CN107758627B - Separation and recovery method of concentrated sulfuric acid and asphalt mixed liquid generated by cleaning oil pipeline equipment - Google Patents
Separation and recovery method of concentrated sulfuric acid and asphalt mixed liquid generated by cleaning oil pipeline equipment Download PDFInfo
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- CN107758627B CN107758627B CN201711154852.6A CN201711154852A CN107758627B CN 107758627 B CN107758627 B CN 107758627B CN 201711154852 A CN201711154852 A CN 201711154852A CN 107758627 B CN107758627 B CN 107758627B
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Abstract
The invention discloses a method for separating and recovering concentrated sulfuric acid and asphalt mixed liquor generated by cleaning oil pipeline equipment, which comprises the steps of pumping the concentrated sulfuric acid and the asphalt mixed liquor into a separator for adsorption and filtration to obtain clear and transparent concentrated sulfuric acid; the filter element of the separator is one or two of active carbon and diatomite; and after the filter element does not have the filtering and adsorbing functions any more, the filter element is carbonized and activated by an activation furnace or a muffle furnace and then is recycled. The method of the invention recovers and recycles a large amount of industrial waste liquid of asphalt attached to oil pipeline equipment, namely concentrated sulfuric acid and asphalt in the mixed liquid of the concentrated sulfuric acid and the asphalt, improves the added value of the asphalt, and has the advantages of low cost, simple and easy operation, zero environmental pollution and recycling.
Description
Technical Field
The invention belongs to the technical field of recovery treatment of cleaning waste liquid of oil-gas engineering equipment, and particularly relates to a method for separating and recovering concentrated sulfuric acid and asphalt mixed liquid generated by cleaning oil pipeline equipment.
Background
Concentrated sulfuric acid is H with the mass fraction of more than or equal to 70 percent2SO4An aqueous solution. At normal temperature, concentrated sulfuric acid can quickly oxidize the surfaces of iron, aluminum and other metals to generate a compact oxide film so as to generate 'passivation'. Therefore, in the maintenance and management process of oil and gas engineering equipment, concentrated sulfuric acid is often used to remove asphalt attached to oil pipeline equipment, thereby producing a large amount of mixed liquid of the waste concentrated sulfuric acid and the asphalt. The ecological environment can be dumped at will, so that the water body and the soil in the ecological environment are seriously polluted, the health of human beings is threatened, and great pressure and burden are caused to enterprises and the environment. At present, the recycling of the waste water is rarely researched in domestic and foreign industries. Therefore, the development of a technology for separating, recycling and reusing the waste materials with low investment, high efficiency and environmental friendliness is urgent.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for separating and recovering concentrated sulfuric acid and asphalt mixed liquor generated by cleaning oil pipeline equipment, which has the advantages of low cost, simple, convenient, safe and easily-regenerated process and environmental protection, realizes the recovery and reutilization of the concentrated sulfuric acid and asphalt mixed liquor after cleaning the oil pipeline equipment, and achieves zero emission.
The invention solves the technical problems by the following technical scheme:
a separation and recovery method of concentrated sulfuric acid and asphalt mixed solution generated by cleaning oil pipeline equipment comprises the steps of pumping the concentrated sulfuric acid and asphalt mixed solution into a separator for adsorption and filtration to obtain clear and transparent concentrated sulfuric acid; the filter element of the separator is one or two of activated carbon and diatomite; the filter element which does not have the filtering and absorbing functions after full absorption of the asphalt is carbonized and activated by an activation furnace or a muffle furnace and then recycled.
The filling height of the filter element of the separator is more than 30% of the height of the mixed liquid of concentrated sulfuric acid and asphalt.
The separator is formed by connecting a plurality of separators in series, in parallel or in series and parallel.
In the plurality of separators, the filter element of at least one separator is one or two of activated carbon and diatomite; the filter element of the other separator is sand or one or two of silicon dioxide powder and silicon carbide powder.
And screening the sand by a screen with 100-400 meshes, and drying the screened objects for 1-2h at 100-150 ℃.
