CN108892270A - A method of amino benzene analog waste water is handled using tubular reactor - Google Patents

A method of amino benzene analog waste water is handled using tubular reactor Download PDF

Info

Publication number
CN108892270A
CN108892270A CN201810743382.5A CN201810743382A CN108892270A CN 108892270 A CN108892270 A CN 108892270A CN 201810743382 A CN201810743382 A CN 201810743382A CN 108892270 A CN108892270 A CN 108892270A
Authority
CN
China
Prior art keywords
waste water
amino benzene
tubular reactor
acid
benzene analog
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810743382.5A
Other languages
Chinese (zh)
Inventor
冯梦龙
马引民
黄卓
李小华
葛海洋
彭敬慧
万琪
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HANGZHOU BAIHE CLARIANT PIGMENT CO Ltd
Original Assignee
HANGZHOU BAIHE CLARIANT PIGMENT CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by HANGZHOU BAIHE CLARIANT PIGMENT CO Ltd filed Critical HANGZHOU BAIHE CLARIANT PIGMENT CO Ltd
Priority to CN201810743382.5A priority Critical patent/CN108892270A/en
Publication of CN108892270A publication Critical patent/CN108892270A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • B01J19/2415Tubular reactors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • B01J19/2415Tubular reactors
    • B01J19/242Tubular reactors in series
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/001Processes for the treatment of water whereby the filtration technique is of importance
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/38Treatment of water, waste water, or sewage by centrifugal separation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/66Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F2001/007Processes including a sedimentation step
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/08Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]

Abstract

The present invention relates to a kind of processing amino benzene analog waste water more particularly to a kind of methods using tubular reactor processing amino benzene analog waste water.A certain amount of acid is added to amino benzene analog waste water, it is acidified, then the amino benzene analog waste water of acidification and sodium nitrite solution are pumped into tubular reactor from different pipelines respectively and carry out diazotising, obtained diazonium salt is after another outlet discharge, it is coupled with azo pigments waste water (containing the organic matter that can be coupled on a small quantity with diazonium salt), coupling solution is transported to settling tank, through separating treatment, filtrate discharge is further processed to sewage treatment plant, filter residue carries out burning disposal after drying, the aniline removal efficiency of waste water is 99% or more, the removal efficiency of COD is 30% or more.Efficiently solve the problems, such as the aniline waste water in Pigment Intermediates DATA (DTTA) production process, realize " with dirty pollution treatment ", saved production cost that there is significant economic benefit and environmental benefit.

Description

A method of amino benzene analog waste water is handled using tubular reactor
Technical field
The present invention relates to a kind of processing amino benzene analog waste waters more particularly to a kind of utilization tubular reactor to handle amino benzene analog waste water Method, be related to carrying out diazotising-to the amino benzene analog waste water that generates in quinacridone intermediate DATA (DTTA) production process Coupling processing.
Background technique
There are many ways to synthesizing quinacridone compound, can be divided into halogen by the raw material or key intermediate difference of use For terephthaldehyde's acid system, hydroquinone or 1,4-benzoquinone method, diethenone process and succinic acid diformazan (second) ester process (DMSS method). The main method generallyd use at present is succinic acid diformazan (second) ester process (DMSS method), divides according to closed loop conditions, can segment For hot closed loop route (HTR), sour closed loop route (PPA), wherein most popular is sour closed loop route (PPA).
Sour closed loop route (PPA route):The first step is succinyl base dimethyl succinate (DMSS) and aniline condensation, second Step is to aoxidize 2,5- diarylamino -3,6- dihydro dimethyl terephthalate (DMT), and hydrolyze and generate key intermediate 2, bis- virtue of 5- Amino terephthalic acid (TPA) (DATA or DTTA), third step are that 2,5- diarylamino terephthalic acid (TPA) closes under PPA high temperature Ring reaction, generates quinacridone.
The plant process synthesis flow of quinacridone intermediate DATA (DTTA):The first step is succinyl base succinic acid diformazan Ester (DMSS) and aniline (para-totuidine) carry out condensation reaction under acid catalysis, obtain 2,5- diarylamino -3,6- dihydro Dimethyl terephthalate (DMT), the input amount of aniline (para-totuidine) are the 110~125% of theoretical amount;Second step is to above-mentioned A large amount of liquid alkaline is added in material, the oxidants such as nitrobenzene, m-nitrobenzene sodium sulfonate or hydrogen peroxide are then added and aoxidize instead It answers, oxidation finishes, and steam distillation removes methanol, is acidified with acid, and intermediate DATA (DTTA) is precipitated, filter, rinsing, dry, Milling, obtains DATA (DTTA) intermediate, excessive aniline (para-totuidine) enters in filtrate.
What is involved is be directed to the aniline generated in quinacridone intermediate DATA (or DTTA) production process (to first for this patent Aniline) waste water, diazotising-coupling processing is carried out, dye wastewater is solved while handling arylamine waste water, realizes and " controlled with dirt It is dirty ", save production cost.
In quinacridone intermediate DATA (or DTTA) production process, the aniline value of aniline (para-totuidine) waste water is up to 23650ppm, COD are up to 36500ppm.
Industrially, the processing method of amino benzene analog waste water has very much.According to the difference of method, common processing method can divide For physical method, chemical method and 3 kinds of bioanalysis, physical method mainly includes absorption method, complexing abstraction, membrane separation process etc., is mainly answered Separation, enrichment for amino benzene analog waste water pretreatment stage;Chemical method includes Electrocatalytic Oxidation, photocatalytic oxidation, chemistry Oxidizing process, supercritical water oxidation method, ClO 2 catalyzed oxidation method etc., the main effect for passing through mass transfer and chemical reaction, by water In organic pollutant separate or be decomposed into innocuous substance;Bioanalysis is fitted using microbial degradation Aniline categories Close processing low concentration aniline waste water.
[research of the macroreticular resin NG-13 processing to n-butyl aniline production waste water, Hu great Bo, Chinese Resources are comprehensive for document It utilizes, 2012,30 (6):33-36] novel macroporous absorbent resin NG-13 is used, to being produced in n-butyl aniline production process Raw high concentration carries out adsorption treatment containing aniline waste water.The result shows that after resin adsorption is handled, Aniline mass concentration 5mg/L is reduced to by about 8500mg/L hereinafter, meeting the three-level discharge of standard GB/T 8978-1996 integrated wastewater discharge standard Standard requirements, aniline recovery rate are greater than 99%, and resin is reusable after being desorbed.
[complex-precipitation technical treatment contains aniline waste water, Liu Yan, dyestuff and dyeing, 2017,54 (3) to document:58-61] it uses Complex-precipitation technical treatment aniline simulated wastewater, has investigated the influence factors such as pH value, reaction time, dosage.Experimental result is aobvious Show:Under conditions of pH value of reaction system 8~10, reaction time 40min, added amount of chemical are 1.5g, waste water nitrogen removal rate >=97%.This technology can be used for phenyl amines and azo waste water.
[membrane extraction handles high-concentration industrial aniline waste water, Wu Lili, Zhou Jiti, Zhang Aili, Xia Yuanhua, Xiao Min, Liu to document Wan Tao, Environmental Pollution and Control, 2007,29 (4):300-302] use membrane extraction process Pharma Inc.'s biodegradability pole The High Concentration Aniline Wastewater of difference.The experimental results showed that flow of inlet water is 3.05L/d, reaction temperature is 50 DEG C, extract liquor pH ≈ 1, under the conditions of the long 18m of membrane tube, when water inlet aniline mass concentration is 33081mg/L, aniline removal rate is stablized 97% or more.
Document [Fenton method handle aniline waste water, Hu Haobo, it is resource-effective with it is environmentally friendly, 2014, (1):122-123] it investigates The factors such as time, temperature, pH value, reagent dosage go the influence of the effect of aniline in water removal to Fenton reagent.The result shows that: Optimal reaction condition is H2O2And Fe2+Concentration than about 10:1, temperature is at 30 DEG C, and pH value is 3 or so, the removal rate of aniline It can reach 95.02%;The progress of the excessively high and too low catalytic oxidation to Fenton reagent of pH value is all unfavorable.Fenton reagent Middle Fe3+It can be with Fe2+Synergistic effect, enhances the catalysis oxidation ability of Fenton reagent.
Document [O3The research of/UV processing aniline waste water, poplar prison peak, Bao Zhiyu, Dong Yanmao, environmental science and technology, 2009,22 (2):5-8] UV, O is respectively adopted3、O33 kinds of modes such as/UV handle aniline waste water, the results showed that O3The treatment effeciency highest of/UV, In O3Intake is 21.4mg/min, under conditions of initial pH value is 6.74 and aniline mass concentration is 100mg/L, reaction The removal rate of aniline is up to 99% when 10min.
[aniline is in SnO for document2Electrochemical oxidation on/Ti electrode, Wang Yuling, Cai Naicai, Huo Yaodong, Chen Hao are physico Learn journal, 2001,17 (7):609-613] it has studied with SnO2/ Ti is the electrochemical degradation characteristic of anodic degradation aniline.Experiment The result shows that comparing with Pt electrode, the SnO of F is mixed2/ Ti electrode is demonstrated by apparent effect to the degradation of aniline;Aniline is in SnO2/ Rates of oxidative degradation depends mainly on the anodic solution behavior of in-between product, the organic film being made of intermediate product on Ti electrode Anodic solution be reaction slow step it is rapid.
Document [the biological reinforced treatment efficiency of aniline waste water SBR technique, Wang Zhe, Wei Li, Ma Fang, Zhao Guang, Zhang Si, Harbin Polytechnical university's journal, 2010,42 (6):949-953] biological reinforcing technology is used, the efficient degrading aniline that laboratory screening is gone out Bacterium JH-9 is put into sbr reactor device, and realization effectively removes aniline.When system stable operation, the removal rate of aniline is 3 It and be respectively 80% or more and 100% after 5 days, while being also able to achieve and COD effectively removed, COD after system stable operation Removal rate reach 92.23%.
The processing method of amino benzene analog waste water has very much, but the place that mostly comes with some shortcomings.If extraction is only to pollution One physical transfer process of object, extractant may cause the secondary pollution of environment;Although membrane separation process is to water treatment effect Preferably, but need periodically to carry out soak cleaning, operating cost is high;Although Fenton oxidation method effect is obvious, reaction condition compared with For harshness, oxidant cost is high and is not easy to store and transport;Biochemical method takes up a large area, and is not suitable for processing high concentration Aniline waste water, and experimental condition is required harsher.
Diazotising-coupling process is the main method for preparing classical azo pigments, the existing a large amount of reports of document.
Document [synthesis and modification of C.I. pigment red 146, Lv Dongjun, Zhang Jichang, dyestuff and dyeing, 2007,44 (6):6- 8] synthetic method and modified situation of pigment red 146 are described.In fast red KD base under conditions of hydrochloric acid, glacial acetic acid coexist, stir After mixing dissolution, ice water is added and cools down at 5 DEG C, sodium nitrite solution is added and carries out diazotising, controls the excess of sodium nitrite Situation.Diazo liquid obtained above is completely added to dissolve sufficient AS-LC solution with sodium hydroxide solution in advance in 1h Middle carry out coupling reaction, temperature rises to 90 DEG C after reacting 1h, keeps the temperature 30min, filters, is washed to neutral, drying, obtains paratonere 146。
