CN104788422A - Continuous production method for preparing sulfolane from crude butadiene sulfone - Google Patents
Continuous production method for preparing sulfolane from crude butadiene sulfone Download PDFInfo
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- CN104788422A CN104788422A CN201510113499.1A CN201510113499A CN104788422A CN 104788422 A CN104788422 A CN 104788422A CN 201510113499 A CN201510113499 A CN 201510113499A CN 104788422 A CN104788422 A CN 104788422A
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- desulfurization
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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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Abstract
The invention discloses a continuous production method for preparing sulfolane from crude butadiene sulfone. The method comprises the following steps: mixing crude butadiene sulfone with a solvent to prepare a butadiene sulfone solution, mixing the butadiene sulfone solution with nitrogen, and allowing the nitrogen mixed solution to go through a first-stage desulphurization mixer (1) and a first-stage desulphurization separator (3) to take away sulfur dioxide by nitrogen in order to decrease the content of sulfur dioxide to 0.05%; neutralizing sulfur dioxide residual in the butadiene sulfone solution after first-stage desulphurization in a second-stage desulphurization mixer (2) by an alkali solution, allowing the second-stage desulphurized butadiene sulfone solution to go through a filter (13) to filter out insoluble substances, allowing the insoluble removed sulfolene solution, hydrogen and a homogeneous catalyst to be mixed and enter a hydrogenation loop reactor (14), and carrying out a hydrogenation reaction; separating out unreacted hydrogen from the above obtained reaction product to obtain crude sulfolane; and washing nitrogen carrying sulfur dioxide, separating, respectively discharging nitrogen and sulfur dioxide from a device, and recycling nitrogen and sulfur dioxide. The continuous production method for preparing sulfolane from crude butadiene sulfone has the advantages of stable production process, large productivity and operational flexibility, high raw material utilization rate and good product quality.
Description
Technical field
The present invention relates to a kind of preparation method of solvent, particularly a kind of thick cyclobufene sultone produces the continuous production method of tetramethylene sulfone.
Background technology
Tetramethylene sulfone is a kind of excellent high temperature resistant, aprotic polar solvent, and can dissolve each other with water, acetone, toluene etc., be the ideal solvent in arene extracting process.Tetramethylene sulfone also can be used for acid gas purifying and recovery, extraction distillation solvent, polymer solvent and all kinds of reaction solvent, evenly applying in fields such as paper industry, oil prodution industry, electronic industry and textile industries in addition, is a kind of purposes fine chemicals very widely.
Industrial tetramethylene sulfone is generally prepared by cyclobufene sultone shortening.Because of containing excessive sulfurous gas in crude product cyclobufene sultone, sulfurous gas need be deviate from before shortening.Desulfurization disclosed in GB1123533, US3622598, US5030737, CN102020632A and hydrogenation process are and adopt tank reactor or tower reactor, and production process is batch process procedures.
Summary of the invention
the object of the present invention is to provide a kind of with thick cyclobufene sultone be desulfurization of raw material, the continuous processing of hydrogenation synthesis cyclobufene sultone.The present invention adopts two-stage desulfurization, sulfur dioxide recovery, annular-pipe reactor hydrogenation, make to realize continuous prodution by thick cyclobufene sultone desulfurization and hydrogenation synthesis tetramethylene sulfone, desulfurization is thorough, raw material availability is high, and production efficiency is high, the residence time is controlled, turndown ratio is large, non-environmental-pollution.
technical scheme of the present invention is as follows:
Thick cyclobufene sultone produces a continuous production method for tetramethylene sulfone, comprises following production equipment and using method:
A. production equipment comprises: solvent dispersion device, one section of desulfurization mixing tank, one section of desulfurization separator, desulfur pump, nitrogen washings device, washing separating tank, absorb flow container, absorb liquid pump, well heater, sulfurous gas flash tank, water cooler, two sections of desulfurization mixing tanks, strainer, hydrogenation annular-pipe reactor, back pressure valve, tetramethylene sulfone separating tank, equipment room connection line, control instruments and annexes;
B. working method comprises:
A. liquid thick cyclobufene sultone and solvent enter solvent dispersion device in proportion and prepare alkene sulfolane solution; The alkene sulfolane solution that alkene sulfolane solution and desulfur pump return and nitrogen converge and enter one section of desulfurization mixing tank and fully mix, and make the sulfurous gas in alkene sulfolane solution transfer in nitrogen; The material going out one section of desulfurization mixing tank carries out two-phase laminated flow in one section of desulfurization separator, and liquid phase enters two sections of desulfurization mixing tanks through the extraction of a desulfur pump part and continues desulfurization, and another part is circulated to one section of desulfurization mixer entrance; In liquid phase (alkene sulfolane solution), the content of sulfurous gas is by-extraction ratio the control that circulates, and circulation-extraction is than larger, and content of sulfur dioxide is lower; Through one section of desulfurization, content of sulfur dioxide in alkene sulfolane solution is down to about 0.05%(massfraction);
B. the nitrogen carrying sulfurous gas secretly is fully mixed through nitrogen washings device by the gaseous phase outlet discharge of one section of desulfurization separator with from the absorption liquid absorbing liquid pump, washs, discharge in washing separating tank gaseous phase outlet, the nitrogen after washing can emptying also reusable edible; