CN104830089B - Dye continuous coupling method with reduced energy consumption - Google Patents
Dye continuous coupling method with reduced energy consumption Download PDFInfo
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- CN104830089B CN104830089B CN201510210678.7A CN201510210678A CN104830089B CN 104830089 B CN104830089 B CN 104830089B CN 201510210678 A CN201510210678 A CN 201510210678A CN 104830089 B CN104830089 B CN 104830089B
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Abstract
The invention relates to a dye continuous coupling method with reduced energy consumption. The method comprises the following steps: mixing a coupling component, water and aids together, pulping to obtain a coupling liquid, continuously pumping the obtained coupling liquid into a coupling reactor through a metering device; at the same time, continuously pumping a diazo salt solution into a multi-stage coupling reactor in batches through a metering device, controlling the mole ratio of diazo salt to the coupling component in a range of 1:0.95-1.05; adjusting the cooling medium flow by the affiliated heat-exchange device of the coupling reactor to control the coupling temperature in a range of -10 to 30 DEG C, carrying out coupling reactions under stirring, after the reaction, pouring out the reaction products, and carrying out a post treatment. The provided method achieves continuous coupling production, the coupling is performed in multiple stages, the production efficiency, product yield and production quality are all improved, furthermore, a tower type reactor is adopted, the reaction fluid is guided by the gravity, and thus the energy consumption during the stirring process is reduced.
Description
Technical field
The present invention relates to a kind of chemical industry continuous automatic production technology, more particularly, to a kind of Dyestuff synthesis in continuous idol
The method closed and reduce energy consumption.
Background technology
The dye species of dye industry more than 60% are all azo-type structures, and diazotising, coupling are to synthesize such type dye institute
Required step, can discharge substantial amounts of heat in diazo reaction, coupling reaction, because the rising of temperature can cause dividing for material
Solution, so as to affect product quality and yield, it is therefore desirable to which carrying out cooling could meet production requirement.
During DYE PRODUCTION, because the stability of diazol component is relatively low, certain acidity and relatively low temperature is needed
Under carry out.There is the side reactions such as decomposition while coupling reaction is carried out, practice have shown that with the rising of temperature, side reaction adds
It is acute.And coupled processes are an exothermic reactions, in order to reduce the decomposition of diazol, often using the method for low temperature.Such knot
Fruit is to need substantial amounts of energy consumption for cooling.The opposing party, low temperature reduces the speed of coupling reaction, makes the time lengthening for completing to react,
Consersion unit is set to become big.
At present in actual production process, coupling reaction generally adopts batch production process, and the volume of reactor is huger, stirs
Mix and preferable mass-and heat-transfer effect is unable to reach when device is stirred to material, the local temperature of system is too high, and diazol is in idol
Unstable in zoarium system, easily there is side reaction in coupled processes, the yield and purity of product is impacted, also, big volume reactor
Surface area is big, and cold consumption is larger.The couple temperature of most of dye species need to be controlled at 0 DEG C or so, be controlling reaction temperature,
Substantial amounts of ice cube is must be added to, also causes wastewater flow rate big.One side dye coupling process thermal discharge is big, and needs are passed through a large amount of coolings
Medium cooling.
A kind of dyestuff continuously coupling and reduction energy consuming process are proposed for problem CN 102796394 A, group will be coupled
Divide, water and auxiliary agent mixing are beaten, the coupling solution for obtaining is continuously pumped in coupling reaction kettle by metering device, meanwhile, diazol
Solution is continuously pumped in coupling reaction kettle by metering device, control charging diazol：The mol ratio of coupling component is 1：0.
95-1.05, by the attached heat-exchanger rig of coupling reaction kettle, adjusts cooling medium consumption and controls couple temperature for -10 DEG C ~ 20 DEG C,
Coupling reaction is carried out under agitation, and coupling reaction to discharge and turn brilliant pot into heat Jing after heat exchange.The reactor of coupling reaction is 2,4
Order reaction kettle, upper level reactor discharges overflow to next stage reactor, and the discharging of afterbody reactor carries out again heat exchange behaviour
Make.Due to feeding diazol：The mol ratio of coupling component is 1：0. 95-1.05 mixes, and there is diazonium group in reactor all the time
Point, to prevent diazol from decomposing, make reaction temperature to control at low temperature, to make the time lengthening for completing to react, set reaction
It is standby to become big.Because the dye precipitated generated in course of reaction is separated out, multi-floating bodies have blocking risk and dynamic equipment in material transfer
The risk for breaking down more.
Same CN201310078687.6；The patents such as CN201310079181.7 are realized continuously using pipeline reactor
Change.Also due to charging diazol：The mol ratio of coupling component is 1：0. 95-1.05 mixes, and there is diazonium in reactor all the time
Component, to prevent diazol from decomposing, makes reaction temperature to control at low temperature, to make the time lengthening for completing to react, and makes reaction
Pipeline is very long and impracticable.Card and line clogging equivalent risk be difficult to ensure and there is reaction time in pipe reaction.
Based on this, the present invention is proposed.
The content of the invention
For the big problem of coupled processes low production efficiency, freezing energy consumption in prior art, it is an object of the invention to provide
A kind of continuous coupling production and the method for reducing energy consumption, coupling component suspension and diazo liquid is in batches continuous by metering device
Pump in coupling reaction kettle, adjust cooling water flow and control couple temperature for -10 DEG C～30 DEG C, segmentation coupling is carried out under agitation
Reaction, has excessive coupling component, it is ensured that the fast reaction of diazol energy is consumed, so as to appropriate high in first order coupling kettle
At a temperature of carry out, reduce chilled water requirement and energy-conservation.Diazol is added in the second level and later coupling reaction kettle and reduce anti-
Reaction is completed at a temperature of answering.Using tower reactor, gravity water conservancy diversion reactant liquor, so as to save the power consumptions such as stirring.
To reach above-mentioned purpose, the present invention is achieved by the following technical solutions：
A kind of method that dyestuff is continuously coupled and reduces energy consumption, comprises the following steps：By the mixing of coupling component, water and auxiliary agent
Beating, the coupling solution for obtaining is continuously pumped in coupling reaction kettle by metering device, meanwhile, diazonium salt solution is by measuring dress
Put, be continuously pumped in batches in multistage coupling reaction kettle, control charging diazol：The mol ratio of coupling component is 1:0.95-1.05；
By the attached heat-exchanger rig of coupling reaction kettle, adjust cooling medium consumption and control couple temperature for -10 DEG C -30 DEG C,
Coupling reaction is carried out under agitation, and discharging after coupling reaction terminates carries out follow-up processing.
In first order coupling reaction kettle control charging diazol：The mol ratio of coupling component is 1：0.05-0.8, by idol
The attached heat-exchanger rig of reactor is closed, cooling medium consumption in heat-exchanger rig is adjusted and is controlled couple temperature for 0 DEG C -30 DEG C；Second
Level and later coupling reaction kettle add diazol 0.02-0.95, by the attached heat-exchanger rig of coupling reaction kettle, adjust heat-exchanger rig
Interior cooling medium consumption controls couple temperature for -10 DEG C -20 DEG C, and coupling reaction is carried out under agitation.Coupling reaction goes out after terminating
Material carries out follow-up processing.
In the first order coupling reaction coupling component excessive 20% and more than, coupling reaction temperature it is higher than the second level 8 DEG C with
On, with 0 DEG C and the low temperature water cooling of the above.
The coupling reaction kettle is tower multi-stage reacting kettle, and upper level reactor discharges nature downstream to next order reaction
Kettle.
The coupling reaction kettle is tower 2-20 order reactions kettle.
The coupling reaction kettle is tower 3-15 order reactions kettle.
Tower tray in the tower reactor is the difunctional plate of water conservancy diversion heat exchange.
The beneficial effects are mainly as follows following several respects：
1st, while realizing serialization coupling production, segmentation coupling is realized, improves production efficiency, product yield and product
Product quality；
2nd, segmentation coupling causes coupling reaction to reach as high as 80% coupling reaction heat, exchanges heat under conditions of relatively relaxing, section
About cold energy；
3rd, coupling reaction is carried out in tower.Tower can be arbitrarily distinguished as multiple reaction zones, and can arbitrarily control difference
The reaction temperature of reaction zone；
4th, the multiple reaction zones in reaction tower, can react the reaction zone of autoclave, or be made up of multiple baffle plates
Runner, so as to reduce the power consumption of stirring；
5th, react in same tower, material flows from top to bottom, reduces and turn material process, can effectively prevent because dyestuff is separated out
And the blockage problem for occurring；
6th, the tower tray between at different levels in reaction tower can be compound with heat exchanger plates so as to exchanges heat bifunctional tower with water conservancy diversion
Disk, saves space, reduces cost.
Description of the drawings
Fig. 1 is present invention process flow chart.
Specific embodiment
With reference to specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to
This.
Dyestuff of the present invention is continuously coupled and reduces energy consuming process, comprises the steps：By the mixing of coupling component, water and auxiliary agent
Beating, the coupling solution for obtaining is continuously pumped in tower reactor by metering device, meanwhile, diazonium salt solution is by measuring dress
Put, be continuously pumped in coupling reaction kettle, in the first reactor control charging diazol：The mol ratio of coupling component is 0.05-
0.8：1, it is ensured that have enough coupling components, by the attached heat-exchanger rig of coupling reaction kettle, adjust cooling medium in heat-exchanger rig
Flow-control couple temperature is 0 DEG C -30 DEG C（Higher temperature）.Diazol 0.02-0.95 is added in the second section of tower, by coupling
The attached heat-exchanger rig of reactor, adjusts cooling medium consumption in heat-exchanger rig and controls couple temperature for -10 DEG C -20 DEG C, in stirring
Under carry out coupling reaction.Follow-up processing is carried out after coupling reaction discharging.
The inventive method it is critical only that control diazol：The different mol ratio of coupling component, makes diazol component first
Quickly it is exhausted in reactor, carries out under conditions of both coupling reaction temperature is slightly higher in the first reactor, realizes energy-conservation energy
Amount, improves reaction rate, reduces the purpose of consersion unit.
Further, dyestuff of the invention is continuously coupled and reduces energy consumption technique, and the series of coupling reaction kettle can be according to reality
Production requirement sets, and coupling reaction kettle can be 20 order reaction kettles, and preferred 3-15 levels, upper level reactor discharges overflow to next stage
Reactor, afterbody reactor discharging carries out again heat exchange operation.Coupling component in the coupling solution and diazo liquid of control addition
It is l with the total moles ratio of folding hundred of diazol：0. 95-1.05, coupling solution disposably adds one-level coupling reaction kettle, diazo liquid to need
Add step by step in reactors at different levels, wherein the first reactor adds diazol：Coupling component is 0.03-0.8：1, it is ensured that coupling
Component has larger excess, and controlling reaction temperature is higher, diazol is quickly run out of, and subsequent reactions kettle adds diazonium
Salt, controls relatively low reaction temperature, prevents diazol from decomposing and makes overall reaction complete.Can also be by diazol in reactors at different levels
In add step by step, control the temperature of each reactor according to the reaction Expenditure Levels of diazol, reach the purpose of energy-conservation.
Further, dyestuff of the present invention is continuously coupled and reduces energy consumption technique, and the series of coupling reaction kettle can basis
Actual production demand sets, and the coupling reaction kettle is tower reactor, identical with the kettle of autoclave first in the first segment of tower, is added
Diazol：Coupling component is 0.03-0.8：1, it is ensured that coupling component has larger excess, controlling reaction temperature is higher.In tower
Two sections and later diazols of adding at different levels make overall reaction complete.In reaction tower it is at different levels between tower tray can be common deflector
Can also be that water conservancy diversion exchanges heat bifunctional division board, preferably water conservancy diversion exchanges heat bifunctional division board.