Document [synthesis of paratonere 170, red legend Piao, Dai Ling, Sichuan chemical industry, 2013 (3):7-10] describe β type pigment Red 170 synthetic method.Firstly, Para Amino Benzamide dissolves in advance in aqueous hydrochloric acid solution, it, will be sub- after being cooled to 0~5 DEG C Sodium nitrate solution, which is added in Para Amino Benzamide solution, carries out diazo-reaction, and control temperature does not exceed 10 DEG C.Reaction It finishes, removes excessive sodium nitrite.This diazo liquid is added in the good AS-PH ethanol solution of preparatory alkali soluble solution and is coupled Reaction is stirred to react to diazonium salt and disappears, as coupling reaction terminal.Further progress filtering, rinsing, drying, obtain β type face Expect red 170.
Document [synthesis of pigment yellow 13 and pigmentation research, Li Chunqing, Yang Jiajun, dye industry, 1996,33 (6):22- 24] synthetic method of pigment yellow 13 is described.Firstly, 3,3 '-dichloro-benzidine are beaten dispersion in hydrochloric acid solution, are cooled to 0 DEG C, sodium nitrite solution is added and carries out diazotising, active carbon decoloring is added, pale yellow transparent filtrate is obtained by filtration.It will be above-mentioned heavy Nitrogen liquid is added in 2, the 4- dimethylacetamide antifebrin slurry pre-processed and carries out coupling reaction, carries out after coupling Then heating and heat preservation operation filters, rinses, is dry, obtaining pigment yellow 13.
[synthesis and application study of organic pigment orange 74, opening and closing are outstanding, Zhang Dongjiang, Shanghai Dyestuffs, 2010,38 (5) for document: 30-31] describe the synthetic method of organic pigment orange 74.With the chloro- N of 4- amino -2,5- two, N- Dimethyl-benzenesulfonamide and Naphthols AS-E (4- chloro-3-hydroxyl -2- naphthanilide) is that starting material is obtained by diazotising, coupling and last handling process To pigment orange 74.
Diazotising-coupling process is a kind of universal important methodology of organic synthesis, is widely used in dyestuff, pigment, medicine etc. Industry.Meanwhile diazotization process is the dangerous chemical process for the first batch of emphasis supervision that national Administration of Work Safety Supervision is assert, reaction is one A exothermic reaction, thermal discharge 219kJ/mol, therefore the enough cooling mediums of configuration (such as ice water is cooling) is usually required, with consumption Dissipate heat of reaction, it is ensured that process safety.
Summary of the invention
The present invention mainly solves the deficiencies in the prior art, provides that one is quinacridone pigment intermediate is raw The amino benzene analog waste water and sodium nitrite solution generated during producing carries out diazo-reaction in tubular reactor, obtained diazonium Salting liquid and the waste water in azo pigments workshop are coupled, reaction solution after filtering, filtrate discharge to sewage treatment plant carry out into The processing of one step, filter residue is after drying into incinerator burning disposal.By above-mentioned processing, the aniline value of waste water, COD are significantly reduced, It realizes " with dirty pollution treatment ", is given up with significant economic benefit and a kind of of environmental benefit using tubular reactor processing phenyl amines The method of water.
Above-mentioned technical problem of the invention is mainly to be addressed by following technical proposals:
A method of amino benzene analog waste water being handled using tubular reactor, is carried out according to the following steps:
(1), processing analysis:
It can be used for handling the amino benzene analog waste water generated in quinacridone intermediate production process and other chemicals production The phenyl amines sewage generated in the process;
The quinacridone intermediate is 2,5- diphenylamino-dimethyl terephthalate (DMT) (DATA), (the 4- methyl of 2,5- bis- Phenylamino)-dimethyl terephthalate (DMT) (DTTA), 2,5- bis- (4- chloroanilino)-dimethyl terephthalate (DMT), bis- (3- of 2,5- Chloroanilino)-dimethyl terephthalate (DMT) is one such;
It is respectively intended to prepare pigment violet 19 (PV19), pigment red 122 (PR122), paratonere 202 (PR202), paratonere 209(PR209);
(2), concrete operations:
Amino benzene analog waste water is first subjected to acidification, amino benzene analog waste water and sodium nitrite solution are then pumped into pipe simultaneously Carried out in formula reactor mixing and diazo-reaction, by reaction solution from the other end of tubular reactor exclude, then with come from azo Waste water in pigment manufacturing process is mixed, is reacted, and after separating treatment, filtrate discharge to sewage treatment plant is carried out further Processing, filter residue carry out burning disposal after drying.
Preferably, the acid of acidification can be selected from hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid related inorganic acid and formic acid, second Sour Related organic acid.
