CN103788706B - Dyestuff controls continuous production method and device automatically - Google Patents
Dyestuff controls continuous production method and device automatically Download PDFInfo
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- CN103788706B CN103788706B CN201410026479.6A CN201410026479A CN103788706B CN 103788706 B CN103788706 B CN 103788706B CN 201410026479 A CN201410026479 A CN 201410026479A CN 103788706 B CN103788706 B CN 103788706B
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Abstract
A kind of dyestuff controls continuous production method and device automatically, by each raw material continuous feeding after metering, through tubular reactor reaction also continuous discharge, it is characterized in that, reactor arranges multiple response behaviour proofing unit, automatically controlled by multiple spot, in time the reaction solution reacted is transferred to subsequent processing; And batching is occurred that the abnormal timely blowback of material is prepared burden again to batching kettle, what achieve dyestuff accurately controls continuous seepage automatically, ensure that the stable of quality product, shorten the production time, improve production efficiency, reduce production cost, decrease the generation of the three wastes, reach the effect of low dirty low consumption, achieve recycling industries and clean production.
Description
The divisional application that the application is the applying date is on March 12nd, 2013, application number is 201310079181.7, denomination of invention is the application of " dyestuff controls continuous production method and device automatically ".
Technical field
The present invention relates to a kind of dyestuff and automatically control continuous production method and device.
Background technology
Dyestuffs industries is one of industry that in Fine Chemical Industry, history is the longest.In recent years along with the development of light and textile industries of China, dyestuffs industries have also been obtained fast development; Especially, since entering the new millennium, China's dyestuffs industries development is more rapid, and output, export volume and consumption leap to the first in the world all.But the mode of production of current China dyestuff still backwardness relatively, automatic control technology is not yet truly applied in DYE PRODUCTION process, and the automation level of enterprise is general lower.Therefore, the automatization level improving this field is the target of insider's unremitting pursue always.
As everyone knows, the preparation of azoic dyestuff is generally made up 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, the requirement of production process to heat transfer is quite high.In coupled reaction, diazonium salt also easily decomposes, if diazonium salt molecule can not collide with coupling component molecule at short notice and react, then will soon decompose.
General batch reactor, is difficult to ensure that each position all stirs.The material proportion of local departs from reaction conditions, and in reactor, the phenomenon such as non-uniform temperature, all can cause diazonium salt to decompose, and various side reaction occurs 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 because the geometrical dimension of conversion zone is little, and is continuous flow reactor, makes to react in a very little interval and evenly mixes and react in the very short time, at utmost avoiding the generation of side reaction.Tubular reactor is better than batch reactor, is mainly reflected in: reaction mass can be mixed evenly instantaneously, is filled with to be beneficial to prevent compound decomposition; Accurate control temperature of reaction, is conducive to improving yield and reaction preference; Online reaction volume is little, ensure that the security of reaction; Continuous reaction, it is poor that reduction is criticized.Therefore, tubular reactor continuous seepage dyestuff tool is adopted to be of great significance.
A kind of method and apparatus of continuously preparing diazonium salt of triarylamine is disclosed in Chinese patent Publication CN1365968A, comprise uncle's arylamine and input a bottom with the tubular reactor of cooling jacket with the mixing solutions of acid continuously together with sodium nitrite solution, reaction product flows out from the top of tubular reactor.This method and device overcome the more diazotizing defects of intermittent type uncle's arylamine, avoid the too high and decomposition of the diazonium salt caused of local temperature, but 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 dyestuff and automatically control continuous production method, described method comprises carries out reaction and continuous discharge by reaction raw materials according to the ratio continuous feeding of regulation to tubular reactor, tubular reactor arranges multiple response behaviour proofing unit, when reaction mass is through response behaviour proofing unit, response behaviour proofing unit detects response behaviour, if determine that reaction completes after testing, then reaction mass is gone to subsequent processing; If determine that reaction not yet completes after testing, then reaction mass enters downstream tubular reactor and proceeds reaction.
Further, the invention provides a kind of dyestuff and automatically control continuous production method, described method comprises prepares burden the ratio continuous feeding of reaction raw materials according to regulation to batching kettle, the material continuous feeding of joining in batching kettle carries out reaction and continuous discharge to tubular reactor, tubular reactor arranges multiple response behaviour proofing unit, when reaction mass is through response behaviour proofing unit, response behaviour proofing unit detects response behaviour, if determine that reaction completes after testing, then reaction mass is gone to subsequent processing; If determine that reaction not yet completes after testing, and reaction mass does not occur that batching is abnormal, then reaction mass enters downstream tubular reactor and proceeds reaction; If determine that reaction not yet completes after testing, and reaction mass occurs that batching is abnormal, then reaction mass is back to batching kettle and again prepares burden.
In aforesaid method, preferably described response behaviour proofing unit is arranged on the reaction end near zone on tubular reactor.
In aforesaid method, the setting of preferred described response behaviour proofing unit on tubular reactor is distributed as after educt flow is dredged to going forward close.
In aforesaid method, preferred described response behaviour proofing unit setting space be in reactor reaction mass flowing 10min ~ 30min the distance of process.
In aforesaid method, preferred described response behaviour proofing unit is polar voltages Controlling System or potential measurement Controlling System.Polar voltages Controlling System and potential measurement Controlling System are respectively by the voltage detected and current potential determination response behaviour.Reaction mass occurs that the detection method that batching is abnormal is: when the current potential of response behaviour proofing unit or voltage readings do not reach reaction end reading, and compared with the current potential of the current potential of this response behaviour proofing unit or voltage readings and last response behaviour proofing unit or voltage readings, numerical value change is less than the value of setting, be then defined as reaction mass and occur that batching is abnormal.
In aforesaid method, the electrode materials of preferred described polar voltages Controlling System or potential measurement Controlling System is be selected from Au, Pt, Ag, Sb, Mo, Cr, the one of graphite or its alloy.
Preferred aforesaid method is the automatic control continuous production method of azoic dyestuff, comprises coupled reaction step, and coupled reaction is monitored by the multiple potential measurement Controlling System be arranged on tubular type coupling reactor.
In aforesaid method, preferably include: diazo solution and coupling component solution to be supplied in batching kettle according to the ratio specified continuously by measuring apparatus and to prepare burden; Material in batching kettle is overflowed by overflow port, flow in tubular type coupling reactor and carries out coupled reaction, controls coupled reaction temperature at-10 DEG C ~ 20 DEG C; Coupled reaction material detects through the potential measurement Controlling System as response behaviour proofing unit, if reacted, then flow to transfer still; If reaction not yet completes, and reaction mass does not occur that batching is abnormal, then reaction mass enters downstream tubular type coupling reactor and proceeds reaction; If reaction not yet completes, and the potential readings of described potential measurement Controlling System is compared with the potential readings of last potential measurement Controlling System, numerical value change is less than the value of setting, then reaction mass is back to batching kettle, again prepares burden by regulating each measuring apparatus; Proceeded in brilliant still by coupled reaction material in transfer still and carry out turning brilliant, controlling to turn brilliant temperature is 40 DEG C ~ 70 DEG C; Be fed into pressure filter carry out press filtration, washing by turning the material after crystalline substance, obtain dyestuff filter-cakes.
In aforesaid method, preferably in coupled reaction step, feed product diazo solution and the flow of coupling component solution and the flow of heat-eliminating medium and temperature of reaction are carried out interlocked control, comprise set temperature upper lower limit value, when temperature of reaction is higher than higher limit, turn or close each feed product flow in proportion down, tune up the flow of heat-eliminating medium simultaneously, when temperature of reaction is lower than lower value, then turn the flow of heat-eliminating medium down, until temperature of reaction is within the scope of bound.
In aforesaid method, preferably described diazonium compound and the mol ratio of coupling component are 1:0.95 ~ 1.05.
In aforesaid method, the mother liquid coming preferably produced press filtration, wash the washing water produced and carry out categorised collection recovery, be mixed with making beating liquid, the mass percent controlling acid in making beating liquid is 2 ~ 15%, for the preparation of coupling component solution.
Aforesaid method preferably also comprises diazotization reaction step, and diazotization reaction is also monitored by multiple polar voltages Controlling System.
In aforesaid method, preferred diazotization reaction step comprises: diazo component, nitrosyl sulfuric acid and optional acid are prepared burden to batching kettle by the ratio continuously feeding of measuring apparatus according to regulation; Streams in batching kettle is in tubular type diazotization reaction device, and controlling diazotization reaction temperature is-10 DEG C ~ 30 DEG C; Diazotization reaction material detects through polar voltages Controlling System, if reacted, then flow to transfer still; If reaction not yet completes, and reaction mass does not occur that batching is abnormal, then reaction mass enters downstream tubular type diazotization reaction device and proceeds reaction; If reaction not yet completes, and occur that batching is abnormal, then reaction mass being back to batching kettle, again preparing burden by regulating each measuring apparatus; Diazo solution in transfer still as the raw material of coupled reaction, for follow-up coupled reaction.
In aforesaid method, preferably in diazotization reaction step, 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 interlocked control, comprise set temperature upper lower limit value, when temperature of reaction is higher than higher limit, turn or close each feed product flow in proportion down, tune up the flow of heat-eliminating medium simultaneously, when temperature of reaction is lower than lower value, then turn the flow of heat-eliminating medium down, until temperature of reaction is within the scope of bound.
In aforesaid method, the mol ratio of preferred diazo component, nitrosyl sulfuric acid, acid is 1:1.0 ~ 1.1:0 ~ 8.
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 is overflowed by overflow port, described 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 be selected from any one in titanium, stainless steel, glass fibre, Carbon fibe, fluoroplastics.
In aforesaid method, 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.
In aforesaid method, automatically control preferably by DCS Controlling System.
The present invention also provides a kind of dyestuff automatically to control continuous production device, comprise: raw material feed device, measuring apparatus, multiple response behaviour proofing units that tubular reactor and tubular reactor are arranged, when described dyestuff controls continuous production device operation automatically, operational process comprises: reaction raw materials carries out reaction and continuous discharge according to the ratio continuous feeding of regulation to tubular reactor, wherein when reaction mass is through response behaviour proofing unit, response behaviour proofing unit detects response behaviour, if determine that reaction completes after testing, then reaction mass is gone to subsequent processing, if determine that reaction not yet completes after testing, then reaction mass enters downstream tubular reactor and proceeds reaction.
Further, production equipment of the present invention also comprises batching kettle, described dyestuff automatically controls continuous production device and also comprises batching kettle, when described dyestuff controls continuous production device operation automatically, operational process comprises: reaction raw materials is prepared burden to batching kettle according to the ratio continuous feeding of regulation, the material continuous feeding of joining in batching kettle carries out reaction and continuous discharge to tubular reactor, wherein, when reaction mass is through response behaviour proofing unit, response behaviour proofing unit detects response behaviour, if determine that reaction completes after testing, then reaction mass is gone to subsequent processing, if determine that reaction not yet completes after testing, and reaction mass does not occur that batching is abnormal, then reaction mass enters downstream tubular reactor and proceeds reaction, if determine that reaction not yet completes after testing, and reaction mass occurs that batching is abnormal, then reaction mass is back to batching kettle and again prepares burden.
In above-mentioned production equipment, preferably described response behaviour proofing unit is arranged on the reaction end near zone on tubular reactor.
In above-mentioned production equipment, the setting of preferred described response behaviour proofing unit on tubular reactor is distributed as after educt flow is dredged to going forward close.
In above-mentioned production equipment, preferred described response behaviour proofing unit is polar voltages Controlling System or potential measurement Controlling System.Polar voltages Controlling System and potential measurement Controlling System are respectively by the voltage detected and current potential determination response behaviour.Reaction mass occurs that the detection method that batching is abnormal is: when the current potential of response behaviour proofing unit or voltage readings do not reach reaction end reading, and compared with the current potential of the current potential of this response behaviour proofing unit or voltage readings and last response behaviour proofing unit or voltage readings, numerical value change is less than the value of setting, be then defined as reaction mass and occur that batching is abnormal.
In above-mentioned production equipment, the electrode materials of preferred described polar voltages Controlling System or potential measurement Controlling System is be selected from Au, Pt, Ag, Sb, Mo, Cr, the one of graphite or its alloy.
Above-mentioned production equipment is preferably the automatic control continuous production device of azoic dyestuff, comprise coupled reaction part, described coupled reaction part comprise tubular type coupling reactor and be arranged on described tubular type coupling reactor as described in the potential measurement Controlling System of response behaviour proofing unit.
In above-mentioned production equipment, preferred described coupled reaction part comprises: raw material feed device, measuring apparatus, batching kettle, tubular type coupling reactor, the potential measurement Controlling System be arranged on tubular type coupling reactor, refrigerating unit, device for monitoring temperature, transfer still, turn brilliant still and pressure filter, when described dyestuff controls continuous production device operation automatically, operational process comprises:
Diazo solution and coupling component solution to be supplied in batching kettle continuously according to the ratio specified by measuring apparatus and to prepare burden;
Material in batching kettle is overflowed by overflow port, flow in tubular type coupling reactor and carries out coupled reaction;
Coupled reaction material detects through potential measurement Controlling System, if reacted, then flow to transfer still; If reaction not yet completes, and reaction mass does not occur that batching is abnormal, then reaction mass enters downstream tubular type coupling reactor and proceeds reaction; If reaction not yet completes, and occur that batching is abnormal, then reaction mass being back to batching kettle, again preparing burden by regulating each measuring apparatus; Coupled reaction material in transfer still proceeds in brilliant still and carries out turning brilliant; Turn the material after crystalline substance to be fed into pressure filter and to carry out press filtration, washing.
