CN207933044U - The preparation facilities of three aluminum hydrides - Google Patents
The preparation facilities of three aluminum hydrides Download PDFInfo
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- CN207933044U CN207933044U CN201820213368.XU CN201820213368U CN207933044U CN 207933044 U CN207933044 U CN 207933044U CN 201820213368 U CN201820213368 U CN 201820213368U CN 207933044 U CN207933044 U CN 207933044U
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Abstract
The utility model discloses a kind of preparation facilities of three aluminum hydrides, belong to inorganic material and prepare and energetic material technology crossing domain.It includes toluene purification devices, ether purification devices, first ether measuring tank, alchlor prepares kettle, pre-reactor, pre-reaction pans, reaction kettle, second ether measuring tank and the first toluene measuring tank, wherein ether purification devices, first ether measuring tank, alchlor prepares kettle, pre-reactor, pre-reaction pans, reaction kettle is sequentially connected with by the road, ether purification devices are also connected with one end of the second ether measuring tank by the road, the other end of second ether measuring tank is connected with pre-reactor by the road, toluene purification devices are connected with one end of the first toluene measuring tank by the road, the other end of first toluene measuring tank is connected with pre-reactor by the road.The utility model is additionally provided with solvent purification apparatus, and reaction condition is mildly easily controllable, moreover it is possible to meet the needs of large-scale production.
Description
Technical field
The utility model is related to a kind of preparation facilities of three aluminum hydrides, belong to inorganic material and prepare and the friendship of energetic material technology
Fork field.
Background technology
Three aluminum hydrides are covalent compounds, and synthetic method has very much, is broadly divided into chemical reaction method and direct method two
Kind：Chemical reaction method is presently the most traditional preparation method, but since three aluminum hydrides are to oxygen and water sensitive, very unstable
Fixed, preparation process is related to a large amount of reaction raw materials and organic solvent, this so that product separating-purifying is difficult, anti-using chemistry at present
Method is answered to be difficult to realize the industrial-scale production of three aluminum hydrides, it is to ensure that its dispersion is steady to reduce the water content in organic solvent
Fixed premise necessary condition.The report that direct method prepares three aluminum hydrides is also very much, but there is also various insufficient and
It is difficult to by industrial applications.Such as：Electrochemical process is reacted in electrolyte solution with ionic hydrogen, environmental protection and energy saving, but secondary
Product is more, low yield and is difficult to purify, and is not suitable for large-scale production；Three aluminum hydride purity prepared by high temperature and high pressure method it is high and
Stablize, but reaction condition is extremely harsh, to equipment requirement height, reaction difficulty is big, dangerous high, safe scale industrial production
There is many difficulties for preparation.How three aluminum hydrides are prepared to safety and scale, needs a kind of new Research Thinking and preparation
Device.
Utility model content
The purpose of the utility model is to provide a kind of preparation facilities of three aluminum hydrides, in addition to preparing the anti-of three aluminum hydrides
Answer device to be additionally provided with the purifier of organic solvent so that flow it is terse it is pollution-free, reaction condition is mildly easily controllable, moreover it is possible to it is full
The demand of sufficient large-scale production, product quality is high, product purity 98%, and yield reaches 90% or more.
In order to solve the above technical problems, the utility model adopts the following technical scheme：
The preparation facilities of three aluminum hydrides includes toluene purification devices, ether purification devices, the first ether measuring tank, tri-chlorination
Aluminium prepares kettle, pre-reactor, pre-reaction pans, reaction kettle, the second ether measuring tank and the first toluene measuring tank, wherein described
Ether purification devices, the first ether measuring tank, alchlor prepare kettle, pre-reactor, pre-reaction pans, reaction kettle by the road
It is sequentially connected with, the ether purification devices are also connected with one end of the second ether measuring tank, the second ether metering by the road
The other end of tank is connected with pre-reactor by the road, and the toluene purification devices are connected with the one of the first toluene measuring tank by the road
The other end at end, the first toluene measuring tank is connected with pre-reactor by the road, and the alchlor prepares kettle, pre-reactor
Material inlet is offered with the top of reaction kettle.Wherein toluene purification devices to toluene be dehydrated refined, ether purifying dress
It sets and carries out the quality that dehydration is refined, prepared by raising product to industrial ether.Wherein the first ether measuring tank and the metering of the second ether
Tank can rationally control the injected volume of refined ether.First toluene measuring tank can rationally control the injected volume of toluene.
