CN101822968A

CN101822968A - Triethylaluminum production device with quantitative discharge reaction kettle and process thereof

Info

Publication number: CN101822968A
Application number: CN 201010179557
Authority: CN
Inventors: 冯书辉; 杨卫东
Original assignee: Tianjin Lianli Chemical Co Ltd
Current assignee: Tianjin Lianli Chemical Co Ltd
Priority date: 2010-05-21
Filing date: 2010-05-21
Publication date: 2010-09-08

Abstract

The invention relates to a triethylaluminum production device with a quantitative discharge reaction kettle and a process thereof, belonging to the field of petrochemical equipment, wherein the reaction kettle comprises a quantitative discharge structure. Triethylaluminum seeds are quantitatively put into the reaction kettle with the quantitative discharge structure according to the preset capacity of liquid level in a kettle body, thereby carrying out hydrogenation reaction; ethylene is added in the reaction kettle with the quantitative discharge structure for carrying out ethylation reaction after finishing the hydrogenation reaction; and the preset quantity of coarse products generated by the reaction are taken by a quantitative discharge pipe and transferred to a distillation system after finishing the ethylation reaction, and the remaining coarse products are the seeds for reaction of the next kettle. The reaction kettle in the scheme cleverly sets the quantitative discharge structure, effectively optimizes the production process and simplifies equipment, and the hydrogenation reaction and the ethylation reaction can be completed in the reaction kettle with the quantitative discharge structure; and an ethylation reactor does not need to be additionally configured for carrying out the ethylation reaction.

Description

Triethyl aluminum production equipment and technology thereof with quantitative discharging reactor

Technical field

The invention belongs to field of petrochemical industrial, particularly relate to hydrogenation and ethylation reaction device and production technology thereof in the production equipment of triethyl aluminum.

Background technology

Producing triethyl aluminum is prior art, as " two-step method " technology that is commonly called as: triethyl aluminum seed and aluminium powder at first mixed being transferred to reactor then in the seed measuring tank, in still, feed hydrogen and carry out hydrogenation, generate ADEH, again reactant liquor all is transferred to ethylation reaction device adding ethene and carries out ethylation reaction, generate the thick product of triethyl aluminum, the product 84%-85% that each still generates turns back to transfer in the hydrogenation reactor after seed measuring tank adding aluminium powder mixes and reacts next time, and remaining product of about 15% enters into Distallation systm rectifying and goes out final products.

Disclosed for another example Chinese patent " synthetic process of 200710060113.0 1 kinds of triethyl aluminums ".

Known technology has the introduction in experimental stage, but it is rare that the information of triethyl aluminum is produced in industrialization, at producing the such dangerous material of triethyl aluminum, the known technology problem is that equipment complexity, technological process simplify, operate easy inadequately inadequately, these have become a difficult problem that hinders production efficiency, the more important thing is that the danger coefficient in the production is difficult to effective control; Market demands operating simpler, safer production technology urgently and equipment comes out.

As the link of aluminium powder charging in the triethyl aluminum production process, prior art generally is that aluminium powder is replaced in a cover system equipment, and the aluminium powder after will replacing again drops into reactor by the equipment that feeds intake;

Disclosed Chinese patent " 00819839.X crystal refiner and method ", though relate to the technology that feeds intake in the chemical products production process, but can not solve such problem: when aluminium powder is thrown in, because there is pressure-fired in the characteristic of aluminium powder self viscous in the reactor usually in addition, aluminium powder is thrown in always not smooth situation, brings the difficulty that feeds intake;

For another example in the triethyl aluminum production process to the metering link of seed, need seed be measured by the seed measuring tank of configuration separately;

Such as in the ethylation reaction of triethyl aluminum production process, need dispose the ethylation reaction device separately and carry out ethylation reaction again;

Also have, the reaction heat in the reactor is removed technology and the not enough optimization of equipment or the like, and industry is demanded the production equipment appearance that the triethyl aluminum simpler and more direct, that security is higher is more simplified, operated to a kind of equipment urgently for this reason.

Summary of the invention

This case problem to be solved is to overcome the above-mentioned defective that aforementioned techniques exists, and a kind of triethyl aluminum production equipment and technology thereof with quantitative discharging reactor is provided,

The present invention solves the reactor technical problem and takes following technical scheme to realize, according to a kind of reactor provided by the invention with quantitative discharging structure, comprise still body 41, wherein, described still body forms container jointly by hollow chamber and upper cover, low head; Preset diameters is D in the hollow chamber of this still body, the liquid level line a that satisfies default liquid level H is set in the still body forms the quantitative structure of energy; Quantitative discharging pipe 9 is arranged in the hollow chamber of still body, and the liquid feeding end 90 of quantitative discharging pipe is provided with the liquid level line a place that is positioned at hollow chamber, and described quantitative discharging pipe has preset length and internal diameter.

Can form reactor thus with quantitative discharging structure.

This case solves the reactor technical problem and can also take following technical scheme further to realize:

Aforesaid reactor with quantitative discharging structure, wherein, described quantitative discharging pipe outlet end opens and closes by valve 91 controls; The outlet end 92 of described quantitative discharging pipe stretches out the still body and docks with external reservoir.

