CN109052776A - A kind of H acid producing waste water integrated conduct method - Google Patents
A kind of H acid producing waste water integrated conduct method Download PDFInfo
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- CN109052776A CN109052776A CN201810933255.1A CN201810933255A CN109052776A CN 109052776 A CN109052776 A CN 109052776A CN 201810933255 A CN201810933255 A CN 201810933255A CN 109052776 A CN109052776 A CN 109052776A
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- waste water
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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
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
-
- 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
-
- 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
- C01D5/16—Purification
-
- 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
- C02F1/26—Treatment of water, waste water, or sewage by extraction
-
- 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
- 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
Abstract
The present invention relates to technical field of waste water processing, and in particular to a kind of H acid producing waste water integrated conduct method, comprising the following steps: (1) collects T acid isolation waste water respectively and H acid isolates waste water;(2) it takes T acid to isolate waste water, adds extractant, collect water phase and extraction phase respectively;Extraction phase is taken, liquid alkaline is added, recycles extractant;Water intaking phase, adjusts pH, and the evaporation concentrated solution of evaporation, the evaporation recycle-water of collection, collection passes through crystallization, obtains ammonium sulfate;(3) it takes H acid to isolate waste water, extractant is added after adjusting pH, collect water phase and extraction phase respectively;Extraction phase is taken, liquid alkaline is added and recycles extractant;Water intaking phase, adjusts pH, and the evaporation concentrated solution of evaporation, the evaporation recycle-water of collection, collection passes through crystallization, obtains sodium sulphate.Using processing method of the invention, the independent processing that waste water and H acid isolation waste water are isolated to T acid is realized, extraction efficiency is high, realizes the recycling to waste water and the recycling of inorganic salts.
Description
Technical field
The present invention relates to technical field of waste water processing, and in particular to a kind of H acid producing waste water integrated conduct method.
Background technique
H acid is a kind of important dyestuff intermediate, generates a large amount of naphthalene sulfonic acids system class waste water, the waste water in production process
COD value is high, coloration is deep, pH 2, belongs to the organic wastewater of high concentration, highly acidity, high salinity and high chroma.H acid producing waste water master
T acid maceration stage and H acid maceration stage are come from, in the prior art when treating wastewater usually generates the two production phases
Wastewater collection to together using extractant extraction, UF membrane, MVR evaporation process, but there are some for above-mentioned processing mode
Disadvantage: (1) H acid technique waste water concentrates in together that wastewater flow rate is very big, and the extractant used in the prior art is to organic in waste water
The effect of extracting of object is poor, and extraction water outlet COD is higher;(2) contain a large amount of inorganic salts in waste water, MVR technique has only recycled portion
Point inorganic salts, there are still a large amount of inorganic salts in waste water, waste water can not recovery, direct emission causes the wave of a large amount of inorganic salts
Take;It is therefore desirable to establish a kind of H acid producing waste water integrated conduct method.
Summary of the invention
It is an object of the invention to be: in view of the deficienciess of the prior art, providing a kind of H acid producing waste water integrated treatment
Method, the processing method improve effect of extracting, reduce extraction water outlet COD, recycled the inorganic salts in waste water and realized
The recycling of waste water.
To achieve the goals above, the technical scheme is that
A kind of H acid producing waste water integrated conduct method, the treating method comprises following steps:
(1) T acid isolation waste water is collected respectively and H acid isolates waste water;
(2) it takes T acid in step (1) to isolate waste water, extractant is added after adjusting pH, stir, extract 2- under the conditions of 25-55 DEG C
3h collects water phase and extraction phase respectively;Extraction phase is taken, liquid alkaline is added, adjusts pH to 8-9, stirring stands 2-2.5h, recycling extraction
Agent;Water intaking phase, adjusts pH to 6-7, is evaporated processing, the evaporation recycle-water of collection is for denitration link and reduction link, collection
Evaporation concentrated solution under the conditions of 110-125 DEG C by crystallization, obtain ammonium sulfate;
(3) it takes H acid in step (1) to isolate waste water, extractant is added after adjusting pH, stir, extract 1- under the conditions of 30-55 DEG C
2h collects water phase and extraction phase respectively;Extraction phase is taken, liquid alkaline is added, adjusts pH to 8-9, stirring stands 2-3h, recycles extractant;
Water intaking phase, adjusts pH to 6-7, is evaporated processing, and the evaporation recycle-water of collection isolates bottom water, the evaporation and concentration of collection for H acid
Liquid, by crystallization, obtains sodium sulphate under the conditions of 105-120 DEG C.
