CN114592123B - Chromium ore powder ball and preparation method thereof - Google Patents
Chromium ore powder ball and preparation method thereof Download PDFInfo
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- CN114592123B CN114592123B CN202111616607.9A CN202111616607A CN114592123B CN 114592123 B CN114592123 B CN 114592123B CN 202111616607 A CN202111616607 A CN 202111616607A CN 114592123 B CN114592123 B CN 114592123B
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- bentonite
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- polyimide
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 75
- 239000011651 chromium Substances 0.000 title claims abstract description 75
- 239000000843 powder Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims description 22
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 106
- 239000000440 bentonite Substances 0.000 claims abstract description 106
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 106
- 229920001721 polyimide Polymers 0.000 claims abstract description 69
- 239000004642 Polyimide Substances 0.000 claims abstract description 63
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910000077 silane Inorganic materials 0.000 claims abstract description 53
- 239000008188 pellet Substances 0.000 claims abstract description 48
- 239000002131 composite material Substances 0.000 claims abstract description 44
- 239000003822 epoxy resin Substances 0.000 claims abstract description 43
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 43
- 239000011230 binding agent Substances 0.000 claims abstract description 29
- 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 19
- 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
- 239000000853 adhesive Substances 0.000 claims abstract description 8
- 230000001070 adhesive effect Effects 0.000 claims abstract description 8
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 7
- 239000011707 mineral Substances 0.000 claims abstract description 7
- 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 32
- 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 22
- 238000001035 drying Methods 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 20
- 238000001556 precipitation Methods 0.000 claims description 19
- 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 16
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000004140 cleaning Methods 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
- 238000000034 method Methods 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 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
- 238000002156 mixing Methods 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 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
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000009830 intercalation Methods 0.000 claims description 5
- 239000010410 layer Substances 0.000 claims description 5
- BLAKAEFIFWAFGH-UHFFFAOYSA-N acetyl acetate;pyridine Chemical compound C1=CC=NC=C1.CC(=O)OC(C)=O BLAKAEFIFWAFGH-UHFFFAOYSA-N 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 230000002687 intercalation Effects 0.000 claims description 3
- 238000010528 free radical solution polymerization reaction Methods 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 claims description 2
- 239000011229 interlayer Substances 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- -1 pyridine acetate anhydride Chemical class 0.000 claims description 2
- 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
- 239000009719 polyimide resin Substances 0.000 description 6
- GAPYKZAARZMMGP-UHFFFAOYSA-N pyridin-1-ium;acetate Chemical compound CC(O)=O.C1=CC=NC=C1 GAPYKZAARZMMGP-UHFFFAOYSA-N 0.000 description 6
- 230000009172 bursting Effects 0.000 description 5
- 229910000599 Cr alloy Inorganic materials 0.000 description 4
- 239000000788 chromium alloy Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 239000000203 mixture 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
- 238000010298 pulverizing process Methods 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
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation 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
- 229910003471 inorganic composite material Inorganic materials 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000005453 pelletization 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Compositions Of Macromolecular Compounds (AREA)
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 mineral 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 dosage of the inorganic binder, avoid the influence on the grade of the chromium ore powder, and 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 in chromium ore required by chromium alloy production, blocky chromium ore is used as the optimal raw material, and in the production process of chromium alloy, the blocky chromium ore and other raw materials enter the furnace, so that the air permeability in the furnace can be improved, the ignition is not easy, the dust is less, the furnace condition can be better controlled, and better economic and technical indexes are obtained. But with the shortage of chromium ore resources, the yield of lump ore is reduced, the grade is reduced, and the price is increased. Correspondingly, the chromium ore powder (particle size is less than 10 mm) obtained by adopting the ore dressing method is more and more, chromium alloy production enterprises gradually start to use the powder ore to produce products such as ferrochrome and the like, and the powder ore use proportion of many enterprises is almost half. However, the direct feeding of the powder ore into the furnace can cause a series of technical problems of poor air permeability, easy ignition, large dust, unstable furnace conditions and the like of the submerged arc furnace. Therefore, the fine ore must be agglomerated or formed into pellets for a large amount of use in electric furnaces for smelting chromium-based alloys.
At present, the method for preparing the chromium ore powder into pellets mainly comprises the cold-pressing pellet process: mixing the chromium mineral powder and the binder, feeding the mixture into a stirrer, conveying the mixture to a ball pressing machine for ball pressing, and airing to obtain the chromium mineral powder balls. For example, the publication No. CN103436694A discloses a method for preparing pellets of powder chrome ore in Chinese patent literature, wherein the preparation process comprises the steps of adding an adhesive, a slag former, a reducing agent and a regulator into the powder chrome ore, uniformly mixing, adding water for humidity adjustment, cold pressing into pellets, natural curing and airing to obtain finished pellets.
However, the chromium ore powder pellets prepared in the prior art have the following disadvantages: 1. the specific gravity of the binder is high, the taste is seriously reduced after balling, and the comprehensive grade of chromium ore entering the furnace is influenced; 2. the pellet has low strength, is easy to damage during transportation and generates secondary pollution; 3. the explosion temperature of the pellets 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, and the organic-inorganic composite binder is adopted to prepare the chromium ore powder into pellets, so that the use amount of the inorganic binder can be reduced, the influence on the grade of the chromium ore powder is avoided, and meanwhile, the strength and the thermal stability of the chromium ore powder pellets can be improved.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
The 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 to 7 parts of silane modified polyimide/bentonite composite material, 3 to 4 parts of silane modified epoxy resin, 0.01 to 0.03 part of dibutyl tin dilaurate and 20 to 30 parts of tetrahydrofuran.
In the chromium ore powder ball, the silane modified polyimide/bentonite composite material and the silane modified epoxy resin are adopted as main raw materials of the binder, and the water absorption performance of bentonite is utilized to reduce the evaporation rate of water in the chromium ore powder ball, so that the vapor pressure in the pellet is reduced, the bursting temperature of the pellet is improved, the bursting pulverization rate of the chromium ore powder ball after being fed into a furnace is reduced, and the furnace condition is stabilized. However, too much bentonite is added as an inorganic substance to influence the grade of pellets, so that the bentonite and the silane modified polyimide are compounded to prepare the organic-inorganic composite material, the consumption of inorganic bentonite is reduced, the organic components in the binder can be burnt and removed in the smelting process, and the slag amount in the smelting process is reduced. Polyimide in the silane modified polyimide/bentonite composite material has good high temperature resistance, is also beneficial to improving the thermal stability of pellets, reduces the bursting rate of chromium ore powder pellets after being fed into a furnace, but has insufficient bonding performance, so the invention adds silane modified epoxy resin into the adhesive, and improves the bonding performance 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, and after the adhesive is mixed with water, the silane groups in the silane modified polyimide and the silane modified epoxy resin are hydrolyzed under the catalysis 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 polyimide and epoxy resin, so that 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 to 1mm. Although the smaller the granularity of the chromium mineral powder is, the easier the pelletization is, but the smaller the granularity is, the denser the prepared pellet is, the water in the pellet is not easy to evaporate, and the vapor pressure in the pellet is larger, so the pellet prepared from the chromium mineral powder with smaller granularity is usually easy to burst and pulverize, and is unfavorable for the stability of furnace conditions. According to the invention, through optimizing the binder component, the chromium ore powder balls with higher bursting temperature can be prepared by using the chromium ore powder with smaller granularity, so that the application of the chromium ore powder balls is facilitated.
Preferably, the preparation method of the silane modified polyimide/bentonite composite material comprises the following steps:
a) Adding bentonite into octadecyl trimethyl ammonium bromide solution, stirring uniformly, performing ultrasonic oscillation reaction for 2-4 hours, separating and drying the product to obtain primarily intercalated bentonite;
b) Dissolving the primarily intercalated bentonite in DMF to obtain DMF solution of bentonite;
c) Dissolving 4,4' -diaminodiphenyl ether in DMF, stirring uniformly, adding hexafluorodianhydride into the solution, stirring to react for 3-4 hours, adding DMF solution of bentonite and isoquinoline, heating to 185-195 ℃ and continuing stirring to react for 8-10 hours; transferring the product to ethanol for precipitation, separating and cleaning the precipitation, and drying to obtain a polyimide/bentonite composite material;
D) Dissolving the polyimide/bentonite composite material in DMF, adding gamma-aminopropyl triethoxysilane into the solution under the protection of nitrogen at 0-4 ℃, stirring and reacting for 2-4 hours, heating to 45-55 ℃, adding isoquinoline and pyridine acetic anhydride, stirring and reacting for 8-10 hours, transferring the product into petroleum ether for precipitation, separating the precipitate, cleaning and drying to obtain the silane modified polyimide/bentonite composite material.
