CN113803988A - Device and method for producing antimony white from antimony oxide powder - Google Patents
Device and method for producing antimony white from antimony oxide powder Download PDFInfo
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- CN113803988A CN113803988A CN202110963731.6A CN202110963731A CN113803988A CN 113803988 A CN113803988 A CN 113803988A CN 202110963731 A CN202110963731 A CN 202110963731A CN 113803988 A CN113803988 A CN 113803988A
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- oxide powder
- antimony oxide
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- 229910000410 antimony oxide Inorganic materials 0.000 title claims abstract description 104
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000000843 powder Substances 0.000 title claims abstract description 89
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 43
- 230000008569 process Effects 0.000 claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 24
- 229910052787 antimony Inorganic materials 0.000 claims description 20
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 19
- 229910052681 coesite Inorganic materials 0.000 claims description 18
- 229910052906 cristobalite Inorganic materials 0.000 claims description 18
- 239000000377 silicon dioxide Substances 0.000 claims description 18
- 229910052682 stishovite Inorganic materials 0.000 claims description 18
- 229910052905 tridymite Inorganic materials 0.000 claims description 18
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000428 dust Substances 0.000 claims description 16
- 239000000779 smoke Substances 0.000 claims description 16
- 238000003723 Smelting Methods 0.000 claims description 13
- 230000009467 reduction Effects 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000003638 chemical reducing agent Substances 0.000 claims description 7
- 230000005674 electromagnetic induction Effects 0.000 claims description 7
- 239000000446 fuel Substances 0.000 claims description 7
- 239000003245 coal Substances 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000000571 coke Substances 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 239000003345 natural gas Substances 0.000 claims description 3
- 238000005453 pelletization Methods 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 33
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 description 14
- 239000002994 raw material Substances 0.000 description 14
- 238000006722 reduction reaction Methods 0.000 description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- YEAUATLBSVJFOY-UHFFFAOYSA-N tetraantimony hexaoxide Chemical compound O1[Sb](O2)O[Sb]3O[Sb]1O[Sb]2O3 YEAUATLBSVJFOY-UHFFFAOYSA-N 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- 238000007664 blowing Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 description 2
- 239000003830 anthracite Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910052950 sphalerite Inorganic materials 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
- F27B5/04—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated adapted for treating the charge in vacuum or special atmosphere
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
- C01G30/004—Oxides; Hydroxides; Oxyacids
- C01G30/005—Oxides
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
- F27B5/06—Details, accessories, or equipment peculiar to furnaces of these types
- F27B5/14—Arrangements of heating devices
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a device and a method for producing antimony white from antimony oxide powder. The device comprises a vacuum furnace, a condensing device and a vacuumizing unit which are horizontally communicated in sequence; wherein, the vacuum furnace comprises a furnace body; the furnace body is internally provided with a heater and is provided with an antimony oxide powder inlet. The device can directly heat and volatilize the antimony oxide powder in vacuum to obtain the antimony white, and has the advantages of simpler operation process flow, lower production cost, higher antimony white recovery rate and higher purity of the obtained antimony white.
Description
Technical Field
The invention relates to the field of metal smelting, in particular to a device and a method for producing antimony white from antimony oxide powder.
Background
The antimony oxide powder is an intermediate product produced by volatilization smelting of antimony concentrate, and is mainly used for producing crude antimony by reduction. Antimony oxide powderIn the form of powder, the main component of which is Sb2O3And also a small amount of SiO2And the like. The antimony white is antimony trioxide (chemical formula: Sb)2O3) Is mainly used as a flame retardant synergist and a catalyst for petrochemical industry and synthetic fibers in the production of flame retardants mainly used for inflammable substances such as plastics, resins, rubber, textiles, paints and the like. The antimony trioxide content in the antimony white is more than 99 percent.
Generally, the production process of antimony white is classified into a fire process and a wet process, and the fire process is classified into an indirect process and a direct process. At present, more than 90% of antimony white at home and abroad is produced by adopting a pyrogenic indirect method, and the antimony white produced by the indirect method is mainly prepared by taking refined antimony as a raw material through oxidation reaction. Of course, there is also an indirect method for producing antimony white, in which antimony oxide powder is used as a raw material, and the antimony oxide powder is subjected to reduction, refining, oxidation and volatilization, etc. to produce antimony white, however, the process flow is complicated and the production cost is high.
Therefore, it is necessary to provide a method for directly producing antimony white from antimony oxide powder, which has the advantages of simple process flow, low production cost and high recovery rate of antimony element.
Disclosure of Invention
The invention mainly aims to provide a device and a method for producing antimony white by using antimony oxide powder, which aim to solve the problems of complex process flow and high production cost when the antimony white is indirectly produced by using the antimony oxide powder as a raw material in the prior art.
In order to accomplish the above objects, according to one aspect of the present invention, there is provided an apparatus for producing antimony white from antimony oxide powder. The device comprises a vacuum furnace, a condensing device and a vacuumizing unit which are horizontally communicated in sequence; wherein, the vacuum furnace comprises a furnace body; the furnace body is internally provided with a heater and is provided with an antimony oxide powder inlet.
Furthermore, the capacity of the vacuum furnace is 1000-5000 kg.
Further, the heater is selected from a resistance furnace wire or an electromagnetic induction coil.
Further, the electromagnetic induction coils are distributed on the side wall of the interior of the furnace body in a surrounding mode.
Furthermore, the inner wall of the furnace body is provided with a heat insulation layer, and the electromagnetic induction coils are distributed on the inner surface of the heat insulation layer in a surrounding mode.
Further, the vacuum-pumping unit is a vacuum pump.
Further, the condensing equipment is a horizontal shell-and-tube condenser, a vertical shell-and-tube condenser, a sleeve-type condenser or a spiral plate condenser.
In order to accomplish the above objects, according to one aspect of the present invention, there is provided a method of producing antimony white from antimony oxide powder. The method for producing antimony white by using the device and taking antimony oxide powder as a raw material comprises the following steps: step S1, adding the first part of antimony oxide powder into a vacuum furnace for vacuum heating volatilization to obtain antimony oxide smoke dust and residue; step S2, condensing the antimony oxide smoke dust by using condensing equipment to obtain antimony white; wherein the temperature in the vacuum furnace is 500-700 ℃ and the pressure is 1-100 Pa.
Further, the antimony oxide powder comprises 40-70 wt% of Sb2O330 to 60 wt% of SiO2(ii) a Preferably, the antimony oxide powder comprises 55-60 wt% of Sb in percentage by weight2O340 to 45 wt% of SiO2The temperature in the vacuum furnace is 600-615 ℃, and the pressure is 35-50 Pa; or the antimony oxide powder comprises 40-54 wt% of Sb according to weight percentage2O346 to 60 wt% of SiO2The temperature in the vacuum furnace is 635-650 ℃, and the pressure is 20-35 Pa; or the antimony oxide powder comprises 61-70 wt% of Sb according to weight percentage2O330 to 39 wt% of SiO2The temperature in the vacuum furnace is 650-700 ℃, and the pressure is 10-20 Pa.
Further, in the vacuum heating volatilization process, the treatment time is 30-180 min, preferably 50-100 min; preferably, in the vacuum heating volatilization process, the power density in the furnace body of the vacuum furnace is 200-1000W/m3。
Further, the method also comprises the step of sequentially granulating and drying the first part of antimony oxide powder before adding the first part of antimony oxide powder into the vacuum furnace.
Further, the granulation mode is pelletizing or briquetting.
Further, the method further comprises: adding the residual material and a second part of antimony oxide powder into a reverberatory furnace for reduction smelting reaction to produce crude antimony; preferably, the weight ratio of the residual material to the second part of antimony oxide powder is (0.1-0.2) to (0.8-0.9).
Further, blowing a reducing agent and fuel into the reverberatory furnace to carry out reduction smelting reaction; preferably the reducing agent is coal and/or coke; preferably the fuel is one or more of coal, coke or natural gas; the temperature of the reduction smelting reaction is preferably 1000-1100 ℃.
Further, before the vacuum heating volatilization step, the step S1 further includes: after the first part of antimony oxide powder is added into a vacuum furnace, vacuumizing operation and heating operation are simultaneously completed; preferably, the heating rate is 5-100 ℃/min.
