CN103333207A - Technology for producing azamethiphos in fully-sealed clean manner - Google Patents
Technology for producing azamethiphos in fully-sealed clean manner Download PDFInfo
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- CN103333207A CN103333207A CN2012105962390A CN201210596239A CN103333207A CN 103333207 A CN103333207 A CN 103333207A CN 2012105962390 A CN2012105962390 A CN 2012105962390A CN 201210596239 A CN201210596239 A CN 201210596239A CN 103333207 A CN103333207 A CN 103333207A
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Abstract
The invention provides a technology for producing azamethiphos in a fully-sealed clean manner. The technology comprises a step of providing a reaction device; a step of preparing a branched-chain chlorinated product, wherein chlorine gas is fed into a cyclone kettle, the cyclone kettle comprises a first body, a first reaction chamber with an inverted conic structure is disposed in the first body in a hollow manner, oxazolo [4,5-b]pyridine-2-(3H)-one, N,N-dimethyl formamide, paraformaldehyde, thionyl chloride and other raw materials are mixed, uniformly dispersed and pumped into the cyclone kettle by using a first powder-liquid mixing pump, and the raw materials are reacted in the first reaction chamber to obtain the branched-chain chlorinated product; a step of preparing thiophosphate ester in a second reaction unit; and a step of preparing the azamethiphos in a third reaction unit. According to the technology provided by the invention, the azamethiphos can be prepared in a fully-sealed environment and in a clean manner.
Description
Technical field
The present invention relates to a kind of production technique for methylpyridine phosphorus, particularly a kind of technology that can hermetically sealedly clean the production methylpyridine phosphorus.
Background technology
Methylpyridine phosphorus has another name called first base pyrrole Evil phosphorus, is a kind of excellent insecticide, 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 World Health Organization (WHO) and recommends the organic phosphorous insecticide that uses.Because make emulsion, sprays, pulvis, wettable powder and sol particle in this methylpyridine phosphorus, therefore be specially adapted to prevent and treat insects such as fly again.
Conventional methylpyridine phosphorus preparation technology mainly comprises three steps: step 1 is raw material with oxazole [4,5-b] pyridine-2 (3H) ketone, generates a kind of intermediate side chain chloro-product of methylpyridine phosphorus then 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 structural representation for preparing the device of described methylpyridine phosphorus, described device comprises 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 first reaction member 100 for the preparation of intermediate product side chain chloro-product.Second reaction member 200 is for the preparation 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 first reaction member 100, described first reaction member 100 comprises one first reactor 10, a plurality of first storage tank that communicates with this first reactor 10, a gas-holder 30 and waste gas withdrawing can 40 and one first whipping appts 50.Described first storage tank comprises an oxazole [4,5-b] pyridine-2 (3H) ketone storage tank 21, one N, dinethylformamide (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 first reactor 10.40 waste gas that produce by the recovery tube (not shown) recovery reaction that extend in first reactor 10 of described waste gas withdrawing can.Described first whipping appts 50 comprises first stirring rod 51 that extends in first reactor 10.When reaction, with oxazole pyridone, N, raw materials such as dinethylformamide (DMF), Paraformaldehyde 96 and sulfur oxychloride add first reactor 10 according to a graded, and feed chlorine, reaction while stirring.See also Fig. 3, be the structural representation of traditional second reaction member 200, described second reaction member 200 comprises one second reactor 210, a plurality of second storage tank that communicates with this second reactor 210 and one second whipping appts 230.Described second storage tank 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 second whipping appts 230 comprises second stirring rod 231 that extends in second reactor 210.When reaction, raw materials such as sulphur storage tank 221, methyl alcohol storage tank 222, sodium methylate storage tank 223 and dimethylphosphite 224 are added second reactor 210 according to a graded, while stirring reaction.When treating that the back reaction is finished, add new raw material again.
Yet, when preparing described side chain chloro-product with traditional prepared, being difficult to accomplish to seal fully, situations such as run, drip, leak appear in described first reaction member 100 easily in preparation process.And the gas (as hydrogenchloride) that described side chain chloro-product produces in preparation process all has strong toxicity and corrodibility, leaks out easy production environment and the human body health of influencing, 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 first reactor 10 at every turn, influences the sealing of described first reactor 10.Second, because described first reactor 10 has first whipping appts 50, seal point between first whipping appts 50 and first reactor 10 is prepared 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, influence the sealing of 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 hermetically sealed technology of producing methylpyridine phosphorus that cleans, to overcome above-mentioned deficiency.
The invention provides a kind of hermetically sealed technology of producing methylpyridine phosphorus that cleans, it comprises the steps: to provide a reaction unit, it comprises one first reaction member, one second reaction member reaches and described first, the 3rd reaction member that 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 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 first reaction member further comprises one first powder liquid mixing pump, the described 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 first import, and described first outlet is communicated with described eddy flow still; Described eddy flow still comprises the taper decollator that one first body and described first body connect, the described first body hollow arranges and forms one first reaction chamber, described first reaction chamber is a conical structure that stands upside down, and described sulfur oxychloride storage tank is arranged on the bigger side of round tangent plane diameter of described first reaction chamber; Defining the direction that the diameter of the round tangent plane of described first reaction chamber in axial direction reduces gradually is first direction, and the diameter of the round tangent plane of described taper decollator increases gradually along first direction; Preparation side chain chloro-product: in the eddy flow still, feed chlorine, suck oxazole [4 from first import according to a definite sequence by the described first powder liquid mixing pump, 5-b] pyridine-2 (3H) ketone, N, dinethylformamide, Paraformaldehyde 96 also evenly disperse, raw material after disperseing is injected described first reaction chamber from the bigger end of described conical structure diameter along the tangential direction of its circle tangent plane from the first outlet output and via described shower nozzle, make the described raw material of injecting under the back cavity rotating fluid that forms between described first body and the taper decollator; In this first reaction chamber dripping thionyl chloride, make oxazole [4,5-b] pyridine-2 (3H) ketone, N, thus dinethylformamide, Paraformaldehyde 96, sulfur oxychloride and chlorine are finished nucleophilic chlorination, hydroxymethylation and side chain chlorination successively at first reaction chamber and are obtained the side chain chloro-product; Preparation thiophosphatephosphorothioate: in reactor, with dimethylphosphite and sulfur reaction, under the effect of sodium methylate, obtain thiophosphatephosphorothioate; Preparation methylpyridine phosphorus: make described side chain chloro-product, thiophosphatephosphorothioate deliver to the 3rd reaction member from first reaction member, second reaction member respectively, and carry out condensation reaction at the 3rd reaction member and generate described methylpyridine phosphorus.
Described eddy flow still also comprises a conduit that is used for input chlorine, and described taper decollator is a hollow structure, and conduit passes described eddy flow still and is plugged in the taper decollator of described hollow structure.
Described conduit is a Venturi tube.
Described taper decollator is arranged in described first body, the dead in line of the axis of described taper decollator and first body.
Described nucleophilic chlorination further comprises the steps: raw material oxazole [4,5-b] pyridine-2 (3H) ketone and solvent N, dinethylformamide is from described oxazole [4,5-b] pyridine-2 (3H) ketone storage tank and N, the dinethylformamide storage tank sucks that the first powder liquid mixing pump mixes and evenly disperses, mixed solution after disperseing is injected the eddy flow still by first opening for feed, carry out the nucleophilic chlorination with chlorine in the eddy flow still and obtain chloro-product.
Described hydroxymethylation comprises the steps: that further Paraformaldehyde 96 is sucked the first powder liquid mixing pump from the Paraformaldehyde 96 storage tank evenly injects the eddy flow still after the dispersion, obtains the methylolation product with described chloro-product generation hydroxymethylation in the eddy flow still.
The step of described preparation side chain chloro-product comprises the steps: that further the solid-liquid two-phase raw material in the eddy flow still is sucked the first powder liquid mixing pump from the first outlet material further to be disperseed, and injects the eddy flow still by shower nozzle then.
Described side chain chlorination further comprises the steps: to add sulfur oxychloride by the sulfur oxychloride storage tank toward the eddy flow still, makes this methylolation product and sulfur oxychloride carry out the side chain chlorination and obtains described side chain chloro-product.
