CN109626696A - A kind of recovery processing technique of vulcanized sodium and sodium sulfite composite waste - Google Patents
A kind of recovery processing technique of vulcanized sodium and sodium sulfite composite waste Download PDFInfo
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- CN109626696A CN109626696A CN201910085253.6A CN201910085253A CN109626696A CN 109626696 A CN109626696 A CN 109626696A CN 201910085253 A CN201910085253 A CN 201910085253A CN 109626696 A CN109626696 A CN 109626696A
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- Prior art keywords
- sodium
- sodium sulfite
- waste
- kettle
- waste water
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Classifications
-
- 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
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/0253—Preparation of sulfur; Purification from non-gaseous sulfur compounds other than sulfides or materials containing such sulfides
-
- 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
- C02F1/041—Treatment of water, waste water, or sewage by heating by distillation or evaporation by means of vapour compression
-
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/101—Sulfur compounds
Abstract
The present invention provides the recovery processing technique of a kind of vulcanized sodium and sodium sulfite composite waste, characterized by the following steps: the first step, at room temperature, alkaline waste water containing a large amount of vulcanized sodium and sodium sulfite is slowly added dropwise in the industrial waste acid of mass percent 30%, and the hydrogen sulfide generated in reaction process and sulfur dioxide gas are passed through 30% lye and absorb slot, the lye containing vulcanized sodium and sodium sulfite is then put into paranitroanilinum reduction kettle.One aspect of the present invention has effectively handled the industrial wastewater with high salt of Containing Sulfur sodium and sodium sulfite, and high-salt wastewater is made to be unlikely to be discharged into a large amount of toxic and acid out the hydrogen sulfide of the total pond chance acidic materials generation of waste water and sulfur dioxide gas.The gas will lead to environmental pollution and neighbouring personnel poisoning.On the other hand it is used in the reaction of product using the less salt Sewage treatment set of the Containing Sulfur sodium and sodium sulfite that are generated after absorption, saves the cost of raw material.The technique is to carry out totally enclosed procedure control, and by-product sulphur is sold as byproduct.Reach, environmental protection, economy, there is practicability and validity.
Description
Technical field
The present invention relates to a kind of Containing Sulfur sodium and sodium sulfite strong basicity waste water reclamation to utilize the production for producing crude product sulphur
Technique, specifically for the strong basicity vulcanized sodium and sodium nitrite waste water generated in dehydrogenated thio para-totuidine production process
Handle the production technology of Recovered sulphur.Belong to chemical technology field.
Background technique
Dehydrogenated thio para-totuidine is dyestuff intermediate, should have field than wide.Manufacturer is also various.For waste water
In vulcanized sodium containing strong basicity and sodium sulfite be difficult to handle always.The waste water is discharged into wastewater disposal basin because containing a large amount of reproducibility
Substance is very big to the lethality of anaerobic bacteria and aerobic bacteria.And it encounters acid waste water and can generate a large amount of hydrogen sulfide and dioxy
Change sulphur, very big ground contamination air and the health for influencing people.Crude product sulphur can be manufactured using recycling for waste water, reacted
Para-nitrotoluene has saved cost in production.
Para-nitrotoluene is reduced to para-totuidine in vulcanized sodium system and has been used as in the production of dehydrogenated thio para-totuidine
In a wastewater treatment scheme.Absorbing lye in this way can sufficiently recycle.MVR desalting processing high-salt wastewater is in production run
In, the waste water that processing terminate directly carries out MVR desalting processing after can neutralizing, intermediate interference-free.Environmental protection is increased for country
With the production dynamics of safety, in order to preferably carry out safety and environmental protection control, while market competition is increasingly fierce, produces Gao Pin
The product of matter is imperative.
The producer for producing the dyestuff intermediate both at home and abroad at present is also very much, and market demand is also very big, Market competition,
It is extremely urgent inexpensive good product to be produced under conditions of high-environmental high safety.
Summary of the invention
The technical problem to be solved by the present invention is to, the shortcomings that overcoming the prior art, provide a kind of Containing Sulfur sodium with high salt and
The waste water treatment process of sodium sulfite；It will cause environmental pollution and people containing a large amount of vulcanized sodium and sodium sulfite discharge in waste water
Member's injury.
