CN205774223U - The industrial production device of 2 chlorine 4 monomethylaniline. 5 sulfonic acid - Google Patents
The industrial production device of 2 chlorine 4 monomethylaniline. 5 sulfonic acid Download PDFInfo
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- CN205774223U CN205774223U CN201620469912.8U CN201620469912U CN205774223U CN 205774223 U CN205774223 U CN 205774223U CN 201620469912 U CN201620469912 U CN 201620469912U CN 205774223 U CN205774223 U CN 205774223U
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Abstract
The industrial production device of a kind of 2 chlorine 4 monomethylaniline. 5 sulfonic acid, rinses exsiccator (501), two strip transmission lines, dissolution kettle, centrifuge, distillating still, two condensers, two vacuum buffer grooves and solvent pump including three dosing pumps (401,402,403), three measuring tanks (301,302,303), one-tenth salt oven (101), sulphonation kettle (102), profit automatic water distributor (304), reaction water dump tank, solvent groove, solvent medial launder, filtrations.Sulphuric acid, 2B oil and solvent is inputted by dosing pump, by measuring tank automatic blending, salt-forming reaction is carried out by becoming salt oven, carried out being dehydrated indexing by sulphonation kettle and generate 2 chlorine 4 monomethylaniline. 5 sulfonic acid, again through dissolving purification, obtaining high-purity 2 chlorine 4 monomethylaniline. 5 sulfonic acid product, automaticity is high, production process total enclosing, and labor intensity is low, good work environment.
Description
Technical field
This utility model relates to the industrial production device of arylamine sulfonic acid, the work of a kind of 2-chloro-4-monomethylaniline .-5-sulfonic acid
Industry process units.
Background technology
2-chloro-4-monomethylaniline .-5-sulfonic acid is extremely important organic pigment intermediate, is current organic pigment intermediate
In one of topmost eight kinds, mainly for the production of C.I. pigment red 48 series red pigment on pigment industry, in recent years
Being also used for C.I. pigment yellow 191 series yellow uitramarine, this pigment is widely used in paint, coating, colored ink, rubber and moulds
Material coloring etc..The 2-chloro-4-monomethylaniline .-5-sulfonic acid process units of existing maturation all uses batch reactor, with 2-chloro-4-first
Base aniline is raw material, carries out sulfonating reaction with 98% sulphuric acid, then carries out filtering, rinses, is dried, packs, and proportioning raw materials is artificial
Setting, artificial input and output material, terminal point determining is difficult, and technique and unstable product quality, environment is poor, labor intensity is big.Chinese patent
ZL201110149524.3 invented a kind of 2B oil (2-chloro-4-monomethylaniline .) sulfonation production 2B acid (2-chloro-4-monomethylaniline .-
5-sulfonic acid) new technology, this 2B oil sulfonation production 2B acid method be by 2B oil enter in liquid dispersant with concentrated sulphuric acid
Row sulfonating reaction, sulfonated products is through filtering, rinse, be dried to obtain 2B acid, and wherein 2B oil uses high-purity 2B oil to be raw material, uses
Inert organic solvents is dispersant, uses low boiling point organic solvent to rinse after filtration.The acid of this 2B oil sulfonation production 2B
Method owing to using high-purity 2B oil to be raw material and inert organic solvents is dispersant, sulfonated products through filtering, rinsing, dry
I.e. can get qualified 2B acid, eliminate that alkali is molten, decolour, filter, acid out, be dehydrated, the subtractive process such as be dried, so that the three wastes are big
For reducing, without solid waste, waste gas, wastewater flow rate are few and disposable, also reduce energy consumption.For process for sulfonation, it is a kind of
Break through, there is conversion ratio height, the advantage of Non-carbonized.This new technology is that the application of chemical process automation provides the foundation.
Summary of the invention
The purpose of this utility model is to propose the industrial production device of a kind of 2-chloro-4-monomethylaniline .-5-sulfonic acid, energy
Chloro-for 2-4-monomethylaniline. is produced 2-chloro-4-monomethylaniline .-5-sulfonic acid with sulphuric acid successive reaction, overcomes raw material charge ratio essence
Spend the defects such as low, terminal point determining is difficult, technique is unstable.
