CN110371933A - A kind of method of purification of spent acid - Google Patents
A kind of method of purification of spent acid Download PDFInfo
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- CN110371933A CN110371933A CN201910685247.4A CN201910685247A CN110371933A CN 110371933 A CN110371933 A CN 110371933A CN 201910685247 A CN201910685247 A CN 201910685247A CN 110371933 A CN110371933 A CN 110371933A
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- China
- Prior art keywords
- spent acid
- purification
- sulfuric acid
- decolorising agent
- acid
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- 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
- C01B17/92—Recovery from acid tar or the like, e.g. alkylation acids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of methods of purification of spent acid, it includes: 1) to decolourize: at 15 ~ 150 DEG C, decolorising agent is slowly added into spent acid, the spent acid and decolorising agent mass ratio is 4 ~ 5:1, the speed of decolorising agent addition is 4 ~ 6g/min, until spent acid becomes colourless or close to colourless, obtains solution A, while recycling the gas that reaction generates；2) purifying sulfuric acid: solution A rectifying at 300 ~ 400 DEG C, gas fraction obtains dilution heat of sulfuric acid through condensation, while obtaining the liquid of bottom；Liquid is filtered, solid residue is removed, obtains the concentrated sulfuric acid；Advantage is: it is simple to operation with method of the invention, it is low in cost；Purify the obtained concentrated sulfuric acid, concentration 97.95%, purity is high；Suitable for industrial production.
Description
Technical field
The invention belongs to waste acid treatment technical fields, and in particular to a kind of method of purification of spent acid.
Background technique
Petroleum sulfonate is to use SO using petroleum and its fraction as raw material3As sulfonating agent carry out sulfonation, then with alkali neutralization and
Manufactured product.It is a kind of surfactant of high-quality, is compounded with surfactant adjuvant, and effect is to reduce grease circle
Face tension, preferably raising displacement efficiency, are mainly used for the displacement of reservoir oil that the phase is adopted in oil field three.
In sulfonation process, extra SO is generally absorbed with the concentrated sulfuric acid3, generate dark-brown spent acid.Spent acid is a kind of liquid
Body, row steals to put steathily comes convenient and hidden than solid waste and exhaust gas, therefore, says from the angle of environmental protection, the improvement of spent acid
It is extremely urgent.Chemically for angle, so-called waste refers to the substance not being utilized, if these substances are used,
Pollution can be not only reduced, while resource can also be saved, there is great economic benefit and environmental benefit.At present mostly at spent acid
The method that reason technology uses is high-temperature roasting, and the gas of generation obtains SO through processing2, reoxidize as SO3, prepare sulfuric acid.This method
Process is complicated, and energy consumption is high, does not meet current requirement.
Summary of the invention
Object of the present invention is to solve the problems, such as that complex process, the energy consumption of the purification of existing spent acid are high, and provide a kind of simple
The method of purification of the spent acid easy, low energy consumption.
A kind of method of purification of spent acid, it includes:
1) it decolourizes: at 15 ~ 150 DEG C, decolorising agent is slowly added into spent acid, the spent acid and decolorising agent mass ratio are 4 ~ 5:
1, the speed of decolorising agent addition is 4 ~ 6g/min, until spent acid becomes colourless or close to colourless, obtains solution A, while recycling instead
The gas that should be generated；
2) purifying sulfuric acid: solution A rectifying at 300 ~ 400 DEG C, gas fraction obtains dilution heat of sulfuric acid through condensation, while obtaining kettle
The liquid at bottom；Solid residue in liquid is removed, the concentrated sulfuric acid is obtained；
Decolorising agent described in step 1) is strong oxidizer；
Solid residue in removing liquid described in step 2 is filtering or is distilled off；
Rectifying described in step 2, temperature are 300 ~ 350 DEG C.
The present invention provides a kind of methods of purification of spent acid, it includes: 1) to decolourize: at 15 ~ 150 DEG C, being delayed into spent acid
Slow that decolorising agent is added, the spent acid and decolorising agent mass ratio are 4 ~ 5:1, and the speed of decolorising agent addition is 4 ~ 6g/min, until
Spent acid becomes colourless or close to colourless, obtains solution A, while recycling the gas that reaction generates；2) purifying sulfuric acid: solution A is 300
Rectifying at ~ 400 DEG C, gas fraction obtains dilution heat of sulfuric acid through condensation, while obtaining the liquid of bottom；Liquid is filtered, is removed
Solid residue obtains the concentrated sulfuric acid；Advantage is: it is simple to operation with method of the invention, it is low in cost；Purify obtained dense sulphur
Acid, concentration 97.95%, purity is high；Suitable for industrial production.
Detailed description of the invention
The mass spectrogram of gas is generated when Fig. 1 decolourizes；
Sulfuric acid comparing result after Fig. 2 spent acid and purification；
The solid residue isolated after Fig. 3 purification.
Specific embodiment
A kind of method of purification of the spent acid of embodiment 1
The purification of spent acid is carried out using hydrogen peroxide as decolorising agent, specific steps are as follows:
(1) it decolourizes: taking spent acid 510g, be placed in beaker, hydrogen peroxide is slowly added dropwise at room temperature, since the concentrated sulfuric acid absorbs water or sends out
Raw oxidation reaction gradually rises spent acid temperature, and when reaching 100 DEG C, reaction is fierce, and releasing a large amount of gas, (about 16 grams, contain
There are vapor, oxygen, carbon dioxide etc., see Fig. 1)；After hydrogen peroxide 110g is added dropwise in 20 min, the temperature of spent acid is raised to
170 DEG C, reach light green solution A at this time；
(2) purifying sulfuric acid: solution A is transferred in quartzy round-bottomed flask, 350 DEG C of rectifying, and gas fraction obtains dilute sulphur through condensation
Sour (colorless and transparent, 99.6 grams, 1.106 g/ml of density)；Contain some impurity in the liquid of bottom, by filtering, obtained liquid
Body is the concentrated sulfuric acid (colorless and transparent, about 500 grams, 1.848 g/ml of density), while being obtained by filtration 1.1 grams of light green solid residue
(Fig. 3).
The sulfuric acid index obtained after measurement processing, the results are shown in Table 1.
A kind of method of purification of the spent acid of embodiment 2
The purification of spent acid is carried out using potassium permanganate as decolorising agent, specific steps are as follows:
(1) it decolourizes: taking spent acid 78.8g, be placed in beaker, be heated to 100 DEG C of stopping heating, it is molten that saturation potassium permanganate is slowly added dropwise
Liquid, due to concentrated sulfuric acid water suction or oxidation reaction, which occurs, gradually rises spent acid temperature, controls temperature at 200 DEG C or so；In 20min
After interior dropwise addition saturation 25 ml of liquor potassic permanganate, yellow solution A is obtained；
(2) purifying sulfuric acid: solution A is transferred in quartzy round-bottomed flask, and 350 DEG C of distillations, gas fraction obtains dilute sulphur through condensation
Sour (colorless and transparent, 28.3 grams, 1.03 g/ml of density)；The liquid of bottom is heated to 400 DEG C of distillations, obtains after fraction is cooling dense
Sulfuric acid (faint yellow, about 73.1 grams, 1.821 g/ml of density), brown solid residue (5.5 grams) in flask.
Claims (4)
1. a kind of method of purification of spent acid, it includes:
1) it decolourizes: at 15 ~ 150 DEG C, decolorising agent is slowly added into spent acid, the spent acid and decolorising agent mass ratio are 4 ~ 5:
1, the speed of decolorising agent addition is 4 ~ 6g/min, until spent acid becomes colourless or close to colourless, obtains solution A, while recycling instead
The gas that should be generated；
2) purifying sulfuric acid: solution A rectifying at 300 ~ 400 DEG C, gas fraction obtains dilution heat of sulfuric acid through condensation, while obtaining kettle
The liquid at bottom；Solid residue in liquid is removed, the concentrated sulfuric acid is obtained.
2. a kind of method of purification of spent acid according to claim 1, it is characterised in that: decolorising agent described in step 1) is strong
Oxidant.
3. a kind of method of purification of spent acid according to claim 2, it is characterised in that: in removing liquid described in step 2
Solid residue is filtering or is distilled off.
