CN115043884A - System and method for preparing magnesium chloride - Google Patents
System and method for preparing magnesium chloride Download PDFInfo
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- CN115043884A CN115043884A CN202210681629.1A CN202210681629A CN115043884A CN 115043884 A CN115043884 A CN 115043884A CN 202210681629 A CN202210681629 A CN 202210681629A CN 115043884 A CN115043884 A CN 115043884A
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- 238000000034 method Methods 0.000 title claims abstract description 10
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 title claims description 16
- 229910001629 magnesium chloride Inorganic materials 0.000 title claims description 8
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 111
- 239000011777 magnesium Substances 0.000 claims abstract description 111
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 94
- ZSWFCLXCOIISFI-UHFFFAOYSA-N endo-cyclopentadiene Natural products C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 claims abstract description 82
- 238000006243 chemical reaction Methods 0.000 claims abstract description 63
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 37
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 37
- 238000000859 sublimation Methods 0.000 claims abstract description 34
- 230000008022 sublimation Effects 0.000 claims abstract description 34
- 238000002309 gasification Methods 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 23
- 239000012043 crude product Substances 0.000 claims abstract description 16
- 238000000746 purification Methods 0.000 claims abstract description 14
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 73
- 239000007789 gas Substances 0.000 claims description 34
- 239000012159 carrier gas Substances 0.000 claims description 14
- 239000011261 inert gas Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000004065 semiconductor Substances 0.000 abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 229910052786 argon Inorganic materials 0.000 description 4
- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000005485 electric heating Methods 0.000 description 4
- QWDJLDTYWNBUKE-UHFFFAOYSA-L magnesium bicarbonate Chemical compound [Mg+2].OC([O-])=O.OC([O-])=O QWDJLDTYWNBUKE-UHFFFAOYSA-L 0.000 description 4
- MHYQBXJRURFKIN-UHFFFAOYSA-N C1(C=CC=C1)[Mg] Chemical compound C1(C=CC=C1)[Mg] MHYQBXJRURFKIN-UHFFFAOYSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000013022 venting Methods 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- USZGMDQWECZTIQ-UHFFFAOYSA-N [Mg](C1C=CC=C1)C1C=CC=C1 Chemical compound [Mg](C1C=CC=C1)C1C=CC=C1 USZGMDQWECZTIQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- 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
- B01J19/0006—Controlling or regulating processes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention discloses a preparation system and a preparation method of magnesium cyclopentadienyl, wherein the preparation system comprises a synthesis device and a purification device, the synthesis device is used for synthesizing cyclopentadiene and magnesium to obtain a magnesium cyclopentadienyl crude product, the purification device is used for purifying the magnesium cyclopentadienyl crude product to obtain high-purity magnesium cyclopentadienyl, and the preparation method comprises the following steps: the synthesis device comprises a first generator, a first receiver and a reaction chamber, wherein the first generator is provided with a fractionating column, the reaction chamber is respectively connected with the first receiver and the fractionating column, and the reaction chamber is internally provided with a plurality of synthesis columns which are vertically distributed; the purification device comprises a second generator, a second receiver, a sublimation pipe and a gasification pipe, wherein the sublimation pipe is connected with the second generator and is vertically distributed, and the gasification pipe is respectively connected with the second receiver and the sublimation pipe. The method can synthesize and purify the high-purity magnesium metallocene directly under normal pressure, can meet the use requirements of the semiconductor industry, has low cost and simple operation, and is suitable for mass production.
Description
Technical Field
The invention belongs to the technical field of preparation of magnesium cyclopentadienyl, and particularly relates to a magnesium cyclopentadienyl preparation system and a magnesium cyclopentadienyl preparation method.
Background
The magnesium cyclopentadienyl is also called bis (cyclopentadienyl) magnesium, white crystal and has the sublimation temperature of 100 ℃. In the prior art, the synthesis of magnesium metallocenes is generally carried out by reacting cyclopentadiene with magnesium metal.
In the existing metallocene magnesium synthesis process, small glass equipment is mainly adopted, the single-batch synthesis of metallocene magnesium is only about 100g, the yield and the efficiency are low, and the synthesized metallocene magnesium has low purity and cannot meet mass production.
Therefore, in order to solve the above technical problems, it is necessary to provide a system and a method for preparing magnesium metallocene.
Disclosure of Invention
In view of the above, the present invention is directed to a system and a method for preparing magnesium metallocene.
