CN114592123A - Chromium ore powder ball and preparation method thereof - Google Patents
Chromium ore powder ball and preparation method thereof Download PDFInfo
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- CN114592123A CN114592123A CN202111616607.9A CN202111616607A CN114592123A CN 114592123 A CN114592123 A CN 114592123A CN 202111616607 A CN202111616607 A CN 202111616607A CN 114592123 A CN114592123 A CN 114592123A
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- bentonite
- chromium ore
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- ore powder
- stirring
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 77
- 239000011651 chromium Substances 0.000 title claims abstract description 77
- 239000000843 powder Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims description 19
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 101
- 239000000440 bentonite Substances 0.000 claims abstract description 101
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 101
- 229920001721 polyimide Polymers 0.000 claims abstract description 66
- 239000004642 Polyimide Substances 0.000 claims abstract description 63
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910000077 silane Inorganic materials 0.000 claims abstract description 54
- 239000008188 pellet Substances 0.000 claims abstract description 49
- 239000003822 epoxy resin Substances 0.000 claims abstract description 43
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 43
- 239000002131 composite material Substances 0.000 claims abstract description 41
- 239000011230 binding agent Substances 0.000 claims abstract description 31
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims abstract description 20
- 239000012975 dibutyltin dilaurate Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 10
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000001070 adhesive effect Effects 0.000 claims abstract description 7
- 239000000853 adhesive Substances 0.000 claims abstract description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 75
- 238000003756 stirring Methods 0.000 claims description 63
- AWJUIBRHMBBTKR-UHFFFAOYSA-N isoquinoline Chemical compound C1=NC=CC2=CC=CC=C21 AWJUIBRHMBBTKR-UHFFFAOYSA-N 0.000 claims description 52
- 238000006243 chemical reaction Methods 0.000 claims description 46
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 18
- SZEMGTQCPRNXEG-UHFFFAOYSA-M trimethyl(octadecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C SZEMGTQCPRNXEG-UHFFFAOYSA-M 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 13
- 238000004140 cleaning Methods 0.000 claims description 13
- 239000002244 precipitate Substances 0.000 claims description 13
- 238000001556 precipitation Methods 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- BLAKAEFIFWAFGH-UHFFFAOYSA-N acetyl acetate;pyridine Chemical compound C1=CC=NC=C1.CC(=O)OC(C)=O BLAKAEFIFWAFGH-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 239000000376 reactant Substances 0.000 claims description 11
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 238000009830 intercalation Methods 0.000 claims description 8
- 230000002687 intercalation Effects 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- 239000003208 petroleum Substances 0.000 claims description 6
- -1 hexafluoro dianhydride Chemical compound 0.000 claims description 4
- 238000003723 Smelting Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 238000003825 pressing Methods 0.000 description 6
- 230000009172 bursting Effects 0.000 description 5
- 229910000599 Cr alloy Inorganic materials 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000000788 chromium alloy Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000009719 polyimide resin Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 229910000604 Ferrochrome Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910003471 inorganic composite material Inorganic materials 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/24—Binding; Briquetting ; Granulating
- C22B1/2406—Binding; Briquetting ; Granulating pelletizing
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/24—Binding; Briquetting ; Granulating
- C22B1/242—Binding; Briquetting ; Granulating with binders
- C22B1/243—Binding; Briquetting ; Granulating with binders inorganic
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/24—Binding; Briquetting ; Granulating
- C22B1/242—Binding; Briquetting ; Granulating with binders
- C22B1/244—Binding; Briquetting ; Granulating with binders organic
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to the field of smelting materials, and discloses a chromium ore powder ball which comprises the following raw materials in parts by weight: 85-95 parts of chromium ore powder, 2-3 parts of binder and 2-3 parts of water; the adhesive comprises the following components in parts by weight: 6-7 parts of silane modified polyimide/bentonite composite material, 3-4 parts of silane modified epoxy resin, 0.01-0.03 part of dibutyltin dilaurate and 20-30 parts of tetrahydrofuran. The invention adopts the organic-inorganic composite binder to prepare the chromium ore powder into pellets, can reduce the use amount of the inorganic binder, avoid the influence on the grade of the chromium ore powder, and simultaneously can improve the strength and the thermal stability of the chromium ore powder pellets.
Description
Technical Field
The invention relates to the technical field of smelting materials, in particular to a chromium ore powder ball and a preparation method thereof.
Background
The chromium ore is the main raw material for smelting chromium alloy, and the blocky chromium ore is the best raw material in the chromium ore required by the production of the chromium alloy, because the blocky chromium ore and other raw materials enter the furnace in the production process of the chromium alloy, the air permeability in the furnace can be improved, the furnace is not easy to ignite, the dust is less, the furnace condition can be better controlled, and better economic and technical indexes can be obtained. But with the shortage of chromium ore resources, the output of lump ore is less and less, the grade is reduced, and the price is improved. Correspondingly, more and more chromium ore powder (the particle size is less than 10mm) is obtained by adopting the ore dressing method, chromium alloy production enterprises gradually start to use the powder ore to produce products such as ferrochrome and the like, and the use proportion of the powder ore of many enterprises is almost half. However, the direct feeding of the fine ore into the furnace can cause a series of process technical problems of poor air permeability of the submerged arc furnace, easy fire stabbing, large dust, unstable furnace condition and the like. Therefore, the fine ore must be agglomerated or pelletized to be used in large quantities for electric furnace smelting of chromium-based alloys.
At present, the method for preparing chromium ore powder into pellets mainly comprises a cold-pressing pellet process: mixing the chromium mineral powder and the binder, feeding the mixture into a stirrer, mixing the mixture, conveying the mixture to a ball press machine for ball pressing, and airing to obtain the chromium mineral powder balls. For example, in the chinese patent document, "a method for preparing pellets of chromium ore" disclosed in publication No. CN103436694A, the process for preparing the pellets comprises adding a binder, a slag former, a reducing agent and a modifier to chromium ore, mixing them uniformly, adding water to adjust the humidity, cold-pressing to prepare pellets, and naturally curing and air-drying to obtain finished pellets.
However, the chromium ore powder pellets prepared in the prior art have the following defects: 1. the specific gravity of the used binder is high, the quality is seriously reduced after the binder is pelletized, and the comprehensive grade of the chromium ore entering the furnace is influenced; 2. the pellet strength is low, the transportation is easy to damage and secondary pollution is generated; 3. the pellet bursting temperature is low, which is not beneficial to stabilizing the furnace condition.
Disclosure of Invention
In order to overcome the problems of the chromium ore powder pellets in the prior art, the invention provides the chromium ore powder pellets and the preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a chromium ore powder ball comprises the following raw materials in parts by weight: 85-95 parts of chromium ore powder, 2-3 parts of binder and 2-3 parts of water; the adhesive comprises the following components in parts by weight: 6-7 parts of silane modified polyimide/bentonite composite material, 3-4 parts of silane modified epoxy resin, 0.01-0.03 part of dibutyltin dilaurate and 20-30 parts of tetrahydrofuran.
In the chromium ore powder ball, the silane modified polyimide/bentonite composite material and the silane modified epoxy resin are used as main raw materials of the binder, and the water absorption performance of the bentonite is utilized to reduce the evaporation speed of water in the chromium ore powder ball, so that the vapor pressure in the ball is reduced, the bursting temperature of the ball is improved, the bursting pulverization rate of the chromium ore powder ball after entering a furnace is reduced, and the furnace condition is stabilized. However, the grade of the pellets is influenced by adding too much bentonite as an inorganic substance, so that the bentonite and the silane modified polyimide are compounded to prepare the organic-inorganic composite material, the using amount of the inorganic bentonite is reduced, organic components in the binder can be burnt and removed in the smelting process, and the slag amount in the smelting process is reduced. The polyimide in the silane modified polyimide/bentonite composite material has good high temperature resistance, is also beneficial to improving the thermal stability of pellets and reducing the burst rate of chromium ore powder pellets after entering a furnace, but the adhesive property of the polyimide is insufficient, so the silane modified epoxy resin is added into the adhesive to improve the adhesive property of the adhesive. In order to improve the strength of the chromium ore powder ball, silane groups are respectively introduced into polyimide and epoxy resin, after the binder is mixed with water, the silane groups in the silane modified polyimide and the silane modified epoxy resin can be hydrolyzed under the catalytic action of dibutyltin dilaurate, so that the polyimide and the epoxy resin are crosslinked and cured at room temperature, the curing temperature is reduced, and the curing time is shortened; and the strength of the chromium ore powder ball is improved through the co-crosslinking of the polyimide and the epoxy resin, and the damage of the ball in the transportation and use processes can be effectively reduced.
Preferably, the particle size of the chromium ore powder is 0-1 mm. Although the smaller the particle size of the chromium ore powder is, the more easy the chromium ore powder is to be pelletized, the smaller the particle size results in the more compact pellets, the moisture in the pellets is not easy to evaporate, and the vapor pressure in the pellets is larger, so the pellets produced by the chromium ore powder with the smaller particle size are usually easy to explode and pulverize, which is not favorable for the stability of the furnace condition. The invention can use chromium ore powder with smaller granularity to prepare chromium ore powder balls with higher bursting temperature by optimizing the components of the binder, and is beneficial to the application of the chromium ore powder balls.
Preferably, the preparation method of the silane modified polyimide/bentonite composite material comprises the following steps:
A) adding bentonite into an octadecyl trimethyl ammonium bromide solution, stirring uniformly, carrying out ultrasonic oscillation reaction for 2-4 h, and separating and drying a product to obtain primarily intercalated bentonite;
B) dissolving the bentonite subjected to preliminary intercalation in DMF to obtain a DMF solution of the bentonite;
C) dissolving 4,4' -diaminodiphenyl ether in DMF, uniformly stirring, adding hexafluoro dianhydride into the solution, stirring for reacting for 3-4 h, then adding a DMF solution of bentonite and isoquinoline, heating to 185-195 ℃, and continuing to stir for reacting for 8-10 h; transferring the product to ethanol for precipitation, separating and cleaning the precipitate, and drying to obtain the polyimide/bentonite composite material;
D) dissolving a polyimide/bentonite composite material in DMF, adding gamma-aminopropyltriethoxysilane into the solution at 0-4 ℃ under the protection of nitrogen, stirring and reacting for 2-4 h, heating to 45-55 ℃, adding isoquinoline and pyridine acetic anhydride, stirring and reacting for 8-10 h, transferring the product to petroleum ether for precipitation, separating and cleaning the precipitate, and drying to obtain the silane modified polyimide/bentonite composite material.
The method comprises the steps of firstly intercalating bentonite through octadecyl trimethyl ammonium bromide to preliminarily enlarge the interlayer spacing of the bentonite, then inserting polyimide into the interlayer of the bentonite by using 4,4' -diaminodiphenyl ether and hexafluoro dianhydride as monomers through a solution polymerization in-situ intercalation method to obtain a polyimide/bentonite composite material; and finally, capping the polyimide by using gamma-aminopropyltriethoxysilane to obtain the silane modified polyimide/bentonite composite material.
According to the invention, silane modified polyimide is inserted between layers of bentonite, and then the silane modified polyimide and silane modified epoxy resin are subjected to co-crosslinking, so that the lamellar structure of the bentonite has a restriction effect on polyimide molecules, and the high temperature resistance of the pellets can be further improved; meanwhile, the bentonite dissociated into the nano-structure can also become a crosslinking point, so that the strength of the pellet is further improved. Therefore, the invention can lead the prepared chromium ore powder ball to have good strength and thermal stability under the condition of less bentonite addition.
Preferably, the concentration of the octadecyl trimethyl ammonium bromide solution in the step A) is 0.5-1.0 mol/L, and the mass-volume ratio of the bentonite to the octadecyl trimethyl ammonium bromide solution is 1g: 50-100 mL; the mass concentration of the DMF solution of the bentonite obtained in the step B) is 1-3%.
Preferably, the molar ratio of the 4,4' -diaminodiphenyl ether to the hexafluoro dianhydride added in the step C) is 1-1.5: 1; the mass ratio of the 4,4' -diaminodiphenyl ether to the bentonite is 3-4: 1; the solid content of the reaction system is 10-15 wt%, and the addition amount of isoquinoline is 3-5% of the total mass of the reaction system.
Preferably, the mass ratio of the polyimide/bentonite composite material added in the step D) to the gamma-aminopropyltriethoxysilane is 12-15: 1, the solid content of the reaction system is 10-15 wt%, the addition amount of isoquinoline is 3-5% of the total mass of the reaction system, and the addition amount of pyridine acetic anhydride is 0.3-0.5% of the total mass of the reactants.
