CN1073536C - Technology for recovering organic mass in naphthalene series dye intermediate waste mother liquor by trialkylamine - Google Patents
Technology for recovering organic mass in naphthalene series dye intermediate waste mother liquor by trialkylamine Download PDFInfo
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- CN1073536C CN1073536C CN96100469A CN96100469A CN1073536C CN 1073536 C CN1073536 C CN 1073536C CN 96100469 A CN96100469 A CN 96100469A CN 96100469 A CN96100469 A CN 96100469A CN 1073536 C CN1073536 C CN 1073536C
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Abstract
The present invention relates to novel technology for extracting and recovering organic substances in waste mother liquid of naphthalene dye intermediate bodies by utilizing trialkyl amine. Waste mother liquid of naphthalene dye intermediate bodies contains characteristic genes of sulfonic acid. The technology comprises: trialkyl amine diluted by coal oil is adopted as extracting agents to extract waste mother liquid at 20 to 50 DEG C for 5 to 10 minutes, and then, the waste mother liquid is separated; the separated organic phase is reversely extracted by NaOH solution at 15 to 50 DEG C for 5 to 10 minutes, the reverse extraction system is separated, and the separated water phase is the product of the present invention. The technology of the present invention is used in the production process of dye intermediate bodies or is used for producing novel dye intermediate bodies.
Description
The present invention relates to a kind of with trialkyl tertiary amine (trade(brand)name N
235, also claim trialkylamine) extract and reclaim organic method in the naphthalene series dye intermediate waste liquor, belong to chemical technology field.
Along with developing rapidly of China's dyestuffs industries, also brought the severe contamination of water surrounding, formed small-sized dye chemical industry factory river of pollution or the phreatic serious situation of big area.According to nineteen ninety statistics, national waste water from dyestuff total release was 1.57 billion cubic meter/years, and the improvement rate only is 22.5%, and improvement qualification rate only 42%.As seen, administering good colourant waste water is the extremely urgent task of China.
Dying industrial wastewater belongs to one of organic industrial sewage of utmost point refractory reason owing to concentration height, dark, the supersalinity of colourity.Particularly dyestuff intermediate is produced waste liquid, adopts conventional water treatment method to be difficult to reach the ideal treatment effect, and the processing costs costliness, and enterprise often is difficult to bear.In " eight or five " tackling of key scientific and technical problems problem, set up dying industrial wastewater comprehensive regulation special topic, purpose is at polluting the most serious several naphthalene series dye intermediate waste liquids, emphasis is explored effective resource utilization----process for comprehensively treating, for control China industrial wastewater pollution is opened up a brand-new approach.
Extraction process is a component separation method commonly used in Chemical Manufacture and the hydrometallurgy, in the world the use experience of existing decades.The mixer-settler liquid-liquid extraction reextraction equipment of using in this technology is a kind of classification counter current contact formula extraction equipment, is standard equipment in industrial application.
Trialkylamine (N235) is a kind of homemade tertiary amine extraction agent commonly used, contain 90%～95% tertiary amine and a spot of substituted amide, it is a kind of flaxen liquid, non-ferrous metal metallurgy be widely used during rare earth element separates, but be used for the organic waste water resource utilization and comprehensive treating process is still rare.
The objective of the invention is to utilize existing mixer-settler liquid-liquid extraction reextraction equipment and existing trialkylamine (trialkyl tertiary amine) extraction agent, extract the organic matter that reclaims in the naphthalene series dye intermediate, to improve the pollution of China's trade effluent.
The present invention reclaims method organic in the naphthalene series dye intermediate with the extraction of trialkyl tertiary amine, comprises following each step:
(1) with kerosene dilution extraction agent trialkyl tertiary amine (trade(brand)name N235 claims trialkylamine again), Dilution ratio is a kerosene: trialkyl tertiary amine=1: 0.2～0.5.
(2) the trialkyl tertiary amine-kerosene after the usefulness dilution is as extraction agent, add in TOBIAS ACID 97MIN.﹠ 98MIN., J acid and the H acid dye intermediate production waste liquor and extract, the pH value of waste liquor is 1.0～1.5, extraction is in a ratio of extraction agent: waste liquor=1: 1～4.5, reaction times is 5～10 minutes, 20～50 ℃ of temperature of reaction;
(3) above-mentioned extraction system is introduced in the mixer-settler, the water of extraction system is separated with organic phase, disengaging time is 20～30 minutes, and the water after the separation is as discharge of wastewater, and organic phase is used for stripping;
(4) with concentration be 24% NaOH solution as strippant, above-mentioned isolated organic phase of the 3rd step is stripped in mixer-settler, stripping is in a ratio of strippant: organic phase=1: 3, back-extraction time 10 minutes, 25 ℃ of reextraction temperature:
(5) above-mentioned reextraction system is introduced in the mixer-settler, water in the reextraction system is separated with organic phase, disengaging time is 20～30 minutes, water after the separation is the organic matter after the waste liquid camber concentrates, return the raw materials for production of making dyestuff, or being used to produce new dyestuff intermediate, organic phase is the trialkylamine and the kerosene of living again, and recycles as extraction agent.
The method of the present invention's design under optimum process condition, is utilized trialkyl tertiary amine-kerosene-H
2SO
4(HCl)-the NaOH extracting-back extraction gets system, dyestuff intermediate useful in the dyestuff intermediate waste liquor can be separated and be used.Studies have shown that, can reclaim in the waste liquid 90～95% dyestuff intermediate, regenerant can directly return production system, can improve product yield and reach 10～30%, make the CODCr value in the waste water be reduced to 1 simultaneously, below the 000mg/l, colourity reduces more than 90%, and can make salinity wherein be back to production technique.
The present invention has obtained the optimum process parameter by repetitious static state and dynamic experiment, during existing five typical embodiment that incite somebody to action wherein are listed in the table below:
Table 1
| The waste liquor title | Thinning ratio (%) | O/A extraction phase ratio | Temperature of reaction ℃ | Department during reaction (min) | Disengaging time (min | Back extraction concentration of lye (%) | Back extraction is compared | Back extraction time m | Back extraction temperature ℃ | Disengaging time (min) | Product yield (% |
| TOBIAS ACID 97MIN.﹠ 98MIN. is useless | 0 | 1/4.5 | 45 | 10 | 25 | 24 | 1/3 | 10 | 25 | 20 | 95 |
| TOBIAS ACID 97MIN.﹠ 98MIN. is useless | 0 | 1/4.5 | 30 | 10 | 25 | 24 | 1/3 | 10 | 25 | 30 | 94 |
| J acid waste water | 20 | 1/2.5 | 40 | 6 | 25 | 24 | 1/3 | 10 | 25 | 30 | 92 |
| J acid waste water | 0 | 1/2.5 | 30 | 10 | 25 | 24 | 1/3 | 10 | 25 | 25 | 90 |
| H acid waste water | 40 | 1/1.2 | 20 | 7 | 25 | 24 | 1/3 | 10 | 25 | 25 | 97.9 |
Claims (1)
1 ,-and kind of method with organic matter in trialkylamine extraction recovery TOBIAS ACID 97MIN.﹠ 98MIN., J acid and the H acid dye intermediate, it is characterized in that this method comprises following a few step:
(1) with kerosene dilution trade(brand)name N
235Extraction agent trialkyl tertiary amine, Dilution ratio is: kerosene: trialkyl tertiary amine=1: 0.2～0.5;
(2) the trialkyl tertiary amine-kerosene after the usefulness dilution is as extraction agent, add in TOBIAS ACID 97MIN.﹠ 98MIN., J acid and the H acid dye intermediate production waste liquor and extract, the pH value of waste liquor is 1.0～1.5, extraction is in a ratio of: extraction agent: waste liquor=1: 1～4.5, reaction times is 5～10 minutes, 20～50 ℃ of temperature of reaction;
