CN207861884U - Three aluminum hydride synthesis systems of recyclable ether - Google Patents
Three aluminum hydride synthesis systems of recyclable ether Download PDFInfo
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- CN207861884U CN207861884U CN201820200907.6U CN201820200907U CN207861884U CN 207861884 U CN207861884 U CN 207861884U CN 201820200907 U CN201820200907 U CN 201820200907U CN 207861884 U CN207861884 U CN 207861884U
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Abstract
The utility model is related to three aluminum hydride synthesis systems, three aluminum hydride synthesis systems of especially recyclable ether.It includes that alchlor prepares kettle, pre-reactor, pre-reaction pans, reaction kettle, first ether measuring tank, second ether measuring tank, first toluene measuring tank, second toluene measuring tank, ether retracting device, first ether measuring tank, alchlor prepares kettle, pre-reactor, pre-reaction pans, reaction kettle and ether retracting device are sequentially connected with by the road, second ether measuring tank and the first toluene measuring tank are connected to pre-reactor by the road, second toluene measuring tank is connected with reaction kettle by the road, alchlor prepares kettle, the top of pre-reactor and reaction kettle offers material inlet.The utility model is easy to operate, reaction condition is mildly easily controllable, at low cost, product quality is high, and yield reaches 90% or more, and is detached to the organic solvent after the preparation of three aluminum hydrides, and is recycled to ether solvent.
Description
Technical field
The utility model is related to three aluminum hydride synthesis systems, three aluminum hydride synthesis systems of especially recyclable ether.
Background technology
Most widely used at present is the metal Al powder for being added in explosive high heating value.It is well known that weapon infinitely chases after
The high-energy of explosive is sought, therefore uses AlH3、B、BeH2Equal anakinetomers replace aluminium powder gradually interested to researchers and research.
Due to AlH3High hydrogen content, heats of combustion, the characteristics such as nontoxic, it can be applied in high-energy fuel field.It is calculated through heat chemistry
Show to use AlH3Replace aluminium that can generate lower flame temperature and higher gas production, can provide more higher than aluminium fuel
Specific impulse.Wherein, AlH3It is combined and is formed by two kinds of strong reducing property atoms, H is generated in its combustion process2, H2It can promote oxidant
Conflagration generates Al2O3And H2O simultaneously releases a large amount of thermal energy.Therefore, three aluminum hydride (AlH3) due to the combustion heat it is high, it is good at gas,
The advantages that nontoxic, can promise to be a kind of novel explosive high energy additive.But the three aluminum hydride production scales in China are mostly
Still it is in laboratory research, small scale is far from meeting the market demand, and there are backward in technique, complex process and lifes for production status
The low feature of production capacity power.In addition, preparing for three aluminum hydrides need to be in the container for being connected with inert gas, and using ether as organic molten
Agent.After prepared by three aluminum hydrides, the ether band as secondary organic solvent is toxic, if direct emission can be to Man ＆ Nature environment
Injury is brought, and is resulted in waste of resources, finds a kind of three aluminum hydride synthesis systems disclosure satisfy that the market demand, and to three hydrogen
Change the method that ether solvent of the aluminum for after is rationally recycled has important meaning for the utilization of resource and the protection of environment
Justice.
Utility model content
The purpose of the utility model is to provide three aluminum hydride synthesis systems of recyclable ether, easy to operate, reaction item
Part is mildly easily controllable, at low cost, product quality is high, and yield reaches 90% or more, and to organic after the preparation of three aluminum hydrides
Solvent is detached, and is recycled to ether solvent, is on the one hand reduced resource waste, and nature ring is on the one hand protected
Border and personal safety.
