CN116376370A - Acid corrosion-resistant paint for inner wall of reaction kettle and preparation method thereof - Google Patents
Acid corrosion-resistant paint for inner wall of reaction kettle and preparation method thereof Download PDFInfo
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- CN116376370A CN116376370A CN202310374697.8A CN202310374697A CN116376370A CN 116376370 A CN116376370 A CN 116376370A CN 202310374697 A CN202310374697 A CN 202310374697A CN 116376370 A CN116376370 A CN 116376370A
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- 230000007797 corrosion Effects 0.000 title claims abstract description 38
- 238000005260 corrosion Methods 0.000 title claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 36
- 239000002253 acid Substances 0.000 title claims abstract description 27
- 239000003973 paint Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 23
- 229920001973 fluoroelastomer Polymers 0.000 claims abstract description 22
- 239000003607 modifier Substances 0.000 claims abstract description 18
- 239000000945 filler Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000002131 composite material Substances 0.000 claims abstract description 9
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 44
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- 238000000967 suction filtration Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000000576 coating method Methods 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 12
- 239000013530 defoamer Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 claims description 4
- ZFVMWEVVKGLCIJ-UHFFFAOYSA-N bisphenol AF Chemical group C1=CC(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C=C1 ZFVMWEVVKGLCIJ-UHFFFAOYSA-N 0.000 claims description 4
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical group CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000006482 condensation reaction Methods 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 238000004073 vulcanization Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 229910021382 natural graphite Inorganic materials 0.000 abstract description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 10
- 239000005562 Glyphosate Substances 0.000 description 7
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 description 7
- 229940097068 glyphosate Drugs 0.000 description 7
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 6
- 239000006229 carbon black Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229930185605 Bisphenol Natural products 0.000 description 3
- 239000004471 Glycine Substances 0.000 description 3
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical group C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- 229940106681 chloroacetic acid Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
- C01B32/196—Purification
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses an acid corrosion resistant paint for the inner wall of a reaction kettle and a preparation method thereof, belonging to the technical field of paint, and comprising the following raw materials in parts by weight: 100-120 parts of fluororubber, 260-280 parts of solvent, 30-35 parts of modifier, 5-8 parts of composite vulcanizing agent, 12-15 parts of filler, 1-2 parts of defoaming agent and 0.5-1 part of leveling agent, wherein the invention adopts an improved Hummers method to oxidize natural graphite, and prepares purified graphene by ultrasonic stripping, and the graphene has excellent high temperature resistance and corrosion resistance.
Description
Technical Field
The invention belongs to the technical field of coatings, and particularly relates to an acid corrosion resistance coating for the inner wall of a reaction kettle and a preparation method thereof.
Background
The glycine method is the most main method for producing glyphosate in China at present, and is also the current process route for producing glyphosate in our company. Firstly, glycine is synthesized by taking chloroacetic acid or hydrocyanic acid and the like as raw materials, and then the glycine reacts with other raw materials to synthesize glyphosate. The technological process mainly comprises synthesis, hydrolysis, crystallization and centrifugal drying.
In the process for producing the glyphosate in the factory, the process mainly comprises the processes of synthesis, acidification, hydrolysis, crystallization, centrifugation, drying and the like, wherein hydrolysis and crystallization are required to be performed by a hydrolysis kettle and a crystallization kettle, fluororubber coating is coated on the inner walls of the hydrolysis kettle and the crystallization kettle in the prior art, and has excellent high temperature resistance and corrosion resistance, but because of the high-temperature process specificity of the production of strong acid of the glyphosate, particularly in the hydrolysis and crystallization stages, the high corrosion characteristics of equipment and facilities are used, the failure rate and maintenance rate of the equipment and the facility are high, and the main problems of limiting the sustainable production of the glyphosate are also solved.
Disclosure of Invention
The invention aims to provide an acid corrosion resistant coating for the inner wall of a reaction kettle and a preparation method thereof, so as to improve the acid corrosion resistance of the reaction kettle in the existing glyphosate production process.
The aim of the invention can be achieved by the following technical scheme:
an acid corrosion resistant paint for the inner wall of a reaction kettle comprises the following raw materials in parts by weight:
100-120 parts of fluororubber, 260-280 parts of solvent, 30-35 parts of modifier, 5-8 parts of composite vulcanizing agent, 12-15 parts of filler, 1-2 parts of defoamer and 0.5-1 part of flatting agent.
Further, the modifier is prepared by the following steps:
and adding p-phenylenediamine and absolute ethyl alcohol into the purified graphene, carrying out reflux condensation reaction for 10 hours at 70 ℃, carrying out suction filtration, and washing with acetone for three times to obtain the modifier.
Further, the dosage ratio of the purified graphene to the p-phenylenediamine to the absolute ethyl alcohol is 20-22g:20g:300mL.
Further, the purified graphene is prepared by the following steps:
a1, stirring and adding H into graphene 3 PO 4 Then 98% of H is added 2 SO 4 Stirring in ice bath for 10min, and slowly adding KMnO 4 Control KMnO 4 The addition rate of the catalyst is ensured to ensure that the temperature of the system is less than 5 ℃;
A2、KMnO 4 after the addition is completed, the ice bath reaction is continued for 2 hours, the temperature is raised to 50-55 ℃, the constant temperature stirring reaction is carried out for 1 hour, the heating is stopped, the cooling is carried out to the room temperature, the ice water added into the reaction kettle is diluted, the ice bath stirring is continued, and 30 percent of H is added into the reaction kettle 2 O 2， Continuously stirring until the solution turns to golden yellow, standing for 24 hours, carrying out suction filtration, stirring and dispersing solid components by using 1% HCl, carrying out suction filtration, and stirring and dispersing solid components by using 70% acetone aqueous solution;
a3, adding 5% NaHCO into the mixture 3 And regulating the pH of the solution to 6.8-7.2, performing ultrasonic oscillation for 4 hours, performing suction filtration, washing with distilled water for three times, and performing suction filtration to obtain the purified graphene.
Further, the graphene and H 3 PO 4 、H 2 SO 4 、KMnO 4 Ice water, H 2 O 2 、HClAnd the dosage ratio of the acetone aqueous solution is 35-40g:130mL:1100mL:110-120g:4000mL:30-35mL:1000mL:1000mL.
Further, the solvent is n-butanol acetate and cyclohexanone according to 3:1, and mixing.
Further, the fluororubber is bisphenol fluororubber GN-47.
Further, the composite vulcanizing agent is bisphenol AF and a vulcanization accelerator BPP according to the mass ratio of 10:1 are mixed and prepared.
Further, the filler is one of carbon black and barium sulfate.
Further, the defoamer is defoamer MAA.
Further, the leveling agent is a leveling agent 232.
Further, the preparation method of the acid corrosion resistant paint on the inner wall of the reaction kettle comprises the following steps:
after the fluororubber is crushed, stirring and adding a solvent at 50-65 ℃, stirring until the fluororubber is completely dissolved, adding a modifier, a filler, a defoaming agent and a leveling agent, stirring for 30min, then introducing a grinder for circulating grinding, dispersing at a high speed by a dispersing agent, filtering, finally adding a compound vulcanizing agent, and stirring for 15-20min to obtain the acid corrosion resistant coating on the inner wall of the reaction kettle.
The invention has the beneficial effects that:
the acid corrosion resistant coating prepared by the invention takes fluororubber as a basic film forming substance, the fluororubber has excellent chemical corrosion resistance, carbon black and barium sulfate are added as fillers, the carbon black and the barium sulfate have chemical inertness, are not easy to react with chemical acid corrosion medium and are not easy to be corroded, and the acid corrosion resistant performance of the barium sulfate is optimal.
According to the invention, the modified Hummers method is adopted to oxidize natural graphite, the purified graphene is prepared by ultrasonic stripping, the graphene has excellent high temperature resistance and corrosion resistance, but the graphene surface has a large number of polar groups, and the defects of difficult dispersion, easy flocculation and the like exist.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparing a modifier:
a1, adding 130mL of H to 35g of graphene under stirring 3 PO 4 1100mL of 98% H are added 2 SO 4 Stirring in ice bath for 10min, and slowly adding 110g KMnO 4 Control KMnO 4 The addition rate of the catalyst is ensured to ensure that the temperature of the system is less than 5 ℃;
A2、KMnO 4 after the addition was completed, the ice bath reaction was continued for 2 hours, the temperature was raised to 50℃and the stirring reaction was continued for 1 hour at constant temperature, then the heating was stopped, the reaction was cooled to room temperature, 4000mL of ice water was added thereto for dilution, the ice bath stirring was continued, and 30mL of 30% H was added thereto 2 O 2， Continuously stirring until the solution turns to golden yellow, standing for 24 hours, carrying out suction filtration, stirring and dispersing solid components by using 1000mL of 1% HCl, carrying out suction filtration, and stirring and dispersing solid components by using 2000mL of 70% acetone aqueous solution;
a3, adding 5% NaHCO into the mixture 3 Adjusting the pH of the solution to 6.8, performing ultrasonic oscillation for 4 hours, performing suction filtration, washing with distilled water for three times, and performing suction filtration to obtain purified graphene;
and A4, adding 20g of p-phenylenediamine and 300mL of absolute ethyl alcohol into 20g of purified graphene, carrying out reflux condensation reaction for 10 hours at 70 ℃, carrying out suction filtration, and washing with acetone for three times to obtain the modifier.
Example 2
Preparing a modifier:
A1130mL of H was added to 40g of graphene with stirring 3 PO 4 1100mL of 98% H are added 2 SO 4 Stirring in ice bath for 10min, and slowly adding 120g KMnO 4 Control KMnO 4 The addition rate of the catalyst is ensured to ensure that the temperature of the system is less than 5 ℃;
A2、KMnO 4 after the addition was completed, the ice bath reaction was continued for 2 hours, the temperature was raised to 55℃and the stirring reaction was continued for 1 hour at constant temperature, then the heating was stopped, the reaction was cooled to room temperature, 4000mL of ice water was added thereto for dilution, the ice bath stirring was continued, and 35mL of 30% H was added thereto 2 O 2， Continuously stirring until the solution turns to golden yellow, standing for 24 hours, carrying out suction filtration, stirring and dispersing solid components by using 1000mL of 1% HCl, carrying out suction filtration, and stirring and dispersing solid components by using 2000mL of 70% acetone aqueous solution;
a3, adding 5% NaHCO into the mixture 3 Adjusting the pH of the solution to 7.2, performing ultrasonic oscillation for 4 hours, performing suction filtration, washing with distilled water for three times, and performing suction filtration to obtain purified graphene;
and A4, adding 20g of p-phenylenediamine and 300mL of absolute ethyl alcohol into 22g of purified graphene, carrying out reflux condensation reaction for 10 hours at 70 ℃, carrying out suction filtration, and washing with acetone for three times to obtain the modifier.
Example 3
Preparing a corrosion-resistant coating:
firstly, the corrosion-resistant coating comprises the following raw materials in parts by weight:
100 parts of fluororubber, 260 parts of solvent, 30 parts of modifier prepared in example 1, 5 parts of composite vulcanizing agent, 12 parts of filler, 1 part of defoamer and 0.5 part of flatting agent;
wherein the solvent is n-butanol acetate and cyclohexanone according to 3:1, mixing;
the fluororubber is bisphenol fluororubber GN-47;
the composite vulcanizing agent is bisphenol AF and vulcanization accelerator BPP according to the mass ratio of 10:1, mixing and preparing;
the filler is carbon black;
the defoamer is defoamer MAA;
the leveling agent is leveling agent 232.
The preparation process comprises the following steps:
after the fluororubber is crushed, stirring and adding a solvent at 50 ℃, stirring until the fluororubber is completely dissolved, adding a modifier, a filler, a defoaming agent and a leveling agent, stirring for 30min, then introducing a grinder for circulating grinding, dispersing at high speed by a dispersing agent, filtering, finally adding a compound vulcanizing agent, and stirring for 15min to obtain the acid corrosion resistant paint for the inner wall of the reaction kettle.
Example 4
Preparing a corrosion-resistant coating:
firstly, the corrosion-resistant coating comprises the following raw materials in parts by weight:
120 parts of fluororubber, 280 parts of solvent, 35 parts of modifier prepared in example 2, 8 parts of composite vulcanizing agent, 15 parts of filler, 2 parts of defoamer and 1 part of flatting agent;
wherein the solvent is n-butanol acetate and cyclohexanone according to 3:1, mixing;
the fluororubber is bisphenol fluororubber GN-47;
the composite vulcanizing agent is bisphenol AF and vulcanization accelerator BPP according to the mass ratio of 10:1, mixing and preparing;
the filler is barium sulfate;
the defoamer is defoamer MAA;
the leveling agent is leveling agent 232.
The preparation process comprises the following steps:
after the fluororubber is crushed, stirring and adding a solvent at 65 ℃, stirring until the fluororubber is completely dissolved, adding a modifier, a filler, a defoaming agent and a leveling agent, stirring for 30min, then introducing a grinder for circulating grinding, dispersing at high speed by a dispersing agent, filtering, finally adding a compound vulcanizing agent, and stirring for 20min to obtain the acid corrosion resistant paint for the inner wall of the reaction kettle.
Comparative example 1:
the modifier prepared in the example 1 is removed from the raw materials in the example 3, the rest raw materials and the preparation process are unchanged, and finally the acid corrosion resistant paint for the inner wall of the reaction kettle is prepared.
Comparative example 2:
and (3) removing the filler in the raw materials in the embodiment 4, and finally preparing the acid corrosion resistant coating on the inner wall of the reaction kettle, wherein the rest raw materials and the preparation process are unchanged.
Performance tests were performed on examples 3-4 and comparative examples 1-2, with the following criteria, and the test results are shown in table 1:
and (3) corrosion resistance detection: each group of corrosion-resistant paint is coated on a plate with the thickness of 10cm x 10cm, and after the plate is dried, the corrosion resistance is detected, and specific detection standards are shown in the following table 1:
TABLE 1
As can be seen from Table 1, the acid corrosion resistant paint for the inner wall of the reaction kettle prepared by the invention has excellent high-temperature acid corrosion resistance.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The acid corrosion resistant paint for the inner wall of the reaction kettle is characterized by comprising the following raw materials in parts by weight:
100-120 parts of fluororubber, 260-280 parts of solvent, 30-35 parts of modifier, 5-8 parts of composite vulcanizing agent, 12-15 parts of filler, 1-2 parts of defoamer and 0.5-1 part of flatting agent;
the modifier is prepared by the following steps:
and adding p-phenylenediamine and absolute ethyl alcohol into the purified graphene, carrying out reflux condensation reaction for 10 hours at 70 ℃, carrying out suction filtration, and washing with acetone for three times to obtain the modifier.
2. The acid corrosion resistant paint for the inner wall of the reaction kettle according to claim 1, wherein the dosage ratio of the purified graphene to the p-phenylenediamine to the absolute ethyl alcohol is 20-22g:20g:300mL.
3. The acid corrosion resistant coating for the inner wall of the reaction kettle according to claim 1, wherein the purified graphene is prepared by the following steps:
a1, stirring and adding H into graphene 3 PO 4 Then 98% of H is added 2 SO 4 Stirring in ice bath for 10min, and slowly adding KMnO 4 Control KMnO 4 The addition rate of the catalyst is ensured to ensure that the temperature of the system is less than 5 ℃;
A2、KMnO 4 after the addition is completed, the ice bath reaction is continued for 2 hours, the temperature is raised to 50-55 ℃, the constant temperature stirring reaction is carried out for 1 hour, the heating is stopped, the cooling is carried out to the room temperature, the ice water added into the reaction kettle is diluted, the ice bath stirring is continued, and 30 percent of H is added into the reaction kettle 2 O 2 Continuously stirring until the solution turns to golden yellow, standing for 24 hours, carrying out suction filtration, stirring and dispersing solid components by using 1% HCl, carrying out suction filtration, and stirring and dispersing solid components by using 70% acetone aqueous solution;
a3, adding 5% NaHCO into the mixture 3 And regulating the pH of the solution to 6.8-7.2, performing ultrasonic oscillation for 4 hours, performing suction filtration, washing with distilled water for three times, and performing suction filtration to obtain the purified graphene.
4. An acid corrosion resistant paint for inner walls of reaction kettles according to claim 3, wherein said graphene and H are as follows 3 PO 4 、H 2 SO 4 、KMnO 4 Ice water, H 2 O 2 The dosage ratio of HCl to acetone aqueous solution is 35-40g:130mL:1100mL:110-120g：4000mL：30-35mL：1000mL：1000mL。
5. the acid corrosion resistant paint for the inner wall of a reaction kettle according to claim 1, wherein the solvent is n-butanol acetate and cyclohexanone according to the following formula 3:1, and mixing.
6. The acid corrosion resistant paint for the inner wall of the reaction kettle as claimed in claim 1, wherein the composite vulcanizing agent is bisphenol AF and vulcanization accelerator BPP according to the mass ratio of 10:1 are mixed and prepared.
7. The method for preparing the acid corrosion resistant paint for the inner wall of the reaction kettle according to claim 1, which is characterized by comprising the following steps:
after the fluororubber is crushed, stirring and adding a solvent at 50-65 ℃, stirring until the fluororubber is completely dissolved, adding a modifier, a filler, a defoaming agent and a leveling agent, stirring for 30min, then introducing a grinder for circulating grinding, dispersing at a high speed by a dispersing agent, filtering, finally adding a compound vulcanizing agent, and stirring for 15-20min to obtain the acid corrosion resistant coating on the inner wall of the reaction kettle.
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