By applying the technical scheme of the invention, the temperature in the vacuum furnace is adjusted to be 500-700 ℃ and the pressure is 1-100 Pa, so that Sb is Sb in the environment2O3Can be directly volatilized to obtain antimony oxide smoke dust, and then the subsequent antimony oxide smoke dust enters a condensing device for condensation to obtain antimony white. Meanwhile, in the environment, other impurity components in the antimony oxide powder are few or even non-volatile, and are retained in the vacuum furnace in the form of solid residues for subsequent use. Therefore, the antimony oxide powder can be directly heated and volatilized in vacuum to obtain antimony white, the operation process flow is simpler, the production cost is lower, the recovery rate of the antimony white is higher, and the purity of the obtained antimony white is also higher.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic view showing an apparatus for producing antimony white from antimony oxide powder according to a preferred embodiment of the present invention; and
fig. 2 is a schematic view showing a process for producing antimony white from antimony oxide powder according to a preferred embodiment of the present invention.
Wherein the figures include the following reference numerals:
10. a vacuum furnace; 20. a condensing device; 30. a vacuum pumping unit;
11. a furnace body; 12. a heater; 13. a rotating device; 14. a vacuum furnace cover; 15. a furnace chamber; 16. a furnace bottom; 17. sealing the flange; 18. specially manufacturing the furnace wall; 101. antimony oxide powder enters the inlet.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
As described in the background art, when antimony oxide powder is used as a raw material to indirectly produce antimony white in the prior art, the process flow is complex and the production cost is high. In order to solve the problem, the present invention provides an apparatus for producing antimony white from antimony oxide powder, as shown in fig. 1, the apparatus comprises a vacuum furnace 10, a condensing device 20 and a vacuum unit 30, which are horizontally connected in sequence; wherein, the vacuum furnace 10 comprises a furnace body 11; the furnace body 11 is internally provided with a heater 12, and the furnace body 11 has an antimony oxide powder inlet 101.
The main component of the antimony oxide powder is Sb2O3The minor component being SiO2And the like. According to the invention, antimony oxide powder is added into a vacuum furnace, and the pressure and the temperature in the vacuum furnace are controlled through the vacuum furnace, a condensing device and a vacuumizing unit which are horizontally communicated in sequence, so that the temperature in the vacuum furnace is promoted to be 500-700 ℃, the pressure in the vacuum furnace is 1-100 Pa, and further Sb is Sb in the vacuum furnace in the environment2O3Can be directly volatilized to obtain antimony oxide smoke dust, and then the subsequent antimony oxide smoke dust enters the condensing equipment through the second communicating channel to be condensed to obtain antimony white. Meanwhile, in the environment, other impurity components in the antimony oxide powder are not volatilized and are reserved in the vacuum furnace in the form of solid residues for subsequent use. Therefore, the device of the invention can directly heat and volatilize the antimony oxide powder in vacuum to obtain the antimony white, the operation process flow is simpler, the production cost is lower, the recovery rate of the antimony white is higher, and the purity of the obtained antimony white is also higher.
In a preferred embodiment, as shown in fig. 1, the apparatus comprises a vacuum furnace 10, a condensing device 20 and a vacuum-pumping unit 30, which are horizontally connected in series. The vacuum furnace 10 comprises a furnace body 11, a heater 12, a rotating device 13, a vacuum furnace cover 14, a furnace chamber 15 and a furnace bottom 16. The vacuum furnace cover is positioned at the upper part of the furnace body, and the vacuum furnace cover, the furnace body and the furnace bottom are encircled to form a furnace chamber. The rotating device is positioned on the outer walls of two sides of the furnace body, and the heater is positioned on the inner walls of two sides of the furnace body. A sealing flange 17 and a furnace wall 18 are arranged between the vacuum furnace cover 14 and the furnace body 11.
Preferably, the capacity of the vacuum furnace is 1000-5000 kg. Based on this, the device of the invention is more suitable for industrial production, and can select the vacuum furnace with adaptive capacity according to the production scale requirement, which can be selected by the person skilled in the art according to the actual working conditions in the actual operation.
In a preferred embodiment, the heater includes, but is not limited to, a resistance furnace wire, an electromagnetic induction coil. More preferably, the electromagnetic induction coils are circumferentially distributed on the side wall and the bottom wall inside the furnace body. Therefore, the antimony oxide powder in the vacuum furnace can be heated more uniformly, and further, Sb in the antimony oxide powder2O3The volatilization is more sufficient, and the conversion rate of the antimony white is higher.
Preferably, the inner wall of the furnace body is provided with a heat preservation and insulation layer. Therefore, the rapid dissipation of heat in the vacuum furnace can be effectively avoided, the energy consumption is saved, and enough temperature can be ensured to promote Sb in the antimony oxide powder2O3More fully volatilizes into antimony oxide smoke dust.
