CN114804035A - Separation and purification process of waste sulfuric acid containing organic matters - Google Patents
Separation and purification process of waste sulfuric acid containing organic matters Download PDFInfo
- Publication number
- CN114804035A CN114804035A CN202210323385.XA CN202210323385A CN114804035A CN 114804035 A CN114804035 A CN 114804035A CN 202210323385 A CN202210323385 A CN 202210323385A CN 114804035 A CN114804035 A CN 114804035A
- Authority
- CN
- China
- Prior art keywords
- sulfuric acid
- tank
- waste sulfuric
- organic matters
- separation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
- C01B17/905—Removal of organic impurities
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a separation and purification process of waste sulfuric acid containing organic matters, which is characterized by comprising the following steps of: the method comprises the following six steps: collecting the waste sulfuric acid containing organic matters to be processed, and storing the waste sulfuric acid containing the organic matters by using an anti-corrosion device; introducing waste sulfuric acid into a dilution tank, and adding water for dilution after introduction; and carrying out vacuum filtration on the waste sulfuric acid containing the organic matters through a filter tank, pumping the filtrate to a trap, passing through a head tank, continuously flowing into a rising film type tube still evaporator under the control of a rotor flow meter, and concentrating at 115 ℃ under the vacuum degree of 660 mmHg. The invention develops a separation and purification process of waste sulfuric acid containing organic matters, which can effectively recover sulfuric acid contained in filter residue by carrying out secondary treatment on the filter residue, and can separate the waste sulfuric acid from a thermal decomposition furnace when the waste sulfuric acid contains inorganic salts, such as ammonium salt, so that nitrogen oxide is not generated, and the recovery effect of the sulfuric acid is good when the waste sulfuric acid is used.
Description
Technical Field
The invention relates to the technical field of waste sulfuric acid processing, in particular to a separation and purification process of waste sulfuric acid containing organic matters.
Background
For many years, the economic and reasonable utilization of available sulfuric acid in wastewater has been closely related to industrial production; in order to reduce the damage of the waste sulfuric acid to the environment, the waste sulfuric acid needs to be treated when in use.
The traditional separation and purification process of the waste sulfuric acid containing organic matters has a common separation and purification effect when the waste sulfuric acid containing organic matters is treated, and has a common effect after recovery in the extraction process.
Disclosure of Invention
The invention aims to provide a separation and purification process of waste sulfuric acid containing organic matters, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a separation and purification process of waste sulfuric acid containing organic matters is characterized in that: the method comprises the following six steps:
the method comprises the following steps: collecting the waste sulfuric acid containing organic matters to be processed, and storing the waste sulfuric acid containing the organic matters by using an anti-corrosion device;
step two: introducing waste sulfuric acid into a dilution tank, and adding water for dilution after introduction;
step three: carrying out vacuum filtration on the waste sulfuric acid containing the organic matters through a filter tank, pumping filtrate to a trap, passing through a head tank, continuously flowing into a rising film type tube still evaporator under the control of a rotor flow meter, and concentrating at 115 ℃ under the vacuum degree of 660 mm Hg;
step four: separating water vapor and acid by a hydrocyclone, pumping water in a circulating water tank into a jet pump by an acid-proof pump to cool and absorb the separated water vapor, and quantitatively and continuously flowing 70% sulfuric acid into a cast iron concentration kettle through a head tank;
step five: pumping water in a circulating water tank into a jet pump by using an acid-resistant pump to circularly absorb sulfuric acid tail gas and water vapor of the cast iron kettle, enabling 93% concentrated sulfuric acid to flow into a cooled enamel oxidation tank, and adding nitric acid from a head tank to oxidize the concentrated sulfuric acid to light yellow;
step six: alkali liquor in the water tank is pumped into the jet pump through the acid-proof pump to circularly absorb the nitrogen oxide tail gas, and 93 percent sulfuric acid flows into the storage tank to be reused.
Furthermore, the dilution tank adopts a closed tank body, water is added into the tank body, and then the tank body is stirred and fused with the waste sulfuric acid containing organic matters to form 30% diluted acid after fusion.
And further, in the third step, filter residues generated after vacuum filtration in the filter tank are put into a thermal decomposition furnace and are incinerated under the condition of air isolation.
Further, the temperature of the cast iron concentration kettle in the fourth step is controlled to be 280-310 ℃, and the vacuum degree is 50-100 mm of water column.
Further, in the fifth step, the temperature of the enamel oxidation tank is controlled to be 210-220 ℃, and the adding amount of nitric acid is 65-70%.
