CN106957297A - A kind of renovation process of inferior sulfolane solvent - Google Patents
A kind of renovation process of inferior sulfolane solvent Download PDFInfo
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- CN106957297A CN106957297A CN201710133155.6A CN201710133155A CN106957297A CN 106957297 A CN106957297 A CN 106957297A CN 201710133155 A CN201710133155 A CN 201710133155A CN 106957297 A CN106957297 A CN 106957297A
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- inferior
- solvent
- sulfolane solvent
- inferior sulfolane
- sulfolane
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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
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- Organic Chemistry (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The present invention relates to the renovation process of inferior sulfolane solvent.Mainly big to solve current inferior sulfolane method for regenerating solvent energy consumption, equipment is more numerous, and speed is slow, system thorough cleaning and should not invent the problem of focus on.By inferior sulfolane solvent and filtering agent mixing and stirring, solid impurity in inferior sulfolane, chlorine and acidic materials formation filtrate is removed by filtration, its filtrate mixes with activated carbon and calcium hydroxide or calcium oxide, filtering, its clear liquid is inferior sulfolane solvent reclamation liquid, and its filter residue is the filtering agent of foregoing inferior sulfolane.Advantage be device general overhaul i.e. thoroughly cleaning when can focus on deterioration sulfolane solvent, regeneration sulfolane solvent is without visible solid state impurity, no suspended substance, lighter so that inferior sulfolane solvent returns to commodity sulfolane solvent level.
Description
Technical field：
The present invention relates to the renovation process of inferior sulfolane solvent, particularly relate to a kind of sulfolane solvent and taken out in aromatic hydrocarbons
Carry, renovation process of C8 extracting phenylethylenes, crude benzole hydrogenation extracting process units longtime running when deteriorating.
Background technology：
At present, industrially generally using sulfolane solvent as Aromatics Extractive Project, C8 extracting phenylethylenes, crude benzole hydrogenation extracting it is molten
Agent, due to being contained acidic materials and chlorine, and the acid that sulfolane solvent is produced in longtime running because degrading in extracting raw material
Property material, make sulfolane solvent pH value decline quality deteriorate.The accumulation of acidic materials and chlorine is made to the hardware in system
Into corrosion, and thus produce solid impurity and extracting efficiency is reduced and fouling of heat exchangers.Chinese patent CN1217367A is disclosed
A kind of renovation process of aromatic hydrocarbon extraction solvent.This method proposes to add solvent equivalent or several times of water, through machinery or bed mistake
Filter, and be dehydrated after 20 ~ 80 mesh granular activated carbons or anion exchange resin absorption.This method needs overall dehydration, and energy consumption is big, set
Standby more numerous, activated carbon pore size is big, easily passes through compared with small molecule, and absorption difficulty is big, and resin adsorption speed also needs regeneration slowly.
In addition CN1076726C discloses the renovation process of inferior sulfolane, and this method is by distilling by inferior sulfolane
Pass through anion exchange resin layer again.This method speed is slow, is only used for lateral line withdrawal function regeneration, and anion exchange resin needs to repeat
Regeneration, system thorough cleaning and should not be focused on.
Other sulfolane solvent is undesirable with resin anion (R.A.) dechlorination effect.
The content of the invention：
The technical problems to be solved by the invention are to provide a kind of renovation process of inferior sulfolane solvent, and this method can be removed and rogued
Solid impurity, chlorine and acidic materials, small suspension, raising pH value in matter sulfolane solvent, make its primary quality measure extensive
The level of commodity sulfolane solvent is arrived again.
What above-mentioned purpose was realized in：By inferior sulfolane solvent and filtering agent mixing and stirring, it is removed by filtration
Solid impurity, chlorine and acidic materials formation filtrate in inferior sulfolane, its filtrate and activated carbon and calcium hydroxide or calcium oxide are mixed
Stirring, filtering are closed, its clear liquid is inferior sulfolane solvent reclamation liquid, and its filter residue is the filtering agent of foregoing inferior sulfolane.Activity
Charcoal consumption regards colourity demand after regeneration and adjusted, and the sulfolane solvent colourity after such as regenerating is deeper, can increase activated carbon dosage, be adopted
With calcium hydroxide or Calcium Oxide Dosage by regenerating after in sulfolane solvent chlorinity adjust.
The mixing temperature of the inferior sulfolane solvent and filtering agent is 25 ~ 60 DEG C.
The water content of the inferior sulfolane solvent is 0.5% ~ 2.5%, if dehydration is needed when water content is more than 2.5%, if not
Moisturizing is needed during foot 0.5%.
It is 35 ~ 60 DEG C that the filtrate mixes temperature with activated carbon and calcium hydroxide or calcium oxide, stirs 40 ~ 60 points
Clock.
The filtrate is 100 with the weight ratio of activated carbon and calcium hydroxide：1~3：0.65~2.
The filtrate is 100 with the weight ratio of activated carbon and calcium oxide：1~3：0.5~1.5.
Used activated carbon is the powdered carbo lignius of micropore, diameter≤1um.
The inferior sulfolane solvent refers to that Aromatics Extractive Project, C8 extracting phenylethylenes, crude benzole hydrogenation extraction device are operating
Sulfolane solvent.
The commodity sulfolane solvent refers to that sterling sulfolane or sulfolane are mixed with other Chemical Solvents and sulfolane contains
Measure ＞ 80% solvent.
First filtering can such as be replaced without filter residue with fresh activity charcoal and calcium hydroxide, inferior sulfolane solvent and activated carbon and
The weight ratio of calcium hydroxide is 100：1~3：0.65~2.
First filtering can such as be replaced without filter residue with fresh activity charcoal and calcium oxide, inferior sulfolane solvent and activated carbon and oxygen
It is 100 to change calcium weight ratio：1~3：0.5~1.5.
The filter residue amount that filter residue consumption obtains for last regeneration.
The advantage of the invention is that device general overhaul can focus on deterioration sulfolane solvent when being thoroughly cleaning, ring is regenerated
Fourth sulfoxide solvent is without visible solid state impurity, no suspended substance, acid number ＜ 0.05mgKOH/g, chlorion ＜ 10ppm, pH value ＞ 7, color
Shoal so that inferior sulfolane solvent returns to commodity sulfolane solvent level.
Embodiment：
By inferior sulfolane solvent and filtering agent mixing and stirring, mixing temperature is 25 ~ 60 DEG C, the water of inferior sulfolane solvent
Content is 0.5% ~ 2.5%, if needing dehydration when water content is more than 2.5%, needs moisturizing when such as less than 0.5%, poor quality is removed by filtration
Solid impurity, chlorine and acidic materials formation filtrate in sulfolane, its filtrate mix with activated carbon and calcium hydroxide or calcium oxide and stirred
Mix, whipping temp is 35 ~ 60 DEG C, stirring is filtered after 40 ~ 60 minutes, its clear liquid is inferior sulfolane solvent reclamation liquid, its filter residue
For the filtering agent of foregoing inferior sulfolane, the filtrate is 100 with the weight ratio of activated carbon and calcium hydroxide：1~3：0.65~2；
The filtrate is 100 with the weight ratio of activated carbon and calcium oxide：1~3：0.5~1.5.Used activated carbon is the powdered wood of micropore
Matter charcoal, diameter≤1um, its consumption regards colourity demand after regeneration and adjusted, and the sulfolane solvent colourity after such as regenerating is deeper, can increase
Activated carbon dosage, chlorinity is adjusted in sulfolane solvent after using calcium hydroxide or Calcium Oxide Dosage by regenerating.
Embodiment 1：
By the inferior sulfolane solvent 100g and filtering agent of Panjin Hua Jin groups device aqueous 2%（Filter residue）Uniformly stirred at 46 DEG C
Vacuum filter after 20 minutes is mixed, residue is removed, and its filtered fluid adds 2g activated carbons and 0.5g calcium oxide is mixed in 60 DEG C of temperature
Vacuum filter obtains sulfolane solvent regenerated liquid after stirring 40 minutes, and filter residue is standby as filtering agent.
Regenerated outcome is shown in Table：
Embodiment 2：
By the inferior sulfolane solvent 100g and filtering agent of golden petrochemical equipment aqueous 0.97% in Ningbo（Filter residue）It is uniform at 35 DEG C
Vacuum filter after stirring 15 minutes, residue is removed, and its filtered fluid adds 2.2g activated carbons and 0.65g calcium hydroxides in 55 DEG C of temperature
It is middle mix 60 minutes after vacuum filter obtain sulfolane solvent regenerated liquid, filter residue is standby as filtering agent.
Regenerated outcome is shown in Table：
Embodiment 3：
By the inferior sulfolane solvent 100g and filtering agent of Hainan Refinery device aqueous 1.2%（Filter residue）The uniform stirring at 45 DEG C
Vacuum filter after 23 minutes, residue is removed, and its filtered fluid adds 3g activated carbons and 1.0g calcium oxide is mixed in 45 DEG C of temperature and stirred
Mix vacuum filter after 50 minutes and obtain sulfolane solvent regenerated liquid, filter residue is standby as filtering agent.