Preferably, the preparation method of the silane modified epoxy resin comprises the following steps: heating epoxy resin to 100-105 ℃, vacuumizing under a stirring state to remove water vapor, adding a solvent for dissolving, uniformly stirring, and then adding methyltrimethoxysilane and dibutyltin dilaurate, wherein the mass ratio of the epoxy resin to the methyltrimethoxysilane is 15-20: 1, and the adding amount of the dibutyltin dilaurate is 0.3-0.5% of the total mass of reactants; stirring and reacting for 3-5 h at 85-95 ℃, and vacuumizing to remove the solvent to obtain the silane modified epoxy resin.
The invention also discloses a preparation method of the chromium ore powder ball, which comprises the following steps: mixing the chromium ore powder and each component in the binder in proportion, adding atomized water, uniformly stirring, performing cold press molding to prepare pellets, and drying the pellets to obtain the chromium ore powder pellets.
Preferably, the pressure in cold press molding is 100 to 500 tons.
Preferably, the particle size of the pellets after cold press molding is 30-50 mm.
Therefore, the invention has the following beneficial effects:
(1) through the matching of bentonite, polyimide and epoxy resin, the prepared chromium ore powder balls have good strength and thermal stability while the binder does not cause great influence on the grade of the chromium ore powder;
(2) silane groups are modified on molecules of polyimide and epoxy resin, and the polyimide and the epoxy resin can be co-crosslinked through hydrolysis of the silane groups, so that the curing temperature is reduced, the curing time is shortened, and the strength of the pellet is improved;
(3) the silane modified polyimide is inserted into the layers of the bentonite, so that the high temperature resistance and the strength of the pellets are further improved.
Detailed Description
The invention is further described with reference to specific embodiments.
Example 1:
a chromium ore powder ball comprises the following raw materials in parts by weight: 90 parts of chromium ore powder with the granularity of 0-1 mm, 2.5 parts of a binder and 2.5 parts of water. The binder comprises the following components in parts by weight: 6.5 parts of silane modified polyimide/bentonite composite material, 3.5 parts of silane modified epoxy resin, 0.02 part of dibutyltin dilaurate and 40 parts of tetrahydrofuran.
The preparation method of the silane modified polyimide/bentonite composite material comprises the following steps:
A) adding bentonite into an octadecyl trimethyl ammonium bromide solution with the concentration of 0.8mol/L, wherein the mass-volume ratio of the bentonite to the octadecyl trimethyl ammonium bromide solution is 1g:80 mL; stirring uniformly, carrying out ultrasonic oscillation reaction for 3h, and separating and drying a product to obtain primarily intercalated bentonite;
B) adding the bentonite of the primary intercalation into DMF, stirring for 4h at 95 ℃ to obtain a DMF solution of the bentonite with the mass concentration of 2%;
C) dissolving 4,4 '-diaminodiphenyl ether in DMF, stirring uniformly, and adding hexafluorodianhydride into the solution, wherein the molar ratio of 4,4' -diaminodiphenyl ether to hexafluorodianhydride is 1.2: 1; stirring for reaction for 3.5h, and then adding a DMF (dimethyl formamide) solution of bentonite and isoquinoline to ensure that the mass ratio of the 4,4' -diaminodiphenyl ether to the bentonite is 3.5:1, the solid content of the reaction system is 12 wt%, and the addition amount of the isoquinoline is 4% of the total mass of the reaction system; heating to 190 ℃, and continuously stirring for reaction for 9 hours; transferring the product to ethanol for precipitation, separating and cleaning the precipitate, and drying to obtain the polyimide/bentonite composite material;
D) dissolving a polyimide/bentonite composite material in DMF (dimethyl formamide), adding gamma-aminopropyltriethoxysilane into the solution at 0 ℃ under the protection of nitrogen, wherein the mass ratio of the polyimide/bentonite composite material to the gamma-aminopropyltriethoxysilane is 13:1, the solid content of a reaction system is 12 wt%, stirring for reaction for 3 hours, heating to 50 ℃, adding isoquinoline and pyridine acetic anhydride, the addition of isoquinoline is 4% of the total mass of the reaction system, the addition of pyridine acetic anhydride is 0.4% of the total mass of a reactant, stirring for reaction for 9 hours, transferring a product to petroleum ether for precipitation, separating, cleaning and drying the precipitate to obtain the silane modified polyimide/bentonite composite material.
