CN118108515A - Method for preparing high-strength stemming from waste refractory materials - Google Patents
Method for preparing high-strength stemming from waste refractory materials Download PDFInfo
- Publication number
- CN118108515A CN118108515A CN202410235059.2A CN202410235059A CN118108515A CN 118108515 A CN118108515 A CN 118108515A CN 202410235059 A CN202410235059 A CN 202410235059A CN 118108515 A CN118108515 A CN 118108515A
- Authority
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- China
- Prior art keywords
- phenolic resin
- heating
- stemming
- simple substance
- aqueous solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 239000002699 waste material Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000011819 refractory material Substances 0.000 title claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 121
- 238000010438 heat treatment Methods 0.000 claims abstract description 110
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 102
- 239000000126 substance Substances 0.000 claims abstract description 84
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 66
- 238000003756 stirring Methods 0.000 claims abstract description 60
- 238000006243 chemical reaction Methods 0.000 claims abstract description 57
- 239000007864 aqueous solution Substances 0.000 claims abstract description 55
- 239000002131 composite material Substances 0.000 claims abstract description 55
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 49
- 229910052796 boron Inorganic materials 0.000 claims abstract description 47
- 238000000227 grinding Methods 0.000 claims abstract description 46
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000005011 phenolic resin Substances 0.000 claims abstract description 45
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 45
- 238000002156 mixing Methods 0.000 claims abstract description 44
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000243 solution Substances 0.000 claims abstract description 39
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 30
- 239000010703 silicon Substances 0.000 claims abstract description 30
- -1 silicon modified phenolic resin Chemical class 0.000 claims abstract description 29
- 239000011230 binding agent Substances 0.000 claims abstract description 27
- 239000004005 microsphere Substances 0.000 claims abstract description 27
- HXITXNWTGFUOAU-UHFFFAOYSA-N phenylboronic acid Chemical compound OB(O)C1=CC=CC=C1 HXITXNWTGFUOAU-UHFFFAOYSA-N 0.000 claims abstract description 26
- ICXMNILZYYOUSS-UHFFFAOYSA-N O1NC=CC2=C1C=CC=C2.[Si] Chemical compound O1NC=CC2=C1C=CC=C2.[Si] ICXMNILZYYOUSS-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000004821 distillation Methods 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 22
- 238000003825 pressing Methods 0.000 claims abstract description 22
- 229920002545 silicone oil Polymers 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 238000007599 discharging Methods 0.000 claims abstract description 11
- 230000001105 regulatory effect Effects 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims description 47
- 235000019441 ethanol Nutrition 0.000 claims description 36
- 238000000498 ball milling Methods 0.000 claims description 35
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 26
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 25
- 229910052804 chromium Inorganic materials 0.000 claims description 24
- 239000011651 chromium Substances 0.000 claims description 24
- 229910052782 aluminium Inorganic materials 0.000 claims description 23
- 239000011812 mixed powder Substances 0.000 claims description 22
- 239000002609 medium Substances 0.000 claims description 20
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 13
- 229920002866 paraformaldehyde Polymers 0.000 claims description 13
- HXLAEGYMDGUSBD-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propan-1-amine Chemical compound CCO[Si](C)(OCC)CCCN HXLAEGYMDGUSBD-UHFFFAOYSA-N 0.000 claims description 12
- 239000012300 argon atmosphere Substances 0.000 claims description 11
- 238000001723 curing Methods 0.000 claims description 11
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 11
- 238000007873 sieving Methods 0.000 claims description 11
- 238000001291 vacuum drying Methods 0.000 claims description 11
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 11
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 9
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000002274 desiccant Substances 0.000 claims description 5
- YYXFJSDMOVHLMJ-UHFFFAOYSA-N (4-hydroxyphenoxy)boronic acid Chemical compound OB(O)OC1=CC=C(O)C=C1 YYXFJSDMOVHLMJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002612 dispersion medium Substances 0.000 claims description 2
- CSDQQAQKBAQLLE-UHFFFAOYSA-N 4-(4-chlorophenyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine Chemical compound C1=CC(Cl)=CC=C1C1C(C=CS2)=C2CCN1 CSDQQAQKBAQLLE-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000002513 implantation Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 230000007935 neutral effect Effects 0.000 description 8
- 230000003628 erosive effect Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000011258 core-shell material Substances 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- TZHYBRCGYCPGBQ-UHFFFAOYSA-N [B].[N] Chemical compound [B].[N] TZHYBRCGYCPGBQ-UHFFFAOYSA-N 0.000 description 3
- 239000010426 asphalt Substances 0.000 description 3
- 229910052810 boron oxide Inorganic materials 0.000 description 3
- 239000000571 coke Substances 0.000 description 3
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 239000007767 bonding agent Substances 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical compound C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 description 1
- BCHZICNRHXRCHY-UHFFFAOYSA-N 2h-oxazine Chemical compound N1OC=CC=C1 BCHZICNRHXRCHY-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 241000283074 Equus asinus Species 0.000 description 1
- 238000006683 Mannich reaction Methods 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical group [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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Abstract
The invention relates to the technical field of stemming and discloses a method for preparing high-strength stemming by using waste refractory materials; comprises the following steps: adding sodium hydroxide solution into phenol, stirring uniformly, adding formaldehyde aqueous solution, heating to 60-65 ℃ for reaction for 1-1.5h, adding acetic acid aqueous solution for regulating pH to neutrality, heating to 78-80 ℃ for reduced pressure distillation, adding phenylboronic acid, heating to 90-95 ℃ for reaction for 1-1.5h, and carrying out reduced pressure distillation to obtain boron phenolic resin; adding silicone oil and boron phenolic resin into ethanol, uniformly stirring, adding oligomeric silazane and silicon benzoxazine, and stirring until no bubbles are generated, thus obtaining a silicon modified phenolic resin binder; adding the waste aggregate and the aggregate into a mixing mill for mixing and grinding, adding a silicon modified phenolic resin binder for mixing and grinding, adding simple substance composite microspheres for mixing and grinding, discharging, pressing, drying, embedding carbon, and performing heat treatment to obtain the high-strength stemming.