In order to achieve the above object, an embodiment of the present invention provides the following technical solutions:
a magnesium cyclopentadienyl preparation system, the preparation system includes synthesizer and purification device, the synthesizer is used for synthesizing cyclopentadiene and magnesium and obtains magnesium cyclopentadienyl crude product, purification device is used for purifying magnesium cyclopentadienyl crude product and obtains high-purity magnesium cyclopentadienyl, wherein:
the synthesis device comprises a first generator, a first receiver and a reaction chamber, wherein the first generator is provided with a fractionating column, the reaction chamber is respectively connected with the first receiver and the fractionating column, and the reaction chamber is internally provided with a plurality of synthesis columns which are vertically distributed;
the purification device comprises a second generator, a second receiver, a sublimation pipe and a gasification pipe, wherein the sublimation pipe is connected with the second generator and is vertically distributed, and the gasification pipe is respectively connected with the second receiver and the sublimation pipe.
In one embodiment, the first generator is provided with a first feeding port, and the reaction chamber is provided with a second feeding port; and/or the presence of a gas in the gas,
the fractionating column is a thorn-shaped fractionating column; and/or the presence of a gas in the gas,
the first receiver is connected with a buffer bottle, and the buffer bottle is connected with a first tail gas bottle.
In one embodiment, a first heating device is arranged outside the reaction chamber; and/or the presence of a gas in the gas,
the reactor is characterized in that a plurality of horizontally distributed baffles are arranged inside the reaction chamber, a plurality of clearance grooves are formed in the baffles, and the size of each clearance groove is 1-2 mm.
In one embodiment, a first temperature sensor and a second temperature sensor are respectively inserted outside the first generator and the reaction chamber through sleeves.
In one embodiment, the second generator is a front or middle distillate bottle; and/or the presence of a gas in the gas,
and the second receiver is connected with a bubble counter, and the bubble counter is connected with a second tail gas cylinder.
In one embodiment, a third temperature sensor and a fourth temperature sensor are respectively inserted outside the second generator and the sublimation pipe through sleeves.
In one embodiment, a second heating device is arranged outside the sublimation pipe; and/or the presence of a gas in the gas,
a third heating device is arranged outside the gasification pipe; and/or the presence of a gas in the gas,
and a bottle opening of the second receiver is provided with a fourth heating device.
The technical scheme provided by another embodiment of the invention is as follows:
a method for preparing a magnesium metallocene, the method comprising:
s1, under the inert atmosphere, introducing cyclopentadiene vapor generated by the first generator into a reaction chamber along with carrier gas, reacting with magnesium in the reaction chamber, and generating a crude product of magnesium diclocide which is deposited in a first receiver;
and S2, adding the crude metallocene magnesium into a second generator for heating rectification, sublimating and gasifying, and collecting high-purity metallocene magnesium through a second receiver.
In an embodiment, the step S1 specifically includes:
introducing inert gas into the synthesis device to ensure that the synthesis device is in an inert atmosphere;
respectively adding 500-900 parts by mass of cyclopentadiene and 90-130 parts by mass of magnesium into a first generator and a reaction chamber;
heating the first generator, and introducing cyclopentadiene vapor generated at the temperature of 100-180 ℃ into a reaction chamber along with carrier gas;
heating a synthesis column in a reaction chamber, reacting cyclopentadiene steam with magnesium at 510-540 ℃, and generating a crude product of magnesium dicocene and settling the crude product in a first receiver.
In an embodiment, the step S2 is specifically:
heating the sublimation pipe to 170-180 ℃, and heating the gasification pipe to 220-240 ℃;
adding the crude magnesium dicocene into a front fraction bottle, heating the front fraction bottle, carrying out heating rectification at the temperature of 190-220 ℃, sublimating and gasifying, and collecting front fraction;
replacing the front fraction bottle with the middle fraction bottle;
heating the sublimation pipe to 170-180 ℃, and heating the gasification pipe to 220-240 ℃;
adding the front fraction into a middle fraction bottle, heating the middle fraction bottle, carrying out heating rectification at the temperature of 190-220 ℃, sublimating, gasifying, and collecting high-purity magnesium metallocene.