The preparation method of the silane modified epoxy resin comprises the following steps: heating epoxy resin E51 to 101 ℃, vacuumizing under a stirring state to remove water vapor, adding toluene to dissolve, uniformly stirring, and then adding methyltrimethoxysilane and dibutyltin dilaurate, wherein the mass ratio of the epoxy resin to the methyltrimethoxysilane is 19:1, and the adding amount of the dibutyltin dilaurate is 0.4% of the total mass of reactants; stirring and reacting for 4h at 90 ℃, and vacuumizing to remove the solvent to obtain the silane modified epoxy resin.
The preparation method of the chromium ore powder ball comprises the following steps: uniformly mixing all components in the binder in proportion; mixing chromium ore powder with a binder, adding atomized water, uniformly stirring, pressing into pellets with the particle size of 50mm by a ball press machine under the pressure of 300 tons, and naturally airing the pellets to obtain the chromium ore powder balls.
Example 2:
a chromium ore powder ball comprises the following raw materials in parts by weight: 85 parts of chromium ore powder with the granularity of 0-1 mm, 2 parts of a binder and 2 parts of water. The binder comprises the following components in parts by weight: 6 parts of silane modified polyimide/bentonite composite material, 3 parts of silane modified epoxy resin, 0.03 part of dibutyltin dilaurate and 20 parts of tetrahydrofuran.
The preparation method of the silane modified polyimide/bentonite composite material comprises the following steps:
A) adding bentonite into an octadecyl trimethyl ammonium bromide solution with the concentration of 0.5mol/L, wherein the mass-volume ratio of the bentonite to the octadecyl trimethyl ammonium bromide solution is 1g:50 mL; stirring uniformly, carrying out ultrasonic oscillation reaction for 2h, and separating and drying a product to obtain primarily intercalated bentonite;
B) adding the bentonite of the primary intercalation into DMF, stirring for 5h at 90 ℃ to obtain a DMF solution of the bentonite with the mass concentration of 1%;
C) dissolving 4,4 '-diaminodiphenyl ether in DMF, stirring uniformly, and adding hexafluorodianhydride into the solution, wherein the molar ratio of 4,4' -diaminodiphenyl ether to hexafluorodianhydride is 1: 1; after stirring and reacting for 3 hours, adding a DMF (dimethyl formamide) solution of bentonite and isoquinoline to ensure that the mass ratio of the 4,4' -diaminodiphenyl ether to the bentonite is 3:1, the solid content of the reaction system is 10 wt%, and the addition amount of the isoquinoline is 3% of the total mass of the reaction system; heating to 185 ℃, and continuously stirring for reaction for 10 hours; transferring the product to ethanol for precipitation, separating and cleaning the precipitate, and drying to obtain the polyimide/bentonite composite material;
D) dissolving a polyimide/bentonite composite material in DMF (dimethyl formamide), adding gamma-aminopropyltriethoxysilane into the solution at 0 ℃ under the protection of nitrogen, wherein the mass ratio of the polyimide/bentonite composite material to the gamma-aminopropyltriethoxysilane is 12:1, the solid content of a reaction system is 10 wt%, stirring for reaction for 2 hours, heating to 45 ℃, adding isoquinoline and pyridine acetic anhydride, the addition of isoquinoline is 3% of the total mass of the reaction system, the addition of pyridine acetic anhydride is 0.3% of the total mass of a reactant, stirring for reaction for 10 hours, transferring a product to petroleum ether for precipitation, separating, cleaning and drying the precipitate to obtain the silane modified polyimide/bentonite composite material.
The preparation method of the silane modified epoxy resin comprises the following steps: heating epoxy resin E51 to 100 ℃, vacuumizing under a stirring state to remove water vapor, adding toluene to dissolve, uniformly stirring, and then adding methyltrimethoxysilane and dibutyltin dilaurate, wherein the mass ratio of the epoxy resin to the methyltrimethoxysilane is 15:1, and the adding amount of the dibutyltin dilaurate is 0.3% of the total mass of reactants; stirring and reacting for 5h at 85 ℃, and vacuumizing to remove the solvent to obtain the silane modified epoxy resin.
The preparation method of the chromium ore powder ball comprises the following steps: uniformly mixing all components in the binder in proportion; mixing chromium ore powder with a binder, adding atomized water, uniformly stirring, pressing into pellets with the particle size of 30mm by a ball press machine under the pressure of 100 tons, and naturally airing the pellets to obtain the chromium ore powder balls.
