CN104830089A - Dye continuous coupling method with reduced energy consumption - Google Patents
Dye continuous coupling method with reduced energy consumption Download PDFInfo
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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, especially relate to continuous coupling in a kind of Dyestuff synthesis and reduce the method for energy consumption.
Background technology
The dye species of dye industry more than 60% is all azo-type structure, diazotization, coupling are the necessary steps of synthesis the type dyestuff, a large amount of heats can be discharged in doazo reaction, coupled reaction, rising due to temperature can cause the decomposition of material, thus affect quality product and yield, therefore needing to carry out cooling could meet production requirement.
In DYE PRODUCTION process, because the stability of diazonium salt component is lower, carry out under needing certain acidity and lower temperature.While carrying out coupled reaction, there is the side reactions such as decomposition, practice shows the rising along with temperature, and side reaction aggravates.And coupled processes is a thermopositive reaction, in order to reduce the decomposition of diazonium salt, often adopt the way of low temperature.Such result needs a large amount of energy consumption for cooling.The opposing party, low temperature reduces the speed of coupled reaction, has made the time lengthening of reaction, makes conversion unit become large.
In current actual production process, coupled reaction generally adopts batch production process, the volume of reactor is huger, and cannot reach good mass-and heat-transfer effect when agitator stirs material, the local temperature of system is too high, diazonium salt is unstable in coupling system, easily there is side reaction in coupled processes, yield and the purity of product are influenced, and, large volume reactor surface-area is large, and cold consumption is larger.The couple temperature of most of dye species need control at about 0 DEG C, for controlling temperature of reaction, must add a large amount of ice cubes, also causing wastewater flow rate large.Dye coupling process thermal discharge is large on the one hand, needs to pass into the cooling of a large amount of heat-eliminating medium.
Propose the continuous coupling of a kind of dyestuff for this problem CN 102796394 A and reduce energy consuming process, by coupling component, water and auxiliary agent mixing making beating, the coupling solution obtained is continuously pumped in coupled reaction still by measuring apparatus, simultaneously, diazonium salt solution passes through measuring apparatus, be continuously pumped in coupled reaction still, control charging diazonium salt: the mol ratio of coupling component is 1:0. 95-1.05, by the attached heat-exchanger rig of coupled reaction still, regulating cooling medium consumption to control couple temperature is-10 DEG C ~ 20 DEG C, under agitation carry out coupled reaction, coupled reaction discharging enters heat and turns brilliant pot after heat exchange.The reactor of coupled reaction is 2,4 order reaction stills, and upper level reactor discharging overflow is to next stage reactor, and the discharging of last step reactor carries out heat exchange operation again.Due to charging diazonium salt: the mol ratio of coupling component is that 1:0. 95-1.05 mixes, and there is diazo component all the time, for preventing diazonium salt from decomposing, making temperature of reaction can only control at low temperatures, having made the time lengthening of reaction in reactor, conversion unit is made to become large.Because the dye precipitated generated in reaction process is separated out, the risk that multi-floating bodies has blocking risk and dynamic equipment to break down in material transfer more.
Same CN201310078687.6; The patents such as CN201310079181.7 adopt pipeline reactor to realize serialization.Same due to charging diazonium salt: the mol ratio of coupling component is that 1:0. 95-1.05 mixes, all the time there is diazo component in reactor, for preventing diazonium salt from decomposing, temperature of reaction can only be controlled at low temperatures, make the time lengthening of reaction, made reacting pipe very long and impracticable.There is reaction time and be difficult to ensure card and line clogging equivalent risk in pipe reaction.
Based on this, the present invention is proposed.
Summary of the invention
For the problem that low, the freezing energy consumption of coupled processes production efficiency in prior art is large, the object of this invention is to provide a kind of continuous coupling produce and reduce the method for energy consumption, coupling component suspension and diazo liquid are continuously pumped in coupled reaction still by measuring apparatus in batches, regulating cooling water flow to control couple temperature is-10 DEG C ~ 30 DEG C, under agitation carry out segmentation coupled reaction, excessive coupling component is had in first step coupling still, ensure that the rapid reaction of diazonium salt energy consumes, thus carry out at suitably high temperature, reduce the requirement of refrigerated water and energy-conservation.Reaction is completed under the second stage and later coupled reaction still are added diazonium salt and reduced temperature of reaction.Adopt tower reactor, gravity water conservancy diversion reaction solution, thus save the power consumptions such as stirring.
For achieving the above object, the present invention is achieved by the following technical solutions:
The method of the continuous coupling of a kind of dyestuff and minimizing energy consumption, comprise the following steps: by coupling component, water and auxiliary agent mixing making beating, the coupling solution obtained is continuously pumped in coupled reaction still by measuring apparatus, simultaneously, diazonium salt solution passes through measuring apparatus, be continuously pumped in multistage coupled reaction still in batches, control charging diazonium salt: the mol ratio of coupling component is 1:0.95-1.05;
By the attached heat-exchanger rig of coupled reaction still, regulating cooling medium consumption to control couple temperature is-10 DEG C-30 DEG C, and under agitation carry out coupled reaction, coupled reaction terminates rear discharging and carries out follow-up processing.
Control charging diazonium salt at first step coupled reaction still: the mol ratio of coupling component is 1:0.05-0.8, by the attached heat-exchanger rig of coupled reaction still, regulate cooling medium consumption control couple temperature in heat-exchanger rig to be 0 DEG C-30 DEG C; Add diazonium salt 0.02-0.95 in the second stage and later coupled reaction still, by the attached heat-exchanger rig of coupled reaction still, regulate cooling medium consumption control couple temperature in heat-exchanger rig to be-10 DEG C-20 DEG C, under agitation carry out coupled reaction.Coupled reaction terminates rear discharging and carries out follow-up processing.
In the described first step coupled reaction coupling component excessive 20% and more than, coupled reaction temperature is higher than the second stage more than 8 DEG C, with 0 DEG C and above water at low temperature cooling.
Described coupled reaction still is tower multi-stage reacting kettle, and upper level reactor discharging nature is downstream to next stage reactor.
Described coupled reaction still is tower 2-20 order reaction still.
Described coupled reaction still is tower 3-15 order reaction still.
Tower tray in described tower reactor is the difunctional plate of water conservancy diversion heat exchange.
Beneficial effect of the present invention is mainly reflected in following several respects:
1, while achieving serialization coupling production, realize segmentation coupling, improve production efficiency, product yield and product quality;
2, segmentation coupling makes coupled reaction reach as high as the coupled reaction heat of 80%, and heat exchange under the condition comparatively relaxed, has saved cold energy;
3, coupled reaction is carried out in tower.Tower can arbitrarily divide into multiple reaction zone, and can control arbitrarily the temperature of reaction in differential responses district;
4, the multiple reaction zones in reaction tower can be the reaction zones of reaction autoclave, the runner that also can be made up of multiple baffle plate, thus reduce the power consumption stirred;
5, react in same tower, material flows from top to bottom, decreases and turns material process, effectively can prevent the blockage problem occurred because dyestuff is separated out;
6, the tower tray between at different levels in reaction tower can with heat exchanger plates compound, make it have the bifunctional tower tray of water conservancy diversion heat exchange, save space, reduce cost.
Accompanying drawing explanation
Fig. 1 is present invention process schema.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to this.
The continuous coupling of dyestuff of the present invention and minimizing energy consuming process, comprise the steps: coupling component, water and auxiliary agent mixing making beating, the coupling solution obtained is continuously pumped in tower reactor by measuring apparatus, simultaneously, diazonium salt solution passes through measuring apparatus, be continuously pumped in coupled reaction still, charging diazonium salt is controlled: the mol ratio of coupling component is 0.05-0.8:1 at the first reactor, ensure enough coupling components, by the attached heat-exchanger rig of coupled reaction still, cooling medium consumption control couple temperature in heat-exchanger rig is regulated to be 0 DEG C-30 DEG C (comparatively high tempss).Add diazonium salt 0.02-0.95 at the second section of tower, by the attached heat-exchanger rig of coupled reaction still, regulate cooling medium consumption control couple temperature in heat-exchanger rig to be-10 DEG C-20 DEG C, under agitation carry out coupled reaction.Follow-up processing is carried out after coupled reaction discharging.
The inventive method key is to control diazonium salt: the mol ratio that coupling component is different, diazonium salt component is exhausted fast in the first reactor, both carry out under the condition that coupled reaction temperature was slightly high in the first reactor, realize energy-conservation energy, improve speed of reaction, reduce the object of conversion unit.
Further, the continuous coupling of dyestuff of the present invention and minimizing energy consumption technique, the progression of coupled reaction still can according to actual production requirements set, coupled reaction still can be 20 order reaction stills, preferred 3-15 level, upper level reactor discharging overflow is to next stage reactor, and the discharging of last step reactor carries out heat exchange operation again.The folding hundred controlling coupling component and diazonium salt in the coupling solution that adds and diazo liquid always mol ratio is l:0. 95-1.05, coupling solution is disposable adds one-level coupled reaction still, diazo liquid need add step by step in reactor at different levels, wherein the first reactor adds diazonium salt: coupling component is 0.03-0.8:1, ensure that coupling component has larger excessive, control temperature of reaction higher, diazonium salt can be run out of fast, diazonium salt added by subsequent reactions still, control lower temperature of reaction, prevent diazonium salt from decomposing and make total reaction complete.Also diazonium salt can be added step by step in reactor at different levels, control the temperature of each reactor according to the reaction Expenditure Levels of diazonium salt, reach energy-conservation object.
Further, the continuous coupling of dyestuff of the present invention and minimizing energy consumption technique, the progression of coupled reaction still can according to actual production requirements set, described coupled reaction still is tower reactor, identical with autoclave first still at the first segment of tower, add diazonium salt: coupling component is 0.03-0.8:1, ensure that coupling component has larger excessive, control temperature of reaction higher.Tower second section and later diazonium salt of adding at different levels make total reaction complete.Tower tray between at different levels in reaction tower can be common flow deflector also can be the bifunctional division board of water conservancy diversion heat exchange, is preferably the bifunctional division board of water conservancy diversion heat exchange.
Further, the continuous coupling of dyestuff of the present invention and minimizing energy consumption technique, the progression of coupled reaction still can according to actual production requirements set, described coupled reaction still is tower reactor, multiple reaction zones in reaction tower, can be the reaction zone of reaction autoclave, the runner that also can be made up of multiple baffle plate, thus reduce the power consumption stirred.
eXAMPLE l
As schemed l, by the 3-acetylaminohydroxyphenylarsonic acid N of folding hundred 926kg, the auxiliary agent TX-10 of the washing water that N-Diethyl Aniline, 10500L lower the temperature through interchanger, 5kg pulls an oar, and obtains the coupling component making beating liquid of 8.1%.
Above-mentioned making beating liquid is continuously pumped in tower first segment reactor with the flow of 3352kg/h, in first segment coupling still, squeeze into 30% 2 with the flow of 1106kg/h simultaneously, 4-dinitrobenzene-6-bromaniline sulfuric acid diazonium salt, control first segment coupling still temperature of reaction 10-15 DEG C, under agitation carry out coupled reaction.First segment coupled reaction discharging overflow is to secondary coupling still, in second section coupling still, squeeze into 30% 2 with the flow of 474kg/h simultaneously, 4-dinitrobenzene-6-bromaniline sulfuric acid diazonium salt, control second section coupling still temperature of reaction 0-5 DEG C, under agitation carry out coupled reaction, naturally reacted after down flowing through n=5 layer column plate after reaction, discharging enters next process.
Through normal process steps such as heat exchange, turn crystalline substance, press filtration, washings after coupling terminates, obtain C.I. 63 ,DIS,PER,SE ,Vio,let, 63 93 dyestuff filter-cakes.
Adopt C.I. 63 ,DIS,PER,SE ,Vio,let, 63 93 dyestuff filter-cakes that the continuous coupling of above-mentioned dyestuff and Energy harvesting technique obtain, achieve the continuous coupling of dyestuff, improve dyestuff quality. relative to interval coupling process, dyestuff yield improves about 1.5%, and filter cake intensity improves about 2.8%.Achieve the saving of freezing energy consumption in coupling production process, the coupled reaction heat of 70% instead of-10 DEG C of refrigerated waters by 5 DEG C of water at low temperature, has saved freezing energy consumption.
embodiment 2: 061#, diazonium, coupling solution are disposable to add, yield 98%
As Fig. 1, by the N-ethyl-N-cyanoethyl aniline of folding hundred 740kg, 11500L through interchanger, the washing water of cooling, the auxiliary agent TX-10 of 5kg pull an oar, and obtain the coupling component making beating liquid of 6%.
