CN103304430A - Process for recovering organic amine from catalyst production wastewater - Google Patents
Process for recovering organic amine from catalyst production wastewater Download PDFInfo
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- CN103304430A CN103304430A CN201310279555XA CN201310279555A CN103304430A CN 103304430 A CN103304430 A CN 103304430A CN 201310279555X A CN201310279555X A CN 201310279555XA CN 201310279555 A CN201310279555 A CN 201310279555A CN 103304430 A CN103304430 A CN 103304430A
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Abstract
The invention discloses a process for recovering organic amine from catalyst production wastewater. The process comprises the following steps: 1, recovering catalyst in wastewater, and intercepting fewer particle molecular sieves in the wastewater by using a microstrainer; 2, adsorbing the organic amine in the wastewater by using a cationic resin through an organic amine adsorption process, and regenerating organic amine salt by using acid; 3, reducing the organic amine salt into organic amine through anion resin exchange, taking the reduced organic amine as production materials for recycling, and regenerating the anion exchange resin by using NaOH.
Description
Technical field
The present invention relates to chemical technology field, is a kind of organic amine technique that reclaims from catalyst production waste water.
Background technology
Organic amine waste water belongs to poisonous and harmful, the high nitrogen low-carbon type waste water of difficult for biological degradation, from waste water, reclaim organic amine many favourable parts are arranged, reclaim the content that technique can significantly reduce COD in the waste water by organic amine, reduce biochemical toxicity, reduce the ammonia nitrogen that produces in the anaerobic process, make that to reclaim behind the organic amine the follow-up biological process of waste water smooth.
Certain extraordinary Catalyst Production process uses TPAOH (this technique reclaims the main component of organic amine) as template and the alkali source of molecular sieve, because it is expensive, reclaiming TPAOH from waste water just has very strong economy.
If this extraordinary containing wastewater from catalyst carries out biochemical treatment after adopting other special methods to process (such as catalyzed oxidation) again, although feasible process, processing cost is higher, and can not reclaim the organic amine product such as expensive TPAOH.
The organic amine products such as the recyclable TPAOH of technical process of the present invention have advantages of that production cost is low, the rate of recovery is high.When the TPAOH that reclaims, contained a small amount of triethylamine can be recovered simultaneously in the waste water, and the organic amine of recovery can return production system and use as raw materials for production.
Summary of the invention
The present invention is a kind of organic amine technique that reclaims from catalyst production waste water, comprises catalyst recovery in the waste water, organic amine absorbing process and organic amine reducing process.
1, catalyst recovery adopts following methods in the waste water: contain a small amount of particulate molecular sieve in the organic amine waste water, with reclaiming after the micro-strainer interception.
2, the organic amine absorbing process may further comprise the steps:
(1) when using first, resin cation (R.C.) is filled in the cationic exchange coloum, is replaced as after the R-H attitude stand-by with hydrochloric acid or sulphuric acid soln;
(2) clear liquid after organic amine waste water filters by micro-strainer enters three (or more than three) cationic exchange coloums successively, at the wastewater outlet pipeline online electricity being housed leads, PH and COD analyser are controlled water inlet and are stopped to move into water by the controlling valu of setting three parameters;
(3) reach in (2) after the set(ting)value when effluent index, stop into water.Water drains by blow-off pipe in the exchange column, and liquid effluent uses as waste water.Afterwards, exchange column begins to carry out next step regenerative operation;
(4) acid regeneration liquid is entered by last exchange column, and the reverse direction with adsorption process enters successively, discharges from the outlet of acid regeneration liquid;
(5) the acid regeneration process is equipped with online PH meter, conductivity meter, COD analyser at acid regeneration liquid outlet conduit, controls the water inlet of acid regeneration liquid and stops to move into water by the controlling valu of setting three parameters;
(6) reach in (5) after the set(ting)value when acid regeneration liquid effluent index, stop into water.Open wash water valve, allow acid solution drains in the exchange column, liquid effluent uses as acid regeneration liquid;
(7) after acid regeneration was finished, waste water reentered, and repeated by 2 ~ 6 processes.
Organic ammonium (M in the above-mentioned waste water
1, M
2) adsorption process with as follows with resolving and the acid regeneration procedural representation of organic amine salt form:
Absorption: R-H+M
1OH(M
2OH) → R-M
1(M
2)+H
2O
Resolve, regenerate: R-M
1(M
2)+HCl → R-H+M
1Cl(M
2Cl).
