CN117606239A - Novel magnesian reduction device - Google Patents
Novel magnesian reduction device Download PDFInfo
- Publication number
- CN117606239A CN117606239A CN202311488604.0A CN202311488604A CN117606239A CN 117606239 A CN117606239 A CN 117606239A CN 202311488604 A CN202311488604 A CN 202311488604A CN 117606239 A CN117606239 A CN 117606239A
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- China
- Prior art keywords
- beryllium
- heating
- reaction
- shell
- discharging
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims abstract description 76
- 229910052790 beryllium Inorganic materials 0.000 claims abstract description 75
- 238000006243 chemical reaction Methods 0.000 claims abstract description 73
- 239000002994 raw material Substances 0.000 claims abstract description 32
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000011777 magnesium Substances 0.000 claims abstract description 23
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims description 61
- 238000007599 discharging Methods 0.000 claims description 34
- 238000002844 melting Methods 0.000 claims description 27
- 230000008018 melting Effects 0.000 claims description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 230000000903 blocking effect Effects 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 3
- 238000011084 recovery Methods 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000002893 slag Substances 0.000 abstract description 3
- 238000009833 condensation Methods 0.000 abstract description 2
- 230000005494 condensation Effects 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- JZKFIPKXQBZXMW-UHFFFAOYSA-L beryllium difluoride Chemical compound F[Be]F JZKFIPKXQBZXMW-UHFFFAOYSA-L 0.000 description 17
- 229910001633 beryllium fluoride Inorganic materials 0.000 description 17
- 239000000047 product Substances 0.000 description 16
- 238000006722 reduction reaction Methods 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000002699 waste material Substances 0.000 description 5
- 239000011324 bead Substances 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 4
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- PWOSZCQLSAMRQW-UHFFFAOYSA-N beryllium(2+) Chemical compound [Be+2] PWOSZCQLSAMRQW-UHFFFAOYSA-N 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 239000003517 fume Substances 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- 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
- F27B17/00—Furnaces of a kind not covered by any preceding group
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D3/00—Charging; Discharging; Manipulation of charge
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
- F28D21/00—Heat-exchange apparatus not covered by any of the groups F28D1/00 - F28D20/00
- F28D21/0001—Recuperative heat exchangers
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to the technical field of beryllium preparation, in particular to a novel magnesium reduction device which comprises a reaction device and a receiving device. The invention has the beneficial effects that the beryllium raw material is fed in liquid phase, so that the continuous operation is convenient; impurities of beryllium raw materials are treated in advance, so that the reaction efficiency is improved; the pollution is small, and the reaction recovery rate is high; the efficiency of beryllium raw materials participating in the reaction is improved by a condensation recovery mode; the high-temperature standing receiving product can fully delaminate slag and the product, the raw materials are volatilized and returned to the reaction device to participate in the reaction, the obtained product is a massive product, the oxidation is difficult, and the product quality is high.
Description
Technical Field
The invention relates to the technical field of beryllium preparation, in particular to a novel magnesium reduction device.
Background
The metal beryllium is a strategic material and is an important material commonly used in the fields of electronic elements, automobile manufacturing, aerospace, nuclear and the like. The general steps for preparing beryllium are that beryllium ore is processed by ore dressing to obtain beryllium concentrate, and then refining, reduction reaction, leaching and other modes are used for producing high-purity metal beryllium. The preparation of metallic beryllium by reduction of beryllium fluoride with metallic magnesium at high temperature is a common process for beryllium production, for example, the U.S. and Kazakhstan and China all use the "magnesiothermic reduction method" to prepare metallic beryllium beads.
"magnesian reduction", the basic principle of which is to use the following reaction:
Mg+BeF 2 →Be+MgF 2
in the prior art, metals Mg and BeF 2 The materials are mixed and then reacted at high temperature. The feeding modes are all beryllium fluoride raw material solid feeding.
In such a feeding mode, dust is easily formed due to the low density of beryllium fluoride. The high temperature environment and the intense magnesium thermal reaction can cause the solid feed process to produce significant amounts of beryllium fluoride fumes.
In the prior art, the technology for reducing beryllium fluoride by magnesium heat always has the problem of low direct yield. The literature indicates that the main reason for low yields (only 40% -45%) is that only 55% -60% of the beryllium fluoride participates in the reaction, the remainder being distributed in the reduction fumes or crude product. Incomplete reaction of beryllium fluoride tends to result in waste of raw materials and an increase in cost.