Description
Technical Field
The invention relates to the technical field of stemming, in particular to a method for preparing high-strength stemming by using waste refractory materials.
Background
Stemming is a widely used material in the manufacture of artillery to fill the internal cavities of the artillery, to increase the structural strength and to provide the support required for the explosion of explosives. The traditional stemming is usually prepared from silicate, quartz sand and other components, however, the materials have the defects of higher cost, complex preparation process, high resource consumption and the like.
With increasing importance on environmental protection and sustainable utilization of resources, the reuse of waste refractory materials is a potentially valuable topic. The waste refractory material is usually composed of alumina, silicate and the like, and can effectively reuse resources, thereby being expected to reduce the production cost and improve the performance of stemming.
In the prior art, the recycling of waste refractory materials is mainly focused on the recovery and smelting stages, and few methods can be directly applied to the preparation of high-performance stemming. Therefore, it is necessary to develop an innovative preparation method for converting waste refractory materials into stemming with high strength and high stability by an effective process means so as to meet the high requirements of military and industrial fields on the material performance. This not only helps to achieve recycling of resources, but also will provide a more economical, environmentally friendly solution for artillery manufacture.
Therefore, the method for preparing the high-strength stemming by using the waste refractory materials has important significance.
Disclosure of Invention
The invention aims to provide a method for preparing high-strength stemming by using waste refractory materials, which aims to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
a method for preparing high-strength stemming by using waste refractory materials comprises the following steps:
S1: adding three simple substance powders of chromium, aluminum and boron into a ball milling tank, ball milling for 6-8h, vacuum drying and sieving to obtain mixed powder; pressing the mixed powder into a blank, placing the blank in an argon atmosphere for heat treatment, and grinding to obtain simple substance composite powder;
The chromium: aluminum: the molar ratio of boron is 2 (1-1.2): 2; in the ball milling process, zirconium oxide is used as a ball milling medium, and absolute ethyl alcohol is used as a dispersion medium; the heat treatment temperature is 900 ℃ and is kept for 1-3 hours, and the heating rate is 5 ℃/min; the grain diameter of the fine powder obtained by grinding is less than or equal to 0.04mm;
S2: adding the simple substance composite powder into formaldehyde aqueous solution, performing ultrasonic dispersion, adding phenol and sodium hydroxide aqueous solution, heating to 80-85 ℃ for reaction for 6-6.5h, and continuously performing heat preservation reaction for 1.5-2h under the vacuum degree of 0.09-0.1MPa to obtain phenolic resin prepolymer; adding p-hydroxyphenylboric acid into formaldehyde aqueous solution under ice bath condition, and stirring uniformly to obtain a substance A; uniformly stirring phenolic resin prepolymer and ethanol, adding the mixture into ethanol solution, adding ethanol solution of a substance A, heating to 75-80 ℃ for reaction for 4-5h, centrifuging, washing, drying, and curing for 2-2.5h in an environment of 150-155 ℃ to obtain simple substance composite microspheres;
The concentration of the formaldehyde aqueous solution is 37-40wt% and the concentration of the sodium hydroxide aqueous solution is 16-20wt%; the simple substance composite powder comprises the following components: the mass ratio of the phenol is (2.5-5) 100; the phenolic resin prepolymer: the mass ratio of the p-hydroxyphenylboric acid is (10-20) to (15-25);
S3: adding sodium hydroxide solution into phenol, stirring uniformly, adding formaldehyde aqueous solution, heating to 60-65 ℃ for reaction for 1-1.5h, adding acetic acid aqueous solution for regulating pH to neutrality, heating to 78-80 ℃ for reduced pressure distillation, adding phenylboronic acid, heating to 90-95 ℃ for reaction for 1-1.5h, and carrying out reduced pressure distillation to obtain boron phenolic resin;
the phenol: formaldehyde: the mass ratio of the phenylboronic acid is 5 (2.6-3) to 0.5; the concentration of the acetic acid aqueous solution is 36-40wt%;
s4: adding paraformaldehyde and a drying agent into a dioxane solution of gamma-aminopropyl methyl diethoxy silane, uniformly stirring, adding phenol, heating to 100-105 ℃ for reaction for 6-6.5h, and purifying to obtain silicon benzoxazine;
The paraformaldehyde: and (3) drying agent: gamma-aminopropyl methyldiethoxysilane: the mass ratio of the phenol is (1-1.5) 1 (3-3.5) 1.5-2;
s5: adding silicone oil and boron phenolic resin into ethanol, uniformly stirring, adding oligomeric silazane and silicon benzoxazine, and stirring until no bubbles are generated, thus obtaining a silicon modified phenolic resin binder;
the silicon modified phenolic resin binder comprises, by mass, 46-47.5 parts of silicone oil, 46-47.5 parts of boron phenolic resin, 4-5 parts of oligomeric silazane and 1.5-3 parts of silicon benzoxazine;
S6: adding the waste aggregate and the aggregate into a mixing mill for mixing and grinding, adding a silicon modified phenolic resin binder for mixing and grinding, adding simple substance composite microspheres for mixing and grinding, discharging, pressing, drying, embedding carbon, and performing heat treatment to obtain the high-strength stemming.
The high-strength stemming comprises, by mass, 100-120 parts of waste aggregate and aggregate, 10-20 parts of a silicon modified phenolic resin binder and 1-3 parts of simple substance composite microspheres; the drying temperature is 100-200 ℃ and the time is 24 hours, and the heat treatment step is to place the blank pressed and formed before at 800 ℃, 1000 ℃, 1200 ℃, 1400 ℃ and 1600 ℃ under the condition of embedding carbon for heat treatment for 3 hours respectively.