Further, dyestuff of the present invention is continuously coupled and reduces energy consumption technique, and the series of coupling reaction kettle can basis
Actual production demand sets, and the coupling reaction kettle is tower reactor, and the multiple reaction zones in reaction tower can be reactor
The reaction zone of formula, or the runner being made up of multiple baffle plates, so as to reduce the power consumption of stirring.
Embodiment l
L is such as schemed, by the 3- acetylaminohydroxyphenylarsonic acid N of hundred 926kg of folding, N- diethylanilines, the washing of 10500L Jing heat exchangers cooling
Water, the auxiliary agent TX-10 of 5kg are beaten, and obtain 8.1% coupling component beating liquid.
Above-mentioned beating liquid is continuously pumped in tower first segment reactor, while with 1106kg/h with the flow of 3352kg/h
Flow to first segment be coupled kettle in squeeze into 30% 2,4- dinitro -6- bromaniline sulphuric acid diazols, control first segment coupling kettle
Reaction temperature 10-15 DEG C, carries out under agitation coupling reaction.First segment coupling reaction discharges overflow to two grades of coupling kettles, while
2, the 4- dinitro -6- bromaniline sulphuric acid diazol of squeezing into 30%, control the are coupled in kettle with the flow of 474kg/h to second section
Two section coupling kettle reaction temperatures 0-5 DEG C, carry out under agitation coupling reaction, down flow through naturally after reaction anti-after n=5 layer column plates
Should complete, discharging enters next process.
Jing is exchanged heat, is turned the normal process steps such as crystalline substance, filter pressing, washing after coupling terminates, and obtains the dyestuff filter-cakes of C.I. disperse violet 93.
Using the above-mentioned dyestuff dyestuff filter-cakes of C.I. disperse violet 93 that continuously coupling and energy utilization technique are obtained, dye is realized
The continuous coupling of material, improves dyestuff quality. and relative to interval coupling process, dyestuff yield improves about 1.5%, and filter cake intensity is carried
It is high by about 2.8%.Realizing the saving that energy consumption is freezed in coupling production process, 70% coupling reaction heat instead of with 5 DEG C of water at low temperature-
10 DEG C of chilled waters, have saved freezing energy consumption.
Embodiment 2：061#, diazonium, coupling solution are disposably added, yield 98%
Such as Fig. 1, will hundred 740kg of folding N- ethyl-N-cyanoethyl anilines, 11500L Jing heat exchangers, the washings of cooling,
The auxiliary agent TX-10 of 5kg is beaten, and obtains 6% coupling component beating liquid.
Above-mentioned beating liquid is continuously pumped into the flow of 3140kg/h and is pumped in tower first segment reactor, while with
The flow of 424kg/h squeezes into the 30% bromo- 4- nitroanilines sulphuric acid diazols of 2,6- bis-, control first segment coupling in coupling kettle
Kettle reaction temperature 14-18 DEG C, carries out under agitation coupling reaction.First segment coupling reaction discharges overflow to two grades of coupling kettles, together
When with the flow of 988kg/h to second section be coupled kettle in squeeze into 30% 2,4- dinitro -6- bromaniline sulphuric acid diazols, control
Second section is coupled kettle reaction temperature 0-5 DEG C, and coupling reaction is carried out under agitation, down flows through naturally after n=12 layer column plates after reaction
Reaction is completed, and discharging enters next process.
Jing is exchanged heat, is turned the normal process steps such as crystalline substance, filter pressing, washing after coupling terminates, and obtains the dyestuff filter-cakes of C.I. disperse oranges 61.
Using the above-mentioned dyestuff dyestuff filter-cakes of C.I. disperse violet 93 that continuously coupling and energy utilization technique are obtained, dye is realized
The continuous coupling of material, improves dyestuff quality. and relative to interval coupling process, dyestuff yield improves about 1.5%, and filter cake intensity is carried
It is high by about 2.8%.Realizing the saving that energy consumption is freezed in coupling production process, 30% coupling reaction heat instead of with 5 DEG C of water at low temperature-
10 DEG C of chilled waters, have saved freezing energy consumption.
Embodiment 3：
Such as Fig. 1, the 2- methoxyl group -5- acetylaminohydroxyphenylarsonic acid N, N- diacetyl oxy ethyl aniline, 12500L Jing of hundred 995kg will be rolled over
The washings of heat exchanger l coolings, the auxiliary agent TX-10 of 5kg are beaten, and obtain 7.4% coupling component beating liquid.