Furthermore, beryllium and its compounds are extremely toxic and belong to a class of carcinogens. The raw material beryllium fluoride has obvious volatility under the reaction temperature condition (800-1000 ℃), and the beryllium fluoride has small density and is easy to form dust, thereby greatly threatening the personal safety of production personnel.
In addition, the beryllium product obtained by the process is the beryllium beads, and the beryllium beads are often exposed in the air environment in the collecting process, so that on one hand, the surface of the metal beryllium is obviously oxidized to reduce the product quality, and on the other hand, a plurality of fine beryllium beads cannot be completely collected, so that the yield of the beryllium product is further reduced.
The existing technology for preparing the metallic beryllium by using the magnesium reduction technology has some problems to be solved. Although some technical solutions to this process are still further improved, there is no development of technology related to the equipment.
Disclosure of Invention
The invention aims to solve the technical problems of providing a novel magnesian reduction device, which can be used for carrying out magnesian reduction on beryllium fluoride under inert protective atmosphere to prepare metal beryllium, and successfully solves the key technical problems of diffusion of high-toxicity beryllium, recovery of beryllium fluoride raw materials, surface oxidation and incomplete recovery of metal beryllium products at high temperature and the like in the production process.
The second key point of the invention is to provide a feeding device matched with a novel feeding mode.
The invention discloses a novel magnesium reduction device, which comprises a reaction device and a receiving device;
the reaction device comprises a first shell, a reaction container and a first heating device; the receiving device comprises a second shell, a receiving container and a second heating device; the reaction container is arranged in the first shell, and the first heating device is arranged between the first shell and the reaction container;
the reaction container comprises a magnesium raw material feed inlet, a molten beryllium raw material feed inlet, a discharge outlet, a condensing device and a discharge device; the molten beryllium raw material feed port is arranged at the top of the reaction container; the magnesium raw material feed inlet is arranged at the side wall position of the upper part of the reaction container; the condensing device is arranged at the upper part of the reaction container; the discharge port is arranged at the bottom of the reaction container; the discharging device is movably arranged at the discharging port and used for controlling discharging;
the receiving device comprises a second shell, a second heating device and a receiving container; the receiving container is arranged inside the second shell, and the second heating device is arranged between the second shell and the receiving container; the receiving container is an open container;
the top of the receiving device is connected with a discharge hole at the bottom of the reaction device.
Further, the reaction vessel adopts a graphite reaction crucible.
Further, the first heating device and the second heating device adopt medium frequency induction heating.
Further, the heating temperature of the first heating device is 600-1350 DEG C
Further, the first heating device is used for controlling the temperature at the outer side of the condensing device and the outer side of the lower part of the reaction container respectively, the temperature at the outer side of the lower part of the reaction container is 800-1350 ℃, and the temperature at the outer side of the condensing device is 600-700 ℃.
Further, the invention also comprises a beryllium raw material melting device which is arranged at the top of the reaction device; the beryllium raw material melting device comprises a third shell, a heating melting furnace body, a third heating device and a beryllium discharging control device;
the bottom of the heating and melting furnace body is provided with a beryllium discharging hole, and the top of the heating and melting furnace body is provided with a beryllium feeding hole and a gas phase passage hole;
the heating and melting furnace body is arranged in the third shell, and the third heating device is arranged between the third shell and the heating and melting furnace body;
the beryllium discharging control device is arranged in the heating melting furnace body, the bottom of the beryllium discharging control device is movably arranged at the beryllium discharging hole, and the outer diameter of the bottom of the beryllium discharging control device is matched with the inner diameter of the beryllium discharging hole in size and is used for blocking the beryllium discharging hole;
the vacuum system and the shielding gas system are respectively connected with the gas phase passage opening through pipelines.
Further, the heating temperature of the third heating device is 1000-1400 ℃.
The invention has the beneficial effects that:
1. the beryllium raw material is fed in a liquid phase, so that continuous operation is convenient;
2. impurities of beryllium raw materials are treated in advance, so that the reaction efficiency is improved;
3. the pollution is small, and the reaction recovery rate is high;
4. the efficiency of beryllium raw materials participating in the reaction is improved by a condensation recovery mode;
5. the high-temperature standing receiving product can fully delaminate slag and the product, the raw materials are volatilized and returned to the reaction device to participate in the reaction, the obtained product is a massive product, the oxidation is difficult, and the product quality is high.
Drawings
FIG. 1 is a schematic diagram of the reaction apparatus;
fig. 2 is a schematic view of the beryllium melting apparatus.
Detailed Description
The following examples are provided to more clearly illustrate the technical examples of the present invention and are not to be construed as limiting the scope of the present invention.