Aforesaid reactor with quantitative discharging structure, wherein, the hollow chamber 410 of described still body is the cylinder die cavity;

Aforesaid reactor with quantitative discharging structure, wherein, the upper cover 411 of described still body is dome head or ellipsoidal head, low head 412 is dome heads;

Aforesaid reactor with quantitative discharging structure wherein, has nitrogen delivery end 43 on the described still body, and the nitrogen tube 8 of valve 81 is equipped with in the nitrogen delivery end configuration of still body;

Aforesaid reactor with quantitative discharging structure, wherein, described quantitative discharging pipe vertically stretches in the hollow chamber; Have reactor charging aperture 44 on the described reactor, drop into thus through displacement back aluminium powder.

The present invention solves the technical problem of triethyl aluminum production equipment and takes following technical scheme to realize, according to a kind of triethyl aluminum production equipment provided by the invention, comprise reactor, this reactor has still body and agitator, wherein, described still body forms container jointly by hollow chamber and upper cover, low head; Preset diameters is D in the hollow chamber of this still body, the liquid level line a that satisfies default liquid level H is set in the still body forms the quantitative structure of energy; Quantitative discharging pipe 9 is arranged in the hollow chamber of still body, and the liquid feeding end 90 of quantitative discharging pipe is provided with the liquid level line a place that is positioned at hollow chamber, and described quantitative discharging pipe has preset length and internal diameter.

This case solves the equipment and technology problem and can also take following technical scheme further to realize:

Aforesaid triethyl aluminum production equipment, wherein, described quantitative discharging pipe outlet end opens and closes by valve 91 controls; The outlet end 92 of described quantitative discharging pipe stretches out the still body and docks with external reservoir; Have nitrogen delivery end 43 on the described still body, the nitrogen tube 8 of valve 81 is equipped with in the nitrogen delivery end configuration of still body.

Aforesaid triethyl aluminum production equipment, wherein, the hollow chamber 410 of described still body is the cylinder die cavity; The upper cover 411 of described still body is dome head or ellipsoidal head, and low head 412 is dome heads.

Aforesaid triethyl aluminum production equipment, wherein, described quantitative discharging pipe vertically stretches in the hollow chamber; Have reactor charging aperture 44 on the described reactor, drop into thus through displacement back aluminium powder.

The present invention solves the technical problem of technology and takes following technical scheme to realize, according to a kind of triethyl aluminum production technology provided by the invention, comprises hydrogenation and ethylation reaction, and wherein, it has subordinate's step:

One, the triethyl aluminum seed is quantitatively rendered in the hydrogenation still the quantitatively triethyl aluminum seed of throwing in direct and aluminium powder mixing in the still body by the preset capacity of still body liquid level; The liquid feeding end setting of quantitative discharging pipe is positioned at the liquid level line place of hollow chamber; The following liquid level capacity of the liquid feeding end of quantitative discharging pipe is through calculating the pre-grain weight of retaining;

Two, in the still body, feed hydrogen and carry out hydrogenation;

Three, hydrogenation finishes, remaining pressure in the release reaction still;

Four, in the still body, add ethene and carry out ethylation reaction;

Five, after ethylation reaction finished, the reaction of getting predetermined amount via the quantitative discharging pipe generated the Distallation systm of transferring to of thick product, the seed that the thick product of surplus amount reacts for next still.

Hydrogenation and ethylation reaction can be finished in same reactor with quantitative discharging structure thus; Do not need to dispose separately the ethylation reaction device and carry out ethylation reaction;

The present invention compared with prior art has significant advantage and beneficial effect.

By above technical scheme as can be known, the present invention has following advantage at least under the structure configuration of excellence:

The ingenious quantitative discharging structure of being provided with in this case reactor with simple structure setting and cheap manufacturing cost, is realized accurate metering output, has solved industry and has failed the quantitative discharging of fine solution and the effective problem of the original amount of control seed all the time; Omit the program that shifts seed, need not complex device such as seed measuring tank, effectively optimized production technology, simplified equipment, effectively reduced the dangerous chance in the production process.Hydrogenation and ethylation reaction can be finished in same reactor with quantitative discharging structure; Do not need to dispose separately the ethylation reaction device and carry out ethylation reaction.

The specific embodiment of the present invention is provided in detail by following examples and accompanying drawing thereof.

Description of drawings

Fig. 1 is this case charging and emptying aluminum powder control system overall structure schematic diagram;

Fig. 2 is a charging device structural representation in this case aluminium powder delivery device;

Fig. 2 a is an A-A cross-sectional view among Fig. 2;

Fig. 2 b is a B-B cross-sectional view among Fig. 2 a;

Fig. 3 is the structural representation of discharging device in this case aluminium powder delivery device;

Fig. 3 a is the structural representation of pull bar coupling assembling in Fig. 3 discharging device;

Fig. 3 b is this case discharging device overhead view face structural representation;

Fig. 3 c is that the blanking piston unit of the another embodiment of this case is configured in the structural representation in the discharging device;

Fig. 3 d is a C-C cross-sectional view among Fig. 3;

Fig. 4 is that the pull bar seal is overlooked the face structural representation in the discharging device;

Fig. 4 a is an A-A cross-sectional view among Fig. 4;

Fig. 4 b is a B-B cross-sectional view among Fig. 4;

Fig. 5 is a reactor overall structure schematic diagram;

Fig. 5 a is the quantitative discharging structural texture schematic diagram of reactor;

Fig. 6 is the schematic diagram that the reactor hexane is removed temperature, condensation, the circulatory system.

The specific embodiment

Below in conjunction with preferred embodiment, to according to the specific embodiment provided by the invention, feature and effect thereof, describe in detail as after; For simple and purpose clearly, hereinafter appropriate omission the description of known technology, in order to avoid those unnecessary details influences are to the description of the technical program.