Compared to prior art, the hermetically sealed technology of producing methylpyridine phosphorus that cleans provided by the present invention, after evenly disperseing the solid-liquid two-phase raw material in the storing pipe by the first powder liquid mixing pump, described first reaction member utilizes that the inwall along this eddy flow still flows down in the pressure directive eddy flow still, and nationality is by the unique texture of described first reaction chamber and taper decollator, between first inner body wall and taper decollator outer wall, form the back cavity that progressively narrow in a space, can not only make described raw material to fall in described back cavity rotation, and can further delay the skyborne residence time of raw material by described first reaction chamber and taper decollator.Be appreciated that by introducing the first powder liquid mixing pump, the eddy flow still with taper first reaction chamber and taper dispersion, the one, make first reaction member need not hand-fed, all reinforced processes all can be carried out under sealed environment; The 2nd, the raw material of solid-liquid two-phase is evenly disperseed and raw material is formed in back cavity under " whirlwind " helical flow by the first powder liquid mixing pump; increase the duration of contact between chlorine and the raw material; can make raw material reach the effect of stirring; thereby can accomplish does not have whipping appts in the eddy flow still; fundamentally stop poisonous gas leakage, be conducive to environment protection.To sum up; the device of preparation methylpyridine phosphorus provided by the present invention; because described side chain chloro-product can prepare by the eddy flow still under hermetically sealed environment; therefore, described eddy flow still can be accomplished to seal fully when the described side chain chloro-product of preparation; situations such as run, drip, leak can not appear in preparation process; the toxic gas that produces can not leak out yet, thereby can not influence production environment and human body health, 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 structural representation of a kind of device for the preparation of methylpyridine phosphorus provided by the invention.
Fig. 2 is the structural representation of first reaction member among Fig. 1.
Fig. 3 is the structural representation of second reaction member among Fig. 1.
Fig. 4 is the structural representation of a kind of reaction unit for the preparation of methylpyridine phosphorus provided by the invention.
Fig. 5 is the structural representation of first reaction member among Fig. 4.
Fig. 6 is the vertical view of the eddy flow still of second reaction member among Fig. 5.
Fig. 7 is the structural representation of 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, and be not intended to limit the scope of the invention.
The hermetically sealed technology of producing methylpyridine phosphorus that cleans provided by the invention comprises the steps:
Step 1 provides a reaction unit.
See also Fig. 4, be the module diagram of described reaction unit, it comprises 400, one second reaction members 500 of first reaction member, and described first, second reaction member 400,500 the 3rd reaction members 600 that connect.
See also Fig. 5, described first reaction member 400 comprises an eddy flow still 410, a plurality of first storage tank that communicates with this eddy flow still 410 (figure does not indicate), a gas-holder 430, a waste gas withdrawing can 440 and one first powder liquid mixing pump 450.
Described first storage tank is used for the various raw materials of the synthetic described side chain chloro-product of deposit.Particularly, described first storage tank comprises an oxazole [4,5-b] pyridine-2 (3H) ketone storage tank 421, one N, dinethylformamide (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 the described 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 the described 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, connecting pipe at 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 is 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, described ventpipe is provided with a control valve (figure does not indicate).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, as recovery tower.
The described first powder liquid mixing pump 450 has takes out material, feeding, and mixes, and the function of evenly disperseing various raw materials is used for solid phase raw material or solid-liquid mixed-phase feed evenly being disperseed 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 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 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 after mixing, evenly disperseing, with certain pressure well-mixed material is pressed to eddy flow still 410 from first outlet 452 from first import 451.Because the suction and the raw material of solid-liquid two-phase or solvent can be mixed and be pressed into eddy flow still 410 automatically automatically of the described first powder liquid mixing pump 450, thereby need not hand-stuff (oxazole [4,5-b] pyridine-2 (3H) ketone that is solid phase as artificial interpolation).Namely carry out filler (oxazole [4,5-b] pyridine-2 (3H) ketone that is solid phase) automatically 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 first body 411, a taper decollator 412 that is arranged in described first body 411, first opening for feed 413 that is arranged on the sidewall of described first body 411,414, one in conduit that passes described taper decollator 412 and be used for input chlorine be used for discharging because of the preparation methylpyridine phosphorus produce the passage 415 of waste gas (as HCl) and one be arranged on as described in first discharge port 416 of first body, 411 sidewalls.
Thereby the 411 hollow settings of described first body 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 first body 411 was made or formed described 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 conical structure yet.In the present embodiment, described reaction chamber is a conical structure that stands upside down, and defining the direction that the diameter of the round tangent plane of described 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 less end of its diameter still has certain width, be diameter of its circle tangent plane at microcosmic and non-vanishing, just the ratio of the diameter of the round tangent plane of the end that the diameter of the round tangent plane of the less end of diameter and diameter are bigger is less.Therefore on macroscopic view, described first reaction chamber is conical structure, and from microcosmic, described first reaction chamber is frustum cone structure.
Described taper decollator 412 is connected with described first body 411 by the less end of circle tangent plane diameter, and the internal surface of the outside surface of this taper decollator 412 and described first body 411 arranges at interval.Wherein, the dead in line of the axis of described taper decollator 412 and first body 411, and the diameter of the round tangent plane of described taper decollator 412 increases gradually along first direction, make the space of winning between reaction chamber and taper decollator 412 outer side walls more and more littler along first direction, thereby nationality forms the back cavity that progressively narrow in a space by the unique texture of described first reaction chamber and taper decollator 412 between first inner body wall and taper decollator 412 outer walls.Can not only make described raw material to form " whirlwind " rotation at described back cavity and fall, delay the skyborne residence time of raw material, 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 first reaction chamber and taper decollator 412 outer side walls.Be appreciated that this taper decollator 412 is also made by the acid resistance material or its surface is coated with the acid resistance material with first body 411.As a same reason, the round tangent plane of the less end of described taper decollator 412 diameters 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 first opening for feed 413 is arranged on the bigger end of diameter of described first reaction chamber circle tangent plane, so that raw material flows to the bigger end of taper decollator 412 diameters from the less end of taper decollator 412 diameters.When raw material after injecting first reaction chamber from 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 first body, 411 internal surfaces and taper decollator 412 outer side walls, the small portion raw material can drop on outside surface or first body, 411 internal surfaces of taper decollator 412 under the effect of gravity, along the outside surface rotation decline of described first body, 411 internal surfaces or taper decollator 412.And the space between described 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 first body 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 first reaction chamber circle tangent plane reduces gradually along first direction, this setting can slow down the dirty speed of the material of the outside surface that drops on taper decollator 412 or first body, 411 internal surfaces, can disperse its contact area simultaneously.Simultaneously, because the space between first reaction chamber and taper decollator 412 outer side walls is more and more littler along first direction, when described raw material descended toward first direction, the space was more crowded, thereby can further slow down the dirty speed of described material.Be appreciated that described raw material is more long in the residence time in space, the contact area between each raw material is more big, 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 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 first body 411 is tangent.Thereby make 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 body 411, and the internal surface at this first body 411 has speed of rotation faster, utilize the centripetal force of himself around the internal surface rotation of this first body 411, thereby delay the time under the described feedstream.
Described conduit 414 can be a Venturi tube, its hermetically passing first body 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 first reaction chamber from described taper decollator 412.Further, when the bigger 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 first body 411 also, is the oxazole pyridone of dissolution with solvents when chlorine and with DMF, Paraformaldehyde 96, and when raw material reactions such as sulfur oxychloride generated waste gas (as HCl), described waste gas can be discharged from this passage 415.
Described first discharge port 416 is communicated with the described first powder liquid mixing pump 450 and the 3rd reaction member 600 simultaneously.The raw material or the product that come out from described eddy flow still 410 for control flow to the first powder liquid mixing pump 450 and the 3rd reaction member 600, are provided with control valve (figure does not indicate) between first import 451 of the described first powder liquid mixing pump 450 and described first discharge port 416.Because described first discharge port 416 is communicated with first entrance 451 of the described first powder liquid mixing pump 450.When reacting imperfect tense, unreacted raw material completely can carry out blending dispersion again by being sent to the described first powder liquid mixing pump 450, directive eddy flow still 410 again after waiting to be 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 second reaction member 500 comprises a reactor 510, a plurality of 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 second storage tank is used for the various raw materials of the synthetic described thiophosphatephosphorothioate of deposit.Particularly, described 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 the described 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 the described second powder liquid mixing pump 530, also can avoid described raw material in the second powder liquid mixing pump 530, to react simultaneously.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 a control valve (figure indicates) separately.
The described second powder liquid mixing pump 530 has takes out material, feeding, and the function of blending dispersion, is used for solid phase raw material (as sulphur) evenly being disperseed and being sent to reactor 510.Particularly, this second powder liquid mixing pump 530 comprises second import 531 and one second outlet 532.Described second import 531 is communicated with described sulphur storage tank 521, and described second outlet 532 is communicated with reactor 510.So that raw material (as sulphur) is sucked and after evenly disperseing, exports the material that will fully disperse with certain pressure 532 from second and press to reactor 510 from second import 531.Automatically be pressed into reactor 510 because the automatic suction of the described second powder liquid mixing pump, 530 energy also can mix the solid phase raw material, thereby need not hand-stuff (sulphur that is solid phase as artificial interpolation).Namely carry out filler automatically 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 second opening for feed 512 and second discharge port 513 that is arranged on described second body 511 bottoms of the sidewall of described second body 511.
Thereby the 511 hollow settings of described second body form second reaction chamber, and the synthetic of described thiophosphatephosphorothioate namely finished in this second reaction chamber.Described second body 511 was made or formed described second reaction chamber by acid resisting material internal surface is coated with acid resisting material.The shape of described second reaction chamber is not limit, and can be barrel-like structure, can be conical structure yet.In the present embodiment, described second reaction chamber is a barrel-like structure that stands upside down.
The axis of the axis of described second opening for feed 512 and described second discharge port 513 arranges at interval, and preferably, the axis of described second opening for feed 512 is vertical mutually with the axis of described second discharge port 513.Described second opening for feed 512 is communicated with second outlet 532 of the described second powder liquid mixing pump 530.
Described second discharge port 513 is communicated with the described second powder liquid mixing pump 530 and the 3rd reaction member 600 simultaneously.The raw material or the product that come out from described reactor 510 for control flow 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 second import 531 of the described second powder liquid mixing pump 530 and described second discharge port 513, also be provided with a control valve (figure does not indicate) between described second discharge port 513 and the 3rd reaction member 600.When reacting imperfect tense, unreacted raw material completely can carry out blending dispersion again by the second powder liquid mixing pump 530, directive reactor 510 again after waiting to be 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 second body 511, and the dead in line of the axis of described stirring rod 541 and second body 511 is to reach best mixing effect.
Step 2, preparation side chain chloro-product.
In eddy flow still 410, feed chlorine, suck oxazole [4 from first import 451 according to a definite sequence by the described first powder liquid mixing pump 450,5-b] pyridine-2 (3H) ketone, N, dinethylformamide, Paraformaldehyde 96 also evenly disperse, raw material after disperseing is injected described first reaction chamber from the bigger end of described conical structure diameter along the tangential direction of its circle tangent plane from first outlet, 452 outputs and via described shower nozzle, make the described raw material of injecting under the back cavity rotating fluid that forms between described first body 411 and the taper decollator 412.In this first reaction chamber dripping thionyl chloride, make oxazole [4,5-b] pyridine-2 (3H) ketone, N, thus dinethylformamide, Paraformaldehyde 96, sulfur oxychloride and chlorine are finished nucleophilic chlorination, hydroxymethylation and side chain chlorination successively at first reaction chamber and are obtained the side chain chloro-product.
Described nucleophilic chlorination further comprises the steps: raw material oxazole [4,5-b] pyridine-2 (3H) ketone and solvent N, dinethylformamide is from described oxazole [4,5-b] pyridine-2 (3H) ketone storage tank 421 and solvent N, the dinethylformamide storage tank 422 suctions first powder liquid mixing pump 450 mixes and evenly disperses.Mixed solution or solution after disperseing are injected eddy flow still 410 by first opening for feed 411, carry out the nucleophilic chlorination with chlorine in the eddy flow still 410 and obtain chloro-product.The reaction formula of described nucleophilic chlorination is as follows:
Described hydroxymethylation comprises the steps: that further Paraformaldehyde 96 is sucked the first powder liquid mixing pump 450 from Paraformaldehyde 96 storage tank 423 evenly injects eddy flow still 410 after the dispersion, obtains the methylolation product with described chloro-product generation hydroxymethylation in eddy flow still 410.The reaction formula of described hydroxymethylation is as follows:
The step of described preparation side chain chloro-product comprises the steps: that further the solid-liquid two-phase raw material in the eddy flow still 410 is sucked the first powder liquid mixing pump 450 from the first outlet material 412 further to be disperseed, and injects eddy flow still 410 by shower nozzle then.Be appreciated that by described raw material is further sucked the first powder liquid mixing pump 450 and disperse, can avoid raw material to be deposited on described eddy flow still 410 bottoms and contact not exclusively, cause reaction not exclusively.Reach the effect that stirs raw material indirectly, improve reaction efficiency.
Described side chain chlorination further comprises the steps: directly to add sulfur oxychloride toward eddy flow still 410 by sulfur oxychloride storage tank 424, makes this methylolation product and sulfur oxychloride carry out the side chain chlorination and obtains described side chain chloro-product.The reaction formula of described side chain chlorination is as follows:
Step 3, the preparation thiophosphatephosphorothioate.
Suck sulphur with the second powder liquid mixing pump mixing pump 530 from sulphur storage tank 521, all with behind the dispersion sulphur described sulphur is injected reactor 510.In described reactor 510, add methyl alcohol, sodium methylate and dimethylphosphite and also stir with described stirring rod 541, make the reaction of described sulphur and sodium methylate and dimethylphosphite, obtain thiophosphatephosphorothioate.The preparation feedback formula of described thiophosphatephosphorothioate is as follows:
The step that thiophosphatephosphorothioate is propped up in described preparation comprises the steps: that further the solid-liquid two-phase raw material in the reactor 510 is sucked the second powder liquid mixing pump 530 from the second outlet material 512 further to be disperseed, and injects reactor 510 then.Be appreciated that by described raw material is further sucked the second powder liquid mixing pump 530 and disperse, can add the effect of strong mixing raw material indirectly, improve reaction efficiency.
Be appreciated that to the technology that makes described methylpyridine phosphorus and more optimize that described step 3 can further include with filtration washing step and an incubation step.By filtration washing, can make the purity of the thiophosphatephosphorothioate of sending from reactor 510 higher.By insulation, can make the temperature of described thiophosphatephosphorothioate be more suitable for the temperature of reaction of step 4.
Step 4, the preparation methylpyridine phosphorus.
Make described side chain chloro-product, thiophosphatephosphorothioate deliver to the 3rd reaction member 600 from first reaction member 400, second reaction member 500 respectively, and carry out condensation reaction at the 3rd reaction member 600 and generate described methylpyridine phosphorus.The preparation feedback formula of described methylpyridine phosphorus is as follows:
Be appreciated that step 4 also can further comprise a washing step in order to obtain the higher methylpyridine phosphorus of purity, by washing, waste products or raw material handled that 4-methyl pyridine phosphorus carries out purifying.Can obtain white or white crystals sprills after the methylpyridine phosphorus drying after the washing.
Further, the hermetically sealed technology of producing methylpyridine phosphorus that cleans among the application is not only applicable to for the preparation of methylpyridine phosphorus, and also other namely need to use mechanical stirring device can produce the chemical substance of obnoxious flavour again applicable to preparation.
Compared to prior art, the hermetically sealed technology of producing methylpyridine phosphorus that cleans provided by the present invention, after evenly disperseing the solid-liquid two-phase raw material in the storing pipe by the first powder liquid mixing pump, described first reaction member utilizes that the inwall along this eddy flow still flows down in the pressure directive eddy flow still, and nationality is by the unique texture of described first reaction chamber and taper decollator, between first inner body wall and taper decollator outer wall, form the back cavity that progressively narrow in a space, can not only make described raw material to fall in described back cavity rotation, and can further delay the skyborne residence time of raw material by described first reaction chamber and taper decollator.Be appreciated that by introducing the first powder liquid mixing pump, the eddy flow still with taper first reaction chamber and taper dispersion, the one, make first reaction member need not hand-fed, all reinforced processes all can be carried out under sealed environment; The 2nd, the raw material of solid-liquid two-phase is evenly disperseed and raw material is formed in back cavity under " whirlwind " helical flow by the first powder liquid mixing pump; increase the duration of contact between chlorine and the raw material; can make raw material reach the effect of stirring; thereby can accomplish does not have whipping appts in the eddy flow still; fundamentally stop poisonous gas leakage, be conducive to environment protection.To sum up; the device of preparation methylpyridine phosphorus provided by the present invention; because described side chain chloro-product can prepare by the eddy flow still under hermetically sealed environment; therefore, described eddy flow still can be accomplished to seal fully when the described side chain chloro-product of preparation; situations such as run, drip, leak can not appear in preparation process; the toxic gas that produces can not leak out yet, thereby can not influence production environment and human body health, is beneficial to cleaning of environment protection and whole production environment.
Be appreciated that, the technology that is used for hermetically sealed preparation methylpyridine phosphorus among the application is not only applicable to for the preparation of methylpyridine phosphorus, also can be applicable in the chemical reaction of most of generation waste gas, especially applicable to the chemical substance that produces and need to use mechanical stirring device equipment in other reaction process of preparation 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 (8)
1. hermetically sealed technology of producing methylpyridine phosphorus that cleans, it comprises the steps:
One reaction unit is provided, 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 N, dinethylformamide 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; It is characterized in that: described first reaction member further comprises one first powder liquid mixing pump, the described 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 first import, and described first outlet is communicated with described eddy flow still; Described eddy flow still comprises the taper decollator that one first body and described first body connect, the described first body hollow arranges and forms one first reaction chamber, described first reaction chamber is a conical structure that stands upside down, and described sulfur oxychloride storage tank is arranged on the bigger side of round tangent plane diameter of described first reaction chamber; Defining the direction that the diameter of the round tangent plane of described first reaction chamber in axial direction reduces gradually is first direction, and the diameter of the round tangent plane of described taper decollator increases gradually along first direction;
Preparation side chain chloro-product: in the eddy flow still, feed chlorine, suck oxazole [4 from first import according to a definite sequence by the described first powder liquid mixing pump, 5-b] pyridine-2 (3H) ketone, N, dinethylformamide, Paraformaldehyde 96 also evenly disperse, raw material after disperseing is injected described first reaction chamber from the bigger end of described conical structure diameter along the tangential direction of its circle tangent plane from the first outlet output and via described shower nozzle, make the described raw material of injecting under the back cavity rotating fluid that forms between described first body and the taper decollator; In this first reaction chamber dripping thionyl chloride, make oxazole [4,5-b] pyridine-2 (3H) ketone, N, thus dinethylformamide, Paraformaldehyde 96, sulfur oxychloride and chlorine are finished nucleophilic chlorination, hydroxymethylation and side chain chlorination successively at first reaction chamber and are obtained the side chain chloro-product;
Preparation thiophosphatephosphorothioate: in reactor, with dimethylphosphite and sulfur reaction, under the effect of sodium methylate, obtain thiophosphatephosphorothioate;
Preparation methylpyridine phosphorus: make described side chain chloro-product, thiophosphatephosphorothioate deliver to the 3rd reaction member from first reaction member, second reaction member respectively, and carry out condensation reaction at the 3rd reaction member and generate described methylpyridine phosphorus.
2. the hermetically sealed technology of producing methylpyridine phosphorus that cleans as claimed in claim 1, it is characterized in that: described eddy flow still also comprises a conduit that is used for input chlorine, described taper decollator is a hollow structure, and conduit passes described eddy flow still and is plugged in the taper decollator of described hollow structure.
3. the hermetically sealed technology of producing methylpyridine phosphorus that cleans as claimed in claim 2, it is characterized in that: described conduit is a Venturi tube.
4. the hermetically sealed technology of producing methylpyridine phosphorus that cleans as claimed in claim 1, it is characterized in that: described taper decollator is arranged in described first body, the dead in line of the axis of described taper decollator and first body.
5. the hermetically sealed technology of producing methylpyridine phosphorus that cleans as claimed in claim 1, it is characterized in that: described nucleophilic chlorination further comprises the steps: raw material oxazole [4,5-b] pyridine-2 (3H) ketone and solvent N, dinethylformamide is from described oxazole [4,5-b] pyridine-2 (3H) ketone storage tank and N, the dinethylformamide storage tank sucks that the first powder liquid mixing pump mixes and evenly disperses, mixed solution after disperseing is injected the eddy flow still by first opening for feed, carry out the nucleophilic chlorination with chlorine in the eddy flow still and obtain chloro-product.
6. the hermetically sealed technology of producing methylpyridine phosphorus that cleans as claimed in claim 5, it is characterized in that: described hydroxymethylation comprises the steps: that further Paraformaldehyde 96 is sucked the first powder liquid mixing pump from the Paraformaldehyde 96 storage tank evenly injects the eddy flow still after the dispersion, obtains the methylolation product with described chloro-product generation hydroxymethylation in the eddy flow still.
7. the hermetically sealed technology of producing methylpyridine phosphorus that cleans as claimed in claim 6, it is characterized in that: the step of described preparation side chain chloro-product comprises the steps: that further the solid-liquid two-phase raw material in the eddy flow still is sucked the first powder liquid mixing pump from the first outlet material further to be disperseed, and injects the eddy flow still by shower nozzle then.
8. as claim 6 or the 7 described hermetically sealed technologies of producing methylpyridine phosphorus that clean, it is characterized in that: described side chain chlorination further comprises the steps: to add sulfur oxychloride by the sulfur oxychloride storage tank toward the eddy flow still, makes this methylolation product and sulfur oxychloride carry out the side chain chlorination and obtains described side chain chloro-product.
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| CN2012105962390A CN103333207A (en) | 2012-12-19 | 2012-12-19 | Technology for producing azamethiphos in fully-sealed clean manner |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109651432A (en) * | 2019-01-17 | 2019-04-19 | 河南省化工研究所有限责任公司 | It is a kind of to prepare O, the method for O- dimethyl-S- (N- methylcarbamoyl methyl) thiophosphate |
| CN114560873A (en) * | 2021-12-27 | 2022-05-31 | 浙江日出药业有限公司 | Preparation method of 3-chloromethyl-6-chloro-oxazole [4,5-b ] pyridine-2 (3H) ketone |
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| CN102336783A (en) * | 2010-07-18 | 2012-02-01 | 李坚 | Isomerization reaction |
| CN202201847U (en) * | 2011-08-02 | 2012-04-25 | 安徽国星生物化学有限公司 | Paraquat producing device |
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| JP2011106857A (en) * | 2009-11-13 | 2011-06-02 | Toppan Forms Co Ltd | Kit and method for separating chemical substance |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109651432A (en) * | 2019-01-17 | 2019-04-19 | 河南省化工研究所有限责任公司 | It is a kind of to prepare O, the method for O- dimethyl-S- (N- methylcarbamoyl methyl) thiophosphate |
| CN109651432B (en) * | 2019-01-17 | 2021-04-09 | 河南省化工研究所有限责任公司 | Method for preparing O, O-dimethyl-S- (N-methyl carbamoylmethyl) thiophosphate |
| CN114560873A (en) * | 2021-12-27 | 2022-05-31 | 浙江日出药业有限公司 | Preparation method of 3-chloromethyl-6-chloro-oxazole [4,5-b ] pyridine-2 (3H) ketone |
| CN114560873B (en) * | 2021-12-27 | 2023-02-28 | 浙江日出药业有限公司 | Preparation method of 3-chloromethyl-6-chloro-oxazole [4,5-b ] pyridine-2 (3H) ketone |
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