The invention has the following beneficial effects:
the invention can synthesize and purify the high-purity magnesium metallocene directly under normal pressure, can meet the use requirements of the semiconductor industry, has simple structure of a preparation system, lower cost of the preparation method and simple operation, and is suitable for mass production.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic block diagram of a magnesium bis-metallocene production system according to the present invention;
FIG. 2 is a schematic flow diagram of a process for preparing a magnesium metallocene according to the present invention;
FIG. 3 is a schematic diagram showing the structure of a synthesizing apparatus in example 1 of the present invention;
FIG. 4 is a schematic structural diagram of a purification apparatus in example 1 of the present invention.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the drawings in the embodiment of the present invention, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the invention discloses a magnesium bis (cyclopentadienyl) preparation system, which comprises a synthesis device 10 and a purification device 20, wherein the synthesis device 10 is used for synthesizing cyclopentadiene and magnesium to obtain a magnesium bis (cyclopentadienyl) crude product, and the purification device 20 is used for purifying the magnesium bis (cyclopentadienyl) crude product to obtain high-purity magnesium bis (cyclopentadienyl).
Referring to fig. 2, the invention also discloses a preparation method of magnesium metallocene, comprising the following steps:
s1, under the inert atmosphere, introducing cyclopentadiene vapor generated by the first generator into a reaction chamber along with carrier gas, reacting with magnesium in the reaction chamber, and generating a crude magnesium cyclopentadienyl product which is deposited in a first receiver;
and S2, adding the crude metallocene magnesium into a second generator for heating rectification, sublimating and gasifying, and collecting high-purity metallocene magnesium through a second receiver.
The present invention is further illustrated by the following specific examples.
Example 1:
referring to fig. 1 in combination with fig. 3 and 4, the system for preparing magnesium metallocene in this embodiment includes a synthesis device 10 and a purification device 20, where the synthesis device 10 is used to synthesize cyclopentadiene and magnesium to obtain crude magnesium metallocene, and the purification device 20 is used to purify the crude magnesium metallocene to obtain high-purity magnesium metallocene.
Referring to fig. 3, the synthesis apparatus 10 includes a first generator 11, a first receiver 12 and a reaction chamber 13, the first generator 11 is provided with a fractionating column 14, the reaction chamber 13 is connected to the first receiver 12 and the fractionating column 14, respectively, and a plurality of synthesis columns (not numbered) are vertically arranged in the reaction chamber 13.
The first generator 11 has a first inlet 111 at the top for introducing cyclopentadiene, and the reaction chamber 13 has a second inlet 131 for introducing magnesium (such as magnesium chips).
The fractionating column 14 in this example is a spur column which is connected to the reaction chamber through a F46 tube.
The reaction chamber is internally provided with a plurality of horizontally distributed baffles, the baffles are provided with a plurality of clearance grooves, the size of each clearance groove is 1-2 mm, and the clearance grooves are used for blocking large-particle magnesium chips and small-particle magnesium chips.
Further, a first temperature sensor (not shown) and a second temperature sensor (not shown) are respectively inserted outside the first generator 11 and the reaction chamber 13 through sleeves; the reaction chamber is externally provided with a first heating device, the outer layer of the reaction chamber is wrapped with an electric heating wire in the embodiment so as to provide the temperature required by the reaction, and the electric heating wire and the temperature sensor are separated by an insulating material.
In addition, the first receiver 12 is connected with a buffer bottle 15 in the embodiment, so that the reacted product is prevented from being carried out by the carrier gas to block the air outlet; a first tail gas cylinder (not shown) is connected to the buffer cylinder 15 for absorbing tail gas and observing gas flow rate.
When the synthesis device is applied to synthesis of magnesium metallocene, magnesium chips are added from the second feeding port in advance, air in the whole device is removed by carrier gas, the reaction chamber is heated to a specified temperature by the electric heating wire, cyclopentadiene vapor generated by the first generator enters the reaction chamber along with the carrier gas through the F46 tube, the cyclopentadiene vapor reacts with magnesium in the reaction chamber, and the generated magnesium metallocene flows down along with the carrier gas through the baffle plate to become solid which is deposited in the first receiver, so that the full isolation of the magnesium metallocene and the raw material magnesium is realized. The magnesium on the baffle reacts with the cyclopentadiene, so that the conversion rate of the reaction is improved, and the cost is saved.
Referring to fig. 4, the purifying device 20 includes a second generator 21, a second receiver 22, a sublimation pipe 23 and a gasification pipe 24, the sublimation pipe 23 is connected to the second generator 21, the sublimation pipe 23 is vertically distributed, and the gasification pipe 24 is connected to the second receiver 22 and the sublimation pipe 23 respectively.
The second generator 21 in this embodiment may be a front cut bottle or a middle cut bottle depending on the distillation process. The second receiver 22 is connected with a bubble counter 25 for observing the discharging condition, and the bubble counter 25 is connected with a second tail gas cylinder (not shown) for absorbing tail gas.
Further, a third temperature sensor and a fourth temperature sensor are respectively inserted outside the second generator 21 and the sublimation pipe 23 through sleeves. The sublimation pipe outside is equipped with second heating device, and the outer parcel of sublimation pipe has electric heating wire in this embodiment to provide the temperature that the sublimation edulcoration of second mao magnesium needs.
In addition, the mouth of the second receiver 22 is provided with a fourth heating device (not shown), and the mouth of the second receiver 22 is wrapped with a heating wire to prevent the mouth from being blocked as in the present embodiment.
When the purifying device is applied to purifying the magnesium bis-cyclopentadienyl, the sublimation pipe is heated to the specified temperature, the magnesium bis-cyclopentadienyl crude product is added into the second generator, and the magnesium bis-cyclopentadienyl is purified by heating and rectifying. In this way, it is possible to obtain, in the second receiver, magnesium dialkoxides of high purity, the purity of which meets the requirements of use in the semiconductor industry.
Example 2:
the preparation method of the magnesium metallocene in the embodiment adopts the preparation system in the embodiment 1 to prepare the magnesium metallocene, and specifically comprises the following steps:
s1, under inert atmosphere, introducing the cyclopentadiene vapor generated by the first generator into the reaction chamber along with the carrier gas, reacting with magnesium in the reaction chamber, and generating crude metallocene magnesium which is deposited in the first receiver.
700g of cyclopentadiene was added to the first generator, 110g of magnesium chips was added to the reaction chamber, the synthesizer was connected to an argon line, and the gas in the first generator was replaced by opening a vent cock on the first generator side and venting at a venting rate of 5L/min for 20 minutes. The first generator side vent cock was closed while the valve behind the buffer bottle was opened to replace the atmosphere in the reaction chamber and the first receiver and vented for 20 minutes.
And adjusting the flow of argon, observing the bubble number of the tail gas cylinder by eye at about 1/s, adjusting the pressure of the synthesis column in the reaction chamber, heating, and recording the voltage and the column temperature.
When the temperature of the synthesis column reaches 500 ℃, cyclopentadiene in the first generator is heated and stirred, and the reaction is started, the column temperature rises, the heating of the synthesis column needs to be reduced, and the column temperature is controlled between 510 ℃ and 540 ℃.
When the temperature of the first generator rises to 180 ℃, stopping heating the first generator, removing the heat preservation, adjusting the flow of argon to enable the bubble counter to bubble continuously, and stopping heating the synthesis column when the temperature of the first generator drops to 100 ℃.
The first receiver was removed and stoppered while argon was cut off and the reaction chamber was sealed with a stoppered vial. The first receiver weighed 600g of crude magnesium metallocene.
And S2, adding the crude metallocene magnesium into a second generator for heating rectification, sublimating and gasifying, and collecting high-purity metallocene magnesium through a second receiver.
The second generator of the rectification of the magnesium chloride is a 3L two-mouth glass flask which is used as a reaction kettle, 1800g of crude magnesium chloride is added into the reaction kettle, and 2 stainless steel fillers are added into the reaction kettle to be used as zeolite;
during heating and rectifying, the heating voltage of the sublimation pipe is adjusted to be 40V, the heating voltage of the gasification pipe is adjusted to be 78V, the column temperature rises to 170 ℃, and the column heating voltage is adjusted to be 25V; the column temperature is not lower than 175 ℃ when the discharging is stable; the temperature of the gasification pipe rises to about 220 ℃, the heating voltage of the gasification pipe is adjusted to be 48V, and the temperature of the gasification pipe is controlled to be about 230 ℃; opening the kettle and heating to obtain a voltage of 150V initially; when the temperature of the kettle rises to 190 ℃, reducing the heating voltage of the kettle to 105V; when the temperature of the kettle is raised to about 210 ℃, the column temperature and the top temperature can be slowly raised; the heating voltage of the kettle is adjusted, and the top temperature range is controlled to be about 170 ℃.
The front cut was received for about 4 hours and the kettle was turned off. When the temperature of the kettle is reduced to 190 ℃, the heating voltage of the gasification tube is closed, the front fraction bottle is detached, and 150g of magnesium metallocene front fraction can be obtained by weighing.
