CN102796394A - Continuous coupling and energy utilization method for dyes - Google Patents
Continuous coupling and energy utilization method for dyes Download PDFInfo
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- CN102796394A CN102796394A CN2012102574730A CN201210257473A CN102796394A CN 102796394 A CN102796394 A CN 102796394A CN 2012102574730 A CN2012102574730 A CN 2012102574730A CN 201210257473 A CN201210257473 A CN 201210257473A CN 102796394 A CN102796394 A CN 102796394A
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Abstract
The invention provides a continuous coupling and energy utilization method for dyes. The method comprises the following steps of: respectively continuously pumping coupling component suspension liquid and diazo liquid into a coupling reaction kettle by a metering device; adjusting flow of cooling water and controlling the coupling temperature to be between -10 and 20 DEG C; performing coupling reaction on the coupling component suspension liquid and the diazo liquid under the stirring condition; and discharging after the coupling reaction is completed and enabling the mixture to enter a thermal transfer crystal pot after the mixture is subjected to the heat exchange. The continuous coupling and energy utilization method has the beneficial effects that the continuous coupling production is realized, so that the production efficiency and the yield are improved, and the product quality is improved and stabilized; the coupling product is subjected to multi-level heat exchange, so that the cold energy and the concentrated condensed water heat energy of the coupling material can be effectively utilized; mother liquid is neutralized, concentrated and crystallized, and ammonium sulfate is recovered, so that the heat energy of the concentrated condensed water is subjected to heat exchange and recovered; the condensed water subjected to temperature reduction is used for washing a filter cake; and the washing water is used for pulping the coupling component, so that the recycling and reclamation of the wastewater are realized, and the drainage of the waste water is greatly reduced.
Description
(1) technical field
The present invention relates to a kind of chemical industry continuous automatic production technology, more specifically, relate to the method that continuous coupling and the energy of a kind of dyestuff in synthetic utilizes.
(2) background technology
In the DYE PRODUCTION process, nearly all chemical reaction process all need be controlled under certain temperature and carry out, and in order to reach and to keep desired temperature, reaction mass often need heat or be cooled to certain temperature, and the heating and cooling process all needs consumed energy.The dye species of dye industry more than 60% all is the azo-type structure; Diazotization, coupling are the synthetic necessary steps of the type dyestuff; Can discharge great amount of heat in doazo reaction, the coupled reaction; Because the rising of temperature can cause the decomposition of material, thereby influences quality product and yield, therefore need cool off and to satisfy production requirement.
In actual production process, coupled reaction generally adopts batch production technology, because the volume of reaction kettle is huger; Can't reach mass-and heat-transfer effect preferably when whisking appliance stirs material, the local temperature of system is too high, and diazonium salt is unstable in the coupling system; The coupling process is prone to side reaction takes place, and the yield and the purity of product are influenced, and; Big volume reaction kettle surface-area is big, and cold consumption is bigger.The coupling temperature of most of dye species need be controlled at about 0 ℃, is control reaction temperature, must add a large amount of ice cubes, also causes wastewater flow rate big.Dye coupling process thermal discharge is big on the one hand; Need a large amount of heat-eliminating mediums coolings of feeding, need to heat up after coupled reaction finishes on the other hand and carry out the brilliant operation of dyestuff commentaries on classics, steam consumes bigger; Owing to be batch operation; The cold and hot ability that material contains can't store and obtain effective recycling, has caused the waste of the energy, is unfavorable for energy-saving and emission-reduction.In addition, also there is the problem of product quality batch difference in batch production.
Intermittently all there is deficiency in the DYE PRODUCTION device of coupling aspect production efficiency, quality product and the operation stability; The production process wastewater flow rate is big, energy consumption is high is still problem to be solved; Improve the production efficiency and the product quality of coupling process; Realize the comprehensive utilization of the energy, reduce production costs, become the key of coupling process innovation.
(3) summary of the invention
Can consume problem big and that can't effectively utilize to production efficiency in the existing intermittently coupling process is low, cold and hot, the present invention provides the method for a kind of continuous coupling production and total energy approach.
