CN207641032U - A kind of ultrasonic wave is used for the continuous crystallization device of DSD acid intermediate DNS - Google Patents

A kind of ultrasonic wave is used for the continuous crystallization device of DSD acid intermediate DNS Download PDF

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Publication number
CN207641032U
CN207641032U CN201721743038.3U CN201721743038U CN207641032U CN 207641032 U CN207641032 U CN 207641032U CN 201721743038 U CN201721743038 U CN 201721743038U CN 207641032 U CN207641032 U CN 207641032U
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Prior art keywords
recirculated water
kettle
crystallization kettle
pipe
crystallization
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CN201721743038.3U
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李将
陈鑫
刘肖晖
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ZHEJIANG HONGDA CHEMICALS Co.,Ltd.
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Lianyungang Leiah Chemical Co Ltd
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Abstract

A kind of ultrasonic wave is used for the continuous crystallization device of DSD acid intermediate DNS, including crystallization kettle, and feed pipe is equipped at the top of crystallization kettle, and lower discharge port is equipped in the bottom of crystallization kettle, and upper flowover-proof type discharge port is equipped on the top of crystallization kettle;It is internally provided with cooling mechanism and rabbling mechanism in crystallization kettle, the rabbling mechanism includes agitating shaft, and several stirrer paddles are equipped on agitating shaft;The cooling mechanism includes recirculated water outlet pipe and recirculated water inlet pipe, and temperature control coil pipe is equipped between recirculated water inlet pipe and recirculated water outlet pipe, supersonic generator is equipped on the recirculated water inlet pipe outside crystallization kettle.The utility model can realize continuous crystallization, in the process temperature plateau, improve crystal quality and purity.

