CN102746139B - Method for recycling dibasic acid byproducts from adipic acid waste liquor - Google Patents
Method for recycling dibasic acid byproducts from adipic acid waste liquor Download PDFInfo
- Publication number
- CN102746139B CN102746139B CN201210246992.7A CN201210246992A CN102746139B CN 102746139 B CN102746139 B CN 102746139B CN 201210246992 A CN201210246992 A CN 201210246992A CN 102746139 B CN102746139 B CN 102746139B
- Authority
- CN
- China
- Prior art keywords
- film evaporator
- climbing
- acid
- falling
- nitric acid
- 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.)
- Active
Links
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention relates to a method for recycling dibasic acid byproducts from adipic acid waste liquor, which comprises steps as follows: dibasic acid waste liquor is preheated by a preheater and enters a climbing film evaporator; the concentrated solution from the climbing film evaporator naturally flows to a falling film evaporator; the discharged material from the bottom of the falling film evaporator is in a molten state; after a seal tank is subjected to vacuum isolation, a safe evaporating tank is operated under normal pressure; and the liquor naturally flows to the safe evaporating tank to be buffered, and enters a flaker to form flakes, thereby obtaining the dibasic acid flake byproducts. Compared with the prior art, the invention enhances the evaporization efficiency, lowers the steam consumption, implements continuous operation of evaporative concentration of adipic acid waste liquor, implements continuous discharge to avoid the possibility of explosion due to overpressure of equipment, ensures the discharge requirement for water content and the stable operation of the flaker, can adapt to great incoming material fluctuation or steam pipe network fluctuation, reasonably utilizes the energy, and lowers the comprehensive energy consumption of the products.
Description
Technical field
The present invention is to extracting the method for diprotic acid byproduct in hexane diacid preparation waste liquid.
Background technology
Hexanodioic acid is to make catalyzer with copper and vanadium, with the reaction of nitric acid oxidation hexalin, generates.In hexanodioic acid is produced, in the waste liquid of generation (DBA waste liquid), contain hexanodioic acid, succinic acid, pentanedioic acid, water and nitric acid.The method of extracting diprotic acid byproduct reclaims hexanodioic acid, succinic acid and pentanedioic acid exactly from mixed waste liquor.
At present from hexanodioic acid waste liquid, reclaim the method for hexanodioic acid, succinic acid, pentanedioic acid, have the intermittently method of evaporating pot method and two climbing-film evaporator serial operations.
But the problem that these two kinds of methods exist has:
1. the vaporization efficiency of evaporating pot is low, and steam consumption is large.
2. evaporating pot vacuum operating needs vacuum breaker before discharge, otherwise cannot blanking, and in vacuum breaker process, because evaporating pot is still used steam heating, easily occurs the phenomenon of evaporating pot superpressure, and rupture disk need to be set.
3. evaporating pot periodical operation, need to establish a plurality of evaporating pots, and feed liquid concentrating degree rule of thumb judges, easily occurs the underproof situation of feed liquid water content, causes the flaker feed liquid of cannot condensing, and the disqualification rate of product is higher.
4. the nitric acid vapor evaporating need to be used circulating water condensing, and energy consumption is large.
5. the flow process of two climbing-film evaporator serial operations generally can not reach the evaporation requirement of diprotic acid water content≤2%, and vaporization efficiency is low, and steam consumption is large.
Summary of the invention
The object of the invention is to improve the treatment process of hexanodioic acid waste liquid, improve vaporization efficiency, reduce energy consumption, solve the problem that blanking needs vacuum breaker, make the evaporation concentration can operate continuously.
Technical scheme of the present invention is as follows:
A kind of method that reclaims diprotic acid byproduct from hexanodioic acid waste liquid, its step is as follows: diprotic acid waste liquid enters climbing-film evaporator after preheater preheating, concentrated solution after climbing-film evaporator is from flowing to falling-film evaporator, falling-film evaporator bottom discharge is molten state, after sealed can cuts off vacuum, the evaporating pot atmospheric operation that makes to ensure public security, flow to security personnel's evaporating pot buffering certainly, then enters flaker knot sheet and obtains diprotic acid section byproduct.
Further, falling-film evaporator is at-50 ~-70kPaA negative-pressure operation, preferably-70kPaA.The heating of employing middle pressure steam, controls the drop temperature of falling-film evaporator at 145 ~ 185 ℃, and preferably 145 ~ 165 ℃, according to equilibrium partial pressure, falling-film evaporator bottom discharge moisture content is down to below 2%.