The industrial production device of this 2-chloro-4-monomethylaniline .-5-sulfonic acid include three dosing pumps, three measuring tanks,
Become salt oven, sulphonation kettle, profit automatic water distributor, reaction water dump tank, solvent groove, solvent medial launder, filter rinsing exsiccator,
Two strip transmission lines, dissolution kettle, centrifuge, distillating still, two condensers, two vacuum buffer grooves and solvent pump.First dosing pump
Outlet be connected with the import of the first measuring tank, second metering delivery side of pump and the second measuring tank import be connected, the 3rd metering
The import of delivery side of pump and the 3rd measuring tank is connected, and the outlet of the first measuring tank is connected with the first charging aperture becoming salt oven, and second
The outlet of measuring tank is connected with the second charging aperture becoming salt oven, and the outlet of the 3rd measuring tank feeds with become salt oven second respectively
Mouth, the second charging aperture of sulphonation kettle, the second charging aperture of filtration rinsing exsiccator are connected.Become discharging opening and the sulphonation kettle of salt oven
First charging aperture is connected, and the gaseous phase outlet of sulphonation kettle is connected with the import of profit automatic water distributor by the first condenser, profit
The outlet of automatic water distributor is connected with the import of reaction water groove, and the oil-out of profit automatic water distributor enters with solvent groove
Mouth is connected, and the oil-out of profit automatic water distributor is also connected with the refluxing opening of sulphonation kettle, the gas phase at profit automatic water distributor top
Outlet is connected with the import of the first vacuum buffer groove.Discharging opening bottom sulphonation kettle and the first charging aperture filtering rinsing exsiccator
It is connected, filters the discharging opening bottom rinsing exsiccator and be connected with the charging aperture of dissolution kettle by the first powder conveying line, dissolution kettle
The discharging opening of bottom is connected with the charging aperture of centrifuge, and discharging opening and the second powder conveying line bottom centrifuge are connected.Filter
The liquid phase discharging opening of rinsing exsiccator side is connected with the charging aperture of distillating still, filters rinsing exsiccator top gas phase outlet and the
The gas phase import of two condensers is connected.The gaseous phase outlet of distillating still and the gas phase import of the second condenser are connected, the second condenser
Liquid-phase outlet be connected with the charging aperture of solvent medial launder, the discharging opening bottom solvent medial launder is connected with the import of solvent pump,
The gas phase mouth at solvent medial launder top and the import of the second vacuum buffer groove are connected.
When producing with the industrial production device of this 2-chloro-4-monomethylaniline .-5-sulfonic acid, defeated by the first dosing pump
Enter sulphuric acid, the second dosing pump input 2B oil, the 3rd dosing pump input solvent, by measuring tank automatic blending, carried out by becoming salt oven
Salt-forming reaction, is carried out being dehydrated indexing by sulphonation kettle and generates 2-chloro-4-monomethylaniline .-5-sulfonic acid, then purify through dissolving, obtain high-purity
Degree 2-chloro-4-monomethylaniline .-5-sulfonic acid product, automaticity is high, production process total enclosing, and labor intensity is low, working environment
Good.The industrial production device of this 2-chloro-4-monomethylaniline .-5-sulfonic acid is also applied for para-totuidine, 3,4-dichloroaniline
It is raw material Deng aromatic amine, uses concentrated sulphuric acid to carry out sulfonation and generate 4-monomethylaniline .-2-sulfonic acid, 3,4-DCA-6-sulfonic acid etc.
In the industrialized production of arylamine sulfonic acid.
Accompanying drawing explanation
Accompanying drawing is the schematic diagram of the industrial production device of 2-chloro-4-monomethylaniline .-5-sulfonic acid.
