shown in Figure 1, centre dirt sample adult is more difficult, its own intensity is higher.
Embodiment 2
(1) by 0.88g calcium chloride, 2.77g ferrous sulfate, 2.81g nickel sulfates and 93.54g MMC-2 catalyst (powder systems
Standby standard is 361 0236-2015 of Q/SH) mixing, obtain basic powder (JCF)；
(2) basic powder (JCF) made from 12g steps (1) with 8g binding agent aluminium dihydrogen phosphates is mixed, obtains blending powder
Body (GHF) then adds in 11ml distilled water, obtains blending slurry (GHLJ-2)；
(3) 304 stainless steel curved beams of 50 × 50 × 5mm specifications are got out, by 304 stainless steel boxes (outside dimension 50mm ×
50mm × 5mm, inside dimension 45mm × 45mm × 5mm) specimen surface is placed in, by step (2) blending slurry (GHLJ-2) obtained
Coated on specimen surface, make slurry that the sample for coating slurry is placed in sintering furnace and is sintered, sintering temperature is full of box
750 DEG C, keep the temperature 4h；Heat preservation program is then shut off, sample is down to room temperature with stove, obtains intermediate dirty sample；
As shown in Fig. 2, foring dirty sample among block after blending fused slurry, adult's both hands are difficult to break into two with one's hands, its own is strong
Degree is high.
Embodiment 3
(1) by 0.88g calcium chloride, 2.77g ferrous sulfate, 2.81g nickel sulfates and 93.54g MMC-2 catalyst (powder systems
Standby standard is 361 0236-2015 of Q/SH) mixing, obtain basic powder (JCF)；
(2) basic powder (JCF) made from 10g steps (1) with 10g binding agent aluminium dihydrogen phosphates is mixed, is blended
Powder (GHF) then adds in 13ml distilled water, obtains blending slurry (GHLJ-3)；
(3) 304 stainless steel curved beams of the surface spraying NiCr-Cr3C2 coatings of 50 × 50 × 5mm specifications are got out, by 304
Stainless steel box (outside dimension 50mm × 50mm × 5mm, inside dimension 45mm × 45mm × 5mm) is placed in coating sample surface, will walk
Suddenly (2) blending slurry (GHLJ-3) obtained makes slurry that will be coated full of box coated on NiCr-Cr3C2 coating samples surface
The coating sample of slurry, which is placed in sintering furnace, to be sintered, and sintering temperature is 680 DEG C, keeps the temperature 3h；It is then shut off heat preservation program, examination
Sample is down to room temperature with stove, obtains intermediate dirty sample；
As shown in figure 3, dirty sample, dirty sample among block are formd after blending fused slurry is firmly adhered to metal box
On, it is difficult to it removes, and both hands of being grown up are difficult to break into two with one's hands, its own intensity is high.After experiment, it is found that intermediate dirty sample is applied with NiCr-Cr3C2
Layer bonds, and illustrates NiCr-Cr3C2 coating not antiscale, this is consistent with the situation in industrial smoke machine.
Comparative example 1
(1) by 0.88g calcium chloride, 2.77g ferrous sulfate, 2.81g nickel sulfates and 93.54g MMC-2 catalyst (powder systems
Standby standard is 361 0236-2015 of Q/SH) mixing, obtain basic powder (JCF)；
(2) 12ml distilled water is added in basic powder (JCF) made from 20g steps (1), forms slurry (LJ-0)；
(3) 304 stainless steel curved beams of 50 × 50 × 5mm specifications are got out, by 304 stainless steel boxes (outside dimension 50mm ×
50mm × 5mm, inside dimension 45mm × 45mm × 5mm) specimen surface is placed in, slurry (LJ-0) made from step (2) is coated on
Specimen surface makes slurry be full of box, the sample for coating slurry is placed in sintering furnace and is sintered, and sintering temperature is 700 DEG C,
Keep the temperature 4h；Heat preservation program is then shut off, sample is down to room temperature with stove.
As shown in figure 4, it is bulky powder after fused slurry, not into dirty sample block, powder constituents are shown in Table 1, with smoke machine row
The ingredient (being shown in Table 2) of the dirty sample of industry industry is close.
