CN113149955A - Regeneration method of inferior sulfolane solvent - Google Patents
Regeneration method of inferior sulfolane solvent Download PDFInfo
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- CN113149955A CN113149955A CN202110505907.3A CN202110505907A CN113149955A CN 113149955 A CN113149955 A CN 113149955A CN 202110505907 A CN202110505907 A CN 202110505907A CN 113149955 A CN113149955 A CN 113149955A
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- sulfolane solvent
- sulfolane
- poor
- solvent
- activated carbon
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D333/00—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom
- C07D333/02—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom not condensed with other rings
- C07D333/46—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom not condensed with other rings substituted on the ring sulfur atom
- C07D333/48—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom not condensed with other rings substituted on the ring sulfur atom by oxygen atoms
Abstract
The invention relates to a regeneration method of an inferior sulfolane solvent. The method is invented for mainly solving the problems of high energy consumption, complex equipment, low speed and unsuitability for thorough cleaning and centralized treatment of a system in the existing inferior sulfolane solvent regeneration method. Mixing and stirring the poor-quality sulfolane solvent and the filtering agent uniformly, filtering to remove solid impurities, chlorine and acidic substances in the poor-quality sulfolane to form filtrate, mixing and stirring the filtrate with activated carbon and calcium hydroxide or calcium oxide, and filtering to obtain clear liquid which is the poor-quality sulfolane solvent regeneration liquid and filter residues which are the filtering agent of the poor-quality sulfolane. The advantage lies in that the device overhauls can centralized processing degradation sulfolane solvent when thorough cleaning promptly greatly, and regeneration sulfolane solvent does not have visible solid-state impurity, does not have the suspended solid, thereby the colour lightens makes the sulfolane solvent of inferior quality resume commodity sulfolane solvent level.
Description
The application is a divisional application with application date of 2017, 03 and 08, application number of 201710133155.6 and invention name of 'a regeneration method of inferior sulfolane solvent'.
Technical Field
The invention relates to a regeneration method of an inferior sulfolane solvent, in particular to a regeneration method of a sulfolane solvent when degradation occurs to a production device for aromatic hydrocarbon extraction, styrene extraction by C8 and hydrogenation extraction of crude benzene for a long time.
Background
At present, the sulfolane solvent is generally adopted in industry as a solvent for aromatic hydrocarbon extraction, C8 extraction of styrene and crude benzene hydrogenation extraction, and because the extracted raw material contains acidic substances and chlorine and the sulfolane solvent degrades the pH value of the sulfolane solvent due to the acidic substances generated by degradation in long-term operation. The accumulation of acidic species and chlorine causes corrosion of the metal equipment in the system and thereby produces solid impurities and reduces the stripping performance and fouling of the heat exchangers. Chinese patent CN1217367A discloses a regeneration method of an aromatic extraction solvent. The method comprises the steps of adding water with the same amount or multiple times of solvent, filtering by a mechanical or bed layer, adsorbing by 20-80-mesh granular active carbon or anion exchange resin, and dehydrating. The method needs integral dehydration, large energy consumption, complex equipment, large aperture of the active carbon, easy passing of small molecules, large adsorption difficulty, low resin adsorption speed and regeneration.
In addition, CN1076726C discloses a process for regenerating poor quality sulfolane by distilling the poor quality sulfolane through an anion exchange resin layer. The method has low speed, can only be used for lateral line extraction and regeneration, and the anion exchange resin needs to be regenerated repeatedly, so that the method is not suitable for thorough cleaning and centralized treatment of the system.
In addition, the dechlorination effect of the sulfolane solvent by using the anion resin is not ideal.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a regeneration method of an inferior sulfolane solvent, which can remove solid impurities, chlorine, acidic substances and tiny suspended matters in the inferior sulfolane solvent, improve the PH value and restore the main quality index to the level of a commercial sulfolane solvent.
The above object is achieved by: mixing and stirring the poor-quality sulfolane solvent and the filtering agent uniformly, removing solid impurities, chlorine and acidic substances in the poor-quality sulfolane through primary filtration to form filtrate, mixing and stirring the filtrate with activated carbon and calcium hydroxide or calcium oxide, and filtering, wherein the clear solution is poor-quality sulfolane solvent regenerated liquid, and the filter residue is the filtering agent of the poor-quality sulfolane. The dosage of the activated carbon is adjusted according to the requirement of the regenerated chroma, if the chroma of the regenerated sulfolane solvent is deeper, the dosage of the activated carbon can be increased, and the dosage of the adopted calcium hydroxide or calcium oxide is adjusted by the content of chlorine in the regenerated sulfolane solvent.
The mixing temperature of the poor sulfolane solvent and the filtering agent is 25-60 ℃.
The water content of the poor sulfolane solvent is 0.5-2.5%, dehydration is needed if the water content exceeds 2.5%, and water is needed if the water content is less than 0.5%.
And mixing and stirring the filtrate, activated carbon and calcium hydroxide or calcium oxide at the temperature of 35-60 ℃ for 40-60 minutes.
The weight ratio of the filtrate to the activated carbon to the calcium hydroxide is 100: 1-3: 0.65 to 2.
The weight ratio of the filtrate to the activated carbon and the calcium oxide is 100: 1-3: 0.5 to 1.5.
The adopted active carbon is microporous powdery wood carbon with the diameter less than or equal to 1 um.
The poor sulfolane solvent refers to a sulfolane solvent in the operation of an aromatic hydrocarbon extraction device, a C8 styrene extraction device and a crude benzene hydrogenation extraction device.
The commercial sulfolane solvent is pure sulfolane or a solvent which is mixed with other chemical solvents and has sulfolane content of more than 80 percent.
If no filter residue is left in the primary filtration, the filter residue can be replaced by fresh activated carbon and calcium hydroxide, and the weight ratio of the inferior sulfolane solvent to the activated carbon and the calcium hydroxide is 100: 1-3: 0.65 to 2.
If no filter residue is filtered for the first time, the filter residue can be replaced by fresh activated carbon and calcium oxide, and the weight ratio of the inferior sulfolane solvent to the activated carbon to the calcium oxide is 100: 1-3: 0.5 to 1.5.
The filter residue consumption is the filter residue amount obtained in the last regeneration.
The invention has the advantages that the device can intensively treat the degraded sulfolane solvent when being overhauled, namely cleaned thoroughly, the regenerated sulfolane solvent has no visible solid impurities and no suspended matters, the acid value is less than 0.05mgKOH/g, the chloride ion is less than 10ppm, the PH value is more than 7, and the color becomes light, thereby leading the poor sulfolane solvent to be recovered to the level of the commodity sulfolane solvent.
Detailed Description
Mixing and stirring an inferior sulfolane solvent and a filtering agent uniformly, wherein the mixing temperature is 25-60 ℃, the water content of the inferior sulfolane solvent is 0.5-2.5%, if the water content exceeds 2.5%, dehydration is required, if the water content is less than 0.5%, water is required, filtering is carried out to remove solid impurities, chlorine and acidic substances in the inferior sulfolane to form a filtrate, the filtrate is mixed and stirred with activated carbon and calcium hydroxide or calcium oxide, the stirring temperature is 35-60 ℃, the filtrate is filtered after being stirred for 40-60 minutes, the clear liquid is an inferior sulfolane solvent regenerated liquid, the filter residue is the filtering agent of the inferior sulfolane, and the weight ratio of the filtrate to the activated carbon and the calcium hydroxide is 100: 1-3: 0.65 to 2; the weight ratio of the filtrate to the activated carbon and the calcium oxide is 100: 1-3: 0.5 to 1.5. The adopted activated carbon is microporous powdery wood carbon with the diameter less than or equal to 1um, the dosage is adjusted according to the requirement of the regenerated chroma, if the chroma of the regenerated sulfolane solvent is deeper, the dosage of the activated carbon can be increased, and the dosage of the adopted calcium hydroxide or calcium oxide is adjusted by the content of chlorine in the regenerated sulfolane solvent.
Example 1:
100g of inferior sulfolane solvent containing 2% of water and a filtering agent (filter residue) are uniformly stirred for 20 minutes at 46 ℃, then vacuum filtration is carried out, the residue is removed, 2g of activated carbon and 0.5g of calcium oxide are added into the filtrate, the mixture is mixed and stirred for 40 minutes at the temperature of 60 ℃, then vacuum filtration is carried out, so as to obtain sulfolane solvent regeneration liquid, and the filter residue is used as the filtering agent for standby.