Detailed description of the invention
As it can be seen, the industrial production device of this 2-chloro-4-monomethylaniline .-5-sulfonic acid include three dosing pumps 401,
402,403, three measuring tanks 301,302,303, become salt oven 101, sulphonation kettle 102, profit automatic water distributor 304, reaction water to connect
Groove 305, solvent groove 306, solvent medial launder 308, filtration rinsing exsiccator 501, two strip transmission lines 601,602, dissolution kettle
202, centrifuge 502, distillating still 204, two condensers 201,203, two vacuum buffer grooves 307,309 and solvent pump 404.The
The outlet of one dosing pump 401 is connected with the import of the first measuring tank 301, the outlet of the second dosing pump 402 and the second measuring tank 302
Import be connected, the outlet of the 3rd dosing pump 403 is connected with the import of the 3rd measuring tank 303；The outlet of the first measuring tank 301 with
The first charging aperture becoming salt oven 101 is connected, and the outlet of the second measuring tank 302 is connected with the second charging aperture becoming salt oven 101, and the 3rd
The outlet of measuring tank 303 is dried with the second charging aperture becoming salt oven 101, the second charging aperture of sulphonation kettle 102, filtration rinsing respectively
Second charging aperture of device 501 is connected.The discharging opening becoming salt oven 101 is connected with the first charging aperture of sulphonation kettle 102, sulphonation kettle 102
Gaseous phase outlet be connected with the import of profit automatic water distributor 304 by the first condenser 201, profit automatic water distributor 304
Outlet is connected with the import of reaction water groove 305, the oil-out of profit automatic water distributor 304 and solvent groove 306 import phase
Even, the oil-out of profit automatic water distributor 304 also refluxing opening with sulphonation kettle 102 is connected, profit automatic water distributor 304 top
The import of gaseous phase outlet and the first vacuum buffer groove 307 is connected；Discharging opening bottom sulphonation kettle 102 rinses exsiccator with filtering
First charging aperture of 501 is connected, and filters the discharging opening bottom rinsing exsiccator 501 and by the first powder conveying line 601 and dissolves
The charging aperture of still 202 is connected, and the discharging opening bottom dissolution kettle 202 is connected with the charging aperture of centrifuge 502, bottom centrifuge 502
Discharging opening and the second powder conveying line 602 charging aperture be connected；Filter liquid phase discharging opening and the steaming of rinsing exsiccator 501 side
The charging aperture evaporating still 204 is connected, and filters gaseous phase outlet and the gas phase import of the second condenser 203 at rinsing exsiccator 501 top
It is connected；The gaseous phase outlet of distillating still 204 and the gas phase import of the second condenser 203 are connected, the liquid-phase outlet of the second condenser 203
Being connected with the charging aperture of solvent medial launder 308, the discharging opening bottom solvent medial launder 308 is connected with the import of solvent pump 404, molten
The gas phase mouth at agent medial launder 308 top and the import of the second vacuum buffer groove 309 are connected.
Production and the automatic control process of the industrial production device of this 2-chloro-4-monomethylaniline .-5-sulfonic acid are as follows:
A, automatic blending: three measuring tanks 301,302,303 are respectively provided with weighing device relevant to three dosing pump power supplys,
In a control program, open 2-chloro-4-monomethylaniline. dosing pump (the second dosing pump 402) and feed to setting weight, be automatically stopped,
System, automatically according to 2-chloro-4-monomethylaniline. feed weight, content, calculates required sulfuric acid dosage and quantity of solvent, automatically turns on
Sulphuric acid dosing pump (the first dosing pump 401), solvent dosing pump (the 3rd dosing pump 403), be automatically stopped to set amount, this automatically
Feed proportioning system, it is ensured that the accuracy of proportioning, it is to avoid manual operation error, it is ensured that raw material reaction fully and is avoided because of mistake
The caused carbonization of amount, this improves technique and quality control stability.