The carbonization and activation method of the filter element comprises the following steps: activating a filter element for 2-5 hours by hydrochloric acid with the mass concentration of 1-5%, performing suction filtration, and washing to be neutral; secondly, activating the filter element obtained in the step one for 5-10 hours by NaOH with the mass concentration of 1% -5%, performing suction filtration, and washing to be neutral; thirdly, the filter element obtained in the second step is placed in an activation furnace or a muffle furnace to be calcined for 1 to 3 hours at the temperature of between 200 and 400 ℃; and fourthly, grinding, crushing, dispersing and drying the filter element obtained in the third step to obtain the filter element.
The separator adopts top pressurization or the side part of the separator is connected with a vacuum pump for suction filtration to improve the speed of filtration and separation.
The invention has the advantages that:
the recycling of industrial and agricultural wastes, zero pollution, simple process, environmental protection and easy regeneration of the filter element are realized, and a high-added-value outlet and direction are provided for recycling the mixed solution of concentrated sulfuric acid and asphalt generated by cleaning oil pipeline equipment.
Detailed Description
The following examples are given to illustrate specific embodiments of the present invention, but should not be construed as limiting the scope of the claims.
Example 1:
a method for separating and recovering concentrated sulfuric acid and asphalt mixed liquid generated by cleaning oil pipeline equipment comprises the steps of pumping the concentrated sulfuric acid and asphalt mixed liquid into a separator for adsorption and filtration, wherein a filter element of the separator is activated carbon, the filling height of the activated carbon is 30% of the height of the concentrated sulfuric acid and asphalt mixed liquid, and colorless clear concentrated sulfuric acid is obtained through separation. The filter element which does not have the filtering and adsorbing functions after full absorption of the asphalt is respectively carbonized and activated and then repeatedly reused.
The carbonization and activation method of the filter element comprises the following steps: activating a filter element for 2-5 hours by hydrochloric acid with the mass concentration of 1-5%, and performing suction filtration to be neutral; secondly, activating the filter element obtained in the step one by NaOH with the mass concentration of 1% -5% for 2-5 h, and performing suction filtration to be neutral; thirdly, the filter element obtained in the second step is placed in an activation furnace or a muffle furnace to be calcined for 1 to 3 hours at the temperature of between 200 and 400 ℃; and fourthly, grinding, crushing and dispersing the filter element obtained in the third step by a grinding crusher, and keeping the filter element dry to obtain the filter element.
Example 2:
a method for separating and recovering concentrated sulfuric acid and asphalt mixed liquid generated by cleaning oil pipeline equipment comprises the steps of pumping the concentrated sulfuric acid and asphalt mixed liquid into a separator for adsorption and filtration, wherein a filter element of the separator is diatomite powder, the filling height of the diatomite powder is 80% of the height of the concentrated sulfuric acid and asphalt mixed liquid, and colorless clear concentrated sulfuric acid is obtained through separation. The filter element which does not have the filtering and adsorbing functions after full absorption of the asphalt is respectively carbonized and activated and then repeatedly reused.
The method of carbonization and activation of the filter element is the same as in example 1.
Example 3:
a method for separating and recovering concentrated sulfuric acid and asphalt mixed liquor generated by cleaning oil pipeline equipment comprises the steps of pumping the concentrated sulfuric acid and asphalt mixed liquor into a first separator for adsorption and filtration, wherein a filter element of the first separator is 100-mesh dry sand, and the filling height of the filter element is 120% of the height of the concentrated sulfuric acid and asphalt mixed liquor. And screening the sand by a 100-mesh screen, and drying the screened objects for 1-2h at 100-150 ℃. And pumping the liquid obtained by separation in the first separator into a second separator for adsorption filtration, wherein a filter element of the second separator is silicon dioxide powder, and the filling height is more than 180% of the height of the mixed liquid of concentrated sulfuric acid and asphalt. And pumping the liquid obtained by separation in the second separator into a third separator for adsorption filtration, wherein a filter element of the third separator is a combination of activated carbon and diatomite in a mass ratio of 1: 1, and the filling height is 200% of the height of the mixed solution of concentrated sulfuric acid and asphalt. The clear liquid separated by the third separator is concentrated sulfuric acid. And in the adsorption and filtration process of the third separator, the adsorption, filtration and separation speed is improved by adopting a vacuum pump suction filtration mode.