3, the reducing process of organic amine may further comprise the steps:
(1) when using first, resin anion(R.A) is filled in the anion-exchange column, is replaced as after the R-OH attitude stand-by with NaOH solution;
(2) the organic amine salt clear liquid that resolve, regeneration produces enters three (or more than three) anion-exchange columns successively, at the By Amine Solutions outlet conduit online electricity being housed leads, PH and COD analyser are controlled the water inlet of organic amine salt clear liquid and are stopped to move into water by the controlling valu of setting three parameters;
(3) organic amine of the clear liquid of anion-exchange column output for reclaiming;
(4) reach in (2) after the set(ting)value when By Amine Solutions outlet effluent index, stop into water.Water drains by blow-off pipe in the exchange column, and liquid effluent uses as machine amine salt clear liquid.Afterwards, exchange column begins to carry out next step regenerative operation;
(5) alkaline regeneration solution is entered by last exchange column, and the reverse direction with adsorption process enters successively, discharges from the alkaline regeneration solution outlet;
(6) the alkali regenerative process is equipped with online PH meter, conductivity meter, COD analyser at the alkaline regeneration solution outlet conduit, controls the alkaline regeneration solution water inlet and stops to move into water by the controlling valu of setting three parameters;
(7) reach in (5) after the set(ting)value when the alkaline regeneration solution effluent index, stop the alkaline regeneration solution water inlet.Open wash water valve, allow alkaline regeneration solution drains in the exchange column, liquid effluent uses as alkaline regeneration solution;
(8) after alkali regeneration was finished, the organic amine salt clear liquid reentered, and repeats by (2) ~ (7) process.
Organic amine salt in the above-mentioned waste water is reduced into the organic amine process and the alkali regenerative process is expressed as follows:
Absorption: R-OH+M
1CL (M
2CL) → R-CL+M
1OH (M
2OH)
Parsing, alkali regeneration: R-CL+OH
-→ R-OH+CL
-
Description of drawings
Accompanying drawing is for reclaiming resin absorption and reclaiming process schema in the organic amine technique.
Embodiment
Embodiment 1:
Certain extraordinary catalyst production waste water is creamy white, and TSS is 3000mg/L, and pH=11.0 mainly contains TPAOH 35000mg/L, triethylamine 1000mg/L, and other contains a small amount of propyl alcohol, butanols and organic amine degradation production.First this waste water is passed through micro-strainer, reclaim molecular sieve catalyst wherein.Clear liquid is successively by three positively charged ion absorption columns, when the outlet wastewater pH〉after 7.0, electricity is led with COD a hop, and at this, absorption effluent control index is COD≤900mg/L, pH＜7.0, specific conductivity≤1000us/cm.Stop into water after reaching arbitrary index, drain waste water in the system.Then carry out the wash-out of organic amine, the hydrochloric acid soln with 2% is by having adsorbed the resin cation (R.C.) of organic amine, till desorb goes out the water management index when being COD≤1000mg/L.At this moment, resin cation (R.C.) is finished regenerative process, can carry out the absorption of organic amine again.The solution that the hydrochloric acid desorb is got off carries out anionresin by anionite-exchange resin, obtains TPAOH and triethylamine.When water outlet pH=8, stop anionite-exchange resin to be regenerated with sodium hydroxide solution into water.
Embodiment 2:
Certain extraordinary catalyst production waste water is creamy white, and TSS is 2500mg/L, and pH=10.5 mainly contains TPAOH 28000mg/L, triethylamine 800mg/L, and other contains a small amount of propyl alcohol, butanols and organic amine degradation production.First this waste water is passed through micro-strainer, reclaim molecular sieve catalyst wherein.Clear liquid is successively by three positively charged ion absorption columns, and absorption effluent control index is COD≤700mg/L, pH＜7.0, specific conductivity≤800us/cm.When the outlet wastewater pH〉after 7.0, electricity is led with COD a hop, and stop into water this moment, drains waste water in the system.Then carry out the wash-out of organic amine.Sulphuric acid soln with 6% is by the resin cation (R.C.) of absorption organic amine, till desorb goes out the water management index when being COD≤1000mg/L.At this moment, resin cation (R.C.) is finished regenerative process, can carry out the absorption of organic amine again.The solution that the sulfuric acid desorb is got off carries out anionresin by anionite-exchange resin, obtains TPAOH and triethylamine.When water outlet pH=8, stop anionite-exchange resin to be regenerated with sodium hydroxide solution into water.
Claims (6)
1. patent of the present invention discloses a kind of organic amine technique that reclaims from catalyst production waste water, comprising: catalyst recovery in (1) waste water, contain in the waste water and reclaim after a small amount of particulate molecular sieve is tackled through micro-strainer; (2) organic amine absorbing process becomes organic amine salt with resin cation (R.C.) absorption is rear with acid regeneration with organic amine in the waste water, controls the index of Inlet and outlet water by online PH meter, conductivity meter, COD analyser in absorption and resolving; (3) organic amine salt is reduced into organic amine by the resin anion(R.A) exchange, and the organic amine of reduction is as the raw materials for production reuse; The resin anion(R.A) exchange is being adsorbed the index of controlling Inlet and outlet water with resolving by online PH meter, conductivity meter, COD analyser with NaOH regeneration.
2. according to right (1) requirement, contain a small amount of particulate molecular sieve in the organic amine waste water and reclaim by the micro-strainer interception is rear.
3. according to right 1 requirement, resin cation (R.C.) with hydrochloric acid or sulphuric acid soln be exchanged into be filled in the cationic exchange coloum after the R-H attitude stand-by.
4. positive and negative ion-exchange contains three (or more than three) ion exchange columns.
5. at positive and negative ion exchange column outlet conduit online electricity is housed and leads, PH and COD analyser are controlled water inlet and are stopped to move into water by the controlling valu of setting three parameters.
6. the positive and negative ion exchange column stops all water in the exchange column to be drained by blow-off pipe behind water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310279555XA CN103304430A (en) | 2013-07-05 | 2013-07-05 | Process for recovering organic amine from catalyst production wastewater |
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|---|---|---|---|
| CN201310279555XA CN103304430A (en) | 2013-07-05 | 2013-07-05 | Process for recovering organic amine from catalyst production wastewater |
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| CN103304430A true CN103304430A (en) | 2013-09-18 |
Family
ID=49130190
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| CN201310279555XA Pending CN103304430A (en) | 2013-07-05 | 2013-07-05 | Process for recovering organic amine from catalyst production wastewater |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106178591A (en) * | 2015-05-08 | 2016-12-07 | 北京思践通科技发展有限公司 | A kind of method purifying organic amine |
| CN117550737A (en) * | 2023-11-14 | 2024-02-13 | 河南海天环境科技有限公司 | Methylamine recovery process for methylamine production wastewater |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002253931A (en) * | 2001-02-28 | 2002-09-10 | Toray Ind Inc | Method and apparatus for manufacturing regenerated tetraalkylammonium hydroxide |
| CN1935652A (en) * | 2006-10-19 | 2007-03-28 | 华东师范大学 | Method for synthesizing ZSM-5 molecular sieve |
| CN102690206A (en) * | 2011-03-25 | 2012-09-26 | 敏森工程有限公司 | Recovery system and method of tetramethylammonium hydroxide |
| CN103080070A (en) * | 2010-12-28 | 2013-05-01 | 德山株式会社 | Process for producing tetraalkylammonium salt, and process for producing tetraalkylammonium hydroxide using same as raw material |
-
2013
- 2013-07-05 CN CN201310279555XA patent/CN103304430A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002253931A (en) * | 2001-02-28 | 2002-09-10 | Toray Ind Inc | Method and apparatus for manufacturing regenerated tetraalkylammonium hydroxide |
| CN1935652A (en) * | 2006-10-19 | 2007-03-28 | 华东师范大学 | Method for synthesizing ZSM-5 molecular sieve |
| CN103080070A (en) * | 2010-12-28 | 2013-05-01 | 德山株式会社 | Process for producing tetraalkylammonium salt, and process for producing tetraalkylammonium hydroxide using same as raw material |
| CN102690206A (en) * | 2011-03-25 | 2012-09-26 | 敏森工程有限公司 | Recovery system and method of tetramethylammonium hydroxide |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106178591A (en) * | 2015-05-08 | 2016-12-07 | 北京思践通科技发展有限公司 | A kind of method purifying organic amine |
| CN106178591B (en) * | 2015-05-08 | 2019-03-15 | 北京思践通科技发展有限公司 | A method of purification organic amine |
| CN117550737A (en) * | 2023-11-14 | 2024-02-13 | 河南海天环境科技有限公司 | Methylamine recovery process for methylamine production wastewater |
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Application publication date: 20130918 |