Shown in Fig. 1-6, a kind of production equipment of triethyl aluminum comprises charging and emptying aluminum powder control system and reactor 4;

Described charging and emptying aluminum powder control system is made up of aluminium powder delivery device and control module 6, and described aluminium powder delivery device comprises that charging device 1 and discharging device 2 constitute, and this charging and emptying aluminum powder control system is delivered aluminium powder by the charging aperture 44 of reactor 4 to reactor;

Described charging device 1 is used for the nitrogen replacement of aluminium powder, shown in Fig. 2, Fig. 2 a, Fig. 2 b, this charging device has nitrogen replacement jar body 11, and described nitrogen replacement jar body is made of 11a of cavity portion that holds aluminium powder and the 11b of hopper portion, this described cavity of adjacency portion of hopper portion; Described hopper portion has the feed opening 110 that docks with the defeated material storage tank 21 of discharging device; End cap seal portion 12 is arranged on the aluminium powder feed end, and described aluminium powder feed end can be located at the upper position of nitrogen replacement jar body cavity portion; Described end cap seal portion 12 has jar body bead 121 and end cap 120, between end cap and jar body bead by sealing ring 124 sealings; End cap and jar body bead are fastening by the fastening unit 125 that can open and close end cap, and it is simpler that structure is set thus, the operation of being more convenient for; This fastening unit is used to allow end cap tight with jar body closure, and fastening unit can be general conventional technology, will not give unnecessary details;

The charging end of nitrogen replacement jar body, sidewall form assembly section 10, the first Pressure gauge B of portion and install by the pressure measurement port one 01 of this assembly section portion; Vacuum valve is installed by the vacuum ports 103 of this assembly section portion;

First nitrogen purging device 17 is arranged in the chamber of nitrogen replacement jar body, near the position of hopper portion, this first nitrogen purging device has delivery end 171 and blower pipe 172, this delivery end 171 is responsible for sending into nitrogen to the jar body, and this blower pipe 172 is responsible for nitrogen is blown into hopper portion; Described thus first nitrogen purging device can be finished two tasks, and the one, blow nitrogen to the jar body, the 2nd, utilize air-flow to blow off hopper portion aluminium powder;

Further, described first nitrogen purging device 17 is made up of the annular snorkel 173 of encircling jar body and blower pipe 172a, the 172b, 172c, the 172d that are communicated with annular snorkel, uniform being configured on the annular snorkel of blower pipe of default number, described blower pipe configurable number includes but not limited to 2 or 4 or 6 or 8, be illustrated as the situation of 4 blower pipe configurations, each blower pipe is constructed the identical industrialization that is more conducive to; Nitrogen delivery end 171 is configured on the annular snorkel; Nitrogen is distributed to each blower pipe uniformly by annular snorkel thus, thereby can make aluminium powder obtain more even, nitrogen protection more fully in descending course of conveying;

Further, described blower pipe 172 stretches into portion 1721 and blower pipe by blower pipe and sweeps the portion of blowing 1722 and form the connecting lever structure, this blower pipe stretches into portion 1721 and is stretched in jar body by annular snorkel, and this blower pipe stretches into portion and is communicated with annular snorkel, and nitrogen enters thus; Described blower pipe is swept the portion of blowing 1722 and is stretched into portion 1721 along blower pipe and turn tapering inclined-plane to hopper portion, form first of the tapering face can purge hopper portion thus and purge angle beta, described first to purge angle be that blower pipe is swept the angle β that the extended line f of the portion of blowing is become with the conical surface m of hopper portion; This first purging angle is set to 15-20 degree or 20-25 degree or 25-30 degree; This setting can either be better comes together in feed opening 110 with the air-flow strength of each blower pipe, can take into account the cleaning effect of each blower pipe to the conical surface of hopper portion again;

Described discharging device 2 is used to transport the aluminium powder from nitrogen replacement jar body, shown in Fig. 3, Fig. 3 a, Fig. 3 b, Fig. 3 c; This discharging device has defeated batch can body 21, and this defeated batch can body is made of hollow feeding chamber 21a and the 21b of discharge bucket portion, and hollow feeding chamber 21a is responsible for holding that aluminium powder is smooth and easy passes through, and the 21b of discharge bucket portion is positioned at this hollow feeding chamber below; The bead 21b-0 of the bead 21a-0 of hollow feeding chamber 21a and the 21b of discharge bucket portion seals fastening assembling by sealing tightening member 20 with usual way, also can be integrally formed structure;

The feed end of described defeated batch can body has the charging aperture 210 that docks with the feed opening 110 of nitrogen replacement jar body, in the defeated batch can chamber body blanking piston unit 23 is set, and is used to control the defeated material mouth 220 that opens and closes defeated batch can body;

Described blanking piston unit 23 is made of pull bar 231, drag link sleeve 232 and piston 233, described drag link sleeve 232 is installed in the hollow feeding chamber of defeated batch can body by fixed

support group

234a, 234b, 234c, drag link sleeve one end is fixed in the position of the pull bar pilot hole 213 of defeated batch can bodies top, this drag link sleeve has the vertically upper and lower drag link sleeve through hole 2320 of pulling freely of appearance pull bar, this drag link sleeve through hole keeps concentric with the pull bar pilot hole 213 of defeated batch can body, draws to guarantee that pull bar can be stretched freely in narrower and small aperture; Drag link sleeve is terminal by the second fixed support 234b or the 3rd fixed support 234c location; The pull bar pilot hole place of defeated batch can body is by pull bar seal 230 assembling pull bars 231, and the pull bar seal is responsible for when lifting pull bar, still can keep sealing in the tank body;

Second nitrogen purging device 27 is arranged in the chamber of the hollow feeding chamber of failing the batch can body, near the position of discharge bucket portion;

23 1 kinds of embodiments of the blanking piston unit that this case provides are shown in Fig. 3 c, and described drag link sleeve is terminal by the 3rd fixed support 234c location;

The internal diameter of the thickness of the tank body degree of depth and pull bar, pull bar sheath should mate adaptation mutually, to avoid because of faults such as meticulous, the long appearance of pull bar are not straight or fracture, therefore the vertical size of tank body big (tank body is deep), relatively under the thinner again situation of pull bar, this case provides a kind of blanking piston unit 23 of embodiment again, as shown in Figure 3;

Described the 3rd fixed support 234c is arranged on the discharge bucket position, limit pull rod cover 232a is fixed among the 21b of discharge bucket portion by the 3rd fixed support 234c, pull bar 231 stretches out by drag link sleeve 232, the end of this pull bar is connected with the second pull bar 231a by pull bar coupling assembling 239, described pull bar coupling assembling is made up of parent part 2391 and component 2392, parent part and pull bar or second pull bar install, the component and second pull bar or pull bar install, described parent part department of assembly forms parent part limiting stand 2391a, can limit the stroke that pull bar makes progress; Described component department of assembly forms component limiting stand 2392a, can limit the downward stroke of second pull bar; Bottom 232a-1 by limit pull rod cover 232a forms the first default spacing L1 to the defeated material mouthful end 220-1; Bottom 232-1 by drag link sleeve 232 forms the second default spacing L2 to the limit pull rod cover bottom 232a-1, and the described first default spacing L1 is equivalent to the length overall L3 that the second default spacing L2 deducts limit pull rod cover and pull bar coupling assembling; Structure makes piston only limit the preset range that lifts hopper thus, is convenient to blanking control; Structure has also formed another blanking piston unit thus;

Further, the extended line that described blower pipe is swept the portion of blowing and the joint d that conical surface became of discharge bucket portion be a little less than limit pull rod cover bottom 232a-1 so that piston when mentioning air-flow discharging opening is formed more effective purging;

Or the extended line that described blower pipe is swept the portion of blowing and the joint d that conical surface became of discharge bucket portion are a little less than drag link sleeve bottom 2320-1, shown in Fig. 3 c; So that piston when mentioning air-flow discharging opening is formed more effective purging;

The second Pressure gauge B ' installs by defeated batch can bodies top pressure measurement port 201;

The vacuum valve (not shown) is installed by defeated batch can bodies top vacuum ports 203;

Pull bar 231 is installed in the drag link sleeve 232, and an end of pull bar has the link 2310 that is connected with second power source 72, and described second power source includes but not limited to cylinder; Second power source 72 can be installed by second bearing; The other end of pull bar has the assembling end 2311 of assembling piston 233; Described piston 233 can be the defeated material mouthful cock body of the defeated batch can body of blocking of arbitrary shape;

Preferred piston is set to round table-like, and this piston has the external conical surface that combines with the circular cone inner surface coupling of hopper portion, and promptly the round platform tapering of piston is consistent with hopper portion tapering; First bottom surface 2331 of piston is towards mouthful installation of defeated material, and first bottom surface of piston is the one side of round platform than minor diameter, and piston first bottom surface is provided with the straight warp of defeated material mouth that diameter is slightly less than defeated batch can body, and sealing effectiveness is better; Second bottom surface 2332 of piston is the larger-diameter one side of round platform, and during the piston shutoff, second bottom surface just forms the bottom of hopper;

Structure forms when pull bar is advanced downwards thus, and along with piston is descending gradually, the piston shutoff is just all the more tight; And when pull bar was upwards advanced, along with piston is up gradually, the round platform of piston structure was more conducive to compacted aluminium powder and is loosened;

Further, defeated batch can bodies top is fixed on the top of drag link sleeve as previously mentioned, drag link sleeve is terminal by the second fixed support 234b or the 3rd fixed support 234c location, in addition, further the first fixed support 234a is set at the drag link sleeve middle part, add strong fix, in defeated batch can body, keep vertically not curved to guarantee drag link sleeve, and safety, firm;

Further, shown in Fig. 3, Fig. 3 c, second nitrogen purging device 27 is identical with first nitrogen purging device, 17 structures, promptly, this second nitrogen purging device has to be responsible for sending into the delivery end 271 of nitrogen and nitrogen being blown into the blower pipe 272 of discharge bucket portion to the jar body, second nitrogen purging device also can be finished two tasks, and the one, blow protective gas to the jar body, the 2nd, utilize air-flow to blow off hopper portion aluminium powder;

The second fixed support 234b is arranged on the position on second nitrogen purging device 27, the dismounting of convenient second nitrogen purging device, the maintenance of being more convenient for;

Further, described second nitrogen purging device is made up of the annular snorkel 273 of encircling jar body and blower pipe 272a, the 272b, 272c, the 272d that are communicated with annular snorkel, uniform being configured on the annular snorkel of blower pipe of default number, the blower pipe configuration includes but not limited to 2 or 4 or 6 or 8; Nitrogen delivery end 271 is configured on the annular snorkel, and nitrogen is distributed to each blower pipe uniformly by annular snorkel thus, thereby can make aluminium powder obtain more even, nitrogen protection more fully in descending course of conveying;

