CN111036642A - Method for removing Fe in dichloroethane industrial waste3+Process for preparing (A) a - Google Patents
Method for removing Fe in dichloroethane industrial waste3+Process for preparing (A) a Download PDFInfo
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- CN111036642A CN111036642A CN201811188628.3A CN201811188628A CN111036642A CN 111036642 A CN111036642 A CN 111036642A CN 201811188628 A CN201811188628 A CN 201811188628A CN 111036642 A CN111036642 A CN 111036642A
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- industrial waste
- dichloroethane
- water
- acidified
- washing
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- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title abstract description 10
- 239000002440 industrial waste Substances 0.000 claims abstract description 77
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 63
- 238000005406 washing Methods 0.000 claims abstract description 60
- 239000002253 acid Substances 0.000 claims abstract description 28
- 230000008569 process Effects 0.000 claims abstract description 25
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229960003750 ethyl chloride Drugs 0.000 claims abstract description 18
- 230000020477 pH reduction Effects 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 11
- 239000003054 catalyst Substances 0.000 abstract description 4
- 238000011112 process operation Methods 0.000 abstract description 2
- 239000013505 freshwater Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 206010043275 Teratogenicity Diseases 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007886 mutagenicity Effects 0.000 description 1
- 231100000299 mutagenicity Toxicity 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 231100000211 teratogenicity Toxicity 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Removal Of Specific Substances (AREA)
- Catalysts (AREA)
Abstract
The invention provides a method for removing Fe in dichloroethane industrial waste3+The process comprises the following steps: s1: acidifying the dichloroethane industrial waste, and separating to obtain circulating acid and the acidified dichloroethane industrial waste; s2: washing the ethyl chloride industrial waste acidified in the step S1 with water in a water washing tower, and separating to obtain water and Fe-removed water3+Industrial waste of dichloroethane. The invention adopts a mode of acidification before water washing, has simple process operation and obvious effect, and can remove Fe in dichloroethane industrial waste3+The concentration is reduced from 1000ppm to less than 110ppm, and the Fe content of a subsequent incineration device is greatly reduced2O3The production amount of the catalyst prolongs the operation time and reduces the production cost.
Description
Technical Field
The invention belongs to the field of petrochemical industry, and particularly relates to a method for removing Fe in dichloroethane industrial waste3+The process of (1).
Background
The industrial waste of dichloroethane generated in the industrial production of dichloroethane, which comprises chlorine-containing dangerous waste and other high-boiling residues, has the effects of carcinogenesis, teratogenicity and mutagenicity. If the treatment is not thorough enough, the health and ecological environment of surrounding residents can be seriously threatened. The components of the dichloroethane industrial waste have the characteristics of complexity, difficult biodegradation, difficult thorough treatment of common treatment means and the like, and the method can thoroughly decompose and convert the dichloroethane industrial waste and reach the emission standard by adopting an incineration treatment technology, and is one of the most thorough methods for treating the dichloroethane industrial waste.
Because the dichloroethane industrial waste contains Fe3+Fe is generated in the course of burning dichloroethane industrial waste2O3And continuously accumulates to block the pipeline, greatly shortens the running time of incineration treatment equipment, and therefore, the Fe in the dichloroethane industrial waste is removed before incineration3+It is imperative.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for removing Fe in dichloroethane industrial waste3+To remove Fe from dichloroethane industrial waste before incineration3+Greatly reduces the Fe content of the subsequent incineration device2O3The production amount of the catalyst is increased, the running time is prolonged, and the production cost is reduced.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
method for removing Fe in dichloroethane industrial waste3+The process comprises the following steps:
s1: acidifying the dichloroethane industrial waste, and separating to obtain circulating acid and the acidified dichloroethane industrial waste;
s2: washing the ethyl chloride industrial waste acidified in the step S1 with water in a water washing tower, and separating to obtain water and Fe-removed water3+Industrial waste of dichloroethane.
Further, the acid used for the acidification in step S1 is any one of hydrochloric acid, sulfuric acid, and nitric acid.
Further, the flow ratio of the dichloroethane industrial waste to the acid upon acidification in step S1 is 0.2 to 5: 1.
Further, in the separation in step S1, a separation tower is used to obtain layered recycle acid and acidified dichloroethane industrial waste, the acidified chloroethane industrial waste flows out from the lower part of the separation tower, the recycle acid flows out from the upper part of the separation tower, and the recycle acid is recycled.
Further, upon acidification in step S1, the acid and the dichloroethane industrial waste are thoroughly mixed in a mixer before entering the separation column.
Further, in the step S2, the washing tower is used for washing, the acidified chloroethane industrial waste flows in from the upper part of the washing tower and flows out from the bottom of the washing tower, the washing water flows in from the lower part of the washing tower and flows out from the top of the washing tower, and the washing water is recycled.
Further, when washing is performed in step S2, the flow ratio of the acidified dichloroethane industrial waste to the washing water is 1: 0.5-6.
Compared with the prior art, the method for removing Fe in dichloroethane industrial waste3+The process has the following advantages:
adopts incineration treatment of dichloroethane industrial waste generated in dichloroethane production process, and Fe in the dichloroethane industrial waste before industrial application of the process3+The content of (A) is about 1000ppm (the main source is the active metal component of the catalyst in the production process), taking the handling capacity of 1 ton/day as an example, the operation needs to be stopped for cleaning a blocked pipeline for about half a month, and the analysis shows that the blocking component is almost all Fe2O3. The process adopts a mode of firstly acidifying and then washing, has simple process operation and obvious effect, and can remove Fe in dichloroethane industrial waste3+The concentration is reduced from 1000ppm to less than 110ppm, and the Fe content of a subsequent incineration device is greatly reduced2O3The production amount of the catalyst prolongs the operation time and reduces the production cost.
Drawings
FIG. 1 shows the removal of industrial waste dichloroethane according to the inventionIn which Fe is present3+A flow chart of the process of (1).
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to the following examples and accompanying drawings.
Example 1
Method for removing Fe in dichloroethane industrial waste3+The process comprises the following steps:
sulfuric acid and Fe-containing3+Introducing the dichloroethane industrial waste into a mixer according to the flow ratio of 0.5:1, and fully mixing. And (3) obtaining layered circulating acid and acidified dichloroethane industrial waste by using a separation tower, wherein the acidified chloroethane industrial waste flows out from the lower part of the separation tower, and the circulating acid flows out from the upper part of the separation tower. The circulating acid is recycled, and the circulating acid needs to be supplemented and discharged periodically.
The acidified chloroethane industrial waste flows in from the upper part of the water washing tower and flows out from the bottom of the water washing tower, the water washing water flows in from the lower part of the water washing tower and flows out from the top of the water washing tower, and the two flows oppositely. The flow ratio of the acidified dichloroethane industrial waste to the washing water is 1: 2. the water washing water is recycled, and fresh water is periodically drained and supplemented.
The process effect is Fe removal3+Has obvious effect and can effectively mix Fe3+From 1000ppm to 108 ppm.
Example 2
Method for removing Fe in dichloroethane industrial waste3+The process comprises the following steps:
nitric acid and Fe3+Introducing the dichloroethane industrial waste into a mixer according to the flow ratio of 1:1, and fully mixing. Using a separation tower to obtain layered recycle acid and acidified dichloroethane industrial waste, wherein the acidified dichloroethane industrial waste flows out from the lower part of the separation tower, and the recycle acid is separatedFlows out of the upper part of the tower. The circulating acid needs to be supplemented and discharged periodically.
The acidified chloroethane industrial waste flows in from the upper part of the water washing tower and flows out from the bottom of the water washing tower, the water washing water flows in from the lower part of the water washing tower and flows out from the top of the water washing tower, and the two flows oppositely. The flow ratio of the acidified dichloroethane industrial waste to the washing water is 1: 2. the water washing water is recycled, and fresh water is periodically drained and supplemented.
The process effect is Fe removal3+Has obvious effect and can effectively mix Fe3+From 1000ppm to 85 ppm.
Example 3
Method for removing Fe in dichloroethane industrial waste3+The process comprises the following steps:
hydrochloric acid and Fe3+Introducing the dichloroethane industrial waste into a mixer according to the flow ratio of 2:1, and fully mixing. And (3) obtaining layered circulating acid and acidified dichloroethane industrial waste by using a separation tower, wherein the acidified chloroethane industrial waste flows out from the lower part of the separation tower, and the circulating acid flows out from the upper part of the separation tower. The circulating acid needs to be supplemented and discharged periodically.
The acidified chloroethane industrial waste flows in from the upper part of the water washing tower and flows out from the bottom of the water washing tower, the water washing water flows in from the lower part of the water washing tower and flows out from the top of the water washing tower, the water washing water and the acidified chloroethane industrial waste are fully mixed, and the water washing water washes the acidified chloroethane industrial waste. The flow ratio of the acidified dichloroethane industrial waste to the washing water is 1: 3. the water washing water is recycled, and fresh water is periodically drained and supplemented.
The process effect is Fe removal3+Has obvious effect and can effectively mix Fe3+From 1000ppm to 72 ppm.
Example 4
Method for removing Fe in dichloroethane industrial waste3+The process comprises the following steps:
nitric acid and Fe3+Introducing the dichloroethane industrial waste into a mixer according to the flow ratio of 1:1, and fully mixing. Using a separation column to obtainThe layer of recycle acid and acidified dichloroethane industrial waste, the acidified chloroethane industrial waste flowing out of the lower part of the separation column and the recycle acid flowing out of the upper part of the separation column. The circulating acid needs to be supplemented and discharged periodically.
The acidified chloroethane industrial waste flows in from the upper part of the water washing tower and flows out from the bottom of the water washing tower, the water washing water flows in from the lower part of the water washing tower and flows out from the top of the water washing tower, the water washing water and the acidified chloroethane industrial waste are fully mixed, and the water washing water washes the acidified chloroethane industrial waste. The flow ratio of the acidified dichloroethane industrial waste to the washing water is 1: 6. the water washing water is recycled, and fresh water is periodically drained and supplemented.
The process effect is Fe removal3+Has obvious effect and can effectively mix Fe3+From 1000ppm to 75 ppm.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. Method for removing Fe in dichloroethane industrial waste3+The process is characterized in that: the method comprises the following steps:
s1: acidifying the dichloroethane industrial waste, and separating to obtain circulating acid and the acidified dichloroethane industrial waste;
s2: washing the ethyl chloride industrial waste acidified in the step S1 with water in a water washing tower, and separating to obtain water and Fe-removed water3+Industrial waste of dichloroethane.
2. The process of claim 1 for removing Fe from industrial waste of dichloroethane3+The process is characterized in that: the acid used for acidification in step S1 is any one of hydrochloric acid, sulfuric acid, and nitric acid.
3. The process of claim 1 for removing Fe from industrial waste of dichloroethane3+The process is characterized in that: and during acidification in the step S1, the flow ratio of the dichloroethane industrial waste to the acid is 0.2-5: 1.
4. The process of claim 1 for removing Fe from industrial waste of dichloroethane3+The process is characterized in that: in the separation in the step S1, a separation tower is adopted to obtain layered recycle acid and acidified dichloroethane industrial waste, the acidified chloroethane industrial waste flows out from the lower part of the separation tower, the recycle acid flows out from the upper part of the separation tower, and the recycle acid is recycled.
5. The method for removing Fe in dichloroethane industrial waste according to claim 43+The process is characterized in that: upon acidification in step S1, the acid and the dichloroethane industrial waste are thoroughly mixed in a mixer before entering the separation column.
6. The process of claim 1 for removing Fe from industrial waste of dichloroethane3+The process is characterized in that: and step S2, the washing tower is adopted for washing, the acidified chloroethane industrial waste flows in from the upper part of the washing tower and flows out from the bottom of the washing tower, the washing water flows in from the lower part of the washing tower and flows out from the top of the washing tower, and the washing water is recycled.
7. The method for removing Fe in dichloroethane industrial waste according to claim 63+The process is characterized in that: and when the washing is carried out in the step S2, the flow ratio of the acidified dichloroethane industrial waste to the washing water is 1: 0.5-6.
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| CN201811188628.3A CN111036642B (en) | 2018-10-12 | 2018-10-12 | Method for removing Fe in dichloroethane industrial waste3+Process for preparing (A) a |
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| CN201811188628.3A CN111036642B (en) | 2018-10-12 | 2018-10-12 | Method for removing Fe in dichloroethane industrial waste3+Process for preparing (A) a |
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Cited By (2)
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| CN113171584A (en) * | 2021-04-26 | 2021-07-27 | 天津海成能源工程技术有限公司 | Iron removing liquid and method for removing iron ions of high-boiling residues of VCM device |
| CN114425175A (en) * | 2020-09-05 | 2022-05-03 | 中国石油化工股份有限公司 | High-boiling-point substance metal ion extraction and removal system and process |
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2018
- 2018-10-12 CN CN201811188628.3A patent/CN111036642B/en active Active
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114425175A (en) * | 2020-09-05 | 2022-05-03 | 中国石油化工股份有限公司 | High-boiling-point substance metal ion extraction and removal system and process |
| CN114425175B (en) * | 2020-09-05 | 2023-04-07 | 中国石油化工股份有限公司 | High-boiling-point substance metal ion extraction and removal system and process |
| CN113171584A (en) * | 2021-04-26 | 2021-07-27 | 天津海成能源工程技术有限公司 | Iron removing liquid and method for removing iron ions of high-boiling residues of VCM device |
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