Temperature thermocouple protection device under high-temperature complex flue gas condition
阅读说明：本技术 一种高温复杂烟气条件下的测温热电偶保护装置 (Temperature thermocouple protection device under high-temperature complex flue gas condition ) 是由 王武钧 杨进行 钮杰 于 2021-10-08 设计创作，主要内容包括：本发明公开了一种高温复杂烟气条件下的测温热电偶保护装置,涉及材料领域,包括保护本体和保护涂层,将壬基酚聚氧乙烯醚、正丁醇与环己烷加入到烧瓶中,向烧瓶中滴加氨水并不断搅拌,滴加正硅酸乙酯,加入ZrOCl-(2)水溶液,将微乳液B加入到微乳液A中,加入助剂,得到该保护涂层；解决了现有的热电偶金属保护装置耐高温性差,易受高温氧化和酸性气体腐蚀的问题；硅酸锆具有高熔点、低热导率、低膨胀系数、优良的化学及相稳定性,同时烧结的硅酸锆具有极好的抗热震性,硅酸锆涂层能耐酸碱,且耐高温,适用于热电偶保护装置在腐蚀环境中的表面保护,从而达到了提高热电偶金属保护装置的耐热性和抗腐蚀的目的。(The invention discloses a temperature thermocouple protection device under a high-temperature complex smoke condition, which relates to the field of materials and comprises a protection body and a protection coating, wherein nonylphenol polyoxyethylene ether, n-butanol and cyclohexane are added into a flask, ammonia water is dropwise added into the flask while stirring continuously, tetraethoxysilane is dropwise added, ZrOCl is added 2 Adding the microemulsion B into the microemulsion A, and adding an auxiliary agent to obtain the protective coating; the problems that the existing thermocouple metal protection device has poor high temperature resistance and is easy to be subjected to high temperature oxidation and acidic gas corrosion are solved; zirconium silicate has high melting point and low heatThe thermal conductivity, the low expansion coefficient and the excellent chemical and phase stability are achieved, meanwhile, the sintered zirconium silicate has excellent thermal shock resistance, and the zirconium silicate coating can resist acid and alkali and high temperature, and is suitable for surface protection of a thermocouple protection device in a corrosive environment, so that the purposes of improving the heat resistance and corrosion resistance of the thermocouple metal protection device are achieved.)
1. A temperature thermocouple protection device under the condition of high-temperature complex flue gas comprises a protection body (1) and a protection coating (2), and is characterized in that the protection coating (2) is arranged on the outer side of the protection body (1);
the protective body (1) is obtained by the following preparation steps:
s1: smelting Fe, Cr, Ni, Mn, Mo and Co under the vacuum condition;
s2: blowing oxygen from the top, simultaneously blowing argon from the bottom to stir the melt for 5-20min, continuously blowing hydrogen from the bottom to stir, blowing nitrogen from the top, and treating for 5-20min to obtain a material E;
s3: adding silica and coke into the material E for deoxidation, desulfurization and slagging, and treating for 10-20 min;
s4: pouring is carried out to obtain the protection body (1).
2. The protection device for the thermocouple for temperature measurement under the high-temperature complex flue gas condition as recited in claim 1, wherein the weight ratio of Fe, Cr, Ni, Mn, Mo and Co in step S1 is 2:29.7:2:0.5:1: 30.1.
3. The protection device for the thermocouple under the high-temperature complex flue gas condition as recited in claim 1, wherein the dosage ratio of the material E, silica and coke in the step S3 is 65.3 g: 8 g: 10 g.
4. The protection device for the thermocouple under the high-temperature complex smoke condition as claimed in claim 1, wherein the protection coating (2) is prepared by the following steps:
s41: adding nonylphenol polyoxyethylene ether, n-butanol and cyclohexane into a flask, dropwise adding ammonia water into the flask and continuously stirring, controlling the dropwise adding speed to be 1-2 drops/s, dropwise adding tetraethoxysilane, controlling the dropwise adding speed to be 1-2 drops/s, and reacting for 4-5 hours to obtain microemulsion A;
s42: adding nonylphenol polyoxyethylene ether, n-butanol and cyclohexane into a flask, dropwise adding ammonia water into the flask while continuously stirring, controlling the dropwise adding speed to be 1-2 drops/s, and adding ZrOCl2Water solution to obtain microemulsion B;
s43: adding the microemulsion B into the microemulsion A, continuously stirring, reacting for 10-12h, adding acetone for demulsification, washing with deionized water and absolute ethyl alcohol, drying in an oven at 120 ℃ for 12-14h, calcining at 800 ℃, 1000 ℃, 1100, 1200 and 1300 ℃ for 2-3h respectively after drying, and adding an auxiliary agent to obtain the protective coating (2).