Further, this blower pipe 272 stretches into portion 2721 and blower pipe by blower pipe and sweeps the portion of blowing 2722 and form the connecting lever structure, described blower pipe stretches into portion 2721 and is stretched in jar body by annular snorkel, and this blower pipe stretches into portion and also is communicated with annular snorkel, and nitrogen enters thus; This blower pipe is swept the portion of blowing and is turned the second purging angle beta that forms the tapering face that can purge hopper portion to the tapering inclined-plane of discharge bucket portion along the blower pipe portion of stretching into ', described second to purge angle be that blower pipe is swept the angle that the extended line f ' of the portion of blowing is become with the conical surface m ' of discharge bucket portion, this second purging angle is set to 15-20 degree or 20-25 degree or 25-30 degree, this setting can either function better come together in discharging opening 220 with the air-flow of each blower pipe, can take into account the cleaning effect of each blower pipe to the conical surface of discharge bucket portion again;

Further, described pull bar seal 230 is made up of base body 2301, base seat lid 2302 and potted component 2303, the base body through hole 23011 that base body has the appearance pull bar to pass through, and this base body through hole can be over against drag link sleeve through hole 2320; Base body one end is packed in defeated batch can bodies top, and the base body other end is a pedestal assembling end 23013; In the pedestal assembled end cavity 23012 of ccontaining potted component 2303 is set, this cavity is the reaming of abuts seat body through hole, and described potted component 2303 can be O-ring seal or other existing airtight and watertight padding; Base seat lid 2302 has holds pull bar base seat lid through hole 23021 that passes through and the base seat lid assembled end 23023 that can combine with pedestal assembled end 23013 couplings, in the base seat lid assembled end boss 23022 of the potted component cavity 23012 that can stretch into the pedestal assembled end is set, this boss is responsible for compressing potted component 2303; Base seat lid and pedestal assembling end combines, and is fastening by securing member by fastener hole 23020, thus with the potted component shutoff in the cavity of base body, form the pull bar seal;

Described control module 6 is made up of nitrogen control module 63, pressure sensing cell 621, B, 622, B ' and vacuum control unit 61;

Described nitrogen control module 63 is made up of the first nitrogen valve gate cell 631,631a and the second nitrogen valve gate cell 632, described first nitrogen valve gate cell and the configuration in parallel of the second nitrogen valve gate cell; This first nitrogen valve gate cell is configured between the nitrogen replacement jar body 11 of source nitrogen N and charging device 1; The second nitrogen valve gate cell 632 is configured between the defeated batch can body 21 of source nitrogen N and discharging device 2; The described first nitrogen valve gate cell can be nitrogen valve 631, the 631a of two parallel connections, also can be a nitrogen valve;

Described pressure sensing cell has and is installed in the first pressure vacuum gauge B on the nitrogen replacement jar body in the charging device and is installed in the second pressure vacuum gauge B ' on the defeated batch can body in the discharging device, the first pressure vacuum gauge B is by 621 controls of first instrument valve, the second pressure vacuum gauge B ' constitutes pressure sensing cell thus by 622 controls of second instrument valve;

Described vacuum control unit 61 is made up of first vacuum control valve 611 and second vacuum control valve 612, the configuration in parallel of this first vacuum control valve and second vacuum control valve, this first vacuum control valve 611 is configured between the nitrogen replacement jar body 11 of vavuum pump and charging device; Second vacuum control valve 612 is configured between the defeated batch can body 21 of vavuum pump and discharging device;

Nitrogen control valve, pressure-control valve and vacuum valve can dispose commercially available product, will not give unnecessary details;

First switching that feeds intake valve 18 between first cylinder 71 control charging device feed openings 110 and the discharging device charging aperture 210; First cylinder 71 is installed by first support 710;

Second cylinder 72 opens and closes by the defeated material mouth 220 of blanking piston unit 23 control discharging devices of discharging device and the one-level between the reactor charging aperture 44; Second cylinder 72 is installed by second support 720; This first support 710, second support 720 are packed in respectively on the discharging device, and system architecture is compacter, the control better effects if;

Discharge valve group 28 is installed in reactor charging aperture 44 places, and this discharge valve group is set to high pressure valve, when valve closing, and the pressure from following preface reactor capable of blocking; This discharge valve group 28 is connected in series with second discharge gate 282 by first discharge gate 281 and constitutes, and forms safer double valve protection, forms the another level control that opens and closes between defeated material mouth 220 of discharging device and the reactor charging aperture 44;

Discharging device allows and fails the pressure of the pressure of batch can chamber body greater than the reactor inner chamber when reactor feed, and when discharge valve group 28 was opened, aluminium powder was pressed into reactor smoothly under air pressure helps; Feed intake after the end, close discharge valve group 28.