(3) above-mentioned extraction system is introduced in the mixer-settler, the water of extraction system is separated with organic phase, disengaging time is 20～30 minutes, and the water after the separation is as discharge of wastewater, and organic phase is used for stripping;
(4) be that 24% NaOH solution is stripped in mixer-settler to above-mentioned isolated organic phase of the 3rd step as strippant with concentration, reextraction is in a ratio of: strippant: organic phase=1: 3, back-extraction time 10 minutes, 25 ℃ of reextraction temperature;
(5) above-mentioned reextraction system is introduced in the mixer-settler, water in the reextraction system is separated with organic phase, disengaging time is 20～30 minutes, water after the separation is the organic matter after the waste liquid camber concentrates, return the raw materials for production of making dyestuff, or being used for the new dyestuff intermediate of F production, organic phase is the trialkylamine and the kerosene of living again, and recycles as extraction agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96100469A CN1073536C (en) | 1996-02-02 | 1996-02-02 | Technology for recovering organic mass in naphthalene series dye intermediate waste mother liquor by trialkylamine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96100469A CN1073536C (en) | 1996-02-02 | 1996-02-02 | Technology for recovering organic mass in naphthalene series dye intermediate waste mother liquor by trialkylamine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1143072A CN1143072A (en) | 1997-02-19 |
| CN1073536C true CN1073536C (en) | 2001-10-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96100469A Expired - Fee Related CN1073536C (en) | 1996-02-02 | 1996-02-02 | Technology for recovering organic mass in naphthalene series dye intermediate waste mother liquor by trialkylamine |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101230025A (en) * | 2008-02-22 | 2008-07-30 | 广东纺织职业技术学院 | Extractive recovery method for aryl sulfonic acid salt in waste water |
| CN101993127A (en) * | 2009-08-11 | 2011-03-30 | 天津市大港宏利染料化工厂 | High-efficiency extractant and extracting method for extracting naphthalenesulfonic acid waste liquid |
| CN102603025B (en) * | 2012-03-31 | 2013-07-31 | 中国中化股份有限公司 | Method for processing wastewater produced in reactive dye production by utilizing complexing extraction technology |
| CN102796397B (en) * | 2012-08-23 | 2013-07-24 | 楚源高新科技集团股份有限公司 | Method for synthesis of active printing dye from T acid mother liquor wastewater |
| CN103408092B (en) * | 2013-08-02 | 2015-01-07 | 浙江吉华集团股份有限公司 | Treatment method for production wastewater of sulfonic acid group dye and dye intermediate of sulfonic acid group dye |
| CN103896438B (en) * | 2014-04-16 | 2015-12-09 | 响水恒利达科技化工有限公司 | The method of the preparation method of J acid and J acid wastewater comprehensive treatment and recycling |
| CN104291398B (en) * | 2014-09-17 | 2016-08-10 | 广东顺德天新环保科技有限公司 | A kind of processing method recycling dyeing residual liquid |
| CN104926024B (en) * | 2015-05-25 | 2017-02-01 | 濮阳市盛源能源科技股份有限公司 | Novel process for treating maleic anhydride wastewater |
| CN107602430B (en) * | 2017-11-02 | 2021-01-08 | 响水恒利达科技化工有限公司 | Method for extracting and recovering tobias acid from tobias acid wastewater |
| CN109748830A (en) * | 2019-01-09 | 2019-05-14 | 江苏吉华化工有限公司 | A kind of processing solution and processing method for H acid mother liquor |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1745684A1 (en) * | 1989-12-05 | 1992-07-07 | Институт неорганической и физической химии АН АзССР | Process for removing acid dyes from waste water |
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1996
- 1996-02-02 CN CN96100469A patent/CN1073536C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1745684A1 (en) * | 1989-12-05 | 1992-07-07 | Институт неорганической и физической химии АН АзССР | Process for removing acid dyes from waste water |
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| CN1143072A (en) | 1997-02-19 |
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