5. The protection device for the temperature thermocouple under the high-temperature complex flue gas condition as recited in claim 4, wherein in step S41, the mass fraction of the ammonia water is 28%, the mass fraction of the ethyl orthosilicate is 20%, and the dosage ratio of the nonylphenol polyoxyethylene ether, the n-butanol and the cyclohexane is 20 mL: 15mL of: 80mL, wherein the dosage of the ammonia water is 10% of the total mass of the nonylphenol polyoxyethylene ether, the n-butyl alcohol and the cyclohexane, and the dosage of the ethyl orthosilicate is 20% of the total mass of the nonylphenol polyoxyethylene ether, the n-butyl alcohol and the cyclohexane.
6. The device as claimed in claim 4, wherein the ZrOCl in step S42 is used for protecting the thermocouple during high temperature complicated smoke condition2The mass fraction of the water solution is 20%, and the dosage ratio of the nonylphenol polyoxyethylene ether, the n-butanol and the cyclohexane is 20 mL: 15mL of: 80mL, wherein the dosage of the ammonia water is 10 percent of the total mass of the nonylphenol polyoxyethylene ether, the n-butanol and the cyclohexane, and the ZrOCl2The dosage of the water solution is 20 percent of the total mass of the nonyl phenol polyoxyethylene ether, the n-butyl alcohol and the cyclohexane.
7. The protection device for the thermocouple for temperature measurement under the high-temperature complex flue gas condition according to claim 4, wherein the dosage ratio of the microemulsion A and the microemulsion B to the auxiliary agent in the step S43 is 10g: 10g to 1 g.
8. The protection device for the temperature thermocouple under the high-temperature complex flue gas condition according to claim 4, wherein the preparation process of the auxiliary agent in the step S43 is as follows:
s81: adding m-phenylenediamine into a three-neck flask, controlling the temperature at 5-7 ℃, adding a solvent N, N-dimethylacetamide, stirring under the protection of nitrogen, adding dry pyromellitic dianhydride, and mechanically stirring for 7-8h to obtain a product D;
s82: b is to be4C and SiO2Uniformly mixing, adding a solvent ethanol and a silane coupling agent, stirring for 2-3h, performing ultrasonic dispersion for 2-3h, and transferring to a drying oven at 80-90 ℃ for drying for 5-6h to obtain a product C;
s83: adding the product D into the product C, stirring for 2-3h, heating to 180-class temperature of 200 ℃ at the speed of 5-6 ℃/min, preserving heat for 2-3h, heating to 240-class temperature of 260 ℃ at the speed of 1-3 ℃/min, preserving heat for 3-4h, and naturally cooling to room temperature to obtain the auxiliary agent.
9. The protection device for the thermocouple under the high-temperature complex flue gas condition according to claim 8, wherein the molar ratio of m-phenylenediamine to pyromellitic dianhydride in step S81 is 1.2-1.3: 1.
10. the protection device for the thermocouple for temperature measurement under the high-temperature complex flue gas condition as claimed in claim 8, wherein the SiO in step S822、B4The dosage ratio of C to the silane coupling agent is 10g: 10g:1g, the dosage ratio of the product C to the product B in the step S83 is 1 g:1g of the total weight of the composition.
Technical Field
The invention relates to the field of materials, in particular to a protection device for a temperature thermocouple under a high-temperature complex smoke condition.
