CN107686203A - A kind of recycling treatment process using cross current solvent extraction method to H acid producing waste waters - Google Patents
A kind of recycling treatment process using cross current solvent extraction method to H acid producing waste waters Download PDFInfo
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- CN107686203A CN107686203A CN201710889346.5A CN201710889346A CN107686203A CN 107686203 A CN107686203 A CN 107686203A CN 201710889346 A CN201710889346 A CN 201710889346A CN 107686203 A CN107686203 A CN 107686203A
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- acid producing
- waste waters
- producing waste
- extractant
- cross current
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
- C02F1/265—Desalination
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/18—Dehydration
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of recycling treatment process using cross current solvent extraction method to H acid producing waste waters, the processing step are as follows：（1）Separating inorganic salts and organic matter：Extractant is added into the H acid producing waste waters of collection, is stirred, one-level or two level extraction is carried out, obtains extraction phase and raffinate phase；（2）Reclaim inorganic salts：Step（1）Raffinate phase handled using MVR equipment, sodium sulphate condensing crystallizing separate out recycle, distilled water carry out technique reuse；（3）Extractant regeneration utilizes：To step（1）Extraction be added to strippant, by step（1）In extractant regeneration utilize, obtained extraction phase concentrate returns to production technology or carries out burning disposal.The technique can not only realize effective removal of COD in H acid producing waste waters, and can realize the recycling of a large amount of sodium sulfate salts in H acid producing waste waters, moreover it is possible to the regeneration that extractant is realized in back extraction is carried out to extractant.
Description
Technical field
The invention belongs to chemical products Wastewater Treatment field, is related to a kind of recycling treatment work of H acid waste water
Skill, more particularly to a kind of technique that recycling treatment is carried out to H acid producing waste waters using cross current solvent extraction method.
Background technology
H acid is widely used in producing reactive dye, direct dyes, acid dyes as important naphthalene series dye intermediate
And the product such as chromotropic acid, H acid producing waste waters can be produced during H acid is produced, are predominantly produced through acid out and filter progress
Raw generation H acid crystal mother liquor waste waters.Its chemical property is stable, and pH value is that 2 or so, CODcr is up to 20000 ~ 50000 mg/L,
Belong to typical organic wastewater with difficult degradation thereby, in general oxidation technology and biochemical process are difficult to effectively handle, and the sulfuric acid in waste water
Na concn is in hypersaturated state, if not handled effectively it, not only environment and human health can be caused seriously to endanger
Evil, can also cause the waste of resource.
At present, mainly there are absorption method, Coagulation Method, extraction, photocatalytic oxidation, ozone to the processing method of H acid waste water
Oxidizing process, wet oxidation process, Fenton and Fenton-like technology, sonication, membrane separation process, biological treatment etc., but
Because H acid waste water has the characteristics that salinity is high, acidity is strong, colourity is deep, COD contents are high, bio-toxicity is big, above method
Had some limitations during reason.
CN103680022 A disclose a kind of handling process of H acid producing waste waters, device and special absorption resin material,
A part of COD compositions are removed by extraction, meanwhile, make its surface double through hydroxy silicon oil and acrylic acid using resin modified technology
Double modifications of cyclopentene base ester, improve the Selective adsorption to pigment organic matter H acid.Extractant used in this method can not be by
Regeneration follows bad utilization, causes to waste, additionally needs to prepare sorbing material and preparation facilities, cost is higher, complex operation.
CN105236623 A disclose a kind of processing method of H acid waste water, handle H acid waste water using Fenton methods, and add
Enter calcium oxide regulation pH, adsorbent and flocculant carry out flocculation sediment, reach the purpose for removing COD.This method needs to heat
And medicament is repeatedly added, and the sodium sulfate salt in H acid waste water could not be recycled utilization, operation is complex, and cost is higher.
Therefore, a kind of effective processing that can realize H acid waste water is found, and can is to a large amount of sulfuric acid for containing in H acid waste water
The treatment technology that sodium is recycled is current urgent problem to be solved.The content of the invention
It is an object of the invention to provide a kind of recycling treatment process using cross current solvent extraction method to H acid producing waste waters, the technique
Effective removal of COD in H acid producing waste waters can be not only realized, and a large amount of sodium sulfate salts in H acid producing waste waters can be realized
Recycle, moreover it is possible to the regeneration that extractant is realized in back extraction is carried out to extractant.