Firstly, intercalating bentonite through octadecyl trimethyl ammonium bromide, primarily expanding the interlayer spacing of the bentonite, and then intercalating polyimide between bentonite layers by using 4,4' -diaminodiphenyl ether and hexafluorodianhydride as monomers through a solution polymerization in-situ intercalation method to obtain a polyimide/bentonite composite material; and finally, capping the polyimide with gamma-aminopropyl triethoxy silane to obtain the silane modified polyimide/bentonite composite material.
According to the invention, the silane modified polyimide is inserted between layers of the bentonite, and then the silane modified polyimide is co-crosslinked with the silane modified epoxy resin, so that the limiting effect of the lamellar structure of the bentonite on polyimide molecules can be further improved, and the high temperature resistance of the pellets can be further improved; meanwhile, bentonite dissociated into nano-structures can be used as a crosslinking point, so that the strength of the pellets 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 bentonite to the octadecyl trimethyl ammonium bromide solution is 1 g: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 4,4' -diaminodiphenyl ether to hexafluorodianhydride added in 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-aminopropyl triethoxysilane is 12-15:1, the solid content of the reaction system is 10-15 wt%, the addition of isoquinoline is 3-5% of the total mass of the reaction system, and the addition of pyridine acetate anhydride is 0.3-0.5% of the total mass of reactants.
Preferably, the preparation method of the silane modified epoxy resin comprises the following steps: heating epoxy resin to 100-105 ℃, vacuumizing to remove water vapor under a stirring state, adding a solvent for dissolution, 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 addition 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, cold-pressing to form pellets, and drying the pellets to obtain the chromium ore powder pellets.
Preferably, the pressure during cold press molding is 100 to 500 tons.
Preferably, the pellet particle size after cold press molding is 30-50 mm.
Therefore, the invention has the following beneficial effects:
(1) The bentonite, polyimide and epoxy resin are matched, so that the adhesive does not greatly influence the grade of the chromium ore powder, and meanwhile, the prepared chromium ore powder ball has good strength and thermal stability;
(2) The silane groups are modified on the polyimide and epoxy resin molecules, and the polyimide and the epoxy resin can be crosslinked together through the hydrolysis of the silane groups, so that the curing temperature is reduced, the curing time is shortened, and the strength of the pellets is improved;
(3) The silane modified polyimide is inserted between the layers of the bentonite, so that the high temperature resistance of the pellets and the strength of the pellets are further improved.
Detailed Description
The invention is further described below in connection with the following detailed description.
Example 1:
The 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 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 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 to 80mL; stirring uniformly, performing ultrasonic oscillation reaction for 3 hours, separating and drying the product to obtain the preliminary intercalated bentonite;
B) Adding the primarily intercalated bentonite into DMF, and stirring for 4 hours at 95 ℃ to obtain DMF solution of bentonite with 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 the 4,4' -diaminodiphenyl ether to the hexafluorodianhydride is 1.2:1; stirring and reacting for 3.5h, then adding DMF solution of bentonite and isoquinoline, wherein the mass ratio of 4,4' -diaminodiphenyl ether to bentonite is 3.5:1, the solid content of the reaction system is 12wt%, and the addition amount of isoquinoline is 4% of the total mass of the reaction system; heating to 190 ℃ and continuing stirring to react for 9 hours; transferring the product to ethanol for precipitation, separating and cleaning the precipitation, and drying to obtain a polyimide/bentonite composite material;
D) Dissolving polyimide/bentonite composite material in DMF, adding gamma-aminopropyl triethoxysilane into the solution under the protection of nitrogen at 0 ℃, wherein the mass ratio of the polyimide/bentonite composite material to the gamma-aminopropyl triethoxysilane is 13:1, the solid content of the reaction system is 12wt%, stirring and reacting for 3 hours, heating to 50 ℃, adding isoquinoline and pyridine acetate, wherein the addition amount of isoquinoline is 4% of the total mass of the reaction system, the addition amount of pyridine acetate is 0.4% of the total mass of the reactants, stirring and reacting for 9 hours, transferring the product into petroleum ether for precipitation, separating the precipitate, cleaning and drying to obtain the silane modified polyimide/bentonite composite material.