As an improvement technical solution, the volume ratio of T acid isolation waste water and extractant is 4-6 in the step (2):
1-1.5, the extractant is by dodeca-tertiary amine, sulfonated kerosene and tributyl phosphate according to the ratio of volume ratio 1-3:4-7:0.5-1
It mixes.
As a kind of perferred technical scheme, the extractant by dodeca-tertiary amine, sulfonated kerosene and tributyl phosphate according to
The ratio of volume ratio 2:5:0.8 mixes.
As an improvement technical solution, the volume ratio of H acid isolation waste water and extractant is 5-7 in the step (3):
1-1.5, the extractant by trioctylamine, sulfonated kerosene and n-octyl alcohol according to volume ratio 2-3:5-8:0.2-1 ratio mixing and
At.
As a kind of perferred technical scheme, the extractant is by trioctylamine, sulfonated kerosene and n-octyl alcohol according to volume ratio
2.5:7:0.5 ratio mix.
As an improvement technical solution, step (2) T acid isolation waste water tune pH to 1-2 in extraction.
As an improvement technical solution, step (3) H acid isolation waste water tune pH to 3-4 in extraction.
As an improvement technical solution, the mass concentration of liquid alkaline is 15%- in the step (2) and step (3)
20%.
As an improvement technical solution, temperature of the water phase collected in the step (2) in evaporation process is 90-
100 DEG C, pressure 0.3-0.45mpa, evaporation time 8-12h.
As an improvement technical solution, temperature of the water phase collected in the step (3) in evaporation process be
100-115 DEG C, pressure 0.25-0.4mpa, evaporation time 10-12h.
The invention adopts the above technical scheme, with prior art volume ratio, has the advantage that
(1) T acid is isolated waste water by the present invention and H acid isolation waste water is respectively processed, and T acid isolates waste water by 12 uncles
Amine, sulfonated kerosene and tributyl phosphate combination extractant extracted under conditions of 25-55 DEG C, H acid isolate waste water by trioctylamine,
It is extracted under conditions of 30-55 DEG C of extractant that sulfonated kerosene and n-octyl alcohol combine, dodeca-tertiary amine, sulfonated kerosene and tributyl phosphate
The extractant of combined extractant and trioctylamine, sulfonated kerosene and n-octyl alcohol combination has highly selective, and extraction efficiency is high,
Extraction time is short, is more conducive to T acid isolation waste water and H acid isolates useless Organic substance in water and enters extractant phase;Extractant easily regenerates,
The liquid alkaline that mass concentration is 15-20% is respectively adopted when back extraction to be stripped, back extraction ratio is high, and no emulsion was stripped
Journey interface is clear, solvent-free entrainment phenomenon.
(2) after the extraction of respective extractant, the water phase of collection is passed through respectively for T acid isolation waste water and H acid isolation waste water
Evaporation, the evaporation recycle-water clear respectively collected do not contain organic matter, and COD value is low, are respectively used to H acid production process, real
Show the recycling of waste water, also reduces scale wastewater treatment burden;The evaporation concentrated solution respectively collected is obtained by crystallization treatment
Byproduct of ammonium sulfate and sodium sulfate byproduct have been arrived, the recycling to inorganic salts in waste water is realized, has greatly reduced evaporation recycling
Content in water in inorganic salts, byproduct of ammonium sulfate and sodium sulfate byproduct are sold, and bring economic interests for enterprise.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, the present invention is carried out further detailed
Explanation.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not intended to limit the present invention.