Background
Along with the development of heavy industry, the requirement on temperature during industrial heat treatment is more and more strict, the thermocouples are widely used in heat treatment temperature control, the thermocouples are a common temperature detection element in industrial furnace production, the accuracy and the durability of the thermocouples directly influence the normal operation of a process device, the thermocouples can be ensured to normally work as a protection device, and the thermocouples bear the infringement of high-temperature oxidation, high-temperature corrosion, high-temperature erosion abrasion of fluid powder, acid gas corrosion, boiler rapping and the like under the actual high-temperature working condition;
the existing thermocouple metal protection device has the characteristics of high mechanical strength, good toughness and good slag resistance, but poor high temperature resistance, and is easy to be subjected to high-temperature oxidation and acid gas corrosion;
a solution is now proposed to address the technical drawback in this respect.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a temperature thermocouple protection device under the high-temperature complex flue gas condition:
(1) adding nonylphenol polyoxyethylene ether, n-butanol and cyclohexane into a flask, dropwise adding ammonia water into the flask while stirring, dropwise adding ethyl orthosilicate, adding nonylphenol polyoxyethylene ether, n-butanol and cyclohexane into the flask, dropwise adding ammonia water into the flask while stirring, adding ZrOCl into the flask while stirring, and adding ZrOCl into the flask2The preparation method comprises the following steps of (1) adding the microemulsion B into the microemulsion A, adding acetone for demulsification, and adding an auxiliary agent to obtain the protective coating, wherein the problems of poor high-temperature resistance, high-temperature oxidation resistance and high acid gas corrosion resistance of the conventional thermocouple metal protection device are solved by preparing the protective coating;
(2) adding m-phenylenediamine into a three-neck flask, adding solvent N, N-dimethylacetamide, adding dried pyromellitic dianhydride to obtain a product D, and adding B4C and SiO2Mixing uniformly, adding solvent ethanol and silane coupling agent to obtain product C, adding product D into product C to obtain the final productThe auxiliary agent is added into the coating, so that the problem that the coating is easy to crack and fall off due to poor thermal shock resistance in the use process of the thermocouple metal protection device is solved.
The purpose of the invention can be realized by the following technical scheme:
a temperature thermocouple protection device under the condition of high-temperature complex flue gas comprises a protection body and a protection coating, wherein the protection coating is arranged on the outer side of the protection body;
wherein the protective body is obtained by the following preparation steps:
s1: smelting Fe, Cr, Ni, Mn, Mo and Co under the vacuum condition;
s2: blowing oxygen from the top, simultaneously blowing argon from the bottom to stir the melt for 5-20min, continuously blowing hydrogen from the bottom to stir, blowing nitrogen from the top, and treating for 5-20min to obtain a material E;
s3: adding silica and coke into the material E for deoxidation, desulfurization and slagging, and treating for 10-20 min;
s4: pouring is carried out to obtain the protection body.
As a further scheme of the invention: in step S1, the weight ratio of Fe, Cr, Ni, Mn, Mo and Co is 2:29.7:2:0.5:1: 30.1.
As a further scheme of the invention: the dosage ratio of the material E, the silica and the coke in the step S3 is 65.3 g: 8 g: 10 g.
As a further scheme of the invention: the protective coating is obtained by the following preparation steps:
s41: adding nonylphenol polyoxyethylene ether, n-butanol and cyclohexane into a flask, dropwise adding ammonia water into the flask and continuously stirring, controlling the dropwise adding speed to be 1-2 drops/s, dropwise adding tetraethoxysilane, controlling the dropwise adding speed to be 1-2 drops/s, and reacting for 4-5 hours to obtain microemulsion A;
s42: adding nonylphenol polyoxyethylene ether, n-butanol and cyclohexane into a flask, dropwise adding ammonia water into the flask while continuously stirring, controlling the dropwise adding speed to be 1-2 drops/s, and adding ZrOCl2Water solution to obtain microemulsion B;
s43: adding the microemulsion B into the microemulsion A, continuously stirring, reacting for 10-12h, adding acetone for demulsification, washing with deionized water and absolute ethyl alcohol, drying in an oven at the temperature of 110-120 ℃ for 12-14h, calcining at the temperature of 800, 1000, 1100, 1200 and 1300 ℃ for 2-3h respectively after drying, and adding an auxiliary agent to obtain the protective coating.
As a further scheme of the invention: in the step S41, the mass fraction of the ammonia water is 28%, the mass fraction of the ethyl orthosilicate is 20%, and the dosage ratio of the nonylphenol polyoxyethylene ether, the n-butanol and the cyclohexane is 20 mL: 15mL of: 80mL, wherein the dosage of the ammonia water is 10% of the total mass of the nonylphenol polyoxyethylene ether, the n-butyl alcohol and the cyclohexane, and the dosage of the ethyl orthosilicate is 20% of the total mass of the nonylphenol polyoxyethylene ether, the n-butyl alcohol and the cyclohexane.
As a further scheme of the invention: ZrOCl in step S422The mass fraction of the water solution is 20%, and the dosage ratio of the nonylphenol polyoxyethylene ether, the n-butanol and the cyclohexane is 20 mL: 15mL of: 80mL, wherein the dosage of the ammonia water is 10 percent of the total mass of the nonylphenol polyoxyethylene ether, the n-butanol and the cyclohexane, and the ZrOCl2The dosage of the water solution is 20 percent of the total mass of the nonyl phenol polyoxyethylene ether, the n-butyl alcohol and the cyclohexane.
As a further scheme of the invention: the dosage ratio of the microemulsion A, the microemulsion B and the auxiliary agent in the step S43 is 10g: 10g to 1 g.
As a further scheme of the invention: the preparation process of the auxiliary agent in the step S43 is as follows:
s81: adding m-phenylenediamine into a three-neck flask, controlling the temperature at 5-7 ℃, adding a solvent N, N-dimethylacetamide, stirring under the protection of nitrogen, adding dry pyromellitic dianhydride, and mechanically stirring for 7-8h to obtain a product D;
s82: b is to be4C and SiO2Uniformly mixing, adding a solvent ethanol and a silane coupling agent, stirring for 2-3h, performing ultrasonic dispersion for 2-3h, and transferring to a drying oven at 80-90 ℃ for drying for 5-6h to obtain a product C;
s83: adding the product D into the product C, stirring for 2-3h, heating to 180-class temperature of 200 ℃ at the speed of 5-6 ℃/min, preserving heat for 2-3h, heating to 240-class temperature of 260 ℃ at the speed of 1-3 ℃/min, preserving heat for 3-4h, and naturally cooling to room temperature to obtain the auxiliary agent.
As a further scheme of the invention: in the step S81, the molar ratio of the m-phenylenediamine to the pyromellitic dianhydride is 1.2-1.3: 1.
as a further scheme of the invention: SiO in step S822、B4The dosage ratio of C to the silane coupling agent is 10g: 10g:1g, the dosage ratio of the product C to the product B in the step S83 is 1 g:1g of the total weight of the composition.
The invention has the beneficial effects that:
(1) adding nonylphenol polyoxyethylene ether, n-butyl alcohol and cyclohexane into a flask, dropwise adding ammonia water into the flask and continuously stirring, dropwise adding ethyl orthosilicate, adding nonylphenol polyoxyethylene ether, n-butyl alcohol and cyclohexane into the flask, dropwise adding ammonia water into the flask and continuously stirring, adding ZrOCl2Adding the microemulsion B into the microemulsion A, adding acetone for demulsification, adding an auxiliary agent to obtain the protective coating, wherein the chemical formula of the zirconium silicate is ZrSiO4The method belongs to a tetragonal system, is a silicate mineral with an island-shaped structure, zirconium silicate has high melting point, low thermal conductivity, low expansion coefficient and excellent chemical and phase stability, the sintered zirconium silicate has excellent thermal shock resistance, a zirconium silicate coating can resist acid, alkali and organic solvents and resist high temperature, the microemulsion method is adopted to prepare the zirconium silicate, and the method has the advantages of simple experimental device, easy operation, manual control of particle size, narrow particle size distribution, good dispersibility, ZrSiO4In the plasma spraying process, the powder is decomposed into tetragonal phase and monoclinic phase ZrO due to the action of high-temperature flame flow2And amorphous Si02The phase change of the coating is basically not generated below 1000 ℃, and ZrO in the coating at 1200 DEG C2And SiO2Starting to generate ZrSiO by synthetic reaction4After which the phase composition is substantially unchanged and converted into stable ZrSiO4The coating is suitable for surface protection of the thermocouple protection device in a corrosive environment, so that the aims of improving the heat resistance and corrosion resistance of the thermocouple metal protection device are fulfilled;