4. a kind of method of purification of spent acid according to claim 3, it is characterised in that: rectifying described in step 2, temperature
It is 300 ~ 350 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910685247.4A CN110371933A (en) | 2019-07-27 | 2019-07-27 | A kind of method of purification of spent acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910685247.4A CN110371933A (en) | 2019-07-27 | 2019-07-27 | A kind of method of purification of spent acid |
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| CN110371933A true CN110371933A (en) | 2019-10-25 |
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| CN201910685247.4A Pending CN110371933A (en) | 2019-07-27 | 2019-07-27 | A kind of method of purification of spent acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113336198A (en) * | 2021-08-05 | 2021-09-03 | 清大国华环境集团股份有限公司 | Method and system for recycling waste sulfuric acid in integrated circuit industry |
| CN116161621A (en) * | 2023-04-23 | 2023-05-26 | 联仕(昆山)化学材料有限公司 | Purification device and purification process of electronic grade hydrochloric acid |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002121581A (en) * | 2000-10-13 | 2002-04-26 | Kanegafuchi Chem Ind Co Ltd | Purified conjugated triene fatty acid-containing fat, and manufacturing method therefor |
| DE102005057913A1 (en) * | 2005-12-02 | 2007-06-06 | Vopelius Chemie Ag | Procedure for removal of impurities and/or decolorization of phosphoric acid, comprises mixing the phosphoric acid with a strong oxidizing agent, and reacting the obtained mixture at above atmospheric pressure |
| CN102923675A (en) * | 2012-11-27 | 2013-02-13 | 武汉工程大学 | Process method for purifying sulfuric acid in fluorobenzene waste acid |
| CN103172033A (en) * | 2013-03-27 | 2013-06-26 | 刘立文 | Method for decoloring sulfuric acid |
| CN103172035A (en) * | 2013-03-27 | 2013-06-26 | 刘立文 | Method for decoloring sulfuric acid by using hydrogen peroxide |
| CN104627967A (en) * | 2013-11-13 | 2015-05-20 | 雷永诚 | System and method of normal temperature recovery of waste sulfuric acid |
| CN107032308A (en) * | 2016-12-01 | 2017-08-11 | 防城港五星化工有限公司 | A kind of waste sulfuric acid from alkylation resource recycle method |
| CN109694043A (en) * | 2018-12-27 | 2019-04-30 | 镇江江南化工有限公司 | A kind of method that Waste Sulfuric Acid integrated treatment recycles |
-
2019
- 2019-07-27 CN CN201910685247.4A patent/CN110371933A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002121581A (en) * | 2000-10-13 | 2002-04-26 | Kanegafuchi Chem Ind Co Ltd | Purified conjugated triene fatty acid-containing fat, and manufacturing method therefor |
| DE102005057913A1 (en) * | 2005-12-02 | 2007-06-06 | Vopelius Chemie Ag | Procedure for removal of impurities and/or decolorization of phosphoric acid, comprises mixing the phosphoric acid with a strong oxidizing agent, and reacting the obtained mixture at above atmospheric pressure |
| CN102923675A (en) * | 2012-11-27 | 2013-02-13 | 武汉工程大学 | Process method for purifying sulfuric acid in fluorobenzene waste acid |
| CN103172033A (en) * | 2013-03-27 | 2013-06-26 | 刘立文 | Method for decoloring sulfuric acid |
| CN103172035A (en) * | 2013-03-27 | 2013-06-26 | 刘立文 | Method for decoloring sulfuric acid by using hydrogen peroxide |
| CN104627967A (en) * | 2013-11-13 | 2015-05-20 | 雷永诚 | System and method of normal temperature recovery of waste sulfuric acid |
| CN107032308A (en) * | 2016-12-01 | 2017-08-11 | 防城港五星化工有限公司 | A kind of waste sulfuric acid from alkylation resource recycle method |
| CN109694043A (en) * | 2018-12-27 | 2019-04-30 | 镇江江南化工有限公司 | A kind of method that Waste Sulfuric Acid integrated treatment recycles |
Non-Patent Citations (1)
| Title |
|---|
| 曹攀等: "电子级硫酸制备工艺及发展现状", 《无机盐工业》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113336198A (en) * | 2021-08-05 | 2021-09-03 | 清大国华环境集团股份有限公司 | Method and system for recycling waste sulfuric acid in integrated circuit industry |
| CN116161621A (en) * | 2023-04-23 | 2023-05-26 | 联仕(昆山)化学材料有限公司 | Purification device and purification process of electronic grade hydrochloric acid |
| CN116161621B (en) * | 2023-04-23 | 2023-07-04 | 联仕(昆山)化学材料有限公司 | Purification device and purification process of electronic grade hydrochloric acid |
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Application publication date: 20191025 |