CN112044362A - Continuous synthesis device for magnesium chloride - Google Patents
Continuous synthesis device for magnesium chloride Download PDFInfo
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- CN112044362A CN112044362A CN202010826702.0A CN202010826702A CN112044362A CN 112044362 A CN112044362 A CN 112044362A CN 202010826702 A CN202010826702 A CN 202010826702A CN 112044362 A CN112044362 A CN 112044362A
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- reactor
- solid material
- tank
- receiving tank
- gas
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- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 20
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 title claims description 8
- 229910001629 magnesium chloride Inorganic materials 0.000 title claims description 4
- 239000011343 solid material Substances 0.000 claims abstract description 47
- 238000005303 weighing Methods 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 13
- 229910052749 magnesium Inorganic materials 0.000 claims description 20
- 239000011777 magnesium Substances 0.000 claims description 20
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- KUCOIJGMWNWHGO-UHFFFAOYSA-N dimethyl carbonate;magnesium Chemical compound [Mg].COC(=O)OC KUCOIJGMWNWHGO-UHFFFAOYSA-N 0.000 abstract description 4
- 239000011521 glass Substances 0.000 abstract description 4
- 238000010924 continuous production Methods 0.000 abstract description 2
- 230000036632 reaction speed Effects 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 38
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000005192 partition Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- -1 and the like Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000004584 weight gain Effects 0.000 description 1
- 235000019786 weight gain Nutrition 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F17/00—Metallocenes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a continuous synthesis device of magnesium dimethyl carbonate, which comprises a solid material high-level tank, a reactor and a receiving tank, wherein the solid material high-level tank is arranged at the upper end of the reactor, the receiving tank is arranged at the lower end of the reactor, a feed valve is arranged between the solid material high-level tank and the reactor, an air inlet pipe is arranged at the upper part of the reactor, a gas flowmeter is arranged on the air inlet pipe, an air outlet pipe is arranged on one side of the upper end of the receiving tank, an air outlet valve is arranged on the air outlet pipe, and weighing equipment is arranged at the lower end of the. The laboratory type device which is synthesized in a small amount by using a glass instrument originally becomes a device which can realize industrial continuous production; the feeding amount of the gas material is accurately controlled, the reaction speed is accurately controlled, the condition of the residual amount of the solid material is judged according to the weight increment of the receiving tank, and the solid material is accurately supplemented by utilizing a weighing device and a control valve on a high-level tank of the solid material, so that the long-time non-stop of the whole synthesis process is realized, and the production capacity of the magnesium dimethyl carbonate is greatly improved.
Description
Technical Field
The invention relates to the field of MO source production, in particular to a continuous synthesis device for magnesium chloride.
Background
At present, in the metallocene magnesium synthesis process of gas-solid reaction of cyclopentadiene and metal magnesium, small-sized glass equipment is mainly adopted for carrying out the gas-solid reaction. The conventional glass equipment is small in size, the yield of a single batch of synthesized magnesium metallocene crude product is only 50-200 g, the device needs to be dismantled after each batch of synthesis is finished, the material can be fed again to carry out the next batch of synthesis after cleaning and drying, and the requirement of mass production level cannot be met. Therefore, it is very important to solve the problem of low yield of the single-batch synthesized magnesium metallocene crude product.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a continuous synthesis device for magnesium dicocene, which can be used for feeding enough solid materials into a high-level tank of the solid materials at one time, interlocking a control valve with a high-level tank weighing device through timing opening and closing, intermittently feeding the materials into a reactor, and accurately controlling the gas feeding amount by using a gas flow regulating device so as to keep the whole synthesis reaction to be continuously and controllably carried out without frequently disassembling and feeding the materials, thereby achieving the purpose of efficiently synthesizing the magnesium dicocene.
The invention provides a continuous synthesis device of magnesium dimethyl carbonate, which comprises a solid material high-level tank, a reactor and a receiving tank, wherein the solid material high-level tank is arranged at the upper end of the reactor, the receiving tank is arranged at the lower end of the reactor, a feed valve is arranged between the solid material high-level tank and the reactor, an air inlet pipe is arranged at the upper part of the reactor, a gas flowmeter is arranged on the air inlet pipe, an air outlet pipe is arranged on one side of the upper end of the receiving tank, an air outlet valve is arranged on the air outlet pipe, weighing equipment is arranged at the lower end of the receiving tank, and a perforated partition plate is arranged at the middle section of the reactor.