Description

A kind of ultrasonic wave is used for the continuous crystallization device of DSD acid intermediate DNS
Technical field
The utility model is related to a kind of chemical mechanical equipment, especially a kind of ultrasonic wave is used for the company of DSD acid intermediate DNS Continuousization crystallization apparatus.
Background technology
The full name 4 of DSD acid, 4'- diaminobenzil -2,2'- disulfonic acid are a kind of important dyestuffs of field of fine chemical Intermediate is the primary raw material for producing talan line fluorescent brightening agent;It is also the important centre of direct dyes, reactive dye Body can produce chrysophene G, directly a kinds up to a hundred such as gorgeous Huang 4R, reactive brilliant yellow KD-3G, everbright fast orange F3G.The synthesis of DSD acid Generally using sulfonation, oxidation, reduction, acid out step:Raw material para-nitrotoluene obtains para-nitrotoluene neighbour through oleum sulfonation Sulfonic acid(PNTS), it is under alkaline condition 4,4'- dinitrostilbene -2,2'- sodium disulfonates through air oxidation, is passed through under high temperature Iron powder reducing obtains 4,4'- diaminobenzil -2,2'- sodium disulfonates, then acid out obtains 4,4'- diaminobenzils -2,2'- Disulfonic acid.
Currently, all water phase air oxidation process of state's internal oxidation process, neutralize PH=7.0-7.5, will aoxidize after oxidation Liquid is squeezed into crystallization kettle, is slowly introducing circulating water cooling first, and the later stage gradually opens greatly;When being cooled to 40 DEG C, recirculated water is closed, It is passed through 5 DEG C of cold water or chilled brine, is cooled to 25-30 DEG C, blowing carries out press filtration.It is asked there are following in this operational process of craft Topic:Using intermittently operated, valve blowing need to be frequently switched on, there are maloperations may;Rate of temperature fall fluctuation is big, not to crystal growth Easily there is small crystals in profit, influences quality;It is easy knot wall in crystal precipitation process, outside coil pipe, influences to exchange heat, needs periodic cleaning; Discontinuum operates, therefore is badly in need of a kind of device for capableing of continuous crystallization.
Invention content
The technical problems to be solved in the utility model is in view of the deficiencies of the prior art, to propose that one kind can solve DNS crystallizations In the process intermittently operated, coil pipe knot wall technique problem ultrasonic wave be used for DSD acid intermediate DNS continuous crystallization device.
The technical problems to be solved in the utility model is achieved through the following technical solutions, and a kind of ultrasonic wave is used for DSD The continuous crystallization device of sour intermediate DNS, its main feature is that:Including crystallization kettle, it is equipped with feed pipe at the top of crystallization kettle, is being tied The bottom of brilliant kettle is equipped with lower discharge port, is equipped with bottom discharge pipe at lower discharge port, goes out equipped with upper flowover-proof type on the top of crystallization kettle Material mouth, upper flowover-proof type discharge outlet are equipped with flowover-proof type discharge nozzle, and discharge nozzle is communicated with flowover-proof type discharge nozzle upwards;In crystallization kettle Be internally provided with cooling mechanism and rabbling mechanism, the rabbling mechanism includes agitating shaft, and several stirrings are equipped on agitating shaft Blade;The cooling mechanism include be arranged crystallization kettle top recirculated water outlet pipe and be arranged recirculated water in crystallization kettle lower part into Pipe is equipped with the temperature control coil pipe for being distributed in stirrer paddle surrounding control temperature in the kettle between recirculated water inlet pipe and recirculated water outlet pipe, The supersonic generator for avoiding temperature control coil pipe that knot wall phenomenon occurs is installed on the recirculated water inlet pipe outside crystallization kettle.
The technical problems to be solved in the utility model can also further realize by the following technical programs, described anti-overflow Formula discharge nozzle Open Side Down setting.
The technical problems to be solved in the utility model can also further realize by the following technical programs, in crystallization kettle On thermometer is installed.
The technical problems to be solved in the utility model can also further realize by the following technical programs, the stirring Axis is vertically arranged, and stirrer paddle equidistantly distributed above and below agitating shaft axial direction has 3.
The technical problems to be solved in the utility model can also further realize by the following technical programs, the stirring The angle of blade and horizontal plane is 45 °.
Compared with prior art, the utility model has the advantages that:
1, using serialization automatic feed, charging is compressed to most short with discharging time, greatly improves equipment capacity;
2, using the temperature control coil pipe between recirculated water inlet pipe and recirculated water outlet pipe, heat exchange area in kettle is increased, Be conducive to heat transfer;Stirrer paddle is utilized simultaneously, controls material directed circulation in kettle, and it is broken to reduce the crystal caused by impact It is broken;
3, using the supersonic generator on recirculated water inlet pipe, for clearing up fouling outside coil pipe, in operating process, Without clear kettle, without stopping charging, and efficiently quickly;
4, continuous crystallization can be achieved, temperature plateau, improves crystal quality and purity in the process.
Description of the drawings
Fig. 1 is the structural schematic diagram of the utility model.
Specific implementation mode
The utility model will in detail describe in the following description in conjunction with attached drawing.The utility model can be in different implementation There is various change in example, all do not depart from the scope of protection of the utility model, explanation and diagram therein inherently as Purposes of discussion rather than limits the present invention.
A kind of ultrasonic wave is used for the continuous crystallization device of DSD acid intermediate DNS, including crystallization kettle 10, in crystallization kettle 10 Top be equipped with feed pipe 11, be equipped with lower discharge port in the bottom of crystallization kettle 10, bottom discharge pipe 3 be installed at lower discharge port, The top of crystallization kettle is equipped with upper flowover-proof type discharge port, and upper flowover-proof type discharge outlet is equipped with flowover-proof type discharge nozzle 1, discharge nozzle 3 to It is upper to be communicated with flowover-proof type discharge nozzle 1;It is internally provided with cooling mechanism and rabbling mechanism in crystallization kettle, the rabbling mechanism includes stirring Axis 2 is mixed, several stirrer paddles 7 are installed on agitating shaft 2;The cooling mechanism includes the recirculated water being arranged on crystallization kettle top Outlet pipe 9 and the recirculated water inlet pipe 5 in crystallization kettle lower part is set, is equipped with and is distributed between recirculated water inlet pipe 5 and recirculated water outlet pipe 9 Stirrer paddle surrounding controls the temperature control coil pipe 8 of temperature in the kettle, is equipped on the recirculated water inlet pipe outside crystallization kettle and avoids temperature control disk The supersonic generator 4 of knot wall phenomenon occurs for pipe.The temperature control coil pipe is double loop cooling coil, recycles water entrance and double back Road cooling coil unicom ensures to be full of in coil pipe using low in and high out mode;The supersonic generator is mainly used for working as coil pipe After outer layer has the fouling that crystalline solid is formed, supersonic generator is periodically opened, is crushed layer of scale using ultrasonic activation, is crushed After be directly entered.
The flowover-proof type discharge nozzle Open Side Down setting.The upper flowover-proof type discharge port utilizes pressure difference control material from bottom Continuous discharge, such as bottom because crystalline solid results in blockage, liquid level, which rises, to be flowed out automatically from upper flowover-proof type discharge port, prevent crystallization kettle It overflows.Thermometer 6 is installed on crystallization kettle.The thermometer 6 maintains certain model with feed pipe chain control temperature in the kettle In enclosing.The agitating shaft is vertically arranged, and stirrer paddle equidistantly distributed above and below agitating shaft axial direction has 3.The stirring The angle of blade and horizontal plane is 45 °.The stirrer paddle is using blade and stirs horizontal plane in angle of 45 degrees, and blade is ellipse Round shape, no protruding parts.
Although the utility model describes the structure of the utility model, but term used be explanation and it is exemplary rather than It is restrictive.Since the utility model can be embodied in various forms without departing from the spirit of the inventions, it is to be understood that Above-described embodiment is not limited to foregoing details, and should widely be explained in claim limited range, therefore falls into right It is required that or the variation in its equivalent scope and remodeling, should be covered by the following claims.

