CN103130679B - Method and device for automatic control continuous production of diazo compound - Google Patents
Method and device for automatic control continuous production of diazo compound Download PDFInfo
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Abstract
The invention relates to a method for automatic control continuous production of a diazo compound. The method comprises the steps of metering raw materials, continuously feeding, reacting in a tubular diazotization reactor, and continuously discharging. The method is characterized in that a plurality of reaction state detection devices are arranged on the reactor, and a completely-reacted reaction solution is continuously discharged in time through multipoint automatic control; and the materials which are abnormal during blending are pumped back into a blending kettle in time for re-blending. By adopting the method, accurate automatic control continuous reaction of diazotization is realized, the stability of the quality of products is ensured, the reaction time is shortened, the production efficiency is improved, the production cost is reduced, the generation of the three wastes is reduced, the effects of low pollution and low consumption are achieved, and cyclic economy and cleaner production are realized.
Description
Technical field
The present invention relates to a kind of automatic control continuous production method and device of diazonium compound.
Background technology
Dyestuffs industries is one of historical the longest industry in Fine Chemical Industry.Along with the development of China light and textile industries, dyestuffs industries is also developed rapidly in recent years; Especially since entering the new millennium, China's dyestuffs industries development is more rapid, and output, export volume and consumption all leap to the first in the world.But the mode of production of China's dyestuff is still relatively backward at present, automatic control technology is not yet truly applied in DYE PRODUCTION process, and the automation level of enterprise is generally lower.Therefore the automatization level that, improves this field is the target of insider's unremitting pursue always.
As everyone knows, the preparation of azoic dyestuff is generally comprised of step diazotization reaction and coupled reaction.In diazotization reaction, diazonium salt at high temperature easily decomposes, and the preparation of diazonium salt is a thermopositive reaction, and therefore, production process is quite high to the requirement of conducting heat.
Conventional batch reactor, is difficult to guarantee that each position all stirs.Local material proportion departs from reaction conditions, and in reactor, the phenomenon such as non-uniform temperature, all can cause diazonium salt to decompose, and various side reactions occur and causes that diazonium salt quality is not good and dyestuffs purity is on the low side, yield is on the low side.
Tubular reactor is because the geometrical dimension of conversion zone is little, and is continuous flow reactor, makes reaction evenly mix and react within a very little interval and very short time, at utmost avoided the generation of side reaction.Tubular reactor is better than batch reactor, is mainly reflected in: reaction mass can be mixed evenly moment, is filled with to be beneficial to prevent compound decomposition; Accurately control temperature of reaction, be conducive to improve yield and reaction preference; Online reaction volume is little, has guaranteed the security of reaction; Continuous reaction, it is poor to reduce to criticize.Therefore, adopting tubular reactor to produce continuously tool is of great significance.
A kind of method and apparatus of continuously preparing diazonium salt of triarylamine is disclosed in Chinese patent Publication CN1365968A, comprise that uncle's arylamine inputs continuously one with the bottom of the tubular reactor of cooling jacket with sour mixing solutions together with sodium nitrite solution, reaction product flows out from the top of tubular reactor.This method and device have overcome the more diazotizing defects of intermittent type uncle's arylamine, avoided the too high and decomposition of the diazonium salt that causes of local temperature, yet this method and device are not described to the accurate control of the continuous preparation process of diazonium salt, therefore, this method and device still need to improve.
Summary of the invention
The invention provides a kind of diazonium compound and automatically control continuous production method, described method comprises reacts reaction raw materials ratio continuous feeding according to the rules continuous discharge to tubular type diazotization reaction device, it is characterized in that, a plurality of polar voltages Controlling System are set on tubular type diazotization reaction device, when reaction mass process polar voltages Controlling System, polar voltages Controlling System detects response behaviour, according to the voltage judgement response behaviour of polar voltages Controlling System, if determine that after testing reaction completes, and carries out continuous discharge; If determine that after testing reaction not yet completes, reaction mass enters downstream tubular type diazotization reaction device and proceeds reaction.