The drying agent is any one of calcium hydride and anhydrous sodium sulfate;
In the waste aggregate and the aggregate, the waste auxiliary materials are recycled electric donkey aluminum material particles; the aggregate comprises any one or more of brown alumina, boron oxide, coke, silicon carbide, ball asphalt and clay.
Compared with the prior art, the invention has the following beneficial effects:
The invention prepares the compound (simple substance composite powder) except the ternary lamellar structure by controlling the raw material proportion of simple substance chromium powder, aluminum powder and boron powder; in order to improve the dispersion performance of the composite powder in stemming blanks, the composite microspheres are prepared by taking the prepared simple substance composite powder, phenol, formaldehyde and parahydroxyphenylboric acid as main raw materials through a suspension polycondensation method; the boron phenolic resin is coated to form a microsphere structure, so that simple substance composite powder can be uniformly dispersed in a silicon modified phenolic resin bonding agent prepared later, the bonding agent is uniformly dispersed in a stemming blank, finally, the internal simple substance composite powder is released by decomposing the outer layer of the simple substance composite microsphere in the heat treatment process of 800-1200 ℃ in a carbon-embedded step-by-step heat treatment mode, the simple substance composite powder is gradually decomposed to form a core-shell structure of aluminum oxide coated chromium boride, and carbon nanotubes and carbon fibers are generated in situ by catalysis of nano chromium and chromium oxide on the surface of the core-shell structure; the core-shell structure is accompanied with the internal in-situ generation of the layered boron nitride coated chromium carbide structure at 1200-1600 ℃, the silicon carbide whisker grows out of the surface of the core-shell structure in-situ, and in the whole structure evolution process, the internal matrix structure of the stemming is promoted to be more tightly combined, the densification is achieved, and the flexural strength of the stemming is further improved.
According to the invention, through Mannich reaction of phenol, paraformaldehyde and gamma-aminopropyl methyl diethoxy silane, silicon benzoxazine with oxazine and siloxane groups is synthesized; the problem of phase separation of silicone oil and phenolic aldehyde co-curing is solved by utilizing a mode of compatible benzoxazine and silamine boron nitrogen coordination, and the compatibility of the silicon oil and phenolic aldehyde co-curing monomer powder microsphere in a silicon modified phenolic resin binder can be further improved as a carrier of the previously prepared monomer powder microsphere, meanwhile, the boron nitrogen coordination resin containing organic silicon can provide higher carbon residue rate for stemming no matter in inert atmosphere or air, and the co-action of the boron nitrogen coordination resin and the organic silicone oil improves the hot corrosion resistance of the stemming, so that the prepared stemming has high-strength fracture resistance and hot corrosion resistance.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but 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.
In the following examples, brown fused alumina sizes of 0-1mm, 1-3mm, 200 mesh, purchased from Yingyang ternary abrasive mill; the boron oxide has a specification of 200 meshes and is purchased from Shanghai Michelin Biochemical technology Co., ltd; the coke specification is 0-1mm and 1-3mm, and is purchased from Shanghai Bao Steel coking plant; silicon carbide with the specification of 0-1mm and 200 meshes is purchased from Anyang Dongrui metallurgical refractory Co., ltd; ball asphalt specification 200 mesh, purchased from new materials technology limited of jersey, all state; clays are purchased from Jilin forest mining development Inc.; chromium powder with a specification of 10 μm, aluminum powder with a specification of 10 μm and boron powder with a specification of 1 μm were purchased from Shanghai lane field nanomaterials limited; silicone oil specification AS100, CAS:63148-58-3; paraformaldehyde was purchased from Shanghai Ala Biochemical technologies Co., ltd; the oligomeric silazanes were purchased from the national academy of sciences of chinese beijing; the rest raw materials are all sold in the market.
The waste aggregate comprises, by mass, 15 parts of waste aggregate, 40 parts of brown corundum, 1 part of boron oxide, 12 parts of coke, 16 parts of silicon nitride, 4 parts of ball asphalt and 12 parts of clay.
Example 1: a method for preparing high-strength stemming by using waste refractory materials comprises the following steps: s1: adding three simple substance powders of chromium, aluminum and boron into a ball milling tank, ball milling zirconium oxide serving as a ball milling medium and absolute ethyl alcohol serving as a dispersing medium for 6 hours, vacuum drying at 110 ℃, and sieving to obtain mixed powder; pressing the mixed powder into a blank, placing the blank in an argon atmosphere, heating to 900 ℃ at a heating rate of 5 ℃/min for heat treatment for 3 hours, and grinding to obtain simple substance composite powder;
wherein, chromium: aluminum: the molar ratio of boron is 2:1:2;
S2: adding 2.5g of simple substance composite powder into 37wt% formaldehyde aqueous solution, performing ultrasonic dispersion, adding 100g of phenol and 16wt% sodium hydroxide aqueous solution, heating to 80 ℃ for reaction for 6 hours, and continuously performing heat preservation reaction for 1.5 hours under the vacuum degree of 0.09MPa to obtain phenolic resin prepolymer; under ice bath condition, adding 15g of parahydroxyphenylboric acid into 37wt% formaldehyde aqueous solution, and uniformly stirring to obtain a substance A; uniformly stirring 10g of phenolic resin prepolymer and ethanol, adding the mixture into an ethanol solution, adding the ethanol solution of a substance A, heating to 75 ℃ for reaction for 4 hours, centrifuging, washing, drying, and curing in an environment of 150 ℃ for 2 hours to obtain simple substance composite microspheres;
S3: adding 16wt% sodium hydroxide solution into 5g of phenol, uniformly stirring, adding a formaldehyde aqueous solution with the concentration of 37wt% and 2.6g, heating to 60 ℃ for reaction for 1h, adding 36wt% acetic acid aqueous solution for regulating the pH to be neutral, heating to 78 ℃ for reduced pressure distillation, adding 0.5g of phenylboronic acid, heating to 90 ℃ for reaction for 1h, and carrying out reduced pressure distillation to obtain boron phenolic resin;
S4: adding 1g of paraformaldehyde and 1g of calcium hydride into 3g of dioxane solution of gamma-aminopropyl methyl diethoxy silane, uniformly stirring, adding 1.5g of phenol, heating to 100 ℃ for reaction for 6 hours, and purifying to obtain silicon benzoxazine;
S5: adding 47.5g of silicone oil and 47.5g of boron phenolic resin into ethanol, uniformly stirring, adding 3g of oligomeric silazane and 1.5g of silicon benzoxazine, and stirring until no bubbles are generated, thus obtaining a silicon modified phenolic resin binder;
S6: adding 100g of waste aggregate and aggregate into a mixing mill for mixing and grinding, adding 10g of silicon modified phenolic resin binder for mixing and grinding, adding 1g of simple substance composite microspheres for mixing and grinding, discharging, pressing, step drying, and respectively performing heat treatment on the pressed and formed blank for 3 hours at 800 ℃, 1000 ℃, 1200 ℃, 1400 ℃ and 1600 ℃ under the condition of carbon implantation to obtain the high-strength stemming.
Example 2: a method for preparing high-strength stemming by using waste refractory materials comprises the following steps: s1: adding three simple substance powders of chromium, aluminum and boron into a ball milling tank, ball milling zirconium oxide serving as a ball milling medium and absolute ethyl alcohol serving as a dispersing medium for 6 hours, vacuum drying at 110 ℃, and sieving to obtain mixed powder; pressing the mixed powder into a blank, placing the blank in an argon atmosphere, heating to 900 ℃ at a heating rate of 5 ℃/min for heat treatment for 3 hours, and grinding to obtain simple substance composite powder;
wherein, chromium: aluminum: the molar ratio of boron is 2:1.2:2;
The remaining steps were the same as in example 1.
Example 3: a method for preparing high-strength stemming by using waste refractory materials comprises the following steps: s1: adding three simple substance powders of chromium, aluminum and boron into a ball milling tank, ball milling zirconium oxide serving as a ball milling medium and absolute ethyl alcohol serving as a dispersing medium for 6 hours, vacuum drying at 110 ℃, and sieving to obtain mixed powder; pressing the mixed powder into a blank, placing the blank in an argon atmosphere, heating to 900 ℃ at a heating rate of 5 ℃/min for heat treatment for 3 hours, and grinding to obtain simple substance composite powder;
wherein, chromium: aluminum: the molar ratio of boron is 2:1.2:2;
S2: adding 5g of simple substance composite powder into 37wt% formaldehyde aqueous solution, performing ultrasonic dispersion, adding 100g of phenol and 16wt% sodium hydroxide aqueous solution, heating to 80 ℃ for reaction for 6 hours, and continuously performing heat preservation reaction for 1.5 hours under the vacuum degree of 0.09MPa to obtain phenolic resin prepolymer; under ice bath condition, adding 15g of parahydroxyphenylboric acid into 37wt% formaldehyde aqueous solution, and uniformly stirring to obtain a substance A; uniformly stirring 10g of phenolic resin prepolymer and ethanol, adding the mixture into an ethanol solution, adding the ethanol solution of a substance A, heating to 75 ℃ for reaction for 4 hours, centrifuging, washing, drying, and curing in an environment of 150 ℃ for 2 hours to obtain simple substance composite microspheres;
S3: adding 16wt% sodium hydroxide solution into 5g of phenol, uniformly stirring, adding a formaldehyde aqueous solution with the concentration of 37wt% and 2.6g, heating to 60 ℃ for reaction for 1h, adding 36wt% acetic acid aqueous solution for regulating the pH to be neutral, heating to 78 ℃ for reduced pressure distillation, adding 0.5g of phenylboronic acid, heating to 90 ℃ for reaction for 1h, and carrying out reduced pressure distillation to obtain boron phenolic resin;
S4: adding 1g of paraformaldehyde and 1g of calcium hydride into 3g of dioxane solution of gamma-aminopropyl methyl diethoxy silane, uniformly stirring, adding 1.5g of phenol, heating to 100 ℃ for reaction for 6 hours, and purifying to obtain silicon benzoxazine;
S5: adding 47.5g of silicone oil and 47.5g of boron phenolic resin into ethanol, uniformly stirring, adding 3g of oligomeric silazane and 1.5g of silicon benzoxazine, and stirring until no bubbles are generated, thus obtaining a silicon modified phenolic resin binder;
S6: adding 100g of waste aggregate and aggregate into a mixing mill for mixing and grinding, adding 10g of silicon modified phenolic resin binder for mixing and grinding, adding 1g of simple substance composite microspheres for mixing and grinding, discharging, pressing, step drying, and respectively performing heat treatment on the pressed and formed blank for 3 hours at 800 ℃, 1000 ℃, 1200 ℃, 1400 ℃ and 1600 ℃ under the condition of carbon implantation to obtain the high-strength stemming.
