CN102060398A - Method for treating dimethylamine waste water by using weakly acidic cation exchange resin - Google Patents
Method for treating dimethylamine waste water by using weakly acidic cation exchange resin Download PDFInfo
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- CN102060398A CN102060398A CN 201010551558 CN201010551558A CN102060398A CN 102060398 A CN102060398 A CN 102060398A CN 201010551558 CN201010551558 CN 201010551558 CN 201010551558 A CN201010551558 A CN 201010551558A CN 102060398 A CN102060398 A CN 102060398A
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Abstract
The invention relates to a method for treating dimethylamine waste water by using weakly acidic cation exchange resin, which comprises the following steps: filtering waste water to remove suspended matters, adsorbing the filtered waste water at ordinary temperature by using weakly acidic cation exchange resin; and after the resin which adsorbs dimethylamine tends to be saturated, eluting the dimethylamine with a phosphoric acid, hydrochloric acid or sulfuric acid solution to regenerate the resin. By using the method, the dimethylamine removal rate in the waste water is higher than 96%, and the waste water can be recycled. After desorption, the dimethylamine forms corresponding dimethylamine salts, and the dimethylamine salts can be recycled or directly discharged into a sewage tank. The method has the advantages of simple technique, reliable technology, low processing cost and no secondary pollution, is convenient to operate, and converts dimethylamine waste water into innocuous substances in deed.
Description
Technical field
The present invention relates to handle in the leatheroid industry method of waste water, particularly adopt weakly acidic cation-exchange resin to handle the method for dimethylamine waste water.
Background technology
Dimethylamine at room temperature is a gas, and the smell of similar ammonia is arranged, and is soluble in water, is dissolved in ethanol and ether, and easy firing has weakly alkaline, generates salt soluble in water with mineral acid.Dimethylamine has strong and stimulating, has unpleasant fish stench when content is low in the waste water, and concentration is higher then can to have the strong impulse effect to eye and respiratory tract.
Dimethylamine (DMA) is most widely used general in the methylamine class material, what have the call is a kind of, be widely used in agricultural chemicals, medicine, organic synthesis, rubber, each industrial circle of leather, and be used to produce plastics, ion exchange resin, catalyzer, additive, lubricated wet goods.At present, the dimethylamine of China nearly 1/3rd is used to produce dimethyl formamide (DMF), when DMF uses as solvent, the general rectification method that adopts reclaims, this moment, it was subjected to thermal hydrolysis to generate dimethylamine and formic acid, therefore can produce the waste water that contains DMA in a large number, according to statistics, the DMA waste water that contains of annual only leather industry discharging just has more than 100,000,000 ton.
What at present, the treatment process of dimethylamine waste water was reported both at home and abroad is less.Because DMA boiling point low (7.4 ℃), the DMA of enterprise waste water majority adopts blow-off method and distillation method both at home and abroad at present.Blow-off method is just transferred to the dimethylamine part desorb in the water in the air the real processing of the dimethylamine of being unrealized; The facility investment of distillation rule is big, energy consumption is high.Also there is document propose to adopt hydrogen peroxide method to handle dimethylamine waste water, but, therefore seeks dimethylamine waste water treatment process efficient, less energy-consumption and have application promise in clinical practice and social effect because of existing working cost height etc. former thereby fail practical application.
In Industrial Wastewater Treatment, ion exchange method can be regenerated because of resin, and it is simple to operate, technical maturity, flow process is short, is widely used in the high purity water preparation at present, is mainly used in aspect wastewater treatment and reclaims heavy metal, precious metal and rare metal, purify toxic substance, remove polar organic matter matter in the waste water such as phenol, acid, amine etc.
Summary of the invention
The present invention is directed to the existing in prior technology deficiency, aim to provide a kind of recyclable DMA and high efficiency resin adsorption method and handle the method for DMA waste water, problem to be solved is the resin of choosing (exchange capacity is big, and the life-span is grown) that can realize the superior performance of adsorbing and adsorbs regeneration after saturated.
For solving above technical problem, this treatment process comprises waste water filtering, resins exchange absorption and resin regeneration, the decolorization filtering of elutriant, and concentrating and complete spray drying unit of elutriant obtains the solid by-product of dimethylamine salt at last.