Compared with the prior art, the invention has the beneficial effects that: the preparation method of the separation and purification process of the waste sulfuric acid containing organic matters can effectively recover the sulfuric acid contained in the filter residue by carrying out secondary treatment on the filter residue, and when the waste acid contains inorganic salts, the waste acid can be separated from a thermal decomposition furnace, such as ammonium salt, so that nitrogen oxide is not generated, and the recovery effect of the sulfuric acid is good when the waste acid is used.
Drawings
FIG. 1 is a schematic diagram showing the ratio of the process for separating and purifying waste sulfuric acid containing organic substances according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "connected," and the like are to be construed broadly, such as "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1
Referring to fig. 1, an embodiment of the present invention: a separation and purification process of waste sulfuric acid containing organic matters is characterized in that: the method comprises the following six steps:
the method comprises the following steps: the waste sulfuric acid containing organic matters to be processed is collected, the waste sulfuric acid containing organic matters is stored by using an anti-corrosion device, the waste sulfuric acid is stored in a cool and ventilated storehouse, the temperature of the storehouse is not more than 35 ℃, the relative humidity is not more than 85%, a container is kept sealed, the waste sulfuric acid is far away from kindling, heat sources, inflammable matters and combustible matters, smoking is strictly prohibited in a workplace, and steam is prevented from leaking into the air of the workplace;
step two: the waste sulfuric acid is introduced into a dilution tank, water is added for dilution after introduction, a stirring shaft is used for promoting the dilution effect in the dilution process, and the reaction time is shortened;
step three: carrying out vacuum filtration on the waste sulfuric acid containing the organic matters through a filter tank, pumping filtrate to a trap, passing through a head tank, continuously flowing into a rising film type tube still evaporator under the control of a rotor flow meter, and concentrating at 115 ℃ under the vacuum degree of 660 mm Hg;
step four: separating water vapor and acid by a hydrocyclone, pumping water in a circulating water tank into a jet pump by an acid-proof pump to cool and absorb the separated water vapor, and quantitatively and continuously flowing 70% sulfuric acid into a cast iron concentration kettle through a head tank;
step five: pumping water in a circulating water tank into a jet pump by using an acid-resistant pump to circularly absorb sulfuric acid tail gas and water vapor of the cast iron kettle, enabling 93% concentrated sulfuric acid to flow into a cooled enamel oxidation tank, and adding nitric acid from a head tank to oxidize the concentrated sulfuric acid to light yellow;
step six: alkali liquor in the water tank is pumped into the jet pump through the acid-proof pump to circularly absorb the nitrogen oxide tail gas, and 93 percent sulfuric acid flows into the storage tank to be reused.
Further, the diluting tank adopts a closed tank body, the diluting tank is stirred and fused with waste sulfuric acid containing organic matters after water is added, liquid in the tank body is detected by using detection equipment in the fusion process, 30% dilute acid is formed after fusion, and the water adding is stopped after the dilute acid is formed.
And further, in the third step, filter residues generated after vacuum filtration in the filter tank are put into a thermal decomposition furnace and are incinerated under the condition of air isolation, the furnace temperature is kept at 1000-1100 ℃, the waste acid is sprayed into a high-temperature region to be thermally decomposed, solids contained in the waste acid are discharged from the furnace bottom, and a secondary combustion furnace is arranged behind the decomposition furnace in order to ensure complete decomposition.
Further, in the fourth step, the temperature of the cast iron concentration kettle is controlled to be 280-310 ℃, the vacuum degree is 50-100 mm of water column, and the cast iron concentration kettle is used for processing sulfuric acid.
Further, in the fifth step, the temperature of the enamel oxidation tank is controlled to be 210-220 ℃, the adding amount of nitric acid is 65-70%, and the nitric acid is stored by adding the nitric acid.
Example 2
A separation and purification process of waste sulfuric acid containing organic matters comprises the following steps:
after vacuum filtration in the filter tank, filter residue with a certain volume is generated, and the filter residue contains a certain content of sulfuric acid besides organic matters, so that secondary processing is needed to improve the separation effect, and the secondary purification and separation comprises a plurality of steps.