Further, the invention provides a kind of diazonium compound and automatically control continuous production method, described method comprises prepares burden reaction raw materials ratio continuous feeding to batching kettle according to the rules, the material continuous feeding of joining in batching kettle reacts and continuous discharge to tubular type diazotization reaction device, it is characterized in that, a plurality of polar voltages Controlling System are set on tubular type diazotization reaction device, when reaction mass process polar voltages Controlling System, polar voltages Controlling System detects response behaviour, according to the voltage judgement response behaviour of polar voltages Controlling System, if determine that after testing reaction completes, carry out continuous discharge, if determine that after testing reaction not yet completes, and reaction mass do not occur that batching is abnormal, and reaction mass enters downstream tubular reactor and proceeds reaction, if determine that after testing reaction not yet completes, and reaction mass occurs that batching is abnormal, is back to batching kettle by reaction mass and again prepares burden.
In aforesaid method, the reaction end near zone of preferred described polar voltages set-up of control system on tubular type diazotization reaction device.
In aforesaid method, the setting of preferred described polar voltages Controlling System on tubular reactor is distributed as after educt flow is dredged to going forward close.
In aforesaid method, preferred described polar voltages set-up of control system spacing be reaction mass in diazotization reaction device flow 10min～30min the distance of process.
In aforesaid method, reaction mass occurs that the abnormal detection method of batching is: when the voltage readings of polar voltages Controlling System does not reach reaction end reading, and the voltage readings of this polar voltages Controlling System is compared with the voltage readings of last polar voltages Controlling System, numerical value change is less than the value of setting, is defined as reaction mass and occurs that batching is abnormal.
In aforesaid method, the electrode materials of preferred described polar voltages Controlling System is a kind of or its alloy that is selected from Au, Pt, Ag, Sb, Mo, Cr, graphite.
Aforesaid method preferably includes:
Diazo component, nitrosyl sulfuric acid and optional acid are prepared burden to batching kettle by measuring apparatus ratio continuously feeding according to the rules;
Streams in batching kettle is to tubular type diazotization reaction device, and controlling diazotization reaction temperature is-10 ℃～30 ℃;
Diazotization reaction material detects through polar voltages Controlling System, if reacted, carries out continuous discharge; If reaction not yet completes, and reaction mass do not occur that batching is abnormal, and reaction mass enters downstream tubular type diazotization reaction device and proceeds reaction; If reaction not yet completes, and occur that batching is abnormal, is back to batching kettle by reaction mass, by regulating each measuring apparatus again to prepare burden.
In aforesaid method, preferably feed product diazo component, optional acid and the flow of nitrosyl sulfuric acid and the flow of heat-eliminating medium and temperature of reaction are carried out to interlocked control, comprise set temperature upper lower limit value, when temperature of reaction is during higher than higher limit, turn in proportion or close each feed product flow down, tune up the flow of heat-eliminating medium simultaneously, when temperature of reaction is during lower than lower value, turn the flow of heat-eliminating medium down, until temperature of reaction is within the scope of bound.
In aforesaid method, preferably diazo component, nitrosyl sulfuric acid and optional sour mol ratio are 1:1.0～3.0:0～10.
In aforesaid method, preferred described batching kettle material is titanium or stainless steel, and the temperature of batching kettle is controlled by this dual-cooled device of shell-and tube condenser in cooling jacket and pipe.
In aforesaid method, preferred described batching kettle is provided with overflow port, material in batching kettle flows out by described overflow port, overflow port place is provided with vibration filters, the filtering net aperture of described vibration filters is 5～40 orders, and the filtering net material of described vibration filters is to be selected from any in titanium, stainless steel, glass fibre, charcoal fiber, fluoroplastics.
In aforesaid method, preferred described tubular type diazotization reaction equipment material adopts titanium or stainless steel, and in pipe, temperature is controlled by this dual-cooled device of shell-and tube condenser in cooling jacket and pipe.
In aforesaid method, preferably it is controlled automatically by DCS Controlling System.
The present invention also provides a kind of diazonium compound automatically to control continuous production device, it is characterized in that comprising: a plurality of polar voltages Controlling System that arrange on tubular type diazotization reaction device and tubular type diazotization reaction device, when described diazonium compound is controlled continuous production device operation automatically, operational process comprises: reaction raw materials ratio continuous feeding according to the rules reacts and continuous discharge to tubular type diazotization reaction device, wherein when reaction mass process polar voltages Controlling System, polar voltages Controlling System is for detecting response behaviour, according to the voltage judgement response behaviour of polar voltages Controlling System, if determine that after testing reaction completes, carry out continuous discharge, if determine that after testing reaction not yet completes, can make reaction mass enter downstream reactor and proceed reaction.
Further, the invention provides a kind of diazonium compound and automatically control continuous production device, it is characterized in that, also comprise batching kettle, when described diazonium compound is controlled continuous production device operation automatically, operational process comprises: reaction raw materials ratio continuous feeding to batching kettle is according to the rules prepared burden, the material continuous feeding of joining in batching kettle reacts and continuous discharge to tubular type diazotization reaction device, wherein when reaction mass process polar voltages Controlling System, polar voltages Controlling System detects response behaviour, according to the voltage judgement response behaviour of polar voltages Controlling System, if determine that after testing reaction completes, carry out continuous discharge, if determine that after testing reaction not yet completes, and reaction mass do not occur that batching is abnormal, and reaction mass enters downstream tubular reactor and proceeds reaction, if determine that after testing reaction not yet completes, and reaction mass occurs that batching is abnormal, is back to batching kettle by reaction mass and again prepares burden.
In said apparatus, the reaction end near zone of preferred described polar voltages set-up of control system on tubular type diazotization reaction device.
In said apparatus, the setting of preferred described polar voltages Controlling System on tubular reactor is distributed as after educt flow is dredged to going forward close.
In said apparatus, preferred described polar voltages set-up of control system spacing be reaction mass in diazotization reaction device flow 10min～30min the distance of process.
In said apparatus, the electrode materials of preferred described polar voltages Controlling System is a kind of or its alloy that is selected from Au, Pt, Ag, Sb, Mo, Cr, graphite.
Said apparatus preferably includes raw material feed device, measuring apparatus, batching kettle, tubular type diazotization reaction device, is arranged on polar voltages Controlling System, refrigerating unit, device for monitoring temperature on tubular type diazotization reaction device, when described diazonium compound is controlled continuous production device operation automatically, operational process comprises:
Diazo component, nitrosyl sulfuric acid and optional acid are prepared burden to batching kettle by measuring apparatus ratio continuously feeding according to the rules;
Streams in batching kettle is carried out diazotization reaction to tubular type diazotization reaction device;
Diazotization reaction material detects through polar voltages Controlling System, if reacted, carries out continuous discharge; If reaction not yet completes, and reaction mass do not occur that batching is abnormal, and reaction mass enters downstream tubular type diazotization reaction device and proceeds reaction; If reaction not yet completes, and the voltage readings of described polar voltages Controlling System is compared with the voltage readings of last polar voltages Controlling System, numerical value change is less than the value of setting, and reaction mass is back to batching kettle, by regulating each measuring apparatus again to prepare burden.
In said apparatus, preferably to measuring apparatus, refrigerating unit, the device for monitoring temperature control that links, thereby in when operation by raw material feed device Raw material diazo component, in nitrosyl sulfuric acid and optional sour flow and refrigerating unit, flow and the temperature of reaction of heat-eliminating medium are carried out interlocked control, control process comprises set temperature upper lower limit value, when temperature of reaction is during higher than higher limit, turn in proportion or close each feed product flow down, tune up the flow of heat-eliminating medium simultaneously, when temperature of reaction is during lower than lower value, turn the flow of heat-eliminating medium down, until temperature of reaction is within the scope of bound.
In said apparatus, preferred described batching kettle material is titanium or stainless steel, and batching kettle temperature is controlled by this dual-cooled device of shell-and tube condenser in cooling jacket and pipe by temperature regulator.
In said apparatus, preferred described batching kettle is provided with overflow port, material in batching kettle flows out by described overflow port, overflow port place is provided with vibration filters, the filtering net aperture of described vibration filters is 5～40 orders, and the filtering net material of described vibration filters is to be selected from any in titanium, stainless steel, glass fibre, charcoal fiber, fluoroplastics.
In said apparatus, preferred described tubular reactor material adopts titanium or stainless steel, and in pipe, temperature is controlled by this dual-cooled device of shell-and tube condenser in cooling jacket and pipe.
Preferably it controls by DCS Controlling System said apparatus automatically.
Diazonium compound of the present invention automatically controls continuous production method and device is controlled by automatic, in time the reaction solution having reacted is carried out to continuous discharge, and the abnormal timely blowback of material to the batching kettle of batching appearance is prepared burden again, realized and accurately automatically controlled serialization production diazonium compound, guaranteed the stable of quality product, shortened the production time, improved production efficiency, reduced production cost, reduced the generation of the three wastes, the effect that has reached low dirty low consumption, has realized recycling industries and clean production.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that diazonium compound of the present invention is controlled continuous production method automatically.
Fig. 2 is the schematic diagram that diazonium compound of the present invention is controlled continuous production device automatically.
In Fig. 2, A is batching kettle; J1, J2 are scale tank; M is cage device; P1 is solid measuring apparatus; P2, P3, P4, P5 are pump or volume pump; H is vibration filters; K1～K6 is polar voltages Controlling System; F is valve; G is tubular type diazotization reaction device, and D is transfer still.
Embodiment
Referring to accompanying drawing, the present invention is further described.
Fig. 2 shown device carries out automatization control by DCS Controlling System.
In Fig. 2, to diazotization reaction raw material measuring apparatus P1, P2, P3, refrigerating unit (shell-and tube condenser in the cooling jacket of batching kettle A and tubular reactor G and pipe, not shown), the control that links of device for monitoring temperature (not shown), by diazo component, in nitrosyl sulfuric acid and optional sour flow and refrigerating unit, flow and the temperature of reaction of heat-eliminating medium are carried out interlocked control, when temperature of reaction is during higher than set higher limit, turn in proportion or close each feed product flow down, tune up the flow of heat-eliminating medium simultaneously, when temperature of reaction lower than set lower value time, turn the flow of heat-eliminating medium down, until temperature of reaction is within the scope of bound.
In Fig. 2, in batching kettle A, diazo component carries out continuously feeding by cage M by measuring apparatus P1, and optional acid and nitrosyl sulfuric acid are by volume pump P2, P3 continuously feeding, and the mol ratio of material is diazo component: nitrosyl sulfuric acid: acid=1:1.0～1.1:0～8.
The material overflowing in batching kettle A, flow in tubular type diazotization reaction device G, controls doazo reaction temperature at-10 ℃～30 ℃.Temperature in described diazotization reaction device G is controlled by this dual-cooled device of shell-and tube condenser in cooling jacket and pipe, and a plurality of polar voltages Controlling System are housed on tubular type diazotization reaction device.
Diazotization reaction material after polar voltages Controlling System detection reaction completes, continuous discharge.If reaction not yet completes, and reaction mass do not occur that batching is abnormal, and reaction mass enters downstream tubular type diazotization reaction device G and proceeds reaction; If reaction not yet completes, and the voltage readings of this polar voltages Controlling System is compared with the voltage readings of last polar voltages Controlling System, numerical value change is less than the value of setting, by pump P4 by reaction mass blowback to batching kettle A, regulate measuring apparatus P1, P2, P3 again to prepare burden.
Embodiment
Embodiment 1
The nitrosyl sulfuric acid (quality percentage composition is 28%) that adds 420kg in batching kettle A, open chilled brine, control temperature in the kettle at 20 ℃～30 ℃, slowly twist into 2, 4-dinitrobenzene-6-chloroaniline 200kg mixes and is made into initiator, open 2, 4-dinitrobenzene-6-chloroaniline (diazo component), nitrosyl sulfuric acid material inlet valve, the two controls input speed by measuring apparatus is respectively 571kg/h, 1200kg/h carries out continuously feeding, mixture flow to tubular reactor G and reacts from overflow port, after polar voltages Controlling System detection reaction completes, reaction product continuous discharge, obtain diazo solution.
Adopt above-mentioned diazonium compound automatically to control continuous production method and device production diazonium compound, realized multiple spot and accurately automatically controlled production continuously, compare with intermittent reaction, cost of labor has declined approximately 35%, and energy consumption has declined approximately 25%.
Embodiment 2: the nitrosyl sulfuric acid (quality percentage composition is 28%) that adds 380kg in batching kettle A, the sulfuric acid of 660kg, open chilled brine, control temperature in the kettle at 0 ℃～5 ℃, slowly twist into 2 cyano 4 nitro 6 bromo aniline 200kg and mix and be made into initiator, join complete, open 2 cyano 4 nitro 6 bromo aniline (diazo component), sulfuric acid and nitrosyl sulfuric acid material inlet valve, three respectively measure control is 300kg/h, 990kg/h, 570kg/h carries out continuously feeding, mixture flow to tubular reactor G and reacts from overflow port, after polar voltages Controlling System detection reaction completes, reaction mass (diazo solution) carries out continuous discharge.When educt flow installs after testing, reading shows when the voltage readings do not reach reaction end and this polar voltages Controlling System is compared numerical value change with the voltage readings of last polar voltages Controlling System and is less than the value of setting, close pump P1, P2 and P3, open pump P4, by reaction mass blowback batching kettle A, by regulating P1, P2 and P3 again to prepare burden.After recovering normally, close pump P4, open pump P1, P2 and P3, return to normal production.