Preferably, the vacuum unit 30 is a vacuum pump, which can be selected by a person skilled in the art according to actual working conditions, and will not be described herein. More preferably, the vacuum pump and the condensing device are communicated through a first communication channel, and a vacuum valve is arranged on the first communication channel. Thus, the pressure in the vacuum furnace can be controlled more easily and more accurately.
In a preferred embodiment, the furnace body 11 is provided with turning devices 13 on both sides. The rotating device can effectively realize the tilting of the furnace body and intermittently discharge the residual materials in the vacuum furnace 10. And when the furnace body tilts, the condensing device can not be driven. In the invention, most Sb is volatilized and separated by heating in vacuum2O3Then, the remnant materials are reduced and smelted, and the method can alsoObviously reduces the reduction smelting difficulty and causes a small amount of residual Sb2O3Can be more fully recovered.
Preferably, the lower part of the furnace body 11 is also provided with a vacuum slag discharge port. Preferably, the condensing apparatus 20 is a horizontal shell-and-tube condenser, a vertical shell-and-tube condenser, a double-tube condenser, or a spiral plate condenser. This is a matter that those skilled in the art can select according to the actual working condition, and will not be described herein. Based on the method, the high-temperature antimony oxide smoke dust can be cooled down in a short time to obtain white powdery antimony white.
The invention also provides a method for producing antimony white from antimony oxide powder, as shown in figure 2, the method takes antimony oxide powder as raw material, adopts the device to produce antimony white, and comprises the following steps: step S1, adding the first part of antimony oxide powder into a vacuum furnace 10 for vacuum heating volatilization to obtain antimony oxide smoke dust and residual materials; step S2, condensing the antimony oxide smoke dust by using a condensing device 20 to obtain antimony white; wherein the temperature in the vacuum furnace 10 is 500-700 ℃ and the pressure is 1-100 Pa.
Based on the above reasons, the antimony oxide powder is added into the vacuum furnace 10, the pressure and the temperature in the vacuum furnace 10 are controlled, the temperature in the vacuum furnace 10 is increased to 500-700 ℃, the pressure is increased to 1-100 Pa, and then Sb is increased in the environment2O3Can be directly volatilized to obtain antimony oxide smoke dust, and then the subsequent antimony oxide smoke dust is condensed in a condensing device 20 to obtain antimony white. Meanwhile, in this environment, other impurity components in the antimony oxide powder do not volatilize and remain in the vacuum furnace 10 in the form of solid residue for subsequent use. Therefore, by the method, the antimony oxide powder can be directly heated and volatilized in vacuum to obtain the antimony white, the operation process flow is simpler, the production cost is lower, the purity of the obtained antimony white is higher, and the recovery rate of antimony elements is higher.
For the purpose of further improving the purity of antimony white, in a preferred embodiment, the composition of antimony oxide powder comprises 40-70 wt% of Sb by weight percent2O330 to 60 wt% of SiO2(ii) a Preferably, the antimony oxide powder comprises 55-60 wt% of Sb2O340 to 45 wt% of SiO2The temperature in the vacuum furnace is 600-615 ℃, and the pressure is 35-50 Pa; preferably, the antimony oxide powder comprises 40-54 wt% of Sb2O346 to 60 wt% of SiO2The temperature in the vacuum furnace is 635-650 ℃, and the pressure is 20-35 Pa; preferably, the antimony oxide powder comprises 61-70 wt% of Sb in percentage by weight2O330 to 39 wt% of SiO2The temperature in the vacuum furnace is 650-700 ℃, and the pressure is 10-20 Pa.
Based on promoting Sb in antimony oxide powder2O3The antimony oxide smoke dust can be more fully volatilized to improve the yield of antimony white, and preferably in the vacuum heating volatilization process, the treatment time is 30-180 min, and more preferably 50-60 min. Preferably, in the vacuum heating volatilization process, the power density inside the furnace body 11 of the vacuum furnace 10 is 200-1000W/m3. Based on the method, the pressure environment and the temperature environment in the vacuum furnace can be further balanced, so that Sb in the antimony oxide powder is promoted2O3The volatilization degree of the (C) is larger, and the volatilization process is more stable.