The preparation method of the silane modified epoxy resin comprises the following steps: heating the epoxy resin E51 to 101 ℃, vacuumizing in a stirring state, adding toluene for dissolution, 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 4 hours 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 the components in the binder according to a proportion; mixing chromium ore powder with a binder, adding atomized water, uniformly stirring, pressing into pellets with the particle size of 50mm by using 300 tons of pressure of a ball press, and naturally airing the pellets to obtain the chromium ore powder pellets.
Example 2:
The 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 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 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:50mL; stirring uniformly, performing ultrasonic oscillation reaction for 2 hours, separating and drying the product to obtain the preliminary intercalated bentonite;
B) Adding the primarily intercalated bentonite into DMF, and stirring for 5 hours at 90 ℃ to obtain DMF solution of 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 the 4,4' -diaminodiphenyl ether to the hexafluorodianhydride is 1:1; stirring and reacting for 3 hours, and then adding DMF solution of bentonite and isoquinoline, wherein the mass ratio of 4,4' -diaminodiphenyl ether to bentonite is 3:1, the solid content of the reaction system is 10wt%, and the addition amount of isoquinoline is 3% of the total mass of the reaction system; heating to 185 ℃ and continuing stirring to react for 10 hours; transferring the product to ethanol for precipitation, separating and cleaning the precipitation, and drying to obtain a polyimide/bentonite composite material;
D) Dissolving polyimide/bentonite composite material in DMF, adding gamma-aminopropyl triethoxysilane into the solution under the protection of nitrogen at 0 ℃, wherein the mass ratio of the polyimide/bentonite composite material to the gamma-aminopropyl triethoxysilane is 12:1, the solid content of the reaction system is 10wt%, stirring and reacting for 2 hours, heating to 45 ℃, adding isoquinoline and pyridine acetate, wherein the addition amount of isoquinoline is 3% of the total mass of the reaction system, the addition amount of pyridine acetate is 0.3% of the total mass of the reactants, stirring and reacting for 10 hours, transferring the product into petroleum ether for precipitation, separating the precipitation, cleaning and drying 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 to remove water vapor under a stirring state, adding toluene for dissolution, 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 5 hours 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 the components in the binder according to a proportion; mixing chromium ore powder with a binder, adding atomized water, uniformly stirring, pressing into pellets with the particle size of 30mm by 100 ton pressure of a ball press, and naturally airing the pellets to obtain the chromium ore powder pellets.
Example 3:
The chromium ore powder ball comprises the following raw materials in parts by weight: 95 parts of chromium mineral powder with the granularity of 0-1 mm, 3 parts of 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 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:100mL; stirring uniformly, performing ultrasonic oscillation reaction for 4 hours, separating and drying the product to obtain the preliminary intercalated bentonite;
b) Adding the primarily intercalated bentonite into DMF, and stirring for 4 hours at 100 ℃ to obtain DMF solution of bentonite with 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 the 4,4' -diaminodiphenyl ether to the hexafluorodianhydride is 1.5:1; stirring and reacting for 4 hours, and then adding DMF solution of bentonite and isoquinoline, wherein the mass ratio of 4,4' -diaminodiphenyl ether to bentonite is 4:1, the solid content of the reaction system is 15wt%, and the addition amount of isoquinoline is 5% of the total mass of the reaction system; heating to 195 ℃ and continuing stirring for reaction for 8 hours; transferring the product to ethanol for precipitation, separating and cleaning the precipitation, and drying to obtain a polyimide/bentonite composite material;
D) Dissolving polyimide/bentonite composite material in DMF, adding gamma-aminopropyl triethoxysilane into the solution under the protection of nitrogen at 4 ℃, wherein the mass ratio of the polyimide/bentonite composite material to the gamma-aminopropyl triethoxysilane is 15:1, the solid content of the reaction system is 15wt%, stirring and reacting for 4 hours, heating to 55 ℃, adding isoquinoline and pyridine acetate, wherein the addition of isoquinoline is 5% of the total mass of the reaction system, the addition of pyridine acetate is 0.5% of the total mass of the reactants, stirring and reacting for 8 hours, transferring the product into petroleum ether for precipitation, separating the precipitate, cleaning and drying to obtain the silane modified polyimide/bentonite composite material.