And (4) after the middle distillate bottle is weighed, replacing the middle distillate bottle, and connecting a tail connecting pipe. And heating the sublimation pipe and the gasification pipe again. Controlling the kettle voltage to be about 110V and the top temperature to be about 185 ℃; when the material is discharged stably, the temperature of the kettle is maintained at a basically stable temperature of about 213 ℃, and when the temperature of the kettle gradually rises to 217 ℃, the kettle is closed for heating; when the temperature of the kettle is reduced to 190 ℃, the heating voltage of the rectifying column and the gasification tube is closed.
The middle distillate bottle was removed and weighed to yield 1350g of highly pure magnesium metallocene at a yield of about 75%.
Example 3:
the preparation method of the magnesium metallocene in the embodiment adopts the preparation system in the embodiment 1 to prepare the magnesium metallocene, and specifically comprises the following steps:
s1, under inert atmosphere, introducing the cyclopentadiene vapor generated by the first generator into the reaction chamber along with the carrier gas, reacting with magnesium in the reaction chamber, and generating crude metallocene magnesium which is deposited in the first receiver.
Introducing inert gas into the synthesis device to enable the synthesis device to be in an inert atmosphere;
500 parts by mass of cyclopentadiene and 90 parts by mass of magnesium are respectively added into a first generator and a reaction chamber;
heating the first generator, and introducing cyclopentadiene vapor generated at 100 ℃ into the reaction chamber along with the carrier gas;
heating the synthesis column in the reaction chamber, reacting cyclopentadiene vapor with magnesium at 510 ℃ to generate crude cyclopentadienyl magnesium, and settling the crude cyclopentadienyl magnesium in a first receiver.
S2, adding the crude metallocene magnesium into a second generator for heating and rectification, sublimating and gasifying, and collecting high-purity metallocene magnesium through a second receiver.
Heating the sublimation pipe to 170 ℃ and the gasification pipe to 2200 ℃;
adding the crude product of magnesium cyclopentadienyl into a front fraction bottle, heating the front fraction bottle, carrying out heating rectification at the temperature of 190 ℃, sublimating and gasifying, and collecting front fraction;
replacing the front fraction bottle with a middle fraction bottle;
heating the sublimation pipe to 170 ℃ and the gasification pipe to 220 ℃;
adding the front fraction into a middle distillate bottle, heating the middle distillate bottle, carrying out heating rectification at 190 ℃, sublimating, gasifying, and collecting high-purity magnesium metallocene.
Example 4:
the preparation method of the magnesium metallocene in the embodiment adopts the preparation system in the embodiment 1 to prepare the magnesium metallocene, and specifically comprises the following steps:
s1, under inert atmosphere, introducing the cyclopentadiene vapor generated by the first generator into the reaction chamber along with the carrier gas, reacting with magnesium in the reaction chamber, and generating crude metallocene magnesium which is deposited in the first receiver.
Introducing inert gas into the synthesis device to enable the synthesis device to be in an inert atmosphere;
adding 900 parts by mass of cyclopentadiene and 130 parts by mass of magnesium into a first generator and a reaction chamber respectively;
heating the first generator, and introducing cyclopentadiene vapor generated at 180 ℃ into the reaction chamber along with the carrier gas;
heating the synthesis column in the reaction chamber, reacting cyclopentadiene vapor with magnesium at 540 ℃, and generating crude magnesium dicocene and settling in a first receiver.
And S2, adding the crude metallocene magnesium into a second generator for heating rectification, sublimating and gasifying, and collecting high-purity metallocene magnesium through a second receiver.
Heating the sublimation pipe to 180 ℃, and heating the gasification pipe to 240 ℃;
adding the crude metallocene magnesium into a front fraction bottle, heating the front fraction bottle, carrying out heating rectification at the temperature of 220 ℃, and collecting front fraction after sublimation and gasification;
replacing the front fraction bottle with the middle fraction bottle;
heating the sublimation pipe to 180 ℃, and heating the gasification pipe to 240 ℃;
adding the front fraction into a middle distillate bottle, heating the middle distillate bottle, carrying out heating rectification at the temperature of 220 ℃, sublimating, gasifying, and collecting high-purity magnesium metallocene.
According to the technical scheme, the invention has the following advantages:
the invention can synthesize and purify the high-purity magnesium metallocene directly under normal pressure, can meet the use requirements of the semiconductor industry, has simple structure of a preparation system, lower cost of the preparation method and simple operation, and is suitable for mass production.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. The preparation system of the magnesium cyclopentadienyl is characterized by comprising a synthesis device and a purification device, wherein the synthesis device is used for synthesizing cyclopentadiene and magnesium to obtain a magnesium cyclopentadienyl crude product, and the purification device is used for purifying the magnesium cyclopentadienyl crude product to obtain high-purity magnesium cyclopentadienyl, wherein:
the synthesis device comprises a first generator, a first receiver and a reaction chamber, wherein the first generator is provided with a fractionating column, the reaction chamber is respectively connected with the first receiver and the fractionating column, and the reaction chamber is internally provided with a plurality of synthesis columns which are vertically distributed;
the purification device comprises a second generator, a second receiver, a sublimation pipe and a gasification pipe, wherein the sublimation pipe is connected with the second generator and is vertically distributed, and the gasification pipe is respectively connected with the second receiver and the sublimation pipe.
2. The system for preparing the magnesium chloride according to claim 1, wherein the first generator is provided with a first feeding port, and the reaction chamber is provided with a second feeding port; and/or the presence of a gas in the gas,
the fractionating column is a thorn-shaped fractionating column; and/or the presence of a gas in the gas,
the first receiver is connected with a buffer bottle, and the buffer bottle is connected with a first tail gas bottle.
3. The system for preparing magnesium dicocene according to claim 1, wherein a first heating device is arranged outside the reaction chamber; and/or the presence of a gas in the atmosphere,
the reactor is characterized in that a plurality of horizontally distributed baffles are arranged inside the reactor, a plurality of clearance grooves are formed in the baffles, and the size of each clearance groove is 1-2 mm.
4. The system for preparing magnesium chloride according to claim 1, wherein a first temperature sensor and a second temperature sensor are respectively inserted outside the first generator and the reaction chamber through sleeves.
5. The system of claim 1, wherein the second generator is a forecut or middle cut vial; and/or the presence of a gas in the gas,
and the second receiver is connected with a bubble counter, and the bubble counter is connected with a second tail gas cylinder.
6. The system for preparing magnesium chloride according to claim 1, wherein a third temperature sensor and a fourth temperature sensor are respectively inserted outside the second generator and the sublimation pipe through sleeves.
7. The system for preparing the magnesium chloride according to claim 1, wherein a second heating device is arranged outside the sublimation pipe; and/or the presence of a gas in the gas,
a third heating device is arranged outside the gasification pipe; and/or the presence of a gas in the gas,
and a bottle opening of the second receiver is provided with a fourth heating device.
8. A preparation method of magnesium metallocene is characterized by comprising the following steps:
s1, under the inert atmosphere, introducing cyclopentadiene vapor generated by the first generator into a reaction chamber along with carrier gas, reacting with magnesium in the reaction chamber, and generating a crude product of magnesium diclocide which is deposited in a first receiver;
and S2, adding the crude metallocene magnesium into a second generator for heating rectification, sublimating and gasifying, and collecting high-purity metallocene magnesium through a second receiver.
9. The method for preparing a magnesium metallocene according to claim 8, wherein the step S1 specifically comprises:
introducing inert gas into the synthesis device to enable the synthesis device to be in an inert atmosphere;
respectively adding 500-900 parts by mass of cyclopentadiene and 90-130 parts by mass of magnesium into a first generator and a reaction chamber;
heating the first generator, and introducing cyclopentadiene vapor generated at the temperature of 100-180 ℃ into a reaction chamber along with carrier gas;
heating a synthesis column in a reaction chamber, reacting cyclopentadiene steam with magnesium at 510-540 ℃, and generating a crude product of magnesium dicocene and settling the crude product in a first receiver.
10. The method for preparing a magnesium metallocene according to claim 8, wherein the step S2 specifically comprises:
heating the sublimation pipe to 170-180 ℃, and heating the gasification pipe to 220-240 ℃;
adding the crude magnesium dicocene into a front fraction bottle, heating the front fraction bottle, carrying out heating rectification at the temperature of 190-220 ℃, sublimating and gasifying, and collecting front fraction;
replacing the front fraction bottle with the middle fraction bottle;
heating the sublimation pipe to 170-180 ℃, and heating the gasification pipe to 220-240 ℃;
adding the front fraction into a middle fraction bottle, heating the middle fraction bottle, carrying out heating rectification at the temperature of 190-220 ℃, sublimating, gasifying, and collecting high-purity magnesium metallocene.
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| WO2024107320A1 (en) * | 2022-11-15 | 2024-05-23 | Entegris, Inc. | Fractional distillation system and method |
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