Example 4: a method for preparing high-strength stemming by using waste refractory materials comprises the following steps: s1: adding three simple substance powders of chromium, aluminum and boron into a ball milling tank, ball milling zirconium oxide serving as a ball milling medium and absolute ethyl alcohol serving as a dispersing medium for 6 hours, vacuum drying at 110 ℃, and sieving to obtain mixed powder; pressing the mixed powder into a blank, placing the blank in an argon atmosphere, heating to 900 ℃ at a heating rate of 5 ℃/min for heat treatment for 3 hours, and grinding to obtain simple substance composite powder;
wherein, chromium: aluminum: the molar ratio of boron is 2:1.2:2;
S2: adding 5g of simple substance composite powder into 37wt% formaldehyde aqueous solution, performing ultrasonic dispersion, adding 100g of phenol and 16wt% sodium hydroxide aqueous solution, heating to 80 ℃ for reaction for 6 hours, and continuously performing heat preservation reaction for 1.5 hours under the vacuum degree of 0.09MPa to obtain phenolic resin prepolymer; under ice bath condition, adding 20g of parahydroxyphenylboric acid into 37wt% formaldehyde aqueous solution, and stirring uniformly to obtain a substance A; uniformly stirring 25g of phenolic resin prepolymer and ethanol, adding the mixture into an ethanol solution, adding the ethanol solution of a substance A, heating to 75 ℃ for reaction for 4 hours, centrifuging, washing, drying, and curing in an environment of 150 ℃ for 2 hours to obtain simple substance composite microspheres;
S3: adding 16wt% sodium hydroxide solution into 5g of phenol, uniformly stirring, adding a formaldehyde aqueous solution with the concentration of 37wt% and 2.6g, heating to 60 ℃ for reaction for 1h, adding 36wt% acetic acid aqueous solution for regulating the pH to be neutral, heating to 78 ℃ for reduced pressure distillation, adding 0.5g of phenylboronic acid, heating to 90 ℃ for reaction for 1h, and carrying out reduced pressure distillation to obtain boron phenolic resin;
S4: adding 1g of paraformaldehyde and 1g of calcium hydride into 3g of dioxane solution of gamma-aminopropyl methyl diethoxy silane, uniformly stirring, adding 1.5g of phenol, heating to 100 ℃ for reaction for 6 hours, and purifying to obtain silicon benzoxazine;
S5: adding 47.5g of silicone oil and 47.5g of boron phenolic resin into ethanol, uniformly stirring, adding 3g of oligomeric silazane and 1.5g of silicon benzoxazine, and stirring until no bubbles are generated, thus obtaining a silicon modified phenolic resin binder;
S6: adding 100g of waste aggregate and aggregate into a mixing mill for mixing and grinding, adding 10g of silicon modified phenolic resin binder for mixing and grinding, adding 1g of simple substance composite microspheres for mixing and grinding, discharging, pressing, step drying, and respectively performing heat treatment on the pressed and formed blank for 3 hours at 800 ℃, 1000 ℃, 1200 ℃, 1400 ℃ and 1600 ℃ under the condition of carbon implantation to obtain the high-strength stemming.
Example 5: a method for preparing high-strength stemming by using waste refractory materials comprises the following steps: s1: adding three simple substance powders of chromium, aluminum and boron into a ball milling tank, ball milling zirconium oxide serving as a ball milling medium and absolute ethyl alcohol serving as a dispersing medium for 6 hours, vacuum drying at 110 ℃, and sieving to obtain mixed powder; pressing the mixed powder into a blank, placing the blank in an argon atmosphere, heating to 900 ℃ at a heating rate of 5 ℃/min for heat treatment for 3 hours, and grinding to obtain simple substance composite powder;
wherein, chromium: aluminum: the molar ratio of boron is 2:1.2:2;
S2: adding 5g of simple substance composite powder into 37wt% formaldehyde aqueous solution, performing ultrasonic dispersion, adding 100g of phenol and 16wt% sodium hydroxide aqueous solution, heating to 80 ℃ for reaction for 6 hours, and continuously performing heat preservation reaction for 1.5 hours under the vacuum degree of 0.09MPa to obtain phenolic resin prepolymer; under ice bath condition, adding 20g of parahydroxyphenylboric acid into 37wt% formaldehyde aqueous solution, and stirring uniformly to obtain a substance A; uniformly stirring 25g of phenolic resin prepolymer and ethanol, adding the mixture into an ethanol solution, adding the ethanol solution of a substance A, heating to 75 ℃ for reaction for 4 hours, centrifuging, washing, drying, and curing in an environment of 150 ℃ for 2 hours to obtain simple substance composite microspheres;
S3: adding 16wt% sodium hydroxide solution into 5g of phenol, uniformly stirring, adding a formaldehyde aqueous solution with the concentration of 37wt% and 2.6g, heating to 60 ℃ for reaction for 1h, adding 36wt% acetic acid aqueous solution for regulating the pH to be neutral, heating to 78 ℃ for reduced pressure distillation, adding 0.5g of phenylboronic acid, heating to 90 ℃ for reaction for 1h, and carrying out reduced pressure distillation to obtain boron phenolic resin;
S4: adding 1g of paraformaldehyde and 1g of calcium hydride into 3g of dioxane solution of gamma-aminopropyl methyl diethoxy silane, uniformly stirring, adding 1.5g of phenol, heating to 100 ℃ for reaction for 6 hours, and purifying to obtain silicon benzoxazine;
s5: adding 46g of silicone oil and 46g of boron phenolic resin into ethanol, uniformly stirring, adding 5g of oligomeric silazane and 3g of silicon benzoxazine, and stirring until no bubbles are generated, thus obtaining a silicon modified phenolic resin binder;
S6: adding 100g of waste aggregate and aggregate into a mixing mill for mixing and grinding, adding 10g of silicon modified phenolic resin binder for mixing and grinding, adding 1g of simple substance composite microspheres for mixing and grinding, discharging, pressing, step drying, and respectively performing heat treatment on the pressed and formed blank for 3 hours at 800 ℃, 1000 ℃, 1200 ℃, 1400 ℃ and 1600 ℃ under the condition of carbon implantation to obtain the high-strength stemming.