The preparation method of the silane modified epoxy resin comprises the following steps: heating the epoxy resin E51 to 105 ℃, vacuumizing in a stirring state, adding toluene for dissolution, 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 3 hours 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 the components in the binder according to a proportion; mixing chromium ore powder with a binder, adding atomized water, uniformly stirring, pressing into pellets with the particle size of 40mm by using 500 tons of pressure of a ball press, and naturally airing the pellets to obtain the chromium ore powder pellets.
Comparative example 1 (bentonite was not intercalated):
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, stirring uniformly, adding hexafluorodianhydride into the solution, wherein the molar ratio of the 4,4' -diaminodiphenyl ether to the hexafluorodianhydride is 1.2:1, stirring and reacting for 3.5 hours, then adding isoquinoline, wherein the solid content of the reaction system is 12wt%, and the adding amount of the isoquinoline is 4% of the total mass of the reaction system; heating to 190 ℃ and continuing stirring to react 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-aminopropyl triethoxysilane into the solution under the protection of nitrogen at 0 ℃, wherein the mass ratio of the polyimide to the gamma-aminopropyl triethoxysilane is 13:1, stirring and reacting for 3 hours, heating to 50 ℃, adding isoquinoline and pyridine acetic anhydride, wherein the addition amount of isoquinoline is 4% of the total mass of the reaction system, the addition amount of pyridine acetic anhydride is 0.4% of the total mass of reactants, stirring and reacting for 9 hours, transferring the product into petroleum ether for precipitation, separating the precipitate, cleaning and drying to obtain the silane modified polyimide.
The remainder was the same as in example 1.
Comparative example 2 (no 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 dibutyl tin dilaurate and 40 parts of tetrahydrofuran.
The preparation method of the polyimide/bentonite composite material comprises the following steps:
a) Adding bentonite into 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 to 80mL; stirring uniformly, performing ultrasonic oscillation reaction for 3 hours, separating and drying the product to obtain the preliminary intercalated bentonite;
B) Adding the primarily intercalated bentonite into DMF, and stirring for 4 hours at 95 ℃ to obtain DMF solution of bentonite with 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 the 4,4' -diaminodiphenyl ether to the hexafluorodianhydride is 1.2:1; stirring and reacting for 3.5h, then adding DMF solution of bentonite and isoquinoline, wherein the mass ratio of 4,4' -diaminodiphenyl ether to bentonite is 3.5:1, the solid content of the reaction system is 12wt%, and the addition amount of isoquinoline is 4% of the total mass of the reaction system; heating to 190 ℃ and continuing stirring to react for 9 hours; transferring the product into ethanol for precipitation, separating and cleaning the precipitate, and drying to obtain the polyimide/bentonite composite material.
The remainder was 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 remainder was the same as in example 1.
The properties of the chromium ore powder balls prepared in the above examples and comparative examples were tested and the results are shown in table 1. Wherein, the dropping strength refers to the number of times that the chromium ore powder balls are freely dropped from a height of 1.5m to the cement floor without fragmentation, and 10 chromium ore powder balls are tested in each group, and the dropping strength is averaged.