The purpose of the present invention is achieved through the following technical solutions：
A kind of recycling treatment process using cross current solvent extraction method to H acid producing waste waters, comprise the following steps：
（1）Separating inorganic salts and organic matter：Extractant is added into the H acid producing waste waters of collection, is stirred, carries out one-level
Or two level extracts, contain large amount of organic in obtained extraction phase, contain a large amount of inorganic salts in raffinate phase；The extractant is by network
Mixture, diluent and cosolvent composition, complexing agent is one kind in trioctylamine, tri-iso-octylamine, n-octyl amine and tributyl phosphate, dilute
It is kerosene to release agent, and cosolvent is n-octyl alcohol, and the volume ratio of diluent, complexing agent and cosolvent is 2 ~ 5:1:0.2；H acid productions are useless
The volume ratio of water and extractant is 1 ~ 8:1；Speed of agitator is 220 ~ 240r/min；Single-stage extraction temperature is 15 ~ 65 DEG C, single-stage extraction
Take 10 ~ 40min of time；
（2）Reclaim inorganic salts：Step（1）Raffinate phase in contain substantial amounts of sodium sulphate, handled using MVR equipment, sulfuric acid
Sodium condensing crystallizing separates out recoverable, and distilled water can carry out technique reuse；
（3）Extractant regeneration utilizes：To step（1）Extraction be added to strippant, by step（1）In extractant regeneration profit
With obtained extraction phase concentrate can return to production technology or carry out burning disposal；The strippant is that sodium hydroxide is molten
The volume ratio of liquid, extraction phase and sodium hydroxide solution is 2 ~ 4:1, concentration of sodium hydroxide solution is 10 ~ 15%.
Preferably, step（1）In, extractant presses volume by complexing agent trioctylamine, diluent kerosene, cosolvent n-octyl alcohol
Than 5:18~22:1 is mixed to prepare.
Preferably, step（1）In, the volume ratio of H acid producing waste waters and extractant is 4.5 ~ 5:1.
Preferably, step（1）In, single-stage extraction temperature is 50 ~ 65 DEG C.
Preferably, step（1）In, the single-stage extraction time is 30 ~ 32min.
Preferably, step（1）In, cross current solvent extraction series is 2 grades.
Preferably, step（3）In, concentration of sodium hydroxide solution 13%.
Preferably, step（3）In, the volume ratio of extraction phase and sodium hydroxide solution is 2:1.
The present invention compared with prior art, has the following advantages that：
1st, extraction efficiency is high, can effectively reduce the COD value in H acid waste water, is advantageous to the next step processing of H acid waste water.
2nd, extractant realizes regeneration after sodium hydroxide solution is stripped, and the extractant after regeneration still has extraction well
Effect, the extraction concentrate obtained after back extraction can return to production technology.
3rd, the inorganic salts sodium sulphate in H acid waste water is after MVR PROCESS FOR TREATMENTs, and its purity is close to 100%.
4th, present invention process is reasonable in design, and flow is simple, extractant reproducible utilization, and regenerant can also carry out secondary use
Or other produce purposes, processing and the recycling of H acid waste water can be effectively realized.
Brief description of the drawings
Fig. 1 is the extraction process flow figure of the present invention；
Fig. 2 is that undressed H acid waste water separates out crystallization（It is left）With sodium sulfate powder（It is right）；
Fig. 3 is that treated H acid waste water separates out crystallization（It is left）With sodium sulfate powder（It is right）.
Embodiment
Technical scheme is further described below in conjunction with the accompanying drawings, but is not limited thereto, it is every to this
Inventive technique scheme is modified or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, all should cover
In protection scope of the present invention.
Embodiment one：Present embodiments provide for a kind of resource using cross current solvent extraction method to H acid producing waste waters
Change handling process, as shown in figure 1, specific implementation step is as follows：
（1）By complexing agent trioctylamine, diluent kerosene, cosolvent n-octyl alcohol by volume 5:18~22:1 is mixed and made into extractant,
By 4.5 ~ 5:1 ratio mixing H acid producing waste waters and extractant, heating mixed solution temperature are stirred solution to 50 ~ 65 DEG C
To mix, mixing speed is 220 ~ 240r/min, stops stirring after extracting 30 ~ 32min, separates extraction phase and raffinate after standing,
Continue second level cross current solvent extraction, extraction conditions is identical with first order extraction conditions, will be extracted twice respectively after the completion of extraction
Obtained extraction phase and raffinate, which merges, to be further processed.
（2）By step（1）The obtained raffinate containing a large amount of sodium sulphate carries out MVR processing, and sodium sulphate is obtained after processing
White powder, purity is close to 100%.
（3）By step（1）The sodium hydroxide solution that concentration is 13% is added in obtained extraction phase to be stripped, and is extracted
It is mutually 2 with the volume ratio of strippant sodium hydroxide solution:1, the regenerating extracting agent water white transparency obtained after the completion of back extraction, extraction
Phase concentrate is taken to carry out incineration disposal as raw materials for production reuse, remainder.
Embodiment two：For present embodiment by taking certain factory H acid producing waste waters as an example, its COD value is 35000mg/L,
Sodium sulphate content 20% or so.
The processing step for carrying out recycling treatment to above-mentioned H acid producing waste waters using cross current solvent extraction method is as follows：
（1）By complexing agent trioctylamine, diluent kerosene, cosolvent n-octyl alcohol by volume 5:18:1 is mixed and made into extractant, presses
4.5:1 ratio mixing H acid producing waste waters and extractant, heating mixed solution temperature is 55 DEG C, and solution is stirred, and is stirred
Speed is 230r/min, stops stirring after extracting 30min, separates extraction phase and raffinate after standing, continue the second level
Cross current solvent extraction, extraction conditions is identical with first order extraction conditions, and extraction phase and extraction will be obtained by extraction after the completion of extraction twice respectively
Extraction raffinate, which merges, to be further processed.Wherein, raffinate COD value is 5750mg/L, and clearance reaches 83.6%.
（2）By step（1）The obtained raffinate containing a large amount of sodium sulphate carries out MVR processing, and sodium sulphate is obtained after processing
White powder, purity is close to 100%.
（3）By step（1）The sodium hydroxide solution that concentration is 13% is added in obtained extraction phase to be stripped, and is extracted
It is mutually 2 with strippant sodium hydroxide solution volume ratio:1, the extractant water white transparency of the regeneration obtained after the completion of back extraction, extraction
Phase concentrate is taken to carry out incineration disposal as raw materials for production reuse, remainder.
Undressed H acid waste water separates out crystallization with sodium sulfate powder as shown in Fig. 2 being handled by present embodiment method
H acid waste water separate out crystallization it is as shown in Figure 3 with sodium sulfate powder.
Embodiment three：For present embodiment by taking certain factory H acid producing waste waters as an example, its COD value is 35000mg/L,
Sodium sulphate content 20% or so.
The processing step for carrying out recycling treatment to above-mentioned H acid producing waste waters using cross current solvent extraction method is as follows：
（1）By complexing agent trioctylamine, diluent kerosene, cosolvent n-octyl alcohol by volume 5:18:1 is mixed and made into extractant, presses
4.5:1 ratio mixing H acid producing waste waters and extractant, heating mixed solution temperature is 55 DEG C, and solution is stirred, and is stirred
Speed is 230r/min, stops stirring after extracting 30min, separates extraction phase and raffinate after standing.Wherein, raffinate COD
It is worth and reaches 60.0% for 13980mg/L, clearance.
（2）By step（1）The obtained raffinate containing a large amount of sodium sulphate carries out MVR processing, and sodium sulphate is obtained after processing
White powder, purity is close to 100%.
（3）By step（1）The sodium hydroxide solution that concentration is 13% is added in obtained extraction phase to be stripped, and is extracted
It is mutually 2 with strippant sodium hydroxide solution volume ratio:1, the extractant water white transparency of the regeneration obtained after the completion of back extraction.
Claims (10)
- A kind of 1. recycling treatment process using cross current solvent extraction method to H acid producing waste waters, it is characterised in that the processing step It is as follows：（1）Separating inorganic salts and organic matter：Extractant is added into the H acid producing waste waters of collection, is stirred, carries out one-level Or two level extraction, extraction phase and raffinate phase are obtained, wherein：The volume ratio of H acid producing waste waters and extractant is 1 ~ 8:1, stirring turns Speed is 220 ~ 240r/min, and single-stage extraction temperature is 15 ~ 65 DEG C, 10 ~ 40min of single-stage extraction time；（2）Reclaim inorganic salts：Step（1）Raffinate phase handled using MVR equipment, sodium sulphate condensing crystallizing separate out recovery profit With distilled water carries out technique reuse；（3）Extractant regeneration utilizes：To step（1）Extraction be added to the volume ratio of strippant, extraction phase and strippant For 2 ~ 4:1, by step（1）In extractant regeneration utilize, obtained extraction phase concentrate returns to production technology or burnt Burning processing.
- 2. the recycling treatment process according to claim 1 using cross current solvent extraction method to H acid producing waste waters, its feature exists In the step（1）In, extractant is made up of complexing agent, diluent and cosolvent, the volume of diluent, complexing agent and cosolvent Than for 2 ~ 5:1:0.2.
- 3. the recycling treatment process according to claim 2 using cross current solvent extraction method to H acid producing waste waters, its feature exists It is one kind in trioctylamine, tri-iso-octylamine, n-octyl amine and tributyl phosphate in the complexing agent, diluent is kerosene, cosolvent For n-octyl alcohol.
- 4. the recycling treatment process according to claim 2 using cross current solvent extraction method to H acid producing waste waters, its feature exists In the extractant by complexing agent trioctylamine, diluent kerosene, cosolvent n-octyl alcohol by volume 5:18~22:1 is mixed to prepare.
- 5. the recycling treatment process using cross current solvent extraction method to H acid producing waste waters according to claim 1,2,3 or 4, It is characterized in that the step（1）In, the volume ratio of H acid producing waste waters and extractant is 4.5 ~ 5:1.
- 6. the recycling treatment process according to claim 1 using cross current solvent extraction method to H acid producing waste waters, its feature exists In the step（1）In, single-stage extraction temperature is 50 ~ 65 DEG C, and the single-stage extraction time is 30 ~ 32min.
- 7. the recycling treatment process according to claim 1 using cross current solvent extraction method to H acid producing waste waters, its feature exists In the step（1）In, cross current solvent extraction series is 2 grades.
- 8. the recycling treatment process according to claim 1 using cross current solvent extraction method to H acid producing waste waters, its feature exists In described（3）In, strippant is sodium hydroxide solution, and concentration of sodium hydroxide solution is 10 ~ 15%.
- 9. the recycling treatment process according to claim 8 using cross current solvent extraction method to H acid producing waste waters, its feature exists In the concentration of sodium hydroxide solution be 13%.
- 10. the recycling treatment process using cross current solvent extraction method to H acid producing waste waters according to claim 1,8 or 9, its It is characterised by the step（3）In, the volume ratio of extraction phase and strippant is 2:1.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109824155A (en) * | 2019-03-04 | 2019-05-31 | 广东益诺欧环保股份有限公司 | A kind of system and method for high concentration COD waste water reclaiming processing |
| CN111747560A (en) * | 2020-06-04 | 2020-10-09 | 广东益诺欧环保股份有限公司 | System and method for treating and recycling J acid |
| CN112320776A (en) * | 2020-10-13 | 2021-02-05 | 东莞市三人行环境科技有限公司 | Chemical waste liquid throwing and washing water regenerated acid recovery system and application thereof |
| CN113248066A (en) * | 2021-05-18 | 2021-08-13 | 顺毅宜昌化工有限公司 | Method for treating waste water of kungfu acid |
| CN113387406A (en) * | 2021-06-21 | 2021-09-14 | 泉州南京大学环保产业研究院 | Treatment process of high-salt high-concentration nitrate nitrogen wastewater |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109824155A (en) * | 2019-03-04 | 2019-05-31 | 广东益诺欧环保股份有限公司 | A kind of system and method for high concentration COD waste water reclaiming processing |
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| CN111747560A (en) * | 2020-06-04 | 2020-10-09 | 广东益诺欧环保股份有限公司 | System and method for treating and recycling J acid |
| CN112320776A (en) * | 2020-10-13 | 2021-02-05 | 东莞市三人行环境科技有限公司 | Chemical waste liquid throwing and washing water regenerated acid recovery system and application thereof |
| CN113248066A (en) * | 2021-05-18 | 2021-08-13 | 顺毅宜昌化工有限公司 | Method for treating waste water of kungfu acid |
| CN113387406A (en) * | 2021-06-21 | 2021-09-14 | 泉州南京大学环保产业研究院 | Treatment process of high-salt high-concentration nitrate nitrogen wastewater |
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Application publication date: 20180213 |