B, one-tenth salt: raw material 2-chloro-4-monomethylaniline., sulphuric acid, solvent are beaten according to setting proportioning the most automatically by dosing pump
Entering measuring tank 301,302,303, after measuring tank has fed, be automatically added to into salt oven 101 successively, by setting, the response time is abundant
Reaction generates 2-chloro-4-methylaniline sulfate.After salt-forming reaction, then carry out next step dehydration indexing, salt will be become to turn with dehydration
Position substep is carried out, and is conducive to into salt adequacy, because becoming salt temperature height to be easily caused local temperature simultaneously when it also avoid one-pot operation
Too high and the phenomenon of carbonization.
C, dehydration indexing: material enters sulphonation kettle 102, heats to azeotropic by sulphonation kettle chuck, carries out the chloro-4-of 2-
Methylaniline sulfate dehydration indexing generates the reaction of 2-chloro-4-monomethylaniline .-5-sulfonic acid, the water that reaction generates and solvent azeotropic,
Gas phase enters profit automatic water distributor 304 after entering the first condenser 201 condensation, and oil phase flows back into sulphonation kettle or separates solvent
Enter solvent groove 306, then be delivered to solvent feed tank recycled；Reaction water, automatically into reaction water groove 305, then drains into
Sewage network.This profit automatic water distributor can realize azeotropic solvent partial reflux, it is to avoid because of altogether boiling solvent take out of in a large number, still
The minimizing of internal solvent amount causes still to stir bad, the problem of mass-and heat-transfer decline；Reaction water groove is provided with weighing device, and and sulphur
Changing still heating jacket conduction oil valve to be associated, according to inventory, system calculates reaction water growing amount automatically, when reaction water is subject to
When in groove, quality no longer changed within the setting time, reaction is reached home, and is automatically switched off heating valve, and alarm, can enter
Enter next-step operation.
D, filtration rinsing are dried: translocation reaction terminates, and feed liquid adds filtration and rinses exsiccator 501, first in vacuum or pressure
Filtering under power effect, filtrate enters distillating still 204；Until substantially without continuous drop time, the solvent adding set amount carries out rinsing behaviour
Making, then carry out nitrogen purging, filtrate enters distillating still in the lump, until without continuous drop, entering drying stage；When being dried, open
Opening heater, top gas phase enters the second condenser 203 and condenses recovery and obtain solvent, solvent pump 404 send to solvent tank,
Recycled.After being dried, crude product powder body passes through the first pipeline 601 to dissolution kettle 202 (crude product also can directly be packed).This
Filtering rinsing dry run uses ripe filtration rinsing to be dried " three-in-one " equipment, whole process closed-loop operation, alleviates labor
Fatigue resistance, improve environment, it is to avoid gap operating material spilling, solvent uncontrollable discharge.
E, dissolving purify: 2-chloro-4-monomethylaniline .-5-sulfonic acid powder body sends into dissolution kettle 202 by the first pipeline, add
Ethanol is also sufficiently stirred for, and makes 2-chloro-4-monomethylaniline .-5-sulfonic acid powder body be completely dispersed, becomes 2-chloro-4-monomethylaniline .-5-sulphur
The alcohol suspension of acid；By centrifuge 502 by chloro-for 2-4-monomethylaniline .-5-sulfonic acid and separation of ethanol；It is molten that filtrate sends to washing
Agent storage tank, refined Posterior circle is applied mechanically；Filter cake put into the second pipeline be delivered to be dried, packaging process, i.e. can get high-purity 2-
Chloro-4-monomethylaniline .-5-sulfonic acid product, in whole dissolving subtractive process, powder body feeds intake and uses carrier automatic feed, centrifuge
Discharging uses pipeline transmission, therefore, feed intake, discharging process all continuously, closed-loop operation, it is to avoid impurity is carried secretly, improves product
Product quality and stability, alleviate labor intensity, eliminates dust pollution.
