Utility model content
In view of the deficiencies in the prior art, the technical problem to be solved by the utility model is to provide a kind of preparations of diborane to fill
It sets, is not only simple in structure, and convenient and efficient.
In order to solve the above-mentioned technical problem, the technical solution of the utility model is: a kind of diborane preparation facilities, including warp
The sequentially connected liquid pool of pipeline, reactor, recycling cold hydrazine, product freezing bottle;
The liquid pool includes closed liquid dispensing container, the liquid dispensing container be equipped with liquid air inlet, with liquid exhaust outlet,
Liquid matching and feeding mouth matches liquid leakage fluid dram, matches liquid sewage draining exit;
The reactor includes closed reaction vessel, the reaction vessel be equipped with reaction air inlet, reaction gas outlet,
Inlet, reaction leakage fluid dram are reacted, the peripheral part of the reaction vessel is equipped with the first closed lagging casing, first heat preservation
It is the first temperature adjustment cavity between shell and reaction vessel, the first temperature adjustment cavity is connect with the first temperature control device;
The recycling cold hydrazine includes closed returnable, and the returnable is equipped with recycling air inlet, recycling outlet
Mouthful, the peripheral part of the returnable is equipped with the second closed lagging casing, between second lagging casing and returnable
For the second temperature adjustment cavity, the second temperature adjustment cavity is connect with the second temperature control device;
Described to connect with liquid leakage fluid dram with reaction inlet, the reaction gas outlet is connect with recycling air inlet, and described time
Gas outlet is received to connect with product freezing bottle.
Preferably, the upper circumference that liquid dispensing container is respectively positioned on liquid air inlet and with liquid exhaust outlet, it is described to match liquid drain
Mouth and the lower circumference that liquid dispensing container is respectively positioned on liquid sewage draining exit, the liquid matching and feeding mouth are located at the top of liquid dispensing container and are bolted with
End cover, the interior bottom that liquid dispensing container is extended to liquid air inlet pipe on liquid air inlet are described on liquid leakage fluid dram
With liquid drain pipe be equipped with filter screen.
Preferably, the reaction inlet and the top reacted gas outlet and be located at reaction vessel, on the reaction air inlet
The supreme interior bottom for extending to reaction vessel down of reaction air inlet pipe, the reaction drain pipe on the reaction leakage fluid dram is located at anti-
The bottom of container is answered, the reaction vessel is equipped with reaction vessel liquidometer.
Preferably, first lagging casing includes the interior shell for setting heat preservation sandwich layer, is packed into pearly-lustre in the heat preservation sandwich layer
Sand keeps the temperature filler, and the bottom of the heat preservation sandwich layer is equipped with the vacuum-pumping tube being controlled to a vacuum pump, and vacuum-pumping tube is equipped with filter screen,
The top of the heat preservation sandwich layer is equipped with feeding port;First temperature control device includes connect circumference under the first temperature adjustment cavity first
Air inlet pipe, the downtake pipe for connecting the first temperature adjustment cavity top, be connected in first air inlet pipe low temperature nitrogen air inlet pipe,
Heated nitrogen air inlet pipe.
Preferably, the recycling gas outlet is located at the top of returnable, and the recycling air inlet is supreme to be extended to down
The interior bottom of returnable;Second lagging casing includes the interior shell for setting heat preservation sandwich layer, is packed into pearl in the heat preservation sandwich layer
Light sand keeps the temperature filler, and the bottom of the heat preservation sandwich layer is equipped with the vacuum-pumping tube being controlled to a vacuum pump, and vacuum-pumping tube is equipped with filtering
The top of net, the heat preservation sandwich layer is equipped with feeding port;Second temperature control device includes circumference under the second temperature adjustment cavity of connection
Second air inlet pipe, the second exhaust pipe for connecting the second temperature adjustment cavity top, be connected in second air inlet pipe liquid nitrogen air inlet pipe,
Hot nitrogen air inlet pipe.
Preferably, the product freezing bottle includes product freezing bottle cold hydrazine, and liquid nitrogen is equipped in the product freezing bottle cold hydrazine
With stainless steel freezing bottle.