Example 3:
a chromium ore powder ball comprises the following raw materials in parts by weight: 95 parts of chromium ore powder with the granularity of 0-1 mm, 3 parts of a binder and 3 parts of water. The binder comprises the following components in parts by weight: 7 parts of silane modified polyimide/bentonite composite material, 4 parts of silane modified epoxy resin, 0.01 part of dibutyltin dilaurate and 30 parts of tetrahydrofuran.
The preparation method of the silane modified polyimide/bentonite composite material comprises the following steps:
A) adding bentonite into an octadecyl trimethyl ammonium bromide solution with the concentration of 1.0mol/L, wherein the mass-volume ratio of the bentonite to the octadecyl trimethyl ammonium bromide solution is 1g:100 mL; stirring uniformly, carrying out ultrasonic oscillation reaction for 4 hours, and separating and drying a product to obtain primarily intercalated bentonite;
B) adding the bentonite subjected to preliminary intercalation into DMF, and stirring for 4h at 100 ℃ to obtain a DMF solution of bentonite with the mass concentration of 3%;
C) dissolving 4,4 '-diaminodiphenyl ether in DMF, stirring uniformly, and adding hexafluorodianhydride into the solution, wherein the molar ratio of 4,4' -diaminodiphenyl ether to hexafluorodianhydride is 1.5: 1; stirring for reaction for 4h, and then adding a DMF (dimethyl formamide) solution of bentonite and isoquinoline to ensure that the mass ratio of the 4,4' -diaminodiphenyl ether to the bentonite is 4:1, the solid content of the reaction system is 15wt%, and the addition amount of the isoquinoline is 5% of the total mass of the reaction system; heating to 195 ℃, and continuously stirring for reaction for 8 hours; transferring the product to ethanol for precipitation, separating and cleaning the precipitate, and drying to obtain the polyimide/bentonite composite material;
D) dissolving a polyimide/bentonite composite material in DMF, adding gamma-aminopropyltriethoxysilane into the solution at 4 ℃ under the protection of nitrogen, wherein the mass ratio of the polyimide/bentonite composite material to the gamma-aminopropyltriethoxysilane is 15:1, the solid content of a reaction system is 15wt%, stirring for reaction for 4 hours, heating to 55 ℃, adding isoquinoline and pyridine acetic anhydride, the addition of isoquinoline is 5% of the total mass of the reaction system, the addition of the pyridine acetic anhydride is 0.5% of the total mass of a reactant, stirring for reaction for 8 hours, transferring a product to petroleum ether for precipitation, separating, cleaning and drying the precipitate to obtain the silane modified polyimide/bentonite composite material.
The preparation method of the silane modified epoxy resin comprises the following steps: heating epoxy resin E51 to 105 ℃, vacuumizing under a stirring state to remove water vapor, adding toluene to dissolve, uniformly stirring, and then adding methyltrimethoxysilane and dibutyltin dilaurate, wherein the mass ratio of the epoxy resin to the methyltrimethoxysilane is 20:1, and the adding amount of the dibutyltin dilaurate is 0.5% of the total mass of reactants; stirring and reacting for 3h at 95 ℃, and vacuumizing to remove the solvent to obtain the silane modified epoxy resin.
The preparation method of the chromium ore powder ball comprises the following steps: uniformly mixing all components in the binder in proportion; mixing chromium ore powder with a binder, adding atomized water, uniformly stirring, pressing into pellets with the particle size of 40mm by a ball press machine under the pressure of 500 tons, and naturally airing the pellets to obtain the chromium ore powder balls.
Comparative example 1 (no intercalation of bentonite):
the binder in comparative example 1 comprises the following components in parts by weight: 6 parts of silane modified polyimide, 0.5 part of bentonite, 3.5 parts of silane modified epoxy resin, 0.02 part of dibutyltin dilaurate and 40 parts of tetrahydrofuran.
The preparation method of the silane modified polyimide comprises the following steps:
A) dissolving 4,4 '-diaminodiphenyl ether in DMF, uniformly stirring, adding hexafluorodianhydride into the solution, wherein the molar ratio of the 4,4' -diaminodiphenyl ether to the hexafluorodianhydride is 1.2:1, stirring for reacting for 3.5h, and then adding isoquinoline, wherein the solid content of the reaction system is 12 wt%, and the addition amount of the isoquinoline is 4% of the total mass of the reaction system; heating to 190 ℃, and continuously stirring for reaction for 9 hours; transferring the product to ethanol for precipitation, separating and cleaning the precipitate, and drying to obtain polyimide;
B) dissolving polyimide in DMF, adding gamma-aminopropyltriethoxysilane into the solution at 0 ℃ under the protection of nitrogen, wherein the mass ratio of the polyimide to the gamma-aminopropyltriethoxysilane is 13:1, the solid content of a reaction system is 12 wt%, stirring for 3h, reacting, heating to 50 ℃, adding isoquinoline and pyridine acetic anhydride, the addition of isoquinoline is 4% of the total mass of the reaction system, the addition of the pyridine acetic anhydride is 0.4% of the total mass of a reactant, stirring for 9h, reacting, transferring the product to petroleum ether for precipitation, separating, cleaning and drying the precipitate to obtain the silane modified polyimide.