Embodiment 1
A kind of H acid producing waste water integrated conduct method, comprising the following steps:
(1) T acid isolation waste water is collected respectively and H acid isolates waste water;
(2) it takes T acid in step (1) to isolate waste water, the extractant (body of T acid isolation waste water and extractant is added after adjusting pH to 1
Product is than being 4:1, and extractant is by dodeca-tertiary amine, sulfonated kerosene and tributyl phosphate according to the ratio mixing of volume ratio 1.5:4:0.5
Into), 20min is stirred, extracts 2h under the conditions of 25 DEG C, collects water phase and extraction phase respectively;Extraction phase is taken, mass concentration is added
For 15% liquid alkaline, pH to 8 is adjusted, stirring stands 2h, recycles extractant;It fetches water phase, adjusts pH to 6, being evaporated processing, (temperature is
90 DEG C, pressure 0.3mpa, evaporation time 8h), the evaporation recycle-water of collection for denitration link and restores link, collection
Evaporation concentrated solution, by crystallization, obtains ammonium sulfate under the conditions of 110 DEG C;
(3) it takes H acid in step (1) to isolate waste water, the extractant (body of H acid isolation waste water and extractant is added after adjusting pH to 3
Product ratio is 5:1, and extractant is mixed by trioctylamine, sulfonated kerosene and n-octyl alcohol according to the ratio of volume ratio 2:5:0.2), it stirs
20min is mixed, extracts 1h under the conditions of 30 DEG C, collects water phase and extraction phase respectively;Extraction phase is taken, addition mass concentration is 15% liquid
Alkali adjusts pH to 8, and stirring stands 2h, recycles extractant;Water intaking phase, adjusts pH to 6, and being evaporated processing, (temperature is 100 DEG C, pressure
Power is 0.25mpa, evaporation time 10h), the evaporation recycle-water of collection isolates bottom water for H acid, and the evaporation concentrated solution of collection exists
By crystallization under the conditions of 105 DEG C, sodium sulphate is obtained.
Embodiment 2
A kind of H acid producing waste water integrated conduct method, comprising the following steps:
(1) T acid isolation waste water is collected respectively and H acid isolates waste water;
(2) it takes in step (1) T acid to isolate waste water, adjusts and extractant is added after pH to 1.5 (T acid isolates waste water and extractant
Volume ratio is 5:1.5, and extractant is mixed by dodeca-tertiary amine, sulfonated kerosene and tributyl phosphate according to the ratio of volume ratio 2:5:0.8
Close), 20-30min is stirred, extracts 2.5h under the conditions of 45 DEG C, collects water phase and extraction phase respectively;Extraction phase is taken, is added
Mass concentration is 18% liquid alkaline, adjusts pH to 8.5, and stirring stands 2.3h, recycles extractant;Water intaking phase, adjusts pH to 6.5, is steamed
Hair processing (temperature be 95 DEG C, pressure 0.35mpa, evaporation time 10h), the evaporation recycle-water of collection for denitration link and
Link is restored, the evaporation concentrated solution of collection, by crystallization, obtains ammonium sulfate under the conditions of 115 DEG C;
(3) it takes in step (1) H acid to isolate waste water, adjusts and extractant is added after pH to 3.5 (H acid isolates waste water and extractant
Volume ratio is 6:1.5, extractant by trioctylamine, sulfonated kerosene and n-octyl alcohol according to the ratio mixing of volume ratio 2.5:7:0.5 and
At), 25min is stirred, extracts 1.5h under the conditions of 42 DEG C, collects water phase and extraction phase respectively;Extraction phase is taken, mass concentration is added
For 18% liquid alkaline, pH to 8.7 is adjusted, stirring stands 2.5h, recycles extractant;Water intaking phase, adjusts pH to 6.8, is evaporated processing
(temperature is 108 DEG C, pressure 0.35mpa, evaporation time 11h), the evaporation recycle-water of collection isolates bottom water for H acid, receives
The evaporation concentrated solution of collection, by crystallization, obtains sodium sulphate under the conditions of 115 DEG C.
Embodiment 3
A kind of H acid producing waste water integrated conduct method, comprising the following steps:
(1) T acid isolation waste water is collected respectively and H acid isolates waste water;
(2) it takes T acid in step (1) to isolate waste water, the extractant (body of T acid isolation waste water and extractant is added after adjusting pH to 2
Product than be 6:1.5, extractant by dodeca-tertiary amine, sulfonated kerosene and tributyl phosphate according to volume ratio 3:7:1 ratio mixing and
At), 30min is stirred, extracts 3h under the conditions of 53 DEG C, collects water phase and extraction phase respectively;Extraction phase is taken, mass concentration, which is added, is
20% liquid alkaline adjusts pH to 9, and stirring stands 2.5h, recycles extractant;It fetches water phase, adjusts pH to 7, being evaporated processing, (temperature is
100 DEG C, pressure 0.45mpa, evaporation time 12h), the evaporation recycle-water of collection is received for denitration link and reduction link
The evaporation concentrated solution of collection, by crystallization, obtains ammonium sulfate under the conditions of 125 DEG C;
(3) it takes H acid in step (1) to isolate waste water, the extractant (body of H acid isolation waste water and extractant is added after adjusting pH to 4
Product ratio is 7:1.5, and extractant is mixed by trioctylamine, sulfonated kerosene and n-octyl alcohol according to the ratio of volume ratio 3:8:1), it stirs
30min is mixed, extracts 2h under the conditions of 55 DEG C, collects water phase and extraction phase respectively;Extraction phase is taken, addition mass concentration is 20% liquid
Alkali adjusts pH to 9, and stirring stands 3h, recycles extractant;Water intaking phase, adjusts pH to 7, and being evaporated processing, (temperature is 115 DEG C, pressure
Power is 0.4mpa, evaporation time 12h), the evaporation recycle-water of collection isolates bottom water for H acid, and the evaporation concentrated solution of collection exists
By crystallization under the conditions of 120 DEG C, sodium sulphate is obtained.
In order to more preferably prove that processing method of the invention has preferable effect, the present invention is also made that several comparative examples.
Comparative example 1
Unlike the operation of embodiment 2, in step (2) when the waste water extraction of T acid isolation, extractant is dodeca-tertiary amine and sulphur
Change kerosene, in step (3) when the waste water extraction of T acid isolation, extractant is trioctylamine and sulfonated kerosene, remaining operation is identical.
Comparative example 2
T acid is isolated into waste water and H acid isolates wastewater collection to together, extractant (trialkyl tertiary amine and sulfonated kerosene is added
Mixed according to the ratio of volume ratio 1:2), it is filtered using film, lye back extraction, MVR evaporation operation.
Table 1 is waste water physicochemical property when H acid producing waste water is untreated, and table 2 and table 3 are 1 He of embodiment 1-3 and comparative example
The physicochemical property index of water phase and distillation recovery water after distillation after 2 extractions.
1 H acid producing waste water main physical and chemical of table
Water phase physicochemical property after the extraction of 2 H acid producing waste water of table
Recycle-water physicochemical property is evaporated after water phase evaporation after the extraction of 3 H acid producing waste water of table
By table 1, data in table 2 and table 3 it can be concluded that, the T acid of collection is isolated waste water by processing method of the invention
Corresponding extractant is respectively adopted with H acid isolation waste water to be extracted, realizes and T acid is isolated in waste water and H acid isolation waste water
Effective extraction of organic matter, then water phase extracted is evaporated to the recycling realized to ammonium sulfate in T acid isolation waste water, H
The recycling of sodium sulphate in acid isolation waste water, the evaporation recycle-water COD collected through pervaporation is low, BOD is low, evaporates the salt in recycle-water
Point content is low, and T acid, which isolates the evaporation recycle-water that waste water is collected after operation, can be used for denitration link and reduction link, H acid from
The evaporation recycle-water that analysis waste water is collected after aforesaid operations can be used for H acid maceration stage;
By 2 data of table it can be concluded that, 1-3 of embodiment of the present invention water phase extracted and the water extracted of comparative example 1 and 2
It compares, COD the and BOD value that water outlet is extracted in embodiment 1-3 is low;By 3 data of table it can be concluded that, 1-3 of the embodiment of the present invention
For the evaporation recycle-water that water phase extracted is recycled through pervaporation compared with comparative example 1 and 2, embodiment 1-3 evaporates the COD of recycle-water
Low, BOD is low, and evaporate the salinity in recycle-water compared in comparative example 1 and 2 evaporate recycle-water content it is few, T acid isolate waste water warp
The evaporation recycle-water pH of processing recycling is crossed in 7.3-8, evaporation recycle-water pH of the H acid isolation waste water by processing recycling, can in 2-3
For the different links of H acid production, the recycling to waste water is realized, the consumption to water resource is greatly reduced.
This patent is not limited to above-mentioned specific embodiment, those skilled in the art from the above idea,
Without creative labor, made various transformation are all fallen within the protection scope of this patent.
Claims (10)
1. a kind of H acid producing waste water integrated conduct method, it is characterised in that the treating method comprises following steps:
(1) T acid isolation waste water is collected respectively and H acid isolates waste water;
(2) it takes T acid in step (1) to isolate waste water, extractant is added after adjusting pH, stir, extract 2-3h under the conditions of 25-55 DEG C,
Water phase and extraction phase are collected respectively;Extraction phase is taken, liquid alkaline is added, adjusts pH to 8-9, stirring stands 2-2.5h, recycles extractant;
Water intaking phase, adjusts pH to 6-7, is evaporated processing, the evaporation recycle-water of collection is for denitration link and reduction link, the steaming of collection
Concentrate is sent out under the conditions of 110-125 DEG C by crystallization, obtains ammonium sulfate;
(3) it takes H acid in step (1) to isolate waste water, extractant is added after adjusting pH, stir, extract 1-2h under the conditions of 30-55 DEG C,
Water phase and extraction phase are collected respectively;Extraction phase is taken, liquid alkaline is added, adjusts pH to 8-9, stirring stands 2-3h, recycles extractant;It takes
Water phase adjusts pH to 6-7, is evaporated processing, and the evaporation recycle-water of collection isolates bottom water, the evaporation concentrated solution of collection for H acid
By crystallization under the conditions of 105-120 DEG C, sodium sulphate is obtained.
2. a kind of H acid producing waste water integrated conduct method according to claim 1, it is characterised in that: in the step (2)
It is 4-6:1-1.5 that T acid, which isolates waste water and the volume ratio of extractant, and the extractant is by dodeca-tertiary amine, sulfonated kerosene and tricresyl phosphate
Butyl ester is mixed according to the ratio of volume ratio 1-3:4-7:0.5-1.
3. a kind of H acid producing waste water integrated conduct method according to claim 2, it is characterised in that: the extractant by
Dodeca-tertiary amine, sulfonated kerosene and tributyl phosphate are mixed according to the ratio of volume ratio 2:5:0.8.
4. a kind of H acid producing waste water integrated conduct method according to claim 1, it is characterised in that: in the step (3)
It is 5-7:1-1.5 that H acid, which isolates waste water and the volume ratio of extractant, and the extractant is pressed by trioctylamine, sulfonated kerosene and n-octyl alcohol
It is mixed according to the ratio of volume ratio 2-3:5-8:0.2-1.
5. a kind of H acid producing waste water integrated conduct method according to claim 4, it is characterised in that: the extractant by
Trioctylamine, sulfonated kerosene and n-octyl alcohol are mixed according to the ratio of volume ratio 2.5:7:0.5.
6. a kind of H acid producing waste water integrated conduct method according to claim 1, it is characterised in that: step (2) T
Acid isolation waste water tune pH to 1-2 in extraction.
7. a kind of H acid producing waste water integrated conduct method according to claim 1, it is characterised in that: step (3) H
Acid isolation waste water tune pH to 3-4 in extraction.
8. a kind of H acid producing waste water integrated conduct method according to claim 7, it is characterised in that: the step (2) and
The mass concentration of liquid alkaline is 15%-20% in step (3).
9. a kind of H acid producing waste water integrated conduct method according to claim 1, it is characterised in that: in the step (2)
Temperature of the water phase of collection in evaporation process is 90-100 DEG C, pressure 0.3-0.45mpa, evaporation time 8-12h.
10. a kind of H acid producing waste water integrated conduct method according to claim 1, it is characterised in that: the step (3)
Temperature of the water phase of middle collection in evaporation process is 100-115 DEG C, pressure 0.25-0.4mpa, evaporation time 10-12h.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112010455A (en) * | 2019-05-30 | 2020-12-01 | 浙江闰土研究院有限公司 | Method for treating denitration material in H acid production process |
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CN105293806A (en) * | 2015-11-13 | 2016-02-03 | 中蓝连海设计研究院 | T acid separation mother liquor waste water comprehensive treatment method |
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JPH0383960A (en) * | 1989-08-25 | 1991-04-09 | Dai Ichi Kogyo Seiyaku Co Ltd | Production of beta-naphthalenesulfonic acid |
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CN112010455A (en) * | 2019-05-30 | 2020-12-01 | 浙江闰土研究院有限公司 | Method for treating denitration material in H acid production process |
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Application publication date: 20181221 |