CN106316961A - Processing device for reducing DAP impurities through carbendazim production - Google Patents
Processing device for reducing DAP impurities through carbendazim production Download PDFInfo
- Publication number
- CN106316961A CN106316961A CN201610665671.9A CN201610665671A CN106316961A CN 106316961 A CN106316961 A CN 106316961A CN 201610665671 A CN201610665671 A CN 201610665671A CN 106316961 A CN106316961 A CN 106316961A
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- CN
- China
- Prior art keywords
- lightness
- dap
- carbendazim
- condenser
- rectifying
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D235/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings
- C07D235/02—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings condensed with carbocyclic rings or ring systems
- C07D235/04—Benzimidazoles; Hydrogenated benzimidazoles
- C07D235/24—Benzimidazoles; Hydrogenated benzimidazoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 2
- C07D235/30—Nitrogen atoms not forming part of a nitro radical
- C07D235/32—Benzimidazole-2-carbamic acids, unsubstituted or substituted; Esters thereof; Thio-analogues thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/84—Purification
Abstract
The invention discloses a processing device for reducing DAP impurities through carbendazim production. The processing device comprises a light component removal tower, a rectifying tower, a reaction kettle and a belt filter. A feed inlet is formed in the side wall of the middle of the light component removal tower, a light material port is formed in the top of the light component removal tower, a first condenser is located on the portion, below the light material port, in the light component removal tower, a discharge opening is formed in the bottom of the light component removal tower, a rectifying inlet is formed in the side end of the lower portion of the rectifying tower, the rectifying inlet is connected with the discharging opening of the light component removal tower through a pipeline, a residual material discharge opening is formed in the bottom of the rectifying tower, a rectifying outlet is formed in the top of the rectifying tower, the rectifying outlet is sequentially connected with a second condenser, a gas-liquid separator and a draw-off pump through pipelines, the draw-off pump is communicated with the side wall of the rectifying tower through an outer backflow pipe, and the outer backflow pipe is connected with a conveying pipe. The processing device is simple in structure and reasonable in design, and can effectively reduce the DAP content and greatly improve product quality.
Description
Technical field
The present invention relates to pesticide producing technical field of processing equipment, a kind of carbendazim produces and reduces DAP impurity
Processing unit (plant).
Background technology
At present, the production of carbendazim is phosgene and methanol mixed to be reacted generation methylchloroformate, then by prepared chlorine
Reacting in the hydrolyzed solution of methyl formate dropping lime nitrogen, reactant liquor obtains cyanamide base methyl formate through filter pressing；Filter pressing is obtained cyanamide base
Methyl formate o-phenylenediamine mixes, and dropping concentrated hydrochloric acid generates carbendazim, and product obtains many bacterium through centrifuge dehydration, drying
Spirit；Existing technology, when producing cyanamide, uses lime nitrogen method to produce, owing to lime nitrogen decomposes in water in alkalescence, therefore gives birth to
When producing cyanamide, easily producing by-product 2,3 diaminophenol piperazine (DAP), the purity causing cyanamide is the highest, affects cyanogen amidocarbonic acid first
The conversion ratio of ester, and then affect purity and the conversion ratio of carbendazim, the number of DAP content directly influences the quality of carbendazim.
Traditional DAP control method is mainly controlled by early stage rectifying column effect, but carbendazim product when rectification effect is bad
Middle DAP content is the highest, and after ultra micro, content is higher, greatly reduces the production quality of carbendazim.
Summary of the invention
It is an object of the invention to provide a kind of simple in construction, reasonable in design, it is possible to effectively to reduce DAP content, significantly carry
The carbendazim of high product quality produces the processing unit (plant) reducing DAP impurity, with the problem solving to propose in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme:
A kind of carbendazim produces the processing unit (plant) reducing DAP impurity, including lightness-removing column, rectifying column, reactor and belt mistake
Filter, described lightness-removing column center side wall is provided with charging aperture, and lightness-removing column top is provided with gently expects mouth, is positioned at below light material mouth
Lightness-removing column is internally provided with the first condenser, is provided with discharging opening bottom lightness-removing column, and below described rectifying column, side is provided with essence
Evaporating import, rectification import is connected with the discharging opening of lightness-removing column by pipeline, and rectifier bottoms is provided with residual discharging opening, rectifying column
Top is provided with rectification outlet, and rectification outlet is connected with the second condenser, gas-liquid separator and draw-off pump in turn by pipeline, takes out
Take pump to be connected with rectifying column sidewall by exteenal reflux pipe, exteenal reflux pipe connects and has conveying pipe, carry the kettle of pipe and reactor
Charging aperture connects, and described reactor top sidewall is provided with feeding device, is provided with kettle discharging opening, discharging bottom reactor
Mouth is connected with the feed end of band filter by pipeline, and the strainer of described band filter is provided with cleaning shower nozzle.