(2) adding m-phenylenediamine into a three-neck flask, adding a solvent N, N-dimethyl acetylAmine, adding dry pyromellitic dianhydride to obtain product D, adding B4C and SiO2Uniformly mixing, adding solvent ethanol and silane coupling agent to obtain a product C, adding the product D into the product C to obtain the auxiliary agent, synthesizing a polyimide resin matrix by m-phenylenediamine and pyromellitic dianhydride, and mixing nano Si02Uniformly dispersed in the matrix, and used for strengthening dispersion in the coating, and when the thermocouple protection device is impacted, the dispersed Si02Absorbing impact energy of microcrack, preventing crack from expanding, transferring stress in the course of compression shearing to raise adhesive strength, in the low-temp. stage, the polyimide resin can be used for mainly adhering, when the temp. is raised to above 400 deg.C, B4C starts to generate oxidation reaction to react with oxygen in the air and gas micromolecules generated by thermal decomposition of polyimide to generate B with high-temperature fluidity and good wettability203At the temperature of over 800 ℃, the organic structure begins to be converted into the inorganic structure, the volume expansion occurs, the volume shrinkage generated during the thermal cracking of the resin can be effectively inhibited, the micro-cracks generated by the coating can be favorably healed, the integrity of the interface is ensured, and B is performed at the high temperature of over 1100 DEG C203Begin to volatilize, Si02Also retains structural integrity, is uniformly dispersed in the coating system, has adhesive effect at high temperature, and is molten B203Can flow to the interface crack to inhibit crack diffusion, so that the coating interface is more densified, thereby achieving the purpose of improving thermal shock resistance.
Drawings
The invention is further described below with reference to the accompanying drawings;
FIG. 1 is a schematic view of the overall structure of a thermocouple protection device under a complex high-temperature flue gas condition according to the present invention;
FIG. 2 is a cross-sectional view of a thermocouple protection device under high temperature complex flue gas conditions in accordance with the present invention;
FIG. 3 is a top view of a thermocouple protector under complex high temperature flue gas conditions in accordance with the present invention;
in the figure: 1. a protection body; 2. and (4) protecting the coating.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
According to the figures 1-3, the protection device for the temperature thermocouple under the high-temperature complex flue gas condition comprises a protection body 1 and a protection coating 2, wherein the protection coating 2 is arranged on the outer side of the protection body 1;
example 1:
the embodiment is a temperature thermocouple protection device under the condition of high-temperature complex flue gas, which comprises a protection body 1 and a protection coating 2;
wherein the protective body 1 is obtained by the following preparation steps:
s1: smelting Fe, Cr, Ni, Mn, Mo and Co under the vacuum condition;
s2: blowing oxygen from the top, simultaneously blowing argon from the bottom to stir the melt for 5min, continuously blowing hydrogen from the bottom to stir, blowing nitrogen from the top, and treating for 5min to obtain a material E;
s3: adding silica and coke into the material E for deoxidation, desulfurization and slagging, and treating for 10 min;
s4: pouring to obtain the protection body 1;
wherein the protective coating 2 is obtained by the following preparation steps:
s41: adding nonylphenol polyoxyethylene ether, n-butanol and cyclohexane into a flask, dropwise adding ammonia water into the flask and continuously stirring, controlling the dropwise adding speed to be 1 drop/s, dropwise adding tetraethoxysilane, controlling the dropwise adding speed to be 1 drop/s, and reacting for 4 hours to obtain microemulsion A;
s42: adding nonylphenol polyoxyethylene ether, n-butanol and cyclohexane into a flask, dropwise adding ammonia water into the flask while continuously stirring, controlling the dropwise adding speed to be 1 drop/s, and adding ZrOCl2An aqueous solution of a carboxylic acid and a carboxylic acid,obtaining microemulsion B;
s43: adding the microemulsion B into the microemulsion A, continuously stirring, reacting for 10h, adding acetone for demulsification, washing with deionized water and absolute ethyl alcohol, drying in an oven at 110 ℃ for 12h, calcining at 800, 1000, 1100, 1200 and 1300 ℃ for 2-3h after drying, adding an auxiliary agent, spraying on the protective body 1 by adopting a plasma spraying technology, and performing heat treatment to obtain the protective coating 2;
the preparation process of the auxiliary agent in the step S43 is as follows:
s81: adding m-phenylenediamine into a three-neck flask, controlling the temperature at 5 ℃, adding a solvent N, N-dimethylacetamide, stirring under the protection of nitrogen, adding dry pyromellitic dianhydride, and mechanically stirring for 7 hours to obtain a product D;
s82: b is to be4C and SiO2Uniformly mixing, adding a solvent ethanol and a silane coupling agent, stirring for 2 hours, ultrasonically dispersing for 2 hours, and transferring to a drying oven at 80 ℃ for drying for 5 hours to obtain a product C;
s83: and adding the product D into the product C, stirring for 2h, heating to 180 ℃ at the speed of 5 ℃/min, preserving heat for 2h, heating to 240 ℃ at the speed of 1 ℃/min, preserving heat for 3h, and naturally cooling to room temperature to obtain the auxiliary agent.
