CN102796394B - Continuous coupling and energy utilization method for dyes - Google Patents
Continuous coupling and energy utilization method for dyes Download PDFInfo
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- CN102796394B CN102796394B CN201210257473.0A CN201210257473A CN102796394B CN 102796394 B CN102796394 B CN 102796394B CN 201210257473 A CN201210257473 A CN 201210257473A CN 102796394 B CN102796394 B CN 102796394B
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- 238000005859 coupling reaction Methods 0.000 title claims abstract description 134
- 238000010168 coupling process Methods 0.000 title claims abstract description 96
- 230000008878 coupling Effects 0.000 title claims abstract description 88
- 239000000975 dye Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 72
- 238000005406 washing Methods 0.000 claims abstract description 33
- 238000007599 discharging Methods 0.000 claims abstract description 28
- 239000012065 filter cake Substances 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000009833 condensation Methods 0.000 claims description 19
- 230000005494 condensation Effects 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 14
- 239000000306 component Substances 0.000 claims description 13
- 238000010009 beating Methods 0.000 claims description 11
- 239000012954 diazonium Substances 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000012452 mother liquor Substances 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 150000001989 diazonium salts Chemical class 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000002826 coolant Substances 0.000 claims description 2
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 23
- 238000004519 manufacturing process Methods 0.000 abstract description 20
- 239000000047 product Substances 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 11
- 125000000664 diazo group Chemical group [N-]=[N+]=[*] 0.000 abstract description 10
- 239000002351 wastewater Substances 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract description 2
- 239000000725 suspension Substances 0.000 abstract 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 abstract 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 abstract 1
- 235000011130 ammonium sulphate Nutrition 0.000 abstract 1
- 239000000498 cooling water Substances 0.000 abstract 1
- 238000004537 pulping Methods 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- -1 oxy ethyl aniline Chemical compound 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 230000002000 scavenging effect Effects 0.000 description 3
- VQIRFOAILLIZOY-UHFFFAOYSA-N 2-[5-acetamido-n-(2-acetyloxyethyl)-4-[(2-bromo-4,6-dinitrophenyl)diazenyl]-2-ethoxyanilino]ethyl acetate Chemical compound C1=C(N(CCOC(C)=O)CCOC(C)=O)C(OCC)=CC(N=NC=2C(=CC(=CC=2Br)[N+]([O-])=O)[N+]([O-])=O)=C1NC(C)=O VQIRFOAILLIZOY-UHFFFAOYSA-N 0.000 description 2
- ROPYWXVRNREIQD-UHFFFAOYSA-N 2-[n-(2-cyanoethyl)-4-[(2,6-dichloro-4-nitrophenyl)diazenyl]anilino]ethyl acetate Chemical compound C1=CC(N(CCC#N)CCOC(=O)C)=CC=C1N=NC1=C(Cl)C=C([N+]([O-])=O)C=C1Cl ROPYWXVRNREIQD-UHFFFAOYSA-N 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 235000019628 coolness Nutrition 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000013505 freshwater Substances 0.000 description 2
- NHNUFAASKXPOQA-UHFFFAOYSA-N (3-acetamido-2-hydroxyphenyl)arsonic acid Chemical compound C(C)(=O)NC=1C(=C(C=CC1)[As](O)(=O)O)O NHNUFAASKXPOQA-UHFFFAOYSA-N 0.000 description 1
- WYRNRZQRKCXPLA-UHFFFAOYSA-N 3-(n-ethylanilino)propanenitrile Chemical compound N#CCCN(CC)C1=CC=CC=C1 WYRNRZQRKCXPLA-UHFFFAOYSA-N 0.000 description 1
- 239000004429 Calibre Substances 0.000 description 1
- OJGMBLNIHDZDGS-UHFFFAOYSA-N N-ethyl-N-phenylamine Natural products CCNC1=CC=CC=C1 OJGMBLNIHDZDGS-UHFFFAOYSA-N 0.000 description 1
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006193 diazotization reaction Methods 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-O diazynium Chemical compound [NH+]#N IJGRMHOSHXDMSA-UHFFFAOYSA-O 0.000 description 1
- 239000000986 disperse dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Treatment Of Water By Ion Exchange (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
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 the continuous coupling of a kind of dyestuff in synthetic and energy utilize.
(2) background technology
In DYE PRODUCTION process, nearly all chemical reaction process all needs control to carry out at a certain temperature, and in order to reach and to keep desired temperature, reaction mass often need heat or be cooled to certain temperature, and heating and cooling process all needs consumed energy.More than 60% dye species of dye industry is all azo-type structure, diazotization, coupling are the synthetic necessary steps of the type dyestuff, in doazo reaction, coupled reaction, can discharge a large amount of heats, because the rising of temperature can cause the decomposition of material, therefore thereby affect quality product and yield, need to carry out coolingly could meeting production requirement.
