CN109133469A - A kind of processing method of 2,6- dihydroxy-benzoic acid production waste water - Google Patents
A kind of processing method of 2,6- dihydroxy-benzoic acid production waste water Download PDFInfo
- Publication number
- CN109133469A CN109133469A CN201811139452.2A CN201811139452A CN109133469A CN 109133469 A CN109133469 A CN 109133469A CN 201811139452 A CN201811139452 A CN 201811139452A CN 109133469 A CN109133469 A CN 109133469A
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- Prior art keywords
- waste water
- processing method
- production waste
- dhba
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses one kind 2,6- dihydroxy-benzoic acid produces the processing method of waste water, and it includes steps: 1) phenol formaldehyde condensation: adjusting 2,6-DHBA and produces waste water pH value, formalin is added and carries out phenol formaldehyde condensation reaction, cooling filters out condensation product not soluble in water after reaction；2) adjust acid-base property: filtrate adjusts pH value with aqueous slkali again；3) it decolourizes, active carbon decolorization filtering filtering: is added；4) it evaporates, be concentrated, crystallization: crystallizing filtered clear liquid concentration and evaporation to obtain inorganic salts.The present invention has been stably obtained inorganic salts that meet national standards by this method, to solve the problems, such as to contain organic matter in production waste water and in by-product inorganic salts.
Description
Technical field
The present invention relates to the process field of wastewater from chemical industry, espespecially a kind of processing side of 2,6-DHBA production waste water
Method.
Background technique
2,6- dihydroxy-benzoic acid is that production new herbicides bispyribac-sodium, pyribenzoxim, pyrithiobac-sodium etc. are crucial intermediate
Body, also serves as medicine intermediate and other organic syntheses, and demand is increasing.
And existing production technology is substantially with resorcinol and CO2The reaction production under alkali metal effect for raw material, then
Through solvent recovery, it is dissolved in water, is acidified and obtains product.However in the waste water generated in the fabrication process, still having a small amount of has
Machine object contains organic matter to cause in by-product inorganic salts, thus affects its quality.
Summary of the invention
To solve the above problems, present invention is primarily aimed at it is useless to provide a kind of removal 2,6-DHBA production
The method of Organic substance in water, to solve the problems, such as to contain organic matter in by-product inorganic salts.
A kind of processing method of 2,6-DHBA production waste water of provided by the invention, it includes steps:
1) phenol formaldehyde condensation:
It adjusts 2,6-DHBA and produces waste water pH value, formalin is added and carries out phenol formaldehyde condensation reaction, after reaction
Cooling filters out condensation product not soluble in water；
2) acid-base property is adjusted:
Filtrate adjusts pH value with aqueous slkali again；
3) it decolourizes, filtering:
Active carbon decolorization filtering is added；
4) it evaporates, be concentrated, crystallization:
It crystallizes filtered clear liquid concentration and evaporation to obtain inorganic salts.
Further, in step 1), the pH value for adjusting 2,6-DHBA production waste water is PH≤1 or is 0.8-
Between 1.
Further, condensation temp is controlled in step 1) in 40-100 DEG C (preferably 70-90 DEG C), reaction time 3-
4h。
Further, the molar ratio of formaldehyde and phenolic hydroxy group organic matter is 0.5-10 in step 1).
Further, the pH value that the waste water is adjusted in step 1) is that addition hydrochloric acid or sulfuric acid are adjusted.
Further, the aqueous slkali used in regulating step in step 2) is NaOH or KOH solution.
Further, it also may include step in order to ensure avoiding generation environment from polluting: 5) throwing the water of concentration and evaporation again
Enter in process and is recycled.
The beneficial effects of the invention are that can be stably obtained that meet national standards inorganic by above-mentioned technical proposal
Salt, to solve the problems, such as to contain organic matter in production waste water and in by-product inorganic salts.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
Below with reference to the embodiments and with reference to the accompanying drawing technical solution of the present invention is described in further detail.
Central scope of the invention is:
The a small amount of organic matter contained in 2,6-DHBA production waste water, major problem is that there are isophthalic two
Phenol, 2,6-DHBA and a small amount of tar etc., and these ingredient recovery difficults are big.The thus skill that inventor uses
Art method is the organic matter removed in waste water containing phenolic hydroxyl group with the method for phenol formaldehyde condensation, then by being added after adjusting acid-base property
Active carbon decoloring, condensing crystallizing, and cover condensed water can and use in production, it is that meet national standards inorganic can be stably obtained
Salt.To solve the problems, such as in production waste water and in by-product inorganic salts containing organic matter.
Wherein, a kind of processing method of 2,6-DHBA of the invention production waste water mainly includes having the following steps
(being process flow diagram of the invention referring to attached drawing 1):
1) pH value of adjustment 2,6-DHBA production waste water, is added formalin and carries out phenol formaldehyde condensation reaction, instead
Should after filter out condensation product not soluble in water.
In this step, pH value≤1 of 2,6-DHBA production waste water is adjusted first, usually 0.8-1, then
Formalin is added, the molar ratio of formaldehyde and phenolic hydroxy group organic matter is 0.5-10, controls temperature at 40-100 DEG C (preferably
70-90 DEG C) under carry out phenol formaldehyde condensation 3-4h, condensation product not soluble in water is filtered out after reaction.
The content of organics for wherein producing the phenolic hydroxy group in waste water can be learnt by liquid-phase chromatographic analysis.
2) filtered clear liquid is adjusted to pH value with aqueous slkali is neutrality, and aqueous slkali can be NaOH or KOH solution.At this
In step, filtered clear liquid can be adjusted to pH value with NaOH or K0H solution is 6-8；
3) active carbon is added in the solution after neutralization to decolourize, is filtered after decoloration；
It is to cross cleaner liquid after adjusting pH value in the step, active carbon decoloring is added, is refiltered after decoloration；It is wherein active
The amount that charcoal is added is the 0.3%-2% of neutralizer；Enter dangerous waste library after filtered active carbon packaging.
4) filtrate after decolourizing is carried out concentration and evaporation crystallization, concentrating filter liquor evaporative crystallization obtains meeting national standard
Inorganic salts；
Filtrate i.e. previous step after decolourizing is evaporated condensing crystallizing through double effect evaporator, the symbol that then can will be obtained
The inorganic salts for closing national standard are packed.
5) further the water of concentration and evaporation effectively can be recycled:
The water that concentration and evaporation obtains can be put into again in the production procedure.
For the superiority and feasibility for verifying treatment method, existing enumeration process specific example, method and step, data are such as
Under:
Example 1.
Take production waste water 500ml that reaction kettle is added, the organic matter of Korea Spro's phenolic hydroxyl group of chromatography detection is 13.25g, and hydrochloric acid is added
PH value is adjusted to 0.87.
40% formalin 40g is added, is heated to cooling after 40-100 DEG C of reaction 3.5g, filters and obtain 27.4g and consolidate
Body condensation product.
Filtered mother liquor KOH aqueous solution adjusts pH value to 7；Then 10g active carbon is added to carry out adsorption bleaching, take out
Filter；The evaporative crystallization of filtrate progress next step.
Filtrate after decoloration is evaporated crystallization and obtains 162g inorganic salts (KCl), the water recovery steamed.
Example 2.
Take production waste water 1000ml that reaction kettle is added, the organic matter of the phenolic hydroxy group of chromatography detection is 26.4g, and hydrochloric acid is added
PH value is adjusted to 0.87.
40% formalin 79g is added, is heated to cooling after 40-100 DEG C of reaction 3.5g, filters and obtain 54.5g and consolidate
Body condensation product.
Filtered mother liquor KOH aqueous solution adjusts pH value to 7；Then 20g active carbon is added to carry out adsorption bleaching, take out
Filter；The evaporative crystallization of filtrate progress next step.
Filtrate after decoloration is evaporated crystallization and obtains 322g inorganic salts (KCl), the water recovery steamed.
In above-mentioned experiment, the method for inspection of use are as follows:
1) pH value detection is counted with PH；
2) the organic matter liquid chromatographic detection in waste water.
The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof, although referring to above-described embodiment pair
The present invention is described in detail, it should be understood by a person of ordinary skill in the art that still can be to of the invention specific
Embodiment is modified or replaced equivalently, and without departing from any modification of spirit and scope of the invention or equivalent replacement,
It is intended to be within the scope of the claims of the invention.
Claims (8)
1. a kind of processing method of 2,6-DHBA production waste water, which is characterized in that include step:
1) phenol formaldehyde condensation:
It adjusts 2,6-DHBA and produces waste water pH value, formalin is added and carries out phenol formaldehyde condensation reaction, cools down after reaction
Filter out condensation product not soluble in water；
2) acid-base property is adjusted:
Filtrate adjusts pH value with aqueous slkali again；
3) it decolourizes, filtering:
Active carbon decolorization filtering is added；
4) it evaporates, be concentrated, crystallization:
It crystallizes filtered clear liquid concentration and evaporation to obtain inorganic salts.
2. the processing method of 1 a kind of 2,6-DHBA production waste water according to claim, which is characterized in that step
Rapid 1) the middle pH value for adjusting 2,6- dihydroxy-benzoic acid production waste water is PH≤1 or is between 0.8-1.
3. the processing method of 1 a kind of 2,6-DHBA production waste water according to claim, which is characterized in that
The aqueous slkali used in regulating step in step 2) is NaOH or KOH solution.
4. the processing method of 1 a kind of 2,6-DHBA production waste water according to claim, which is characterized in that
Control condensation temp is at 70-90 DEG C in step 1), reaction time 3-4h.
5. the processing method of 1 a kind of 2,6-DHBA production waste water according to claim, which is characterized in that
Control condensation temp is at 40-100 DEG C in step 1), reaction time 3-4h.
6. the processing method of 1 a kind of 2,6-DHBA production waste water according to claim, it is characterised in that:
The molar ratio of formaldehyde and phenolic hydroxy group organic matter is 0.5-10 in step 1).
7. the processing method of 1 a kind of 2,6-DHBA production waste water according to claim, it is characterised in that:
The pH value that the waste water is adjusted in step 1) is that addition hydrochloric acid or sulfuric acid are adjusted.
8. the processing method of 1 a kind of 2,6-DHBA production waste water according to claim, which is characterized in that also
Include step: 5) recycling the water of concentration and evaporation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811139452.2A CN109133469A (en) | 2018-09-28 | 2018-09-28 | A kind of processing method of 2,6- dihydroxy-benzoic acid production waste water |
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| CN201811139452.2A CN109133469A (en) | 2018-09-28 | 2018-09-28 | A kind of processing method of 2,6- dihydroxy-benzoic acid production waste water |
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| CN201811139452.2A Pending CN109133469A (en) | 2018-09-28 | 2018-09-28 | A kind of processing method of 2,6- dihydroxy-benzoic acid production waste water |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110330189A (en) * | 2019-07-25 | 2019-10-15 | 四川恒泰环境技术有限责任公司 | A kind of wastewater treatment method containing benzoic acid |
| CN110803820A (en) * | 2019-12-12 | 2020-02-18 | 南通市天时化工有限公司 | Treatment process for zero discharge of benzoic acid mother liquor wastewater |
| CN113979583A (en) * | 2021-11-04 | 2022-01-28 | 武汉瑞阳化工有限公司 | Method for treating acidic wastewater generated in 1-fluoronaphthalene synthesis process |
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| CN104787955A (en) * | 2015-04-17 | 2015-07-22 | 青岛科技大学 | Method for removing organic matters in phenolic wastewater |
| US20180170773A1 (en) * | 2016-12-15 | 2018-06-21 | Ada Carbon Solutions, Llc | Sorbent compositions for the removal of boron from aqueous mediums |
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Patent Citations (3)
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| CN102580701A (en) * | 2012-01-18 | 2012-07-18 | 西安蓝晓科技新材料股份有限公司 | Preparation method of arsenic removal resin |
| CN104787955A (en) * | 2015-04-17 | 2015-07-22 | 青岛科技大学 | Method for removing organic matters in phenolic wastewater |
| US20180170773A1 (en) * | 2016-12-15 | 2018-06-21 | Ada Carbon Solutions, Llc | Sorbent compositions for the removal of boron from aqueous mediums |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110330189A (en) * | 2019-07-25 | 2019-10-15 | 四川恒泰环境技术有限责任公司 | A kind of wastewater treatment method containing benzoic acid |
| CN110330189B (en) * | 2019-07-25 | 2022-03-08 | 四川恒泰环境技术有限责任公司 | Treatment method of wastewater containing benzoic acid |
| CN110803820A (en) * | 2019-12-12 | 2020-02-18 | 南通市天时化工有限公司 | Treatment process for zero discharge of benzoic acid mother liquor wastewater |
| CN113979583A (en) * | 2021-11-04 | 2022-01-28 | 武汉瑞阳化工有限公司 | Method for treating acidic wastewater generated in 1-fluoronaphthalene synthesis process |
| CN113979583B (en) * | 2021-11-04 | 2023-09-22 | 武汉瑞阳化工有限公司 | Treatment method of acid wastewater generated in process of synthesizing 1-fluoronaphthalene |
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