Example 2:
the embodiment is a temperature thermocouple protection device under the condition of high-temperature complex flue gas, which comprises a protection body 1 and a protection coating 2;
wherein the protective body 1 is obtained by the following preparation steps:
s1: smelting Fe, Cr, Ni, Mn, Mo and Co under the vacuum condition;
s2: blowing oxygen from the top, simultaneously blowing argon from the bottom to stir the melt for 10min, continuously blowing hydrogen from the bottom to stir, blowing nitrogen from the top, and treating for 10min to obtain a material E;
s3: adding silica and coke into the material E for deoxidation, desulfurization and slagging, and treating for 10 min;
s4: pouring to obtain the protection body 1;
wherein the protective coating 2 is obtained by the following preparation steps:
s41: adding nonylphenol polyoxyethylene ether, n-butanol and cyclohexane into a flask, dropwise adding ammonia water into the flask and continuously stirring, controlling the dropwise adding speed to be 1 drop/s, dropwise adding tetraethoxysilane, controlling the dropwise adding speed to be 1 drop/s, and reacting for 4 hours to obtain microemulsion A;
s42: adding nonylphenol polyoxyethylene ether, n-butanol and cyclohexane into a flask, dropwise adding ammonia water into the flask while continuously stirring, controlling the dropwise adding speed to be 1 drop/s, and adding ZrOCl2Water solution to obtain microemulsion B;
s43: adding the microemulsion B into the microemulsion A, continuously stirring, reacting for 10h, adding acetone for demulsification, washing with deionized water and absolute ethyl alcohol, drying in an oven at 110 ℃ for 12h, calcining at 800, 1000, 1100, 1200 and 1300 ℃ for 3h after drying, adding an auxiliary agent, spraying on the protective body 1 by adopting a plasma spraying technology, and performing heat treatment to obtain the protective coating 2;
the preparation process of the auxiliary agent in the step S43 is as follows:
s81: adding m-phenylenediamine into a three-neck flask, controlling the temperature at 5 ℃, adding a solvent N, N-dimethylacetamide, stirring under the protection of nitrogen, adding dry pyromellitic dianhydride, and mechanically stirring for 7 hours to obtain a product D;
s82: b is to be4C and SiO2Uniformly mixing, adding a solvent ethanol and a silane coupling agent, stirring for 3 hours, ultrasonically dispersing for 3 hours, and transferring to a drying oven at 90 ℃ for drying for 6 hours to obtain a product C;
s83: and adding the product D into the product C, stirring for 3h, heating to 200 ℃ at the speed of 6 ℃/min, preserving heat for 3h, heating to 260 ℃ at the speed of 3 ℃/min, preserving heat for 4h, and naturally cooling to room temperature to obtain the auxiliary agent.