The preparation facilities of three aluminum hydride above-mentioned, the connecting tube between the toluene purification devices and the first toluene measuring tank
Road is toluene delivery main road, and the toluene purification devices include toluene seepage slope device connected in sequence, toluene by the road
Primary Receive tank, toluene decontaminating column and toluene Secondary Receive tank, the toluene Secondary Receive tank also connect through toluene delivery main road
It is connected to the first toluene measuring tank.The utility model further includes toluene level-one sampling line and toluene two level sampling line, the first
Branch line, i.e. toluene level-one sampling line are additionally provided on connecting line between benzene Primary Receive tank and toluene decontaminating column；Institute
It states and also is provided with branch line on the connecting line between toluene Secondary Receive tank and the first toluene measuring tank, i.e., toluene two level samples
Pipeline makes the utility model have on-line period function, ensures toluene refining effect.
The preparation facilities of three aluminum hydride above-mentioned further includes the second toluene measuring tank and the first toluene conveying branches pipeline, institute
It states toluene delivery main road and offers branch line i.e. the first toluene conveying branches pipeline, the first toluene conveying branches pipe
The end on road is connected with the second toluene measuring tank, and the second toluene measuring tank is also connected with reaction kettle by the road.
The preparation facilities of three aluminum hydride above-mentioned, the connecting tube between the ether purification devices and the first ether measuring tank
Road is ether delivery main road, and the ether purification devices include ether seepage slope device connected in sequence, ether by the road
Primary Receive tank, ether decontaminating column and ether Secondary Receive tank, the ether Secondary Receive tank also connect through ether delivery main road
It is connected to the first ether measuring tank.The utility model further includes ether level-one sampling line and ether two level sampling line, the second
Branch line, i.e. ether level-one sampling line are additionally provided on connecting line between ether Primary Receive tank and ether decontaminating column；Institute
It states and also is provided with branch line on the connecting line between ether Secondary Receive tank and the first ether measuring tank, i.e., ether two level samples
Pipeline makes the utility model have on-line period function, ensures industrial ether refining effect.
The preparation facilities of three aluminum hydride above-mentioned further includes that third ether measuring tank, catalyst preparation kettle and the second ether are defeated
Send branch line, the ether delivery main road offers branch line i.e. the second ether conveying branches pipeline, and described second
The end of ether conveying branches pipeline is connected with third ether measuring tank, and the third ether measuring tank is also connected with by the road urges
Agent prepares kettle, and the catalyst preparation kettle is also connected with reaction kettle by the road, and the top of the catalyst preparation kettle also opens up
There is material inlet.Three aluminum hydrides of high-purity can be obtained by the configuration of catalyst.
The preparation facilities of three aluminum hydride above-mentioned further includes the first ether conveying branches pipeline, ether delivery main road
On offer branch line i.e. the first ether conveying branches pipeline, the end of the first ether conveying branches pipeline is connected with
Diethyl ether measuring tank.
The preparation facilities of three aluminum hydride above-mentioned further includes delivery pump, the toluene Primary Receive tank and toluene decontaminating column it
Between connecting line on delivery pump is installed, on the connecting line between the toluene Secondary Receive tank and the first toluene measuring tank
Delivery pump is also installed.Delivery pump is as actuating unit so that the toluene that need to be purified is pumped into toluene from toluene seepage slope device
Then decontaminating column is transported to each measuring tank under the action of delivery pump, improves treatment effeciency.
The preparation facilities of three aluminum hydride above-mentioned further includes delivery pump, the ether Primary Receive tank and ether decontaminating column it
Between connecting line on delivery pump is installed, on the connecting line between the ether Secondary Receive tank and the first ether measuring tank
Delivery pump is also installed.Delivery pump is as actuating unit so that the industrial ether that need to be purified is pumped into from ether seepage slope device
Then ether decontaminating column is transported to each measuring tank under the action of delivery pump, improves treatment effeciency, further increase purification effect
Fruit.
The preparation facilities of three aluminum hydride above-mentioned further includes first filter, and one end of the first filter connects by the road
It is connected to pre-reactor, the other end of the first filter is connected with pre-reaction pans by the road.The setting of first filter
The purity of product can be improved.
The preparation facilities of three aluminum hydride above-mentioned further includes the second filter, and one end of second filter connects by the road
It is connected to catalyst preparation kettle, the other end of second filter is connected with reaction kettle by the road.Further, the tri-chlorination
The inside that aluminium prepares kettle, pre-reactor, reaction kettle and catalyst preparation kettle is mounted on agitating device.Pass through the second filter
The purity for further increasing product is set.By the stirring of agitating device, reaction speed is further increased, shortens the reaction time.
Compared with prior art, the utility model is beneficial in that：
(1) in addition to the reaction unit of three aluminum hydrides of preparation, it is additionally provided with the purifier of organic solvent, it can be to participating in preparing
The toluene of process and industrial ether are refined so that flow is terse pollution-free, improves the preparation quality of product；
(2) use delivery pump as actuating unit so that the organic solvent that need to be purified is pumped into purification from seepage slope device
Column, treatment effeciency higher, clean-up effect are more preferable；
(3) it is provided with sampling line, makes the online sampled functions of the utility model set, monitors the purification of organic solvent in real time
Effect；
(4) reaction condition is mildly easily controllable, moreover it is possible to meet the needs of large-scale production, product quality is high, product purity
It is 98%, and yield reaches 90% or more；
(5) the utility model is also provided with catalyst preparation kettle, larger using crystal particle diameter obtained by this synthesizer, can
Meets the needs of big grain size product.
Description of the drawings
Fig. 1 is the connection relationship diagram of the utility model.
The meaning of reference numeral：1- toluene purification devices, 2- ether purification devices, 3- the first ether measuring tanks, 4- trichlorines
Change aluminium and prepares kettle, 5- pre-reactors, 6- pre-reaction pans, 7- reaction kettles, 8- the second ether measuring tanks, the metering of 9- third ether
Tank, 10- the first toluene measuring tanks, 11- the second toluene measuring tanks, 12- first filters, the second filters of 13-, 14- catalyst
Prepare kettle, 15- toluene delivery mains road, 16- the first toluene conveying branches pipelines, 17- ether delivery mains road, the first second of 18-
Ether conveying branches pipeline, 19- the second ether conveying branches pipelines, 20- toluene seepage slope devices, 21- toluene Primary Receive tanks,
22- toluene decontaminating columns, 23- toluene Secondary Receive tanks, 24- ether seepage slope devices, 25- ether Primary Receive tanks, 26- ether
Decontaminating column, 27- ether Secondary Receive tanks, 28- delivery pumps, 29- toluene level-one sampling lines, 30- toluene two level sampling lines,
31- ether level-one sampling lines, 32- ether two level sampling lines.
The utility model is further described with reference to the accompanying drawings and detailed description.