As the further scheme of the present invention, in described reactor, it is provided with stirring paddle.
As the further scheme of the present invention, described cleaning shower nozzle is connected with cleaning water tank by pipeline, described rinse water
Heater it is provided with in case.
As the further scheme of the present invention, the pipeline between described cleaning water tank and cleaning shower nozzle is provided with and draws water
Pump.
As the further scheme of the present invention, the discharging opening of described lightness-removing column is by the first return duct and lightness-removing column lower end side
Wall connects, and the first return duct is provided with the first reboiler.
As the further scheme of the present invention, described in be positioned on the lightness-removing column above the first condenser be provided with cold with first
What condenser connected is condensed out pipe, is positioned on the lightness-removing column below the first condenser and is provided with the condensation being connected with the first condenser and enters
Pipe.
As the further scheme of the present invention, the residual discharging opening of described rectifying column is by under the second return duct and rectifying column
Side wall connection, the second return duct is provided with the second reboiler.
Compared with prior art, the invention has the beneficial effects as follows: during production, o-phenylenediamine rectification uses double-tower type continuous fine
Evaporating, early stage uses lightness-removing column, sloughs wherein light component, the throat-fed arranged on lightness-removing column center side wall, uses in tower
Internal reflux, bottom discharge is entered inside rectifying column from rectification import by pipeline；Rectification uses exteenal reflux, suppresses heavy constituent, from
O-phenylenediamine is derived in the rectification outlet that rectifying column top is arranged, and o-phenylenediamine content now is more than 99.5%, and DAP/HAP is controlled
System is at below 20ppm, and the second condenser condenser is lowered the temperature；The carbendazim of derivation is entered from the kettle of reactor by pipeline
Expect that mouth adds inside reactor, after condensation insulation terminates a period of time, add suitable additive with DAP knot by feeding device
Close, stir, after question response is thorough, material is imported belt vacuum filter from the kettle discharging opening of reactor, in belt
The leading portion of vacuum filter removes mother solution, then washes away this complex, to reduce DAP's by cleaning shower nozzle hot water classification
Purpose, after material drying, ultra micro, DAP/HAP substantially examines and does not measures, it is possible to effectively reduces DAP content, is greatly improved product product
Matter.Present configuration is simple, reasonable in design, it is possible to effectively reduces DAP content, is greatly improved product quality.
Accompanying drawing explanation
Fig. 1 is the structural representation that a kind of carbendazim produces the processing unit (plant) reducing DAP impurity.
In figure: 1-lightness-removing column, 2-rectifying column, 3-reactor, 4-cleans water tank, 5-band filter, 6-charging aperture, 7-
One condenser, 8-gently expects mouth, and 9-is condensed out pipe, and 10-condenses inlet pipe, 11-discharging opening, 12-the first reboiler, 13-rectification import,
14-remains discharging opening, 15-the second reboiler, and 16-rectification exports, 17-exteenal reflux pipe, 18-the second condenser, 19-gas-liquid separation
Device, 20-draw-off pump, 21-feeding device, 22-kettle charging aperture, 23-kettle discharging opening, 24-cleans shower nozzle, 25-suction pump,
26-stirring paddle.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Describe, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments wholely.Based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under not making creative work premise
Embodiment, broadly falls into the scope of protection of the invention.
Referring to Fig. 1, in the embodiment of the present invention, a kind of carbendazim produces the processing unit (plant) reducing DAP impurity, including de-light
Tower 1, rectifying column 2, reactor 3 and band filter 5, described lightness-removing column 1 center side wall is provided with charging aperture 6, and lightness-removing column 1 pushes up
Portion is provided with light material mouth 8, is positioned at the lightness-removing column 1 below light material mouth 8 and is internally provided with the first condenser 7, arranges bottom lightness-removing column 1
Having discharging opening 11, below described rectifying column 2, side is provided with rectification import 13, and rectification import 13 is by pipeline and lightness-removing column 1
Discharging opening 11 connects, and is provided with residual discharging opening 14 bottom rectifying column 13, and rectifying column 13 top is provided with rectification outlet 16, rectification
Outlet 16 is connected with the second condenser 18, gas-liquid separator 19 and draw-off pump 20 in turn by pipeline, and draw-off pump 20 is returned by outer
Flow tube 17 connects with rectifying column 2 sidewall, exteenal reflux pipe 17 connects and has conveying pipe, and the kettle charging aperture with reactor 3 is managed in conveying
22 connect, and described reactor 3 top sidewall is provided with feeding device 21, is provided with kettle discharging opening 23, goes out bottom reactor 3
Material mouth 23 is connected with the feed end of band filter 5 by pipeline, and the strainer of described band filter 5 is provided with cleaning shower nozzle
24。
Wherein, it is provided with stirring paddle 26 in described reactor 3.
Wherein, described cleaning shower nozzle 24 is connected with cleaning water tank 4 by pipeline, is provided with heating in described cleaning water tank 4
Device.
Wherein, the pipeline between described cleaning water tank 4 and cleaning shower nozzle 24 is provided with suction pump 25.
Wherein, the discharging opening 11 of described lightness-removing column 1 is connected with lightness-removing column 1 lower end sidewall by the first return duct, first time
The first reboiler 12 it is provided with in flow tube.
Wherein, it is positioned at described in and on the lightness-removing column 1 above the first condenser 7, is provided with the condensation being connected with the first condenser 7
Go out pipe 9, be positioned at and on the lightness-removing column 1 below the first condenser 7, be provided with the condensation inlet pipe 10 being connected with the first condenser 7.
Wherein, the residual discharging opening 14 of described rectifying column 2 is connected with rectifying column 2 lower end sidewall by the second return duct, the
The second reboiler 15 it is provided with on two return ducts.
The operation principle of the present invention is: o-phenylenediamine rectification uses double-tower type continuous rectification, and early stage uses lightness-removing column 1, de-
Going wherein light component, tower top temperature controls below 40 DEG C, and the charging aperture 6 arranged on lightness-removing column 1 center side wall feeds, temperature
Controlling at about 150 DEG C, system vacuum controls at-0.09MPa, uses internal reflux in tower, and bottom discharge mouth 11 passes through pipeline
Rectifying column 2 is entered internal from rectification import 13；Rectification uses exteenal reflux, suppresses heavy constituent, the rectification arranged from rectifying column 2 top
Outlet 16 derivation o-phenylenediamine, content is more than 99.5%, and DAP/HAP controls at below 20ppm, and tower top temperature controls at 150-
170 DEG C, vacuum degree control is at-0.09MPa, and the second condenser 18 condenser uses 130-135 DEG C of vapours cooling；By derive
Carbendazim adds reactor 3 inside by pipeline from the kettle charging aperture 22 of reactor 3, after condensation insulation terminates a period of time,
Add suitable additive by feeding device 21 to combine with DAP, after stirring 30 minutes, enter belt vacuum filter 5, at band
The leading portion of formula vacuum filter 5 removes mother solution, then washes away this complex by cleaning shower nozzle 24 with the hot water classification of about 90 DEG C,
To reduce the purpose of DAP, after material drying, ultra micro, DAP/HAP substantially examines and does not measures, it is possible to effectively reduces DAP and contains
Amount, substantially increases product quality.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of the spirit or essential attributes of the present invention, it is possible to realize the present invention in other specific forms.Therefore, no matter
From the point of view of which point, all should regard embodiment as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all by fall in the implication of equivalency and scope of claim
Change is included in the present invention.Should not be considered as limiting involved claim by any reference in claim.
Although moreover, it will be appreciated that this specification is been described by according to embodiment, but the most each embodiment only wraps
Containing an independent technical scheme, this narrating mode of description is only that for clarity sake those skilled in the art should
Description can also be formed those skilled in the art through appropriately combined as an entirety, the technical scheme in each embodiment
May be appreciated other embodiments.
Claims (7)
1. carbendazim produces the processing unit (plant) reducing DAP impurity, filters including lightness-removing column, rectifying column, reactor and belt
Machine, it is characterised in that be provided with charging aperture on described lightness-removing column center side wall, lightness-removing column top is provided with gently expects mouth, is positioned at light
Lightness-removing column below material mouth is internally provided with the first condenser, is provided with discharging opening, described rectifying column lower side bottom lightness-removing column
End is provided with rectification import, and rectification import is connected with the discharging opening of lightness-removing column by pipeline, and rectifier bottoms is provided with and remains out
Material mouth, rectifying column top is provided with rectification outlet, and rectification outlet is connected with the second condenser, gas-liquid separator in turn by pipeline
And draw-off pump, draw-off pump is connected with rectifying column sidewall by exteenal reflux pipe, exteenal reflux pipe connects and has conveying pipe, and conveying pipe is with anti-
The kettle charging aperture answering still connects, and described reactor top sidewall is provided with feeding device, is provided with kettle bottom reactor
Discharging opening, discharging opening is connected with the feed end of band filter by pipeline, the strainer of described band filter is provided with clear
Wash shower nozzle.
A kind of carbendazim the most according to claim 1 produces the processing unit (plant) reducing DAP impurity, it is characterised in that described
Stirring paddle it is provided with in reactor.
A kind of carbendazim the most according to claim 1 produces the processing unit (plant) reducing DAP impurity, it is characterised in that described
Clean shower nozzle to be connected with cleaning water tank by pipeline, in described cleaning water tank, be provided with heater.
A kind of carbendazim the most according to claim 3 produces the processing unit (plant) reducing DAP impurity, it is characterised in that described
Clean and be provided with suction pump on the pipeline between water tank and cleaning shower nozzle.
A kind of carbendazim the most according to claim 1 produces the processing unit (plant) reducing DAP impurity, it is characterised in that described
The discharging opening of lightness-removing column is connected with lightness-removing column lower end sidewall by the first return duct, the first return duct is provided with first and boils
Device.
A kind of carbendazim the most according to claim 1 produces the processing unit (plant) reducing DAP impurity, it is characterised in that described
It is positioned on the lightness-removing column above the first condenser to be provided with and is condensed out pipe with the first condenser is connected, be positioned under the first condenser
It is provided with, on the lightness-removing column of side, the condensation inlet pipe being connected with the first condenser.
A kind of carbendazim the most according to claim 1 produces the processing unit (plant) reducing DAP impurity, it is characterised in that described
The residual discharging opening of rectifying column is connected with rectifying column lower end sidewall by the second return duct, the second return duct is provided with second again
Boiling device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610665671.9A CN106316961A (en) | 2016-08-13 | 2016-08-13 | Processing device for reducing DAP impurities through carbendazim production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610665671.9A CN106316961A (en) | 2016-08-13 | 2016-08-13 | Processing device for reducing DAP impurities through carbendazim production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106316961A true CN106316961A (en) | 2017-01-11 |
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ID=57740312
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610665671.9A Pending CN106316961A (en) | 2016-08-13 | 2016-08-13 | Processing device for reducing DAP impurities through carbendazim production |
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| Country | Link |
|---|---|
| CN (1) | CN106316961A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012160A (en) * | 2012-12-21 | 2013-04-03 | 江苏扬农化工集团有限公司 | Preparation method of o-phenylenediamine |
| CN104069672A (en) * | 2014-05-22 | 2014-10-01 | 安徽东至广信农化有限公司 | Vacuum belt-type filter for high-quality carbendazim production |
| CN104961685A (en) * | 2015-06-11 | 2015-10-07 | 安徽东至广信农化有限公司 | Method for reducing carbendazim impurity DAP in production process of carbendazim |
| CN204768680U (en) * | 2015-06-11 | 2015-11-18 | 安徽东至广信农化有限公司 | A reation kettle for producing reduce impurity DAP in carbendazim |
-
2016
- 2016-08-13 CN CN201610665671.9A patent/CN106316961A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012160A (en) * | 2012-12-21 | 2013-04-03 | 江苏扬农化工集团有限公司 | Preparation method of o-phenylenediamine |
| CN104069672A (en) * | 2014-05-22 | 2014-10-01 | 安徽东至广信农化有限公司 | Vacuum belt-type filter for high-quality carbendazim production |
| CN104961685A (en) * | 2015-06-11 | 2015-10-07 | 安徽东至广信农化有限公司 | Method for reducing carbendazim impurity DAP in production process of carbendazim |
| CN204768680U (en) * | 2015-06-11 | 2015-11-18 | 安徽东至广信农化有限公司 | A reation kettle for producing reduce impurity DAP in carbendazim |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170111 |
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| RJ01 | Rejection of invention patent application after publication |