In actual production process, coupled reaction generally adopts batch production technique, because the volume of reactor is huger, when stirring material, agitator cannot reach good mass-and heat-transfer effect, and the local temperature of system is too high, diazonium salt is unstable in coupling system, easily there is side reaction in coupling process, yield and the purity of product are influenced, and, large volume reactor surface-area is large, and cold consumption is larger.The coupling temperature of most of dye species need be controlled at 0 ℃ of left and right, for controlling temperature of reaction, must add a large amount of ice cubes, also causes wastewater flow rate large.Dye coupling process thermal discharge is large on the one hand, need to pass into a large amount of heat-eliminating medium coolings, coupled reaction needs after finishing to heat up and carries out dyestuff and turn brilliant operation on the other hand, steam consumes larger, owing to being batch operation, the cold and hot energy that material contains cannot 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.
DYE PRODUCTION device equal Shortcomings aspect production efficiency, quality product and operation stability of coupling at intermittence, production process wastewater flow rate is large, energy consumption is high is still problem to be solved, improve 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
Large for low, the cold heat energy consumption of production efficiency in existing coupling at intermittence process and cannot effectively utilize problem, the invention provides a kind of method of continuous coupling production and total energy approach.
For achieving the above object, the technical solution adopted in the present invention is:
The continuous coupling of a kind of dyestuff and energy utilize method, described method comprises: by coupling component, water and auxiliary agent mix making beating, the coupling solution obtaining 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 control coupling temperature in heat-exchanger rig is-10 ℃ ~ 20 ℃, under agitation carry out coupled reaction, coupled reaction discharging enters heat and turns brilliant pot after heat exchange recovered energy, optionally pass into brilliant temperature to 35 ~ 65 ℃ of steam regulating rotary, turn brilliant 0.5 ~ 3h, turn brilliant discharging through press filtration, washing obtains dyestuff filter cake, heat exchange is carried out in the washing water of water washing process separation and the low temperature discharging after coupled reaction, water outlet after heat exchange is as 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, the continuous coupling of dyestuff of the present invention and energy utilize technique, coupling component, diazo liquid continuously feeding, coupling product continuous discharge, coupling product enters and turns brilliant pot after interchanger heat exchange, preferably, by two-stage heat exchange, when realizing production process heat energy and cold energy, effectively utilizes.The heat-exchanger rig of described secondary heat exchange is comprised of interchanger 1 and interchanger 2, described coupled reaction discharging and washing water carry out energy (cold energy) exchange in interchanger 1, the washing water of cooling are as coupled reaction process water, the coupled reaction liquid raising through first heat-exchange temperature and concentrated water of condensation again carry out energy (heat energy) exchange in interchanger 2, coupled reaction liquid after again heating up enters and turns brilliant pot and turn brilliant, and the water of condensation after cooling can suitably supplement part fresh water for dyestuff filter cake washing according to the needs of washing.Turn brilliant discharging and obtain mother liquor through press filtration separation, the concentrated water of condensation (50 ~ 95 ℃) of mother liquor after neutralizing, concentrating, as the thermal source of interchanger 2.
Further, the continuous coupling of dyestuff of the present invention and energy utilize technique, the progression of coupled reaction still can be according to actual production requirements set, described coupled reaction still can be 2 ~ 4 order reaction stills (preferably 2 ~ 3 grades), upper level reactor discharging overflow is to next stage reactor, and heat exchange operation is carried out in the discharging of last step reactor again.In the coupling solution that control adds and diazo liquid, the total mol ratio of folding hundred of coupling component and diazonium salt is 1:0.95 ~ 1.05, the disposable one-level coupled reaction still that adds of coupling solution, diazo liquid can disposablely add one-level coupled reaction still, also can in reactors at different levels, add step by step.
The attached heat-exchanger rig of coupled reaction still generally can adopt still external jacket, internal exchanger (as coil pipe), external heat exchanger or its combination.Described 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 and produced, improved production efficiency, product yield and product quality;
2. coupling discharging, through multi-stage heat exchanger, is all utilized effectively coupling material cold energy and concentrated water of condensation heat energy;
3. the mother liquor of separation can separately or be concentrated and process, and mother liquid coming is through neutralization, condensing crystal reclaim(ed) sulfuric acid ammonium, and water of condensation is for dyestuff filter cake washing, and wash water is further used as coupling process water after heat exchange.The higher washes of acidity that washing produces also can adopt this method to process.The method has realized useless Water reuse and resource utilization, significantly reduces discharge of wastewater.
(4) accompanying drawing explanation
Fig. 1 is 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.
By 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.
Flow by above-mentioned making beating liquid with 3857kg/h is continuously pumped in one-level coupled reaction still, simultaneously with the flow of 870kg/h to squeeze in three grades of coupling stills 30% 2,4-dinitrobenzene-6-chloroaniline sulfuric acid diazonium salt solution, under agitation carry out coupled reaction, it is 1:1.01 that control adds folding hundred mol ratios of diazonium salt and coupling component in pan feeding, and diazo liquid adds respectively one ~ tri-grade of coupling still 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, controls 0 ~ 5 ℃ of each coupling still temperature of reaction.
The discharging of three grades of coupling stills is carried out heat exchange with the washing water from wash water dashpot 2 in interchanger 1, wash water after cooling enters process water dashpot as coupling component making beating water, coupling material is warming up to approximately 15 ℃ and enters in interchanger 2, with in mother liquor and the high-temperature condensation water of rear concentration process carry out heat exchange, coupling material is warming up to approximately 35 ℃ and enters heat and turn brilliant pot, turns brilliant 2h, turns brilliant discharging press filtration, water of condensation washing with after interchanger 2 coolings, obtains C.I. Disperse Blue-79 dyestuff filter cake.
The acid mother liquid of press filtration separation is through ammonia neutralization, purification, the concentrated 70 ℃ of water of condensation that produce of scavenging solution are as the thermal source of interchanger 2, after carrying out heat exchange with the coupling product after interchanger 1 heats up, enter wash water dashpot 1, add supplementary 9800kg water, for the washing of dyestuff filter cake.
The C.I. Disperse Blue-79 dyestuff filter cake that adopts the continuous coupling of above-mentioned dyestuff and energy to utilize technique to obtain, realized the continuous coupling of dyestuff, improved dyestuff quality, with respect to coupling process at intermittence, dyestuff yield improves 1.4%, filter cake intensity improves 2.1%, realized effective utilization of the hot and cold energy of coupling production process, capacity usage ratio reaches 80%, also realized useless Water reuse and resource utilization, the identical comparable calibre of the washing water yield that waste water from dyestuff quantity discharged minimizing ~ 77%(adopts identical coupling concentration, filter cake washing to consume according to batch technology is adjusted).
Embodiment 2:
By 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.
Flow by above-mentioned making beating liquid with 3352kg/h is continuously pumped in one-level coupled reaction still, simultaneously with the flow of 1580kg/h to squeeze in coupling still 30% 2,4-dinitrobenzene-6-bromaniline sulfuric acid diazonium salt, under agitation carry out coupled reaction, it is 1:1.03 that control diazo liquid and coupling solution are rolled over hundred mol ratios, and the ratio that diazo liquid adds in secondary coupling still is 7:3.One-level coupled reaction discharging overflow, to secondary coupling still, is controlled 0 ~ 5 ℃ of each coupling still temperature of reaction.
The discharging of secondary coupling still is carried out heat exchange with the washing water from wash water dashpot 2 in interchanger 1, wash water after cooling enters process water dashpot, continue to serve as coupling component making beating water, coupling material is warming up to approximately 20 ℃ and enters in interchanger 2, with in mother liquor and the approximately 10000L high-temperature condensation water of rear concentration process carry out heat exchange, water of condensation after cooling enters wash water dashpot and adds after 10000L fresh water for dyestuff filter cake washing, coupling material is warming up to approximately 44 ℃ and enters heat and turn brilliant pot, turn brilliant 3h, turn brilliant discharging through press filtration, with the water of condensation washing after heat exchange cooling, obtain C.I. 63 ,DIS,PER,SE ,Vio,let, 63 93 dyestuff filter cakes.
Ammonia neutralization, purification for the acid mother liquid of press filtration separation.The concentrated 80 ℃ of water of condensation that produce of scavenging solution are as the thermal source of interchanger 2, enter wash water dashpot 1 after carrying out heat exchange, for the washing of dyestuff filter cake with the coupling product after interchanger 1 heats up.
The C.I. 63 ,DIS,PER,SE ,Vio,let, 63 93 dyestuff filter cakes that adopt the continuous coupling of above-mentioned dyestuff and energy to utilize technique to obtain, realized the continuous coupling of dyestuff, improved dyestuff quality, with respect to coupling process at intermittence, dyestuff yield improves approximately 1.5%, and filter cake intensity improves approximately 3%, realized effective utilization of the hot and cold energy of coupling production process, capacity usage ratio reaches 85%, has also realized useless Water reuse and resource utilization, and waste water from dyestuff quantity discharged reduces more than 64%.
Embodiment 3:O61#, diazonium, coupling solution is disposable adds, yield 98%
The N-ethyl-N-cyanoethyl aniline of folding hundred 740kg, 11500L 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.
Flow by above-mentioned making beating liquid with 3140kg/h is continuously pumped in one-level coupled reaction still, simultaneously with the flow of 1412kg/h to squeeze in coupling still 30% 2, the bromo-4-N-methyl-p-nitroaniline of 6-bis-sulfuric acid diazonium salt, under agitation carry out coupled reaction, it is 1:1.04 that control diazo liquid and coupling solution are rolled over hundred mol ratios, and diazo liquid all adds in 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, controls 0 ~ 5 ℃ of each coupling still temperature of reaction.
The discharging of three grades of coupling stills is carried out heat exchange with the washing water from wash water dashpot 2 in interchanger 1, wash water after cooling enters end water dashpot and circulates as water at the bottom of coupling component making beating water and coupled reaction, coupling material is warming up to approximately 18 ℃ and enters in interchanger 2, with in mother liquor and the high-temperature condensation water of rear concentration process carry out heat exchange, water of condensation after cooling enters wash water dashpot for dyestuff filter cake washing, coupling material is warming up to approximately 38 ℃ and enters heat and turn brilliant pot, turn brilliant 3h, turn brilliant discharging through press filtration, with the water of condensation washing after heat exchange cooling, obtain C.I. DISPERSE ORANGE 30 200 61 dyestuff filter cakes.
Ammonia neutralization, purification for the acid mother liquid of press filtration separation.The concentrated 80 ℃ of water of condensation that produce of scavenging solution are as the thermal source of interchanger 2, enter wash water dashpot 1 after carrying out heat exchange, for the washing of dyestuff filter cake with the coupling product after interchanger 1 heats up.
The C.I. DISPERSE ORANGE 30 200 61 dyestuff filter cakes that adopt the continuous coupling of above-mentioned dyestuff and energy to utilize technique to obtain, realized the continuous coupling of dyestuff, improved dyestuff quality, with respect to coupling process at intermittence, dyestuff yield improves approximately 1.7%, and filter cake intensity improves approximately 4%, realized effective utilization of the hot and cold energy of coupling production process, capacity usage ratio reaches 75%, has realized useless Water reuse and resource utilization, and waste water from dyestuff quantity discharged reduces.
Claims (3)
1. the continuous coupling of dyestuff and energy utilize method, described method comprises: by coupling component, water and auxiliary agent mix making beating, the coupling solution obtaining 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 coupling temperature is-10 ℃～20 ℃, under agitation carry out coupled reaction, coupled reaction discharging enters heat and turns brilliant pot after heat exchange, brilliant temperature to 35～65 ℃ of regulating rotary, turn brilliant 0.5～3h, turn brilliant discharging through press filtration, washing obtains dyestuff filter cake, heat exchange is carried out in washing water and the discharging after coupled reaction of water washing process separation, water outlet after heat exchange is as coupled reaction process water.
2. the method for claim 1, it is characterized in that described coupled reaction discharging is 2 grades of heat exchanges, heat-exchanger rig is comprised of interchanger 1 and interchanger 2, discharging after described coupled reaction and washing water carry out energy exchange in interchanger 1, the washing water of cooling are as coupled reaction process water, the coupled reaction liquid and the concentrated water of condensation that through first heat-exchange temperature, raise again carry out energy exchange in interchanger 2, coupled reaction liquid after again heating up enters and turns brilliant pot and turn brilliant, and the water of condensation after cooling is for dyestuff filter cake washing; Turn brilliant discharging and obtain mother liquor through press filtration separation, 50～95 ℃ concentrated water of condensation of mother liquor after neutralizing, concentrating, as the thermal source of interchanger 2.
3. the method for claim 1, is characterized in that described coupled reaction still is 2～4 order reaction stills, and upper level reactor discharging overflow is to next stage reactor, and heat exchange operation is carried out in the discharging of last step reactor again.
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| 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 |
| CN103146221B (en) * | 2013-03-12 | 2014-01-29 | 浙江迪邦化工有限公司 | Method and device for continuously producing dyes |
| CN103709791B (en) * | 2013-12-23 | 2015-09-02 | 浙江花蝶染料化工有限公司 | The dispersed dye prepared the method for dispersed dye and institute's using appts and obtain |
| CN105440737B (en) * | 2014-08-29 | 2017-08-08 | 浙江迪邦化工有限公司 | A kind of preparation method of energy saving and environment friendly disperse dyes |
| CN104830089B (en) * | 2015-04-29 | 2017-04-19 | 绍兴文理学院 | Dye continuous coupling method with reduced energy consumption |
| CN105348847B (en) * | 2015-11-13 | 2017-10-10 | 浙江闰土研究院有限公司 | A kind of continuous coupling process of dyestuff |
| CN108047751B (en) * | 2017-12-29 | 2019-11-22 | 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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