Basic powder (JCF) the 700 DEG C of sintered X-ray power spectrum ingredients of table 1
The X-ray power spectrum ingredient of the dirty sample of 2 industry of table
Comparative example 2
(1) by 0.88g calcium chloride, 2.77g ferrous sulfate, 2.81g nickel sulfates and 93.54g MMC-2 catalyst (powder systems
Standby standard is 361 0236-2015 of Q/SH) mixing, obtain basic powder (JCF)；
(2) basic powder (JCF) made from 18g steps (1) with 2g binding agents aluminium dihydrogen phosphate is blended, prepares blending powder
Body (GHF) then adds in 12ml distilled water, obtains blending slurry (GHLJ-4)；
(3) 304 stainless steel curved beams of 50 × 50 × 5mm specifications are got out, by 304 stainless steel boxes (outside dimension 50mm ×
50mm × 5mm, inside dimension 45mm × 45mm × 5mm) specimen surface is placed in, prepared blending slurry (GHLJ-4) is coated on
Specimen surface makes slurry be full of box；The sample for coating slurry is placed in sintering furnace and is sintered, sintering temperature is 720 DEG C,
Keep the temperature 4h；Heat preservation program is then shut off, sample is down to room temperature with stove.
As shown in figure 5, it is bulky powder after blending fused slurry, not into dirty sample block.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. dirty sample among a kind of, it is characterised in that include component basis powder and binding agent；
The basic powder, includes component as follows in parts by mass：
2. dirty sample among according to claim 1, it is characterised in that：
The binding agent is aluminium dihydrogen phosphate.
3. dirty sample among according to claim 2, it is characterised in that：
The dosage of the aluminium dihydrogen phosphate is binding agent and the 30~50% of basic powder gross mass.
4. dirty sample among according to claim 1, it is characterised in that：
The preparation standard of the MMC-2 catalyst is 361 0236-2015 of Q/SH.
5. the preparation method of dirty sample among Claims 1 to 4 any one of them, it is characterised in that comprise the following steps：
(1) calcium chloride, ferrous sulfate, nickel sulfate and MMC-2 catalyst are mixed, obtains basic powder；
(2) basic powder made from step (1) with binding agent is mixed, obtains blending powder, then add in water, obtain blend composition
Slurry；
(3) by step (2) blending slurry high temperature sintering obtained, cooling obtains intermediate dirty sample.
6. the preparation method of dirty sample among according to claim 5, it is characterised in that：
The dosage of water described in step (2) is：Per 100g, the amount of water of blending powder is 55~65mL.
7. the preparation method of dirty sample among according to claim 5, it is characterised in that：
The condition of sintering described in step (3) is 680~750 DEG C, keeps the temperature 2~4h.
8. application of the dirty sample in scale prevention coating screening field among Claims 1 to 4 any one of them.
A kind of 9. method for screening scale prevention coating, it is characterised in that comprise the following steps：
(1) calcium chloride, ferrous sulfate, nickel sulfate and MMC-2 catalyst are mixed, obtains basic powder；
(2) basic powder made from step (1) with binding agent is mixed, obtains blending powder, then add in water, obtain blend composition
Slurry；
(3) by step (2) blending slurry obtained coated on coating sample, high temperature sintering, cooling obtains the same of intermediate dirty sample
When, if intermediate dirt sample is not bonded with coating sample, illustrate that coating sample has antiscaling effect；If intermediate dirt sample is tried with coating
Sample bonds, and illustrates that coating sample does not have antiscaling effect.
10. the method for screening scale prevention coating according to claim 9, it is characterised in that：
The condition of sintering described in step (3) is 680~750 DEG C, keeps the temperature 2~4h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2760253C1 (en) * | 2021-03-24 | 2021-11-23 | Акционерное общество "Пермский завод "Машиностроитель" | Method for evaluating the cohesive strength of powder metal coatings |
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Cited By (1)
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| RU2760253C1 (en) * | 2021-03-24 | 2021-11-23 | Акционерное общество "Пермский завод "Машиностроитель" | Method for evaluating the cohesive strength of powder metal coatings |
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