The further improvement lies in that: the solid material weighing device is characterized in that a corrugated hose is arranged between the solid material high-level tank and the feeding valve, a weighing device is arranged on the solid material high-level tank, and materials in the solid material high-level tank are weighed through the weighing device.
The further improvement lies in that: the reactor is wrapped by a heating device with a temperature control device, and the reactor is heated and controlled in temperature by the heating device.
The further improvement lies in that: an eccentric baffle is arranged in the receiving tank and is arranged beside the air outlet pipe.
The further improvement lies in that: the reactor is provided with a thermometer sleeve, and a thermometer is inserted into the thermometer sleeve to detect the temperature.
The reactor is provided with an automatically controlled gas inlet device and an automatically controlled solid material supplementing device, the solid material is supplemented with the solid material through the opening and closing of a feed valve according to the instruction of an automatic control system, and the gas material accurately controls the gas feeding amount through a gas flowmeter, preferably a mass flowmeter.
The material of the reactor and the thermo-well tube can be other metal materials which do not react with gas materials, such as copper, and the like, and non-metal materials which do not react with gas, such as graphite, and the like; the heating device of the device is an aluminum heating block with a temperature control device, an eccentric baffle is designed in the receiving tank of the device, so that the gas circulation path can be effectively increased, and the risk that the product powder is taken out of the receiving tank is reduced.
The synthesis device high-level tank is designed to be large in size and provided with a replacement port, so that a large amount of solid materials can be added at one time, the solid materials can be supplemented in time under the condition that the feed valve is closed, and clean air is replaced through the replacement port so as to supplement the solid materials under the condition that the synthesis reaction is not stopped; the corrugated hose is designed under the high-level tank, so that the stress can be greatly reduced, and the measurement accuracy of the weighing module is improved.
A weighing device is designed at the bottom of the receiving tank, and the reaction proportion of the solid materials can be calculated according to the weight gain of the receiving tank in the reflecting process, so that the solid materials can be supplemented in time.
The heating device is designed into a heating aluminum block with a temperature control system, and the temperature of the reaction zone is uniform and stable by means of indirect heat transfer between the temperature controller and the aluminum block.
The device can be divided into a reactor, a receiving tank, a high-level tank, a connecting pipeline and the like, the interface of the high-temperature part uses knife edge flange rice flour, the interface of the low-temperature part uses a tetrafluoro or rubber sealing washer for sealing, and the whole device can be conveniently disassembled so as to be conveniently cleaned and maintained regularly.
The device can be applied to other gas-solid reactions, such as the synthesis preparation of ferrocene by cyclopentadiene and metallic iron at high temperature.
The invention has the beneficial effects that: the laboratory type device which is synthesized in a small amount by using a glass instrument originally becomes a device which can realize industrial continuous production; the feeding amount of the gas material is accurately controlled, the reaction speed is accurately controlled, the condition of the residual amount of the solid material is judged according to the weight increment of the receiving tank, and the solid material is accurately supplemented by utilizing a weighing device and a control valve on a high-level tank of the solid material, so that the long-time non-stop of the whole synthesis process is realized, and the production capacity of the magnesium dimethyl carbonate is greatly improved.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Wherein: 1-solid material high-level tank, 2-reactor, 3-receiving tank, 4-feed valve, 5-gas inlet pipe, 6-gas flowmeter, 7-gas outlet pipe, 8-gas outlet valve, 9-weighing device, 10-corrugated hose, 11-weighing device, 12-heating device, 13-eccentric baffle, 14-thermometer sleeve and 15-perforated partition plate.
Detailed Description
In order to further understand the present invention, the following detailed description will be made with reference to the following examples, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
As shown in fig. 1, this embodiment provides a magnesium carbonate continuous synthesis device, including solid material high-order jar 1, reactor 2 and receiving tank 3, solid material high-order jar 1 sets up the upper end at reactor 2, receiving tank 3 sets up the lower extreme at reactor 2, be provided with feed valve 4 between solid material high-order jar 1 and the reactor 2, 2 upper portions of reactor are provided with intake pipe 5, be provided with gas flowmeter 6 in the intake pipe 5, receiving tank 3 upper end one side is provided with outlet duct 7, be provided with air outlet valve 8 on the outlet duct 7, receiving tank 3 lower extreme is provided with weighing-appliance 9, reactor 2 middle section is provided with the baffle 15 that punches. Be provided with corrugated hose 10 between solid material high-order jar 1 and the feed valve 4, be provided with weighing device 11 on the solid material high-order jar 1, weigh the material in the solid material high-order jar 1 through weighing device 11. The reactor 2 is externally wrapped with a heating device 12 with a temperature control device, and the heating device 12 is used for heating and controlling the temperature of the reactor 2. An eccentric baffle 13 is arranged in the receiving tank 3, and the eccentric baffle 13 is arranged beside the air outlet pipe 7. The reactor 2 is provided with a thermo-well tube 14, and a thermometer is inserted into the thermo-well tube 14 to detect the temperature.
The solid material high-level tank 1 and the reactor 2 are vertically arranged or obliquely arranged, and the angle is more than 45 degrees, so that the solid material can fall down by weight; the feeding speed of the gas material is controlled by a gas flowmeter 6; a thermo-well tube 14 is welded to the side of the reactor 2 to measure the real temperature of the reactor 2; the center of the reactor 2 is welded with a perforated clapboard 15 for supporting solid materials, the perforated clapboard 15 is provided with densely distributed small holes so as to facilitate the gas to pass through the product steam produced by the reaction, the aperture of the perforated clapboard 15 is designed according to the volume of the solid materials and the flow rate of the gas, and the aperture is reduced as much as possible on the premise that the aperture of the general clapboard meets the requirement of the gas flow in the process so as to reduce the solid materials to fall into a receiving tank through the small holes; the heating device 12 is designed according to the size of the reaction area of the reactor and is provided with an automatic temperature control device and a heat insulation layer; an eccentric baffle 13 is designed in the receiving tank 3, the eccentric baffle 13 forces the gas to flow through the lower end of the eccentric baffle 13, the gas path in the receiving tank 3 is increased, the cooling and collection of the synthesized product are facilitated, and the eccentric baffle 13 is close to the end of the gas outlet pipe 7, so that the storage space of the corresponding synthesized product is larger; unreacted gas materials can be discharged to a tail gas treatment device through the gas outlet valve 8, and after the gas outlet valve 8 is closed, external air can be effectively prevented from entering the receiving tank 3 to influence the product quality.
Firstly, adding enough magnesium chips into a solid material high-level tank 1, opening a feed valve 4, allowing a proper amount of magnesium chips to fall on a perforated partition plate 15 in a reactor 2, and then closing the feed valve 4; opening an air outlet valve 8 and a gas flowmeter 6 and purging the whole reaction system by using cyclopentadiene and argon gas with proper flow; then the whole device is heated to a proper temperature through a heating device 12 to initiate the reaction of cyclopentadiene and magnesium chips, the magnesium metallocene produced by the reaction is carried by argon gas at a high temperature to pass through a receiving tank 3 and is cooled in the receiving tank 3 to be solid and reserved, and the argon gas and a small amount of unreacted cyclopentadiene gas are discharged to a tail gas treatment device through a gas outlet valve 8. Along with the reaction, the receiving tank 3 continuously increases the weight because of the increase of the amount of the magnesium cyclopentadienyl, the residual amount of the magnesium chips on the partition plate is calculated according to the weight increasing value of the weighing device 11, when the residual amount of the magnesium chips is less than 30% of the initial feeding amount, the gas flow meter 6 is adjusted, the feeding valve 4 is opened, the proper amount of the magnesium chips are supplemented to the punching partition plate 15 according to the weight reducing value displayed by the weighing device 11 on the solid material high-level tank 1, then the gas flow meter 6 is adjusted to control the flow to the optimal air inflow, and the continuous synthesis process for preparing the magnesium cyclopentadienyl solid at high temperature by using the gas cyclopentadiene and the solid magnesium chips is realized.
Claims (5)
1. A continuous synthesis device of magnesium chloride is characterized in that: including solid material overhead tank (1), reactor (2) and receiving tank (3), solid material overhead tank (1) sets up the upper end in reactor (2), receiving tank (3) set up the lower extreme in reactor (2), be provided with feed valve (4) between solid material overhead tank (1) and reactor (2), reactor (2) upper portion is provided with intake pipe (5), be provided with gas flowmeter (6) on intake pipe (5), receiving tank (3) upper end one side is provided with outlet duct (7), be provided with air outlet valve (8) on outlet duct (7), receiving tank (3) lower extreme is provided with weighing-appliance (9), reactor (2) middle section is provided with baffle (15) that punches.
2. The continuous synthesis device of magnesium dicocene as claimed in claim 1, characterized in that: the solid material weighing device is characterized in that a corrugated hose (10) is arranged between the solid material high-level tank (1) and the feeding valve (4), a weighing device (11) is arranged on the solid material high-level tank (1), and materials in the solid material high-level tank (1) are weighed through the weighing device (11).
3. The continuous synthesis device of magnesium dicocene as claimed in claim 1, characterized in that: the reactor (2) is externally wrapped with a heating device (12) with a temperature control device, and the heating device (12) is used for heating and controlling the temperature of the reactor (2).
4. The continuous synthesis device of magnesium dicocene as claimed in claim 1, characterized in that: an eccentric baffle (13) is arranged in the receiving tank (3), and the eccentric baffle (13) is arranged beside the air outlet pipe (7).
5. The continuous synthesis device of magnesium dicocene as claimed in claim 1, characterized in that: the reactor (2) is provided with a thermo-well tube (14), and a thermometer is inserted into the thermo-well tube (14) to detect the temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010826702.0A CN112044362A (en) | 2020-08-17 | 2020-08-17 | Continuous synthesis device for magnesium chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010826702.0A CN112044362A (en) | 2020-08-17 | 2020-08-17 | Continuous synthesis device for magnesium chloride |
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| Publication Number | Publication Date |
|---|---|
| CN112044362A true CN112044362A (en) | 2020-12-08 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010826702.0A Pending CN112044362A (en) | 2020-08-17 | 2020-08-17 | Continuous synthesis device for magnesium chloride |
Country Status (1)
| Country | Link |
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| CN (1) | CN112044362A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115043884A (en) * | 2022-06-15 | 2022-09-13 | 江苏南大光电材料股份有限公司 | System and method for preparing magnesium chloride |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1765486A (en) * | 2004-10-28 | 2006-05-03 | 中国石油化工股份有限公司 | Continuous high temperature gas solid reactor |
| CN102153594A (en) * | 2011-02-15 | 2011-08-17 | 江苏南大光电材料股份有限公司 | Magnesocene synthesizer |
| US20150202582A1 (en) * | 2014-01-20 | 2015-07-23 | Johnson Matthey Process Technologies, Inc. | Addition system and process for adding material to one or more units |
| CN109331747A (en) * | 2018-11-09 | 2019-02-15 | 成都蜀菱科技发展有限公司 | A kind of gas-solid reaction device and production equipment that silicon tetrachloride is mass produced |
| CN212651789U (en) * | 2020-08-17 | 2021-03-05 | 安徽亚格盛电子新材料有限公司 | Continuous synthesis device for magnesium chloride |
-
2020
- 2020-08-17 CN CN202010826702.0A patent/CN112044362A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1765486A (en) * | 2004-10-28 | 2006-05-03 | 中国石油化工股份有限公司 | Continuous high temperature gas solid reactor |
| CN102153594A (en) * | 2011-02-15 | 2011-08-17 | 江苏南大光电材料股份有限公司 | Magnesocene synthesizer |
| US20150202582A1 (en) * | 2014-01-20 | 2015-07-23 | Johnson Matthey Process Technologies, Inc. | Addition system and process for adding material to one or more units |
| CN109331747A (en) * | 2018-11-09 | 2019-02-15 | 成都蜀菱科技发展有限公司 | A kind of gas-solid reaction device and production equipment that silicon tetrachloride is mass produced |
| CN212651789U (en) * | 2020-08-17 | 2021-03-05 | 安徽亚格盛电子新材料有限公司 | Continuous synthesis device for magnesium chloride |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115043884A (en) * | 2022-06-15 | 2022-09-13 | 江苏南大光电材料股份有限公司 | System and method for preparing magnesium chloride |
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