In above-mentioned production equipment, preferably to the measuring apparatus of coupling reactive moieties, refrigerating unit, device for monitoring temperature carries out coordinated signals, thus operationally the flow of heat-eliminating medium in the flow of raw material feed device Raw material diazo solution and coupling component solution and refrigerating unit and temperature of reaction are carried out interlocked control, control process comprises set temperature upper lower limit value, when temperature of reaction is higher than higher limit, turn or close each feed product flow in proportion down, tune up the flow of heat-eliminating medium simultaneously, when temperature of reaction is lower than lower value, then turn the flow of heat-eliminating medium down, until temperature of reaction is within the scope of bound.
Above-mentioned production equipment preferably also comprises diazotization reaction part, and described diazotization reaction part comprises tubular type diazotization reaction device and is arranged on the polar voltages Controlling System as response behaviour proofing unit on described tubular type diazotization reaction device.
In above-mentioned production equipment, described diazotization reaction part preferably includes raw material feed device, measuring apparatus, batching kettle, tubular type diazotization reaction device, polar voltages Controlling System, refrigerating unit, device for monitoring temperature, the transfer still be arranged on tubular type diazotization reaction device, when described dyestuff controls continuous production device operation automatically, the operational process of diazotization reaction part comprises:
Diazo component, nitrosyl sulfuric acid and optional acid are prepared burden to batching kettle by the ratio continuously feeding of measuring apparatus according to regulation; Streams in batching kettle carries out diazotization reaction to tubular type diazotization reaction device;
Diazotization reaction material detects through polar voltages Controlling System, if reacted, then flow to transfer still; If reaction not yet completes, and reaction mass does not occur that batching is abnormal, then reaction mass enters downstream tubular type diazotization reaction device and proceeds reaction; If reaction not yet completes, and the voltage readings stating polar voltages Controlling System is compared with the last voltage readings stating polar voltages Controlling System, numerical value change is less than the value of setting, then reaction mass is back to batching kettle, again prepares burden by regulating each measuring apparatus;
Diazo solution is wherein supplied to follow-up coupled reaction as one of the raw material feed device of coupled reaction by transfer still.
In above-mentioned production equipment, preferably to the measuring apparatus of diazotization reaction part, refrigerating unit, device for monitoring temperature carries out coordinated signals, thus operationally by raw material feed device Raw material diazo component, in the flow of nitrosyl sulfuric acid and optional acid and refrigerating unit, the flow of heat-eliminating medium and temperature of reaction carry out interlocked control, control process comprises set temperature upper lower limit value, when temperature of reaction is higher than higher limit, turn or close each feed product flow in proportion down, tune up the flow of heat-eliminating medium simultaneously, when temperature of reaction is lower than lower value, then turn the flow of heat-eliminating medium down, until temperature of reaction is within the scope of bound.
In above-mentioned production equipment, 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 above-mentioned production equipment, preferred described batching kettle is provided with overflow port, and the material in batching kettle is overflowed by overflow port.Preferred described overflow port place is provided with vibration filters, and the filtering net aperture of described vibration filters is 5 ~ 40 orders.The filtering net material of preferred described vibration filters is be selected from any one in titanium, stainless steel, glass fibre, Carbon fibe, fluoroplastics.
Described in above-mentioned production equipment, tubular reactor material preferably 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.
Automatically controlled by DCS Controlling System in preferred above-mentioned production equipment.
Dyestuff of the present invention automatically controls continuous production method and device is controlled by automatic, in time the reaction solution reacted is transferred to subsequent processing, and batching is occurred that the abnormal timely blowback of material is prepared burden again to batching kettle, achieve and accurately automatically control serialization DYE PRODUCTION, ensure that the stable of quality product, shorten the production time, improve production efficiency, reduce production cost, decrease the generation of the three wastes, reach the effect of low dirty low consumption, achieve recycling industries and clean production.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that azoic dyestuff of the present invention controls continuous production method automatically.
Fig. 2, Fig. 3 are the schematic diagram that azoic dyestuff of the present invention controls continuous production device automatically.
In figure, A1, A2 are batching kettle; J1, J2 are scale tank; M is cage device; P1 is solid metering device; P2, P3, P4, P5, P6, P7, P8 are pump or volume pump; H1, H2 are vibration filters; K1, K2 ... K6 be polar voltages Controlling System, K ' 1, K ' 2 ... K ' 6 is potential measurement Controlling System; F is valve; D1, D2 are transfer still; G1 is tubular type diazotization reaction device, and G2 is tubular type coupling reactor; X is coupling component solution; Y is for turning brilliant still.
Embodiment
Referring to accompanying drawing, the present invention is further described.
Fig. 2, Fig. 3 shown device carries out Automated condtrol by DCS Controlling System.