Regenerated outcome is shown in Table：
Embodiment 4：
By the inferior sulfolane solvent 100g and filtering agent of water content 0.5% after Guangxi petrochemical equipment aqueous 6.85%, dehydration（Filter
Slag）Uniform stirring vacuum filter after 20 minutes at 25 DEG C, residue is removed, and its filtered fluid adds 1g activated carbons and 1.6g hydroxides
Vacuum filter obtains sulfolane solvent regenerated liquid after calcium is mixed 40 minutes in 35 DEG C of temperature, and filter residue is standby as filtering agent
With.
Regenerated outcome is shown in Table：
Embodiment 5：
By the inferior sulfolane solvent 100g of water content 2.5% and filtering agent after Shanxi Yang Mei groups device aqueous 5.95%, dehydration（Filter
Slag）Uniform stirring vacuum filter after 23 minutes at 60 DEG C, residue is removed, and its filtered fluid adds 2g activated carbons and 1.5g calcium oxide
Vacuum filter obtains sulfolane solvent regenerated liquid after being mixed 50 minutes in 45 DEG C of temperature, and filter residue is standby as filtering agent.
Regenerated outcome is shown in Table：
Embodiment 6：
By the inferior sulfolane solvent 100g and filtering agent of Hainan Refinery device aqueous 1.4%（Filter residue）The uniform stirring at 50 DEG C
Vacuum filter after 22 minutes, residue is removed, and its filtered fluid adds 3g activated carbons and 2.0g calcium hydroxides are mixed in 45 DEG C of temperature
Vacuum filter obtains sulfolane solvent regenerated liquid after stirring 50 minutes, and filter residue is standby as filtering agent.
Regenerated outcome is shown in Table：
Note：Chloride test method：ASTM D512-89（1999）Chlorion in water, detection method；
Regeneration sample is compared with company standard：
Note：Regenerated solvent includes other solvents, therefore does not do purity, density, boiling range detection.
Claims (6)
1. a kind of renovation process of inferior sulfolane solvent, it is characterized in that：Inferior sulfolane solvent and filtering agent are mixed
Uniformly, solid impurity in inferior sulfolane, chlorine and acidic materials formation filtrate, its filtrate and activated carbon and hydrogen-oxygen is removed by filtration
Change calcium or calcium oxide is mixed, filtering, its clear liquid is inferior sulfolane solvent reclamation liquid, its filter residue is foregoing inferior sulfolane
Filtering agent.
2. according to the renovation process of the inferior sulfolane solvent described in claim 1, it is characterized in that：The inferior sulfolane solvent
Mixing temperature with filtering agent is 25 ~ 60 DEG C.
3. according to the renovation process of the inferior sulfolane solvent described in claim 1 or 2, it is characterized in that：The inferior sulfolane
The water content of solvent is 0.5% ~ 2.5%, if needing dehydration when water content is more than 2.5%, moisturizing is needed when such as less than 0.5%.
4. according to the renovation process of the inferior sulfolane solvent described in claim 1, it is characterized in that：The filtrate and activated carbon and
It is 35 ~ 60 DEG C that calcium hydroxide or calcium oxide, which mix temperature, is stirred 40 ~ 60 minutes.
5. according to the renovation process of the inferior sulfolane solvent described in claim 1, it is characterized in that：The filtrate and activated carbon and
The weight ratio of calcium hydroxide is 100：1~3：0.65~2；The filtrate is 100 with the weight ratio of activated carbon and calcium oxide：1~3：
0.5~1.5。
6. according to the renovation process of the inferior sulfolane solvent described in claim 1, it is characterized in that：Used activated carbon is micropore
Powdered carbo lignius, diameter≤1um.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110505907.3A CN113149955A (en) | 2016-12-31 | 2017-03-08 | Regeneration method of inferior sulfolane solvent |
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| CN2016112666953 | 2016-12-31 | ||
| CN201611266695 | 2016-12-31 |
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| CN202110505907.3A Division CN113149955A (en) | 2016-12-31 | 2017-03-08 | Regeneration method 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 (5)
| 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 |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076726C (en) * | 1998-03-26 | 2001-12-26 | 中国石油化工集团公司 | Regeneration process of inferior sulfolane |
-
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 (5)
| 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 |
| 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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