Discharge gate can be commercially available high pressure valve, and cylinder is also commercially available, will not give unnecessary details;

In defeated material mouth 220 places of discharging device, the position of discharge valve group 28, configuration emptying valve 29; The described first emptying valve is used to prevent that reason first valve 18 that feeds intake from leaking the situation that causes gas to return scurrying; The described second emptying valve is in opening when reactor is worked, be used to prevent that 28 leakages of reason discharge valve group from causing gases at high pressure to scurry into the interior situation of charging device; The emptying valve is commercially available air bleeding valve, will not give unnecessary details;

Carry out charging and emptying aluminum powder by described charging and emptying aluminum powder control system:

The first step drops into aluminium powder, airtight nitrogen replacement jar body; Feed end by nitrogen replacement jar body drops into aluminium powder in charging device 1, and makes that by end cap seal portion 12 nitrogen replacement jar body is airtight;

Second step vacuumized, and allowed the intrinsic operating pressure of nitrogen replacement jar be lower than standard atmospheric pressure; Open first vacuum valve 611, the first instrument valve 621 of nitrogen replacement jar body is in normally open all the time, by the first Pressure gauge B pressure measurement, when presenting negative pressure value in the nitrogen replacement jar body of charging device, closes first vacuum valve;

The 3rd step, in nitrogen replacement jar body, carry nitrogen for the first time, by the first Pressure gauge B pressure measurement, when presenting normal pressure in the nitrogen replacement jar body of charging device, close first nitrogen valve 631;

The 4th step repeated the operation of second step, allowed the intrinsic operating pressure of nitrogen replacement jar be lower than standard atmospheric pressure; Open first vacuum valve 611,, when presenting negative pressure value in the nitrogen replacement jar body of charging device, close first vacuum valve by the first Pressure gauge B pressure measurement;

The 5th step, in nitrogen replacement jar body, carry nitrogen for the second time, pressure measurement once more when arriving preset pressure value in the nitrogen replacement jar body, is closed first nitrogen valve 631;

Described nitrogen can be carried by first nitrogen purging device 17, and also available other known technology is carried;

Described preset pressure value is provided with by existing nitrogen replacement knowledge, includes but not limited to 0.4 ± 0.2 MPa, will not give unnecessary details; Described nitrogen replacement includes but not limited to finish for 1 time or 2 times or 3 times, and the displacement number of times can be a prior art, will not give unnecessary details;

So far finished the nitrogen replacement of aluminium powder;

In the 6th step, allow be vacuum state in the defeated batch can body of discharging device; Open second vacuum valve 612 and be evacuated to vacuum, the second instrument valve 622 of defeated batch can body is in normally open all the time, by the second Pressure gauge B ' pressure measurement, when presenting vacuum in the defeated batch can body of discharging device, closes second vacuum valve 612;

In the 7th step, the aluminium powder safety of finishing nitrogen replacement is moved in the defeated batch can body 21 of discharging device; Open the first nitrogen valve gate cell 631a,, provide protective gas and pressure aluminium powder by first nitrogen purging device, 17 supplying nitrogens; Simultaneously open between control charging device and the discharging device first valve 18 that feeds intake by first power source 71, described first power source includes but not limited to cylinder; At this moment, after the defeated batch can body of the discharging device of vacuum shape and the nitrogen replacement jar body of barotropic state are communicated with, aluminium powder enters defeated batch can body under the effect of positive and negative pressure reduction, by the blowing of first nitrogen purging device 17, finish the aluminium powder of nitrogen replacement and delivered in the defeated batch can body of discharging device by safety again; Close first valve 18 that feeds intake and make that the defeated batch can body of discharging device is airtight;

Finished the safe transfer of displacement back aluminium powder thus;

In the 8th step, supplying nitrogen in defeated batch can body is opened the second nitrogen valve gate cell 632, by the second Pressure gauge B ' pressure measurement, when reaching preset pressure value in the defeated batch can body of discharging device, closes the second nitrogen valve gate cell 632;

Described nitrogen can be carried by second nitrogen purging device 27, and also available other known technology is carried;

Described preset pressure value is provided with by existing nitrogen replacement knowledge, includes but not limited to 0.4 ± 0.2 MPa,

The 9th step, open the passage between defeated material mouth 220 of discharging device and the reactor charging aperture 44, carry the aluminium powder material to reactor; After confirming to be responsible for 29 one-tenth closed conditions of emptying valve of emptying residual air, open discharge valve group 28; Simultaneously lift piston, open " door " between defeated material of discharging device mouthfuls 220 and the reactor charging aperture 44 by the blanking piston unit 23 of second cylinder 72 by discharging device; At this moment, aluminium powder is headed on by air pressure and enters defeated batch can body under pressure, again by the blowing of second nitrogen purging device 27, and the aluminium powder material is thrown in work from realization that can safety to reactor;

The tenth step, close discharge valve group 28, the piston of let-down blanking piston unit is closed " door " between defeated material mouth of discharging device and the reactor charging aperture, opens atmospheric valve 29.

Thus, this case charging and emptying aluminum powder control system can make aluminium powder more optimize in the displacement and the technology of throwing in link, operate saferly, easy, and system energy consumption is lower, and the structure setting of this case more helps docking with electronic control part, the realization Electronic Control; Described aluminium powder delivery device is equally applicable to the material identical with aluminium powder character and throws in.

Further, on the nitrogen replacement jar body 11 of charging device 1, hopper wall vibrator (not shown) is installed; On the defeated batch can body 21 of discharging device 2, hopper wall vibrator (not shown) is installed also, is used for the aluminium powder that more effective removing is attached to jar body; Described hopper wall vibrator prior art will not be given unnecessary details, and can select the commercially available product configuration for use;

Further, the 11b of hopper portion at charging device nitrogen replacement jar body installs stuff level switch (not shown); On the 21b of discharge bucket portion of the defeated batch can body of discharging device, stuff level switch (not shown) is installed also, is used to judge whether aluminium powder is thoroughly shifted; Stuff level switch claims level switch again, belongs to level controller, and it can detect the variation of testee in production equipment accurately, is prior art, will not give unnecessary details; Described stuff level switch includes but not limited to that tuning-fork type, condenser type also can make blocking rotary type or other forms, and switch output signal after the thorough emptying of aluminium powder can use on-site signal, also can use remote transfer signal.

Reactor 4 has the quantitative discharging structure, described reactor comprises still body 41 and agitator 42, this agitator 42 is driven by motor M, have reactor charging aperture 44 on the described reactor 4, drop into thus through displacement back aluminium powder, wherein, described still body has closed hollow chamber 410, this hollow chamber 410 can be the cylinder die cavity, and the upper cover 411 of still body can be that dome head also can be an ellipsoidal head, and low head 412 is a dome head; Hollow chamber and upper cover, low head form closed still body jointly; Have nitrogen delivery end 43 on the still body, the nitrogen tube 8 of valve 81 is equipped with in the nitrogen delivery end configuration of still body; This still body is made as dosing container, preset diameters is D in the hollow chamber of still body, the liquid level line a that satisfies default liquid level H is set in the still body, the liquid level volume that can preset the still body by default liquid level H value and default still body hollow chamber inside diameter D value is set thus, and described liquid level volume is meant by reactor bottom this body bulk of still to liquid level line a; Can determine the default grain weight that to retain by pre-determining the liquid level volume thus;

Quantitative discharging pipe 9 is arranged in the hollow chamber of still body, described quantitative discharging pipe vertically stretches in the hollow chamber, the liquid feeding end 90 of quantitative discharging pipe is provided with the liquid level line a place that is positioned at hollow chamber, the outlet end 92 of quantitative discharging pipe stretches out the still body and docks with the reservoir (not shown) of external shown liquid measure, and quantitative discharging pipe outlet end opens and closes by valve 91 controls; Described quantitative discharging pipe has preset length and internal diameter;

Thus, form reactor with quantitative discharging structure; During operation, triethyl aluminum seed and aluminium powder are directly mixed in reactor, described triethyl aluminum seed input amount is the capacity of still body liquid level a;

Can in still, feed hydrogen with the prior art means and carry out hydrogenation; Because of the liquid level capacity of quantitative discharging pipe liquid feeding end below 90 in the reactor is through calculating the pre-grain weight of retaining, when dropping into aluminium powder through over hydrogenation, behind the ethylation reaction, when the liquid level of reactant liquor is elevated to the second liquid level h, exceed the default liquid level line a at quantitative discharging pipe liquid feeding end 90 places, therefore during discharging, under the nitrogen pressure effect, reactant liquor in the still shifts to reservoir via discharge nozzle, when liquid level is lower than the discharge nozzle liquid feeding end, liquid is no longer discharged, can effectively control grain weight in the still thus and remain constantly, load can be shown by the liquid level gauge that is arranged on the reservoir.

Hydrogenation adds ethene with the prior art means again and carries out ethylation reaction after finishing in still; After ethylation reaction finishes, get the Distallation systm of transferring to of the thick product that the reaction of predetermined amount generates (can be reaction give birth to thick product 15% ± 5) by quantitative discharging pipe 9; Remaining thick product is stayed (surplus can be that the living thick product of reaction is 85% ± 5) in the reactor, for seed is made in next still reaction;

Simple thus structure is provided with, the technical purpose that solves quantitative discharging and the original amount of effective control seed cheap for manufacturing cost; The industry common recognition, how a the dangerous material production equipment is how a complicated with regard to hidden danger, so this case is with very simple and direct structure, effectively shorten production procedure, optimized operation, saved the time of reciprocal transfer seed, reduce the danger coefficient in the production process, shown significant technological progress;

Further, the configuration hexane is removed thermotectonics 46 in the reactor 4; It is one deck or two-layer coil pipe that described hexane is removed thermotectonics, this coil pipe spirals in the hollow chamber of still body by support 460, described first coil pipe 461 is twined by hollow siphunculus spiral and forms, and this first coil pipe is that mandrel is installed in the hollow chamber of still body with support 460; This first coil pipe input is connected with the output of hexane storage tank A; The output of hexane storage tank can be connected with the first coil pipe input via circulating pump A-1; Between the first coil pipe input and the circulating pump hexane control valve 52 is set; This first coil pipe output is connected with the input of hexane storage tank A, and the input of hexane storage tank can be connected with the first coil pipe output via hexane condenser A-2; The spiral coil 4610 of first coil pipe equates with default spacing between the spiral coil, forms better heat absorption effect;

Second coil pipe is arranged between first coil pipe and the still body hollow chamber inwall, and this second coil pipe 462 is identical with first coil pipe, 461 structures; Two-layer coil pipe is provided with import and outlet respectively, imports and exports in parallel the use for two, and purpose is to increase the effective heat exchange area; The second coil pipe input is connected with the output of hexane storage tank A; This second coil pipe output is connected with the input of hexane storage tank A, has hexane control valve 52 between the second coil pipe input and the circulating pump, and first, second coil pipe can be shared a hexane control valve certainly, also can divide usefulness separately, all belongs to the design and conceives scope; The spiral coil of second coil pipe equates with default spacing between the spiral coil; The axle center of support is left and is held the space that the quantitative discharging pipe vertically stretched into wherein and do not influence agitator work;

The structure of two-layer coil pipe preferably, first coil pipe 461 is in parallel with the hexane stream of second coil pipe 462, is divided into two-way from the hexane liquid of hexane storage tank and carries, and one the tunnel supplies first coil pipe 461, enter from the input of first coil pipe, get rid of from the output of first coil pipe; Second coil pipe 462 is supplied on another road, enters from the input of second coil pipe, gets rid of from the output of second coil pipe; Form the structure of two-layer coil pipe stream dispensing in parallel hexane thus, can more effective raising remove the thermal efficiency;

When hexane when circulating pump, control valve enter into the coil pipe of reactor, heated by the temperature of still body internal reaction deposits yields, and then vaporization, hexane in the coil pipe is absorbing reaction heat by liquid phase in the conversion process of gas phase, reach hexane and remove the technique effect of heat, hexane after the vaporization, earlier through the hexane condenser condenses, the liquid that the condensation row becomes flows back to the hexane storage tank via the coil pipe output.Circulating pump is meant the circulate pump of utilization of hexane liquid.

Further, add cover 47 and be sleeved on the still body outer wall, be responsible for helping reactor to heat up; The described cover that adds has a hollow sandwich, and this adds cover and includes but not limited to annulus, and this adds and can hold conduction oil in the interlayer of cover and cycle through, and this adds cover and has conduction oil input 471 and conduction oil output 472; This conduction oil input 471 that adds cover is provided with conduction oil control valve 51;

Further, reactor temperature element 49 is installed in the still body, and the external part of reactor temperature element is connected with dividing process control adjuster 5; Divide process control adjuster 5 one ends to be connected with reactor temperature element 49, the other end is told two-way, and one the tunnel is connected with conduction oil control valve 51; Another road is connected with hexane control valve 52; This minute process control adjuster is responsible for controlling the temperature of reactor; Temperature element and branch process control adjuster can be the commercially available prod, will not give unnecessary details; Thus, reactor can utilize the conduction oil that adds circulation in the cover to heat up;

Divide the configuration of process control adjuster can realize the adjustment of reactor is controlled.

Claims

1. the reactor with quantitative discharging structure comprises still body (41), it is characterized in that described still body forms container jointly by hollow chamber and upper cover, low head; Preset diameters in the hollow chamber of this still body is provided with the liquid level line that satisfies default liquid level and forms the quantitative structure of energy in the still body;

Quantitative discharging pipe (9) is arranged in the hollow chamber of still body, and the liquid feeding end of quantitative discharging pipe (90) setting is positioned at the liquid level line place of hollow chamber, and described quantitative discharging pipe has preset length and internal diameter.

2. the reactor with quantitative discharging structure as claimed in claim 1 is characterized in that, described quantitative discharging pipe outlet end opens and closes by valve (91) control; The outlet end of described quantitative discharging pipe (92) stretches out the still body and docks with external reservoir.

3. as described in claim 2, have the reactor that quantitative discharging is constructed, it is characterized in that the hollow chamber of described still body (410) is the cylinder die cavity.

4. the reactor with quantitative discharging structure as claimed in claim 3 is characterized in that the upper cover (411) of the still body of described still body is dome head or ellipsoidal head, and low head (412) is an ellipsoidal head.

5. the reactor with quantitative discharging structure as claimed in claim 4 is characterized in that having nitrogen delivery end (43) on the described still body, and the nitrogen tube (8) of valve (81) is equipped with in the nitrogen delivery end configuration of still body.

6. the reactor with quantitative discharging structure as claimed in claim 5 is characterized in that described quantitative discharging pipe vertically stretches in the hollow chamber; Have reactor charging aperture (44) on the described reactor, drop into thus through displacement back aluminium powder.

7. a triethyl aluminum production equipment comprises reactor, and this reactor has still body and agitator, it is characterized in that, described still body forms container jointly by hollow chamber and upper cover, low head; Preset diameters in the hollow chamber of this still body is provided with the liquid level line that satisfies default liquid level and forms the quantitative structure of energy in the still body; Quantitative discharging pipe (9) is arranged in the hollow chamber of still body, and the liquid feeding end of quantitative discharging pipe (90) setting is positioned at the liquid level line place of hollow chamber, and described quantitative discharging pipe has preset length and internal diameter.

8. triethyl aluminum production equipment as claimed in claim 7 is characterized in that, described quantitative discharging pipe outlet end opens and closes by valve (91) control; The outlet end of described quantitative discharging pipe (92) stretches out the still body and docks with external reservoir; Have nitrogen delivery end (43) on the described still body, the nitrogen tube (8) of valve (81) is equipped with in the nitrogen delivery end configuration of still body.

9. as triethyl aluminum production equipment as described in the claim 8, it is characterized in that the hollow chamber of described still body (410) is the cylinder die cavity; The upper cover of described still body (411) is dome head or ellipsoidal head, and low head (412) is a dome head.

10. triethyl aluminum production equipment as claimed in claim 9 is characterized in that, described quantitative discharging pipe vertically stretches in the hollow chamber; Have reactor charging aperture (44) on the described reactor, drop into thus through displacement back aluminium powder.

11. a triethyl aluminum production technology comprises hydrogenation and ethylation reaction, it is characterized in that, it has subordinate's step:

One, the triethyl aluminum seed is quantitatively rendered in the reactor with quantitative discharging structure the quantitatively triethyl aluminum seed of throwing in direct and aluminium powder mixing in the still body by the preset capacity of still body liquid level; The liquid feeding end setting of quantitative discharging pipe is positioned at the liquid level line place of hollow chamber; The following liquid level capacity of the liquid feeding end of quantitative discharging pipe is through calculating the pre-grain weight of retaining;

Two, in the still body, feed hydrogen and carry out hydrogenation;

Four, in the still body, add ethene and carry out ethylation reaction;