CN105129893A - High efficiency extractant and extraction method of H-acid mother liquor - Google Patents
High efficiency extractant and extraction method of H-acid mother liquor Download PDFInfo
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- CN105129893A CN105129893A CN201510565747.6A CN201510565747A CN105129893A CN 105129893 A CN105129893 A CN 105129893A CN 201510565747 A CN201510565747 A CN 201510565747A CN 105129893 A CN105129893 A CN 105129893A
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Abstract
The invention relates to a high efficiency extraction method of H-acid mother liquor, and belongs to the field of an H-acid production waste water treatment. The method provided by the invention is composed of extraction and back extraction, the extraction employs the H acid mother liquor as a processing object and employs a high efficiency extractant, and the high efficiency extractant is composed of a tertiary amine solvent, a diluent and a cosolvent, after extraction, the H acid mother liquor is prepared into a inorganic salt water layer and an acidic complex layer; inorganic salt and water are removed, the back extraction is carried out for the acidic complex layer, and a stripping agent is added till pH value of an organic water phase prepared by the back extraction is 7-11. The invention is applied into the H-acid production, thereby avoiding generation of solid waste with simple operation and effectively reducing the production cost, and the recovered objects can be used for the second times.
Description
Technical field
The invention belongs to a kind of Chemicals, particularly a kind of efficient extraction agent for extracting H acid mother liquor and extracting process.
Background technology
H acid belongs to the important intermediate of naphthalene series dye chemical industry, and current domestic traditional technology H acid product per ton produces the H acid segregation mother liquor of 8-12T, and its COD is at 20000mg/L, and sodium sulphate content 220g/L, belongs to high COD, high in salt.Trade effluent, is difficult to carry out routine biochemistry process, and under current environment-protecting high-pressure situation, more domestic research institutions and Some Enterprises are all constantly probing into new production technique and post-treating method, but are all in the experimental demonstration stage.At present, the multiple treatment process of H acid mother liquor, comparatively speaking, only has extraction process could alleviate current environmental protection pressure, for the survival and development of enterprise gain time.In this context, many enterprises also go up one after another and extract project at once, in succession also there is the H acid mother liquor process Patent Publication of different editions, as CN101780994A, but due to the proportioning of extraction agent and the difference of extracting process, percentage extraction is on the low side, after extraction, inorganic salt purity is not high, regeneration cost increase, does not realize resource circulation utilization effectively, rationally reduces production cost.
Based on this, make subject application.
Summary of the invention
The object of the invention is to overcome above-mentioned the deficiencies in the prior art, and a kind of efficient extraction H acid segregation extraction agent of mother liquor and extracting process are provided, for the cleaner production of H acid and the recycle of resource provide a practical feasible method.
For achieving the above object, the technical scheme taked of the present invention is as follows:
For extracting an efficient extraction agent for H acid mother liquor, this efficient extraction agent is made up of complexing agent, thinner and solubility promoter, and complexing agent is wherein tertiary amines solvent, and thinner is sulfonated kerosene or dodecylbenzene, and solubility promoter is tributyl phosphate or n-Octanol.
Further, as preferably:
Described tertiary amines solvent is dodeca-tertiary amine or three pungent/certain herbaceous plants with big flowers base tertiary amine.
Described efficient extraction agent is by three pungent, certain herbaceous plants with big flowers base tertiary amines, and sulfonated kerosene and octanol ternary component mixture form, and its mixture volume ratio is: three pungent, certain herbaceous plants with big flowers base tertiary amine 2-6 parts, sulfonated kerosene 3-7 part, octanol 0.5-1.5 part.
Described three pungent, certain herbaceous plants with big flowers base tertiary amines, the mixture volume ratio of sulfonated kerosene and octanol is: 5:4:1.
Simultaneously, the object of second aspect present invention is to provide the method for a kind of H acid mother liquor extraction, the method is formed primarily of extraction and back-extraction two operations, described extraction with H acid mother liquor for handling object, and adopt efficient extraction agent, this efficient extraction agent is made up of tertiary amines solvent, thinner and solubility promoter, the profit of extraction agent and H acid mother liquor is in a ratio of 1:1-5, process temperature is 30-50 DEG C, extraction process acid adding amount is identical with tertiary amines solvent mole number, and after extraction, H acid mother liquor forms inorganic salt solution and acid complex layer; Remove inorganic salt solution, acid complex layer is carried out back extraction; In described strip stages, reverse-extraction agent is MgO, CaO, CaCO
3, Ca(OH)
2, NaOH, NH
3 .h
2one in O, back extraction temperature 25-65 DEG C, the organic aqueous phase pH to 7-11 being added into back extraction formation of reverse-extraction agent.