Being continuously pumped into the flow of 3140kg/h by above-mentioned making beating liquid pumps in tower first segment reactor, in coupling still, squeeze into 30% 2 with the flow of 424kg/h simultaneously, 6-bis-bromo-4-N-methyl-p-nitroaniline sulfuric acid diazonium salt, control first segment coupling still temperature of reaction 14-18 DEG C, under agitation carry out coupled reaction.First segment coupled reaction discharging overflow is to secondary coupling still, in second section coupling still, squeeze into 30% 2 with the flow of 988kg/h simultaneously, 4-dinitrobenzene-6-bromaniline sulfuric acid diazonium salt, control second section coupling still temperature of reaction 0-5 DEG C, under agitation carry out coupled reaction, naturally reacted after down flowing through n=12 layer column plate after reaction, discharging enters next process.
Through normal process steps such as heat exchange, turn crystalline substance, press filtration, washings after coupling terminates, obtain C.I. DISPERSE ORANGE 30 200 61 dyestuff filter-cakes.
Adopt C.I. 63 ,DIS,PER,SE ,Vio,let, 63 93 dyestuff filter-cakes that the continuous coupling of above-mentioned dyestuff and Energy harvesting technique obtain, achieve the continuous coupling of dyestuff, improve dyestuff quality. relative to interval coupling process, dyestuff yield improves about 1.5%, and filter cake intensity improves about 2.8%.Achieve the saving of freezing energy consumption in coupling production process, the coupled reaction heat of 30% instead of-10 DEG C of refrigerated waters by 5 DEG C of water at low temperature, has saved freezing energy consumption.
embodiment 3:
As Fig. 1, by the 2-methoxyl group-5-acetylaminohydroxyphenylarsonic acid N of folding hundred 995kg, the washing water that N-diacetyl oxy ethyl aniline, 12500L lower the temperature through interchanger l, the auxiliary agent TX-10 of 5kg pull an oar, and obtain the coupling component making beating liquid of 7.4%.
Above-mentioned making beating liquid is continuously pumped in one-level coupled reaction still with the flow of 3857kg/h, in three grades of coupling stills, squeeze into 30% 2 with the flow of 870kg/h simultaneously, 4-dinitrobenzene-6-chloroaniline sulfuric acid diazonium salt solution, under agitation carry out coupled reaction, folding hundred mol ratio controlling to add diazonium salt and coupling component in pan feeding is 1:1.01, and wherein diazo liquid adds 1-3 level coupling still respectively in the ratio of 6:3:1.One-level coupled reaction discharging overflow is to secondary coupling still, secondary coupling still discharging overflow to three grade coupling still, with the water at low temperature cooling first step coupling still of 5 DEG C, controls temperature of reaction 12-17 DEG C, with water at low temperature cooling reactor secondary, three grades of coupling stills of-10 DEG C, control temperature of reaction 0-5 DEG C.
Through normal process steps such as heat exchange, turn crystalline substance, press filtration, washings after coupling terminates, obtain C.I. Disperse Blue-79 dyestuff filter-cakes.
Adopt the C.I. Disperse Blue-79 dyestuff filter-cakes that the continuous coupling of above-mentioned dyestuff and minimizing energy consumption technique obtain, achieve the continuous coupling of dyestuff, improve dyestuff quality, relative to interval coupling process, dyestuff yield improves 1.5%, and filter cake intensity improves 2.3%, achieves the saving of freezing energy consumption in coupling production process, the coupled reaction heat of 60% instead of-10 DEG C of refrigerated waters by 5 DEG C of water at low temperature, has saved freezing energy consumption.
embodiment 4: 061#, diazonium, coupling solution are disposable to add, yield 98%
As Fig. 1, the auxiliary agent TX-10 of the N-ethyl-N-cyanoethyl aniline of folding hundred 740kg, washing water that 11500L lowers the temperature through interchanger l, 5kg is pulled an oar, obtain the coupling component making beating liquid of 6%.
Being continuously pumped into the flow of 3140kg/h by above-mentioned making beating liquid pumps in tower first segment reactor, in coupling still, squeeze into 30% 2 with the flow of 1412kg/h simultaneously, 6-bis-bromo-4-N-methyl-p-nitroaniline sulfuric acid diazonium salt, control coupling still temperature of reaction 0-5 DEG C, under agitation carry out coupled reaction, naturally down flow through m=0 after reaction, reacted after n=18 layer column plate, discharging enters next process.
Through normal process steps such as heat exchange, turn crystalline substance, press filtration, washings after coupling terminates, obtain C.I. DISPERSE ORANGE 30 200 61 dyestuff filter-cakes.
Adopt C.I. 63 ,DIS,PER,SE ,Vio,let, 63 93 dyestuff filter-cakes that the continuous coupling of above-mentioned dyestuff and Energy harvesting technique obtain, achieve the continuous coupling of dyestuff, improve dyestuff quality.Relative to interval coupling process, dyestuff yield improves about 1.5%, and filter cake intensity improves about 3.1%.Whole tower only needs a stirring, decreases stirring energy consumption.
Coupling component suspension and diazo liquid are continuously pumped in coupled reaction still by measuring apparatus by the present invention in batches, regulating cooling water flow to control couple temperature is-10 DEG C ~ 30 DEG C, under agitation carry out segmentation coupled reaction, excessive coupling component is had in first step coupling still, ensure that the rapid reaction of diazonium salt energy consumes, thus carry out at suitably high temperature, reduce the requirement of refrigerated water and energy-conservation.Reaction is completed under the second stage and later coupled reaction still are added diazonium salt and reduced temperature of reaction.Adopt tower reactor, gravity water conservancy diversion reaction solution, thus save the power consumptions such as stirring.
Above-described embodiment only illustrates inventive concept of the present invention for explaining, but not the restriction to rights protection of the present invention, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should fall into protection scope of the present invention.
Claims (7)
1. the method for the continuous coupling of dyestuff and minimizing energy consumption, it is characterized in that comprising the following steps: by coupling component, water and auxiliary agent mixing making beating, the coupling solution obtained is continuously pumped in coupled reaction still by measuring apparatus, simultaneously, diazonium salt solution passes through measuring apparatus, be continuously pumped in multistage coupled reaction still in batches, control charging diazonium salt: the mol ratio of coupling component is 1:0.95-1.05;
By the attached heat-exchanger rig of coupled reaction still, regulating cooling medium consumption to control couple temperature is-10 DEG C-30 DEG C, and under agitation carry out coupled reaction, coupled reaction terminates rear discharging and carries out follow-up processing.
2. the continuous coupling of dyestuff and reduce the method for energy consumption as claimed in claim 1, is characterized in that:
Control charging diazonium salt at first step coupled reaction still: the mol ratio of coupling component is 1:0.05-0.8, by the attached heat-exchanger rig of coupled reaction still, regulate cooling medium consumption control couple temperature in heat-exchanger rig to be 0 DEG C-30 DEG C; Diazonium salt 0.02-0.95 is added in the second stage and later coupled reaction still, by the attached heat-exchanger rig of coupled reaction still, regulate cooling medium consumption control couple temperature in heat-exchanger rig to be-10 DEG C-20 DEG C, under agitation carry out coupled reaction, coupled reaction terminates rear discharging and carries out follow-up processing.
3. the continuous coupling of dyestuff and reduce the method for energy consumption as claimed in claim 1, is characterized in that: in the described first step coupled reaction coupling component excessive 20% and more than, coupled reaction temperature is higher than the second stage more than 8 DEG C, cools with 0 DEG C and above water at low temperature.
4. the continuous coupling of dyestuff and reduce the method for energy consumption as claimed in claim 1, it is characterized in that: described coupled reaction still is tower multi-stage reacting kettle, upper level reactor discharging nature is downstream to next stage reactor.
5. the continuous coupling of dyestuff and reduce the method for energy consumption as claimed in claim 4, is characterized in that: described coupled reaction still is tower 2-20 order reaction still.
6. the continuous coupling of dyestuff and reduce the method for energy consumption as claimed in claim 5, is characterized in that: described coupled reaction still is tower 3-15 order reaction still.
7. the continuous coupling of dyestuff and reduce the method for energy consumption as claimed in claim 4, is characterized in that: the tower tray in described tower reactor is the difunctional plate of water conservancy diversion heat exchange.
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| CN113842858A (en) * | 2021-09-24 | 2021-12-28 | 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 |
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