Specific implementation mode
The embodiments of the present invention 1：As shown in Figure 1, the preparation facilities of three aluminum hydrides includes toluene purification devices 1, second
Ether purification devices 2, the first ether measuring tank 3, alchlor prepare kettle 4, pre-reactor 5, pre-reaction pans 6, reaction kettle 7,
Second ether measuring tank 8 and the first toluene measuring tank 10, wherein the ether purification devices 2, the first ether measuring tank 3, trichlorine
Change aluminium preparation kettle 4, pre-reactor 5, pre-reaction pans 6, reaction kettle 7 to be sequentially connected with by the road, the ether purification devices 2 are also
It is connected with one end of the second ether measuring tank 8 by the road, the other end of the second ether measuring tank 8 is connected with pre- anti-by the road
Kettle 5, the toluene purification devices 1 is answered to be connected with one end of the first toluene measuring tank 10, the first toluene measuring tank by the road
10 other end is connected with pre-reactor 5 by the road, and the alchlor prepares the top of kettle 4, pre-reactor 5 and reaction kettle 7
Offer material inlet.Wherein toluene purification devices 1 to toluene be dehydrated refined, and ether purification devices 2 are to industrial ether
Carry out the quality that dehydration is refined, prepared by raising product.Wherein the first ether measuring tank 3 and the second ether measuring tank 8 can be reasonable
Control refines the injected volume of ether.First toluene measuring tank 10 can rationally control the injected volume of toluene.The toluene purifying dress
Set 1 and the first connecting line between toluene measuring tank 10 be toluene delivery main road 15, the toluene purification devices 1 include warp
Pipeline toluene seepage slope device 20 connected in sequence, toluene Primary Receive tank 21, toluene decontaminating column 22 and toluene Secondary Receive
Tank 23, the toluene Secondary Receive tank 23 are also connected with the first toluene measuring tank 10 through toluene delivery main road 15.This practicality is new
Type further includes toluene level-one sampling line 29 and toluene two level sampling line 30, and the toluene Primary Receive tank 21 is purified with toluene
Branch line, i.e. toluene level-one sampling line 29 are additionally provided on connecting line between column 22；The toluene Secondary Receive tank 23
It also is provided with branch line, i.e. toluene two level sampling line 30 on connecting line between the first toluene measuring tank 10, makes this reality
Have on-line period function with novel, ensures toluene refining effect.The preparation facilities of three aluminum hydrides further includes the metering of the second toluene
It is defeated to offer branch line i.e. the first toluene on toluene delivery main road 15 for tank 11 and the first toluene conveying branches pipeline 16
Send branch line 16, the end of the first toluene conveying branches pipeline 16 is connected with the second toluene measuring tank 11, and described second
Toluene measuring tank 11 is also connected with reaction kettle 7 by the road.
Embodiment 2：As shown in Figure 1, the preparation facilities of three aluminum hydrides include toluene purification devices 1, ether purification devices 2,
First ether measuring tank 3, alchlor prepare kettle 4, pre-reactor 5, pre-reaction pans 6, reaction kettle 7, the metering of the second ether
Tank 8 and the first toluene measuring tank 10, wherein the ether purification devices 2, the first ether measuring tank 3, alchlor preparation kettle 4,
Pre-reactor 5, pre-reaction pans 6, reaction kettle 7 are sequentially connected with by the road, and the ether purification devices 2 are also connected with by the road
The other end of one end of the second ether measuring tank 8, the second ether measuring tank 8 is connected with pre-reactor 5, the first by the road
Benzene purification devices 1 are connected with one end of the first toluene measuring tank 10, the other end warp of the first toluene measuring tank 10 by the road
Piping connection has pre-reactor 5, the top that the alchlor prepares kettle 4, pre-reactor 5 and reaction kettle 7 to offer material
Import.Wherein toluene purification devices 1 to toluene be dehydrated refined, and ether purification devices 2 carry out dehydration to industrial ether and refine,
Improve quality prepared by product.Wherein the first ether measuring tank 3 and the second ether measuring tank 8 can rationally control refined ether
Injected volume.First toluene measuring tank 10 can rationally control the injected volume of toluene.2 and first ether meter of the ether purification devices
Connecting line between measuring tank 3 is ether delivery main road 17, and the ether purification devices 2 include second connected in sequence by the road
Ether seepage slope device 24, ether Primary Receive tank 25, ether decontaminating column 26 and ether Secondary Receive tank 27, the ether two level
Receiving tank 27 is also connected with the first ether measuring tank 3 through ether delivery main road 17.The utility model further includes that ether level-one takes
Sample pipeline 31 and ether two level sampling line 32, the connecting line between the ether Primary Receive tank 25 and ether decontaminating column 26
On be additionally provided with branch line, i.e. ether level-one sampling line 31；The ether Secondary Receive tank 27 and the first ether measuring tank 3 it
Between connecting line on also be provided with branch line, i.e. ether two level sampling line 32, so that the utility model is had on-line period work(
Can, ensure industrial ether refining effect.The preparation facilities of three aluminum hydrides further includes the first ether conveying branches pipeline 18, the second
Branch line i.e. the first ether conveying branches pipeline 18, the first ether conveying branches pipe are offered on ether delivery main road 17
The end on road 18 is connected with the second ether measuring tank 8.Further, the preparation facilities of three aluminum hydrides further includes delivery pump 28, institute
It states and delivery pump 28 is installed on the connecting line between ether Primary Receive tank 25 and ether decontaminating column 26, the ether two level connects
Delivery pump 28 is also installed on connecting line between closed cans 27 and the first ether measuring tank 3.Delivery pump 28 is used as actuating unit,
So that the industrial ether that need to be purified is pumped into ether decontaminating column 26 from ether seepage slope device 24, then in the effect of delivery pump 28
Under be transported to each measuring tank, improve treatment effeciency, further increase clean-up effect.
Embodiment 3：As shown in Figure 1, the preparation facilities of three aluminum hydrides include toluene purification devices 1, ether purification devices 2,
First ether measuring tank 3, alchlor prepare kettle 4, pre-reactor 5, pre-reaction pans 6, reaction kettle 7, the metering of the second ether
Tank 8 and the first toluene measuring tank 10, wherein the ether purification devices 2, the first ether measuring tank 3, alchlor preparation kettle 4,
Pre-reactor 5, pre-reaction pans 6, reaction kettle 7 are sequentially connected with by the road, and the ether purification devices 2 are also connected with by the road
The other end of one end of the second ether measuring tank 8, the second ether measuring tank 8 is connected with pre-reactor 5, the first by the road
Benzene purification devices 1 are connected with one end of the first toluene measuring tank 10, the other end warp of the first toluene measuring tank 10 by the road
Piping connection has pre-reactor 5, the top that the alchlor prepares kettle 4, pre-reactor 5 and reaction kettle 7 to offer material
Import.Wherein toluene purification devices 1 to toluene be dehydrated refined, and ether purification devices 2 carry out dehydration to industrial ether and refine,
Improve quality prepared by product.Wherein the first ether measuring tank 3 and the second ether measuring tank 8 can rationally control refined ether
Injected volume.First toluene measuring tank 10 can rationally control the injected volume of toluene.The preparation facilities of three aluminum hydrides further includes first
One end of filter 12, the first filter 12 is connected with pre-reactor 5, the other end of the first filter 12 by the road
It is connected with pre-reaction pans 6 by the road.The setting of first filter 12 can improve the purity of product.Specifically, the first mistake
Filter 12 is G5 filters.