In order to solve the above technical problems, the present invention provides the recovery processing of a kind of vulcanized sodium and sodium sulfite composite waste
Technique, it is characterised in that the following steps are included:
The alkaline waste water containing a large amount of vulcanized sodium and sodium sulfite is slowly added dropwise into quality for the first step, at room temperature
In the industrial waste acid of percentage 30%, and the hydrogen sulfide generated in reaction process and sulfur dioxide gas are passed through 30% lye and absorbed
Then lye containing vulcanized sodium and sodium sulfite is put into paranitroanilinum reduction kettle by slot；
Second step, with jacket steam reduction reaction kettle temperature degree is gradually increased to 50 in alkaline waste water and industrial waste acid reaction later period ~
60 DEG C, sulphur crystallization is generated successively until vulcanized sodium and sodium sulphite waste water droplet add entirely, and the paranitroanilinum reduction kettle
When middle pressure and lye absorb pressure balance in slot, reduction reaction kettle is warming up to 70 ~ 80 DEG C with jacket steam, persistently stirs 1
The suction filtration bucket for filtering drying integrated kettle will be put into after hour containing the waste liquid that sulphur crystallizes to filter；
Waste liquid after suction filtration is added in neutralization kettle third step, into MVR after adding alkali to be adjusted to neutrality in the neutralization chamber of Xiang Zhonghe kettle
System carries out desalting processing；
Sulphur after separation is crystallized drying and packaging by the 4th step.
The technical solution that the present invention further uses is adds movable top lid filtering bucket, carries out tail gas suction in second step
It receives, exhaust fan sucks remaining a small amount of exhaust gas in sulphur.
Further, in the first step, it is connect in the bottom of wastewater treatment reduction reaction kettle and offers the ring of one group of aperture
Shape pipeline, top connect an air inlet pipe connecting with air-pressure equipment, are slowly passed through air.
Further, in the first step, after reaction in mother liquor PH less than 5.
Further, in third step, the waste water generated after bucket filters that filters is introduced into high-salt wastewater collecting tank,
Then 30% liquid alkaline is added in filtered acid waste water, adjusting PH is 8, then squeezes into MVR concentration, and the condensed water distilled enters
Wastewater equalization pond, abraum salt pack storage.
The beneficial effects of the present invention are: one aspect of the present invention has effectively handled the high salt worker of Containing Sulfur sodium and sodium sulfite
Industry waste water makes high-salt wastewater be unlikely to be discharged into a large amount of toxic and acid out the hydrogen sulfide and two of the total pond chance acidic materials generation of waste water
Sulfur oxide gas.The gas will lead to environmental pollution and neighbouring personnel poisoning.On the other hand the Containing Sulfur generated after absorption is utilized
The less salt Sewage treatment set of sodium and sodium sulfite is used in the reaction of product, and the cost of raw material is saved.The technique is to carry out entirely
Closed procedure control, by-product sulphur are sold as byproduct.Reach, environmental protection, economy, there is practicability and validity.
Detailed description of the invention
Fig. 1 is the process flow chart of the embodiment of the present invention 1.
Fig. 2 is the structural schematic diagram of paranitroanilinum reduction kettle.
Specific embodiment
The present invention is described further with reference to the accompanying drawings and detailed description.
Embodiment 1
The recovery processing technique of a kind of vulcanized sodium and sodium sulfite composite waste provided in this embodiment, is at least wrapped as shown in Figure 1:
Include following steps:
The alkaline waste water containing a large amount of vulcanized sodium and sodium sulfite is slowly added dropwise into quality for the first step, at room temperature
In the industrial waste acid of percentage 30%, and the hydrogen sulfide generated in reaction process and sulfur dioxide gas are passed through 30% lye and absorbed
Then lye containing vulcanized sodium and sodium sulfite is put into paranitroanilinum reduction kettle by slot；In wastewater treatment reduction reaction kettle
Bottom connect the circulating line for offering one group of aperture, top connects an air inlet pipe connecting with air-pressure equipment, slowly leads to
Enter air.As shown in Figure 2.The basicity of waste water and the acidity of spent acid, inventory have been verified the previous provisioning request metering of waste water is added dropwise
Strict measurement guarantees that PH is less than 5 in mother liquor after reaction, and is acid condition.Otherwise the titanium dioxide thiol generated not to the utmost,
Influence the quality of wastewater treatment.