The method comprises the following steps: the thermal decomposition of the waste acid is carried out in a vertical thermal decomposition furnace, the compressed air is used for spraying the waste sulfuric acid from the upper part of the furnace through spray head spraying, heavy oil is sprayed from the side surface of the furnace for combustion, the temperature of the furnace is kept between 1000 and 1100 ℃, the thermal decomposition is carried out after the waste acid is sprayed into a high-temperature region, the solid contained in the waste acid is discharged from the bottom of the furnace, and a secondary combustion furnace is arranged behind the decomposition furnace for ensuring the complete decomposition;
step two: the decomposed gas of about 1000 ℃ coming out of the decomposing furnace enters a natural circulation type water tube boiler to be cooled to about 350 ℃, simultaneously, high-pressure superheated steam of 56 kg/cm pressure and 400 ℃ can be generated, inorganic salts in raw materials and ash in combustion are deposited at the bottom of the decomposing furnace, and one part of the inorganic salts and the ash in combustion are attached to the tube wall of the waste heat boiler, so that high-pressure steam is used for blowing or washing at proper time intervals;
step three: the decomposition gas at about 350 ℃ from the waste heat boiler contains SO 2 、O 2 、 CO 2 、N 2 、H 2 O, and small amount of SO 3 And the residue, which must be refined, by quenching the decomposed gas to room temperature using a cooling tower and a washing tower lined with acid-proof bricks, and then condensing SO with a large amount of condensed water 3 Absorbing and cleaning, discharging as acidic water, removing acid mist from the cleaned gas through an electric demister, sending the acid mist into a drying tower, and contacting concentrated sulfuric acid in the tower to completely remove water;
step four: the refined sulfur dioxide gas is oxidized into sulfur trioxide through catalysis, and then the sulfur trioxide is absorbed by concentrated sulfuric acid to prepare 98.5 percent sulfuric acid;
step five: and (3) neutralizing the tail gas with ammonia water, then feeding the neutralized tail gas back to the decomposing furnace for thermal decomposition, performing closed cycle, and washing the tail gas to reduce the concentration of sulfur-containing oxides to 100-150 ppm.
The sulfuric acid contained in the filter residue can be effectively recovered by performing secondary treatment on the filter residue, and when the waste acid contains inorganic salts, the inorganic salts can be separated from the thermal decomposition furnace, such as ammonium salts, and can be controlled not to generate nitrogen oxides.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (5)
1. A separation and purification process of waste sulfuric acid containing organic matters is characterized in that: the method comprises the following six steps:
the method comprises the following steps: collecting the waste sulfuric acid containing organic matters to be processed, and storing the waste sulfuric acid containing the organic matters by using an anti-corrosion device;
step two: introducing waste sulfuric acid into a dilution tank, and adding water for dilution after introduction;
step three: carrying out vacuum filtration on the waste sulfuric acid containing the organic matters through a filter tank, pumping filtrate to a trap, passing through a head tank, continuously flowing into a rising film type tube still evaporator under the control of a rotor flow meter, and concentrating at 115 ℃ under the vacuum degree of 660 mm Hg;
step four: separating water vapor and acid by a hydrocyclone, pumping water in a circulating water tank into a jet pump by an acid-proof pump to cool and absorb the separated water vapor, and quantitatively and continuously flowing 70% sulfuric acid into a cast iron concentration kettle through a head tank;
step five: pumping water in a circulating water tank into a jet pump by using an acid-resistant pump to circularly absorb sulfuric acid tail gas and water vapor of the cast iron kettle, enabling 93% concentrated sulfuric acid to flow into a cooled enamel oxidation tank, and adding nitric acid from a head tank to oxidize the concentrated sulfuric acid to light yellow;
step six: alkali liquor in the water tank is pumped into the jet pump through the acid-proof pump to circularly absorb the nitrogen oxide tail gas, and 93 percent sulfuric acid flows into the storage tank to be reused.
2. The process of claim 1, wherein the separation and purification process comprises the following steps: the diluting tank adopts a closed tank body, water is added into the tank body, and then the tank body is stirred and fused with waste sulfuric acid containing organic matters to form 30% diluted acid.
3. The process of claim 1, wherein the separation and purification process comprises the following steps: and in the third step, filter residues generated after vacuum filtration in the filter tank are put into a thermal decomposition furnace and are incinerated under the condition of isolating air.
4. The process of claim 1, wherein the separation and purification process comprises the following steps: and in the fourth step, the temperature of the cast iron concentration kettle is controlled to be 280-310 ℃, and the vacuum degree is 50-100 mm of water column.
5. The process of claim 1, wherein the separation and purification process comprises the following steps: in the fifth step, the temperature of the enamel oxidation tank is controlled to be 210-220 ℃, and the adding amount of nitric acid is 65-70%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210323385.XA CN114804035A (en) | 2022-03-30 | 2022-03-30 | Separation and purification process of waste sulfuric acid containing organic matters |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210323385.XA CN114804035A (en) | 2022-03-30 | 2022-03-30 | Separation and purification process of waste sulfuric acid containing organic matters |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114804035A true CN114804035A (en) | 2022-07-29 |
Family
ID=82532071
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210323385.XA Pending CN114804035A (en) | 2022-03-30 | 2022-03-30 | Separation and purification process of waste sulfuric acid containing organic matters |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114804035A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445219A (en) * | 2008-12-30 | 2009-06-03 | 上虞市金冠化工有限公司 | Method for recycling waste acid |
| US20120168298A1 (en) * | 2009-09-15 | 2012-07-05 | De Dietrich Process Systems Gmbh | Method and plant for reprocessing waste sulphuric acids from nitriding processes |
| CN105152142A (en) * | 2015-06-02 | 2015-12-16 | 南京鹳山化工科技有限公司 | Method for recovering sulfuric acid from waste acid produced by anthraquinone production |
-
2022
- 2022-03-30 CN CN202210323385.XA patent/CN114804035A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445219A (en) * | 2008-12-30 | 2009-06-03 | 上虞市金冠化工有限公司 | Method for recycling waste acid |
| US20120168298A1 (en) * | 2009-09-15 | 2012-07-05 | De Dietrich Process Systems Gmbh | Method and plant for reprocessing waste sulphuric acids from nitriding processes |
| CN105152142A (en) * | 2015-06-02 | 2015-12-16 | 南京鹳山化工科技有限公司 | Method for recovering sulfuric acid from waste acid produced by anthraquinone production |
Non-Patent Citations (1)
| Title |
|---|
| 刘生林: "废硫酸的净化和浓缩技术", 《化工环保》, vol. 8, no. 2, pages 102 - 104 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110833754B (en) | Device for absorbing ethylene oxide waste gas and method for treating ethylene oxide waste gas | |
| CN106430116B (en) | A method of the sulphur-bearing waste solution extracting sulfuric acid generated using coal gas wet oxidation method | |
| CN101810992A (en) | Purification system for flue gas generated by burning wastes and purification process thereof | |
| CN105080310A (en) | Waste incineration flue gas purification system and integral solution process | |
| CN106268179B (en) | A kind of energy saving technique and system of synthetical recovery sulfuric acid purification spent acid | |
| CN107601605B (en) | Technology and system for improving yield of regenerated nitric acid from stainless steel pickling waste liquid | |
| CN109052335A (en) | A kind of method of sulfur gas reduction Waste Sulfuric Acid sulfur dioxide liquid and sulfuric acid | |
| CN110314505B (en) | Device and method for treating ammonia-containing tail gas in ammonium drying section in alkali industry | |
| CN108083538A (en) | The recycling processing method and its device of coking desulfurization salt bearing liquid wastes | |
| CN104383801B (en) | Method and system for treating electronic scrap smoke | |
| CN102423612A (en) | Method for producing thiosulfate and recovering carbon dioxide by utilizing industrial flue gas | |
| CN201701866U (en) | Garbage incineration flue gas purification system | |
| CN110282606A (en) | The wet processing system and technique of aqueous sulphur cream and desulfurization waste liquor | |
| US11376546B2 (en) | Method and a system for producing hydrochloric acid from flue gases | |
| CN110332552B (en) | Resourceful treatment system and method for chlorine-sulfur-containing organic waste liquid | |
| CN113883543A (en) | High-chlorine-content hazardous waste incineration flue gas purification and hydrochloric acid recycling system and method | |
| CN204973575U (en) | Garbage incineration flue gas purification system | |
| CN204093290U (en) | A kind of flue gas desulfur device | |
| CN211274164U (en) | Ammonia-containing tail gas treatment device for dry ammonium workshop section in alkali industry | |
| CN112499589A (en) | Acid regeneration water-to-acid mode acid mist chimney red smoke emission treatment method | |
| CN205528524U (en) | Utilize phenol sodium salt to prepare device of crude carbolic acid | |
| CN111544972A (en) | Method and system for waste gas purification and resource recovery of lithium battery recovery | |
| CN114804035A (en) | Separation and purification process of waste sulfuric acid containing organic matters | |
| CN209161488U (en) | A kind of system of sulfur gas reduction Waste Sulfuric Acid sulfur dioxide liquid and sulfuric acid | |
| CN109260873B (en) | Plasma melting tail gas purification system and method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |