CN102030774A - Reaction process for producing ethyl chloride by using continuous chlorination process - Google Patents
Reaction process for producing ethyl chloride by using continuous chlorination process Download PDFInfo
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Abstract
The invention provides a reaction process for producing an ethyl chloride by using a continuous chlorination process. The reaction process comprises the following steps of: 1. continuously conveying ethyl sulfide into a circulating system formed by connecting a raw material mixer, a raw material tank, a reaction mixer, a tube type reactor, a gas-liquid separator and a reactor in series; 2. charging chlorine into the reaction mixer and immediately entering the tube type reactor after fast primary reaction; 3. continuously reacting raw materials in the tube type reactor and transferring heat to the outside at the same time, enabling the raw materials subjected to the reaction to flow into the gas-liquid separator and the reactor to generate a crude ethyl chloride; and 4. enabling the crude ethyl chloride to flow out of the reactor, wherein one path of the crude ethyl chloride leaves from the circulating system and enters a curing reactor, and the other path of the crude ethyl chloride goes back to the raw material mixer for diluting the ethyl sulfide and returns to the circulating reaction system. In the invention, the product is used for diluting the reactant to control reaction temperature; a gas-liquid mixer is used for strengthening mass transfer; the tube type reactor is used for strengthening heat transfer; and the continuous reaction process shortens the chlorination time greatly.
Description
Technical field
The present invention relates to a kind of production technique of diethylaluminum monochloride, particularly a kind of continuous chlorination is produced the reaction process of diethylaluminum monochloride.
Technical background
The formal name used at school of diethylaluminum monochloride is an o,o-diethylthiophosphoryl chloride, is a kind of important pesticide intermediate, and very strong corrodibility is arranged.The production technique that generally adopts is at present: (1) thiophosphoric anhydride and dehydrated alcohol reaction generate diethyldithiophosphoric acid, are commonly called as thioethyl ether; (2) thioethyl ether and chlorine reaction generate o,o-diethylthiophosphoryl chloride, are commonly called as thick diethylaluminum monochloride (thick muriate), are the mixing solutions of diethylaluminum monochloride and disulphur dichloride; (3) thick diethylaluminum monochloride reacts with sodium sulfide solution again, and disulphur dichloride is changed into sodium-chlor and sulphur.(4) diethylaluminum monochloride obtains finished product through purification step such as washing, removal of impurities.A wherein crucial step is (2), because the chlorination reaction thermal discharge is big, corrodibility is strong, to temperature controlled strict, is the committed step of production process.
Thioethyl ether is a kind of beige liquid, density 1.18g/cm
3, certain corrodibility is arranged.The reaction of thioethyl ether and chlorine is strong exothermic process, generally needs control reaction temperature below 50 ℃, to suppress side reaction.Therefore can in time remove the key issue that reaction heat just becomes chlorination reactor type selecting and design.
The chlorination reactor of thioethyl ether generally adopts glassed steel reaction vessels, interrupter method production at present.In reactor, put into earlier the thioethyl ether of metering, stir and constantly feed chlorine down.The chlorination reaction liberated heat passes away via the chilled brine in the glassed steel reaction vessels chuck.Chlorine feeding speed depends on the heat-transfer capability of reactor.
There are some limitation in glassed steel reaction vessels: the chuck heat transfer area is limited, and the ratio heat transfer area of large vol reactor is littler; Owing to have enamel layer, reduced overall heat transfer coefficient.So its total heat-transfer capability is less.
Industrially adopt chilled brine as heat-transfer medium usually in order to accelerate the heat transfer rate of chlorination reaction still, poor to enlarge heat transfer temperature.But this can increase investment in fixed assets and process cost, and the heat transfer temperature difference value also has only about 60 ℃, still can not satisfy the requirement that in time passes reaction heat rapidly.Exactly because heat transfer rate has limited chlorination reaction velocity.Make the chlorination reaction cycle reach 10-12h sometimes.