Second step, with jacket steam temperature of reaction kettle is gradually increased to 50 in alkaline waste water and industrial waste acid reaction later period ~
60 DEG C, sulphur crystallization is generated successively until vulcanized sodium and sodium sulphite waste water droplet add entirely, and the paranitroanilinum reduction kettle
When middle pressure and lye absorb pressure balance in slot, reaction kettle is warming up to 70 ~ 80 DEG C with jacket steam, and absorb by lye
Slot opens water vacuum and continues the exhaust gas generated in absorbing reaction kettle, will put containing the waste liquid that sulphur crystallizes after persistently stirring 1 hour
The suction filtration bucket for entering to filter drying integrated kettle filters.Lye absorbs slot slightly vacuum, remaining sulfur dioxide in absorption system.When the step
Between want 1 hour or so, guarantee remaining sulfur dioxide absorb cleanly.
Strength of fluid can not be too high in consersion unit, and the high sulphur generated of concentration is easy agglomeration, the sad filter of material.Simultaneously
Temperature does not get higher than 70-80 DEG C finally yet, and answering the fusing point of sulphur is 114 DEG C, and the too high sulphur of temperature is easy softening, is easy to form big
Block.The mixing speed of reaction kettle cannot be below 60 turns/min, and mixing speed is less than the sulphur of generation all sinks to bottom and is also easy shape
At bulk, lead to bad blowing.The gas generated in its reaction is put into the production of dehydrogenated thio para-totuidine after lye absorbs
Middle para-nitrotoluene reaction kettle, interior vulcanized sodium can react production para-totuidine for doing in DTT production with para-nitrotoluene
Raw material.
Waste liquid after suction filtration is added in neutralization kettle third step, adds alkali to be adjusted to neutrality in the neutralization chamber of Xiang Zhonghe kettle laggard
Enter MVR system and carries out desalting processing；MVR is very high for the oil requirement in high-salt wastewater, so being to be layered very in processing waste water
Important, the para-nitrotoluene and para-totuidine of oiliness cannot be brought into sewage treatment equipment, and otherwise the time has grown influence energy consumption,
Increase processing cost.
Sulphur after separation is crystallized drying and packaging by the 4th step.
It is that will contain a large amount of vulcanized sodium and Asia during the reaction to ensure that reaction carries out in acid condition always
The alkaline waste water of sodium sulphate is slowly added dropwise in 30% industrial waste acid, generates excessive hydrogen sulfide and dioxy during the reaction
Change the entrance 30% lye absorption slot that sulphur is not in time for reaction, pays attention to that vacuum absorption, temperature cannot be used during starting to be added dropwise
Degree control is added at room temperature, and gas extraction duct adds check-valves, prevents liquid alkaline into sucting reaction equipment.
In the step 2 reaction later period, after temperature rise comes, temperature is not so high, and otherwise moisture is all steamed to lye absorption
In slot, while air bubbling not opened excessive, observe in pot subject to volume do not rise, otherwise waste water loss is larger.Increase energy
Consumption.
In second step vacuum process, vacuum degree can not be excessively high, guarantees tiny structure in kettle, a large amount of gas are wanted on liquid level surface
Bubble generates, and liquid level can not break bounds in kettle, and vacuum, air stripping were at 1 hour.Filtering and packaging in device should have
Tail gas absorption cover draws remaining minimal amount of sulfur dioxide, pays attention to good safeguard procedures, crude product sulphur storage.
The present invention contains vulcanized sodium and sodium sulfite primarily with respect to what is generated in dehydrogenated thio para-totuidine production process
High-salt wastewater handled, according to hydrogen sulfide and sulfur dioxide reaction production sulphur basis mechanism and make, two in production
The molar ratio of sulfur oxide and hydrogen sulfide is enough to react the hydrogen sulfide generated completely according to reaction basis mechanism sulfur dioxide close to 1:2, raw
Production operation operation also facilitates feasible.The sulfur dioxide and hydrogen sulfide not reacted can return to circular response in system again.
The spent acid involved in the invention is 30% filtrate spent acid of dehydrogenated thio para-totuidine list sulfonic acid by-product or orchid in production
30% acid absorbed in A tail gas.The lye of neutralization is the liquid alkaline replaced in tail gas absorption, basicity about 20% or so.Waste water
Processing cost can be effectively saved using spent acid and salkali waste completely in treatment process.
It, can be good when confirming pH value as spent acid and salkali waste mixing storage tank should be used in advance using DCS control in production
Control use.Guarantee that solution is at acidity in wastewater treatment reaction process, waste water is at weak base before entering MVR system after processing
Property, also reach and corrective maintenance is acted on.
In second step Vacuum Degassing Process and necessary using air stripping, the water solubility of sulfur dioxide is larger, must
It need can just be caught up with by air stripping and be dissolved in sulfur dioxide in waste water to the greatest extent.Control temperature is to reduce titanium dioxide in 70 DEG C of effects
The solubility of sulphur in water, convenient for degassing.Because the fusing point of by-product sulphur is 114 DEG C, the temperature of degassing can not be excessively high, otherwise sulphur
Crystallization can be very big, increases difficulty to blowing and filtering.The sulfur dioxide gas generated when in order to reduce filtering to human injury,
Degassing time will be at 1 hour or so, and sulphur material place should have device for absorbing tail gas out.Operator is also required to wear labour
Protective articles.Air stripping entrance should connect in reactor bottom, be uniformly distributed, to increase the stripping effect of sulfur dioxide.
The sulphur specific gravity of generation is big compared with water, and the sulfur deposition of generation is in the lower part of reaction kettle, thus the stirring of reaction kettle is imitated
Fruit will get well, can not be too slow, and the concentration for handling water also cannot be excessively high, form evenly dispersed particle convenient for crystallization.
In addition to the implementation, the present invention can also have other embodiments.It is all to use equivalent substitution or equivalent transformation shape
At technical solution, fall within the scope of protection required by the present invention.
Claims (5)
1. the recovery processing technique of a kind of vulcanized sodium and sodium sulfite composite waste, it is characterised in that the following steps are included:
The alkaline waste water containing a large amount of vulcanized sodium and sodium sulfite is slowly added dropwise into quality for the first step, at room temperature
In the industrial waste acid of percentage 30%, and the hydrogen sulfide generated in reaction process and sulfur dioxide gas are passed through 30% lye and absorbed
Then lye containing vulcanized sodium and sodium sulfite is put into paranitroanilinum reduction kettle by slot；
Second step, with jacket steam reduction reaction kettle temperature degree is gradually increased to 50 in alkaline waste water and industrial waste acid reaction later period ~
60 DEG C, sulphur crystallization is generated successively until vulcanized sodium and sodium sulphite waste water droplet add entirely, and the paranitroanilinum reduction kettle
When middle pressure and lye absorb pressure balance in slot, reduction reaction kettle is warming up to 70 ~ 80 DEG C with jacket steam, persistently stirs 1
The suction filtration bucket for filtering drying integrated kettle will be put into after hour containing the waste liquid that sulphur crystallizes to filter；
Waste liquid after suction filtration is added in neutralization kettle third step, into MVR after adding alkali to be adjusted to neutrality in the neutralization chamber of Xiang Zhonghe kettle
System carries out desalting processing；
Sulphur after separation is crystallized drying and packaging by the 4th step.
2. the recovery processing technique of vulcanized sodium according to claim 1 and sodium sulfite composite waste, it is characterised in that:
In second step, adds movable top lid filtering bucket, carry out tail gas absorption, exhaust fan sucks remaining a small amount of exhaust gas in sulphur.
3. the recovery processing technique of vulcanized sodium according to claim 2 and sodium sulfite composite waste, it is characterised in that:
In first step, the circulating line for offering one group of aperture is connect in the bottom of wastewater treatment reduction reaction kettle, top meets one and sky
The air inlet pipe for pressing equipment connection, is slowly passed through air.
4. the recovery processing technique of vulcanized sodium according to claim 3 and sodium sulfite composite waste, it is characterised in that:
In first step, after reaction in mother liquor PH less than 5.
5. the recovery processing technique of vulcanized sodium according to claim 4 and sodium sulfite composite waste, it is characterised in that:
In third step, the waste water generated after bucket filters that filters is introduced into high-salt wastewater collecting tank, then by filtered acidity
30% liquid alkaline is added in waste water, and adjusting PH is 8, then squeezes into MVR concentration, and the condensed water distilled enters wastewater equalization pond, abraum salt pack
Storage.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910085253.6A CN109626696A (en) | 2019-01-29 | 2019-01-29 | A kind of recovery processing technique of vulcanized sodium and sodium sulfite composite waste |
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| CN201910085253.6A CN109626696A (en) | 2019-01-29 | 2019-01-29 | A kind of recovery processing technique of vulcanized sodium and sodium sulfite composite waste |
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| CN109626696A true CN109626696A (en) | 2019-04-16 |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1488735A (en) * | 1974-09-05 | 1977-10-12 | Inst Francais Du Petrole | Treatment of ammonium sulphate-containing aqueous liquids for recovery of ammonia and sulphur |
| CN85109460A (en) * | 1984-12-04 | 1986-07-23 | 凯洛格总公司 | Hydrogen sulfide in the oxidation removal gas |
| US4937057A (en) * | 1984-06-27 | 1990-06-26 | Outokumpu Oy | Method for removing sulphur in elemental form from gases containing sulphur dioxide or sulphur dioxide and hydrogen sulphide |
| US7081233B2 (en) * | 2004-05-18 | 2006-07-25 | Dynamax Engineering Ltd. | Method and apparatus for degassing liquid sulfur |
| CN104692573A (en) * | 2015-04-14 | 2015-06-10 | 江西晨光新材料有限公司 | Wastewater treatment method in process of synthesizing bis-[gamma-triethoxysilylpropyl]-tetrasulfide through aqueous phase method |
| CN105254070A (en) * | 2015-11-03 | 2016-01-20 | 西南石油大学 | Method for recovering elemental sulfur from high-sulfur-content wastewater through reaction and separation coupling |
| CN107902675A (en) * | 2017-11-28 | 2018-04-13 | 湖北迅达药业股份有限公司 | One kind synthesis innoxious recovery and treatment method of felbinac accessory substance |
| CN108910830A (en) * | 2018-08-07 | 2018-11-30 | 中国恩菲工程技术有限公司 | The method for preparing sulphur using the sulfur dioxide in flue gas |
-
2019
- 2019-01-29 CN CN201910085253.6A patent/CN109626696A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1488735A (en) * | 1974-09-05 | 1977-10-12 | Inst Francais Du Petrole | Treatment of ammonium sulphate-containing aqueous liquids for recovery of ammonia and sulphur |
| US4937057A (en) * | 1984-06-27 | 1990-06-26 | Outokumpu Oy | Method for removing sulphur in elemental form from gases containing sulphur dioxide or sulphur dioxide and hydrogen sulphide |
| CN85109460A (en) * | 1984-12-04 | 1986-07-23 | 凯洛格总公司 | Hydrogen sulfide in the oxidation removal gas |
| US7081233B2 (en) * | 2004-05-18 | 2006-07-25 | Dynamax Engineering Ltd. | Method and apparatus for degassing liquid sulfur |
| CN104692573A (en) * | 2015-04-14 | 2015-06-10 | 江西晨光新材料有限公司 | Wastewater treatment method in process of synthesizing bis-[gamma-triethoxysilylpropyl]-tetrasulfide through aqueous phase method |
| CN105254070A (en) * | 2015-11-03 | 2016-01-20 | 西南石油大学 | Method for recovering elemental sulfur from high-sulfur-content wastewater through reaction and separation coupling |
| CN107902675A (en) * | 2017-11-28 | 2018-04-13 | 湖北迅达药业股份有限公司 | One kind synthesis innoxious recovery and treatment method of felbinac accessory substance |
| CN108910830A (en) * | 2018-08-07 | 2018-11-30 | 中国恩菲工程技术有限公司 | The method for preparing sulphur using the sulfur dioxide in flue gas |
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| Title |
|---|
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