Example 6: a method for preparing high-strength stemming by using waste refractory materials comprises the following steps: s1: adding three simple substance powders of chromium, aluminum and boron into a ball milling tank, ball milling zirconium oxide serving as a ball milling medium and absolute ethyl alcohol serving as a dispersing medium for 6 hours, vacuum drying at 110 ℃, and sieving to obtain mixed powder; pressing the mixed powder into a blank, placing the blank in an argon atmosphere, heating to 900 ℃ at a heating rate of 5 ℃/min for heat treatment for 3 hours, and grinding to obtain simple substance composite powder;
wherein, chromium: aluminum: the molar ratio of boron is 2:1.2:2;
S2: adding 5g of simple substance composite powder into 37wt% formaldehyde aqueous solution, performing ultrasonic dispersion, adding 100g of phenol and 16wt% sodium hydroxide aqueous solution, heating to 80 ℃ for reaction for 6 hours, and continuously performing heat preservation reaction for 1.5 hours under the vacuum degree of 0.09MPa to obtain phenolic resin prepolymer; under ice bath condition, adding 20g of parahydroxyphenylboric acid into 37wt% formaldehyde aqueous solution, and stirring uniformly to obtain a substance A; uniformly stirring 25g of phenolic resin prepolymer and ethanol, adding the mixture into an ethanol solution, adding the ethanol solution of a substance A, heating to 75 ℃ for reaction for 4 hours, centrifuging, washing, drying, and curing in an environment of 150 ℃ for 2 hours to obtain simple substance composite microspheres;
S3: adding 16wt% sodium hydroxide solution into 5g of phenol, uniformly stirring, adding a formaldehyde aqueous solution with the concentration of 37wt% and 2.6g, heating to 60 ℃ for reaction for 1h, adding 36wt% acetic acid aqueous solution for regulating the pH to be neutral, heating to 78 ℃ for reduced pressure distillation, adding 0.5g of phenylboronic acid, heating to 90 ℃ for reaction for 1h, and carrying out reduced pressure distillation to obtain boron phenolic resin;
S4: adding 1g of paraformaldehyde and 1g of calcium hydride into 3g of dioxane solution of gamma-aminopropyl methyl diethoxy silane, uniformly stirring, adding 1.5g of phenol, heating to 100 ℃ for reaction for 6 hours, and purifying to obtain silicon benzoxazine;
s5: adding 46g of silicone oil and 46g of boron phenolic resin into ethanol, uniformly stirring, adding 5g of oligomeric silazane and 3g of silicon benzoxazine, and stirring until no bubbles are generated, thus obtaining a silicon modified phenolic resin binder;
S6: adding 100g of waste aggregate and aggregate into a mixing mill for mixing and grinding, adding 20g of silicon modified phenolic resin binder for mixing and grinding, adding 3g of simple substance composite microspheres for mixing and grinding, discharging, pressing, step drying, and respectively performing heat treatment on the pressed and formed blank for 3 hours at 800 ℃, 1000 ℃, 1200 ℃, 1400 ℃ and 1600 ℃ under the condition of carbon implantation to obtain the high-strength stemming.
Comparative example 1: a method for preparing high-strength stemming by using waste refractory materials comprises the following steps: s1: adding three simple substance powders of chromium, aluminum and boron into a ball milling tank, ball milling zirconium oxide serving as a ball milling medium and absolute ethyl alcohol serving as a dispersing medium for 6 hours, vacuum drying at 110 ℃, and sieving to obtain mixed powder; pressing the mixed powder into a blank, placing the blank in an argon atmosphere, heating to 900 ℃ at a heating rate of 5 ℃/min for heat treatment for 3 hours, and grinding to obtain simple substance composite powder;
wherein, chromium: aluminum: the molar ratio of boron is 2:1:2;
S2: adding 16wt% sodium hydroxide solution into 5g of phenol, uniformly stirring, adding a formaldehyde aqueous solution with the concentration of 37wt% and 2.6g, heating to 60 ℃ for reaction for 1h, adding 36wt% acetic acid aqueous solution for regulating the pH to be neutral, heating to 78 ℃ for reduced pressure distillation, adding 0.5g of phenylboronic acid, heating to 90 ℃ for reaction for 1h, and carrying out reduced pressure distillation to obtain boron phenolic resin;
S3: adding 1g of paraformaldehyde and 1g of calcium hydride into 3g of dioxane solution of gamma-aminopropyl methyl diethoxy silane, uniformly stirring, adding 1.5g of phenol, heating to 100 ℃ for reaction for 6 hours, and purifying to obtain silicon benzoxazine;
s4: adding 47.5g of silicone oil and 1.5g of boron phenolic resin into ethanol, uniformly stirring, adding 3g of oligomeric silazane and 47.5g of silicon benzoxazine, and stirring until no bubbles are generated, thus obtaining a silicon modified phenolic resin binder;
s5: adding 100g of waste aggregate and aggregate into a mixing mill for mixing and grinding, adding 10g of silicon modified phenolic resin binder for mixing and grinding, adding 1g of simple substance composite powder for mixing and grinding, discharging, pressing, step drying, and respectively performing heat treatment on the pressed and formed blank for 3 hours at 800 ℃, 1000 ℃, 1200 ℃, 1400 ℃ and 1600 ℃ under the condition of carbon implantation to obtain the high-strength stemming.
Comparative example 2: a method for preparing high-strength stemming by using waste refractory materials comprises the following steps: s1: adding three simple substance powders of chromium, aluminum and boron into a ball milling tank, ball milling zirconium oxide serving as a ball milling medium and absolute ethyl alcohol serving as a dispersing medium for 6 hours, vacuum drying at 110 ℃, and sieving to obtain mixed powder; pressing the mixed powder into a blank, placing the blank in an argon atmosphere, heating to 900 ℃ at a heating rate of 5 ℃/min for heat treatment for 3 hours, and grinding to obtain simple substance composite powder;
wherein, chromium: aluminum: the molar ratio of boron is 2:1:2;
S2: adding 2.5g of simple substance composite powder into 37wt% formaldehyde aqueous solution, performing ultrasonic dispersion, adding 100g of phenol and 16wt% sodium hydroxide aqueous solution, heating to 80 ℃ for reaction for 6 hours, and continuously performing heat preservation reaction for 1.5 hours under the vacuum degree of 0.09MPa to obtain phenolic resin prepolymer; under ice bath condition, adding 15g of parahydroxyphenylboric acid into 37wt% formaldehyde aqueous solution, and uniformly stirring to obtain a substance A; uniformly stirring 10g of phenolic resin prepolymer and ethanol, adding the mixture into an ethanol solution, adding the ethanol solution of a substance A, heating to 75 ℃ for reaction for 4 hours, centrifuging, washing, drying, and curing in an environment of 150 ℃ for 2 hours to obtain simple substance composite microspheres;
S3: adding 16wt% sodium hydroxide solution into 5g of phenol, uniformly stirring, adding a formaldehyde aqueous solution with the concentration of 37wt% and 2.6g, heating to 60 ℃ for reaction for 1h, adding 36wt% acetic acid aqueous solution for regulating the pH to be neutral, heating to 78 ℃ for reduced pressure distillation, adding 0.5g of phenylboronic acid, heating to 90 ℃ for reaction for 1h, and carrying out reduced pressure distillation to obtain boron phenolic resin;
s4: adding 47.5g of silicone oil and 47.5g of boron phenolic resin into ethanol, uniformly stirring, adding 3g of oligomeric silazane, and stirring until no bubbles are generated, thus obtaining a silicon modified phenolic resin binder;
S5: adding 100g of waste aggregate and aggregate into a mixing mill for mixing and grinding, adding 10g of silicon modified phenolic resin binder for mixing and grinding, adding 1g of simple substance composite microspheres for mixing and grinding, discharging, pressing, step drying, and respectively performing heat treatment on the pressed and formed blank for 3 hours at 800 ℃, 1000 ℃, 1200 ℃, 1400 ℃ and 1600 ℃ under the condition of carbon implantation to obtain the high-strength stemming.
Comparative example 3: a method for preparing high-strength stemming by using waste refractory materials comprises the following steps: s1: adding three simple substance powders of chromium, aluminum and boron into a ball milling tank, ball milling zirconium oxide serving as a ball milling medium and absolute ethyl alcohol serving as a dispersing medium for 6 hours, vacuum drying at 110 ℃, and sieving to obtain mixed powder; pressing the mixed powder into a blank, placing the blank in an argon atmosphere, heating to 900 ℃ at a heating rate of 5 ℃/min for heat treatment for 3 hours, and grinding to obtain simple substance composite powder;
wherein, chromium: aluminum: the molar ratio of boron is 2:1:2;
s2: adding 10g of simple substance composite powder into 37wt% formaldehyde aqueous solution, performing ultrasonic dispersion, adding 100g of phenol and 16wt% sodium hydroxide aqueous solution, heating to 80 ℃ for reaction for 6 hours, and continuously performing heat preservation reaction for 1.5 hours under the vacuum degree of 0.09MPa to obtain phenolic resin prepolymer; under ice bath condition, adding 15g of parahydroxyphenylboric acid into 37wt% formaldehyde aqueous solution, and uniformly stirring to obtain a substance A; uniformly stirring 10g of phenolic resin prepolymer and ethanol, adding the mixture into an ethanol solution, adding the ethanol solution of a substance A, heating to 75 ℃ for reaction for 4 hours, centrifuging, washing, drying, and curing in an environment of 150 ℃ for 2 hours to obtain simple substance composite microspheres;
S3: adding 16wt% sodium hydroxide solution into 5g of phenol, uniformly stirring, adding a formaldehyde aqueous solution with the concentration of 37wt% and 2.6g, heating to 60 ℃ for reaction for 1h, adding 36wt% acetic acid aqueous solution for regulating the pH to be neutral, heating to 78 ℃ for reduced pressure distillation, adding 0.5g of phenylboronic acid, heating to 90 ℃ for reaction for 1h, and carrying out reduced pressure distillation to obtain boron phenolic resin;
S4: adding 1g of paraformaldehyde and 1g of calcium hydride into 3g of dioxane solution of gamma-aminopropyl methyl diethoxy silane, uniformly stirring, adding 1.5g of phenol, heating to 100 ℃ for reaction for 6 hours, and purifying to obtain silicon benzoxazine;
S5: adding 47.5g of silicone oil and 47.5g of boron phenolic resin into ethanol, uniformly stirring, adding 3g of oligomeric silazane and 1.5g of silicon benzoxazine, and stirring until no bubbles are generated, thus obtaining a silicon modified phenolic resin binder;
S6: adding 100g of waste aggregate and aggregate into a mixing mill for mixing and grinding, adding 10g of silicon modified phenolic resin binder for mixing and grinding, adding 5g of simple substance composite microspheres for mixing and grinding, discharging, pressing, step drying, and respectively performing heat treatment on the pressed and formed blank for 3 hours at 800 ℃, 1000 ℃, 1200 ℃, 1400 ℃ and 1600 ℃ under the condition of carbon implantation to obtain the high-strength stemming.
And (3) testing: mechanical property test:
The sample bars pressed by the above examples and comparative examples are cylindrical samples with the specification of phi 50mm multiplied by 50 mm; the normal temperature compressive strength was measured according to GB/T5072-2008. The high-temperature flexural strength is tested according to GB/T3007-2004;
Slag erosion resistance:
The sample bars pressed by the above examples and comparative examples are of a crucible sample with the external shape phi 50mm multiplied by 50mm and the internal diameter phi 30mm multiplied by 25mm, and after being dried for 24 hours at 200 ℃, slag is added, and after a cover plate is added, the sample bars are heat treated for 3 hours in a reducing atmosphere at 1450 ℃, the axes are cooled and observed, and the erosion condition is observed; wherein the slag components are 8.6wt% of alumina, 38.25wt% of silicon dioxide, 42.66wt% of calcium oxide, 7.4wt% of magnesium oxide, 1.58wt% of ferric oxide and 0.51wt% of manganese oxide; the boundary shape of the sample after erosion is studied, and the erosion degree of the sample is represented by the change of the boundary shape. According to the fractal dimension theory, the fractal dimension Rf of the refractory material after erosion is defined, the Rf takes a value of 1-2, and the smaller Rf is, the better the erosion resistance is.
Table high strength stemming capability test data table
Conclusion: the high-strength stemming prepared by the method has excellent mechanical property and hot erosion resistance; the direct addition of the simple substance composite powder in comparative example 1 results in reduced dispersion performance, the lack of compatibility of the silicon benzoxazine in comparative example 2 results in reduced compatibility, and the inclusion of excessive simple substance powder in the stemming blank in comparative example 3 results in reduced internal oxygen partial pressure and excessive filling of pores, which is unfavorable for growth of silicon carbide whiskers and eventually leads to reduced performance.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing high-strength stemming by using waste refractory materials is characterized by comprising the following steps: comprises the following steps:
S1: adding sodium hydroxide solution into phenol, stirring uniformly, adding formaldehyde aqueous solution, heating to 60-65 ℃ for reaction for 1-1.5h, adding acetic acid aqueous solution for regulating pH to neutrality, heating to 78-80 ℃ for reduced pressure distillation, adding phenylboronic acid, heating to 90-95 ℃ for reaction for 1-1.5h, and carrying out reduced pressure distillation to obtain boron phenolic resin;
S2: adding silicone oil and boron phenolic resin into ethanol, uniformly stirring, adding oligomeric silazane and silicon benzoxazine, and stirring until no bubbles are generated, thus obtaining a silicon modified phenolic resin binder;
S3: adding the waste aggregate and the aggregate into a mixing mill for mixing and grinding, adding a silicon modified phenolic resin binder for mixing and grinding, adding simple substance composite microspheres for mixing and grinding, discharging, pressing, drying, embedding carbon, and performing heat treatment to obtain the high-strength stemming.
2. The method for preparing high-strength stemming from waste refractory materials according to claim 1, wherein the method comprises the following steps: the preparation method of the simple substance composite microsphere comprises the following steps:
Adding the simple substance composite powder into formaldehyde aqueous solution, performing ultrasonic dispersion, adding phenol and sodium hydroxide aqueous solution, heating to 80-85 ℃ for reaction for 6-6.5h, and continuously performing heat preservation reaction for 1.5-2h under the vacuum degree of 0.09-0.1MPa to obtain phenolic resin prepolymer; adding p-hydroxyphenylboric acid into formaldehyde aqueous solution under ice bath condition, and stirring uniformly to obtain a substance A; stirring phenolic resin prepolymer and ethanol uniformly, adding ethanol solution of substance A, heating to 75-80 ℃ for reacting for 4-5h, centrifuging, washing, drying, and curing for 2-2.5h in 150-155 ℃ environment to obtain the simple substance composite microsphere.
3. The method for preparing high-strength stemming from waste refractory materials according to claim 2, wherein: the concentration of the formaldehyde aqueous solution is 37-40wt% and the concentration of the sodium hydroxide aqueous solution is 16-20wt%; the simple substance composite powder comprises the following components: the mass ratio of the phenol is (2.5-5) 100; the phenolic resin prepolymer: the mass ratio of the parahydroxyphenylboric acid is (10-20) to (15-25).
4. The method for preparing high-strength stemming from waste refractory materials according to claim 2, wherein: the preparation method of the simple substance composite powder comprises the following steps:
Adding three simple substance powders of chromium, aluminum and boron into a ball milling tank, ball milling for 6-8h, vacuum drying and sieving to obtain mixed powder; pressing the mixed powder into a blank, placing the blank in an argon atmosphere for heat treatment, and grinding to obtain the simple substance composite powder.
5. The method for preparing high-strength stemming from waste refractory materials according to claim 4, wherein: the chromium: aluminum: the molar ratio of boron is 2 (1-1.2): 2; in the ball milling process, zirconium oxide is used as a ball milling medium, and absolute ethyl alcohol is used as a dispersion medium; the heat treatment temperature is 900 ℃ and is kept for 1-3 hours, and the heating rate is 5 ℃/min; the grain diameter of the fine powder obtained by grinding is less than or equal to 0.04mm.
6. The method for preparing high-strength stemming from waste refractory materials according to claim 1, wherein the method comprises the following steps: the preparation method of the silicon benzoxazine comprises the following steps:
adding paraformaldehyde and a drying agent into a dioxane solution of gamma-aminopropyl methyl diethoxy silane, uniformly stirring, adding phenol, heating to 100-105 ℃ for reaction for 6-6.5h, and purifying to obtain the silicon benzoxazine.
7. The method for preparing high-strength stemming from waste refractory materials according to claim 6, wherein: the paraformaldehyde: and (3) drying agent: gamma-aminopropyl methyldiethoxysilane: the mass ratio of the phenol is (1-1.5) 1 (3-3.5) 1.5-2.
8. The method for preparing high-strength stemming from waste refractory materials according to claim 1, wherein the method comprises the following steps: in step S1, the phenol: formaldehyde: the mass ratio of the phenylboronic acid is 5 (2.6-3) to 0.5; the concentration of the acetic acid aqueous solution is 36-40wt%.
9. The method for preparing high-strength stemming from waste refractory materials according to claim 1, wherein the method comprises the following steps: in the step S2, the silicon modified phenolic resin binder comprises 46-47.5 parts of silicone oil, 46-47.5 parts of boron phenolic resin, 4-5 parts of oligomeric silazane and 1.5-3 parts of silicon benzoxazine according to parts by weight.
10. The method for preparing high-strength stemming from waste refractory materials according to claim 1, wherein the method comprises the following steps: in the step S3, the proportion of each component in the high-strength stemming is calculated according to the mass parts, 100-120 parts of waste aggregate and aggregate, 10-20 parts of silicon modified phenolic resin binder and 1-3 parts of simple substance composite microspheres; the drying temperature is 100-200 ℃ and the time is 24 hours, and the heat treatment step is to place the blank pressed and formed before at 800 ℃, 1000 ℃, 1200 ℃, 1400 ℃ and 1600 ℃ under the condition of embedding carbon for heat treatment for 3 hours respectively.
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