Adopt above-mentioned diazonium compound automatically to control continuous production method and device production diazonium compound, realized multiple spot and accurately automatically controlled, the production cycle is 6 hours, and Qualified Products Rate is 100%.Compare with general continuous production technology, this production cycle has shortened 25%.
Embodiment 3:
The nitrosyl sulfuric acid (quality percentage composition is 28%) that adds 690kg in batching kettle A, open chilled brine, control temperature in the kettle at 20 ℃～30 ℃, slowly twist into 2, 4-dinitrobenzene-6-bromaniline 330kg is hybridly prepared into initiator, join complete, open 2, 4-dinitrobenzene-6-bromaniline (diazo component), nitrosyl sulfuric acid material inlet valve, the two respectively measure control be 495kg/h, 1035kg/h carries out continuously feeding, mixture flow to tubular reactor G and reacts from overflow port, after polar voltages Controlling System detection reaction completes, diazo solution carries out continuous discharge.
Adopt above-mentioned diazonium compound automatically to control continuous production method and device production diazonium compound, realized multiple spot and accurately automatically controlled, the qualification rate of quality product is 100%.Compare with general continuous production technology, the production cycle of this dyestuff has shortened 20%, and energy consumption declines to a great extent, and has reduced production cost.
Claims (26)
1. a diazonium compound is controlled continuous production method automatically, described method comprises reacts reaction raw materials ratio continuous feeding according to the rules continuous discharge to tubular type diazotization reaction device, it is characterized in that, a plurality of polar voltages Controlling System are set on tubular type diazotization reaction device, when reaction mass process polar voltages Controlling System, polar voltages Controlling System detects response behaviour, according to the voltage judgement response behaviour of polar voltages Controlling System, if determine that after testing reaction completes, and carries out continuous discharge; If determine that after testing reaction not yet completes, reaction mass enters downstream tubular type diazotization reaction device and proceeds reaction.
2. diazonium compound as claimed in claim 1 is controlled continuous production method automatically, described method comprises prepares burden reaction raw materials ratio continuous feeding to batching kettle according to the rules, the material continuous feeding of joining in batching kettle reacts and continuous discharge to tubular type diazotization reaction device, a plurality of polar voltages Controlling System are set on tubular type diazotization reaction device, when reaction mass process polar voltages Controlling System, polar voltages Controlling System detects response behaviour, according to the voltage judgement response behaviour of polar voltages Controlling System, if determine that after testing reaction completes, carry out continuous discharge, if determine that after testing reaction not yet completes, and reaction mass do not occur that batching is abnormal, and reaction mass enters downstream tubular reactor and proceeds reaction, if determine that after testing reaction not yet completes, and reaction mass occurs that batching is abnormal, is back to batching kettle by reaction mass and again prepares burden.
3. diazonium compound as claimed in claim 1 or 2 is controlled continuous production method automatically, it is characterized in that, the reaction end near zone of described polar voltages set-up of control system on tubular type diazotization reaction device.
4. diazonium compound as claimed in claim 1 or 2 is controlled continuous production method automatically, it is characterized in that, the setting of described polar voltages Controlling System on tubular reactor is distributed as after educt flow is dredged to going forward close.
5. diazonium compound as claimed in claim 1 or 2 is controlled continuous production method automatically, it is characterized in that described polar voltages set-up of control system spacing be reaction mass in diazotization reaction device flow 10min～30min the distance of process.
6. diazonium compound as claimed in claim 2 is controlled continuous production method automatically, it is characterized in that, reaction mass occurs that the abnormal detection method of batching is: when the voltage readings of polar voltages Controlling System does not reach reaction end reading, and the voltage readings of this polar voltages Controlling System is compared with the voltage readings of last polar voltages Controlling System, numerical value change is less than the value of setting, is defined as reaction mass and occurs that batching is abnormal.
7. diazonium compound as claimed in claim 6 is controlled continuous production method automatically, it is characterized in that, the electrode materials of described polar voltages Controlling System is a kind of or its alloy that is selected from Au, Pt, Ag, Sb, Mo, Cr, graphite.
8. the diazonium compound as described in claim 2,6,7 any one is controlled continuous production method automatically, it is characterized in that comprising:
Diazo component, nitrosyl sulfuric acid and optional acid are prepared burden to batching kettle by measuring apparatus ratio continuously feeding according to the rules;
Streams in batching kettle is to tubular type diazotization reaction device, and controlling diazotization reaction temperature is-10 ℃～30 ℃;
Diazotization reaction material detects through polar voltages Controlling System, if reacted, carries out continuous discharge; If reaction not yet completes, and reaction mass do not occur that batching is abnormal, and reaction mass enters downstream tubular type diazotization reaction device and proceeds reaction; If reaction not yet completes, and occur that batching is abnormal, is back to batching kettle by reaction mass, by regulating each measuring apparatus again to prepare burden.
9. diazonium compound as claimed in claim 8 is controlled continuous production method automatically, it is characterized in that, feed product diazo component, optional acid and the flow of nitrosyl sulfuric acid and the flow of heat-eliminating medium and temperature of reaction are carried out to interlocked control, comprise set temperature upper lower limit value, when temperature of reaction is during higher than higher limit, turn in proportion or close each feed product flow down, tune up the flow of heat-eliminating medium simultaneously, when temperature of reaction is during lower than lower value, turn the flow of heat-eliminating medium down, until temperature of reaction is within the scope of bound.
10. diazonium compound as claimed in claim 8 is controlled continuous production method automatically, and wherein diazo component, nitrosyl sulfuric acid and optional sour mol ratio are 1:1.0～3.0:0～10.
11. diazonium compounds as described in claim 2,6,7 any one are controlled continuous production method automatically, it is characterized in that described batching kettle material is titanium or stainless steel, the temperature of batching kettle is controlled by this dual-cooled device of shell-and tube condenser in cooling jacket and pipe.
12. diazonium compounds as described in claim 2,6,7 any one are controlled continuous production method automatically, it is characterized in that, described batching kettle is provided with overflow port, material in batching kettle flows out by described overflow port, overflow port place is provided with vibration filters, the filtering net aperture of described vibration filters is 5～40 orders, and the filtering net material of described vibration filters is to be selected from any in titanium, stainless steel, glass fibre, charcoal fiber, fluoroplastics.
13. diazonium compounds as described in claim 1,2,6,7 any one are controlled continuous production method automatically, wherein said tubular type diazotization reaction equipment material adopts titanium or stainless steel, and in pipe, temperature is controlled by this dual-cooled device of shell-and tube condenser in cooling jacket and pipe.
14. diazonium compounds as described in claim 1,2,6,7 any one are controlled continuous production method automatically, and it is controlled automatically by DCS Controlling System.
15. 1 kinds of diazonium compounds are controlled continuous production device automatically, it is characterized in that comprising: a plurality of polar voltages Controlling System that arrange on tubular type diazotization reaction device and tubular type diazotization reaction device, when described diazonium compound is controlled continuous production device operation automatically, operational process comprises: reaction raw materials ratio continuous feeding according to the rules reacts and continuous discharge to tubular type diazotization reaction device, wherein when reaction mass process polar voltages Controlling System, polar voltages Controlling System is for detecting response behaviour, according to the voltage judgement response behaviour of polar voltages Controlling System, if determine that after testing reaction completes, carry out continuous discharge, if determine that after testing reaction not yet completes, can make reaction mass enter downstream reactor and proceed reaction.
16. diazonium compounds as claimed in claim 15 are controlled continuous production device automatically, it is characterized in that, also comprise batching kettle, when described diazonium compound is controlled continuous production device operation automatically, operational process comprises: reaction raw materials ratio continuous feeding to batching kettle is according to the rules prepared burden, the material continuous feeding of joining in batching kettle reacts and continuous discharge to tubular type diazotization reaction device, wherein when reaction mass process polar voltages Controlling System, polar voltages Controlling System detects response behaviour, according to the voltage judgement response behaviour of polar voltages Controlling System, if determine that after testing reaction completes, carry out continuous discharge, if determine that after testing reaction not yet completes, and reaction mass do not occur that batching is abnormal, and reaction mass enters downstream tubular reactor and proceeds reaction, if determine that after testing reaction not yet completes, and reaction mass occurs that batching is abnormal, is back to batching kettle by reaction mass and again prepares burden.
17. diazonium compounds as described in claim 15 or 16 are controlled continuous production device automatically, it is characterized in that the reaction end near zone of described polar voltages set-up of control system on tubular type diazotization reaction device.
18. diazonium compounds as described in claim 15 or 16 are controlled continuous production device automatically, it is characterized in that, the setting of described polar voltages Controlling System on tubular reactor is distributed as after educt flow is dredged to going forward close.
19. diazonium compounds as described in claim 15 or 16 are controlled continuous production device automatically, it is characterized in that described polar voltages set-up of control system spacing be reaction mass in diazotization reaction device flow 10min～30min the distance of process.
20. diazonium compounds as described in claim 15 or 16 are controlled continuous production device automatically, it is characterized in that, the electrode materials of described polar voltages Controlling System is a kind of or its alloy that is selected from Au, Pt, Ag, Sb, Mo, Cr, graphite.
21. diazonium compounds as claimed in claim 16 are controlled continuous production device automatically, comprise raw material feed device, measuring apparatus, batching kettle, tubular type diazotization reaction device, be arranged on polar voltages Controlling System, refrigerating unit, device for monitoring temperature on tubular type diazotization reaction device, when described diazonium compound is controlled continuous production device operation automatically, operational process comprises:
Diazo component, nitrosyl sulfuric acid and optional acid are prepared burden to batching kettle by measuring apparatus ratio continuously feeding according to the rules;
Streams in batching kettle is carried out diazotization reaction to tubular type diazotization reaction device;
Diazotization reaction material detects through polar voltages Controlling System, if reacted, carries out continuous discharge; If reaction not yet completes, and reaction mass do not occur that batching is abnormal, and reaction mass enters downstream tubular type diazotization reaction device and proceeds reaction; If reaction not yet completes, and the voltage readings of described polar voltages Controlling System is compared with the voltage readings of last polar voltages Controlling System, numerical value change is less than the value of setting, and reaction mass is back to batching kettle, by regulating each measuring apparatus again to prepare burden.
22. diazonium compounds as claimed in claim 21 are controlled continuous production device automatically, it is characterized in that, to measuring apparatus, refrigerating unit, the device for monitoring temperature control that links, thereby in when operation by raw material feed device Raw material diazo component, in nitrosyl sulfuric acid and optional sour flow and refrigerating unit, flow and the temperature of reaction of heat-eliminating medium are carried out interlocked control, control process comprises set temperature upper lower limit value, when temperature of reaction is during higher than higher limit, turn in proportion or close each feed product flow down, tune up the flow of heat-eliminating medium simultaneously, when temperature of reaction is during lower than lower value, turn the flow of heat-eliminating medium down, until temperature of reaction is within the scope of bound.
23. diazonium compounds as described in claim 16,21,22 any one are controlled continuous production device automatically, it is characterized in that described batching kettle material is titanium or stainless steel, batching kettle temperature is controlled by this dual-cooled device of shell-and tube condenser in cooling jacket and pipe by temperature regulator.
24. diazonium compounds as described in claim 16,21,22 any one are controlled continuous production device automatically, it is characterized in that, described batching kettle is provided with overflow port, material in batching kettle flows out by described overflow port, overflow port place is provided with vibration filters, the filtering net aperture of described vibration filters is 5～40 orders, and the filtering net material of described vibration filters is to be selected from any in titanium, stainless steel, glass fibre, charcoal fiber, fluoroplastics.
25. diazonium compounds as described in claim 15,16,21,22 any one are controlled continuous production device automatically, wherein said tubular reactor material adopts titanium or stainless steel, and in pipe, temperature is controlled by this dual-cooled device of shell-and tube condenser in cooling jacket and pipe.
26. diazonium compounds as described in claim 15,16,21,22 any one are controlled continuous production device automatically, and it is controlled automatically by DCS Controlling System.
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|---|---|---|---|---|
| CN105367443B (en) * | 2014-08-29 | 2017-12-01 | 浙江迪邦化工有限公司 | The continuous production processes and device of a kind of diazonium compound |
| CN110433755B (en) * | 2019-07-29 | 2021-04-09 | 浙江迪邦化工有限公司 | Method and device for continuously preparing diazo compound |
| CN113527136B (en) * | 2021-08-19 | 2023-08-04 | 浙江迪邦化工有限公司 | System and process for producing diazonium salt of p-nitroaniline |
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| CN1365968A (en) * | 2001-01-19 | 2002-08-28 | 上海家化（集团）有限公司 | Process for equipment for continuously preparing diazonium salt of triarylamine |
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|---|---|
| CN103130679A (en) | 2013-06-05 |
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