Above-mentioned beating liquid is continuously pumped in one-level coupling reaction kettle, while with 870kg/h's with the flow of 3857kg/h
Flow is coupled in kettle 2, the 4- dinitro -6- chloroaniline sulphuric acid diazonium salt solutions for squeezing into 30% to three-level, is coupled under agitation
Reaction, controls to add diazol and the mol ratio of folding hundred of coupling component in pan feeding to be 1：1.01, wherein diazo liquid presses 6:3:1 ratio
It is separately added into 1-3 levels coupling kettle.One-level coupling reaction discharges overflow to two grades of coupling kettles, and two grades of coupling kettles discharge overflow to three-level
Coupling kettle, with 5 DEG C of the low temperature water cooling first order kettle, controlling reaction temperature 12-17 DEG C, with -10 DEG C of low temperature water cooling are coupled
Two grades of kettle, three-level coupling kettle, controlling reaction temperature 0-5 DEG C.
Jing is exchanged heat, is turned the normal process steps such as crystalline substance, filter pressing, washing after coupling terminates, and obtains C.I. Disperse Blue-79 dyestuff filter-cakes.
Using the above-mentioned dyestuff C.I. Disperse Blue-79 dyestuff filter-cakes that continuously coupling and reduction energy consumption technique are obtained, dye is realized
The continuous coupling of material, improves dyestuff quality, and relative to interval coupling process, dyestuff yield improves 1.5%, and filter cake intensity is improved
2.3%, the saving that energy consumption is freezed in coupling production process is realized, 60% coupling reaction heat instead of -10 DEG C with 5 DEG C of water at low temperature
Chilled water, has saved freezing energy consumption.
Embodiment 4：061#, diazonium, coupling solution are disposably added, yield 98%
Such as Fig. 1, will the N- ethyl-N-cyanoethyl anilines of hundred 740kg of folding, the washings of 11500L Jing heat exchangers l coolings,
The auxiliary agent TX-10 of 5kg is beaten, and obtains 6% coupling component beating liquid.
Above-mentioned beating liquid is continuously pumped into the flow of 3140kg/h and is pumped in tower first segment reactor, while with
The flow of 1412kg/h squeezes into the 30% bromo- 4- nitroanilines sulphuric acid diazols of 2,6- bis-, control coupling kettle reaction in coupling kettle
Temperature 0-5 DEG C, carries out under agitation coupling reaction, down flows through m=0 after reaction naturally, reacts after n=18 layer column plates and completes, and goes out
Material enters next process.
Jing is exchanged heat, is turned the normal process steps such as crystalline substance, filter pressing, washing after coupling terminates, and obtains the dyestuff filter-cakes of C.I. disperse oranges 61.
Using the above-mentioned dyestuff dyestuff filter-cakes of C.I. disperse violet 93 that continuously coupling and energy utilization technique are obtained, dye is realized
The continuous coupling of material, improves dyestuff quality.Relative to interval coupling process, dyestuff yield improves about 1.5%, and filter cake intensity is carried
It is high by about 3.1%.Whole tower only needs a stirring, reduces stirring energy consumption.
The present invention is continuously pumped into coupling component suspension and diazo liquid in coupling reaction kettle by metering device in batches, adjusts
Section cooling water flow controls couple temperature for -10 DEG C～30 DEG C, and segmentation coupling reaction is carried out under agitation, and in the first order kettle is coupled
In have excessive coupling component, it is ensured that the fast reaction of diazol energy is consumed, and so as to carry out at appropriate high temperature, reduces freezing
The requirement of water and energy-conservation.Diazol is added in the second level and later coupling reaction kettle and reaction is completed under reducing reaction temperature.Adopt
With tower reactor, gravity water conservancy diversion reactant liquor, so as to save the power consumptions such as stirring.
Above-described embodiment is only used for illustrating the inventive concept of the present invention, rather than the restriction to rights protection of the present invention,
All changes for carrying out unsubstantiality to the present invention using this design, all should fall into protection scope of the present invention.
Claims (6)
1. a kind of method that dyestuff is continuously coupled and reduces energy consumption, it is characterised in that comprise the following steps：By coupling component, water and
Auxiliary agent mixing beating, the coupling solution for obtaining is continuously pumped in coupling reaction kettle by metering device, meanwhile, diazonium salt solution passes through
Metering device, is continuously pumped in multistage coupling reaction kettle in batches, control charging diazol：The mol ratio of coupling component is 1:
0.95-1.05；
By the attached heat-exchanger rig of coupling reaction kettle, adjust cooling medium consumption and control couple temperature for -10 DEG C -30 DEG C, stirring
Mixing down carries out coupling reaction, and discharging after coupling reaction terminates carries out follow-up processing；The coupling reaction kettle is tower multistage anti-
Kettle, upper level reactor is answered to discharge nature downstream to next stage reactor.
2. the method that dyestuff as claimed in claim 1 is continuously coupled and reduces energy consumption, it is characterised in that：In first order coupling reaction
Kettle control charging diazol：The mol ratio of coupling component is 0.05-0.8：1, by the attached heat-exchanger rig of coupling reaction kettle, adjust
Cooling medium consumption controls couple temperature for 0 DEG C -30 DEG C in heat-exchanger rig；Diazonium is added in the second level and later coupling reaction kettle
Salt 0.02-0.95mol, by the attached heat-exchanger rig of coupling reaction kettle, adjusts cooling medium consumption control coupling in heat-exchanger rig
Temperature is -10 DEG C -20 DEG C, and coupling reaction is carried out under agitation, and discharging after coupling reaction terminates carries out follow-up processing.
3. the method that dyestuff as claimed in claim 1 is continuously coupled and reduces energy consumption, it is characterised in that：The first order coupling is anti-
Should in coupling component excessive 20% and more than, coupling reaction temperature is higher than the second level more than 8 DEG C, with 0 DEG C and the low temperature water-cooled of the above
But.
4. the method that dyestuff as claimed in claim 1 is continuously coupled and reduces energy consumption, it is characterised in that：The coupling reaction kettle is
Tower 2-20 order reactions kettle.
5. the method that as claimed in claim 4 dyestuff is continuously coupled and reduces energy consumption, it is characterised in that：The coupling reaction kettle is
Tower 3-15 order reactions kettle.
6. the method that dyestuff as claimed in claim 1 is continuously coupled and reduces energy consumption, it is characterised in that：In the tower reactor
Tower tray be that water conservancy diversion exchanges heat difunctional plate.
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| CN107961755B (en) * | 2017-12-06 | 2020-05-19 | 南京大学盐城环保技术与工程研究院 | Azo dye coupling reaction continuous production device and production method |
| CN113842858B (en) * | 2021-09-24 | 2022-11-01 | 中国科学院山西煤炭化学研究所 | Reaction tower with reaction shallow pool and method for preparing ethylene carbonate by using reaction tower |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2021132B (en) * | 1978-02-14 | 1982-07-21 | Ici Ltd | Azo coupling process |
| DE2844634A1 (en) * | 1978-10-13 | 1980-04-24 | Hoechst Ag | METHOD FOR THE CONTINUOUS PRODUCTION OF AZOPIGMENTS |
| GB2129434B (en) * | 1982-10-08 | 1986-04-16 | Ciba Geigy Ag | Production of azo compounds |
| EP1652893B1 (en) * | 2004-10-21 | 2011-11-02 | Dainichiseika Color & Chemicals Mfg. Co. Ltd. | Production process and system for insoluble azo pigments |
| CN102796394B (en) * | 2012-07-24 | 2014-05-07 | 浙江龙盛集团股份有限公司 | Continuous coupling and energy utilization method for dyes |
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