Embodiment 4：As shown in Figure 1, the preparation facilities of three aluminum hydrides include toluene purification devices 1, ether purification devices 2,
First ether measuring tank 3, alchlor prepare kettle 4, pre-reactor 5, pre-reaction pans 6, reaction kettle 7, the metering of the second ether
Tank 8 and the first toluene measuring tank 10, wherein the ether purification devices 2, the first ether measuring tank 3, alchlor preparation kettle 4,
Pre-reactor 5, pre-reaction pans 6, reaction kettle 7 are sequentially connected with by the road, and the ether purification devices 2 are also connected with by the road
The other end of one end of the second ether measuring tank 8, the second ether measuring tank 8 is connected with pre-reactor 5, the first by the road
Benzene purification devices 1 are connected with one end of the first toluene measuring tank 10, the other end warp of the first toluene measuring tank 10 by the road
Piping connection has pre-reactor 5, the top that the alchlor prepares kettle 4, pre-reactor 5 and reaction kettle 7 to offer material
Import.Wherein toluene purification devices 1 to toluene be dehydrated refined, and ether purification devices 2 carry out dehydration to industrial ether and refine,
Improve quality prepared by product.Wherein the first ether measuring tank 3 and the second ether measuring tank 8 can rationally control refined ether
Injected volume.First toluene measuring tank 10 can rationally control the injected volume of toluene.2 and first ether meter of the ether purification devices
Connecting line between measuring tank 3 is ether delivery main road 17, and the ether purification devices 2 include second connected in sequence by the road
Ether seepage slope device 24, ether Primary Receive tank 25, ether decontaminating column 26 and ether Secondary Receive tank 27, the ether two level
Receiving tank 27 is also connected with the first ether measuring tank 3 through ether delivery main road 17.The utility model further includes that ether level-one takes
Sample pipeline 31 and ether two level sampling line 32, the connecting line between the ether Primary Receive tank 25 and ether decontaminating column 26
On be additionally provided with branch line, i.e. ether level-one sampling line 31；The ether Secondary Receive tank 27 and the first ether measuring tank 3 it
Between connecting line on also be provided with branch line, i.e. ether two level sampling line 32, so that the utility model is had on-line period work(
Can, ensure industrial ether refining effect.
Further, the preparation facilities of three aluminum hydrides further includes third ether measuring tank 9, catalyst preparation kettle 14 and second
Ether conveying branches pipeline 19 offers branch line i.e. the second ether conveying branches pipeline on ether delivery main road 17
19, the end of the second ether conveying branches pipeline 19 is connected with third ether measuring tank 9, the third ether measuring tank 9
It is also connected with catalyst preparation kettle 14 by the road, the catalyst preparation kettle 14 is also connected with reaction kettle 7, the catalysis by the road
The top that kettle 14 is prepared in agent also offers material inlet.Three aluminum hydrides of high-purity can be obtained by the configuration of catalyst.Three
The preparation facilities of aluminum hydride further includes the second filter 13, and one end of second filter 13 is connected with catalyst and matches by the road
The other end of kettle 14 processed, second filter 13 is connected with reaction kettle 7 by the road.Further, the alchlor is prepared
Kettle 4, pre-reactor 5, reaction kettle 7 and catalyst preparation kettle 14 inside be mounted on agitating device.Pass through the second filter 13
Setting further increase the purity of product.Specifically, the second filter 13 is G5 filters.
A kind of course of work of the utility model：Three aluminum hydrides are prepared by the preparation facilities of three aluminum hydrides, may include
Following steps：(1) toluene is refined；(2) anhydrous ether is refined；(3) anhydrous AlCl3With the preparation of ether mixed solution；(4)
LiAlH4With anhydrous AlCl3The preparation of mixed solution；(5) preparation of catalyst；The preparation of (6) three aluminum hydrides.
Specific steps are as follows：
(1) toluene is refined；
It is passed through inert gas in advance from the import of toluene seepage slope device 20, removes the oxygen in purification devices, then
It takes the organic solvent (toluene) that needs purify to inject in toluene seepage slope device 20 to purify, toluene is under the action of delivery pump 28
It is purified followed by toluene Primary Receive tank 21, toluene decontaminating column 22 and toluene Secondary Receive tank 23, passes through toluene during purification
30 sample detection clean-up effect of level-one sampling line 29 and toluene two level sampling line, the toluene after refining are respectively put into the first first
It is spare in benzene measuring tank 10 and the second toluene measuring tank 11；
(2) anhydrous ether is refined
It is passed through inert gas in advance from the import of ether seepage slope device 24, removes the oxygen in purification devices, then
It takes the organic solvent (industrial ether) that needs purify to inject in ether seepage slope device 24 to purify, industrial ether is in delivery pump 28
Under the action of followed by ether Primary Receive tank 25, ether decontaminating column 26 and ether Secondary Receive tank 27 purify, during purification
By the sample detection clean-up effect of ether level-one sampling line 31 and ether two level sampling line 32, the anhydrous ether after refining
It is respectively put into spare in the first ether measuring tank 3, the second ether measuring tank 8 and third ether measuring tank 9；
(3) anhydrous AlCl3With the preparation of ether mixed solution；
Take anhydrous AlCl3It prepares in kettle 4 through material inlet input alchlor, is slowly dripped by the first ether measuring tank 3
Add refined anhydrous ether, the agitating device in kettle 4 is prepared by alchlor after being added dropwise and is stirred to AlCl3It is completely dissolved；
(4)LiAlH4With anhydrous AlCl3The preparation of mixed solution；
By the second ether measuring tank 8 discharge refine anhydrous ether enter in pre-reactor 5, while by material inlet to
It is put into pre-reactor 5 and refines lithium aluminium hydride reduction, after stirring a period of time by the agitating device inside pre-reactor 5, side stirring
While alchlor, which is slowly added dropwise, prepares the anhydrous AlCl of gained in kettle 43With ether mixed solution, continue one section of stirring after being added dropwise
Then refined toluene, stirring a period of time, precipitation, LiAlH is added by the first toluene measuring tank 10 in time4With anhydrous AlCl3
Mixed solution is filtered by first filter 12, is flowed into spare in pre-reaction pans 6；
(5) preparation of catalyst；
Anhydrous ether is discharged by third ether measuring tank 9 to enter in catalyst preparation kettle 14, weighs catalyst through material
Import is put into catalyst preparation kettle 14, is mixed to and is completely dissolved with anhydrous ether therein, spare；
The preparation of (6) three aluminum hydrides.
Refined toluene is discharged by the second toluene measuring tank 11 to be placed in reaction kettle 7, and reaction kettle 7 is vacuumized, is led to
Enter the operation of inert gas, remove the oxygen in reaction kettle 7, after repeating the operation three times, institute in catalyst preparation kettle 14 is added
Catalyst is obtained, at reflux stirring heating, temperature controls at 75 DEG C~94 DEG C, then begins to distill, and be slowly added dropwise pre-
React the LiAlH in pans 64With anhydrous AlCl3Mixed solution after being added dropwise, then carries out temperature rising reflux for a period of time, with
After continue to distill, temperature control at 94 DEG C~107 DEG C and flow back a period of time, be slowly dropped to room temperature, stratification discards supernatant
Liquid, then refined toluene is discharged by the second toluene measuring tank 11 and is washed repeatedly, until without apparent floating material, then in vacuum degree
It is that dry 3~6h obtains three aluminum hydrides at 280~470mmHg and 40~60 DEG C.
Claims (10)
1. the preparation facilities of three aluminum hydrides, which is characterized in that including toluene purification devices (1), ether purification devices (2), first
Ether measuring tank (3), alchlor prepare kettle (4), pre-reactor (5), pre-reaction pans (6), reaction kettle (7), the second second
Ether measuring tank (8) and the first toluene measuring tank (10), wherein the ether purification devices (2), the first ether measuring tank (3), three
Aluminium chloride is prepared kettle (4), pre-reactor (5), pre-reaction pans (6), reaction kettle (7) and is sequentially connected with by the road, the ether
Purification devices (2) are also connected with one end of the second ether measuring tank (8) by the road, the second ether measuring tank (8) it is another
End is connected with pre-reactor (5) by the road, and the toluene purification devices (1) are connected with the first toluene measuring tank (10) by the road
The other end of one end, the first toluene measuring tank (10) is connected with pre-reactor (5) by the road, and the alchlor prepares kettle
(4), the top of pre-reactor (5) and reaction kettle (7) offers material inlet.