Example 1
A novel magnesian reduction device comprises a reaction device 1 and a receiving device 2;
the reaction device 1 comprises a first shell 11, a reaction container 12 and a first heating device 13; the receiving device 2 comprises a second housing 21, a receiving container 22, and a second heating device 23; the reaction vessel 12 is disposed inside the first housing 11, and the first heating device 13 is disposed between the first housing 11 and the reaction vessel 12;
the reaction vessel 12 includes a magnesium raw material feed port 121, a molten beryllium raw material feed port 122, a discharge port 123, a condensing device 124, and a discharge device 125; the molten beryllium raw material feed port 122 is provided at the top of the reaction vessel 12; the magnesium raw material feed port 121 is provided at the upper side wall position of the reaction vessel 12; the condensing unit 124 is disposed at the upper portion of the reaction vessel 12; the discharge port 123 is arranged at the bottom of the reaction vessel 12; the discharging device 125 is movably arranged at the discharging hole 123 and is used for controlling discharging;
the receiving device 2 comprises a second housing 21, a second heating device 23, a receiving container 22; the receiving container 22 is disposed inside the second housing 21, and the second heating device 23 is disposed between the second housing 21 and the receiving container 22; the receiving container 22 is an open container;
the top of the receiving device 2 is connected with a discharge port 123 at the bottom of the reaction device 1.
In the embodiment, the reaction vessel 12 is a graphite reaction crucible.
In the embodiment, the first heating device 13 and the second heating device 23 adopt medium frequency induction heating.
In the embodiment, the temperature of the first heating device 13 is controlled at the outside of the condensing device 124 and the outside of the lower portion of the reaction vessel 12, the outside temperature of the lower portion of the reaction vessel 12 is 800-1350 ℃, and the outside temperature of the condensing device 124 is 600-700 ℃.
The invention further comprises a beryllium raw material melting device 3, wherein the beryllium raw material melting device 3 is arranged at the top of the reaction device 1; the beryllium raw material melting device 3 comprises a third shell 31, a heating melting furnace body 32, a third heating device 33 and a beryllium discharging control device 323;
a beryllium discharging port 324 is arranged at the bottom of the heating and melting furnace body 32, and a beryllium feeding port 321 and a gas phase passage port 322 are arranged at the top of the heating and melting furnace body 32;
the heating and melting furnace body 32 is disposed inside the third housing 31, and the third heating device 33 is disposed between the third housing 31 and the heating and melting furnace body 32;
the beryllium discharging control device 323 is arranged in the heating and melting furnace body 32, the bottom of the beryllium discharging control device is movably arranged at the beryllium discharging port 324, and the outer diameter of the bottom of the beryllium discharging control device 323 is matched with the inner diameter of the beryllium discharging port 324 in size and is used for blocking the beryllium discharging port 324;
the vacuum system and the shielding gas system are respectively connected with the gas phase passage opening 322 through pipelines.
In the embodiment, the heating temperature of the third heating device 33 is 1000-1400 ℃.
In order to further illustrate the beneficial effects of the present invention, the following application examples are specifically set:
application example 1
Adding 500g of beryllium fluoride, setting the temperature of the reaction vessel 12 at 900-1000 ℃ and setting the temperature of the condenser at 650 ℃; 235g of magnesium metal particles are added, after 1 hour of reaction, the reaction vessel 12 is quickly heated to 1350 ℃ and kept for 15 minutes. The discharging device 125 was turned on, and the reaction product and magnesium fluoride waste slag were discharged into the reaction product receiving device 2, and the temperature of the receiving device 2 was set to 1300 ℃ and kept for 20min.
After the reaction was completed, the condenser was weighed, and the mass of beryllium fluoride attached was 45g after calculation. The oxygen content in the metal beryllium product in the receiving device 2 is 0.075%, the mass of the beryllium product is 72.8g, and the comprehensive direct recovery rate of the beryllium product reaches 85.2%. The volatilization loss mass of the beryllium fluoride is 7.8g, and the residual mass of beryllium element in the magnesium fluoride waste residue is 12.8g.