For realizing above-mentioned purpose, the technical scheme that the present invention adopted is:
Continuous coupling of a kind of dyestuff and energy utilize method, and said method comprises: coupling component, water and auxiliary agent are mixed making beating, and the coupling solution that obtains is continuously pumped in the coupled reaction still through WT-MSR; Simultaneously, diazonium salt solution is continuously pumped in the coupled reaction still through WT-MSR; Control charging diazonium salt: the mol ratio of coupling component is 1:0.95 ~ 1.05; Through the attached heat-exchanger rig of coupled reaction still, regulating heat-exchanger rig internal cooling rate-of flow control coupling temperature is-10 ℃ ~ 20 ℃, under agitation carries out coupled reaction; The coupled reaction discharging gets into heat behind the heat exchange recovered energy change brilliant pot; Optionally feeding steam regulate to change brilliant temperature to 35 ~ 65 ℃, changes brilliant 0.5 ~ 3h, changes brilliant discharging and obtains the dyestuff filter cake through press filtration, washing; Heat exchange is carried out in low temperature discharging after isolating washing water of water washing process and the coupled reaction, and the water outlet after the heat exchange is as the coupled reaction process water.
The inventive method key is that intermittently coupling is improved to continuous coupling, realizes the online recycle of energy, is applicable to the production of existing azo type disperse dyes.
Further, continuous coupling of dyestuff of the present invention and energy utilize technology, coupling component, the continuously feeding of diazonium liquid; The continuous discharging of coupling product; Coupling product gets into after the interchanger heat exchange changes brilliant pot, preferably through the two-stage heat exchange, effectively utilizes when realizing production process heat energy and cold energy.The heat-exchanger rig of said secondary heat exchange is made up of interchanger 1 and interchanger 2; Said coupled reaction discharging and washing water carry out energy (cold energy) exchange in interchanger 1; The washing water of cooling are as the coupled reaction process water; The coupled reaction liquid and the concentrated water of condensation that raise through first heat exchange temperature carry out energy (heat energy) exchange once more in interchanger 2; Coupled reaction liquid after heating up once more gets into the brilliant pot of commentaries on classics changes brilliant, and the water of condensation after the cooling can suitably replenish the part fresh water according to the needs that wash be used for the dyestuff filter cake washing.Change brilliant discharging and obtain mother liquor through the press filtration separation, the concentrated water of condensation (50 ~ 95 ℃) of mother liquor after neutralizing, concentrating is as the thermal source of interchanger 2.
Further; Continuous coupling of dyestuff of the present invention and energy utilize technology; The progression of coupled reaction still can be according to the actual production requirements set; Said coupled reaction still can be 2 ~ 4 order reaction stills (preferred 2 ~ 3 grades), and upper level reaction kettle discharging overflow is to the next stage reaction kettle, and heat exchange operation is carried out in the discharging of last step reaction kettle again.Folding hundred total mol ratios of coupling component and diazonium salt are 1:0.95 ~ 1.05 in coupling solution that control adds and the diazonium liquid; The disposable adding one-level of coupling solution coupled reaction still; Diazonium liquid can disposable adding one-level coupled reaction still, also can in reaction kettles at different levels, add step by step.
The attached heat-exchanger rig of coupled reaction still generally can adopt still external jacket, internal exchanger (like coil pipe), external heat exchanger or its combination.Said heat-eliminating medium can adopt chilled brine or water at low temperature etc.
Beneficial effect of the present invention is mainly reflected in following several respects:
1. realize serialization coupling production, improved production efficiency, product yield and product quality;
2. the coupling discharging makes coupling material cold energy and concentrated water of condensation heat energy all be utilized effectively through multi-stage heat exchanger;
3. isolating mother liquor can separately or be concentrated and handle, and mother liquor water is through neutralization, condensing crystal reclaim(ed) sulfuric acid ammonium, and water of condensation is used for the dyestuff filter cake washing, and wash water further is used as the coupling process water after heat exchange.The higher washes of acidity that washing produces also can adopt this method to handle.This method has realized useless Water reuse and resource utilization, significantly reduces discharge of wastewater.
(4) description of drawings
Fig. 1 is a process flow sheet of the present invention.
(5) embodiment
Below in conjunction with specific embodiment the present invention is described further, but protection scope of the present invention is not limited in this:
Embodiment 1:
Schema is referring to Fig. 1.
With 2-methoxyl group-5-acetylaminohydroxyphenylarsonic acid N of folding hundred 995kg, N-diacetyl oxy ethyl aniline, 12500L pull an oar through the washing water of interchanger 1 cooling, the auxiliary agent TX-10 of 5kg, obtain 7.4% coupling component making beating liquid.
The flow of above-mentioned making beating liquid with 3857kg/h is continuously pumped in the one-level coupled reaction still; Simultaneously with the flow of 870kg/h in three grades of coupling stills, squeeze into 30% 2; 4-dinitrobenzene-6-chloroaniline sulfuric acid diazonium salt solution; Under agitation carry out coupled reaction, control adds that folding hundred mol ratios of diazonium salt and coupling component are 1:1.01 in the pan feeding, and diazonium liquid adds one ~ three grade of coupling still respectively in the ratio of 6:3:1.One-level coupled reaction discharging overflow is to secondary coupling still, and secondary coupling still discharging overflow to three grade coupling still is controlled 0 ~ 5 ℃ of each coupling still temperature of reaction.
The discharging of three grades of coupling stills is carried out heat exchange in interchanger 1 with from the washing water of wash water dashpot 2, the wash water after the cooling gets into the process water dashpot as coupling component making beating water, and the coupling material is warming up in about 15 ℃ of entering interchanger 2; Carry out heat exchange with the high-temperature condensation water of in the mother liquor and back concentration process; The coupling material is warming up to about 35 ℃ and gets into the brilliant pot of heat commentaries on classics, changes brilliant 2h, changes brilliant discharging press filtration; Use the water of condensation washing after interchanger 2 coolings, obtain C.I. Disperse Blue-79 dyestuff filter cake.
The isolating acid mother liquid of press filtration is through ammonia neutralization, purification; Scavenging solution concentrates the thermal source that 70 ℃ of water of condensation that produce are used as interchanger 2; Get into wash water dashpot 1 with the coupling product after heating up through interchanger 1 after carrying out heat exchange, add additional 9800kg water, be used for the dyestuff washing filter cakes.
The C.I. Disperse Blue-79 dyestuff filter cake that adopts continuous coupling of above-mentioned dyestuff and energy to utilize technology to obtain; Realized the continuous coupling of dyestuff, improved the dyestuff quality, with respect to the coupling process at intermittence; The dyestuff yield improves 1.4%; Filter cake intensity improves 2.1%, has realized effective utilization of the hot and cold ability of coupling production process, and capacity usage ratio reaches 80%; Also realized useless Water reuse and resource utilization, the waste water from dyestuff quantity discharged reduces by ~ 77% (comparable calibre that the washing water yield that adopts identical coupling concentration, filter cake washing to consume according to batch technology is identical is adjusted).
Embodiment 2:
With the 3-acetylaminohydroxyphenylarsonic acid N of folding hundred 926kg, N-Diethyl Aniline, 10500L pull an oar through the washing water of interchanger 1 cooling, the auxiliary agent TX-10 of 5kg, obtain 8.1% coupling component making beating liquid.
The flow of above-mentioned making beating liquid with 3352kg/h is continuously pumped in the one-level coupled reaction still; Simultaneously with the flow of 1580kg/h in the coupling still, squeeze into 30% 2; 4-dinitrobenzene-6-bromaniline sulfuric acid diazonium salt; Under agitation carry out coupled reaction, it is 1:1.03 that control diazonium liquid and coupling solution are rolled over hundred mol ratios, and the ratio that diazonium liquid adds in secondary coupling still is 7:3.One-level coupled reaction discharging overflow is controlled 0 ~ 5 ℃ of each coupling still temperature of reaction to secondary coupling still.
The discharging of secondary coupling still is carried out heat exchange in interchanger 1 with from the washing water of wash water dashpot 2; Wash water after the cooling gets into the process water dashpot, continues to serve as coupling component making beating water, and the coupling material is warming up in about 20 ℃ of entering interchanger 2; Carry out heat exchange with about 10000L high-temperature condensation water of in the mother liquor and back concentration process; Water of condensation after the cooling gets into and is used for the dyestuff filter cake washing after the wash water dashpot is added the 10000L fresh water, and the coupling material is warming up to about 44 ℃ and gets into the brilliant pot of heat commentaries on classics, changes brilliant 3h; Change brilliant discharging through press filtration, obtain C.I. 63 ,DIS,PER,SE ,Vio,let, 63 93 dyestuff filter cakes with the water of condensation washing after the heat exchange cooling.
The isolating acid mother liquid of press filtration is with ammonia neutralization, purification.80 ℃ of water of condensation that scavenging solution concentrate to produce are as the thermal source of interchanger 2, get into wash water dashpot 1 with coupling product after heating up through interchanger 1 after carrying out heat exchange, are used for the dyestuff washing filter cakes.
The C.I. 63 ,DIS,PER,SE ,Vio,let, 63 93 dyestuff filter cakes that adopt continuous coupling of above-mentioned dyestuff and energy to utilize technology to obtain have been realized the continuous coupling of dyestuff, have improved the dyestuff quality; With respect to the coupling process at intermittence, it is about 1.5% that the dyestuff yield improves, and filter cake intensity improves about 3%; Realized effective utilization of the hot and cold ability of coupling production process; Capacity usage ratio reaches 85%, has also realized useless Water reuse and resource utilization, and the waste water from dyestuff quantity discharged reduces more than 64%.
Embodiment 3:O61#, diazonium, the disposable adding of coupling solution, yield 98%
N-ethyl-N-cyanoethyl aniline, the 11500L of folding hundred 740kg are pulled an oar through the washing water of interchanger 1 cooling, the auxiliary agent TX-10 of 5kg, obtain 6% coupling component making beating liquid.
The flow of above-mentioned making beating liquid with 3140kg/h is continuously pumped in the one-level coupled reaction still; Simultaneously with the flow of 1412kg/h in the coupling still, squeeze into 30% 2; 6-two bromo-4-N-methyl-p-nitroaniline sulfuric acid diazonium salts; Under agitation carry out coupled reaction, it is 1:1.04 that control diazonium liquid and coupling solution are rolled over hundred mol ratios, and diazonium liquid all adds in the one-level coupled reaction still.One-level coupled reaction discharging overflow is to secondary coupling still, and secondary coupling still discharging overflow to three grade coupling still is controlled 0 ~ 5 ℃ of each coupling still temperature of reaction.
The discharging of three grades of coupling stills is carried out heat exchange in interchanger 1 with from the washing water of wash water dashpot 2; Wash water after the cooling gets into end water dashpot and circulates as water at the bottom of coupling component making beating water and the coupled reaction; The coupling material is warming up in about 18 ℃ of entering interchanger 2, and carries out heat exchange with the high-temperature condensation water of back concentration process in the mother liquor, and water of condensation after the cooling gets into the wash water dashpot and is used for the dyestuff filter cake washing; The coupling material is warming up to about 38 ℃ and gets into the brilliant pot of heat commentaries on classics; Change brilliant 3h, change brilliant discharging, obtain C.I. DISPERSE ORANGE 30 200 61 dyestuff filter cakes with the water of condensation washing after the heat exchange cooling through press filtration.
The isolating acid mother liquid of press filtration is with ammonia neutralization, purification.80 ℃ of water of condensation that scavenging solution concentrate to produce are as the thermal source of interchanger 2, get into wash water dashpot 1 with coupling product after heating up through interchanger 1 after carrying out heat exchange, are used for the dyestuff washing filter cakes.
The C.I. DISPERSE ORANGE 30 200 61 dyestuff filter cakes that adopt continuous coupling of above-mentioned dyestuff and energy to utilize technology to obtain have been realized the continuous coupling of dyestuff, have improved the dyestuff quality; With respect to the coupling process at intermittence, it is about 1.7% that the dyestuff yield improves, and filter cake intensity improves about 4%; Realized effective utilization of the hot and cold ability of coupling production process; Capacity usage ratio reaches 75%, has realized useless Water reuse and resource utilization, and the waste water from dyestuff quantity discharged reduces.
Claims (3)
1. continuous coupling of dyestuff and energy utilize method, and said method comprises: coupling component, water and auxiliary agent are mixed making beating, and the coupling solution that obtains is continuously pumped in the coupled reaction still through WT-MSR; Simultaneously, diazonium salt solution is continuously pumped in the coupled reaction still through WT-MSR; Control charging diazonium salt: the mol ratio of coupling component is 1:0.95 ~ 1.05, and through the attached heat-exchanger rig of coupled reaction still, regulating cooling medium consumption control coupling temperature is-10 ℃ ~ 20 ℃; Under agitation carry out coupled reaction, the coupled reaction discharging gets into heat after heat exchange change brilliant pot, regulates and change brilliant temperature to 35 ~ 65 ℃; Change brilliant 0.5 ~ 3h; Change brilliant discharging and obtain the dyestuff filter cake through press filtration, washing, heat exchange is carried out in the discharging after isolating washing water of water washing process and the coupled reaction, and the water outlet after the heat exchange is as the coupled reaction process water.
2. the method for claim 1; It is characterized in that said coupled reaction discharging is 2 grades of heat exchanges; Heat-exchanger rig is made up of interchanger 1 and interchanger 2; Discharging after the said coupled reaction and washing water carry out energy exchange in interchanger 1, the washing water of cooling are as the coupled reaction process water, carry out energy exchange at interchanger 2 in once more through coupled reaction liquid that first heat exchange temperature raises and concentrated water of condensation; Coupled reaction liquid after heating up once more gets into the brilliant pot of commentaries on classics changes brilliant, and the water of condensation after the cooling is used for the dyestuff filter cake washing; Change brilliant discharging and obtain mother liquor through the press filtration separation, 50 ~ 95 ℃ concentrated water of condensation of mother liquor after neutralizing, concentrating are as the thermal source of interchanger 2.
3. the method for claim 1 is characterized in that said coupled reaction still is 2 ~ 4 order reaction stills, and upper level reaction kettle discharging overflow is to the next stage reaction kettle, and heat exchange operation is carried out in the discharging of last step reaction kettle again.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103146221A (en) * | 2013-03-12 | 2013-06-12 | 浙江迪邦化工有限公司 | Method and device for continuously producing dyes |
| CN103709791A (en) * | 2013-12-23 | 2014-04-09 | 浙江花蝶染料化工有限公司 | Method and device for preparing disperse dye and obtained disperse dye |
| CN103965649A (en) * | 2013-02-05 | 2014-08-06 | 浙江龙盛集团股份有限公司 | Preparation method for azo disperse dye with stable crystal form |
| CN104830089A (en) * | 2015-04-29 | 2015-08-12 | 绍兴文理学院 | Dye continuous coupling method with reduced energy consumption |
| CN105348847A (en) * | 2015-11-13 | 2016-02-24 | 浙江闰土研究院有限公司 | A continuous coupling process for dye |
| CN105440737A (en) * | 2014-08-29 | 2016-03-30 | 浙江迪邦化工有限公司 | Preparation method of energy-efficient and environmentally-friendly disperse dye |
| CN108047751A (en) * | 2017-12-29 | 2018-05-18 | 沈阳化工研究院有限公司 | A kind of band ester group azo dispersion dyes serialization coupling process |
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Cited By (12)
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| CN103965649A (en) * | 2013-02-05 | 2014-08-06 | 浙江龙盛集团股份有限公司 | Preparation method for azo disperse dye with stable crystal form |
| CN103965649B (en) * | 2013-02-05 | 2016-08-17 | 浙江龙盛集团股份有限公司 | A kind of method preparing stable crystal form azo dispersion dyes |
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| CN105440737A (en) * | 2014-08-29 | 2016-03-30 | 浙江迪邦化工有限公司 | Preparation method of energy-efficient and environmentally-friendly disperse dye |
| CN104830089A (en) * | 2015-04-29 | 2015-08-12 | 绍兴文理学院 | Dye continuous coupling method with reduced energy consumption |
| CN105348847A (en) * | 2015-11-13 | 2016-02-24 | 浙江闰土研究院有限公司 | A continuous coupling process for dye |
| CN108047751A (en) * | 2017-12-29 | 2018-05-18 | 沈阳化工研究院有限公司 | A kind of band ester group azo dispersion dyes serialization coupling process |
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