In order to solve the above technical problems, the utility model adopts the following technical scheme：
Three aluminum hydride synthesis systems of recyclable ether include alchlor prepare kettle, pre-reactor, pre-reaction pans,
Reaction kettle, the first ether measuring tank, the second ether measuring tank, the first toluene measuring tank, the second toluene measuring tank, ether recycling dress
It sets, the first ether measuring tank, alchlor prepare kettle, pre-reactor, pre-reaction pans, reaction kettle and ether recycling dress
It sets and is sequentially connected with by the road.The second ether measuring tank and the first toluene measuring tank are connected to pre-reactor by the road, institute
It states the second toluene measuring tank and is connected with reaction kettle by the road, the alchlor prepares the top of kettle, pre-reactor and reaction kettle
Offer material inlet.Organic solvent after ether retracting device therein can be prepared three aluminum hydrides detaches, right
Ether solvent is recycled, and is reduced resource waste.
Three aluminum hydride synthesis systems of recyclable ether above-mentioned, the ether retracting device include being sequentially connected with by the road
Condensation, receiving tank, solvent tanker and solvent separation unit, the condensation is also connected to the top of reaction kettle by the road
Portion.Ether enters condensation by the road from reaction kettle, and boiling point is cold far below the solvent of condensation and other impurities at this time
Solidifying to pass back into reaction kettle, most of ether steam, which enters in condensation, to be condensed, and condensed liquid ether is by the road sequentially
It flows into receiving tank, solvent tanker, finally flows into solvent separation unit by the road, the further separation for carrying out ether solvent carries
It is pure.
Three aluminum hydride synthesis systems of recyclable ether above-mentioned further include third ether measuring tank, the second filter and urge
Agent prepares kettle, is sequentially connected with by the road between the third ether measuring tank, catalyst preparation kettle and the second filter, described
The other end of second filter is connected with reaction kettle by the road, and the top of the catalyst preparation kettle also offers material inlet.
Three aluminum hydrides of high-purity can be obtained by the configuration of catalyst.
Three aluminum hydride synthesis systems of recyclable ether above-mentioned further include first filter, and the one of the first filter
End is connected with pre-reactor by the road, and the other end of the first filter is connected with pre-reaction pans by the road.Wherein
One filter can be G5 filters, can improve the purity of three aluminum hydride products.
Three aluminum hydride synthesis systems of recyclable ether above-mentioned, the condensation include be connected with each other by the road it is vertical
Formula reflux condenser and horizontal condenser, the vertical reflux condenser is also connected to the top of reaction kettle by the road, described sleeping
Formula condenser is also connected to the top of receiving tank by the road.It is that the cooperation of vertical reflux condenser is horizontal cold by the way that condensation is arranged
Condensing mode as condenser so that the most of impurity and solvent being entrained in ether steam, which are condensed back to, to be flowed into reaction kettle,
So that the ether steam by vertical reflux condenser is more pure, it can largely condense and flow into horizontal condenser and connect
Secondary use is used in closed cans.
Three aluminum hydride synthesis systems of recyclable ether above-mentioned, the solvent separation unit is interior equipped with molecular sieve, described
The diameter of molecular sieve is more than the molecular diameter of ether, improves the reclaiming clean purity of ether.
Three aluminum hydride synthesis systems of recyclable ether above-mentioned further include switch valve, and the alchlor prepares kettle and the
Connecting line between one ether measuring tank is equipped with switch valve, and the alchlor is prepared between kettle and the second ether measuring tank
Connecting line be equipped with switch valve, the connecting line that the alchlor is prepared between kettle and the first toluene measuring tank is equipped with
Switch valve, connecting line between the reaction kettle and the second toluene measuring tank are equipped with switch valve, the pre-reactor and pre-
The connecting line between pans is reacted equipped with switch valve, on the connecting line between the pre-reaction pans and reaction kettle
Equipped with switch valve.By the way that switch valve is arranged on the pipeline between each equipment and automatic switch is arranged in solvent tanker, add
The strong control to solvent circulation.
Compared with prior art, the utility model is beneficial in that：
(1) three aluminum hydrides of present apparatus synthesis are at low cost, provide three aluminum hydride synthesis systems of recyclable ether, operation letter
Single, reaction condition is mildly easily controllable, at low cost, product quality is high, and three aluminum hydrides synthesized by the utility model, yield reaches
To 90% or more；
(2) by the configuration of ether measuring tank, the injected volume of ether can rationally be controlled；Pass through matching for toluene measuring tank
It sets, can rationally control the injected volume of toluene；
(3) the utility model is provided with catalyst preparation kettle, larger using crystal particle diameter obtained by this synthesizer, Neng Gouman
The demand of the big grain size product of foot；
(4) a kind of ether retracting device is also provided, the organic solvent after being prepared to three aluminum hydrides detaches, molten to ether
Agent is recycled, and is on the one hand reduced resource waste, and natural environment and personal safety are on the one hand protected.
Description of the drawings
Fig. 1 is the connection relationship diagram of the utility model.
The meaning of reference numeral：1- alchlors prepare kettle, 2- pre-reactors, 3- pre-reaction pans, 4- reaction kettles, 5-
First ether measuring tank, 6- the second ether measuring tanks, 7- third ether measuring tanks, 8- the first toluene measuring tanks, the second toluene of 9-
Measuring tank, 10- first filters, the second filters of 11-, 12- catalyst preparation kettles, 13- ether retracting devices, 14- condensation groups
Part, 15- receiving tanks, 16- solvent tankers, 17- solvent separation units, the vertical reflux condensers of 18-, 19- horizontal condensers.
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, three aluminum hydride synthesis systems of recyclable ether include tri-chlorination
Aluminium prepares kettle 1, pre-reactor 2, pre-reaction pans 3, reaction kettle 4, the first ether measuring tank 5, the second ether measuring tank 6, the
One toluene measuring tank 8, the second toluene measuring tank 9, ether retracting device 13, the first ether measuring tank 5, alchlor are prepared
Kettle 1, pre-reactor 2, pre-reaction pans 3, reaction kettle 4 and ether retracting device 13 are sequentially connected with by the road.Second second
Ether measuring tank 6 and the first toluene measuring tank 8 are connected to pre-reactor 2 by the road, and the second toluene measuring tank 9 connects by the road
It is connected to reaction kettle 4, the top that the alchlor prepares kettle 1, pre-reactor 2 and reaction kettle 4 offers material inlet.Wherein
Ether retracting device 13 can to three aluminum hydrides prepare after organic solvent detach, to ether solvent carry out recycling profit
With reducing resource waste.The ether retracting device 13 include by the road condensation 14 connected in sequence, receiving tank 15,
Solvent tanker 16 and solvent separation unit 17, the condensation 14 are also connected to the top of reaction kettle 4 by the road.Ether is from anti-
It answers and enters condensation 14 in kettle 4 by the road, boiling point is far below the solvent and other impurities condensing reflux of condensation 14 at this time
Enter in reaction kettle 4, most of ether steam, which enters in condensation 14, to be condensed, and condensed liquid ether sequentially flows by the road
In receiving tank 15, solvent tanker 16, finally flows into solvent separation unit 17 by the road, carry out the further separation of ether solvent
Purification.Three aluminum hydride synthesis systems of recyclable ether further include that third ether measuring tank 7, the second filter 11 and catalyst are matched
Kettle 12 processed is sequentially connected with, institute by the road between the third ether measuring tank 7, catalyst preparation kettle 12 and the second filter 11
The other end for stating the second filter 11 is connected with reaction kettle 4 by the road, and the top of the catalyst preparation kettle 12 also offers object
Expect import.Three aluminum hydrides of high-purity can be obtained by the configuration of catalyst.Three aluminum hydride synthesis systems of recyclable ether
Further include first filter 10, one end of the first filter 10 is connected with pre-reactor 2, the first filter by the road
10 other end is connected with pre-reaction pans 3 by the road.Wherein first filter 10 can be G5 filters, can improve three
The purity of aluminum hydride product.