The regeneration results are shown in the table:
example 2:
100g of inferior sulfolane solvent containing 0.97% of water in a Ningbo gold petrochemical device and a filtering agent (filter residue) are uniformly stirred for 15 minutes at 35 ℃, then vacuum filtration is carried out, the residue is removed, 2.2g of activated carbon and 0.65g of calcium hydroxide are added into the filtrate, the mixture is mixed and stirred for 60 minutes at the temperature of 55 ℃, then vacuum filtration is carried out, so that sulfolane solvent regeneration liquid is obtained, and the filter residue is used as the filtering agent for standby.
The regeneration results are shown in the table:
example 3:
100g of inferior sulfolane solvent containing 1.2% of water in a Hainan refining device and a filtering agent (filter residue) are uniformly stirred for 23 minutes at 45 ℃, then vacuum filtration is carried out, the residue is removed, 3g of activated carbon and 1.0g of calcium oxide are added into the filtrate, the mixture is mixed and stirred for 50 minutes at 45 ℃, then vacuum filtration is carried out, so that sulfolane solvent regeneration liquid is obtained, and the filter residue is used as the filtering agent for standby.
The regeneration results are shown in the table:
example 4:
100g of inferior sulfolane solvent with 6.85% of water content and 0.5% of dehydrated water content in Guangxi petrochemical plant and filtering agent (filter residue) are uniformly stirred for 20 minutes at 25 ℃, then vacuum filtration is carried out, the residue is removed, 1g of activated carbon and 1.6g of calcium hydroxide are added into the filtrate, the mixture is mixed and stirred for 40 minutes at 35 ℃, then vacuum filtration is carried out, thus obtaining sulfolane solvent regeneration liquid, and the filter residue is used as the filtering agent for standby.
The regeneration results are shown in the table:
example 5:
100g of inferior sulfolane solvent with the water content of 5.95 percent and the water content of 2.5 percent after dehydration and a filtering agent (filter residue) are uniformly stirred for 23 minutes at the temperature of 60 ℃, then vacuum filtration is carried out, the residue is removed, 2g of active carbon and 1.5g of calcium oxide are added into the filtrate, the mixture is mixed and stirred for 50 minutes at the temperature of 45 ℃, then vacuum filtration is carried out, thus obtaining the sulfolane solvent regeneration liquid, and the filter residue is used as the filtering agent for standby.
The regeneration results are shown in the table:
example 6:
100g of inferior sulfolane solvent containing 1.4 percent of water in a Hainan refining device and a filtering agent (filter residue) are uniformly stirred for 22 minutes at 50 ℃, then vacuum filtration is carried out, the residue is removed, 3g of active carbon and 2.0g of calcium hydroxide are added into the filtrate, the mixture is mixed and stirred for 50 minutes at 45 ℃, then vacuum filtration is carried out, so as to obtain sulfolane solvent regeneration liquid, and the filter residue is used as the filtering agent for standby.
The regeneration results are shown in the table:
note: the chloride ion detection method comprises the following steps: ASTM D512-89(1999) method for detecting chloride ion in water;
comparing the regenerated sample with the enterprise standard:
note: the regenerated solvent contains other solvents, so the purity, density and distillation range detection is not carried out.
Claims (3)
1. The regeneration method of the poor sulfolane solvent is characterized by comprising the following steps:
mixing and stirring the poor-quality sulfolane solvent and the filtering agent uniformly, and removing solid impurities, chlorine and acidic substances in the poor-quality sulfolane through primary filtration to form filtrate; the mixing and stirring temperature is 25-60 ℃; the water content of the poor sulfolane solvent is 0.5% -2.5%, when the water content exceeds 2.5%, dehydration is carried out, and when the water content is less than 0.5%, water is supplemented; the poor sulfolane solvent is a sulfolane solvent in the operation of an aromatic hydrocarbon extraction device, a C8 styrene extraction device and a crude benzene hydrogenation extraction device;
mixing and stirring the filtrate with activated carbon and calcium hydroxide or calcium oxide at the stirring temperature of 35-60 ℃ for 40-60 minutes, and filtering to obtain a clear liquid and filter residues, wherein the clear liquid is an inferior sulfolane solvent regeneration liquid, and the filter residues are the filtering agent of the inferior sulfolane;
the weight ratio of the filtrate to the activated carbon to the calcium hydroxide is 100: 1-3: 0.65 to 2; the weight ratio of the filtrate to the activated carbon and the calcium oxide is 100: 1-3: 0.5 to 1.5;
the adopted active carbon is microporous powdery wood carbon with the diameter less than or equal to 1 mu m.