Claims (1)
1. an industrial production device for 2-chloro-4-monomethylaniline .-5-sulfonic acid, including three dosing pumps (401,402,403),
Three measuring tanks (301,302,303), one-tenth salt oven (101), sulphonation kettle (102), profit automatic water distributor (304), reaction water connect
Groove (305), solvent groove (306), solvent medial launder (308), filter rinsing exsiccator (501), two strip transmission lines (601,
602), dissolution kettle (202), centrifuge (502), distillating still (204), two condensers (201,203), two vacuum buffer grooves
(307,309) and solvent pump (404), is characterized in that the outlet of the first dosing pump (401) and the import phase of the first measuring tank (301)
Even, the outlet of the second dosing pump (402) is connected with the import of the second measuring tank (302), the outlet of the 3rd dosing pump (403) and the
The import of three measuring tanks (303) is connected, and the outlet of the first measuring tank (301) is connected with the first charging aperture becoming salt oven (101), the
The outlet of two measuring tanks (302) with become salt oven (101) the second charging aperture be connected, the outlet of the 3rd measuring tank (303) respectively with
Become the second charging aperture of salt oven (101), the second charging aperture of sulphonation kettle (102), filter the second charging rinsing exsiccator (501)
Mouth is connected；The discharging opening becoming salt oven (101) is connected with the first charging aperture of sulphonation kettle (102), the gaseous phase outlet of sulphonation kettle (102)
It is connected by the import of the first condenser (201) with profit automatic water distributor (304), the water outlet of profit automatic water distributor (304)
Mouth is connected with the import of reaction water groove (305), and the oil-out of profit automatic water distributor (304) enters with solvent groove (306)
Mouthful being connected, the oil-out of profit automatic water distributor (304) also refluxing opening with sulphonation kettle (102) is connected, profit automatic water distributor
(304) gaseous phase outlet at top and the import of the first vacuum buffer groove (307) are connected；Sulphonation kettle (102) bottom discharging opening with
The first charging aperture filtering rinsing exsiccator (501) is connected, and filters the discharging opening of rinsing exsiccator (501) bottom by the first powder
Body pipeline (601) is connected with the charging aperture of dissolution kettle (202), the discharging opening of dissolution kettle (202) bottom and centrifuge (502)
Charging aperture is connected, and the discharging opening of centrifuge (502) bottom and the charging aperture of the second powder conveying line (602) are connected；Filter rinsing
The liquid phase discharging opening of exsiccator (501) side is connected with the charging aperture of distillating still (204), filters rinsing exsiccator (501) top
Gaseous phase outlet and the second condenser (203) gas phase import be connected；The gaseous phase outlet of distillating still (204) and the second condenser
(203) gas phase import is connected, and the liquid-phase outlet of the second condenser (203) is connected with the charging aperture of solvent medial launder (308), molten
The discharging opening of agent medial launder (308) bottom is connected with the import of solvent pump (404), the gas phase mouth at solvent medial launder (308) top
Import with the second vacuum buffer groove (309) is connected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620469912.8U CN205774223U (en) | 2016-05-20 | 2016-05-20 | The industrial production device of 2 chlorine 4 monomethylaniline. 5 sulfonic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620469912.8U CN205774223U (en) | 2016-05-20 | 2016-05-20 | The industrial production device of 2 chlorine 4 monomethylaniline. 5 sulfonic acid |
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| CN201620469912.8U Expired - Fee Related CN205774223U (en) | 2016-05-20 | 2016-05-20 | The industrial production device of 2 chlorine 4 monomethylaniline. 5 sulfonic acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800512A (en) * | 2017-01-06 | 2017-06-06 | 浙江荣耀生物科技有限公司 | The preparation method and preparation facilities of a kind of 3,5 dinitro o methyl benzoic acid |
| CN107266342A (en) * | 2017-08-04 | 2017-10-20 | 吴赣药业（苏州）有限公司 | A kind of industrial sulfanilamide (SN) production system |
-
2016
- 2016-05-20 CN CN201620469912.8U patent/CN205774223U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800512A (en) * | 2017-01-06 | 2017-06-06 | 浙江荣耀生物科技有限公司 | The preparation method and preparation facilities of a kind of 3,5 dinitro o methyl benzoic acid |
| CN107266342A (en) * | 2017-08-04 | 2017-10-20 | 吴赣药业（苏州）有限公司 | A kind of industrial sulfanilamide (SN) production system |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20161207 |