Further, security personnel's evaporating pot is provided with two, as security device, in steam pipe system fluctuation or evaporation feed liquor fluctuation situation, if drop temperature does not reach 145 ~ 185 ℃, can improve the residence time of feed liquid in evaporating pot, the feed liquid water content that assurance enters flaker is qualified.If drop temperature deviation is larger, can switch to an other evaporating pot, adopt the pattern of periodical operation, after feed liquid water content in tank to be evaporated is up to standard, deliver to again flaker knot sheet, guaranteed the continuous production of device.If operation is normal, evaporating pot, only as surge tank, has been realized the concentrated operate continuously of hexanodioic acid waste liquid evaporation.Security personnel's evaporating pot, with vapor pipe, enters the airing system of adipic acid plant after the nitric acid vapor in condenser condenses exhaust, and evaporating pot can be realized continuous pulp discharge, does not need vacuum breaker, and there will not be superpressure explosion phenomenon.
Further, the nitric acid concentration tower that the nitric acid vapor evaporating is delivered to adipic acid plant reclaims nitric acid.Because the temperature of steam is higher, deliver to nitric acid concentration tower and can be used as thermal source, reduce the steam consumption of nitric acid concentration tower reboiler, nitric acid vapor need not be used circulating water condensing simultaneously, reduces recirculated water consumption, has reduced adipic acid plant energy consumption of unit product.
Further, in a kind of method that reclaims diprotic acid byproduct from hexanodioic acid waste liquid of the present invention, diprotic acid retrieving arrangement designs independently vacuum unit as standby, be that climbing-film evaporator and falling-film evaporator are also connected with independently vacuum unit afterwards, when adipic acid plant nitric acid concentration tower fluctuation of service, can switch to independently vacuum unit, guarantee the steady running of diprotic acid upgrading unit.After vacuum unit, be connected with nitric acid lime set tank and nitric acid lime set pump in turn, nitric acid liquid is collected to nitric acid lime set tank, by nitric acid lime set pump, entered in adipic acid plant and again utilized production hexanodioic acid, recover materials has been carried out recycle fully again.
Advantage of the present invention:
Advantage and positively effect that compared with the prior art the present invention had are:
1. adopt climbing-film evaporator and falling-film evaporator serial operation, the vaporization efficiency that rises film and falling-film evaporator is all much higher compared with evaporating pot, has improved vaporization efficiency, has reduced steam consumption.
2. adopt climbing-film evaporator and falling-film evaporator serial operation, realize the concentrated operate continuously of hexanodioic acid waste liquid evaporation.
3. the evaporating pot atmospheric operation of ensuring public security, realizes continuous pulp discharge, avoids the possibility of equipment superpressure blast.
4. by controlling falling-film evaporator drop temperature, guarantee the requirement of discharging water content, guarantee the stable operation of flaker.
5. security personnel's evaporating pot is set, makes device operator scheme flexible, can adapt to larger supplied materials fluctuation or steam pipe system fluctuation.
6. the nitric acid vapor evaporating is delivered to adipic acid plant nitric acid concentration tower and is reclaimed nitric acid, rationally utilizes energy, reduces product comprehensive energy consumption.
Accompanying drawing explanation
Fig. 1 is a kind of process flow diagram that reclaims the method for diprotic acid byproduct from hexanodioic acid waste liquid of the present invention.
In figure:
1, preheater 2, climbing-film evaporator 3, falling-film evaporator 4, cyclonic separator
5, nitric acid concentration tower 6, sealed can 7, security personnel's evaporating pot 8, flaker
9, vacuum unit 10, adipic acid plant airing system 11, adipic acid plant 12, nitric acid lime set tank
13, nitric acid lime set pump
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but do not limit protection scope of the present invention.
Embodiment 1
From hexanodioic acid waste liquid, reclaim a method for diprotic acid byproduct, hexanodioic acid DBA waste liquid is delivered to preheater 1 use steam condensate through transferpump and is heated to 75 ℃, then enters climbing-film evaporator 2 evaporation concentration.Climbing-film evaporator 2 temperature outs are controlled at 90 ℃, at-20 ~-40kPa A negative-pressure operation.Together with the steam of discharging with falling-film evaporator 3 tops after the drop that the steam that discharge at climbing-film evaporator 2 tops is carried secretly through cyclonic separator 4 separation, send into nitric acid concentration tower 5 and reclaim nitric acid.In climbing-film evaporator 2 dischargings, moisture content is down to 40% left and right, certainly flow to the further evaporation concentration of falling-film evaporator 3.Falling-film evaporator 3, in-70kPaA operation, adopts middle pressure steam heating, controls bottom discharge temperature at 160 ℃.Falling-film evaporator bottom discharge moisture content is down to 2% left and right, is molten state, through sealed can 6, cuts off after vacuum, certainly flow to a buffering in two security personnel's evaporating pots 7, then enters flaker 8 knot sheets and obtains diprotic acid section byproduct.If there is fluctuation in the discharging moisture content of falling-film evaporator 3, can not meet the requirement of knot sheet, can adjust the residence time of feed liquid in security personnel's evaporating pot, to guarantee that discharging moisture content is no more than 2%.In the time of necessary, can switch to other security personnel's evaporating pot, adopt andnon-continuous operation manner.Security personnel's evaporating pot 7, with vapor pipe, enters adipic acid plant airing system 10 after the nitric acid vapor in condenser condenses exhaust, and security personnel's evaporating pot 7 can be realized continuous pulp discharge, does not need vacuum breaker, and there will not be superpressure explosion phenomenon.
After climbing-film evaporator 2 and falling-film evaporator 3, be also connected with independently vacuum unit 9, when adipic acid plant nitric acid concentration tower fluctuation of service, can switch to independently vacuum unit 9, guarantee the steady running of diprotic acid upgrading unit.After vacuum unit 9, be connected with nitric acid lime set tank 12 and nitric acid lime set pump 13 in turn, nitric acid liquid is collected to nitric acid lime set tank 12, by nitric acid lime set pump 13, entered in adipic acid plant 11 and again utilized production hexanodioic acid, recover materials has been carried out recycle fully again.
A kind of method that reclaims diprotic acid byproduct from hexanodioic acid waste liquid of the present invention, compared to general evaporating pot method at intermittence, saves energy consumption and reaches 40% ~ 50%; Compared to the method for two climbing-film evaporator serial operations, adopt method of the present invention, material evaporation below 2%, improved the quality of product, and the method ordinary material water content of two joint climbing-film evaporator serial operations is in 20% can left and right to water content.
Claims (1)
1. from hexanodioic acid waste liquid, reclaim a method for diprotic acid byproduct, it is characterized in that: step is as follows:
Diprotic acid waste liquid enters climbing-film evaporator after preheater is preheated to 75 ℃, and climbing-film evaporator temperature out is controlled at 90 ℃, at-20～-40kPa A negative-pressure operation; Concentrated solution moisture content after climbing-film evaporator is down to 40%, from flowing to falling-film evaporator, falling-film evaporator is in-70kPaA operation, the heating of employing middle pressure steam, controls bottom discharge temperature at 160 ℃, and falling-film evaporator bottom discharge is molten state, after sealed can cuts off vacuum, the evaporating pot atmospheric operation that makes to ensure public security, flow to security personnel's evaporating pot buffering certainly, then enters flaker knot sheet and obtains diprotic acid section byproduct;
Described falling-film evaporator bottom discharge moisture content is down to below 2%;
Described security personnel's evaporating pot is provided with two, and security personnel's evaporating pot is with vapor pipe;
The nitric acid concentration tower that the nitric acid vapor evaporating from climbing-film evaporator is delivered to adipic acid plant reclaims nitric acid;
After described climbing-film evaporator and falling-film evaporator, be also connected with independently vacuum unit.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210246992.7A CN102746139B (en) | 2012-07-17 | 2012-07-17 | Method for recycling dibasic acid byproducts from adipic acid waste liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210246992.7A CN102746139B (en) | 2012-07-17 | 2012-07-17 | Method for recycling dibasic acid byproducts from adipic acid waste liquor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102746139A CN102746139A (en) | 2012-10-24 |
| CN102746139B true CN102746139B (en) | 2014-11-05 |
Family
ID=47026699
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210246992.7A Active CN102746139B (en) | 2012-07-17 | 2012-07-17 | Method for recycling dibasic acid byproducts from adipic acid waste liquor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102746139B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105923673A (en) * | 2016-05-23 | 2016-09-07 | 江苏瑞升华能源科技有限公司 | Adipic acid waste water evaporation and concentration process and device thereof |
| CN105906122A (en) * | 2016-05-23 | 2016-08-31 | 江苏瑞升华能源科技有限公司 | Treatment technology of high-organic matter high-salt wastewater and treatment device thereof |
| CN112457186B (en) * | 2020-11-25 | 2021-09-14 | 重庆华峰化工有限公司 | Device and method for separating and recovering dibasic acid and catalyst in adipic acid production |
| CN112439216A (en) * | 2020-12-14 | 2021-03-05 | 河南久圣化工有限公司 | Tertiary evaporation system for recovering dicarboxylic acid from adipic acid waste liquid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362607A (en) * | 2008-08-12 | 2009-02-11 | 山东洪业化工集团有限公司 | Process for treating waste water from hexane diacid production system |
| CN102211992A (en) * | 2011-04-18 | 2011-10-12 | 湖南百利工程科技有限公司 | Process for reclaiming dibasic acid from adipic acid production waste solution |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5908589A (en) * | 1997-12-08 | 1999-06-01 | Twenty-First Century Research Corporation | Methods for separating catalyst from oxidation mixtures containing dibasic acids |
-
2012
- 2012-07-17 CN CN201210246992.7A patent/CN102746139B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362607A (en) * | 2008-08-12 | 2009-02-11 | 山东洪业化工集团有限公司 | Process for treating waste water from hexane diacid production system |
| CN102211992A (en) * | 2011-04-18 | 2011-10-12 | 湖南百利工程科技有限公司 | Process for reclaiming dibasic acid from adipic acid production waste solution |
Non-Patent Citations (2)
| Title |
|---|
| 双效升降膜蒸发器的设计使用;方鸿元;《医药设计》;19841231(第6期);说明书第6页左栏倒数第3段 * |
| 方鸿元.双效升降膜蒸发器的设计使用.《医药设计》.1984,(第6期),说明书第6页左栏倒数第3段. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102746139A (en) | 2012-10-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102211992B (en) | Process for reclaiming dibasic acid from adipic acid production waste solution | |
| CN102746139B (en) | Method for recycling dibasic acid byproducts from adipic acid waste liquor | |
| CN109232352B (en) | N-methyl pyrrolidone decompression purification system and purification method | |
| CN107286022A (en) | The method and device of dimethylamine is extracted in a kind of high kjeldahl nitrogen waste water from Sucralose | |
| CN109776482A (en) | The method of the continuous preparation high-purity lactide of industrialization | |
| CN103215135A (en) | Method for synchronously extracting sage clary essential oil and sclareol from sage clary | |
| CN201244371Y (en) | Climbing film vaporising device | |
| CN104130105B (en) | The method that in D-4-methylsulfonylphserine serine ethyl ester production, ethanol is recycled | |
| CN105315132A (en) | System and method used for energy utilization between ethylene glycol device dehydrating tower and refining tower | |
| CN109231635B (en) | Wastewater treatment process | |
| CN105396315A (en) | Ethyl vanillin rectification device | |
| CN203677978U (en) | Vapor-compression type alcohol recovery tower | |
| CN104447216B (en) | A kind of beta naphthal continuous rectificating technique | |
| CN205115421U (en) | High -efficient extraction device that retrieves of plant extract fragrance | |
| CN103086854A (en) | Method and device for reducing methanol content in formaldehyde process by silver method | |
| CN104844444A (en) | Method for extracting acetic acid in salt-containing acetic acid aqueous solution by one-sided line heat integration azeotropic rectification method | |
| CN110294665A (en) | The recyclable device and recovery method of ethyl alcohol in Doxycycline Hyclate refinement mother liquor | |
| CN109467497A (en) | A kind of recovery process and device of polyvinyl alcohol alcohol hydrolysis mother liquor | |
| CN213077530U (en) | Isopropyl alcohol dewatering equipment | |
| CN211284206U (en) | Caprolactam purification device in 6-aminocapronitrile preparation process | |
| CN113813625A (en) | Device and method for recovering light alcohol by combining MVR with recovery tower | |
| CN106744720A (en) | The circulation recycling system and its operation process of trichloroacetaldehyde by-product dilute sulfuric acid | |
| CN113563188A (en) | Method for recovering vinyl acetate from vinyl acetate waste liquid | |
| CN208166892U (en) | A kind of cyanoacetate or malonate recyclable device | |
| CN206337191U (en) | A kind of continuous device for extracting medical grade propylene glycol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |