CN103073593A - Reaction device for fully hermetically producing azamethiphos - Google Patents
Reaction device for fully hermetically producing azamethiphos Download PDFInfo
- Publication number
- CN103073593A CN103073593A CN201210596230XA CN201210596230A CN103073593A CN 103073593 A CN103073593 A CN 103073593A CN 201210596230X A CN201210596230X A CN 201210596230XA CN 201210596230 A CN201210596230 A CN 201210596230A CN 103073593 A CN103073593 A CN 103073593A
- Authority
- CN
- China
- Prior art keywords
- storage tank
- reaction
- communicated
- reaction chamber
- hermetically sealed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
Abstract
The invention provides a reaction device for fully hermetically producing azamethiphos, which includes a first reaction unit, a second reaction unit and a third reaction unit, wherein the first reaction unit includes a rotational-flow kettle, an oxazole [4,5-b] pyridine-2(3H) ketone storage tank, an N,N-dimethylformamide storage tank, a paraformaldehyde storage tank and a thionyl chloride storage tank, wherein the first reaction unit includes a first powder-liquid mixing pump; the first powder-liquid mixing pump includes a first inlet and a first outlet; the oxazole [4,5-b] pyridine-2(3H) ketone storage tank, the N,N-dimethylformamide storage tank and the paraformaldehyde storage tank are communicated with the first inlet; the first outlet is communicated with the rotational-flow kettle; the rotational-flow kettle includes a first main body; the first main body is hollow and forms a first reaction chamber; and the first reaction chamber is an inverted cone structure. The reaction device provided by the invention radically avoids harmful gas leakage and facilitates the environmental protection.
Description
Technical field
The present invention relates to a kind of equipment for the production of methylpyridine phosphorus, particularly a kind of reaction unit that can hermetically sealed production methylpyridine phosphorus.
Background technology
Methylpyridine phosphorus has another name called first base pyrrole Evil phosphorus, is a kind of good sterilant, chemistry S-[6-chloro-oxazole by name (4,5-b) pyridine-2 (3 hydrogen)-ketone group-methyl]-O, O-dimethyl sulphide substituted phosphate, molecular formula is C
9H
10ClN
2O
5PS, molecular weight is for 324.68.Methylpyridine phosphorus is a kind of good miticide, have insecticidal activity concurrently, belong to and tagging and the stomach toxicity medicament, long-lasting is good, and insecticidal spectrum is wide, can be used for cotton, fruit tree, vegetables and livestock, public health and family, prevent and treat various mite classes and stupid, aphid, leaf lice, small kernel-eating insect, colorado potato bug and fly, cockroach etc., this agent is to people and animals' low toxicity, the safe medicament that belongs to efficient, low toxicity, low residue, so methylpyridine phosphorus becomes the organic phosphorous insecticide of the World Health Organization (WHO) recommendation.Because make emulsion, sprays, pulvis, wettable powder and sol particle in this methylpyridine phosphorus, therefore be specially adapted to prevent and treat the insects such as fly again.
Conventional picoline production of phosphorus mainly comprises three steps: step 1 is raw material with oxazole [4,5-b] pyridine-2 (3H) ketone, then generates a kind of intermediate side chain chloro-product of methylpyridine phosphorus through nucleophilic chloro, methylolation; Step 2 with dimethylphosphite and sulfur reaction, under the effect of sodium methylate, generates the another kind of intermediate thiophosphatephosphorothioate of methylpyridine phosphorus; Step 3 is at last by side chain chloro-product and the further synthesizing methyl pyridine of thiophosphoric acid ester condensation reaction phosphorus.Please refer to Fig. 1, be the existing module diagram of producing the device of described methylpyridine phosphorus, described device comprises the first reaction member 100, the second reaction members 200, and the 3rd reaction member 300 that is connected with described first, second reaction member 100,200.At described the first reaction member 100 for the production of intermediate product side chain chloro-product.The second reaction member 200 is for the production of the intermediate product thiophosphatephosphorothioate.Above-mentioned two kinds of intermediate products are that side chain chloro-product and thiophosphatephosphorothioate enter the 3rd reaction member 300 at last, produce the finished product methylpyridine phosphorus.
See also Fig. 2, be the structural representation of traditional the first reaction member 100, described the first reaction member 100 comprises one first reactor 10, a plurality of the first storage tank 20 that communicates with this first reactor 10, a gas-holder 30 and waste gas withdrawing can 40 and one first whipping appts 50.Described the first storage tank 20 comprises an oxazole [4,5-b] pyridine-2 (3H) ketone storage tank 21, one DMFs (DMF) storage tank 22, a Paraformaldehyde 96 storage tank 23 and monochlor(in)ate sulfoxide storage tank 24.Described gas-holder 30 stores chlorine, when reaction, by a ventpipe (not shown) gas is imported the first reactor 10.Institute's waste gas is stated 40 waste gas that produce by the recovery tube (not shown) recovery reaction that extend in the first reactor 10 of withdrawing can.Described the first whipping appts 50 comprises the first stirring rod 51 that extends in the first reactor 10.When reaction, the raw materials such as oxazole pyridone, DMF (DMF), Paraformaldehyde 96 and sulfur oxychloride are added the first reactor 10 according to a graded, and pass into chlorine, while stirring reaction.See also Fig. 3, be the structural representation of traditional the second reaction member 200, described the second reaction member 200 comprises one second reactor 210, a plurality of the second storage tank 220 that communicates with this second reactor 210 and one second whipping appts 230.Described the second storage tank 220 comprises a sulphur storage tank 221, a methyl alcohol storage tank 222, a sodium methylate storage tank 223 and a dimethylphosphite storage tank 224.Described the second whipping appts 230 comprises the second stirring rod 231 that extends in the second reactor 210.When reaction, the raw materials such as sulphur storage tank 221, methyl alcohol storage tank 222, sodium methylate storage tank 223 and dimethylphosphite 224 are added the second reactor 210 according to a graded, while stirring reaction.When treating that back treats that the back reaction is finished, add again new raw material.
Yet, when described the first reaction member 100 is produced described side chain chloro-product, being difficult to accomplish to seal fully, the situations such as run, drip, leak appear in process of production easily.And the gas (such as hydrogenchloride) that described side chain chloro-product produces in production process all has stronger toxicity and corrodibility, leaks out easy production environment and the human body health of affecting, and is unfavorable for environment protection.Reason has two: the first, because described oxazole [4,5-b] pyridine-2 (3H) ketone is solid feed, when feeding in raw material, all need hand-fed, and hand-fed must be opened described the first reactor 10 at every turn, affects the sealing of described the first reactor 10.Second, because described the first reactor 10 has the first whipping appts 50, seal point between the first whipping appts 50 and the first reactor 10 is produced raw material such as sulfur oxychloride and the gas that produces such as the corrosion of hydrogenchloride of described side chain chloro-product easily in reaction, affect the sealing of the first reactor 10, become the hidden danger point that to stop poisonous gas leakage.
Summary of the invention
In view of this, be necessary to provide a kind of reaction unit that is used for hermetically sealed production methylpyridine phosphorus that whole production environment cleans that is beneficial to, to overcome above-mentioned deficiency.
The invention provides a kind of reaction unit for hermetically sealed production methylpyridine phosphorus, it comprises one first reaction member, one second reaction member and the 3rd reaction member that is communicated with respectively with described first, second reaction member.This first reaction member comprises an eddy flow still, an oxazole [4,5-b] pyridine-2 (3H) ketone storage tank, a DMF storage tank, a Paraformaldehyde 96 storage tank, monochlor(in)ate sulfoxide storage tank, a gas-holder and a waste gas withdrawing can.Described sulfur oxychloride storage tank is communicated with described eddy flow still, and described gas-holder and waste gas withdrawing can all are communicated with described eddy flow still.Described the first reaction member further comprises one first powder liquid mixing pump, and described the first powder liquid mixing pump comprises one first import and one first outlet.Described oxazole [4,5-b] pyridine-2 (3H) ketone storage tank, DMF storage tank and Paraformaldehyde 96 storage tank are communicated with described the first import, and described the first outlet is communicated with described eddy flow still.Described eddy flow still comprises a first noumenon, and described the first noumenon hollow arranges and forms one first reaction chamber, and described the first reaction chamber is a conical structure that stands upside down.Described eddy flow still comprises the first opening for feed and the first discharge port on the sidewall that is separately positioned on described the first noumenon.This first opening for feed is near the larger side of round tangent plane diameter of described the first reaction chamber.This first discharge port is near the less side of round tangent plane diameter of described the first reaction chamber, and described the first opening for feed is provided with a shower nozzle.Defining the direction that the diameter of the round tangent plane of described the first reaction chamber in axial direction reduces gradually is first direction, and the axial direction due of described shower nozzle and described first direction have an angle.
The axial direction due of described the first discharge port overlaps with the axial direction due of the first reaction chamber.
The axial direction due of described shower nozzle and the angle of described first direction are 90 degree.
The axial direction due of described shower nozzle and the internal surface of described the first noumenon are tangent.
Described shower nozzle is hollow tubular structure.
Described eddy flow still further comprises the passage of the sidewall top that is arranged on described the first noumenon, described passage near the larger side of the round tangent plane diameter of the first reaction chamber and be communicated with the waste gas withdrawing can.
Described the second reaction member comprises a reactor, a sulphur storage tank, a methyl alcohol storage tank, a sodium methylate storage tank, a dimethylphosphite storage tank and a whipping appts.Described methyl alcohol storage tank, sodium methylate storage tank and dimethylphosphite storage tank are communicated with described reactor.Described whipping appts comprises the stirring rod that extends in the reactor.
Described the second reaction member further comprises one second powder liquid mixing pump, and described the second powder liquid mixing pump comprises one second import and one second outlet.Described sulphur storage tank is communicated with described the second import, and described the second outlet is communicated with described reactor.
Described reactor comprises one second body, and described the second body hollow arranges and forms one second reaction chamber, described the second reaction chamber be shaped as tubbiness.
Described stirring rod extends in described the second body, the dead in line of the axis of described stirring rod and the second body.
Compared to prior art, in the device of production methylpyridine phosphorus provided by the present invention, described the first reaction member utilizes by the first powder liquid mixing pump that the inwall along this eddy flow still flows down in the pressure directive eddy flow still after with the solid-liquid two-phase raw material Uniform Dispersion in the storing pipe, and nationality is arranged by the gradient of the first reaction chamber of described eddy flow still and the position of shower nozzle, descend so that described raw material can be at the inwall of this first reaction chamber spiral, delay described raw material along time that the inwall of described the first reaction chamber flows down.Be appreciated that by introducing the first powder liquid mixing pump and have the eddy flow still of taper the first reaction chamber, the one, make the first reaction member need not hand-fed, all reinforced processes all can be carried out under sealed environment; The 2nd, by the first powder liquid mixing pump with the raw material Uniform Dispersion of solid-liquid two-phase and raw material spiral in the first reaction chamber is stayed; increase the duration of contact between chlorine and the raw material; can make raw material reach the effect of stirring; thereby can accomplish in the eddy flow still without whipping appts; fundamentally stop poisonous gas leakage, be conducive to environment protection.To sum up; the device of production methylpyridine phosphorus provided by the present invention; because described side chain chloro-product can be produced by the eddy flow still under hermetically sealed environment; therefore, described eddy flow still can be accomplished to seal fully when producing described side chain chloro-product; the situations such as run, drip, leak can not appear in process of production; the toxic gas that produces can not leak out yet, thereby it is healthy can not affect production environment and human body, is beneficial to cleaning of environment protection and whole production environment.
Description of drawings
Below in conjunction with accompanying drawing embodiments of the invention are described, wherein:
Fig. 1 is the module diagram of traditional device for the production of methylpyridine phosphorus.
Fig. 2 is the structural representation of the first reaction member among Fig. 1.
Fig. 3 is the structural representation of the second reaction member among Fig. 1.
Fig. 4 is the module diagram of a kind of reaction unit for hermetically sealed production methylpyridine phosphorus provided by the invention.
Fig. 5 is the structural representation of the first reaction member among Fig. 4.
Fig. 6 is shower nozzle among Fig. 5 and the structural representation of the first noumenon.
Fig. 7 is the structural representation of the second reaction member among Fig. 4.
Embodiment
Below based on accompanying drawing specific embodiments of the invention are further elaborated.Should be appreciated that specific embodiment described herein as just embodiment, the protection domain that is not intended to limit the present invention.
See also Fig. 4, be the module diagram of a kind of reaction unit for hermetically sealed production methylpyridine phosphorus provided by the present invention.Described device comprises 400, one the second reaction members 500 of first reaction member, and described first, second reaction member 400,500 the 3rd reaction members 600 that connect.Described the first reaction member 400 is for the production of intermediate product side chain chloro-product.Described the second reaction member 500 is for the production of the intermediate product thiophosphatephosphorothioate.Above-mentioned two kinds of intermediate products are that side chain chloro-product and thiophosphatephosphorothioate enter the 3rd reaction member 600 at last, generate the finished product methylpyridine phosphorus after the condensation reaction.
See also Fig. 5, described the first reaction member 400 comprises an eddy flow still 410, a plurality of the first storage tank that communicates with this eddy flow still 410, a gas-holder 430, a waste gas withdrawing can 440 and one first powder liquid mixing pump 450.
Described the first storage tank (figure does not indicate) is used for the various raw materials of the synthetic described side chain chloro-product of deposit.Particularly, described the first storage tank comprises an oxazole [4,5-b] pyridine-2 (3H) ketone storage tank 421, one DMFs (DMF) storage tank 422, a Paraformaldehyde 96 storage tank 423 and monochlor(in)ate sulfoxide storage tank 424.Wherein, described oxazole [4,5-b] pyridine-2 (3H) ketone storage tank 421, DMF storage tank 422 and Paraformaldehyde 96 storage tank 423 are communicated with described eddy flow still 410 by described the first powder liquid mixing pump 450.424 of described sulfur oxychloride storage tanks directly are communicated with described eddy flow still 410, to prevent that described sulfur oxychloride from directly entering the first powder liquid mixing pump 450 and then described the first powder liquid mixing pump 450 of corrosion damage, prevent that also various raw materials from reacting simultaneously in the first powder liquid mixing pump 450.In order to control described oxazole [4,5-b] switch and the flow of pyridine-2 (3H) ketone storage tank 421, DMF storage tank 422 and Paraformaldehyde 96 storage tank 423, on the connecting pipe of this oxazole [4,5-b] pyridine-2 (3H) ketone storage tank 421, DMF storage tank 422 and Paraformaldehyde 96 storage tank 423 and the first powder liquid mixing pump 450, be provided with three control valves (figure does not indicate).Being appreciated that ground, is switch and the flow of control sulfur oxychloride storage tank 424, also is provided with a control valve (figure indicates) on the connecting pipe of this sulfur oxychloride storage tank 424 and eddy flow still 410.
Described gas-holder 430 stores chlorine, when reaction, by a ventpipe (figure does not indicate) gas is imported eddy flow still 410.Be switch and the flow of control gas-holder 430, be provided with a control valve (figure does not indicate) at described ventpipe.440 waste gas that produce by a recovery tube (figure indicates) the recovery reaction that extend in the eddy flow still 410 of described waste gas withdrawing can.Described waste gas mainly comprises hydrogenchloride.It is emphasized that described waste gas withdrawing can 440 means that all can collect the device of described waste gas, such as recovery tower.
Described the first powder liquid mixing pump 450 has takes out material, feeding, and mixes, and the function of the various raw materials of Uniform Dispersion is used for Solid raw materials or solid-liquid mixed-phase feed being carried out Uniform Dispersion and being sent to eddy flow still 410 and reacting.Particularly, this first powder liquid mixing pump 450 comprises first import 451 and one first outlet 452.Described the first import 451 is communicated with described oxazole [4,5-b] pyridine-2 (3H) ketone storage tank 421, DMF storage tank 422 and Paraformaldehyde 96 storage tank 423, and described the first outlet 452 is communicated with eddy flow still 410.So that raw material (oxazole [4,5-b] pyridine-2 (3H) ketone, DMF and Paraformaldehyde 96) is sucked and through mixing, behind the Uniform Dispersion, with certain pressure well-mixed material being pressed to eddy flow still 410 from the first outlet 452 from the first import 451.Because described the first powder liquid mixing pump 450 can automatic material-absorbing and the raw material of solid-liquid two-phase or solvent can be mixed and automatically be pressed into eddy flow still 410, thereby need not hand-stuff (oxazole [4,5-b] pyridine-2 (3H) ketone that is solid phase such as artificial interpolation).Namely automatically carry out filler (oxazole [4,5-b] pyridine-2 (3H) ketone that is solid phase) by the first powder liquid mixing pump 450, can improve reaction efficiency, be conducive to the optimization of employee's healthy and reaction process.
Described eddy flow still 410 comprises a first noumenon 411, a taper decollator 412 that is arranged in the described the first noumenon 411, first opening for feed 413 that is arranged on the sidewall of described the first noumenon 411,414, one in conduit that passes described taper decollator 412 and be used for input chlorine be used for discharging because of produce methylpyridine phosphorus produce the passage 415 of waste gas (such as HCl) and one be arranged on as described in the first discharge port 416 of the first noumenon 411 sidewalls.
Thereby described the first noumenon 411 hollow settings are surrounded by its internal surface and are formed first reaction chamber, and the synthetic of described side chain chloro-product namely finished in this first reaction chamber.Described the first noumenon 411 was made or formed described the first reaction chamber by acid resisting material internal surface is coated with acid resisting material.The shape of described reaction chamber is not limit, and can be barrel-like structure, can be the cone structure yet.In the present embodiment, described reaction chamber is a cone structure of standing upside down, and defining the direction that the diameter of the round tangent plane of described the first reaction chamber in axial direction reduces gradually is first direction.It is to be noted, this section and even conical structure mentioned in this article, the end that its diameter is less still has one fixed width, the diameter that is its circle tangent plane is also non-vanishing at microcosmic, and the ratio of the diameter of the round tangent plane of the end that the diameter of the round tangent plane of the end that just diameter is less and diameter are larger is less.Therefore on macroscopic view, described the first reaction chamber is conical structure, and from microcosmic, described the first reaction chamber is frustum cone structure.
Described taper decollator 412 is arranged in the described the first noumenon 411, and the internal surface interval of the outside surface of this taper decollator 412 and described the first noumenon 411 arranges.Wherein, the dead in line of the axis of described taper decollator 412 and the first noumenon 411, and the diameter of the round tangent plane of described taper decollator 412 increases gradually along first direction.Thereby so that the space between the first reaction chamber and taper decollator 412 outer side walls is more and more less along first direction, thereby be conducive to improve reaction efficiency for increasing the contact area of powder liquid and the lowering speed of reduction powder liquid.Described taper decollator 412 is a hollow structure, to pass described conduit 414.That is, described chlorine passes through from described taper decollator 412 inside, and other raw materials then pass through from the space between described reaction chamber and taper decollator 412 outer side walls.Be appreciated that with the first noumenon 411 this taper decollator 412 is also made by the acid resistance material or its surface is coated with the acid resistance material.The round tangent plane of the end that as a same reason, described taper decollator 412 diameters are less at microcosmic and non-vanishing.Therefore on macroscopic view, described taper decollator 412 is conical structure, and from microcosmic, described taper decollator 412 is frustum cone structure.
Described the first opening for feed 413 is arranged on the larger end of diameter of described the first reaction chamber circle tangent plane, so that raw material flows to the larger end of taper decollator 412 diameters from the less end of taper decollator 412 diameters.When raw material after injecting the first reaction chamber from the first opening for feed 413 under the pressure behind the less end of taper decollator 412 diameters, most of raw material can descend around described taper decollator 412 rotations in the space between described the first noumenon 411 internal surfaces and taper decollator 412 outer side walls, the small portion raw material can drop on outside surface or the first noumenon 411 internal surfaces of taper decollator 412 under action of gravitation, along the outside surface rotation decline of described the first noumenon 411 internal surfaces or taper decollator 412.And the space between described the first reaction chamber and taper decollator 412 outer side walls is dropped on the outside surface of taper decollator 412 or the internal surface of the first noumenon 411 around the raw material of described taper decollator 412 rotations more and more along with highly descending.Because the diameter of taper decollator 412 circle tangent planes increases gradually along first direction, and the diameter of described the first reaction chamber circle tangent plane reduces gradually along first direction, this setting can slow down the lower Flow Velocity of the material of the outside surface that drops on taper decollator 412 or the first noumenon 411 internal surfaces, can disperse its contact area simultaneously.Simultaneously, because the space between the first reaction chamber and taper decollator 412 outer side walls is more and more less along first direction, when described raw material descended toward first direction, the space was more crowded, thereby can further slow down the lower Flow Velocity of described material.Be appreciated that described raw material is longer in the residence time in space, the contact area between each raw material is larger, contacts more fully, and reaction efficiency is higher.
In the present embodiment, longer in the residence time in space for making described raw material, described the first opening for feed 413 is one to have the shower nozzle of hollow tubular structure, and the axial direction due of described shower nozzle and described first direction have an angle, and described angle is more than or equal to 45 degree.Please in the lump referring to Fig. 6, preferably, the axial direction due of described shower nozzle and the angle of described first direction are 90 degree, and the internal surface of the axial direction due of described shower nozzle and described the first noumenon 411 is tangent.Thereby so that the raw material that shoots out from this shower nozzle substantially can both be along under the internal surface rotating fluid of this first noumenon 411, and the internal surface at this first noumenon 411 has faster speed of rotation, utilize the centripetal force of himself around the internal surface rotation of this first noumenon 411, thereby delay the time under the described feedstream.
Described conduit 414 can be a Venturi tube, its hermetically passing the first noumenon 411, and be plugged in the taper decollator 412 of hollow structure, thereby fix the position of this conduit 414, simultaneously can also make the chlorine that from conduit 414, enters to rising, and then fully contact with defluent raw material, further reach the purpose of abundant reaction.Be appreciated that the sidewall of described taper decollator 412 also can evenly be provided with a plurality of through holes (figure is sign) in order to make described chlorine evenly flow out and increase the contact area of being detained skyborne raw material with the first reaction chamber from described taper decollator 412.Further, when the larger end of described taper decollator 412 diameters was covered by reaction solution (solution behind raw material and the chlorine reaction), by described through hole, described chlorine can directly contact with raw material.
Described passage 415 is salable being arranged on the first noumenon 411 also, when chlorine and the oxazole pyridone take DMF as dissolution with solvents, and Paraformaldehyde 96, when the raw material reactions such as sulfur oxychloride generated waste gas (such as HCl), described waste gas can be discharged from this passage 415.
Described the first discharge port 416 is communicated with described the first powder liquid mixing pump 450 and the 3rd reaction member 600 simultaneously.For control from described eddy flow still 410 out raw material or product stream to the first powder liquid mixing pump 450 and the 3rd reaction member 600, be provided with control valve (figure sign) between the first import 451 of described the first powder liquid mixing pump 450 and described the first discharge port 416.Because described the first discharge port 416 is communicated with the first entrance 451 of described the first powder liquid mixing pump 450.When reaction is not finished, unreacted completely raw material can carry out blending dispersion again by being sent to described the first powder liquid mixing pump 450, directive eddy flow still 410 again after being uniformly dispersed, thereby raising reaction efficiency, avoid raw material to be deposited on described eddy flow still 410 bottoms and contact not exclusively, cause reaction not exclusively.When reaction was finished, described reacted product can flow to the 3rd reaction member 600, carries out next step reaction.
See also Fig. 7, described the second reaction member 500 comprises a reactor 510, a plurality of the second storage tank that communicates with this reactor 510 (figure does not indicate), one second powder liquid mixing pump 530 and a whipping appts 540.
Described the second storage tank is used for the various raw materials of the synthetic described thiophosphatephosphorothioate of deposit.Particularly, described the second storage tank comprises a sulphur storage tank 521, a methyl alcohol storage tank 522, a sodium methylate storage tank 523 and a dimethylphosphite storage tank 524.Described sulphur storage tank 521 is communicated with described reactor 510 by described the second powder liquid mixing pump 530.Described methyl alcohol storage tank 522, sodium methylate storage tank 523 and 524 of dimethylphosphite storage tanks directly are communicated with described reactor 510, to avoid described raw material directly to enter the second powder liquid mixing pump 530 and then to corrode described the second powder liquid mixing pump 530, also can avoid simultaneously described raw material in the second powder liquid mixing pump 530, to react.For switch and the flow of controlling described sulphur storage tank 521, be respectively arranged with control valve (figure indicates) at the connecting pipe of this sulphur storage tank 521 and the second powder liquid mixing pump 530.Be appreciated that ground, for controlling switch and the flow of described methyl alcohol storage tank 522, sodium methylate storage tank 523 and dimethylphosphite storage tank 524, on the connecting pipe of this methyl alcohol storage tank 522, sodium methylate storage tank 523 and dimethylphosphite storage tank 524 and reactor 510, also be provided with separately a control valve (figure indicates).
Described the second powder liquid mixing pump 530 has takes out material, feeding, and the function of blending dispersion, is used for Solid raw materials (such as sulphur) Uniform Dispersion and is sent to reactor 510.Particularly, this second powder liquid mixing pump 530 comprises second import 531 and one second outlet 532.Described the second import 531 is communicated with described sulphur storage tank 521, and described the second outlet 532 is communicated with reactor 510.So that raw material (such as sulphur) is sucked and behind Uniform Dispersion, exports the material that will fully disperse with certain pressure 532 from second and press to reactor 510 from the second import 531.Automatically be pressed into reactor 510 because described the second powder liquid mixing pump 530 energy automatic material-absorbings also can mix Solid raw materials, thereby need not hand-stuff (sulphur that is solid phase such as artificial interpolation).Namely automatically carry out filler by the second powder liquid mixing pump 530, can improve reaction efficiency, be conducive to the optimization of employee's healthy and reaction process.
Described reactor 510 comprises that 511, one of second body is arranged on the second opening for feed 512 and second discharge port 513 that is arranged on described the second body 511 bottoms of the sidewall of described the second body 511.
Thereby the 511 hollow settings of described the second body form second reaction chamber, and described thiophosphoric acid ester synthesis is namely finished in this second reaction chamber.Described the second body 511 was made or formed described the second reaction chamber by acid resisting material internal surface is coated with acid resisting material.The shape of described the second reaction chamber is not limit, and can be barrel-like structure, can be the cone structure yet.In the present embodiment, described the second reaction chamber is a barrel-like structure that stands upside down.
The axis interval of the axis of described the second opening for feed 512 and described the second discharge port 513 arranges, and preferably, the axis of described the second opening for feed 512 is mutually vertical with the axis of described the second discharge port 513.Described the second opening for feed 512 is communicated with the second outlet 532 of described the second powder liquid mixing pump 530.
Described the second discharge port 513 is communicated with described the second powder liquid mixing pump 530 and the 3rd reaction member 600 simultaneously.For control from described reactor 510 out raw material or product stream to the second powder liquid mixing pump 530 and the 3rd reaction member 600, be provided with a control valve (figure does not indicate) between the second import 531 of described the second powder liquid mixing pump 530 and described the second discharge port 513, also be provided with a control valve (figure does not indicate) between described the second discharge port 513 and the 3rd reaction member 600.When reaction is not finished, unreacted completely raw material can carry out blending dispersion again by the second powder liquid mixing pump 530, directive reactor 510 again after being uniformly dispersed, thereby raising reaction efficiency, avoid raw material to be deposited on described reactor 510 bottoms and contact not exclusively, cause reaction not exclusively.When reaction was finished, described reacted product can flow to the 3rd reaction member 600, carries out next step reaction.
Described whipping appts 540 is used for when reaction raw material being stirred, with the raw material in the abundant dispersion reactor 510.This whipping appts 540 comprises the stirring rod 541 that extends in described the second body 511, and the dead in line of the axis of described stirring rod 541 and the second body 511 is to reach best mixing effect.
Compared to prior art, in the device of production methylpyridine phosphorus provided by the present invention, described the first reaction member utilizes by the first powder liquid mixing pump that the inwall along this eddy flow still flows down in the pressure directive eddy flow still after with the solid-liquid two-phase raw material Uniform Dispersion in the storing pipe, and nationality is arranged by the gradient of the first reaction chamber of described eddy flow still and the position of shower nozzle, descend so that described raw material can be at the inwall of this first reaction chamber spiral, delay described raw material along time that the inwall of described the first reaction chamber flows down.Be appreciated that by introducing the first powder liquid mixing pump and have the eddy flow still of taper the first reaction chamber, the one, make the first reaction member need not hand-fed, all reinforced processes all can be carried out under sealed environment; The 2nd, by the first powder liquid mixing pump with the raw material Uniform Dispersion of solid-liquid two-phase and raw material spiral in the first reaction chamber is stayed; increase the duration of contact between chlorine and the raw material; can make raw material reach the effect of stirring; thereby can accomplish in the eddy flow still without whipping appts; fundamentally stop poisonous gas leakage, be conducive to environment protection.To sum up; the device of production methylpyridine phosphorus provided by the present invention; because described side chain chloro-product can be produced by the eddy flow still under hermetically sealed environment; therefore, described eddy flow still can be accomplished to seal fully when producing described side chain chloro-product; the situations such as run, drip, leak can not appear in process of production; the toxic gas that produces can not leak out yet, thereby it is healthy can not affect production environment and human body, is beneficial to cleaning of environment protection and whole production environment.
Be appreciated that, the reaction unit that is used for hermetically sealed production methylpyridine phosphorus among the application is not only applicable to for the production of methylpyridine phosphorus, also can be applicable in the chemical reaction of most of generation waste gas, especially applicable to producing the chemical substance that produces and need to use mechanical stirring device equipment in other reaction process with obnoxious flavour.
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all interior any modifications of doing in the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included in protection scope of the present invention in.
Claims (10)
1. reaction unit that is used for hermetically sealed production methylpyridine phosphorus, it comprises one first reaction member, one second reaction member reaches and described first, the 3rd reaction member that the second reaction member is communicated with respectively, this first reaction member comprises an eddy flow still, one oxazole [4,5-b] pyridine-2 (3H) ketone storage tank, one N, the dinethylformamide storage tank, one Paraformaldehyde 96 storage tank, monochlor(in)ate sulfoxide storage tank, one gas-holder and a waste gas withdrawing can, described sulfur oxychloride storage tank directly is communicated with described eddy flow still, and described gas-holder and waste gas withdrawing can all are communicated with described eddy flow still; It is characterized in that: described the first reaction member further comprises one first powder liquid mixing pump, described the first powder liquid mixing pump comprises one first import and one first outlet, described oxazole [4,5-b] pyridine-2 (3H) ketone storage tank, N, dinethylformamide storage tank and Paraformaldehyde 96 storage tank are communicated with described the first import, and described the first outlet is communicated with described eddy flow still; Described eddy flow still comprises a first noumenon, and described the first noumenon hollow arranges and forms one first reaction chamber, and described the first reaction chamber is a conical structure that stands upside down, and described sulfur oxychloride storage tank is arranged on the larger side of round tangent plane diameter of described the first reaction chamber; Described eddy flow still comprises the first opening for feed and the first discharge port on the sidewall that is separately positioned on described the first noumenon, this first opening for feed is near the larger side of round tangent plane diameter of described the first reaction chamber, and this first discharge port is near the less side of round tangent plane diameter of described the first reaction chamber; Described the first opening for feed is a shower nozzle, and defining the direction that the diameter of the round tangent plane of described the first reaction chamber in axial direction reduces gradually is first direction, and the axial direction due of described shower nozzle and described first direction have an angle, and described angle is more than or equal to 45 degree.
2. the reaction unit for hermetically sealed production methylpyridine phosphorus as claimed in claim 1, it is characterized in that: the axial direction due of described the first discharge port overlaps with the axial direction due of the first reaction chamber.
3. the reaction unit for hermetically sealed production methylpyridine phosphorus as claimed in claim 1 is characterized in that: the axial direction due of described shower nozzle and the angle of described first direction are 90 degree.
4. the reaction unit for hermetically sealed production methylpyridine phosphorus as claimed in claim 3, it is characterized in that: the axial direction due of described shower nozzle and the internal surface of described the first noumenon are tangent.
5. the reaction unit for hermetically sealed production methylpyridine phosphorus as claimed in claim 3, it is characterized in that: described shower nozzle is hollow tubular structure.
6. the reaction unit for hermetically sealed production methylpyridine phosphorus as claimed in claim 1, it is characterized in that: described eddy flow still further comprises the passage of the sidewall top that is arranged on described the first noumenon, described passage near the larger side of the round tangent plane diameter of the first reaction chamber and be communicated with the waste gas withdrawing can.
7. the reaction unit for hermetically sealed production methylpyridine phosphorus as claimed in claim 1, it is characterized in that: described the second reaction member comprises a reactor, a sulphur storage tank, a methyl alcohol storage tank, a sodium methylate storage tank, a dimethylphosphite storage tank and a whipping appts, described methyl alcohol storage tank, sodium methylate storage tank and dimethylphosphite storage tank are communicated with described reactor, and described whipping appts comprises the stirring rod that extends in the reactor.
8. the reaction unit for hermetically sealed production methylpyridine phosphorus as claimed in claim 7, it is characterized in that: described the second reaction member further comprises one second powder liquid mixing pump, described the second powder liquid mixing pump comprises one second import and one second outlet, described sulphur storage tank is communicated with described the second import, and described the second outlet is communicated with described reactor.
9. the reaction unit for hermetically sealed production methylpyridine phosphorus as claimed in claim 7, it is characterized in that: described reactor comprises one second body, described the second body hollow arranges and forms one second reaction chamber, described the second reaction chamber be shaped as tubbiness.
10. the reaction unit for hermetically sealed production methylpyridine phosphorus as claimed in claim 9, it is characterized in that: described stirring rod extends in described the second body, the dead in line of the axis of described stirring rod and the second body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210596230.XA CN103073593B (en) | 2012-12-19 | 2012-12-19 | Reaction device for fully hermetically producing azamethiphos |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210596230.XA CN103073593B (en) | 2012-12-19 | 2012-12-19 | Reaction device for fully hermetically producing azamethiphos |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103073593A true CN103073593A (en) | 2013-05-01 |
| CN103073593B CN103073593B (en) | 2015-06-03 |
Family
ID=48150310
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210596230.XA Expired - Fee Related CN103073593B (en) | 2012-12-19 | 2012-12-19 | Reaction device for fully hermetically producing azamethiphos |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103073593B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2280483Y (en) * | 1996-10-30 | 1998-05-06 | 卢保源 | Automatic powder pouring-in water and mixing device |
| CN1386741A (en) * | 2001-05-22 | 2002-12-25 | 中国科学院福建物质结构研究所 | Process for synthesizing methylpyridyl phosphide |
| CN101234308A (en) * | 2008-03-05 | 2008-08-06 | 聂如国 | Powder-liquid mixer |
| CN201157761Y (en) * | 2008-03-05 | 2008-12-03 | 聂如国 | Powder-liquor mixer homogeneous homogenization system |
| CN101575285A (en) * | 2009-04-29 | 2009-11-11 | 李普选 | Technical method for continuously producing fatty glyceride and special equipment thereof |
| CN201664601U (en) * | 2010-04-22 | 2010-12-08 | 海门贝斯特精细化工有限公司 | Vacuum automatic feeding device |
| CN102329253A (en) * | 2011-03-22 | 2012-01-25 | 江苏中丹集团股份有限公司 | Reaction apparatus for resorcinol neutralization reaction section and reaction technology thereof |
| CN202989026U (en) * | 2012-12-19 | 2013-06-12 | 宁波远利化工有限公司 | Reaction device used for full-sealed production of azamethiphos |
-
2012
- 2012-12-19 CN CN201210596230.XA patent/CN103073593B/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2280483Y (en) * | 1996-10-30 | 1998-05-06 | 卢保源 | Automatic powder pouring-in water and mixing device |
| CN1386741A (en) * | 2001-05-22 | 2002-12-25 | 中国科学院福建物质结构研究所 | Process for synthesizing methylpyridyl phosphide |
| CN101234308A (en) * | 2008-03-05 | 2008-08-06 | 聂如国 | Powder-liquid mixer |
| CN201157761Y (en) * | 2008-03-05 | 2008-12-03 | 聂如国 | Powder-liquor mixer homogeneous homogenization system |
| CN101575285A (en) * | 2009-04-29 | 2009-11-11 | 李普选 | Technical method for continuously producing fatty glyceride and special equipment thereof |
| CN201664601U (en) * | 2010-04-22 | 2010-12-08 | 海门贝斯特精细化工有限公司 | Vacuum automatic feeding device |
| CN102329253A (en) * | 2011-03-22 | 2012-01-25 | 江苏中丹集团股份有限公司 | Reaction apparatus for resorcinol neutralization reaction section and reaction technology thereof |
| CN202989026U (en) * | 2012-12-19 | 2013-06-12 | 宁波远利化工有限公司 | Reaction device used for full-sealed production of azamethiphos |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103073593B (en) | 2015-06-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN205830880U (en) | A kind of pesticide spraying device | |
| CN107376718A (en) | A kind of agricultural irrigation pestsides synthesis device for formulating | |
| CN202989026U (en) | Reaction device used for full-sealed production of azamethiphos | |
| CN202989027U (en) | Reaction device used for full-sealed preparation of azamethiphos | |
| CN202989029U (en) | Reaction device used for full-sealed clean preparation of azamethiphos | |
| CN103073596B (en) | A kind of technique for hermetically sealed cleanly production methylpyridine phosphorus | |
| CN202989028U (en) | Reaction device used for full-sealed production of azamethiphos | |
| CN202989031U (en) | Reaction device used for full-sealed preparation of azamethiphos | |
| CN103333207A (en) | Technology for producing azamethiphos in fully-sealed clean manner | |
| CN103087104A (en) | Reaction device for preparing azamethiphos in fully sealed way | |
| CN103073595B (en) | Hermetically sealedly clean the technique preparing methylpyridine phosphorus | |
| CN103073593A (en) | Reaction device for fully hermetically producing azamethiphos | |
| CN103073591A (en) | Reaction device for fully hermetically and cleanly preparing azamethiphos | |
| CN103073592A (en) | Reaction device for hermetically sealed production of azamethiphos | |
| CN103073594A (en) | Reaction device for fully hermetically preparing azamethiphos | |
| CN203079888U (en) | Reaction device for producing azamethiphos | |
| CN202989030U (en) | Reaction equipment for preparing azamethiphos | |
| CN114471413B (en) | Supply and discharge device with multiple chambers for pesticide processing reaction tank | |
| CN103535295A (en) | Automatic feeding device | |
| CN211329027U (en) | Pesticide sprays mixing arrangement in farming | |
| CN102602893A (en) | Chlorine dioxide liquor generator for pesticide-free crop virus killing | |
| CN212261959U (en) | Multifunctional chlorine dioxide sterilizing cabinet with functions of instant preparation and use and self-diffusion | |
| CN211329002U (en) | A stirring filling equipment for preparation of biological medicine | |
| CN209362254U (en) | Chemicals dosing plant | |
| CN203633379U (en) | Voltage stabilization speed adjustable electric sprayer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150603 Termination date: 20201219 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |