CN203360342U - Production device for preparing 2, 6-dichlorobenzonitrile - Google Patents

Production device for preparing 2, 6-dichlorobenzonitrile Download PDF

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Publication number
CN203360342U
CN203360342U CN 201320449097 CN201320449097U CN203360342U CN 203360342 U CN203360342 U CN 203360342U CN 201320449097 CN201320449097 CN 201320449097 CN 201320449097 U CN201320449097 U CN 201320449097U CN 203360342 U CN203360342 U CN 203360342U
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China
Prior art keywords
still
hydrolysis
feed
opening
nitrilation
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Withdrawn - After Issue
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CN 201320449097
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Chinese (zh)
Inventor
陈国云
王瑛
王晨
潘明生
刘润兴
王正军
余辉
罗瑞
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TIANCHEN FINE CHEMICAL CO Ltd YANGZHOU
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TIANCHEN FINE CHEMICAL CO Ltd YANGZHOU
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Abstract

The utility model provides a production device for preparing 2, 6-dichlorobenzonitrile, and relates to the technical field of production of 2, 6-dichlorobenzonitrile through chemical synthesis. The production device comprises an evaporator, a buffer tank, a hydrogen chloride recovery tank, a chlorination kettle, a first rectifying still and a hydrolysis quaternized kettle. The production device is reasonable in design, convenient to control, small in raw material consumption and low in production cost, and reduces solid waste and emission of nitrogenous nitroso waste gas, therefore, the production device is an industrial practical cleaning production device, can save energy and reduce emission, and is environment-friendly.

Description

A kind of production equipment for preparing 2,6-dichlorobenzonitrile
Technical field
The utility model relates to chemosynthesis 2, the production technical field of 6-dichlorobenzonitrile.
Background technology
2, the 6-dichlorobenzonitrile is the synthetic intermediate of the broad spectrum novel agrochemical benzoyl urea of high-efficiency low-toxicity, form agricultural chemicals and have efficiently, low toxicity, noresidue, do not injure the characteristics of crop, can be used for producing Insecticides (tech) & Herbicides (tech), also can be used for the production of dyestuff, medicine, agricultural chemicals and extraordinary high polymer material.
Existing 2,6-dichlorobenzonitrile synthetic method has toluene direct chlorination method, para-nitrotoluene method, Ortho Nitro Toluene method, p-tert-butyltoluene method, o-toluenesulfonyl chloride chlorination decomposition method etc., but above various 2, the defect that the production of 6-dichlorobenzonitrile exists is: the production control difficulty, yield poorly, cost is high, can not be applicable to its market requirement.
The utility model content
The utility model purpose is to propose a kind of production control, preparation 2 that output is high, production equipment of 6-dichlorobenzonitrile of being easy to.
The utility model comprises vaporizer, surge tank, the hydrogenchloride withdrawing can, chlorination tank, the first rectifying still and hydrolysis nitrilation still, light source is set in chlorination tank, vaporizer is connected to an opening for feed of chlorination tank by surge tank, also arrange respectively 2 on chlorination tank, 6-toluene dichloride opening for feed and phosphorus pentachloride opening for feed, the chuck of chlorination tank connects the first condenser, the entrance end of hydrogenchloride withdrawing can be arranged on chlorination tank on the air outlet on top be connected, under chlorination tank, the discharge port on top is connected with an opening for feed of the first rectifying still, be connected with rectifying tower on the first rectifying still, the discharge port of the first rectifying still lower end is connected with an opening for feed of hydrolysis nitrilation still, hydrolysis nitrilation still also arranges acid solvent, zinc chloride and oxammonium hydrochloride opening for feed, the chuck of hydrolysis nitrilation still connects the second condenser, hydrolysis nitrilation still upper end is put with hydrogenchloride and is reclaimed tank connected air outlet, hydrolysis nitrilation still lower end arranges discharge port.
In chlorination tank, under the katalysis of phosphorus pentachloride and light, by 2,6-toluene dichloride and chlorine carry out chlorination reaction, reaction obtains 2,6-dichloro benzyl dichloride, major product 2,6-dichloro benzyl dichloride enters the first rectifying still by the discharge port on top under chlorination tank, and the HCl of chlorination reaction Cheng Sheng enters the hydrogenchloride withdrawing can by the air outlet on top on chlorination tank; In the first rectifying still, rectifying goes out 2,6-dichloro benzyl dichloride enters in hydrolysis nitrilation still, the reaction that is hydrolyzed under acid solvent and zinc chloride effect, then through the oxammonium hydrochloride cyanation, lower end discharge port at hydrolysis nitrilation still is obtained 2 of crystallization, the thick finished product of 6-dichlorobenzonitrile.
The utility model adopts 2, the 6-toluene dichloride is starting raw material, through chlorination, makes 2,6-dichloro benzyl dichloride, make 2 through hydrolysis, nitrilation again, 6-dichlorobenzonitrile crude product, production unit is reasonable in design, convenient control, raw material consumption is few, production cost is low, also reduced solid waste generation, reduced the discharge of nitrogenous nitroso-group thing waste gas, be the industrialization practicality process for cleanly preparing of a kind of energy-conservation, reduction of discharging, environmental protection.
The hydrogen chloride gas that the utility model produces in chlorination and hydrolysis nitrilation two steps absorbs with water the hydrochloric acid produced and can be used as by-product sale, the excessive chlorine of chlorinating step absorbs with 11% sodium hydroxide or 10% lime aqueous solution, can generate clorox or calcium hypochlorite solution, also can be used as byproduct and sell.
In addition, in order to improve the purity of product, the discharge port of described hydrolysis nitrilation still lower end is connected to the opening for feed of the second rectifying still, and the discharge port of the second rectifying still is connected with dryer.
After refining, obtain 2,6-dichlorobenzonitrile elaboration.Product purity is 99.8~99.95%, and fusing point is 141.0~144.0 ℃, water ratio≤0.1%.
The accompanying drawing explanation
Fig. 1 is a kind of structure principle chart of the present utility model.
Embodiment
The utility model is provided with vaporizer 1, surge tank 2, hydrogenchloride withdrawing can 3, chlorination tank 4, the first rectifying still 5, hydrolysis nitrilation still 6, the second rectifying still 7, dryer 8, the first condenser 9, the second condenser 10 and rectifying tower 11.
The interior light source that arranges of chlorination tank 4, vaporizer 1 is connected to an opening for feed of chlorination tank 4 by surge tank 2,2,6-DCT opening for feed and phosphorus pentachloride opening for feed also are set respectively on chlorination tank 4, the chuck of chlorination tank 4 connects the first condenser 9, with the material in chlorination tank 4, carries out temperature control.
The entrance end of hydrogenchloride withdrawing can 3 be arranged on chlorination tank 4 on the air outlet on top be connected.
The discharge port on 4 times tops of chlorination tank is connected with an opening for feed of the first rectifying still 5, on the first rectifying still 5, is connected with rectifying tower 11.The discharge port of the first rectifying still 5 lower ends is connected with an opening for feed of hydrolysis nitrilation still 6.
Hydrolysis nitrilation still 6 also arranges acid solvent, zinc chloride and oxammonium hydrochloride opening for feed, and the chuck of hydrolysis nitrilation still 6 connects the second condenser 10, and the air outlet be connected with hydrogenchloride withdrawing can 3 is put in hydrolysis nitrilation still 6 upper ends, and hydrolysis nitrilation still 6 lower ends arrange discharge port.
The discharge port of hydrolysis nitrilation still 6 lower ends is connected to the opening for feed of the second rectifying still 7 by water extracter 12, the discharge port of the second rectifying still 7 is connected with dryer 8 by water extracter 13.

Claims (2)

1. one kind prepares 2, the production equipment of 6-dichlorobenzonitrile, it is characterized in that comprising vaporizer, surge tank, the hydrogenchloride withdrawing can, chlorination tank, the first rectifying still and hydrolysis nitrilation still, light source is set in chlorination tank, vaporizer is connected to an opening for feed of chlorination tank by surge tank, also arrange respectively 2 on chlorination tank, 6-toluene dichloride opening for feed and phosphorus pentachloride opening for feed, the chuck of chlorination tank connects the first condenser, the entrance end of hydrogenchloride withdrawing can be arranged on chlorination tank on the air outlet on top be connected, under chlorination tank, the discharge port on top is connected with an opening for feed of the first rectifying still, be connected with rectifying tower on the first rectifying still, the discharge port of the first rectifying still lower end is connected with an opening for feed of hydrolysis nitrilation still, hydrolysis nitrilation still also arranges acid solvent, zinc chloride and oxammonium hydrochloride opening for feed, the chuck of hydrolysis nitrilation still connects the second condenser, hydrolysis nitrilation still upper end is put with hydrogenchloride and is reclaimed tank connected air outlet, hydrolysis nitrilation still lower end arranges discharge port.
2. a kind of production equipment for preparing 2,6-dichlorobenzonitrile according to claim 1, is characterized in that the discharge port of described hydrolysis nitrilation still lower end is connected to the opening for feed of the second rectifying still, and the discharge port of the second rectifying still is connected with dryer.
CN 201320449097 2013-07-26 2013-07-26 Production device for preparing 2, 6-dichlorobenzonitrile Withdrawn - After Issue CN203360342U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201320449097 CN203360342U (en) 2013-07-26 2013-07-26 Production device for preparing 2, 6-dichlorobenzonitrile

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201320449097 CN203360342U (en) 2013-07-26 2013-07-26 Production device for preparing 2, 6-dichlorobenzonitrile

Publications (1)

Publication Number Publication Date
CN203360342U true CN203360342U (en) 2013-12-25

Family

ID=49808134

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201320449097 Withdrawn - After Issue CN203360342U (en) 2013-07-26 2013-07-26 Production device for preparing 2, 6-dichlorobenzonitrile

Country Status (1)

Country Link
CN (1) CN203360342U (en)

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Granted publication date: 20131225

Effective date of abandoning: 20140917

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