Preferably, before the first part of the antimony oxide powder is charged into the vacuum furnace 10, the method further comprises: and sequentially granulating and drying the first part of antimony oxide powder. The granulation can prevent the antimony oxide powder from splashing in the vacuum furnace 10, effectively prevent the antimony oxide powder from entering the subsequent condensing equipment 20 in the form of powder without fully volatilizing, and the drying treatment can remove the redundant moisture in the antimony oxide powder. By doing so, the purity of antimony white can be further improved. In a preferred embodiment, the granulation is pelletizing or briquetting.
In a preferred embodiment, the method further comprises: and mixing the residual material and the second part of antimony oxide powder, and adding the mixture into a reverberatory furnace to perform reduction smelting reaction to produce crude antimony. Mixing the residual material in the vacuum furnace 10 with the second part of antimony oxide powder, adding the mixture into a reverberatory furnace for reduction reaction, and continuously producing crude antimony. After the vacuum heating and volatilization treatment, a small amount of Sb inevitably remains in the residual material2O3Based on the above operation, the volatilized residue can be further utilizedThe method is used for producing crude antimony and improving the recovery rate of antimony. Particularly, the invention is to separate most Sb by heating and volatilizing in vacuum2O3Then, the residual materials are reduced and smelted, so that the reduction smelting difficulty can be obviously reduced, and a small amount of residual Sb2O3Can be more fully recovered.
Preferably, blowing a reducing agent and a fuel into the reverberatory furnace to perform a reduction reaction; preferably, the reducing agent is H2One or more of CO, coal powder or coke powder; preferred fuels are anthracite and/or natural gas. The temperature of the reduction smelting reaction is preferably 1000-1100 ℃. Thus, the reduction atmosphere in the reverberatory furnace can be better provided, and further, Sb in more defective materials is promoted2O3Converting into crude antimony, and further improving the recovery rate of antimony.
For the purpose of further balancing the pressure and temperature in the vacuum furnace 10, step S1 further includes, before the vacuum heating volatilization step: after the first part of antimony oxide powder is added into the vacuum furnace 10, the vacuumizing operation and the heating operation are completed simultaneously; preferably, the heating rate is 5-100 ℃/min.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
The raw material sources are as follows: the antimony oxide powder is produced by a blast furnace workshop of antimony smelting plants of the limited liability company of antimony industry of tin mine sphalerite, and comprises the following components:
| name of material | Sb2O3 | S | Al2O3 | SiO2 | CaO | FeO | Fe2O3 | MgO |
| Antimony oxide powder (g) | 58.26 | 0.25 | - | 40.26 | 0.050 | 0.02 | 1.05 | 0.11 |
The production of antimony white from the above raw materials using the plant diagram shown in FIG. 1 comprises the following steps:
100kg of the above antimony oxide powder was briquetted (size: 20X 36mm) and dried to obtain antimony oxide briquettes.
Adding the antimony oxide block into a vacuum furnace, vacuumizing the vacuum furnace by a vacuum pump and a heater and simultaneously heating (the heating rate is 20 ℃/min) to ensure that the pressure in the furnace is 40Pa and the temperature is 600 ℃. Keeping the temperature for 30min under the above conditions, and heating and volatilizing antimony oxide powder in a vacuum furnace in vacuum.
The generated antimony oxide smoke dust enters a condensing device for condensation to obtain 56.3kg of antimony white, wherein Sb in the antimony white is Sb2O3The content is 99.4 percent, and the recovery rate of antimony white is 96.6 percent.
Taking out the produced residual material from the vacuum furnace, mixing the residual material with 100kg of the antimony oxide powder, adding the mixture into the reverberatory furnace, and simultaneously blowing fuel coal powder and reducer anthracite into the reverberatory furnace for reduction reaction to obtain crude antimony, wherein the recovery rate of antimony element is 70.2%.
Example 2
The only difference from example 1 is that the temperature in the vacuum furnace was 615 ℃. 56.8kg of antimony white is obtained, and Sb in the antimony white is2O3The content is 99.5 percent, and the recovery rate of antimony white is 97.5 percent. The recovery rate of antimony element is 71.5%.
Example 3
The only difference from example 1 was that the pressure in the vacuum furnace was 35 Pa.
56.5kg of antimony white is obtained, and Sb in the antimony white is2O3The content is 99.6 percent, and the recovery rate of antimony white is 97.0 percent. The recovery rate of antimony element is 70.9%.