Table 1: and (5) testing the performance of the chromium ore powder ball.
| Compressive strength (MPa) | Drop strength (times) | Burst 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 balls prepared by the method of the invention in examples 1 to 3 have high compressive strength and dropping strength, and are convenient for transportation; meanwhile, the furnace has higher bursting temperature, and burst and pulverization phenomena are not easy to occur after the furnace is charged. In comparative example 1, the silane-modified polyimide was not inserted between bentonite layers, but bentonite was directly blended with the silane-modified polyimide and the silane-modified epoxy resin, and the pellet strength and high temperature resistance were reduced as compared with those in example 1; the polyimide or epoxy resin in comparative examples 2 and 3 was not modified with silane, and the polyimide and epoxy resin could not be co-crosslinked, resulting in a significant decrease in pellet strength and high temperature resistance.
Claims (10)
1. The chromium ore powder ball is characterized by comprising the following raw materials in parts by weight: 85-95 parts of chromium mineral 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;
Firstly, intercalation is carried out on bentonite through octadecyl trimethyl ammonium bromide, the interlayer spacing of the bentonite is enlarged preliminarily, then 4,4' -diaminodiphenyl ether and hexafluorodianhydride are taken as monomers, polyimide is intercalated between bentonite layers through a solution polymerization in-situ intercalation method, and a polyimide/bentonite composite material is obtained; and finally, capping the polyimide with gamma-aminopropyl triethoxy silane to obtain the silane modified polyimide/bentonite composite material.
2. The chromium ore powder ball according to claim 1, wherein the particle size of the chromium ore powder is 0 to 1mm.
3. The chrome ore powder ball according to claim 1, wherein the preparation method of the silane modified polyimide/bentonite composite material comprises the following steps:
a) Adding bentonite into octadecyl trimethyl ammonium bromide solution, uniformly stirring, performing ultrasonic oscillation reaction for 2-4 hours, separating and drying a product to obtain primarily intercalated bentonite;
b) Dissolving the primarily intercalated bentonite in DMF to obtain DMF solution of bentonite;
C) Dissolving 4,4' -diaminodiphenyl ether in DMF, stirring uniformly, adding hexafluorodianhydride into the solution, stirring to react for 3-4 hours, adding DMF solution of bentonite and isoquinoline, heating to 185-195 ℃ and continuing stirring to react for 8-10 hours; transferring the product to ethanol for precipitation, separating and cleaning the precipitation, and drying to obtain a polyimide/bentonite composite material;
d) And dissolving the polyimide/bentonite composite material in DMF, adding gamma-aminopropyl triethoxysilane into the solution under the protection of nitrogen at 0-4 ℃, stirring and reacting for 2-4 hours, heating to 45-55 ℃, adding isoquinoline and pyridine acetic anhydride, stirring and reacting for 8-10 hours, transferring the product into petroleum ether for precipitation, separating the precipitate, cleaning and drying to obtain the silane modified polyimide/bentonite composite material.
4. The chromium ore powder ball according to claim 3, wherein 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 bentonite to the octadecyl trimethyl ammonium bromide solution is 1 g:50-100 mL; the mass concentration of the DMF solution of the bentonite obtained in the step B) is 1-3%.
5. The chromium ore powder ball according to claim 3, wherein the molar ratio of the 4,4' -diaminodiphenyl ether to the hexafluorodianhydride added in the 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 powder ball according to claim 3, wherein the mass ratio of the polyimide/bentonite composite material added in the step D) to the gamma-aminopropyl triethoxysilane 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 acetate anhydride is 0.3-0.5% of the total mass of reactants.
7. The chrome ore powder ball according to claim 3, wherein the preparation method of the silane-modified epoxy resin comprises the following steps: heating epoxy resin to 100-105 ℃, vacuumizing to remove water vapor under a stirring state, adding a solvent for dissolution, 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 addition amount of the dibutyltin dilaurate is 0.3-0.5% of the total mass of reactants; stirring and reacting for 3-5 hours at the temperature of 85-95 ℃, and vacuumizing to remove the solvent to obtain the silane modified epoxy resin.
8. A method for preparing the chromium ore powder ball according to claim 1, comprising the steps of: mixing the chromium ore powder and each component in the binder in proportion, adding atomized water, uniformly stirring, cold-pressing to form pellets, and drying the pellets to obtain the chromium ore powder pellets.
9. The method according to claim 8, wherein the pressure during cold press molding is 100 to 500 tons.
10. The preparation method of claim 8, wherein the particle size of the pellets after cold press molding is 30-50 mm.
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