CN106565774A - Continuous tower-type washing method of O,O-dimethylphosphoroamidothioate crude product - Google Patents

Continuous tower-type washing method of O,O-dimethylphosphoroamidothioate crude product Download PDF

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Publication number
CN106565774A
CN106565774A CN201610969386.6A CN201610969386A CN106565774A CN 106565774 A CN106565774 A CN 106565774A CN 201610969386 A CN201610969386 A CN 201610969386A CN 106565774 A CN106565774 A CN 106565774A
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tower
heavy
phase
extraction tower
heavy phase
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Inventor
刘安平
殷宏
薛光才
王洪群
刘孝平
段然
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Hubei Shalongda Co Ltd
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Hubei Shalongda Co Ltd
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Priority to CN201610969386.6A priority Critical patent/CN106565774A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00Compounds containing elements of Groups 5 or 15 of the Periodic Table
    • C07F9/02Phosphorus compounds
    • C07F9/06Phosphorus compounds without P—C bonds
    • C07F9/22Amides of acids of phosphorus
    • C07F9/24Esteramides
    • C07F9/2454Esteramides the amide moiety containing a substituent or a structure which is considered as characteristic
    • C07F9/2458Esteramides the amide moiety containing a substituent or a structure which is considered as characteristic of aliphatic amines

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention discloses a continuous tower-type washing method of O,O-dimethylphosphoroamidothioate crude product. The method includes the following steps that (1) the O,O-dimethylphosphoroamidothioate crude product serves as a raw material, and pure water serves as an extraction agent; (2) the O,O-dimethylphosphoroamidothioate crude product serves as a heavy phase to be continuously injected into an extraction tower from a heavy phase inlet of the extraction tower, the pure water serves as a light phase to be continuously injected into the extraction tower from a light phase inlet of the extraction tower, after the light phase and the heavy phase are in sufficient contact, the heavy phase flows out of a heavy phase outlet of the extraction tower, and the light phase flows out of a light phase outlet of the extraction tower; and (3) timing is carried out when water flows out from the light phase outlet of the extraction tower, heavy phase samples flowing out from the heavy phase outlet of the extraction tower start to be collected after 4 h to 6 h, the content of ammonium chloride in the heavy phase samples is detected, and the heavy phase flowing out from the heavy phase outlet starts to be stored after the content of ammonium chloride in the heavy phase samples is smaller than 0.1%. By means of the method, the content of ammonium chloride in the O,O-dimethylphosphoroamidothioate crude product can be effectively reduced.