Claims (5)

1. a kind of ultrasonic wave is used for the continuous crystallization device of DSD acid intermediate DNS, it is characterised in that:Including crystallization kettle, tying The top of brilliant kettle is equipped with feed pipe, is equipped with lower discharge port in the bottom of crystallization kettle, is equipped with bottom discharge pipe at lower discharge port, is tying The top of brilliant kettle is equipped with upper flowover-proof type discharge port, and upper flowover-proof type discharge outlet is equipped with flowover-proof type discharge nozzle, discharge nozzle upwards with Flowover-proof type discharge nozzle communicates;It is internally provided with cooling mechanism and rabbling mechanism in crystallization kettle, the rabbling mechanism includes agitating shaft, Several stirrer paddles are installed on agitating shaft;The cooling mechanism include be arranged crystallization kettle top recirculated water outlet pipe and set The recirculated water inlet pipe in crystallization kettle lower part is set, is equipped between recirculated water inlet pipe and recirculated water outlet pipe and is distributed in stirrer paddle surrounding The temperature control coil pipe of temperature in the kettle is controlled, is equipped on the recirculated water inlet pipe outside crystallization kettle and avoids temperature control coil pipe that knot wall phenomenon occurs Supersonic generator.
2. ultrasonic wave according to claim 1 is used for the continuous crystallization device of DSD acid intermediate DNS, it is characterised in that: The flowover-proof type discharge nozzle Open Side Down setting.
3. ultrasonic wave according to claim 1 is used for the continuous crystallization device of DSD acid intermediate DNS, it is characterised in that: Thermometer is installed on crystallization kettle.
4. ultrasonic wave according to claim 1 is used for the continuous crystallization device of DSD acid intermediate DNS, it is characterised in that: The agitating shaft is vertically arranged, and stirrer paddle equidistantly distributed above and below agitating shaft axial direction has 3.
5. ultrasonic wave according to claim 4 is used for the continuous crystallization device of DSD acid intermediate DNS, it is characterised in that: The angle of the stirrer paddle and horizontal plane is 45 °.
CN201721743038.3U 2017-12-14 2017-12-14 A kind of ultrasonic wave is used for the continuous crystallization device of DSD acid intermediate DNS Active CN207641032U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113717114A (en) * 2021-09-23 2021-11-30 济南悟通生物科技有限公司 2-acetylpyrazine continuous recrystallization device, method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113717114A (en) * 2021-09-23 2021-11-30 济南悟通生物科技有限公司 2-acetylpyrazine continuous recrystallization device, method and application thereof
CN113717114B (en) * 2021-09-23 2022-12-02 济南悟通生物科技有限公司 2-acetylpyrazine continuous recrystallization device, method and application thereof

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Effective date of registration: 20210721

Address after: 312399 Shangyu economic and Technological Development Zone, Hangzhou Bay, Shaoxing City, Zhejiang Province

Patentee after: ZHEJIANG HONGDA CHEMICALS Co.,Ltd.

Address before: 222200 No.5, Weiyi Road, Lingang Industrial Zone, Guanyun County, Lianyungang City, Jiangsu Province

Patentee before: LIANYUNGANG LION CHEMICAL Co.,Ltd.

TR01 Transfer of patent right