Preferably, acid is to select hydrochloric acid.
Preferably, the concentration range of hydrochloric acid is 10%~40%;The dosage of hydrochloric acid be aniline category matter mole 3~ 6 times.
Preferably, the concentration range of hydrochloric acid is 30%~35%, the dosage of hydrochloric acid be aniline category matter mole 3~ 4 times.
Preferably, the waste water in azo pigments production process comes from pigment yellow 74, pigment yellow 83, pigment red 146, pigment The waste water of red 170 relative production process, can individually one or more of waste water mixing.
Preferably, diazo liquid and azo plant effluent simultaneous pumping carry out being coupled instead into another tubular reactor It answers;Coupling reaction is carried out or, directly diazo liquid is discharged into the storage tank of dye wastewater.
Preferably, separating treatment is centrifuge separation, plate and frame type filter-press filtering or standing sedimentation separation.
Preferably, separating treatment is plate and frame type filter-press filtering.
The present invention has the advantages that:
1, method of the invention is simple and easy, is capable of handling the amino benzene analog waste water that aniline value is up to 23650ppm, and not Need to consume a large amount of ice for cooling down, whole process is safe, controllable, energy saving, efficient;
2, the sewage of method comprehensive treatment difference workshop section of the invention, realizes " with dirty pollution treatment ", and not only treatment effeciency is high, And it is at low cost, there is significant economic benefit and environmental benefit.
Therefore, a kind of method using tubular reactor processing amino benzene analog waste water of the invention, processing mode is efficient, into one Step protection environment.
Detailed description of the invention
Fig. 1 is diazotising-coupling process flow diagram of amino benzene analog waste water;
Fig. 2 is diazonium coupled reaction of the amino benzene analog waste water in tubular reactor.
Specific embodiment
Below with reference to the embodiments and with reference to the accompanying drawing the technical solutions of the present invention will be further described.
Embodiment 1:It as shown, in the present invention, and is contained after the aniline category matter diazotising in amino benzene analog waste water Active group, dissolution azo pigments waste water be coupled, highly toxic aniline category matter and other organic compounds also from It is precipitated out in waste water, the aniline value and COD of waste water significantly reduce, and subsequent processing pressure greatly reduces.It is specifically shown in following reality Apply example.
Embodiment 1:
The aniline waste water (aniline value 23650ppm, COD 36500ppm) of the workshop 500ml intermediate workshop section is taken, is added The hydrochloric acid of metering, material become the solution of clear.It is on the rocks to be cooled to 0 DEG C or so, start the nitrous that metering is added under liquid Acid sodium solution controls the addition speed of sodium nitrite solution, until diazo-reaction is substantially completely.Above-mentioned diazo liquid is added drop-wise to In waste water (aniline value 96.3ppm, COD 20470ppm) in 74 production process of 500ml pigment yellow, pay attention to observing material feelings Condition, and the excessive situation of diazo liquid is detected, when detecting the micro- excess of diazo liquid and can't detect azoic coupling component, it is complete to be considered as coupling reaction Entirely.Continue after stirring 30min, filtering, the aniline value for being coupled filtrate is 72ppm, COD 18660ppm, entire diazotising-coupling The removal efficiency that the removal efficiency for reacting aniline is 99.40%, COD is 34.53%.
Embodiment 2:
In the constant situation of 1 other conditions of embodiment, the diazo-reaction of aniline waste water, benzene are carried out in tubular reactor The removal efficiency that the removal efficiency of amine is 99.70%, COD is 32.46%.
Embodiment 3:
In the constant situation of 1 other conditions of embodiment, aniline waste water is successively carried out in two continuous tubular reactors Diazo-reaction and its coupling reaction with 74 waste water of pigment yellow, the removal efficiency that the removal efficiency of aniline is 99.69%, COD be 35.03%.
In conclusion by after the aniline category matter diazotising in amino benzene analog waste water, with the azo containing active group, dissolution Pigment wastewater is coupled, and highly toxic aniline category matter and other organic compounds are also precipitated out from waste water, waste water Aniline value and COD are significantly reduced, and subsequent processing pressure greatly reduces.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow Ring substantive content of the invention.

Claims (9)

1. a kind of method using tubular reactor processing amino benzene analog waste water, it is characterised in that carry out according to the following steps:
(1), processing analysis:
It can be used for handling the amino benzene analog waste water generated in quinacridone intermediate production process and other chemicals production process The phenyl amines sewage of middle generation;
The quinacridone intermediate is 2,5- diphenylamino-dimethyl terephthalate (DMT) (DATA), (the 4- methyl phenylamino of 2,5- bis- Base)-dimethyl terephthalate (DMT) (DTTA), 2,5- bis- (4- chloroanilino)-dimethyl terephthalate (DMT), (the 3- chlorobenzene of 2,5- bis- Amino)-dimethyl terephthalate (DMT) is one such;
It is respectively intended to prepare pigment violet 19 (PV19), pigment red 122 (PR122), paratonere 202 (PR202), paratonere 209 (PR209);
(2), concrete operations:
Amino benzene analog waste water is first subjected to acidification, it is anti-that amino benzene analog waste water and sodium nitrite solution are then pumped into tubular type simultaneously Answer carried out in device mixing and diazo-reaction, by reaction solution from the other end of tubular reactor exclude, then with come from azo pigments Waste water in production process is mixed, is reacted, and after separating treatment, filtrate discharge to sewage treatment plant is further located Reason, filter residue carry out burning disposal after drying.
2. a kind of method using tubular reactor processing amino benzene analog waste water according to claim 1, it is characterised in that:Acid The acid for changing processing can be selected from hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid related inorganic acid and formic acid, acetic acid Related organic acid.
3. a kind of method using tubular reactor processing amino benzene analog waste water according to claim 2, it is characterised in that:Acid To select hydrochloric acid.
4. a kind of method using tubular reactor processing amino benzene analog waste water according to claim 3, it is characterised in that:Salt The concentration range of acid is 10%~40%;The dosage of hydrochloric acid is 3~6 times of aniline category matter mole.
5. a kind of method using tubular reactor processing amino benzene analog waste water according to claim 4, it is characterised in that:Salt The concentration range of acid is 30%~35%, and the dosage of hydrochloric acid is 3~4 times of aniline category matter mole.
6. a kind of method using tubular reactor processing amino benzene analog waste water according to claim 1, it is characterised in that:It is even Waste water in nitrogen pigment manufacturing process is from pigment yellow 74, pigment yellow 83, pigment red 146,170 relative production process of paratonere Waste water, can individually one or more of waste water mixing.
7. a kind of method using tubular reactor processing amino benzene analog waste water according to claim 3, it is characterised in that:Weight Nitrogen liquid and azo plant effluent simultaneous pumping carry out coupling reaction into another tubular reactor;Or, directly diazo liquid is arranged It is put into the storage tank of dye wastewater and carries out coupling reaction.
8. a kind of method using tubular reactor processing amino benzene analog waste water according to claim 3, it is characterised in that:Point It is centrifuge separation, plate and frame type filter-press filtering or standing sedimentation separation from processing.
9. a kind of method using tubular reactor processing amino benzene analog waste water according to claim 8, it is characterised in that:Point It is plate and frame type filter-press filtering from processing.
CN201810743382.5A 2018-07-09 2018-07-09 A method of amino benzene analog waste water is handled using tubular reactor Pending CN108892270A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810743382.5A CN108892270A (en) 2018-07-09 2018-07-09 A method of amino benzene analog waste water is handled using tubular reactor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810743382.5A CN108892270A (en) 2018-07-09 2018-07-09 A method of amino benzene analog waste water is handled using tubular reactor

Publications (1)

Publication Number Publication Date
CN108892270A true CN108892270A (en) 2018-11-27

Family

ID=64348163

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810743382.5A Pending CN108892270A (en) 2018-07-09 2018-07-09 A method of amino benzene analog waste water is handled using tubular reactor

Country Status (1)

Country Link
CN (1) CN108892270A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3789352A1 (en) * 2019-09-04 2021-03-10 Clariant Plastics & Coatings Ltd Process for treatment of wastewater containing phenol, aniline or derivatives thereof
CN113603264A (en) * 2021-08-24 2021-11-05 北京盖雅环境科技有限公司 Method for treating wastewater in DNS acid reduction section

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4343263A1 (en) * 1993-12-17 1995-06-22 Oekologische Sanierungs Und En Removal of phenol and aromatic amine from waste water
CN103613511A (en) * 2013-12-11 2014-03-05 江苏吉华化工有限公司 Dilute sulfuric acid diazotization process of substituted phenylamine
CN103756359A (en) * 2013-12-25 2014-04-30 浙江劲光化工有限公司 Treatment method for p-beta hydroxyethyl sulfone acetanilide mother liquor waste water

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4343263A1 (en) * 1993-12-17 1995-06-22 Oekologische Sanierungs Und En Removal of phenol and aromatic amine from waste water
CN103613511A (en) * 2013-12-11 2014-03-05 江苏吉华化工有限公司 Dilute sulfuric acid diazotization process of substituted phenylamine
CN103756359A (en) * 2013-12-25 2014-04-30 浙江劲光化工有限公司 Treatment method for p-beta hydroxyethyl sulfone acetanilide mother liquor waste water

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
韩长日等: "《精细化工品实用生产技术手册 颜料制造与色料应用技术》", 30 June 2001, 北京:科学技术文献出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3789352A1 (en) * 2019-09-04 2021-03-10 Clariant Plastics & Coatings Ltd Process for treatment of wastewater containing phenol, aniline or derivatives thereof
CN113603264A (en) * 2021-08-24 2021-11-05 北京盖雅环境科技有限公司 Method for treating wastewater in DNS acid reduction section

Similar Documents

Publication Publication Date Title
Su et al. Effect of operating parameters on decolorization and COD removal of three reactive dyes by Fenton's reagent using fluidized-bed reactor
Lee et al. Decolorization and toxicity of reactive anthraquinone textile dyes under methanogenic conditions
CN101412571B (en) Technique for reclaiming waste water of azoic dye production
CN103755097B (en) Advanced oxidation-biological treatment device for non-biodegradable waste water
CN102078807B (en) Er<3+>:YAlO3/TiO2-loaded photocatalyst and preparation method thereof
Thanekar et al. Degradation of benzene present in wastewater using hydrodynamic cavitation in combination with air
CN102516195B (en) Production method of 6-nitro-1,2,4-sulfonic acid
CN102161526B (en) Application of magnesium oxide-loaded ferrocobalt metal magnetic nanometer material on degrading orange colour II in wastewater
CN100436346C (en) Multiple phase catalytic oxidation-coagulation precipitation method for processing active dye printing waste water
CN102050535A (en) Processing method for resource recovery of acidic dye waste water
US20140291256A1 (en) Method for treatment of dyeing wastewater by using uv/acetylacetone oxidation process
CN108892270A (en) A method of amino benzene analog waste water is handled using tubular reactor
CN204689706U (en) A kind of Multistage external circulating formula ozone contact reaction device
CN102407128B (en) Preparation method and application of Gd, Pr or Yb doped fenton catalyst
CN103641274B (en) Technology for processing dye wastewater by combining advanced oxidation technology with biofilm process
CN205442755U (en) A fragrant iron ion follows device that ring method handled organic waste water
CN102757153B (en) Method for treating wastewater generated during production of 12-hydroxy stearic acid
CN102863071B (en) Advanced treatment method for decolorizing yeast wastewater
CN114014431A (en) Fenton catalyst regeneration recycling method
CN103272614A (en) Special palladium catalyst for sewage treatment and application thereof
CN103771656B (en) A kind of process for reclaiming of refinery water
CN101863524A (en) Photocatalytic oxidation degradation method of wastewater containing dye
CN104876397B (en) A kind of method processing weak acid blue AS waste water in dye production
CN109912007B (en) Degradation method and degradation system for organic wastewater
CN113663737A (en) CMC-Fe-based microsphere and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20181127

RJ01 Rejection of invention patent application after publication