Application example 2
750g of beryllium fluoride is added, the temperature of the reaction vessel 12 is kept between 850 and 1000 ℃, and the temperature of the condenser is set at 700 ℃; 350g of magnesium metal particles are added, after 1.5h of reaction, the temperature of the reaction vessel 12 is quickly raised to 1350 ℃, and the temperature is kept for 20min. The discharge device 125 was turned on, and the reaction product and magnesium fluoride waste were discharged into the reaction product receiving device 2, and the temperature of the receiving device 2 was set to 1350 deg.c and kept for 90min. Continuous vacuumizing operation is carried out on the receiving device 2, so that magnesium metal in the beryllium metal product is fully volatilized and removed in a high-temperature vacuum environment
After the reaction was completed, the condenser was weighed, and the mass of beryllium fluoride attached was calculated to be 70g. The oxygen content of the metal beryllium product in the receiving device 2 is 0.1%, the magnesium element content is only 0.11%, the quality of the beryllium product is 107.4g, and the comprehensive direct yield of the beryllium product reaches 84.1%. The volatilization loss mass of the beryllium fluoride is 13.9g, and the residual mass of the beryllium element in the magnesium fluoride waste residue is 20.1g.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (7)
1. The novel magnesium reduction device is characterized by comprising a reaction device (1) and a receiving device (2);
the reaction device (1) comprises a first shell (11), a reaction container (12) and a first heating device (13); the receiving device (2) comprises a second shell (21), a receiving container (22) and a second heating device (23); the reaction vessel (12) is arranged inside the first shell (11), and the first heating device (13) is arranged between the first shell (11) and the reaction vessel (12);
the reaction vessel (12) comprises a magnesium raw material feed port (121), a molten beryllium raw material feed port (122), a discharge port (123), a condensing device (124) and a discharge device (125); the molten beryllium raw material feed port (122) is arranged at the top of the reaction container (12); the magnesium raw material feeding port (121) is arranged at the side wall position of the upper part of the reaction container (12); the condensing device (124) is arranged at the upper part of the reaction vessel (12); the discharge port (123) is arranged at the bottom of the reaction container (12); the discharging device (125) is movably arranged at the discharging opening (123) and is used for controlling discharging;
the receiving device (2) comprises a second shell (21), a second heating device (23) and a receiving container (22); the receiving container (22) is arranged inside the second shell (21), and the second heating device (23) is arranged between the second shell (21) and the receiving container (22); the receiving container (22) is an open container;
the top of the receiving device (2) is connected with a discharge hole (123) at the bottom of the reaction device (1).
2. The novel magnesium reduction device according to claim 1, wherein the reaction vessel (12) employs a graphite reaction crucible.
3. The novel magnesium reduction device according to claim 1, wherein the first heating device (13) and the second heating device (23) adopt medium frequency induction heating.
4. The novel magnesium reduction device according to claim 1, wherein the heating temperature of the first heating device (13) is 600-1350 ℃.
5. The novel magnesium reduction device according to claim 1, wherein the first heating device (13) is respectively controlled in temperature outside the condensing device (124) and outside the lower part of the reaction vessel (12), the temperature outside the lower part of the reaction vessel (12) is 800-1350 ℃, and the temperature outside the condensing device (124) is 600-700 ℃.
6. The novel magnesium reduction device according to any one of claims 1 to 5, further comprising a beryllium raw material melting device (3), wherein the beryllium raw material melting device (3) is arranged at the top of the reaction device (1); the beryllium raw material melting device (3) comprises a third shell (31), a heating melting furnace body (32), a third heating device (33) and a beryllium discharging control device (323);
a beryllium discharging hole (324) is formed in the bottom of the heating and melting furnace body (32), and a beryllium feeding hole (321) and a gas phase passage hole (322) are formed in the top of the heating and melting furnace body (32);
the heating and melting furnace body (32) is arranged in the third shell (31), and the third heating device (33) is arranged between the third shell (31) and the heating and melting furnace body (32);
the beryllium discharging control device (323) is arranged in the heating and melting furnace body (32), the bottom of the beryllium discharging control device is movably arranged at the beryllium discharging hole (324), and the outer diameter of the bottom of the beryllium discharging control device (323) is matched with the inner diameter of the beryllium discharging hole (324) in size and is used for blocking the beryllium discharging hole (324);
the vacuum system and the shielding gas system are respectively connected with the gas phase passage opening (322) through pipelines.
7. The novel magnesium reduction device according to claim 6, wherein the heating temperature of the third heating device (33) is 1000-1400 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311488604.0A CN117606239A (en) | 2023-11-09 | 2023-11-09 | Novel magnesian reduction device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311488604.0A CN117606239A (en) | 2023-11-09 | 2023-11-09 | Novel magnesian reduction device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117606239A true CN117606239A (en) | 2024-02-27 |
Family
ID=89952504
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311488604.0A Pending CN117606239A (en) | 2023-11-09 | 2023-11-09 | Novel magnesian reduction device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117606239A (en) |
-
2023
- 2023-11-09 CN CN202311488604.0A patent/CN117606239A/en active Pending
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