Dimethylamine generates the organic amine radical ion owing to dissociating in the aqueous solution and hydroxide ion is alkalescence, the ultimate principle of ion exchange method be in waste water the organic amine radical ion when the weakly acidic cation-exchange resin, carry out ion-exchange with tradable hydrogen ion on the resin, the amine radical ion is attracted on the resin in the waste water, and the hydrogen ion on the resin is substituted and gets off to fall into waste water and hydroxide ion water generation reaction, its result makes that the concentration of dimethylamine reduces significantly in the waste water, and waste water is purified.Resin obtains regeneration through desorb after saturated absorption, reuse the pending material that desorb obtains---the recyclable utilization of dimethylamine salt.
Because dimethylamine is polarity in the aqueous solution, therefore ion-exchange can be carried out in Zeo-karb and it, can realize that except strong acidic ion resin the ion-exchange, weakly acidic cation-exchange resin can be realized ion-exchange too, the experiment proved that really so.
The preferred DK110 of described weakly acidic cation-exchange resin, 110/111,724 type weakly acidic cation-exchange resins, with the strong acidic ion resin difference be that their mass exchange capacity is big, approximately be 2.5 times of storng-acid cation exchange resin.
Ion exchange column adopts conventional following current or adverse current continous way fixed bed.Waste water is then looked DMA concentration and resin loadings in the waste water through the flow velocity of switching equipment, is determined by experiment, is generally 2-15m3/h.
Regeneration adopt inorganic acid solution, mineral acid select for use phosphoric acid, hydrochloric acid, sulfuric acid all can, then can obtain different byproducts respectively and own with different mineral acids.(, can only consider that the lower concentration waste liquid of phosphoric acid factory replaces) because of phosphoric acid costs an arm and a leg
Because adopt diluted acid regeneration, so the concentration of elutriant is also lower, directly send the drying installation drying must cause the energy consumption height, present technique still comprises the reverse osmosis membrane technology concentrate eluant that employing is suitable for this reason, send drying installation to be dried to solid by-product again.Select suitable drying installation, can not make the dimethylamine salt be subjected to pyrolytic decomposition, can not allow this salt glue wall (wall built-up) again, through various dried forms relatively after, the drying installation that present technique is selected for use is to adopt the spraying drying suite of equipment.
This treatment process has following characteristics: dimethylamine clearance height＞96%, and technology is simple, and easy handling does not have secondary pollution, and the waste water after the improvement can send the workshop reuse, has really realized the harmless treatment of dimethylamine waste water; Regenerative elution liquid is recycled into byproduct dimethylamine salt.This method can cut down the consumption of energy significantly than existing distillation method, saves cost, has good economic benefits and social benefit.
Utilization about regenerative elution liquid:
1. obtain dimethylamine hydrochloric acid dilute solution with regeneration of hydrochloric acid, should adopt reverse osmosis membrane technology to concentrate in order to save energy consumption, the drying device is dried to solid again after concentrating, and can be used as the raw material of organic synthesis.
2. use the dilute phosphoric acid spent solution regeneration, regenerated liquid makes it form the Magnesium Ammonium Phosphate precipitation with magnesium chloride or sal epsom, and throw out is the Magnesium Ammonium Phosphate compound manure through centrifugation.This fertilizer is insoluble, so can be used as base manure, but this fertilizer appears in the end in the market, introduces to the market to acquire a certain degree of difficulty, and needs department's test such as academy of agricultural sciences and reaches a conclusion.
3. the garden Sewage Plant is sent after unified the processing in the direct blowdown of regenerated liquid pond.
Embodiment
Embodiment 1Absorption
30g 110 type weakly acidic cation-exchange resins are packed in the adsorption column, and (φ 30 * 600mm).With the DMA waste water (800-1000mg/L) under the room temperature, by resin bed, treatment capacity is 11000ml-12000ml with the flow of 5-15ml/min, and after plastic resin treatment, DMA content is lower than 24-30mg/L in the waste water, DMA clearance 96%.
Embodiment 2Absorption
30g 111 type weakly acidic cation-exchange resins are packed in the adsorption column, and (φ 30 * 600mm).With the DMA waste water (800-1000mg/L) under the room temperature, by resin bed, treatment capacity is 11000ml-12000ml with the flow of 5-15ml/min, and after plastic resin treatment, DMA content is lower than 24-30mg/L in the waste water, DMA clearance 96%.
Embodiment 3Absorption
30g DK110 type weakly acidic cation-exchange resin packed in the adsorption column, and (φ 30 * 600mm).With the DMA waste water (800-1000mg/L) under the room temperature, by resin bed, treatment capacity is 8000ml-9000ml with the flow of 20ml/min, and after plastic resin treatment, DMA content is lower than 24-30mg/L in the waste water, DMA clearance 96%.
Embodiment 4Absorption
30g 724 type weakly acidic cation-exchange resins are packed in the adsorption column, and (φ 30 * 600mm).With the DMA waste water (800-1000mg/L) under the room temperature, by resin bed, treatment capacity is 9000ml-10000ml with the flow of 20ml/min, and after plastic resin treatment, DMA content is lower than 24-30mg/L in the waste water, DMA clearance 96%.
Embodiment 5Desorb
Use 100-200ml, dilute sulphuric acid (0.5-4M) at room temperature carries out desorption with the flow following current of 2-10ml/min by adsorbing saturated resin bed, and the DMA eluting rate is more than 95%.Elutriant under the desorb is the dimethylamine vitriol of 2-3M.After resin desorb operation, the DMA rate of recovery＞90%, the reduction of resin absorption capacity is no more than 1%.
Embodiment 6Desorb
At room temperature carry out desorption with the flow following current of 2-10ml/min by absorption saturated resin bed with 100-200mL dilute hydrochloric acid (concentration is 0.5-4M), the DMA eluting rate is more than 95%.Elutriant under the desorb is the dimethylamine hydrochloride of 3-6M.
Claims (4)
1. a weakly acidic cation-exchange resin is handled the method for dimethylamine waste water, comprise waste water filtering, resins exchange absorption and resin regeneration, it is characterized in that: dimethylamine waste water after filtering and weakly acidic cation-exchange resin carry out resins exchange absorption at normal temperatures, when resin becomes saturated mode by ADSORPTION STATE, any with phosphoric acid, hydrochloric acid, sulphuric acid soln, the dimethylamine that wash-out is adsorbed, make resin regeneration, acid solutions is controlled at 0.5%-10%, and elutriant forms corresponding dimethylamine salt respectively.
2. a kind of weakly acidic cation-exchange resin according to claim 1 is handled the method for dimethylamine waste water, and it is characterized in that: the model of described weakly acidic cation-exchange resin is DK110,110/111,724 types.
3. a kind of weakly acidic cation-exchange resin according to claim 1 is handled the method for dimethylamine waste water, it is characterized in that: described elutriant adopts membrane technique to concentrate.
4. according to the method for claim 1 or 3 described a kind of weakly acidic cation-exchange resins processing dimethylamine waste waters, it is characterized in that: the elutriant after concentrating carries out spraying drying again and obtains byproduct dimethylamine salt solid.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260020A (en) * | 2011-05-27 | 2011-11-30 | 河南省科学院化学研究所有限公司 | Deep processing method of leather production biochemical tail water with resin adsorption method |
| CN102674607A (en) * | 2012-05-03 | 2012-09-19 | 江苏健谷化工有限公司 | Method for treating acid wastewater of 2-methyl-4-chlorophenoxyacetic acid through extraction, neutralization and distillation integration |
| CN103224305A (en) * | 2013-05-09 | 2013-07-31 | 浙江东天虹环保工程有限公司 | Treatment method of wastewater containing dimethylamine |
| CN103466838A (en) * | 2013-09-23 | 2013-12-25 | 杭州天创环境科技股份有限公司 | Processing method of rectifying tower condensate of wastewater containing dimethyl formamide |
| CN104176867A (en) * | 2013-05-22 | 2014-12-03 | 北京思践通科技发展有限公司 | Recovery method for amine |
| CN106669657A (en) * | 2016-12-06 | 2017-05-17 | 湖北工业大学 | Method for treating low-concentration ethanediamine wastewater |
| CN106984139A (en) * | 2017-04-25 | 2017-07-28 | 安徽三星树脂科技有限公司 | Anion exchange resin produces the handling process of waste gas |
| CN107572557A (en) * | 2017-08-15 | 2018-01-12 | 南京大学盐城环保技术与工程研究院 | Salt slag refined highly effective combined depth processing method |
| CN108069844A (en) * | 2016-11-10 | 2018-05-25 | 浙江新和成特种材料有限公司 | The process for purification of acetone solvent used and its application in a kind of polyphenylene sulfide manufacture |
| CN108276293A (en) * | 2017-01-06 | 2018-07-13 | 上海凯赛生物技术研发中心有限公司 | A kind of separation method of 1,5- pentanediamines |
| CN109052741A (en) * | 2016-01-19 | 2018-12-21 | 青岛大学 | A kind of synchronous decoloration of printing waste water and nitrogen recovery and treatment method |
| CN112811670A (en) * | 2021-01-29 | 2021-05-18 | 浙江金潮实业有限公司 | Oily synthetic leather wastewater treatment and recovery system and method |
Citations (1)
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| CN101337707A (en) * | 2008-08-08 | 2009-01-07 | 合肥工业大学 | Method for processing dimethylamine waste water by ion-exchange method |
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2010
- 2010-11-12 CN CN 201010551558 patent/CN102060398A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101337707A (en) * | 2008-08-08 | 2009-01-07 | 合肥工业大学 | Method for processing dimethylamine waste water by ion-exchange method |
Non-Patent Citations (1)
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| 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 20091115 潘高峰 合成革工业废水中低浓度二甲胺的分离研究 第B027-400页，第4.1.1、4.1.3.4、4.1.3.5、4.2.2.5、4.2.4.1、4.2.4.2、4.2.5节 1-4 , 第11期 2 * |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260020A (en) * | 2011-05-27 | 2011-11-30 | 河南省科学院化学研究所有限公司 | Deep processing method of leather production biochemical tail water with resin adsorption method |
| CN102674607A (en) * | 2012-05-03 | 2012-09-19 | 江苏健谷化工有限公司 | Method for treating acid wastewater of 2-methyl-4-chlorophenoxyacetic acid through extraction, neutralization and distillation integration |
| CN103224305A (en) * | 2013-05-09 | 2013-07-31 | 浙江东天虹环保工程有限公司 | Treatment method of wastewater containing dimethylamine |
| CN103224305B (en) * | 2013-05-09 | 2014-12-03 | 浙江东天虹环保工程有限公司 | Treatment method of wastewater containing dimethylamine |
| CN104176867A (en) * | 2013-05-22 | 2014-12-03 | 北京思践通科技发展有限公司 | Recovery method for amine |
| CN103466838A (en) * | 2013-09-23 | 2013-12-25 | 杭州天创环境科技股份有限公司 | Processing method of rectifying tower condensate of wastewater containing dimethyl formamide |
| CN103466838B (en) * | 2013-09-23 | 2015-05-27 | 杭州天创环境科技股份有限公司 | Processing method of rectifying tower condensate of wastewater containing dimethyl formamide |
| CN109052741A (en) * | 2016-01-19 | 2018-12-21 | 青岛大学 | A kind of synchronous decoloration of printing waste water and nitrogen recovery and treatment method |
| CN109052742A (en) * | 2016-01-19 | 2018-12-21 | 青岛大学 | A kind of decoloration of printing waste water and nitrogen recovery method |
| CN109052741B (en) * | 2016-01-19 | 2021-08-03 | 青岛大学 | Synchronous decoloring and nitrogen recovery treatment method for printing wastewater |
| CN109052742B (en) * | 2016-01-19 | 2021-08-03 | 青岛大学 | Method for decoloring printing wastewater and recovering nitrogen |
| CN108069844A (en) * | 2016-11-10 | 2018-05-25 | 浙江新和成特种材料有限公司 | The process for purification of acetone solvent used and its application in a kind of polyphenylene sulfide manufacture |
| CN108069844B (en) * | 2016-11-10 | 2021-03-16 | 浙江新和成特种材料有限公司 | Method for refining acetone solvent used in polyphenylene sulfide production and application thereof |
| CN106669657A (en) * | 2016-12-06 | 2017-05-17 | 湖北工业大学 | Method for treating low-concentration ethanediamine wastewater |
| CN108276293A (en) * | 2017-01-06 | 2018-07-13 | 上海凯赛生物技术研发中心有限公司 | A kind of separation method of 1,5- pentanediamines |
| CN106984139A (en) * | 2017-04-25 | 2017-07-28 | 安徽三星树脂科技有限公司 | Anion exchange resin produces the handling process of waste gas |
| CN107572557A (en) * | 2017-08-15 | 2018-01-12 | 南京大学盐城环保技术与工程研究院 | Salt slag refined highly effective combined depth processing method |
| CN112811670A (en) * | 2021-01-29 | 2021-05-18 | 浙江金潮实业有限公司 | Oily synthetic leather wastewater treatment and recovery system and method |
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Application publication date: 20110518 |