Preferably, the low temperature nitrogen air inlet pipe is equipped with valve A, heated nitrogen air inlet pipe is equipped with valve B, first row
Tracheae is equipped with valve C.
Preferably, the liquid nitrogen air inlet pipe is equipped with valve D, hot nitrogen air inlet pipe is equipped with valve E, the second air inlet pipe is set
There is valve F.
Preferably, described with being connected with liquid air inlet pipe and air inlet supervisor on liquid air inlet, it is described on liquid leakage fluid dram
It is connect with liquid drain pipe with reaction inlet, is also connected with the first air intake branch and the second air intake branch on the air inlet supervisor,
It is described to be connected in parallel on air inlet supervisor with liquid air inlet pipe, the first air intake branch, the second air intake branch, first air intake branch
The other end connection match liquid drain pipe, second air intake branch the other end connection reaction air inlet reaction air inlet pipe, institute
It states reaction air inlet pipe and is also connected with boron chloride adding tube, the air inlet supervisor is equipped with valve one, described in liquid air inlet pipe
It is described to be equipped with valve three with liquid exhaust pipe with liquid exhaust outlet equipped with valve two, it is described to be equipped with valve four with liquid drain pipe,
First air intake branch is equipped with valve five, and second air intake branch is equipped with valve six, the boron chloride adding tube
On along direction of advance be successively arranged valve seven, valve eight;Along airflow direction on reaction escape pipe on the reaction gas outlet
It is successively arranged valve nine, valve ten, valve 11, reacts the external product steel cylinder framed bent in escape pipe end, the reaction escape pipe
Blow-down pipe and valve 12 are connected with before valve nine, the reaction escape pipe is connected with back between valve nine and valve ten
The recycling air inlet pipe of port is taken in, recycling air inlet pipe is equipped with valve 13, sets on the recycling escape pipe of the recycling gas outlet
There is valve 14 and is connected to reacting on escape pipe between valve ten and valve 11;It is connected on the recycling escape pipe true
Blank pipe, vacuum tube are successively arranged valve 15, valve 16, vacuum pump along airflow direction, are connected with and put on the vacuum tube
The product air inlet pipe of blank pipe and valve 17, the product freezing bottle reacts outlet between recycling escape pipe, valve 11
Pipe connection, product air inlet pipe are equipped with valve 18.
Compared with prior art, the utility model has the following beneficial effects: the diborane preparation facilities not only structure is set
Meter is simple, reasonable, and preparation effect is good, high-efficient, has broad application prospects.
The utility model is described in more detail with reference to the accompanying drawings and detailed description.
Specific embodiment
In order to make the above-mentioned features and advantages of the utility model more obvious and understandable, special embodiment below, and cooperate attached drawing,
It is described in detail below.
As shown in Fig. 1 ~ 4, a kind of diborane preparation facilities, including through the sequentially connected liquid pool 1 of pipeline, reactor 2, return
Receive cold hydrazine 3, product freezing bottle 4;
The liquid pool includes closed liquid dispensing container 5, and the liquid dispensing container is equipped with liquid air inlet 6, with liquid and is vented
Mouth 7, liquid matching and feeding mouth 8 match liquid leakage fluid dram 9, match liquid sewage draining exit 10;Sodium borohydride is solid-state white crystals, and boron chloride is low
Liquefied gas is pressed, the two is reacted, it is necessary to which certain solvent dissolves by sodium borohydride.Glycol dimethyl ether is a kind of band
There is the water white neutral liquid of ether taste, property is stablized, is not susceptible to react, and can dissolve sodium borohydride and boron chloride, liquid pool
It is sodium borohydride and glycol dimethyl ether mixed dissolution container, sealing device should be arranged in container, and is passed through helium and is stirred, with
Just the acceleration dissolution of sodium borohydride.