In fig. 2, to diazotization reaction dispenser P1, P2 and P3, refrigerating unit (cooling jacket of batching kettle A1 and tubular reactor G1 and the interior shell-and tube condenser of pipe, not shown), device for monitoring temperature (not shown) carries out coordinated signals, by diazo component, in the flow of nitrosyl sulfuric acid and optional acid and refrigerating unit, the flow of heat-eliminating medium and temperature of reaction carry out interlocked control, when temperature of reaction is higher than set higher limit, turn or close each feed product flow in proportion down, tune up the flow of heat-eliminating medium simultaneously, when temperature of reaction is lower than set lower value, then turn the flow of heat-eliminating medium down, until temperature of reaction is within the scope of bound.
In figure 3, to coupling reaction raw materials measuring apparatus P5 and P6, refrigerating unit (cooling jacket of batching kettle A2 and tubular reactor G2 and the interior shell-and tube condenser of pipe, not shown), device for monitoring temperature (not shown) carries out coordinated signals, the flow of heat-eliminating medium in the flow of diazo solution and coupling component solution and refrigerating unit and temperature of reaction are carried out interlocked control, when temperature of reaction is higher than set higher limit, turn or close each feed product flow in proportion down, tune up the flow of heat-eliminating medium simultaneously, when temperature of reaction is lower than set lower value, then turn the flow of heat-eliminating medium down, until temperature of reaction is within the scope of bound.
With reference to figure 2, in batching kettle A1, diazo component cage M carries out continuously feeding by solid metering device P1, and nitrosyl sulfuric acid and optional acid are by volume pump P2, P3 continuously feeding, and the mol ratio of diazo component, nitrosyl sulfuric acid, optional acid is 1:1.0 ~ 1.1:0 ~ 8.
The material overflowed in batching kettle A1, flow in tubular type diazotization reaction device G1, controls doazo reaction temperature at-10 DEG C ~ 30 DEG C.Temperature in described diazotization reaction device G1 is controlled by this dual-cooled device of shell-and tube condenser in cooling jacket and pipe, tubular type diazotization reaction device is equipped with more than 2 polar voltages Controlling System K1, K2 ...
Diazotization reaction material, after polar voltages Controlling System detection reaction completes, flow in transfer still D1; If reaction not yet completes, and reaction mass does not occur that batching is abnormal, then reaction mass enters downstream tubular type diazotization reaction device G1 and proceeds reaction; If reaction not yet completes, and the voltage readings of 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, then pass through pump P4 by reaction mass blowback to batching kettle A1, adjustment solid metering device P1, volume pump P2, P3 prepare burden again.
With reference to figure 3, diazo solution in transfer still D1 and coupling component solution are that 1:0.95 ~ 1.05 continuous pump is prepared burden to batching kettle A2 by volume pump P5, P6 according to the mol ratio of diazonium compound and coupling component, in batching kettle, material is flow in tubular type coupling reactor G2 by overflow port and carries out coupled reaction, and controlling coupled reaction temperature is-10 DEG C ~ 20 DEG C;
Coupled reaction material, after potential measurement Controlling System detection reaction completes, flow in transfer still D2; If reaction not yet completes, and reaction mass does not occur that batching is abnormal, then reaction mass enters downstream tubular type coupling reactor G2 and proceeds reaction; If reaction not yet completes, and the potential readings of potential measurement Controlling System is compared with the potential readings of last potential measurement Controlling System, numerical value change is less than the value of setting, then by pump P7, reaction mass is back to batching kettle A2, again prepares burden by regulating the flow of volume pump P5, P6.
Coupled reaction material in transfer still D2 proceeds in brilliant still Y through pump P8 and carries out turning brilliant, and controlling to turn brilliant temperature is 40 DEG C ~ 70 DEG C.
Turn the material after crystalline substance and enter pressure filter press filtration, washing, obtains dyestuff filter-cakes.Filter cake mother liquid coming, washing water are carried out categorised collection, is configured to liquid of pulling an oar, for the making beating of coupling component to prepare coupling component solution.The mass percent controlling acid in making beating liquid is 2% ~ 15%.
Embodiment
Embodiment 1
In coupling component making beating pot, drop into 1980kg N, N-diethyl-3-acetylaminoaniline, pulls an oar with the making beating liquid that 20000kg sulfuric acid mass percent is 3%, obtains coupling component solution X, stand-by.
The nitrosyl sulfuric acid (mass percentage is 28%) of 420kg is added in batching kettle A1, open chilled brine, control temperature in the kettle at 20 DEG C ~ 30 DEG C, slowly twist into 2, 4-dinitrobenzene-6-chloroaniline (diazo component) 200kg carries out mixing and is made into initiator, open 2, 4-dinitrobenzene-6-chloroaniline (diazo component), nitrosyl sulfuric acid material inlet valve, the two controls input speed respectively by measuring apparatus is 571kg/h, 1200kg/h carries out Automatic continuous charging, mixture flow to tubular reactor G1 from overflow port and reacts, after polar voltages Controlling System detection reaction completes, reaction mass (diazo solution) flow to transfer still D1.
In transfer still D1 2, compound solution after 4-dinitrobenzene-6-chloroaniline diazotization and N, N-diethyl-3-acetylaminoaniline coupling component solution X is continuously pumped into batching kettle A2 with the flow of 1771kg/h and 5770kg/h respectively by volume pump P5, P6 and prepares burden, control 2, the diazonium compound of 4-dinitrobenzene-6-chloroaniline and the mol ratio of N, N-diethyl-3-acetylaminoaniline coupling component are 1:1.04.
Material in batching kettle A2 flow in tubular type coupling reactor G2 through overflow port and reacts, and temperature controls at 0 ± 2 DEG C.
Coupling material is after potential measurement Controlling System detection reaction completes, and reaction mass flow to transfer still D2.
Material in transfer still D2, goes to brilliant still Y through pump P8, controls to turn brilliant temperature 50 ± 2 DEG C.Turn brilliant rear material and enter pressure filter, through press filtration, washing, obtain 63 DISPERSE Violet 63 93:1 dyestuff filter-cakes.Yield is 95%, and purity is 90%, and filter cake intensity is 520%.Filter cake mother liquid coming, washing water respectively pump, to mother liquid coming, washing water storage tank, after mother liquid coming, washing mixing regulate the mass percent of acid, are mixed with making beating liquid and carry out recycled.
The method and apparatus of above-mentioned continuous seepage dyestuff is adopted to prepare 63 DISPERSE Violet 63 93:1 dyestuff filter-cakes, achieve multiple spot and accurately automatically control continuous seepage, compared with intermittent reaction, dyestuff yield improves about 3.2%, filter cake purity improves about 2.8%, filter cake intensity improves about 4%, and cost of labor have dropped about 35%.
Embodiment 2:
In coupling component making beating pot, drop into the N of 700kg, N-diethyl-3-acetylaminoaniline, pulls an oar with the making beating liquid that 15000kg sulfuric acid mass percent is 4.5%, obtains coupling component solution X, stand-by.The nitrosyl sulfuric acid (mass percentage is 28%) of 380kg is added in batching kettle A1, the sulfuric acid of 660kg, open chilled brine, control temperature in the kettle at 0 DEG C ~ 5 DEG C, slow strand is carried out mixing into 2 cyano 4 nitro 6 bromo aniline 200kg and is 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 Automatic continuous charging, mixture flow to tubular reactor G1 from overflow port and reacts, after polar voltages Controlling System detection reaction completes, reaction mass (diazo solution) flow to transfer still D1.When reaction mass detects through polar voltages Controlling System, reading display do not reach reaction end and two adjacent polar voltages Controlling System reading changes are less than the value of setting time, then close pump P1, P2, P3, open pump P4, by reaction mass blowback batching kettle A1, and by regulating pump P1, P2, P3 again to prepare burden.Recover normally, close pump P4, open pump P1, P2, P3, return to normal production.
Compound solution after 2 cyano 4 nitro 6 bromo aniline diazotization in transfer still D1 and N, N-diethyl-3-acetylaminoaniline coupling component solution X is continuously pumped in batching kettle A2 with the flow of 1860kg/h and 6262kg/h respectively by volume pump P5, P6 and prepares burden, the mol ratio controlling the compound after 2 cyano 4 nitro 6 bromo aniline diazotization and N, N-diethyl-3-acetylaminoaniline coupling component is 1:1.02.
Material in batching kettle A2 flow in tubular type coupling reactor G2 through overflow port and reacts, and temperature controls at 8 ± 2 DEG C.Coupled reaction material is after potential measurement Controlling System detection reaction completes, and reaction mass flow to transfer still D2.Coupled reaction material in transfer still D2 goes to brilliant still Y through pump P8, controls to turn brilliant temperature 60 ± 2 DEG C.Turn brilliant rear material and enter pressure filter, through press filtration, washing, obtain EX-SF DISPERSE BLUE EX-SF 300 183:1 dyestuff filter-cakes.Filter cake mother liquid coming, washing water respectively pump, to mother liquid coming, washing water storage tank, are applied mechanically through regulating the mass percent Posterior circle of acid.
Adopt the method and apparatus of above-mentioned continuous seepage dyestuff to prepare EX-SF DISPERSE BLUE EX-SF 300 183:1 dyestuff filter-cakes, achieve multiple spot and accurately automatically control, the production cycle is 12 hours, and Qualified Products Rate is 100%.Compared with general continuous production technology, the production cycle of this dyestuff shortens 15%.
Embodiment 3:
The 3-(N of 2050kg is put into, N-diallyl in coupling component making beating pot) amino-4-methoxyacetanilide, pull an oar with the making beating liquid that 20000kg sulfuric acid mass percent is 6%, obtain coupling component solution X, stand-by.
The nitrosyl sulfuric acid (mass percentage is 28%) of 690kg is added in batching kettle A1, open chilled brine, control temperature in the kettle at 20 DEG C ~ 30 DEG C, slowly twist into 2, 4-dinitrobenzene-6-bromaniline 330kg carries out being 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 G1 from overflow port and reacts, after polar voltages Controlling System detection reaction completes, diazo solution flow to transfer still D1, through volume pump P5 pump to batching kettle A2.
In transfer still D1 2, compound solution after 4-dinitrobenzene-6-bromaniline diazotization and 3-(N, N-diallyl) amino-4-methoxyacetanilide coupling component solution X is continuously pumped into batching kettle A2 with the flow of 1530kg/h and 6615kg/h respectively, and the mol ratio controlling diazonium compound and coupling component is 1:1.04.
Material in batching kettle A2 flow in tubular reactor G2 through overflow port and reacts, and temperature controls at 0 ± 2 DEG C.Coupled reaction streams is after potential measurement Controlling System detection reaction completes, and streams is to transfer still D2; When coupled reaction material detects through potentiometric detection Controlling System, reading display do not reach reaction end and two adjacent potentiometric detection Controlling System reading changes are less than the value of setting time, then close pump P5, P6, open pump P7, coupled reaction product pump being back to batching kettle A2, again preparing burden by regulating P5, P6.Recover normally, close pump P7, open pump P5, P6, return to normal production.
The streams that coupled reaction completes, in transfer still D2, goes to brilliant still Y through pump P8, controls to turn brilliant temperature 50 ± 2 DEG C.Turn brilliant rear material and enter pressure filter, through press filtration, washing, obtain EX-SF DISPERSE BLUE EX-SF 300 291:1 dyestuff filter-cakes.Filter cake mother liquid coming, washing water respectively pump, to mother liquid coming, washing water storage tank, carry out recycled after regulating the mass percent of acid.
Adopt the method and apparatus of above-mentioned continuous seepage dyestuff to prepare EX-SF DISPERSE BLUE EX-SF 300 291:1 dyestuff filter-cakes, achieve multiple spot and accurately automatically control, the qualification rate of quality product is 100%.Compared with general continuous production technology, the production cycle of this dyestuff shortens 20%, and energy consumption declines to a great extent, and reduces production cost.
Claims (19)
1. a dyestuff controls continuous production method automatically, described method comprises carries out reaction and continuous discharge by reaction raw materials according to the ratio continuous feeding of regulation to tubular reactor, it is characterized in that, tubular reactor arranges multiple response behaviour proofing unit, when reaction mass is through response behaviour proofing unit, response behaviour proofing unit detects response behaviour, if determine that reaction completes after testing, then reaction mass is gone to subsequent processing; If determine that reaction not yet completes after testing, then reaction mass enters downstream tubular reactor and proceeds reaction.
2. dyestuff as claimed in claim 1 controls continuous production method automatically, and it is characterized in that, described response behaviour proofing unit is arranged on the reaction end near zone on tubular reactor.
3. dyestuff as claimed in claim 1 or 2 controls continuous production method automatically, it is characterized in that, the setting of described response behaviour proofing unit on tubular reactor is distributed as after educt flow is dredged to going forward close.
4. dyestuff as claimed in claim 1 or 2 controls continuous production method automatically, it is characterized in that described response behaviour proofing unit setting space be in reactor reaction mass flowing 10min ~ 30min the distance of process.
5. dyestuff as claimed in claim 1 or 2 controls continuous production method automatically, it is characterized in that, described response behaviour proofing unit is polar voltages Controlling System or potential measurement Controlling System, and polar voltages Controlling System and potential measurement Controlling System are respectively by the voltage detected and current potential determination response behaviour.
6. dyestuff as claimed in claim 5 controls continuous production method automatically, it is characterized in that, the electrode materials of described polar voltages Controlling System or potential measurement Controlling System is be selected from Au, Pt, Ag, Sb, Mo, Cr, the one of graphite or its alloy.
7. the dyestuff as described in claim 1,2 or 6 controls continuous production method automatically, it is characterized in that, be the automatic control continuous production method of azoic dyestuff, comprise coupled reaction step, coupled reaction is monitored by the multiple potential measurement Controlling System be arranged on tubular type coupling reactor.