Example 3:
the embodiment is a temperature thermocouple protection device under the condition of high-temperature complex flue gas, which comprises a protection body 1 and a protection coating 2;
wherein the protective body 1 is obtained by the following preparation steps:
s1: smelting Fe, Cr, Ni, Mn, Mo and Co under the vacuum condition;
s2: blowing oxygen from the top, simultaneously blowing argon from the bottom to stir the melt for 20min, continuously blowing hydrogen from the bottom to stir, blowing nitrogen from the top, and treating for 20min to obtain a material E;
s3: adding silica and coke into the material E for deoxidation, desulfurization and slagging, and treating for 20 min;
s4: pouring to obtain the protection body 1;
wherein the protective coating 2 is obtained by the following preparation steps:
s41: adding nonylphenol polyoxyethylene ether, n-butanol and cyclohexane into a flask, dropwise adding ammonia water into the flask and continuously stirring, controlling the dropwise adding speed to be 2 drops/s, dropwise adding tetraethoxysilane, controlling the dropwise adding speed to be 2 drops/s, and reacting for 5 hours to obtain microemulsion A;
s42: adding nonylphenol polyoxyethylene ether, n-butanol and cyclohexane into a flask, dropwise adding ammonia water into the flask while continuously stirring, controlling the dropwise adding speed to be 2 drops/s, and adding ZrOCl2Water solution to obtain microemulsion B;
s43: adding the microemulsion B into the microemulsion A, continuously stirring, reacting for 12h, adding acetone for demulsification, washing with deionized water and absolute ethyl alcohol, drying in an oven at 120 ℃ for 14h, calcining at 800, 1000, 1100, 1200 and 1300 ℃ for 3h after drying, adding an auxiliary agent, spraying on the protective body 1 by adopting a plasma spraying technology, and performing heat treatment to obtain the protective coating 2;
the preparation process of the auxiliary agent in the step S43 is as follows:
s81: adding m-phenylenediamine into a three-neck flask, controlling the temperature at 7 ℃, adding a solvent N, N-dimethylacetamide, stirring under the protection of nitrogen, adding dry pyromellitic dianhydride, and mechanically stirring for 8 hours to obtain a product D;
s82: b is to be4C and SiO2Uniformly mixing, adding a solvent ethanol and a silane coupling agent, stirring for 3 hours, ultrasonically dispersing for 3 hours, and transferring to a drying oven at 90 ℃ for drying for 6 hours to obtain a product C;
s83: and adding the product D into the product C, stirring for 3h, heating to 200 ℃ at the speed of 6 ℃/min, preserving heat for 3h, heating to 260 ℃ at the speed of 3 ℃/min, preserving heat for 4h, and naturally cooling to room temperature to obtain the auxiliary agent.
Comparative example 1:
compared with the embodiment 1, the comparative example adopts the inorganic dry powder coating to replace the protective coating 2, and the rest steps are the same;
comparative example 2:
compared with the example 1, the comparative example does not add the auxiliary agent, and the rest steps are the same;
the coating materials of the temperature thermocouple protection devices in the embodiments 1-3 and the comparative examples 1-2 under the high-temperature complex smoke condition are subjected to an acid corrosion resistance test through heat treatment, the corrosion resistance of the materials is tested by adopting a weight loss method, the materials are weighed on a balance, and then 300mL of 0.1mol/L HCI and H are respectively placed in the balance2SO4And H3PO4Keeping the temperature in the solution at 105 ℃, taking out a sample after 24 hours of corrosion, cleaning and drying the sample, and weighing the weight of the sample;
the results are shown in the following table:
as can be seen from the above table, under the same test conditions, the average mass before corrosion of the experimental examples was 0.5220g, and the average mass after corrosion reached 0.512-0.517g, whereas the average mass before corrosion of comparative example 1 using the inorganic dry powder paint in place of the protective coating 2 was 0.5213g, the average mass after corrosion was 0.352g, the average mass before corrosion of comparative example 2 without the addition of the auxiliary agent was 0.5109g, the average mass after corrosion was 0.495g, and the average corrosion rate of the experimental examples was 1.5924X 10-6-1.5936×10-6g/mm2h, while comparative example 1, in which an inorganic dry powder coating was used instead of the protective coating 2, had an average corrosion rate of 2.098X 10- 6g/mm2h, average Corrosion Rate of 1.854X 10 for comparative example 2 without addition of adjuvant-6g/mm2h, the data of the experimental examples are superior to those of the comparative examples, which shows that the addition of the auxiliary agent can improve the corrosion resistance of the coating and ensure that the protective coating 2 can more effectively reduce acidThe corrosion speed of the environment can protect the protection body 1 and the thermocouple.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
- 上一篇：一种医用注射器针头装配设备
- 下一篇：一种热电偶组合式速度电势探针及测量方法