Wherein, as preferably:
Described tertiary amines solvent is dodeca-tertiary amine or three pungent, certain herbaceous plants with big flowers alkyl tertiary amines, and thinner is sulfonated kerosene or dodecylbenzene, and solubility promoter is tributyl phosphate or n-Octanol.
Described tertiary amines solvent is three pungent, certain herbaceous plants with big flowers alkyl tertiary amines, and thinner is sulfonated kerosene, and solubility promoter is n-Octanol, and three pungent, certain herbaceous plants with big flowers alkyl tertiary amine is 5:4:1 with the mol ratio that mixes of sulfonated kerosene, n-Octanol three, and the profit of extraction agent and H acid mother liquor is in a ratio of 1:4.
When described reverse-extraction agent is preferably NaOH, back extraction temperature 50-60 DEG C, concentration of anti-stripping agent is 15-40%, the organic aqueous phase pH to 10-11 being added into back extraction formation of reverse-extraction agent; More preferred, concentration of anti-stripping agent is 25%.
Described reverse-extraction agent is preferably NH
3 .h
2during O, back extraction temperature 50-60 DEG C, concentration of anti-stripping agent is 15-25%, the organic aqueous phase pH to 9-10 being added into back extraction formation of reverse-extraction agent; More preferred, concentration of anti-stripping agent is 20-25%.
In the application, three pungent, certain herbaceous plants with big flowers alkyl tertiary amine is N235.
Principle of work of the present invention and beneficial effect as follows:
The application by several optional extraction agent in conjunction with extraction experiments, carry out extraction agent component preferred, again by composite adjustment proportioning, to reaching the highest percentage extraction and extraction phase ratio, at the composition of the preferred reverse-extraction agent of strip stages, concentration, add-on and system temperature, while reduction extraction cost, obtain the effect of extraction agent extraction minimization of loss.
1,
extraction agent component is preferred:theoretical according to complexometric extraction, in the application, extraction agent is made up of complexing agent, thinner, solubility promoter three kinds of compositions.
(1)
complexing agent is preferred:using tertiary amines solvent as complexing agent, add equivalent sulfuric acid, make complexing agent protonated, then the H acid mother liquor adding certain volume fully mixes rear leaving standstill, primary part observation aqueous phase colourity changes.By to dodeca-tertiary amine and three pungent, certain herbaceous plants with big flowers alkyl tertiary amine two kinds of complexing agents extraction contrasts, three pungent, certain herbaceous plants with big flowers alkyl tertiary amine effect is better than dodeca-tertiary amine, and aqueous phase colourity is low.
(2)
thinner is preferred:with cheap, quality is pure, toxicological harmless, the principle that viscosity is low, added by thinner in the extraction system of three pungent, certain herbaceous plants with big flowers alkyl tertiary amine and H acid mother liquor, by sulfonated kerosene, dodecylbenzene two kinds of thinner effect comparison, sulfonated kerosene diluent effect is better than dodecylbenzene.
(3)
solubility promoter is preferred:solubility promoter requires there is higher partition ratio in complexing agent, thinner, is conducive to protonated complexing agent in the dispersion of system camber, improves Complexation Efficiency.By to hydrotropy Liu tributyl phosphate, the solubilization-aid effect contrast of n-Octanol, tributyl phosphate easily forms emulsion layer at water-oil interface as solubility promoter, and the water-oil interface layering of n-Octanol is clear, without emulsification, so the preferred n-Octanol of solubility promoter.
In sum, H acid mother liquor extraction agent best composition is: three pungent, certain herbaceous plants with big flowers alkyl tertiary amines, sulfonated kerosene, n-Octanol.
2,
proportion optimization:how many complexing agent proportions in extraction agent is the deciding factor that impact extracts usefulness, and the amount of thinner, solubility promoter is also key factor simultaneously, only has complex system to debug dispersion, just can reach effective extraction.
Passing ratio regulation experiment, draws optimal volume proportioning: three pungent, certain herbaceous plants with big flowers alkyl tertiary amines: sulfonated kerosene: n-Octanol=5:4:1.