8. dyestuff as claimed in claim 7 controls continuous production method automatically, and it is characterized in that, described method also comprises diazotization reaction step, and diazotization reaction is monitored by multiple polar voltages Controlling System.
9. dyestuff as claimed in claim 8 controls continuous production method automatically, and 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.
10. the dyestuff described in claim 7 or 8 controls continuous production method automatically, and it is controlled automatically by DCS Controlling System.
11. 1 kinds of dyestuffs control continuous production device automatically, it is characterized in that comprising raw material feed device, measuring apparatus, tubular reactor, multiple response behaviour proofing units that tubular reactor is arranged, when described dyestuff controls continuous production device operation automatically, operational process comprises: reaction raw materials carries out reaction and continuous discharge according to the ratio continuous feeding of regulation to tubular reactor, wherein when reaction mass is through response behaviour proofing unit, response behaviour proofing unit detects response behaviour, if determine that reaction completes after testing, then reaction mass is gone to subsequent processing, if determine that reaction not yet completes after testing, then reaction mass enters downstream tubular reactor and proceeds reaction.
12. dyestuffs as claimed in claim 11 control continuous production device automatically, and it is characterized in that, described response behaviour proofing unit is arranged on the reaction end near zone on tubular reactor.
13. dyestuffs as described in claim 11 or 12 control continuous production device automatically, it is characterized in that, the setting of described response behaviour proofing unit on tubular reactor is distributed as after educt flow is dredged to going forward close.
14. dyestuffs as described in claim 11 or 12 control continuous production device automatically, and it is characterized in that, described response behaviour proofing unit is polar voltages Controlling System or potential measurement Controlling System.
15. dyestuffs as claimed in claim 14 control continuous production device automatically, it is characterized in that, the electrode materials of described polar voltages Controlling System or potential measurement Controlling System is be selected from Au, Pt, Ag, Sb, Mo, Cr, the one of graphite or its alloy.
16. dyestuffs as described in claim 11 or 12 control continuous production device automatically, it is the automatic control continuous production device of azoic dyestuff, comprise coupled reaction part, described coupled reaction part comprises tubular type coupling reactor and is arranged on the potential measurement Controlling System as response behaviour proofing unit on described tubular type coupling reactor.
17. dyestuffs as claimed in claim 16 control continuous production device automatically, also comprise diazotization reaction part, described diazotization reaction part comprises tubular type diazotization reaction device and is arranged on the polar voltages Controlling System as response behaviour proofing unit on described tubular type diazotization reaction device.
18. dyestuffs as described in claim 11,12,15 or 17 control continuous production device automatically, and 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.
19. dyestuffs as described in claim 11,12,15 or 17 control 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 |
| CN110128845A (en) * | 2019-04-30 | 2019-08-16 | 江苏彩瑞实业有限公司 | A kind of technical process producing high light-fast fastness, high durable fastness pigment yellow 74 |
| CN110041725A (en) * | 2019-04-30 | 2019-07-23 | 江苏彩瑞实业有限公司 | A kind of technical process producing high light-fast fastness, high durable fastness pigment red 146 |
| CN110845860A (en) * | 2019-11-20 | 2020-02-28 | 浙江工业大学 | Production process and synthesis system for automatic continuous liquid azo dye |
| CN114160066A (en) * | 2021-12-03 | 2022-03-11 | 启东亚太药业有限公司 | Equipment and method for producing diazotized phenylhydrazine hydrochloride based on microreactor |
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| CN203269845U (en) * | 2013-03-12 | 2013-11-06 | 浙江迪邦化工有限公司 | Automatic-control continuous dye production device |
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| US6346361B1 (en) * | 1999-10-06 | 2002-02-12 | Clariant Finance (Bvi) Limited | Method for synthesizing polymeric AZO dyes |
| WO2001059013A1 (en) * | 2000-02-09 | 2001-08-16 | Clariant International Ltd | Method for production of azo dyes in microreactors |
| CN100999446B (en) * | 2007-01-15 | 2010-05-26 | 浙江寿尔福化学有限公司 | Production method of m-bromophonol and production device thereof |
| DE102009012685A1 (en) * | 2009-03-11 | 2010-09-16 | Clariant International Limited | C.I. Pigment Red 112 with improved dispersibility |
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| US4246171A (en) * | 1978-09-07 | 1981-01-20 | Ciba-Geigy Corporation | Continuous diazotization process, wherein the rate of addition of inorganic nitrite is automatically controlled by polarovoltric means |
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| CN103160145B (en) | 2014-01-22 |
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