Simultaneously because the agitator speed of glassed steel reaction vessels is slower, stirring rake efficient is lower, and is strong inadequately to the crushing force of chlorine bubbles, thereby limited gas-liquid contact area and mass transfer velocity.In whole liquid phase, local cl concn is higher, and degree of depth chlorination side reaction easily takes place; And the fringe region cl concn is very low, and speed of response is very slow.
In addition, the facility investment of glassed steel reaction vessels unit's reaction volume and stirring power consumption are also bigger, have increased production cost.
Chlorination reaction belongs to the heterogeneous rapid reaction of gas-liquid, and the major influence factors of speed of response is two-phase contact area rather than liquid phase volume.So chlorination reaction is suitable for adopting useful volume little and contact area and the big reactor of heat transfer area.
Substitute the chlorination reactor of glassed steel reaction vessels, need (1) to have the good gas-liquid effect that contacts; (2) has the superior corrosion resistance energy; (3) has powerful heat-transfer capability; (4) keep clear not blocked; (5) be convenient to realize continuous operation and control automatically.
Task of the present invention is, the chlorination reaction process of thioethyl ether is analyzed, and proposes to strengthen the measure of chlorination reaction process mass-and heat-transfer, makes chlorination reaction process realize serialization or semicontinuous, shortens the time of chlorination reaction, improves the process yield.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of continuous chlorination and produce the reaction process of diethylaluminum monochloride, by the concentration that adopts the resultant diethylaluminum monochloride to come the thioethyl ether of one of diluting reaction thing, thereby control chlorination reaction velocity and heat release speed, adopt gas liquid mixer to strengthen the mass transfer of inhomogeneous reaction thing simultaneously, adopt the strong corrosion-resistant multitubular reactor strengthening heat transfer of heat-transfer capability, improve reaction efficiency.
The present invention realizes by following technical scheme:
A kind of continuous chlorination is produced the reaction process of diethylaluminum monochloride, is to realize by following step:
(1) fresh thioethyl ether mixes with the thick diethylaluminum monochloride of certain flow and round-robin, imports the recycle system of being made up of material mixer, head tank, reaction mixer, shell and tube reactor, gas-liquid separator, reaction water cooler and reactors in series continuously;
(2) chlorine is fed described reaction mixer, and carry out initial reaction with thioethyl ether therein, the mixture with certain transformation efficiency evenly flows into shell and tube reactor;
(3) after mixture evenly flows into each root tubulation of shell and tube reactor, being plug flow in shell and tube reactor flows through, proceed chlorination reaction on one side, heat transferring medium spreads out of reaction heat outside tubulation on one side, gas-liquid separator is gone in the post reaction mixture materials flow, isolate byproduct hydrogen chloride gas therein, enter the absorption tower and generate hydrochloric acid.The reactor cooling that is cooled is gone in the liquid form mixt materials flow, and unreacted material further reacts, and generates thick diethylaluminum monochloride;
(4) behind the thick continuous outflow reactor of diethylaluminum monochloride, the one tunnel leaves this recycle system, enters the after-ripening reactor by discharging pump; One the tunnel loops back material mixer, and the dilution thioethyl ether is proceeded chlorination reaction.By diluting reaction raw material thioethyl ether, controlled speed of response and heat release speed, rapid absorption reaction heat, effective control reaction temperature, thus improved the efficient of reacting.Shorten the time of chlorination reaction greatly.
Described head tank, shell-and-tube reactor, reaction water cooler, reactor and after-ripening reactor all have the heat exchange refrigerating function.Head tank, reactor and after-ripening reactor are all at the outside cooling jacket that coats of kettle, raw material thioethyl ether and the thick diethylaluminum monochloride of round-robin resultant before circulating reaction through in advance the cooling, the chlorination reaction liberated heat takes place in reaction mixer like this can more be absorbed by material itself, reaches the purpose of removing reaction heat rapidly.Each step of circulating reaction can both be controlled at below the specified temperature.
Described material mixer and reaction mixer adopt corrosion resistant material to make.Reaction solution and chlorine can Rapid and uniform mixing in reaction mixer, and chlorination reaction takes place immediately.Described corrosion-resistant mixing tank also can the tolerance response temperature.Gas-liquid two-phase flow at high speed in reaction mixer produces strong turbulence, promotes mass transfer between the two-phase, accelerates main reaction speed, reduces the growing amount of by product simultaneously.
Described shell and tube reactor can provide sizable heat transfer ratio surface-area, can in time reaction heat be passed to heat transferring medium, and temperature of reaction is effectively controlled, and its reaction compartment can satisfy gas-liquid two-phase quick response needs simultaneously.
Described after-ripening reactor can be 1,2 or some series connection, guarantees that wherein unreacted thioethyl ether is all transformed with chlorine reaction.
Described diethylaluminum monochloride continuous processing production technique can be 80-85% with the transformation efficiency of controlling chlorination reaction by the flow of regulating pump flow, chlorine flowrate, thioethyl ether flow and refrigerant body, can avoid occurring sulfidal under this transformation efficiency, reaction solution keeps the clear solution state.
A kind of continuous chlorination is produced the system and device of the reaction process of diethylaluminum monochloride, comprise raw material storage tanks, material mixer, head tank, reaction mixer, shell and tube reactor, gas-liquid separator, the reaction water cooler, reactor, the after-ripening reactor, the chlorine plenum system, feedstock pump and recycle pump, described material mixer, head tank, feedstock pump, reaction mixer, shell and tube reactor, gas-liquid separator, the reaction water cooler, reactor and recycle pump are serially connected in loop successively, described raw material storage tanks connects material mixer, described chlorine plenum system ligation mixing tank, described after-ripening reactor one end ligation device, the other end connects the chlorine plenum system.
Described chlorine plenum system comprises liquid chlorine cylinder and chlorine vaporization surge tank; The external discharging pump of described after-ripening reactor.
The system and device of the reaction process of described continuous chlorination production diethylaluminum monochloride can be simplified according to its principle, according to practice in factory, realizes semicontinuous chlorination reaction process with less equipment, improves the speed of reaction than interrupter method chloridization process.In described semicontinuous chlorination reaction flow process, with the disposable input reactor of a collection of thioethyl ether, extract out with recycle pump, in reaction mixer, also react with the chlorine short mix, directly enter the coronite cooling of shell and tube reactor limit then, material flows into reactor again and carries out gas-liquid separation, and byproduct hydrogen chloride gas is absorbed tower absorption becoming hydrochloric acid, original mixing of materials is even in liquid phase material and the reactor, is pumped to reaction mixer and chlorine reaction by recycle pump again.So constantly circulating reaction, cooling, the transformation efficiency of thioethyl ether progressively improves, and up to reaching desired transformation efficiency, begins the next batch operation after the discharging again.
Beneficial effect of the present invention is:
(1) adopts corrosion resistant material mixer, reaction mixer and shell and tube reactor, have good gas-liquid mass transfer effect and powerful heat-transfer capability, can absorb or remove chlorination reaction heat rapidly, accelerate the speed that chlorine feeds, shorten the time of chlorination reaction;
(2) adopt the thick diethylaluminum monochloride diluting reaction of resultant thing thioethyl ether, control reactant concn and speed of response, rapid absorption reaction liberated heat, effective control reaction temperature, thus improve the selectivity of reaction;
(3) by the continuous reaction method, the transformation efficiency of Control Circulation reactive system reacts under optimum transformation efficiency, and by product is few.The production of serialization simultaneously helps adopting automatic control, reduces facility investment, stabilized product quality.
Description of drawings
Fig. 1 is the general flow chart of diethylaluminum monochloride successive reaction production technique
Fig. 2 is the general flow chart of the semicontinuous reaction production technique of diethylaluminum monochloride
Embodiment
Below in conjunction with drawings and Examples, the present invention will be further described.
As Fig. 1, be the general flow chart of diethylaluminum monochloride successive reaction production technique, be the explanation that the method for diethylaluminum monochloride successive reaction production technique is specially a whole set of device for carrying out said.Comprise raw material storage tanks 1, feedstock pump 2 and 6, material mixer 3, head tank 4, strainer 5, material flow meter 7, reaction mixer 8, shell and tube reactor 9, gas-liquid separator 22, reaction water cooler 10, reactor 11, recycle pump 12, circular flow meter 13, discharging flow meter 14, after-ripening reactor 15, discharging pump 16, liquid chlorine cylinder 17, chlorine vaporization surge tank 18, chlorine main flow meter 19, the secondary under meter 20 of chlorine.Wherein, material mixer 3, head tank 4, strainer 5, feedstock pump 6, material flow meter 7, reaction mixer 8, shell and tube reactor 9, gas-liquid separator 22, reaction water cooler 10, reactor 11, recycle pump 12, the circular flow meter 13 formation loop that is connected in series is successively formed continuous circulation system; Raw material storage tanks 1 is connected material mixer 3 by feedstock pump 2 with material flow meter 21 successively; Liquid chlorine cylinder 17 connects Chlorine Buffer Vessel 18, and chlorine vaporization surge tank 18 connects after-ripening reactor 15 again by chlorine main flow meter 19 ligation mixing tanks 8 by the secondary under meter 20 of chlorine; After-ripening reactor 15 is by discharging flow meter 14 ligation devices 11; Gas-liquid separator 22 also connects hydrochloric acid absorption tower at the top.
The flow process of diethylaluminum monochloride successive reaction production technique is as follows:
(1) in the circulation loop system that is composed in series successively by material mixer 3, head tank 4, strainer 5, feedstock pump 6, material flow meter 7, reaction mixer 8, shell and tube reactor 9, gas-liquid separator 22, reaction water cooler 10, recycle pump 12, circular flow meter 13, there is thick diethylaluminum monochloride to circulate, one of reaction raw materials thioethyl ether is from raw material storage tanks 1, pass through the control of feedstock pump 6 and material flow meter 21 successively, thioethyl ether is pumped into material mixer 3 with certain flow, mix with the thick diethylaluminum monochloride of circulation therein.With the thick diethylaluminum monochloride of round-robin dilution thioethyl ether reducing its concentration, thereby can reduce follow-up chlorination reaction velocity that carries out and heat release speed.The said mixture material feeds head tank 4, and its outside coats cooling jacket, has heat exchange refrigerative function.Can be to its inner refrigerant body, for example chilled brine of feeding.Acting as of head tank 4 cooled off mixture in advance, can more be absorbed in chlorination reaction institute liberated heat takes place in the subsequent reactions mixing tank, reaches effective control reaction temperature, accelerates the purpose that chlorine feeds speed.
After pre-cooled mixture is removed particulate contamination by the strainer 5 of its connection in head tank 4, by feedstock pump 6 and material flow meter 7, be admitted to reaction mixer 8 successively.
Above-mentioned material mixer 3 and reaction mixer 8 all adopt corrosion resistant material to make.Mixture and chlorine can Rapid and uniform mixing in reaction mixer, and chlorination reaction takes place immediately.Above-mentioned corrosion-resistant material mixer 3 and reaction mixer 8 also can the tolerance response temperature.Gas-liquid two-phase flow at high speed in reaction mixer produces strong turbulence, promotes mass transfer between the two-phase, accelerates main reaction speed, reduces the growing amount of by product simultaneously.
(2) chlorine in the liquid chlorine cylinder 17 enters chlorine vaporization surge tank 18 by valve, in chlorine vaporization surge tank 18, can control the temperature and pressure of chlorine, makes it within the scope that chlorination reaction requires.By chlorine main flow meter 19 chlorine is fed reaction mixer 8 then.Because the mixture that feeds from head tank 4 is lowered the temperature in advance before, so the preliminary chlorination reaction liberated heat that carries out in reaction mixer can more be absorbed by reaction mass itself.Thereby make chlorination reaction liquid be lower than design temperature (for example 50 ℃) all the time.Temperature sensor control chlorine by reaction mixer 8 exits adds speed.Mixture with certain transformation efficiency evenly flows into shell and tube reactor 9.
(3) after mixture evenly flows into each root tubulation of shell and tube reactor 9, in shell and tube reactor 9, be plug flow and flow through, Yi Bian the chlorination reaction of proceeding, Yi Bian heat transferring medium spreads out of reaction heat outside tubulation.Described shell and tube reactor 9 can provide sizable heat transfer ratio surface-area, can in time reaction heat be passed to heat transferring medium, and temperature of reaction is effectively controlled, and its reaction compartment can satisfy gas-liquid two-phase quick response needs simultaneously.
Gas-liquid separator 22 is gone in the post reaction mixture materials flow, isolates byproduct hydrogen chloride gas therein, enters hydrochloric acid absorption tower and generates by-product hydrochloric acid.The liquid form mixt material is further lowered the temperature by reaction water cooler 10, and inflow reactor 11 then, the reactor 11 outside cooling jackets that coat, inner refrigerant body, for example chilled brine of feeding.Unreacted thioethyl ether can further react, and generates thick diethylaluminum monochloride.
In whole chlorination reaction process, flow by Control Circulation pump 12 flows, chlorine flowrate, thioethyl ether flow and refrigerant body, the chlorination reaction transformation efficiency that comes the Control Circulation loop is 80-85%, can avoid occurring sulfidal under this transformation efficiency, keeps reaction solution clear solution state.
(4) the thick diethylaluminum monochloride of Sheng Chenging flows out from reactor 11 bottoms, is divided into two-way: lead up to recycle pump 12 and discharging flow meter 14, leave this recycle system, enter after-ripening reactor 15.Chlorine feeds after-ripening reactor 15 through the secondary under meter 20 of chlorine simultaneously, to improve chlorination reaction.After-ripening reactor 15 can be 1,2 or some series connection, guarantees that wherein unreacted thioethyl ether all transforms.After-ripening reactor 15 bottoms are delivered to follow-up quaternization and refining manufacturing procedure by discharging pump 16 and discharging flow meter 141 with thick diethylaluminum monochloride.
The thick diethylaluminum monochloride in another road of reactor 11 bottom discharges returns material mixer 3 by recycle pump 12 and circular flow meter 13, carries out the chlorination reaction circulation of a new round.
Part circulation by above-mentioned thick diethylaluminum monochloride, diluting reaction raw material thioethyl ether, effectively controls reaction speed and heat release speed, absorption reaction liberated heat rapidly, thereby effective control reaction temperature, the efficient of raising chlorination reaction.Shorten the time of chlorination reaction greatly.
According to the ultimate principle of above-mentioned diethylaluminum monochloride continuous processing production technique, can simplify flow process according to the practical situation of factory, adopt diethylaluminum monochloride semi-continuous production technology.
As Fig. 2, the general flow chart of the semicontinuous reaction production technique of diethylaluminum monochloride.Comprise raw material storage tanks 23, reactor 24, strainer 25, recycle pump 26, circular flow meter 27, reaction mixer 28, shell and tube reactor 29, liquid chlorine cylinder 30, liquid chlorine vaporizing jar 31, Chlorine Buffer Vessel 32, chlorine main flow meter 33, the secondary under meter 34 of chlorine.Wherein reactor 24, strainer 25, recycle pump 26, circular flow meter 27, reaction mixer 28, shell and tube reactor 29 are composed in series circulation loop successively, after liquid chlorine cylinder 30, liquid chlorine vaporizing jar 31, Chlorine Buffer Vessel 32 connect successively, by chlorine main flow meter 33 ligation mixing tanks 28; By the secondary under meter 34 ligation stills 24 of chlorine.
The aforesaid reaction vessel 24 outside cooling jackets that coat, the inner refrigerant body that feeds can be by heat exchange effect cooling reaction mass.
Thioethyl ether in the raw material storage tanks 23 is imported reactor 24, and feeding refrigerant body is pre-cooled to thioethyl ether in reactor 24 chucks, by strainer 25 and recycle pump 26, thioethyl ether is pumped into reaction mixer 28 afterwards.
Liquid chlorine in the liquid chlorine cylinder 30 feeds liquid chlorine vaporizing jar 31, Chlorine Buffer Vessel 32, adjust temperature and pressure after, by chlorine main flow meter 33, chlorine is sent into reaction mixer 28, react with wherein thioethyl ether.Because reaction mass cools off in advance, so the heat that preliminary chlorination reaction produces in reaction mixer is absorbed rapidly by material itself.Mixture enters shell and tube reactor 29 further reaction and externally heat transfer immediately, and cooled material returns reactor 24, and is even with original mixing of materials in the reactor.Extract the chlorination reaction circulation of carrying out a new round out with recycle pump once more.So constantly react-refrigeration cycle, the transformation efficiency of thioethyl ether improves constantly, until reacting completely.The wherein related reaction principle and the advantage of shell and tube reactor are identical with the continuous production flow process.
Below in conjunction with embodiment, the flow process of above-mentioned diethylaluminum monochloride successive reaction production technique and the flow process of the semicontinuous reaction production technique of diethylaluminum monochloride are described.
Embodiment 1
The flow process of diethylaluminum monochloride successive reaction production technique
Leave the thioethyl ether of raw material storage tanks in, extract out with feedstock pump, flow is 120L/h.Thick diethylaluminum monochloride is extracted out with recycle pump from reactor, and flow is about 1300L/h.Two strands of materials mix in material mixer, and flowing through area is 5m
2The shell and tube cooler tube side, shell side is lowered the temperature with chilled brine, enters the head tank of 1000L then.The hybrid reaction material pumps into reaction mixer with feedstock pump, mixes with the chlorine of 0.2-0.3MPa therein.The flow of chlorine is regulated according to the reaction mixer temperature out, and top temperature is controlled at below 60 ℃.
The effusive reaction solution of reaction mixer enters shell and tube reactor, proceeds chlorination reaction in its tubulation.Simultaneously reaction heat is passed to mobile chilled brine in the shell side.The heat transfer area of shell and tube reactor is 10m
2
The reaction mass temperature of leaving shell and tube reactor is 35 ℃, enters gas-liquid separator, isolates hydrogen chloride gas.The hydrogenchloride water absorbs produces by-product hydrochloric acid.Liquid phase stream is crossed the tube side of shell and tube cooler, and its heat interchanging area is 5m
2, shell side cools off with chilled brine.Reaction mass cooling back temperature is reduced to 22 ℃, and flowing into volume is the reactor of 2000L.Thioethyl ether transformation efficiency wherein is not higher than 85%.Material is divided into two-way and flows out in the reactor: leading up to recycle pump and circular flow meter returns material mixer as recycle stock.The after-ripening reactor of 2000L is sent into by recycle pump and discharging flow meter in another road, further improves reaction with the chlorine that replenishes therein, and it is yellow muddy that reaction solution is become.The transformation efficiency of thioethyl ether reaches more than 99%.The reaction solution of after-ripening reactor is extracted out with discharging pump, sends into thick muriate storage tank continuously, carries out next step operation.
Embodiment 2
The flow process of the semicontinuous reaction production technique of diethylaluminum monochloride
In the 2000L glassed steel reaction vessels, put into the 1200kg thioethyl ether.Be cooled to 30 ℃ with the chuck chilled brine.Thioethyl ether is extracted out with recycle pump, and flow is 3600L/h, sends into reaction mixer.Mix with the chlorine of 0.2-0.3MPa therein.The flow of regulating chlorine is lower than 60 ℃ with the temperature of controlling the reaction mixer exit.The reaction mass heat transfer area of flowing through then is 10m
2The tube side of shell and tube reactor.Its shell side is made heat-transfer medium with chilled brine.The temperature that material leaves shell and tube reactor is 28-35 ℃, turns back in the glassed steel reaction vessels.Material in reactor is further cooled off by the chuck chilled brine, and temperature drops to 22-28 ℃.Reactor internal reaction thing is constantly extracted out with pump, sends in the reaction mixer and chlorine reaction.Thioethyl ether constantly reduces in the reactive system.React to 4.0h, reaction solution becomes yellow muddy, detects to reach reaction end.Stop to feed chlorine, continue stirring reaction 30min, discharging.Consume chlorine 515kg altogether in a collection of semicontinuous reaction process.
Claims (10)
1. a continuous chlorination is produced the reaction process of diethylaluminum monochloride, it is characterized in that being realizing by following step:
(1) fresh thioethyl ether mixes with the thick diethylaluminum monochloride of certain flow and round-robin, imports the recycle system of being made up of material mixer, head tank, reaction mixer, shell and tube reactor, gas-liquid separator, reaction water cooler and reactors in series continuously;
(2) chlorine is fed described reaction mixer, and carry out initial reaction with thioethyl ether therein, the mixture with certain transformation efficiency evenly flows into shell and tube reactor;
(3) after mixture evenly flows into each root tubulation of shell and tube reactor, be plug flow therein and flow through, Yi Bian the chlorination reaction of proceeding, Yi Bian heat transferring medium spreads out of reaction heat outside tubulation.Gas-liquid separator is gone in the post reaction mixture materials flow, isolate byproduct hydrogen chloride gas therein, enter the absorption tower and generate hydrochloric acid, the liquid form mixt materials flow is gone into reactor and is cooled, unreacted raw material is further reaction in reactor, generates thick diethylaluminum monochloride;
(4) behind the thick continuous outflow reactor of diethylaluminum monochloride, the one tunnel leaves this recycle system, sends into the after-ripening reactor by discharging pump and improves chlorination reaction, and one the tunnel loops back material mixer dilution thioethyl ether, returns the recycle system and continues chlorination reaction.
2. continuous chlorination as claimed in claim 1 is produced the reaction process of diethylaluminum monochloride, it is characterized in that the kettle of described head tank, reactor and after-ripening reactor coats cooling jacket outward.
3. continuous chlorination as claimed in claim 1 is produced the reaction process of diethylaluminum monochloride, it is characterized in that described material mixer, head tank, reaction mixer, shell and tube reactor, gas-liquid separator, reactor, after-ripening reactor all adopt corrosion resistant material to make.
4. continuous chlorination as claimed in claim 1 is produced the reaction process of diethylaluminum monochloride, it is characterized in that described after-ripening reactor can be 1,2 or some series connection.
5. continuous chlorination as claimed in claim 1 is produced the reaction process of diethylaluminum monochloride, it is characterized in that and can control reaction process by adjusting fresh feed pump, recycle pump, chlorine flowrate, refrigerant body flow, making the transformation efficiency of the chlorination reaction liquid that flows out the described recycle system is 80-85%.
6. a continuous chlorination is produced the system and device of the reaction process of diethylaluminum monochloride, comprise raw material storage tanks, material mixer, head tank, reaction mixer, shell and tube reactor, gas-liquid separator, the reaction water cooler, reactor, the after-ripening reactor, the chlorine plenum system, feedstock pump and recycle pump, it is characterized in that described material mixer, head tank, feedstock pump, reaction mixer, shell and tube reactor, gas-liquid separator, the reaction water cooler, reactor and recycle pump are serially connected in loop successively, described raw material storage tanks connects material mixer, described chlorine plenum system ligation mixing tank, described after-ripening reactor one end ligation device, the other end connects the chlorine plenum system.
7. continuous chlorination as claimed in claim 6 is produced the system and device of the reaction process of diethylaluminum monochloride, it is characterized in that described chlorine plenum system comprises liquid chlorine cylinder, chlorine vaporization surge tank; The external discharging pump of described after-ripening reactor.
8. continuous chlorination as claimed in claim 6 is produced the system and device of the reaction process of diethylaluminum monochloride, it is characterized in that described after-ripening reactor can be 1,2 or some series connection.
9. continuous chlorination as claimed in claim 6 is produced the system and device of the reaction process of diethylaluminum monochloride, it is characterized in that the kettle of described head tank, reactor and after-ripening reactor coats cooling jacket outward.
10. continuous chlorination as claimed in claim 6 is produced the system and device of the reaction process of diethylaluminum monochloride, it is characterized in that carrying out device simplifies, comprise raw material storage tanks, reactor, strainer, recycle pump, the circular flow meter, reaction mixer, shell and tube reactor, liquid chlorine cylinder, the liquid chlorine vaporizing jar, Chlorine Buffer Vessel, chlorine main flow meter, the secondary under meter of chlorine, it is characterized in that raw material storage tanks, reactor, strainer, recycle pump, the circular flow meter, reaction mixer, shell and tube reactor is composed in series the recycle system successively, liquid chlorine cylinder, the liquid chlorine vaporizing jar, after Chlorine Buffer Vessel connects successively, by chlorine main flow meter ligation mixing tank, by the secondary under meter ligation of chlorine device.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103664698A (en) * | 2013-12-18 | 2014-03-26 | 湖南化工研究院 | 2-cyanophenol preparing method |
| CN107325046A (en) * | 2017-06-19 | 2017-11-07 | 南京大学 | The liquid phase chlorination method production technology and device of a kind of cyanopyridine of tetrachloro 2 |
| CN109022035A (en) * | 2018-08-15 | 2018-12-18 | 安徽绿色谷创客空间股份有限公司 | A kind of efficient process units and production method of chlorinated paraffin |
| CN117563534A (en) * | 2024-01-17 | 2024-02-20 | 河南嘉颖生物科技有限公司 | Continuous flow reaction device and method for high-purity O, O-dialkyl thiophosphoryl chloride |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4287136A (en) * | 1980-06-16 | 1981-09-01 | Ciba-Geigy Corporation | Process for the preparation of O,O-dialkylthionophosphoric acid chlorides |
| CN101293897A (en) * | 2008-06-06 | 2008-10-29 | 武汉工程大学 | Method for preparing O,O-ethyl thioether substituted phosphorus oxychloride |
-
2010
- 2010-04-07 CN CN 201010141353 patent/CN102030774A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4287136A (en) * | 1980-06-16 | 1981-09-01 | Ciba-Geigy Corporation | Process for the preparation of O,O-dialkylthionophosphoric acid chlorides |
| CN101293897A (en) * | 2008-06-06 | 2008-10-29 | 武汉工程大学 | Method for preparing O,O-ethyl thioether substituted phosphorus oxychloride |
Non-Patent Citations (1)
| Title |
|---|
| 《现代农药》 20061231 田昌明等 合成中间体O,O-二乙基硫代磷酰氯的工艺改进 第14-15页 1-10 第5卷, 第6期 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103664698A (en) * | 2013-12-18 | 2014-03-26 | 湖南化工研究院 | 2-cyanophenol preparing method |
| CN103664698B (en) * | 2013-12-18 | 2015-12-09 | 湖南化工研究院 | The preparation method of o-hydroxy nitrile |
| CN107325046A (en) * | 2017-06-19 | 2017-11-07 | 南京大学 | The liquid phase chlorination method production technology and device of a kind of cyanopyridine of tetrachloro 2 |
| CN109022035A (en) * | 2018-08-15 | 2018-12-18 | 安徽绿色谷创客空间股份有限公司 | A kind of efficient process units and production method of chlorinated paraffin |
| CN117563534A (en) * | 2024-01-17 | 2024-02-20 | 河南嘉颖生物科技有限公司 | Continuous flow reaction device and method for high-purity O, O-dialkyl thiophosphoryl chloride |
| CN117563534B (en) * | 2024-01-17 | 2024-04-05 | 河南嘉颖生物科技有限公司 | Continuous flow reaction device and method for high-purity O, O-dialkyl thiophosphoryl chloride |
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