The rest is the same as in example 1.
Comparative example 2 (without silane modification of polyimide/bentonite composite):
the binder in comparative example 2 comprises the following components in parts by weight: 6.5 parts of polyimide/bentonite composite material, 3.5 parts of silane modified epoxy resin, 0.02 part of dibutyltin dilaurate and 40 parts of tetrahydrofuran.
The preparation method of the polyimide/bentonite composite material comprises the following steps:
A) adding bentonite into an octadecyl trimethyl ammonium bromide solution with the concentration of 0.8mol/L, wherein the mass-volume ratio of the bentonite to the octadecyl trimethyl ammonium bromide solution is 1g:80 mL; stirring uniformly, carrying out ultrasonic oscillation reaction for 3h, and separating and drying a product to obtain primarily intercalated bentonite;
B) adding the primarily intercalated bentonite into DMF, and stirring at 95 ℃ for 4 hours to obtain a DMF solution of bentonite with the mass concentration of 2%;
C) dissolving 4,4 '-diaminodiphenyl ether in DMF, stirring uniformly, and adding hexafluorodianhydride into the solution, wherein the molar ratio of 4,4' -diaminodiphenyl ether to hexafluorodianhydride is 1.2: 1; stirring for reaction for 3.5h, and then adding a DMF (dimethyl formamide) solution of bentonite and isoquinoline to ensure that the mass ratio of the 4,4' -diaminodiphenyl ether to the bentonite is 3.5:1, the solid content of the reaction system is 12 wt%, and the addition amount of the isoquinoline is 4% of the total mass of the reaction system; heating to 190 ℃, and continuously stirring for reaction for 9 hours; and transferring the product to ethanol for precipitation, separating and cleaning the precipitate, and drying to obtain the polyimide/bentonite composite material.
The rest is the same as in example 1.
Comparative example 3 (no silane modification of epoxy resin):
the binder in comparative example 3 comprises the following components in parts by weight: 6.5 parts of silane modified polyimide/bentonite composite material, 3.5 parts of epoxy resin E51, 0.02 part of dibutyltin dilaurate and 40 parts of tetrahydrofuran. The rest is the same as in example 1.
The properties of the chromium ore pellets obtained in the above examples and comparative examples were measured, and the results are shown in table 1. Wherein the falling strength refers to the times that the chromium ore powder balls are freely dropped onto the cement ground from a height of 1.5m without being broken, 10 chromium ore powder balls are tested in each group, and the falling strength is averaged.
Table 1: and (5) testing the performance of the chromium ore powder balls.
| Compressive strength (MPa) | Drop strength (times) | Bursting temperature (. degree.C.) | |
| Example 1 | 20.6 | 26.7 | 793 |
| Example 2 | 21.1 | 28.2 | 775 |
| Example 3 | 20.0 | 26.1 | 784 |
| Comparative example 1 | 16.2 | 17.8 | 673 |
| Comparative example 2 | 10.8 | 12.5 | 568 |
| Comparative example 3 | 12.4 | 13.9 | 581 |
As can be seen from Table 1, the chromium ore powder pellets prepared by the method of the present invention in examples 1 to 3 had high compressive strength and drop strength, and were convenient for transportation; meanwhile, the cracking furnace has higher cracking temperature, and is not easy to crack and pulverize after entering the furnace. In the comparative example 1, the silane modified polyimide is not inserted between the bentonite layers, but the bentonite, the silane modified polyimide and the silane modified epoxy resin are directly blended, so that the strength and the high temperature resistance of the pellet are reduced compared with those in the example 1; in comparative examples 2 and 3, the polyimide or the epoxy resin is not modified by silane, and the polyimide and the epoxy resin can not be co-crosslinked, so that the strength and the high-temperature resistance of the pellet are also obviously reduced.
Claims (10)
1. A chromium ore powder ball is characterized by comprising the following raw materials in parts by weight: 85-95 parts of chromium ore powder, 2-3 parts of binder and 2-3 parts of water; the adhesive comprises the following components in parts by weight: 6-7 parts of silane modified polyimide/bentonite composite material, 3-4 parts of silane modified epoxy resin, 0.01-0.03 part of dibutyltin dilaurate and 20-30 parts of tetrahydrofuran.
2. The chromium ore powder pellet as claimed in claim 1, wherein the particle size of said chromium ore powder is 0 to 1 mm.
3. The chromium ore pellet as claimed in claim 1, wherein the silane-modified polyimide/bentonite composite material is prepared by the following steps:
A) adding bentonite into an octadecyl trimethyl ammonium bromide solution, stirring uniformly, carrying out ultrasonic oscillation reaction for 2-4 h, and separating and drying a product to obtain primarily intercalated bentonite;
B) dissolving the bentonite subjected to preliminary intercalation in DMF to obtain a DMF solution of the bentonite;
C) dissolving 4,4' -diaminodiphenyl ether in DMF, uniformly stirring, adding hexafluoro dianhydride into the solution, stirring for reacting for 3-4 h, then adding the DMF solution of bentonite and isoquinoline, heating to 185-195 ℃, and continuing to stir for reacting for 8-10 h; transferring the product to ethanol for precipitation, separating and cleaning the precipitate, and drying to obtain the polyimide/bentonite composite material;
D) dissolving a polyimide/bentonite composite material in DMF, adding gamma-aminopropyltriethoxysilane into the solution at 0-4 ℃ under the protection of nitrogen, stirring and reacting for 2-4 h, heating to 45-55 ℃, adding isoquinoline and pyridine acetic anhydride, stirring and reacting for 8-10 h, transferring the product to petroleum ether for precipitation, separating and cleaning the precipitate, and drying to obtain the silane modified polyimide/bentonite composite material.
4. The chromium ore powder pellet as claimed in claim 3, wherein the concentration of the octadecyl trimethyl ammonium bromide solution in step A) is 0.5 to 1.0mol/L, and the mass-to-volume ratio of bentonite to the octadecyl trimethyl ammonium bromide solution is 1g:50 to 100 mL; the mass concentration of the DMF solution of the bentonite obtained in the step B) is 1-3%.
5. The chromium ore powder pellet as claimed in claim 3, wherein the molar ratio of 4,4' -diaminodiphenyl ether to hexafluorodianhydride added in step C) is 1 to 1.5: 1; the mass ratio of the 4,4' -diaminodiphenyl ether to the bentonite is 3-4: 1; the solid content of the reaction system is 10-15 wt%, and the addition amount of isoquinoline is 3-5% of the total mass of the reaction system.
6. The chromium ore fines pellet as claimed in claim 3, wherein the mass ratio of the polyimide/bentonite composite material to the gamma-aminopropyltriethoxysilane added in step D) is 12-15: 1, the solid content of the reaction system is 10-15 wt%, the addition amount of isoquinoline is 3-5% of the total mass of the reaction system, and the addition amount of acetic anhydride pyridine is 0.3-0.5% of the total mass of the reactants.
7. The chromium ore powder pellet as claimed in claim 3, wherein said silane-modified epoxy resin is prepared by the method comprising: heating epoxy resin to 100-105 ℃, vacuumizing under a stirring state to remove water vapor, adding a solvent for dissolving, uniformly stirring, and then adding methyl trimethoxy silane and dibutyltin dilaurate, wherein the mass ratio of the epoxy resin to the methyl trimethoxy silane is 15-20: 1, and the adding amount of the dibutyltin dilaurate is 0.3-0.5% of the total mass of reactants; stirring and reacting for 3-5 h at 85-95 ℃, and vacuumizing to remove the solvent to obtain the silane modified epoxy resin.
8. The method for preparing chromium ore powder pellets as claimed in claim 1, comprising the steps of: mixing chromium ore powder and each component in the binder in proportion, adding atomized water, uniformly stirring, performing cold press molding to prepare pellets, and drying the pellets to obtain the chromium ore powder pellets.
9. The method according to claim 8, wherein the pressure in the cold press molding is 100 to 500 tons.
10. The preparation method of claim 8, wherein the pellet size after cold press molding is 30-50 mm.
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