2. the preparation facilities of three aluminum hydride according to claim 1, which is characterized in that the toluene purification devices (1) with
Connecting line between first toluene measuring tank (10) is toluene delivery main road (15), and the toluene purification devices (1) include
Toluene seepage slope device (20) connected in sequence, toluene Primary Receive tank (21), toluene decontaminating column (22) and toluene by the road
Secondary Receive tank (23), the toluene Secondary Receive tank (23) are also connected with the metering of the first toluene through toluene delivery main road (15)
Tank (10).
3. the preparation facilities of three aluminum hydride according to claim 2, which is characterized in that further include the second toluene measuring tank
(11) and the first toluene conveying branches pipeline (16), branch line i.e. the first first is offered on toluene delivery main road (15)
The end of benzene conveying branches pipeline (16), the first toluene conveying branches pipeline (16) is connected with the second toluene measuring tank
(11), the second toluene measuring tank (11) is also connected with reaction kettle (7) by the road.
4. the preparation facilities of three aluminum hydride according to claim 1, which is characterized in that the ether purification devices (2) with
Connecting line between first ether measuring tank (3) is ether delivery main road (17), and the ether purification devices (2) include warp
Pipeline ether seepage slope device (24) connected in sequence, ether Primary Receive tank (25), ether decontaminating column (26) and ether two
Grade receiving tank (27), the ether Secondary Receive tank (27) are also connected with the first ether measuring tank through ether delivery main road (17)
(3)。
5. the preparation facilities of three aluminum hydride according to claim 4, which is characterized in that further include third ether measuring tank
(9), catalyst preparation kettle (14) and the second ether conveying branches pipeline (19) offer on ether delivery main road (17)
The end of branch line i.e. the second ether conveying branches pipeline (19), the second ether conveying branches pipeline (19) is connected with
Three ether measuring tanks (9), the third ether measuring tank (9) are also connected with catalyst preparation kettle (14), the catalysis by the road
Agent prepares kettle (14) and is also connected with reaction kettle (7) by the road, the top of the catalyst preparation kettle (14) also offer material into
Mouthful.
6. the preparation facilities of three aluminum hydride according to claim 4, which is characterized in that further include the first ether conveying branches
Pipeline (18) offers branch line i.e. the first ether conveying branches pipeline (18), institute on ether delivery main road (17)
The end for stating the first ether conveying branches pipeline (18) is connected with the second ether measuring tank (8).
7. the preparation facilities of three aluminum hydride according to claim 2, which is characterized in that further include delivery pump (28), it is described
Delivery pump (28), the toluene two are installed on the connecting line between toluene Primary Receive tank (21) and toluene decontaminating column (22)
Delivery pump (28) is also installed on connecting line between grade receiving tank (23) and the first toluene measuring tank (10).
8. the preparation facilities of three aluminum hydride according to claim 4, which is characterized in that further include delivery pump (28), it is described
Delivery pump (28), the ether two are installed on the connecting line between ether Primary Receive tank (25) and ether decontaminating column (26)
Delivery pump (28) is also installed on connecting line between grade receiving tank (27) and the first ether measuring tank (3).
9. the preparation facilities of three aluminum hydride according to claim 1, which is characterized in that further include first filter (12),
One end of the first filter (12) is connected with pre-reactor (5), the other end warp of the first filter (12) by the road
Piping connection has pre-reaction pans (6).
10. the preparation facilities of three aluminum hydride according to claim 5, which is characterized in that further include the second filter (13),
One end of second filter (13) is connected with catalyst preparation kettle (14) by the road, second filter (13) it is another
End is connected with reaction kettle (7) by the road.
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| CN115301184A (en) * | 2022-08-01 | 2022-11-08 | 东莞市颖兴金属表面处理材料有限公司 | Full-automatic lubricant preparation and subpackaging structure and subpackaging method thereof |
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| CN115301184A (en) * | 2022-08-01 | 2022-11-08 | 东莞市颖兴金属表面处理材料有限公司 | Full-automatic lubricant preparation and subpackaging structure and subpackaging method thereof |
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