Embodiment 2：Kettle 1, pre- is prepared as shown in Figure 1, three aluminum hydride synthesis systems of recyclable ether include alchlor
Reaction kettle 2, pre-reaction pans 3, reaction kettle 4, the first ether measuring tank 5, the second ether measuring tank 6, the first toluene measuring tank
8, the second toluene measuring tank 9, ether retracting device 13, the first ether measuring tank 5, alchlor prepare kettle 1, pre-reactor
2, pre-reaction pans 3, reaction kettle 4 and ether retracting device 13 are sequentially connected with by the road.The second ether measuring tank 6 and
One toluene measuring tank 8 is connected to pre-reactor 2 by the road, and the second toluene measuring tank 9 is connected with reaction kettle 4 by the road,
The top that the alchlor prepares kettle 1, pre-reactor 2 and reaction kettle 4 offers material inlet.Ether recycling dress therein
The organic solvent after the preparation of three aluminum hydrides can be detached by setting 13, be recycled to ether solvent, reduced resource
Waste.The condensation 14 includes the vertical reflux condenser 18 being connected with each other by the road and horizontal condenser 19, described vertical
Formula reflux condenser 18 is also connected to the top of reaction kettle 4 by the road, and the horizontal condenser 19 is also connected to reception by the road
The top of tank 15.It is that vertical reflux condenser 18 coordinates condensation side as horizontal condenser 19 by the way that condensation 14 is arranged
Formula so that the most of impurity and solvent being entrained in ether steam, which are condensed back to, to be flowed into reaction kettle 4, so that passing through vertical time
The ether steam of flow condenser 18 is more pure, can largely condense and be flowed into receiving tank 15 in horizontal condenser 19 and is used for
Secondary use.Further, the temperature for especially controlling vertical reflux condenser 18 is 20 DEG C~30 DEG C, horizontal condenser 19
When temperature is -5 DEG C~-15 DEG C, the refining effect of ether is preferable；Preferably, the temperature of vertical reflux condenser 18 is 20 DEG C, crouch
The temperature of formula condenser 19 is -10 DEG C.Molecular sieve is equipped in the solvent separation unit 17, the diameter of the molecular sieve is more than second
The molecular diameter of ether improves the reclaiming clean purity of ether.
Embodiment 3：Kettle 1, pre- is prepared as shown in Figure 1, three aluminum hydride synthesis systems of recyclable ether include alchlor
Reaction kettle 2, pre-reaction pans 3, reaction kettle 4, the first ether measuring tank 5, the second ether measuring tank 6, the first toluene measuring tank
8, the second toluene measuring tank 9, ether retracting device 13, the first ether measuring tank 5, alchlor prepare kettle 1, pre-reactor
2, pre-reaction pans 3, reaction kettle 4 and ether retracting device 13 are sequentially connected with by the road.The second ether measuring tank 6 and
One toluene measuring tank 8 is connected to pre-reactor 2 by the road, and the second toluene measuring tank 9 is connected with reaction kettle 4 by the road,
The top that the alchlor prepares kettle 1, pre-reactor 2 and reaction kettle 4 offers material inlet.Ether recycling dress therein
The organic solvent after the preparation of three aluminum hydrides can be detached by setting 13, be recycled to ether solvent, reduced resource
Waste.Three aluminum hydride synthesis systems of recyclable ether further include switch valve, and the alchlor prepares kettle 1 and the first ether meter
Connecting line between measuring tank 5 is equipped with switch valve, and the alchlor prepares the company between kettle 1 and the second ether measuring tank 6
It takes over road and is equipped with switch valve, the connecting line between the alchlor preparation kettle 1 and the first toluene measuring tank 8, which is equipped with, to be opened
Close valve, connecting line between the reaction kettle 4 and the second toluene measuring tank 9 is equipped with switch valve, the pre-reactor 2 and pre-
The connecting line reacted between pans 3 is equipped with switch valve, the connecting tube between the pre-reaction pans 3 and reaction kettle 4
Road is equipped with switch valve.It is opened automatically by the way that switch valve is arranged on the pipeline between each equipment and is arranged in solvent tanker 16
It closes, strengthens the control circulated to solvent.