3,
profit is compared preferably:first a certain amount of extraction agent is added equimolar sulfuric acid, then 1:1,1:2,1:3,1:4,1:5 is compared according to profit, carry out acid complexometric extraction respectively, under the state of 45 DEG C, leave standstill after extraction agent and H acid mother liquor are fully mixed 15 minutes, be separated the colourity of sour water according to range estimation after layering, finally determine that the best is in a ratio of 1:4.
4,
back extraction condition optimization:
(1)
reverse-extraction agent is preferred:under whipped state, in extraction liquid, evenly add reverse-extraction agent (MgO, CaO, CaCO
3, Ca(OH)
2, NaOH, NH
3 .h
2o), process temperature 60-65 DEG C, add and maintain stirring stratification after 0.5 hour, after water-oil interface are clear, extraction agent is separated with organic water layer.
By comparing the rate of recovery of extraction agent, with MgO, CaO, CaCO
3, Ca(OH)
2deng being reverse-extraction agent, solvent loss at 1-1.5%, organic water layer contain a small amount of become the oil in water emulsion of colloid, subsequent disposal relative complex, and NaOH, NH
3 .h
2o is as reverse-extraction agent, and their extraction and recovery is lost in 1-1.5 ‰.Therefore, by NaOH, NH
3 .h
2o is first-selected as reverse-extraction agent.
(2)
back extraction temperature is preferred:by to extraction liquid persistently overheating observation within the scope of 25-60 DEG C, material fluidity is good, viscosity is low at 50-60 DEG C for system, therefore, determines that 50-60 DEG C for best back extraction temperature.
(3)
concentration of anti-stripping agent is preferred:
1. NaOH with 15%, 20%, 25%, 30%, 40% concentration carry out back extraction respectively and add, consider the bulk factor of oil-water separation and organic aqueous phase, the liquid caustic soda of first-selected 25% is optimum concn.
2. NH
3 .h
2o carries out back extraction respectively add with the concentration of 15%, 20%, 25%, has good oil-water separation, considers production practical situation, with the ammoniacal liquor of 20-25% for optimum concn.
4,
reverse-extraction agent consumption preferred:
Because back extraction system is a nonhomogeneous system, have certain difference with common acid-base neutralisation, finding by controlling organic aqueous phase PH:7.0,8.0,9.0,10,11 in stripping process, take NaOH as reverse-extraction agent, best organic aqueous phase PH: be 10-11, with NH
3 .h
2when O is reverse-extraction agent, best organic aqueous phase PH is 9.0-10.
In sum, reverse-extraction agent consumption is with organic aqueous phase PH for controlling terminal, and take NaOH as reverse-extraction agent, organic aqueous phase PH is 10-11, with NH
3 .h
2when O is reverse-extraction agent, organic aqueous phase PH is 9.0-10.
effect of the present invention:profit of the present invention is in a ratio of 1:4, and extraction usefulness is 2-4 times of usual manner, and reverse-extraction agent is the key factor of extraction cost, and adopt NaOH back extraction, its cost is 2 times of ammoniacal liquor back extraction; Because the present invention have employed PH terminal point control to back extraction terminal, the loss of its extraction agent is all at 1-1.5 ‰, and organic aqueous phase oil length is low, and comprehensive cost declines.
Accompanying drawing explanation
Fig. 1 is extraction process flow figure of the present invention;
Fig. 2 is stripping process schema of the present invention.
Embodiment
Embodiment 1
A kind of efficient extraction agent for extracting H acid mother liquor of the present embodiment and extracting process, wherein:
(1) efficient extraction agent preparation: measure that 500ml tri-is pungent, certain herbaceous plants with big flowers alkyl tertiary amine respectively, 400ml sulfonated kerosene, 100ml n-Octanol adds in 5000ml four-hole boiling flask, starts and stirs and heat up.
(2) complexometric extraction: when extraction agent temperature is at 30-40 DEG C, add the H acid mother liquor of 4000ml, adding 50-55g concentration under whipped state is 98% sulfuric acid, process temperature is 45 DEG C, stir and proceed to separating funnel after 20 minutes, leave standstill after 0.5 hour, isolate the inorganic salt solution of lower floor's clear, the acid complex layer on upper strata waits until subsequent disposal.