Example 4
The difference from example 1 is in the source of the raw materials and the temperature and pressure in the vacuum furnace.
Raw materials: the antimony oxide powder comprises the following components:
| name of material | Sb2O3 | S | Al2O3 | SiO2 | FeO |
| Antimony oxide powder (g) | 53.71 | 0.05 | 0.13 | 45.26 | 0.85 |
The temperature in the vacuum furnace is 650 ℃ and the pressure is 35 Pa.
51.7kg of antimony white is obtained, wherein Sb is contained in the antimony white2O3The content is 99.7 percent, and the recovery rate of antimony white is 96.0 percent. The recovery rate of antimony element is 70.6%.
Example 5
The only difference from example 4 is that the temperature in the vacuum furnace is 635 ℃ and the pressure is 20 Pa.
51.9kg of antimony white is obtained, Sb in the antimony white2O3The content is 99.6 percent, and the recovery rate of antimony white is 96.4 percent. The recovery rate of antimony element is 71.1%.
Example 6
The difference from example 1 is in the source of the raw material and the vacuum furnace internal pressure.
The raw material sources are as follows: the antimony oxide powder comprises the following components:
| name of material | Sb2O3 | S | Al2O3 | SiO2 | FeO |
| Antimony oxide powder (g) | 41.7 | 0.05 | 0.13 | 37.36 | 20.76 |
The pressure in the vacuum furnace was 35 Pa.
40.5kg of antimony white is obtained, and Sb in the antimony white is2O3The content is 99.6 percent, and the recovery rate of antimony white is 97.1 percent. The recovery rate of antimony element is 71.0%.
Example 7
The only difference from example 6 is that the pressure in the vacuum furnace was 20Pa and the temperature was 650 ℃.
40.2kg of antimony white is obtained, and Sb in the antimony white is2O3The content is 99.6 percent, and the recovery rate of antimony white is 96.4 percent. The recovery rate of antimony element is 70.9%.
Example 8
The only difference from example 1 is that the holding time in the vacuum furnace was 180 min.
55.2kg of antimony white is obtained, and Sb in the antimony white is2O3The content is 99.5 percent, and the recovery rate of antimony white is 94.7 percent. The recovery rate of antimony element is 70.5%.
Example 9
The only difference from example 1 is that the holding time in the vacuum furnace was 15 min.
55.8kg of antimony white is obtained, and Sb in the antimony white is2O3The content is 99.5 percent, and the recovery rate of antimony white is 95.8 percent. The recovery rate of antimony element is 70.2%.
Example 10
The difference from example 1 is in the source of the raw materials and the temperature and pressure in the vacuum furnace.
Raw materials: the antimony oxide powder comprises the following components:
| name of material | Sb2O3 | S | Al2O3 | SiO2 | FeO |
| Antimony oxide powder (g) | 65.71 | 0.05 | 0.13 | 33.26 | 1.39 |
The temperature in the vacuum furnace is 650 ℃ and the pressure is 10 Pa.
55.7kg of antimony white is obtained, and Sb in the antimony white is2O3The content is 99.7 percent, and the recovery rate of antimony white is 95.6 percent. The recovery rate of antimony element is 70.6%.
Example 11
The only difference from example 10 is that the temperature in the vacuum furnace was 700 ℃ and the pressure was 20 Pa.
55.9kg of antimony white is obtained, and Sb in the antimony white is2O3The content is 99.8 percent, and the recovery rate of antimony white is 96.0 percent. The recovery rate of antimony element is 71.6%.
Comparative example 1
The only difference from example 1 is that the temperature in the vacuum furnace is 1000 ℃.
Obtaining the antimony white49.0kg of Sb in antimony white2O3The content is 95.5 percent, and the recovery rate of antimony white is 84.1 percent. The recovery rate of antimony element is 60.3%.
Comparative example 2
50.1kg of antimony white was obtained, differing from example 1 only in that the vacuum furnace internal pressure was 80 Pa.
Sb in antimony white2O3The content is 94.4 percent, and the recovery rate of antimony white is 86.0 percent. The recovery rate of antimony element is 60.2%.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (13)
1. The device for producing antimony white from antimony oxide powder is characterized by comprising a vacuum furnace (10), a condensing device (20) and a vacuumizing unit (30), wherein the vacuum furnace, the condensing device and the vacuumizing unit are horizontally communicated in sequence; wherein the vacuum furnace (10) comprises a furnace body (11); the heating furnace is characterized in that a heater (12) is arranged inside the furnace body (11), and the furnace body (11) is provided with an antimony oxide powder inlet (101).
2. The apparatus according to claim 1, wherein the capacity of the vacuum furnace (10) is 1000 to 5000 kg.
3. The device according to claim 1 or 2, characterized in that the heater (12) is selected from a resistance furnace wire or an electromagnetic induction coil.
4. The apparatus according to claim 3, characterized in that the electromagnetic coils are distributed around the inner side wall of the furnace body (11).
5. The device according to claim 4, characterized in that the inner wall of the furnace body (11) is provided with a heat insulation layer, and the electromagnetic induction coil is distributed around the inner surface of the heat insulation layer.
6. A method for producing antimony white from antimony oxide powder, characterized in that the apparatus of any one of claims 1 to 5 is used to produce antimony white from antimony oxide powder, the method comprising the steps of:
step S1, adding the first part of antimony oxide powder into a vacuum furnace (10) for vacuum heating volatilization to obtain antimony oxide smoke dust and residual materials;
step S2, condensing the antimony oxide smoke dust by using condensing equipment (20) to obtain antimony white;
wherein the temperature in the vacuum furnace (10) is 500-700 ℃, and the pressure is 1-100 Pa.
7. The method according to claim 6, wherein the antimony oxide powder has a composition comprising, in weight percent, 40 to 70 wt% of Sb2O330 to 60 wt% of SiO2(ii) a Preferably, the first and second electrodes are formed of a metal,
the antimony oxide powder comprises 55-60 wt% of Sb according to weight percentage2O340 to 45 wt% of SiO2The temperature in the vacuum furnace (10) is 600-615 ℃, and the pressure is 35-50 Pa; alternatively, the first and second electrodes may be,
the antimony oxide powder comprises, by weight, 40-54 wt% of Sb2O346 to 60 wt% of SiO2The temperature in the vacuum furnace (10) is 635-650 ℃, and the pressure is 20-35 Pa; alternatively, the first and second electrodes may be,
the antimony oxide powder comprises 61-70 wt% of Sb according to weight percentage2O330 to 39 wt% of SiO2The temperature in the vacuum furnace (10) is 650-700 ℃, and the pressure is 10-20 Pa.
8. The method according to claim 6 or 7, wherein in the vacuum heating volatilization process, the treatment time is 30-180 min, preferably 50-100 min; preferably, in the vacuum heating volatilization process, the power density inside the furnace body (11) of the vacuum furnace (10) is 200-1000W/m3。
9. The method according to claim 6 or 7, wherein the first part of antimony oxide powder is sequentially granulated and dried before being charged into the vacuum furnace (10).
10. The method of claim 9, wherein the granulation is pelletizing or briquetting.
11. The method according to any one of claims 6 to 10, further comprising: adding the residual material and a second part of antimony oxide powder into a reverberatory furnace for reduction smelting reaction to produce crude antimony; preferably, the weight ratio of the residual material to the second part of antimony oxide powder is (0.1-0.2): (0.8-0.9).
12. The method of claim 11, wherein a reducing agent and a fuel are bubbled into the reverberatory furnace to carry out the reduction smelting reaction; preferably the reductant is coal and/or coke; preferably the fuel is one or more of coal, coke or natural gas; preferably, the temperature of the reduction smelting reaction is 1000-1100 ℃.
13. The method according to claim 6, wherein step S1 further comprises, before the vacuum heat volatilizing step: after the first part of antimony oxide powder is added into the vacuum furnace (10), vacuumizing operation and heating operation are simultaneously completed; preferably, the heating rate is 5-100 ℃/min.
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| CN109628761A (en) * | 2018-12-29 | 2019-04-16 | 焱鑫环保科技有限公司 | A method of stibium trioxide is produced using high antimony secondary smoke dearsenification |
| CN111156820A (en) * | 2020-01-20 | 2020-05-15 | 中国恩菲工程技术有限公司 | Antimony concentrate vacuum smelting device |
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| GB1525588A (en) * | 1974-09-30 | 1978-09-20 | Billiton Research Bv | Process for the preparation of lead and also antimony oxide |
| CN1031214A (en) * | 1988-06-16 | 1989-02-22 | 昆明工学院 | Technology of smelting low grade antimony oxide ore |
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