A kind of operation principle of the utility model：By three aluminum hydride synthesis systems prepare three aluminum hydrides, may include with
Lower step：(1) anhydrous AlCl3With the preparation of ether mixed solution；(2)LiAlH4With anhydrous AlCl3The preparation of mixed solution；(3)
The preparation of catalyst；The preparation of (4) three aluminum hydrides；(5) ether solvent recycles；
Specific steps are as follows：
Industrial ether is respectively put into the first ether measuring tank 5, the second ether measuring tank 6 by being refining to obtain anhydrous ether
With it is spare in third ether measuring tank 7；Toluene after refined is respectively put into the first toluene measuring tank 8 and the second toluene measuring tank 9
In it is spare；
(1) anhydrous AlCl3With the preparation of ether mixed solution
Take anhydrous AlCl3It prepares in kettle 1 through material inlet input alchlor, is slowly dripped by the first ether measuring tank 5
Add refined anhydrous ether, the agitating device in kettle 1 is prepared by alchlor after being added dropwise and is stirred to AlCl3It is completely dissolved；
(2)LiAlH4With anhydrous AlCl3The preparation of mixed solution
By the second ether measuring tank 6 discharge refine anhydrous ether enter in pre-reactor 2, while by material inlet to
It is put into pre-reactor 2 and refines lithium aluminium hydride reduction, after stirring a period of time by the agitating device inside pre-reactor 2, side stirring
While alchlor, which is slowly added dropwise, prepares the anhydrous AlCl of gained in kettle 13With 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 8 in time4With anhydrous AlCl3It is mixed
It closes solution to filter by first filter 10, flow into spare in pre-reaction pans 3；
(3) preparation of catalyst
Anhydrous ether is discharged by third ether measuring tank 7 to enter in catalyst preparation kettle 12, weighs catalyst through material
Import is put into catalyst preparation kettle 12, is mixed to and is completely dissolved with anhydrous ether therein, spare；
The preparation of (4) three aluminum hydrides
Refined toluene is discharged by the second toluene measuring tank 9 to be placed in reaction kettle 4, and reaction kettle 4 is vacuumized, is passed through
The operation of inert gas removes the oxygen in reaction kettle 4, and gained catalyst in catalyst preparation kettle 12 is then added, is flowing back
Heating is stirred under state, temperature controls at 75 DEG C~94 DEG C, then begins to distill, and be slowly added dropwise in pre-reaction pans 3
LiAlH4With anhydrous AlCl3Mixed solution after being added dropwise, then carries out temperature rising reflux, continues thereafter with distillation, and temperature is controlled 94
DEG C~107 DEG C and flow back a period of time, be slowly dropped to room temperature, stratification discards supernatant liquid, then passes through the second toluene measuring tank
9 release refined toluenes wash repeatedly, and until without apparent floating material, three aluminum hydrides are then obtained by filtration；
(5) ether solvent recycles
In three aluminum hydride preparation process, reaction temperature is higher than 34.6 DEG C of ether boiling point, is less than 110.6 DEG C of toluene boiling point, because
This toluene keeps liquid, and ether largely evaporates, and the ether of evaporation enters vertical reflux condenser by the road from reaction kettle 4
18, boiling point is far below the solvent of vertical reflux condenser 18 at this time and other impurities are condensed back to and flow into reaction kettle 4, most of second
Ether steam, which enters in the lower horizontal condenser of temperature 19, to be condensed, and condensed liquid ether sequentially flows into receiving tank by the road
15, in solvent tanker 16, and in the last solvent separation unit 17 of inflow by the road, the further separation for carrying out ether solvent carries
It is pure.Molecular sieve wherein inside solvent separation unit 17 adsorbs ether, and the molecular sieve that ether is adsorbed with by heating obtains ether,
So that the molecular sieve in solvent separation unit 17 can be with cycling and reutilization.
Claims (7)
1. three aluminum hydride synthesis systems of recyclable ether, which is characterized in that prepare kettle (1), pre-reactor including alchlor
(2), pre-reaction pans (3), reaction kettle (4), the first ether measuring tank (5), the second ether measuring tank (6), the first toluene meter
Measuring tank (8), the second toluene measuring tank (9), ether retracting device (13), the first ether measuring tank (5), alchlor are prepared
Kettle (1), pre-reactor (2), pre-reaction pans (3), reaction kettle (4) and ether retracting device (13) are sequentially connected with by the road,
The second ether measuring tank (6) and the first toluene measuring tank (8) are connected to pre-reactor (2), second first by the road
Benzene measuring tank (9) is connected with reaction kettle (4) by the road, and the alchlor prepares kettle (1), pre-reactor (2) and reaction kettle (4)
Top offer material inlet.
2. three aluminum hydride synthesis systems of recyclable ether according to claim 1, which is characterized in that the ether recycling
Device (13) includes that condensation (14) connected in sequence, receiving tank (15), solvent tanker (16) detach dress with solvent by the road
It sets (17), the condensation (14) is also connected to the top of reaction kettle (4) by the road.
3. three aluminum hydride synthesis systems of recyclable ether according to claim 2, which is characterized in that further include third second
Ether measuring tank (7), the second filter (11) and catalyst preparation kettle (12), the third ether measuring tank (7), catalyst preparation
It is sequentially connected with by the road between kettle (12) and the second filter (11), the other end of second filter (11) connects by the road
There are reaction kettle (4), the top of the catalyst preparation kettle (12) also to offer material inlet.
4. three aluminum hydride synthesis systems of recyclable ether according to claim 3, which is characterized in that further include the first mistake
One end of filter (10), the first filter (10) is connected with pre-reactor (2) by the road, the first filter (10)
The other end is connected with pre-reaction pans (3) by the road.
5. three aluminum hydride synthesis systems of recyclable ether according to claim 2, which is characterized in that the condensation
(14) include the vertical reflux condenser (18) being connected with each other by the road and horizontal condenser (19), the vertical reflux condenser
(18) it is also connected to the top of reaction kettle (4) by the road, the horizontal condenser (19) is also connected to receiving tank (15) by the road
Top.
6. three aluminum hydride synthesis systems of recyclable ether according to claim 5, which is characterized in that the solvent separation
Molecular sieve is equipped in device (17), the diameter of the molecular sieve is more than the molecular diameter of ether.
7. three aluminum hydride synthesis systems of recyclable ether according to claim 1, which is characterized in that further include switch
Valve, the alchlor prepare the connecting line between kettle (1) and the first ether measuring tank (5) equipped with switch valve, and described three
Aluminium chloride prepares the connecting line between kettle (1) and the second ether measuring tank (6) and is equipped with switch valve, and the alchlor is prepared
Connecting line between kettle (1) and the first toluene measuring tank (8) is equipped with switch valve, the reaction kettle (4) and the second toluene meter
Connecting line between measuring tank (9) is equipped with switch valve, the connection between the pre-reactor (2) and pre-reaction pans (3)
Pipeline is equipped with switch valve, and the connecting line between the pre-reaction pans (3) and reaction kettle (4) is equipped with switch valve.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201820200907.6U CN207861884U (en) | 2018-02-06 | 2018-02-06 | Three aluminum hydride synthesis systems of recyclable ether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201820200907.6U CN207861884U (en) | 2018-02-06 | 2018-02-06 | Three aluminum hydride synthesis systems of recyclable ether |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114956137A (en) * | 2022-06-07 | 2022-08-30 | 湖北航天化学技术研究所 | Preparation method of gamma-aluminum hydride |
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2018
- 2018-02-06 CN CN201820200907.6U patent/CN207861884U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114956137A (en) * | 2022-06-07 | 2022-08-30 | 湖北航天化学技术研究所 | Preparation method of gamma-aluminum hydride |
| CN114956137B (en) * | 2022-06-07 | 2023-09-15 | 湖北航天化学技术研究所 | Preparation method of gamma-aluminum hydride |
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