(3) back extraction: the acid complex layer after the separation in separating funnel is proceeded in four-hole boiling flask, be warming up to 50 DEG C, the slow NaOH(mass percent adding about 1.4 moles is 25%), make organic aqueous phase pH at 10-11, process temperature is 55-65 DEG C, stir 20 minutes after adding reverse-extraction agent, then proceed to the standing separation after 1 hour of separating funnel.
Embodiment 2
The present embodiment is identical with principle of work with the setting of embodiment 1, and difference is:
(1) efficient extraction agent preparation: measure that 500ml tri-is pungent, certain herbaceous plants with big flowers alkyl tertiary amine respectively, 400ml sulfonated kerosene, 100ml n-Octanol adds in 5000ml four-hole boiling flask, starts and stirs and heat up.
(2) complexometric extraction: when extraction agent temperature is at 30-40 DEG C, add the H acid mother liquor of 4000ml, adding 50-55g concentration under whipped state is 98% sulfuric acid, process temperature is 45 DEG C, stir and proceed to separating funnel after 20 minutes, leave standstill after 0.5 hour, isolate the inorganic salt solution of lower floor's clear, the acid complex layer on upper strata waits until subsequent disposal.
(3) back extraction: the acid complex layer after the separation in separating funnel is proceeded in four-hole boiling flask, be warming up to 50 DEG C, the slow ammonia soln (mass percent is 25%) adding about 1.4 moles, make organic aqueous phase pH at 9.0-10, process temperature is 55-65 DEG C, stir 20 minutes after adding reverse-extraction agent, then proceed to the standing separation after 1 hour of separating funnel.
Embodiment 3
The present embodiment is identical with principle of work with the setting of embodiment 1, and difference is:
(1) efficient extraction agent preparation: measure that 600ml tri-is pungent, certain herbaceous plants with big flowers alkyl tertiary amine respectively, 700ml sulfonated kerosene, 150ml n-Octanol adds in 5000ml four-hole boiling flask, starts and stirs and heat up.
(2) complexometric extraction: when extraction agent temperature is at 30-40 DEG C, add the H acid mother liquor of 3650ml, adding 50-55g concentration under whipped state is 98% sulfuric acid, process temperature is 50 DEG C, stir and proceed to separating funnel after 30 minutes, leave standstill after 0.5 hour, isolate the inorganic salt solution of lower floor's clear, the acid complex layer on upper strata waits until subsequent disposal.
(3) back extraction: the acid complex layer after the separation in separating funnel is proceeded in four-hole boiling flask, be warming up to 55 DEG C, the slow ammonia soln (mass percent is 20%) adding about 1.4 moles, make organic aqueous phase pH at 9.0-10, process temperature is 55-65 DEG C, stir 20 minutes after adding reverse-extraction agent, then proceed to the standing separation after 1 hour of separating funnel.
Embodiment 4
This enforcement is identical with principle of work with the setting of embodiment 1, and difference is:
(1) efficient extraction agent preparation: measure that 500ml tri-is pungent, certain herbaceous plants with big flowers alkyl tertiary amine respectively, 380ml dodecylbenzene, 120ml n-Octanol adds in 5000ml four-hole boiling flask, starts and stirs and heat up.
(2) complexometric extraction: when extraction agent temperature is at 30-40 DEG C, add the H acid mother liquor of 4000ml, adding 50-55g concentration under whipped state is 98% sulfuric acid, process temperature is 45 DEG C, stir and proceed to separating funnel after 20 minutes, leave standstill after 0.5 hour, isolate the inorganic salt solution of lower floor's clear, the acid complex layer on upper strata waits until subsequent disposal.
(3) back extraction: the acid complex layer after the separation in separating funnel is proceeded in four-hole boiling flask, is warming up to 50 DEG C, the slow Ca(OH adding about 1.4 moles)
2(dry powder), make organic aqueous phase pH at 9-10, process temperature is 50-55 DEG C, stirs 40 minutes after adding reverse-extraction agent, then proceeds to the standing separation after 1 hour of separating funnel.
Embodiment 5
The present embodiment is identical with principle of work with the setting of embodiment 1, and difference is:
(1) efficient extraction agent preparation: measure 200ml dodeca-tertiary amine respectively, 300ml dodecylbenzene, 50ml tributyl phosphate adds in 3000ml four-hole boiling flask, starts and stirs and heat up.
(2) complexometric extraction: when extraction agent temperature is at 30-40 DEG C, add the H acid mother liquor of 2750ml, adding 50-55g concentration under whipped state is 98% sulfuric acid, process temperature is 30 DEG C, stir and proceed to separating funnel after 30 minutes, leave standstill after 1.0 hours, isolate the inorganic salt solution of lower floor's clear, the acid complex layer on upper strata waits until subsequent disposal.
(3) back extraction: the acid complex layer after the separation in separating funnel is proceeded in four-hole boiling flask, be warming up to 50 DEG C, the slow MgO(dry powder adding about 1.5 moles), make organic aqueous phase pH at 7-9, process temperature is 50-55 DEG C, stir 40 minutes after adding reverse-extraction agent, then proceed to the standing separation after 1 hour of separating funnel.
For embodiment 1, the effect of the application is slightly poor, after process, the tributyl phosphate having 7-8mL in the drainage of every 1000mL remains, the volume of organic sour water can float, therefore, in subsequent processes accordingly to some extent, concentrated cost and comprehensive treating process cost can comparatively embodiment 1 be slightly high, but still lower than the extracting process of routine.
Embodiment 6
This enforcement is identical with principle of work with the setting of embodiment 1, and difference is:
(1) efficient extraction agent preparation: measure that 500ml tri-is pungent, certain herbaceous plants with big flowers alkyl tertiary amine respectively, 400ml sulfonated kerosene, 100ml n-Octanol adds in 5000ml four-hole boiling flask, starts and stirs and heat up.
(2) complexometric extraction: when extraction agent temperature is at 30-40 DEG C, add the H acid mother liquor of 4000ml, adding 50-55g concentration under whipped state is 98% sulfuric acid, process temperature is 45 DEG C, stir and proceed to separating funnel after 20 minutes, leave standstill after 0.5 hour, isolate the inorganic salt solution of lower floor's clear, the acid complex layer on upper strata waits until subsequent disposal.
(3) back extraction: the acid complex layer after the separation in separating funnel is proceeded in four-hole boiling flask, is warming up to 50 DEG C, the slow CaCO adding about 1.4 moles
3(dry powder), make organic aqueous phase pH at 8-10, process temperature is 50-55 DEG C, stirs 40 minutes after adding reverse-extraction agent, then proceeds to the standing separation after 1 hour of separating funnel.
Embodiment 7
This enforcement is identical with principle of work with the setting of embodiment 1, and difference is:
(1) efficient extraction agent preparation: measure 200ml dodeca-tertiary amine respectively, 300ml dodecylbenzene, 50ml tributyl phosphate adds in 3000ml four-hole boiling flask, starts and stirs and heat up.
(2) complexometric extraction: when extraction agent temperature is at 30-40 DEG C, add the H acid mother liquor of 2750ml, adding 50-55g concentration under whipped state is 98% sulfuric acid, process temperature is 30 DEG C, stir and proceed to separating funnel after 30 minutes, leave standstill after 1.0 hours, isolate the inorganic salt solution of lower floor's clear, the acid complex layer on upper strata waits until subsequent disposal.
(3) back extraction: the acid complex layer after the separation in separating funnel is proceeded in four-hole boiling flask, be warming up to 50 DEG C, the slow NaOH solution (mass percent is 25%) adding about 1.4 moles, make organic aqueous phase pH at 10-11, process temperature is 55-65 DEG C, stir 20 minutes after adding reverse-extraction agent, then proceed to the standing separation after 1 hour of separating funnel.
Embodiment 8
This enforcement is identical with principle of work with the setting of embodiment 1, and difference is:
(1) efficient extraction agent preparation: measure that 400ml tri-is pungent, certain herbaceous plants with big flowers alkyl tertiary amine respectively, 500ml dodecylbenzene, 100ml tributyl phosphate adds in 5000ml four-hole boiling flask, starts and stirs and heat up.
(2) complexometric extraction: when extraction agent temperature is at 30-40 DEG C, add the H acid mother liquor of 4000ml, adding 50-55g concentration under whipped state is 98% sulfuric acid, process temperature is 45 DEG C, stir and proceed to separating funnel after 20 minutes, leave standstill after 0.5 hour, isolate the inorganic salt solution of lower floor's clear, the acid complex layer on upper strata waits until subsequent disposal.
(3) back extraction: the acid complex layer after the separation in separating funnel is proceeded in four-hole boiling flask, be warming up to 50 DEG C, the slow CaO(dry powder adding about 1.4 moles), make organic aqueous phase pH at 7-9, process temperature is 50-55 DEG C, stir 40 minutes after adding reverse-extraction agent, then proceed to standing after the 1 hour point of separation of separating funnel.
Comparative example
The technical scheme provided with CN101780994A, CN104086017A embodiment as a comparison.
Effect analysis
The various embodiments described above are reclaimed the product obtained and compares analysis, specifically as shown in table 1.
Effect comparison table under table 1 different technology conditions
。
As can be seen from Table 1, in the acid complexation extraction described by comparative example, its profit is compared and is respectively 1:1,1:2, and profit of the present invention is in a ratio of 1:4, extract 2-4 times that usefulness is the two, reverse-extraction agent is the key factor of extraction cost, and adopt NaOH back extraction, its cost is 2 times of ammoniacal liquor back extraction.Simultaneously, adopt extraction agent provided by the present invention, extraction usefulness can well be improved, reduce the organic residue of the inorganic sour water of extraction, thus effectively by the salt extraction contained in mother liquor out and remove, final drainage is inorganic salt solution (COD reduces by more than 90%), this drainage can directly drop into follow-up application, and not affecting the quality of subsequent product, organic water phase volume V reduces, thus follow-up concentrated cost is controlled; Meanwhile, no longer containing organism in acid complex compound, thus saltiness is made relatively to be increased to 3-5 percentage point.Because the present invention have employed PH terminal point control to back extraction terminal, the loss of its extraction agent is all at 1-1.5 ‰, and organic aqueous phase oil length is low, and comprehensive cost declines.
Above content is the further description done provided technical scheme in conjunction with the preferred embodiment of the present invention; can not assert that the present invention specifically implements to be confined to these explanations above-mentioned; for general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (9)
1. one kind for extracting the efficient extraction agent of H acid mother liquor, it is characterized in that: described efficient extraction agent is made up of complexing agent, thinner and solubility promoter, complexing agent is wherein tertiary amines solvent, and thinner is sulfonated kerosene or dodecylbenzene, and solubility promoter is tributyl phosphate or n-Octanol.
2. a kind of efficient extraction agent for extracting H acid mother liquor as claimed in claim 1, is characterized in that: described tertiary amines solvent is dodeca-tertiary amine or three pungent, certain herbaceous plants with big flowers base tertiary amines.
3. a kind of efficient extraction agent for extracting H acid mother liquor as claimed in claim 1 or 2, it is characterized in that: described efficient extraction agent is by three pungent, certain herbaceous plants with big flowers base tertiary amines, sulfonated kerosene and octanol ternary component mixture form, its mixture volume ratio is: three pungent, certain herbaceous plants with big flowers base tertiary amine 2-6 parts, sulfonated kerosene 3-7 part, octanol 0.5-1.5 part.
4. a kind of efficient extraction agent for extracting H acid mother liquor as claimed in claim 3, it is characterized in that, described three pungent, certain herbaceous plants with big flowers base tertiary amines, the mixture volume ratio of sulfonated kerosene and octanol is: 5:4:1.
5. a H acid mother liquor extracting process, it is characterized in that: the method is made up of extraction and back-extraction, described extraction with H acid mother liquor for handling object, and adopt efficient extraction agent, this efficient extraction agent is made up of tertiary amines solvent, thinner and solubility promoter, and the profit of extraction agent and H acid mother liquor is in a ratio of 1:1-5, and process temperature is 30-50 DEG C, extraction process acid adding amount is identical with tertiary amines solvent mole number, and after extraction, H acid mother liquor forms inorganic salt solution and acid complex layer; Remove inorganic salt solution, acid complex layer is carried out back extraction; In described strip stages, reverse-extraction agent is MgO, CaO, CaCO
3, Ca(OH)
2, NaOH, NH
3 .h
2one in O, back extraction temperature 25-65 DEG C, the organic aqueous phase pH to 7-11 being added into back extraction formation of reverse-extraction agent.
6. a kind of H acid mother liquor extracting process as claimed in claim 5, is characterized in that: described tertiary amines solvent is dodeca-tertiary amine or three pungent, certain herbaceous plants with big flowers alkyl tertiary amines, and thinner is sulfonated kerosene or dodecylbenzene, and solubility promoter is tributyl phosphate or n-Octanol.
7. a kind of H acid mother liquor extracting process as described in claim 5 or 6, it is characterized in that: described tertiary amines solvent is three pungent, certain herbaceous plants with big flowers alkyl tertiary amines, thinner is sulfonated kerosene, solubility promoter is n-Octanol, three pungent, certain herbaceous plants with big flowers alkyl tertiary amine is 5:4:1 with the mol ratio that mixes of sulfonated kerosene, n-Octanol three, and the profit of extraction agent and H acid mother liquor is in a ratio of 1:4.
8. a kind of H acid mother liquor extracting process as claimed in claim 5, it is characterized in that: when described reverse-extraction agent is NaOH, back extraction temperature 50-60 DEG C, concentration of anti-stripping agent is 15-40%, the organic aqueous phase pH to 10-11 being added into back extraction formation of reverse-extraction agent.
9. a kind of H acid mother liquor extracting process as claimed in claim 5, is characterized in that: described reverse-extraction agent is NH
3 .h
2during O, back extraction temperature 50-60 DEG C, concentration of anti-stripping agent is 15-25%, the organic aqueous phase pH to 9-10 being added into back extraction formation of reverse-extraction agent.
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| CN105753744A (en) * | 2016-02-29 | 2016-07-13 | 江苏吉华化工有限公司 | Energy-saving H-acid preparation device |
| CN105948350A (en) * | 2016-04-26 | 2016-09-21 | 天津理工大学 | Recycling process and system for high-salt and high-concentration non-biodegradable organic matter-containing H acid wastewater |
| CN107118138A (en) * | 2017-05-16 | 2017-09-01 | 扬州联博药业有限公司 | A kind of method that sulfosalicylic acid is reclaimed in the alkalization mother liquor from fortimicin |
| CN107602430A (en) * | 2017-11-02 | 2018-01-19 | 响水恒利达科技化工有限公司 | A kind of method of extraction recovery tobias acid in waste water from tobias acid |
| CN109052776A (en) * | 2018-08-16 | 2018-12-21 | 山东裕源集团有限公司 | A kind of H acid producing waste water integrated conduct method |
| 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 |
| CN110294561A (en) * | 2019-06-13 | 2019-10-01 | 北京国电富通科技发展有限责任公司 | The processing method of extractant and high phenol waste water with high salt |
| CN110357796A (en) * | 2019-07-03 | 2019-10-22 | 山东万山集团有限公司 | The preparation method of continuous extraction process and extractant, naphthalene sulfonic acids and water-reducing agent |
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| CN105753744A (en) * | 2016-02-29 | 2016-07-13 | 江苏吉华化工有限公司 | Energy-saving H-acid preparation device |
| CN105753744B (en) * | 2016-02-29 | 2017-06-16 | 江苏吉华化工有限公司 | A kind of H acid preparation facilities with energy-saving effect |
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| CN105948350B (en) * | 2016-04-26 | 2019-04-05 | 天津理工大学 | H acid waste water reclaiming technique and system containing high-concentration hardly-degradable organic matter with high salt |
| CN107118138A (en) * | 2017-05-16 | 2017-09-01 | 扬州联博药业有限公司 | A kind of method that sulfosalicylic acid is reclaimed in the alkalization mother liquor from fortimicin |
| CN107118138B (en) * | 2017-05-16 | 2022-06-28 | 扬州联博药业有限公司 | Method for recovering sulfosalicylic acid from doxycycline alkalization mother liquor |
| CN107602430A (en) * | 2017-11-02 | 2018-01-19 | 响水恒利达科技化工有限公司 | A kind of method of extraction recovery tobias acid in waste water from tobias acid |
| 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 |
| CN109052776A (en) * | 2018-08-16 | 2018-12-21 | 山东裕源集团有限公司 | A kind of H acid producing waste water integrated conduct method |
| 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 |
| CN110294561A (en) * | 2019-06-13 | 2019-10-01 | 北京国电富通科技发展有限责任公司 | The processing method of extractant and high phenol waste water with high salt |
| CN110357796A (en) * | 2019-07-03 | 2019-10-22 | 山东万山集团有限公司 | The preparation method of continuous extraction process and extractant, naphthalene sulfonic acids and water-reducing agent |
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