The reactor includes closed reaction vessel 11, and the reaction vessel is equipped with reaction air inlet 12, reflects
Port 13, reaction inlet 14, reaction leakage fluid dram 15, the peripheral part of the reaction vessel are equipped with the first closed lagging casing
16, it is the first temperature adjustment cavity 17, the first temperature adjustment cavity and the first temperature control between first lagging casing and reaction vessel
Device connection;The reaction principle of diborane is generated according to sodium borohydride and boron trichloride reaction, reaction process is carried out in two steps, the
One step controls temperature within the scope of 0~25 DEG C, and second step controls temperature within the scope of 25~50 DEG C, and therefore, reactor needs to design
First temperature control device carries out the offer and temperature control of cold and heat source.
The recycling cold hydrazine includes closed returnable 81, and the returnable is equipped with recycling air inlet 18, recycling
Gas outlet 19, the peripheral part of the returnable are equipped with the second closed lagging casing 20, second lagging casing and recycling
It is the second temperature adjustment cavity 21 between container, the second temperature adjustment cavity is connect with the second temperature control device;
Described to connect with liquid leakage fluid dram with reaction inlet, the reaction gas outlet is connect with recycling air inlet, and described time
Gas outlet is received to connect with product freezing bottle.
In the utility model embodiment, the last week that liquid dispensing container is respectively positioned on liquid air inlet and with liquid exhaust outlet
Portion, it is described to hold with the lower circumference for being respectively positioned on liquid dispensing container with liquid sewage draining exit, the liquid matching and feeding mouth positioned at liquid with liquid leakage fluid dram
The top of device and it is bolted with end cover 22, the interior bottom that liquid dispensing container is extended to liquid air inlet pipe on liquid air inlet
Portion, the liquid drain pipe 23 of matching on liquid leakage fluid dram are equipped with filter screen 24.
In the utility model embodiment, the reaction inlet and the top reacted gas outlet and be located at reaction vessel, institute
The supreme interior bottom for extending to reaction vessel down of reaction air inlet pipe on reaction air inlet is stated, it is anti-on the reaction leakage fluid dram
Drain pipe is answered to be located at the bottom of reaction vessel, the reaction vessel is equipped with reaction vessel liquidometer 25.
In the utility model embodiment, first lagging casing includes the interior shell for setting heat preservation sandwich layer 26, the guarantor
It is packed into pearlife in warm interlayer and keeps the temperature filler, the bottom of the heat preservation sandwich layer is equipped with the vacuum-pumping tube 28 connecting with vacuum pump 27,
Vacuum-pumping tube is equipped with filter screen 29, and heat preservation sandwich layer bottom evacuates mouth and is pumped into negative pressure, to improve heat insulation effect, the heat preservation sandwich layer
Top be equipped with feeding port 30;First temperature control device include connect the first temperature adjustment cavity under circumference the first air inlet pipe 31,
The downtake pipe 32 on the first temperature adjustment cavity top is connected, low temperature nitrogen air inlet pipe 33 is connected in first air inlet pipe, is added
Hot nitrogen air inlet pipe 34.
In the utility model embodiment, the recycling gas outlet is located at the top of returnable, the recycling air inlet
The supreme interior bottom for extending to returnable down;Second lagging casing includes the interior shell for setting heat preservation sandwich layer, the guarantor
It is packed into pearlife in warm interlayer and keeps the temperature filler, the bottom of the heat preservation sandwich layer is equipped with the vacuum-pumping tube being controlled to a vacuum pump, and takes out true
Blank pipe is equipped with filter screen, and heat preservation sandwich layer bottom evacuates mouth and is pumped into negative pressure, to improve heat insulation effect, the top of the heat preservation sandwich layer
Equipped with feeding port;Second temperature control device includes connecting the second air inlet pipe 35 of circumference under the second temperature adjustment cavity, connection second
The second exhaust pipe 36 on temperature adjustment cavity top is connected with liquid nitrogen air inlet pipe 37, hot nitrogen air inlet pipe 38 in second air inlet pipe.
In the utility model embodiment, the product freezing bottle includes product freezing bottle cold hydrazine 39, the product freezing
Liquid nitrogen 40 and stainless steel freezing bottle 41 are equipped in bottle cold hydrazine.
In the utility model embodiment, the low temperature nitrogen air inlet pipe is equipped in valve A42, heated nitrogen air inlet pipe
Valve C44 is equipped with equipped with valve B43, downtake pipe.
In the utility model embodiment, the liquid nitrogen air inlet pipe is equipped with valve D45, hot nitrogen air inlet pipe is equipped with valve
Door E46, the second air inlet pipe are equipped with valve F47.
In the utility model embodiment, the liquid air inlet pipe 48 of matching on liquid air inlet being connect with air inlet supervisor 49,
The liquid drain pipe of matching on liquid leakage fluid dram being connect with reaction inlet, is also connected with the first air inlet branch on the air inlet supervisor
Pipe 50 and the second air intake branch 51, it is described to be connected in air inlet master in parallel with liquid air inlet pipe, the first air intake branch, the second air intake branch
Liquid drain pipe is matched in Guan Shang, the other end connection of first air intake branch, and the other end of second air intake branch connects reaction
The reaction air inlet pipe 52 of air inlet, the reaction air inlet pipe are also connected with boron chloride adding tube 53, set on the air inlet supervisor
There is valve 1, it is described to be equipped with valve 2 55 with liquid air inlet pipe, it is described to be equipped with valve with liquid exhaust pipe 56 with liquid exhaust outlet
Door 3 57, it is described with liquid drain pipe be equipped with valve 4 58, first air intake branch be equipped with valve 5 59, described second into
Gas branch pipe is equipped with valve 6 60, is successively arranged valve 7 61, valve 8 62 along direction of advance in the boron chloride adding tube;
Valve 9 64, valve 10, valve ten are successively arranged along airflow direction on reaction escape pipe 63 on the reaction gas outlet
One 66, the external product steel cylinder framed bent in escape pipe end is reacted, the reaction escape pipe is connected with blow-down pipe 67 before valve nine
With valve 12, the reaction escape pipe is connected with the recycling air inlet pipe of recycling air inlet between valve nine and valve ten
69, recycling air inlet pipe is equipped with valve 13, and the recycling escape pipe 71 of the recycling gas outlet is equipped with valve 14 simultaneously
It is connected to reacting on escape pipe between valve ten and valve 11;Vacuum tube 73, vacuum are connected on the recycling escape pipe
Pipe is successively arranged valve 15, valve 16, vacuum pump along airflow direction, be connected on the vacuum tube blow-down pipe with
The product air inlet pipe 77 of valve 17, the product freezing bottle reacts escape pipe between recycling escape pipe, valve 11
Connection, product air inlet pipe are equipped with valve 18;The reaction drain pipe 79 for reacting leakage fluid dram is equipped with valve 19.
In the utility model embodiment, the reaction equation of diborane is generated such as using sodium borohydride and boron trichloride reaction
Under:
Above-mentioned reaction is carried out in two steps, and the first step controls temperature within the scope of 0~25 DEG C, and boron hydrogen is added in 7 to 1 ratio
Change sodium and boron chloride;Second step controls temperature within the scope of 25~50 DEG C, continuously adds boron chloride in 3 to 1 ratio, with
Being stepped up for temperature, diborane constantly gasify to collecting in special container.From the reactions above as can be seen that byproduct chlorine
Change sodium (salt) is nontoxic, is easily processed.
A kind of preparation method of diborane preparation facilities, sequentially includes the following steps:
(1) technical parameter: diborane yield: 0.35kg/ times, sodium borohydride consumption: 0.845 kg/ times, boron chloride consumption
Amount: 0.873 kg/ time: first step addition: 1 hour 0.374kg(reaction time);Second step is added: the 0.499kg(reaction time 3
Hour), glycol dimethyl ether dosage: 6 liters/time, glycol dimethyl ether consumption: when 1.8 liters/time (recycling 70%), each reaction
Between: 4 hours/time, reactor operating pressure: 0.3Mpa, reactor operating temperature: step 1: 0~25 DEG C;Step 2: 25~50
DEG C, recycling cold hydrazine operating temperature: -80~90 DEG C, product freezing bottle operating temperature: -196 DEG C (liquid nitrogen temperature);
(2) preparation: 1. evacuate to whole device and removes foreign gas with helium replacement with vacuum pump, including
The pipe-line system of each feed(raw material)inlet opens valve two, four, five, six, eight, 12,13,15,16,14, ten, 18;
2. spraying liquid nitrogen toward the second temperature adjustment cavity discontinuity by liquid nitrogen air inlet pipe, the second temperature adjustment cavity temperature T2 of control is -80~-90
℃;3. pouring into liquid nitrogen in product freezing bottle cold hydrazine, it is slowly inserted in stainless steel freezing bottle, stainless steel freezing bottle is made to be cooled to -196
℃;4. pouring into 6 liters of glycol dinitrate ether solvents in liquid dispensing container, weighs 845 grams of sodium borohydrides and pour into liquid dispensing container and second two
The mixing of diethylene glycol dimethyl ether solvent, then covers sealing for liquid pool, and the valve one, two for slightly opening helium is sent into helium, while slightly
Valve opening door three pays attention to observing the not super 0.1MPa of pressure gauge P1 on liquid dispensing container, be stirred to mixed liquor, and exclude liquid pool
Interior moisture and foreign gas;
(3) first step operation: the moisture and foreign gas displacement 1. when mixed liquor stirs evenly, and in liquid pool are dry
After net, valve four is opened, mixed liquor is sent into reaction vessel, pays attention to observing response tank ga(u)ge L1 instruction about 40%;2. leading to
It crosses low temperature nitrogen inlet duct and is passed through low temperature nitrogen toward the first temperature adjustment cavity, control reaction vessel temperature T1 within the scope of 0~25 DEG C;
3. boron chloride gas cylinder is placed on electronic scale, then it is connect with stainless steel high-pressure hose with boron chloride adding tube, record electricity
The weight number of sub- scale, opens boron chloride bottle valve, slightly valve opening door seven, valve eight, with 6.25 grams of flow per minute to reaction
Container is sent into boron trichloride gas, after electronic scale, which is shown, is sent into 375 grams of boron chlorides to reaction vessel (about 1 hour), closes
Close boron chloride bottle valve and valve eight;4. opening valve nine and valve 13, a small amount of by reaction process generation is with methane
Main tail gas imports returnable, and diborane is frozen collection, and interruption opens valve 15,17, the methane that will be frozen
And other impurities are along blow-down pipe discharge system;5. being interrupted slightly valve opening door five, reactor, recycling cold hydrazine and system are carried out with helium
Displacement, blows out the foreign gas of system, is then shut off all valves, and first step reaction terminates;
(4) second step operation: being 1. passed through heated nitrogen toward the first temperature adjustment cavity by heated nitrogen air inlet pipe, control
Reaction vessel temperature T1 is within the scope of 25~50 DEG C;2. boron chloride bottle valve, slightly valve opening door seven, eight are opened, with per minute
5.52 grams of flow is sent into boron trichloride gas to reaction vessel, is sent into 497 grams of trichlorines to reaction vessel when electronic scale is shown
After change boron (about 1.5 hours), boron chloride bottle valve and valve seven, eight are closed;3. valve nine, ten, 18 is opened, by diborane
Freeze into product freezing bottle;4. illustrating diborane in reaction vessel when the pressure gauge P3 being mounted on reaction escape pipe falls to zero
All freeze into product freezing bottle, has closed valve nine, ten;
(5) product fills bottle: 1. unloading product freezing bottle cold hydrazine, is heated, made to stainless steel freezing bottle with normal-temperature water
Diborane in stainless steel freezing bottle, which gasifies, to boost, and pressure gauge P6 thereon is gradually increasing;2. being said when pressure gauge P6 stops rising
Diborane in bright stainless steel freezing bottle has been gasified totally, and opens valve 11, diborane product is filled with to external product steel
Bottle framed bent;3. closing when pressure gauge P6 shows pressure and the pressure balance of product steel cylinder and filling product steel cylinder cylinder valve, open another
Residual compression is filled with another product steel cylinder by branch product steel cylinder cylinder valve, and so on, until by product in stainless steel freezing bottle
Packing finishes.
The utility model is not limited to above-mentioned preferred forms, anyone can obtain under the enlightenment of the utility model
Other various forms of diborane preparation facilities out.All equivalent changes done according to present utility model application the scope of the patents with repair
Decorations, should all belong to the covering scope of the utility model.