The first separator, the second separator and the third separator are filter elements which do not have filtering and adsorbing functions after full absorption of asphalt, and are repeatedly reused after carbonization and activation respectively.
The method of carbonization and activation of the filter element is the same as in example 1.
Example 4:
a method for separating and recovering concentrated sulfuric acid and asphalt mixed liquor generated by cleaning oil pipeline equipment comprises the steps of pumping the concentrated sulfuric acid and asphalt mixed liquor into a first separator for adsorption and filtration, wherein a filter element of the first separator is 300-mesh dry sand, and the filling height of the filter element is 200% of the height of the concentrated sulfuric acid and asphalt mixed liquor. And screening the sand by a 300-mesh screen, and drying the screened objects for 1-2h at 100-150 ℃. And the liquid obtained by the separation of the first separator is pumped into a second separator for adsorption filtration, a filter element of the second separator is silicon carbide powder, and the filling height is 180% of the height of the mixed liquid of concentrated sulfuric acid and asphalt. And pumping the liquid obtained by separation in the second separator into a third separator for adsorption filtration, wherein a filter element of the third separator is formed by combining 80% of activated carbon and 20% of diatomite by mass ratio, and the filling height is 300% of the height of the mixed solution of concentrated sulfuric acid and asphalt. The clear liquid separated by the third separator is concentrated sulfuric acid. In the adsorption filtration process of the third separator, the pressure of 0.01MPa is applied to the top of the third separator to accelerate the adsorption filtration separation rate.
The first separator, the second separator and the third separator are filter elements which do not have filtering and adsorbing functions after adsorption and filtration, and are repeatedly reused after being respectively carbonized and activated.
The carbonization and activation method of the filter element is the same as that of the embodiment 1.
Example 5:
a method for separating and recovering concentrated sulfuric acid and asphalt mixed liquor generated by cleaning oil pipeline equipment comprises the steps of pumping the concentrated sulfuric acid and asphalt mixed liquor into a first separator for adsorption and filtration, wherein a filter element of the first separator is 400-mesh dry sand, and the filling height of the filter element is 300% of the height of the concentrated sulfuric acid and asphalt mixed liquor. And (3) screening the sand by a 400-mesh screen, and drying the screened objects for 1-2h at 100-150 ℃. And the liquid obtained by the separation of the first separator is pumped into a second separator for adsorption filtration, a filter element of the second separator is a combination of silicon dioxide powder and silicon carbide powder with the mass ratio of 1: 1, and the filling height is 350% of the height of the mixed liquid of concentrated sulfuric acid and asphalt. And pumping the liquid obtained by separation in the second separator into a third separator for adsorption filtration, wherein a filter element of the third separator is formed by combining 30% of activated carbon and 70% of diatomite by mass ratio, and the filling height is 350% of the height of the mixed solution of concentrated sulfuric acid and asphalt. The clear liquid separated by the third separator is concentrated sulfuric acid. And in the adsorption and filtration process of the third separator, a vacuum pump is connected to the side part of the separator for suction filtration to accelerate the adsorption, filtration and separation rate of the third separator.
The first separator, the second separator and the third separator are filter elements which do not have filtering and adsorbing functions after adsorption and filtration, and are repeatedly reused after being respectively carbonized and activated.
The carbonization and activation methods of the filter elements of the first separator, the second separator and the third separator are the same as the example 1.
Claims (4)
1. A separation and recovery method of concentrated sulfuric acid and asphalt mixed liquor generated by cleaning oil pipeline equipment is characterized in that the concentrated sulfuric acid and asphalt mixed liquor is pumped into a separator for adsorption and filtration to obtain clear and transparent concentrated sulfuric acid; the filter element of the separator is one or two of activated carbon and diatomite; the filter element which does not have the filtering and adsorbing functions after full absorption of the asphalt is carbonized and activated by an activation furnace or a muffle furnace and then is recycled;
the separator is formed by connecting a plurality of separators in series, in parallel or in series and parallel;
in the plurality of separators, the filter element of at least one separator is one or two of activated carbon and diatomite; the filter elements of the other separators are sand or one or two of silicon dioxide powder and silicon carbide powder;
the filter element is activated for 2-5 h by hydrochloric acid with the mass concentration of 1-5%, filtered and washed to be neutral; secondly, activating the filter element obtained in the step one by NaOH with the mass concentration of 1% -5% for 5-10 hours, performing suction filtration, and washing the filter element to be neutral; thirdly, the filter element obtained in the second step is placed in an activation furnace or a muffle furnace to be calcined for 1 to 3 hours at the temperature of between 200 and 400 ℃; and fourthly, grinding, crushing, dispersing and drying the filter element obtained in the third step to obtain the filter element.
2. The method according to claim 1, wherein the filling height of the filter element of the separator is 30% or more of the height of the mixed solution of concentrated sulfuric acid and asphalt.
3. The method for separating and recovering the mixed solution of concentrated sulfuric acid and asphalt produced by cleaning oil pipeline equipment according to claim 1, wherein the sand is screened by a screen with 100-400 meshes, and the undersize product is dried for 1-2h at 100-150 ℃.
4. The method for separating and recovering the concentrated sulfuric acid and the asphalt mixture produced by the equipment for cleaning the oil transportation pipeline according to claim 1, wherein the separator adopts top pressurization or suction filtration by connecting a vacuum pump at the side part of the separator to improve the filtration and separation rate.
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| CN107758627B true CN107758627B (en) | 2020-10-13 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4508851A (en) * | 1982-06-23 | 1985-04-02 | Toho Beslon Co., Ltd. | Fibrous activated carbon and process of producing it |
| CN102755884A (en) * | 2012-04-13 | 2012-10-31 | 山东轻工业学院 | Method for regenerating waste active carbon by chemical medicament |
| CN104342327A (en) * | 2013-08-08 | 2015-02-11 | 厦门泰益新洁净科技有限公司 | Oil-stain cleaning agent as well as preparation method and use method thereof |
| CN104445836A (en) * | 2014-12-26 | 2015-03-25 | 常州大学 | High-concentration asphalt waste water treatment method and device |
| CN105585208A (en) * | 2015-11-24 | 2016-05-18 | 佛山高富中石油燃料沥青有限责任公司 | Asphalt wastewater treatment system |
| CN206198986U (en) * | 2016-08-31 | 2017-05-31 | 天津领先正华能源科技发展有限公司 | A kind of pitch waste gas cleaning system |
| CN107281868A (en) * | 2016-04-01 | 2017-10-24 | 中弘环境工程（北京）有限公司 | Bitumen flue gas processing method and equipment |
-
2017
- 2017-11-20 CN CN201711154852.6A patent/CN107758627B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4508851A (en) * | 1982-06-23 | 1985-04-02 | Toho Beslon Co., Ltd. | Fibrous activated carbon and process of producing it |
| CN102755884A (en) * | 2012-04-13 | 2012-10-31 | 山东轻工业学院 | Method for regenerating waste active carbon by chemical medicament |
| CN104342327A (en) * | 2013-08-08 | 2015-02-11 | 厦门泰益新洁净科技有限公司 | Oil-stain cleaning agent as well as preparation method and use method thereof |
| CN104445836A (en) * | 2014-12-26 | 2015-03-25 | 常州大学 | High-concentration asphalt waste water treatment method and device |
| CN105585208A (en) * | 2015-11-24 | 2016-05-18 | 佛山高富中石油燃料沥青有限责任公司 | Asphalt wastewater treatment system |
| CN107281868A (en) * | 2016-04-01 | 2017-10-24 | 中弘环境工程（北京）有限公司 | Bitumen flue gas processing method and equipment |
| CN206198986U (en) * | 2016-08-31 | 2017-05-31 | 天津领先正华能源科技发展有限公司 | A kind of pitch waste gas cleaning system |
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