2. The regeneration method of claim 1, wherein no filter residue after primary filtration is replaced by fresh activated carbon and calcium hydroxide, and the weight ratio of the inferior sulfolane solvent to the activated carbon and calcium hydroxide is 100: 1-3: 0.65 to 2.
3. The regeneration method of claim 1, wherein no filter residue after primary filtration is replaced by fresh activated carbon and calcium oxide, and the weight ratio of the inferior sulfolane solvent to the activated carbon and calcium oxide is 100: 1-3: 0.5 to 1.5.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
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| CN2016112666953 | 2016-12-31 | ||
| CN201611266695 | 2016-12-31 | ||
| CN201710133155.6A CN106957297A (en) | 2016-12-31 | 2017-03-08 | A kind of renovation process of inferior sulfolane solvent |
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| CN201710133155.6A Division CN106957297A (en) | 2016-12-31 | 2017-03-08 | A kind of renovation process of inferior sulfolane solvent |
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| CN201710133155.6A Pending CN106957297A (en) | 2016-12-31 | 2017-03-08 | A kind of renovation process of inferior sulfolane solvent |
| CN202110505907.3A Pending CN113149955A (en) | 2016-12-31 | 2017-03-08 | Regeneration method of inferior sulfolane solvent |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07101953A (en) * | 1993-10-06 | 1995-04-18 | Kawasaki Steel Corp | Purification of used sulfolane |
| CN1217367A (en) * | 1997-11-11 | 1999-05-26 | 中国石油化工总公司 | Process for regenerating aromatic hydrocarbon extraction solvent |
| CN1230545A (en) * | 1998-03-26 | 1999-10-06 | 中国石油化工总公司 | Regeneration process of inferior sulfolane |
| CN1634917A (en) * | 2004-10-12 | 2005-07-06 | 南京工业大学 | Method for removing corrosive impurity from inferior sulfolane |
| CN1644581A (en) * | 2004-11-25 | 2005-07-27 | 中国石化集团天津石油化工公司 | Method for removing chlorine and corrosion negative ions from poor sulfolane |
| CN102686294A (en) * | 2009-10-19 | 2012-09-19 | 台湾中油股份有限公司 | Process and apparatus for online rejuvenation of contaminated sulfolane solvent |
-
2017
- 2017-03-08 CN CN201710133155.6A patent/CN106957297A/en active Pending
- 2017-03-08 CN CN202110505907.3A patent/CN113149955A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07101953A (en) * | 1993-10-06 | 1995-04-18 | Kawasaki Steel Corp | Purification of used sulfolane |
| CN1217367A (en) * | 1997-11-11 | 1999-05-26 | 中国石油化工总公司 | Process for regenerating aromatic hydrocarbon extraction solvent |
| CN1230545A (en) * | 1998-03-26 | 1999-10-06 | 中国石油化工总公司 | Regeneration process of inferior sulfolane |
| CN1634917A (en) * | 2004-10-12 | 2005-07-06 | 南京工业大学 | Method for removing corrosive impurity from inferior sulfolane |
| CN1644581A (en) * | 2004-11-25 | 2005-07-27 | 中国石化集团天津石油化工公司 | Method for removing chlorine and corrosion negative ions from poor sulfolane |
| CN102686294A (en) * | 2009-10-19 | 2012-09-19 | 台湾中油股份有限公司 | Process and apparatus for online rejuvenation of contaminated sulfolane solvent |
Non-Patent Citations (3)
| Title |
|---|
| 于涛: ""降低环丁砜抽提系统腐蚀性与工业应用"", 《腐蚀与防护》 * |
| 李明玉: ""抽提蒸馏单元高胶质含量环丁砜净化方法研究"", 《现代化工》 * |
| 李明玉等: ""芳烃抽提装置中环丁砜循环系统设备腐蚀原因及对策"", 《石油炼制与化工》 * |
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Application publication date: 20210723 |