Description

The continuous tower-type method for washing of O, O- dimethyl thiophosphoryl amide crude product
Technical field
The present invention relates to organophosphorus pesticide field, more particularly to a kind of continuous tower of O, O- dimethyl thiophosphoryl amide crude product Formula method for washing.
Background technology
O, O- dimethyl thiophosphoryl amide is the important intermediate of organophosphorus insecticide orthene, the end of the year 2015, entirely Ball often produces O, about 100,000 tons of O- dimethyl thiophosphoryl amides per year, and my company often produces O per year, about 40,000 tons of O- dimethyl thiophosphoryl amides, The 40% of whole world annual output is accounted for, a certain amount of ammonium chloride can be mingled with during producing O, O- dimethyl thiophosphoryl amides, be mingled with Ammonium chloride content it is higher when, during follow-up vacuum dehydration spermine, have more ammonium chloride distillation blocking true Vacant duct and vacuum pump, cause to overhaul frequency height so that production efficiency declines, production cost is raised.
In prior art, the method for O, O- dimethyl thiophosphoryl amide crude product separating ammonium chloride is that tubular type is washed, i.e. O, O- Dimethyl thiophosphoryl amide crude product and water first mixes with pump by a certain percentage, separation water and thick amine in phase separator again, this kind of The isolated O of mode, in O- dimethyl thiophosphoryl amides the content of ammonium chloride more than 0.5%, the content of ammonium chloride still compared with Height, during follow-up spermine processed, can still block vacuum pipe and vacuum pump.
The content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art, there is provided a kind of to reduce O, O- dimethyl thiophosphoryl amide crude products The continuous tower-type method for washing of middle ammonium chloride content.
A kind of continuous tower-type method for washing of O, O- dimethyl thiophosphoryl amide crude product, comprises the following steps:
1) raw material and extractant are prepared:Raw material is O, O- dimethyl thiophosphoryl amide crude products, O, O- dimethyl thio phosphinylidyne Amine crude product is the mixture of O, O- dimethyl thiophosphoryl amides and ammonium chloride;Extractant is pure water;Pure water and O, O- dimethyl disulfide It is immiscible for phosphamide, and dissolubility of the ammonium chloride in pure water is more than the dissolving in O, O- dimethyl thiophosphoryl amides Degree, can efficiently extract ammonium chloride as extractant using pure water, and pure water is nontoxic, low price.
2) continuous washing:O, O- dimethyl thiophosphoryl amide crude product is continuously noted from the heavy liquid inlet of extraction tower as heavy phase Enter;Pure water is continuously injected into from the light phase inlet of extraction tower as light phase;Heavy phase is constantly settled downwards, light phase continuous rising, light phase After being fully contacted with heavy phase, heavy phase is flowed out from the heavy out of extraction tower, and the light phase light phase export from extraction tower flows out;
3) sample, analysis:Start timing when the light phase export of extraction tower there are flowing out, start to collect after 4~6 hours from extraction The heavy phase sample that the heavy out of tower flows out is taken, the content of ammonium chloride in heavy phase sample is tested and analyzed;The chlorine in heavy phase sample After the content of change ammonium is less than 0.1%, start to store from heavy out the heavy phase for flowing out;When the content of ammonium chloride in heavy phase sample it is little In 0.1%, be conducive to the process in follow-up vacuum dehydration spermine, prevent vacuum pipe and vacuum pump blocking.
Preferably, the extraction tower is turntable extracting tower or packed extraction tower.
Preferably, the extraction tower is turntable extracting tower, and the rotating speed for controlling turntable extracting tower is 300~500r/ Min, controls O, and the charging rate of O- dimethyl thiophosphoryl amide crude products is 5000~7000kg/h, controls the speed of pure water feed For 500~700kg/h, the temperature for controlling turntable extracting tower is 25~35 DEG C, and the turntable extracting tower is high 14~16 meters, rotating disk extraction A diameter of 0.8~1.0 meter of tower is taken, a diameter of 0.5~0.7 meter of rotating disk, plate spacing is 0.3~0.5 meter, and the number of column plate is 30~40 pieces;By the rotating speed for controlling turntable extracting tower, the parameter such as charging rate and temperature realizes pure water and O, O- dimethyl Thio-phosphamide crude product is preferably contacted, and reaches preferably effect of extracting.
Preferably, step 2) continuous washing combines washing process using turntable extracting tower with packed extraction tower, i.e., O, O- dimethyl thiophosphoryl amide crude product carries out initial water wash first with turntable extracting tower, by the heavy out of turntable extracting tower The heavy phase of outflow is passed through the heavy liquid inlet of packed extraction tower and further washes;Largely can go first with turntable extracting tower Except O, the ammonium chloride in O- dimethyl thiophosphoryl amide crude products, then ammonium chloride is further removed using packed extraction tower, it is maximum Limit ground removes O, ammonium chloride in O- dimethyl thiophosphoryl amide crude products.
It is an advantage of the current invention that:The method can be effectively reduced O, ammonium chloride in O- dimethyl thiophosphoryl amide crude products Content, prevents ammonium chloride during follow-up vacuum dehydration spermine, blocks vacuum pipe and vacuum pump, and the method is simple, It is easy to operate, it is using pure water as extractant, nontoxic, reduce to environment ground contamination.
Description of the drawings
Structural representations of the Fig. 1 for the turntable extracting tower of embodiment 1~3;
Fig. 2 combines water washing device structural representation for the turntable extracting tower of embodiment 4 with packed extraction tower;
In figure, each part numbers are as follows:The heavy liquid inlet 1.1, turntable extracting tower of turntable extracting tower 1, turntable extracting tower it is light The heavy out 1.4 of the light phase export 1.3, turntable extracting tower of phase entrance 1.2, turntable extracting tower, packed extraction tower 2, filler extraction Take the light phase export 2.3, packed extraction tower of the light phase inlet 2.2, packed extraction tower of the heavy liquid inlet 2.1, packed extraction tower of tower Heavy out 2.4.
Specific embodiment
To more fully understand the present invention, invention is described in detail below with reference to accompanying drawing and instantiation.
To solve to there is O in prior art, the higher problem of the content of ammonium chloride in O- dimethyl thiophosphoryl amide crude products, The present invention provides a kind of reduction O, and the continuous tower-type method for washing of the content of ammonium chloride in O- dimethyl thiophosphoryl amide crude products should By extracting tower apparatus, method realizes that, specifically, by O, used as heavy phase, pure water is used as light for O- dimethyl thiophosphoryl amides crude product Phase, the dissolubility using ammonium chloride in pure water realize O, O- diformazans more than the dissolubility in O, O- dimethyl thiophosphoryl amides Ammonium chloride in base thio-phosphamide crude product is transferred in pure water, and reduces O from realization, in O- dimethyl thiophosphoryl amide crude products The content of ammonium chloride.Below by by specific embodiment come to the present invention optimal way be described in detail.
Embodiment 1
A kind of continuous tower-type method for washing of O, O- dimethyl thiophosphoryl amide crude product, with reference to shown in Fig. 1, is extracted by rotating disk Take tower 1 to realize, specifically include following steps:
1) raw material and extractant are prepared:Raw material is O, O- dimethyl thiophosphoryl amide crude products, O, O- dimethyl thio phosphinylidyne Amine crude product is the mixture of O, O- dimethyl thiophosphoryl amides and ammonium chloride, and wherein the content of ammonium chloride is 0.56%;Extractant For pure water;
2) continuous washing:O, O- dimethyl thiophosphoryl amide crude product as heavy phase, from the heavy liquid inlet 1.1 of turntable extracting tower It is continuously injected into;Pure water is continuously injected into from the light phase inlet 1.2 of turntable extracting tower as light phase;The rotating speed of control turntable extracting tower For 300r/min, the charging rate of O, O- dimethyl thiophosphoryl amide crude product is 5000kg/h, and the speed of pure water feed is 500kg/h, the temperature of turntable extracting tower is 25 DEG C, and the turntable extracting tower is high 15 meters, a diameter of 0.9 meter of turntable extracting tower, A diameter of 0.6 meter of rotating disk, plate spacing are 0.4 meter, and the number of column plate is 35 pieces;
In the presence of the rotating disk of rotation, heavy phase is constantly settled downwards, light phase continuous rising, light phase to be fully contacted with heavy phase Afterwards, heavy phase is flowed out from the heavy out 1.4 of turntable extracting tower, light phase to flow out from the light phase export 1.3 of turntable extracting tower;
3) sample, analysis:The light phase export 1.3 of turntable extracting tower starts timing when there are flowing out, start to collect after 5 hours From the heavy phase sample that the heavy out 1.4 of turntable extracting tower flows out, the content of ammonium chloride in heavy phase sample is tested and analyzed;Jing is examined Survey, the content of ammonium chloride is 0.07% in heavy phase sample, reach the standard of the content of ammonium chloride less than 0.1%, start to store from The heavy phase that the heavy out 1.4 of turntable extracting tower flows out.
Embodiment 2
A kind of continuous tower-type method for washing of O, O- dimethyl thiophosphoryl amide crude product, with reference to shown in Fig. 1, is extracted by rotating disk Take tower 1 to realize, specifically include following steps:
1) raw material and extractant are prepared:Raw material is O, O- dimethyl thiophosphoryl amide crude products, O, O- dimethyl thio phosphinylidyne Amine crude product is the mixture of O, O- dimethyl thiophosphoryl amides and ammonium chloride, and wherein the content of ammonium chloride is 0.56%;Extractant For pure water;
2) continuous washing:O, O- dimethyl thiophosphoryl amide crude product as heavy phase, from the heavy liquid inlet 1.1 of turntable extracting tower It is continuously injected into;Pure water is continuously injected into from the light phase inlet 1.2 of turntable extracting tower as light phase;The rotating speed of control turntable extracting tower For 400r/min, the charging rate of O, O- dimethyl thiophosphoryl amide crude product is 6000kg/h, and the speed of pure water feed is 600kg/h, the temperature of turntable extracting tower is 30 DEG C, and the turntable extracting tower is high 14 meters, a diameter of 0.8 meter of turntable extracting tower, A diameter of 0.5 meter of rotating disk, plate spacing are 0.3 meter, and the number of column plate is 30 pieces;
In the presence of the rotating disk of rotation, heavy phase is constantly settled downwards, light phase continuous rising, light phase to be fully contacted with heavy phase Afterwards, heavy phase is flowed out from the heavy out 1.4 of turntable extracting tower, light phase to flow out from the light phase export 1.3 of turntable extracting tower;
3) sample, analysis:The light phase export 1.3 of turntable extracting tower starts timing when there are flowing out, start to collect after 4 hours From the heavy phase sample that the heavy out 1.4 of turntable extracting tower flows out, the content of ammonium chloride in heavy phase sample is tested and analyzed;Jing is examined Survey, the content of ammonium chloride is 0.095% in heavy phase sample, reach the standard of the content of ammonium chloride less than 0.1%, start to store from The heavy phase that the heavy out 1.4 of turntable extracting tower flows out.
Embodiment 3
A kind of continuous tower-type method for washing of O, O- dimethyl thiophosphoryl amide crude product, with reference to shown in Fig. 1, is extracted by rotating disk Take tower 1 to realize, specifically include following steps:
1) raw material and extractant are prepared:Raw material is O, O- dimethyl thiophosphoryl amide crude products, O, O- dimethyl thio phosphinylidyne Amine crude product is the mixture of O, O- dimethyl thiophosphoryl amides and ammonium chloride, and wherein the content of ammonium chloride is 0.56%;Extractant For pure water;
2) continuous washing:O, O- dimethyl thiophosphoryl amide crude product as heavy phase, from the heavy liquid inlet 1.1 of turntable extracting tower It is continuously injected into;Pure water is continuously injected into from the light phase inlet 1.2 of turntable extracting tower as light phase;The rotating speed of control turntable extracting tower For 500r/min, the charging rate of O, O- dimethyl thiophosphoryl amide crude product is 7000kg/h, and the speed of pure water feed is 700kg/h, the temperature of turntable extracting tower is 35 DEG C, and the turntable extracting tower is high 16 meters, a diameter of 1.0 meters of turntable extracting tower, A diameter of 0.7 meter of rotating disk, plate spacing are 0.5 meter, and the number of column plate is 40 pieces;
In the presence of the rotating disk of rotation, heavy phase is constantly settled downwards, light phase continuous rising, light phase to be fully contacted with heavy phase Afterwards, heavy phase is flowed out from the heavy out 1.4 of turntable extracting tower, light phase to flow out from the light phase export 1.3 of turntable extracting tower;
3) sample, analysis:The light phase export 1.3 of turntable extracting tower starts timing when there are flowing out, start to collect after 6 hours From the heavy phase sample that the heavy out 1.4 of turntable extracting tower flows out, the content of ammonium chloride in heavy phase sample is tested and analyzed;Jing is examined Survey, the content of ammonium chloride is 0.065% in heavy phase sample, reach the standard of the content of ammonium chloride less than 0.1%, start to store from The heavy phase that the heavy out 1.4 of turntable extracting tower flows out.
Embodiment 4
A kind of continuous tower-type method for washing of O, O- dimethyl thiophosphoryl amide crude product, with reference to shown in Fig. 2, is extracted by rotating disk Take tower 1 to realize with packed extraction tower 2, specifically include following steps:
1) raw material and extractant are prepared:Raw material is O, O- dimethyl thiophosphoryl amide crude products, O, O- dimethyl thio phosphinylidyne Amine crude product is the mixture of O, O- dimethyl thiophosphoryl amides and ammonium chloride, and wherein the content of ammonium chloride is 0.56%;Extractant For pure water;
2) continuous washing:O, O- dimethyl thiophosphoryl amide crude product as heavy phase, from the heavy liquid inlet 1.1 of turntable extracting tower It is continuously injected into;Pure water is continuously injected into from the light phase inlet 1.2 of turntable extracting tower as light phase;In the presence of the rotating disk of rotation, Heavy phase is constantly settled downwards, light phase continuous rising, after light phase and heavy phase is fully contacted, heavy out of the heavy phase from turntable extracting tower 1.4 flow out, light phase to flow out from the light phase export 1.3 of turntable extracting tower;The heavy phase that turntable extracting tower heavy out 1.4 is flowed out is again The heavy liquid inlet 2.1 of packed extraction tower is passed through, the light phase inlet 2.2 of packed extraction tower is passed through pure water, in the presence of filler, weight Mutually constantly settle downwards, light phase continuous rising, after light phase and heavy phase is fully contacted, heavy out of the heavy phase from packed extraction tower 2.4 flow out, and pure water is flowed out from the light phase export 2.3 of packed extraction tower;
3) sample, analysis:Start timing when there are flowing out from the light phase export 2.3 of packed extraction tower, start to receive after 6 hours Collect from the heavy out 2.4 of packed extraction tower the heavy phase sample for flowing out, test and analyze the content of ammonium chloride in heavy phase sample;Jing is examined Survey, the content of ammonium chloride is 0.015% in heavy phase sample, reach the standard of the content of ammonium chloride less than 0.1%, start to store from The heavy phase that the heavy out 2.4 of packed extraction tower flows out.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more concrete and detailed, but and Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art For, without departing from the inventive concept of the premise, some deformations and improvement can also be made, these belong to the guarantor of the present invention Shield scope.Therefore, the protection domain of patent of the present invention should be defined by claims.

Claims (4)

1. a kind of O, the continuous tower-type method for washing of O- dimethyl thiophosphoryl amide crude products, it is characterised in that:Comprise the following steps:
1) raw material and extractant are prepared:Raw material is O, and O- dimethyl thiophosphoryl amide crude products, O, O- dimethyl thiophosphoryl amide are thick Product are the mixture of O, O- dimethyl thiophosphoryl amides and ammonium chloride;Extractant is pure water;
2) continuous washing:O, O- dimethyl thiophosphoryl amide crude product is continuously injected into from the heavy liquid inlet of extraction tower as heavy phase;It is pure Water is continuously injected into from the light phase inlet of extraction tower as light phase;Heavy phase is constantly settled downwards, light phase continuous rising, light phase and weight After being mutually fully contacted, heavy phase is flowed out from the heavy out of extraction tower, and the light phase light phase export from extraction tower flows out;
3) sample, analysis:Start timing when the light phase export of extraction tower there are flowing out, start to collect after 4~6 hours from extraction tower Heavy out flow out heavy phase sample, test and analyze heavy phase sample in ammonium chloride content;The ammonium chloride in heavy phase sample Content less than after 0.1%, starting to store from heavy out the heavy phase that flows out.
2. O according to claim 1, the continuous tower-type method for washing of O- dimethyl thiophosphoryl amide crude products, its feature exist In:The extraction tower is turntable extracting tower or packed extraction tower.
3. O according to claim 1, the continuous tower-type method for washing of O- dimethyl thiophosphoryl amide crude products, its feature exist In:The extraction tower is turntable extracting tower, and the rotating speed for controlling turntable extracting tower is 300~500r/min, controls O, O- dimethyl The charging rate of thio-phosphamide crude product is 5000~7000kg/h, and the speed for controlling pure water feed is 500~700kg/h, is controlled The temperature of turntable extracting tower processed be 25~35 DEG C, the turntable extracting tower is high 14~16 meters, turntable extracting tower a diameter of 0.8~ 1.0 meters, a diameter of 0.5~0.7 meter of rotating disk, plate spacing is 0.3~0.5 meter, and the number of column plate is 30~40 pieces.
4. O according to claim 1, the continuous tower-type method for washing of O- dimethyl thiophosphoryl amide crude products, its feature exist In:Step 2) continuous washing combines washing process, i.e. O, O- dimethyl thio phosphinylidynes using turntable extracting tower with packed extraction tower Amine crude product carries out initial water wash first with turntable extracting tower, and the heavy phase that the heavy out of turntable extracting tower flows out is passed through filler The heavy liquid inlet of extraction tower is further washed.
CN201610969386.6A 2016-10-27 2016-10-27 Continuous tower-type washing method of O,O-dimethylphosphoroamidothioate crude product Pending CN106565774A (en)

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CN110504489A (en) * 2019-08-12 2019-11-26 河南华瑞高新材料有限公司 A kind of 5V high-voltage lithium nickel manganate anode lithium-ion battery electrolytes

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CN109011694A (en) * 2018-09-21 2018-12-18 山东泓达生物科技有限公司 A kind of novel energy-conserving composite stirring extraction tower
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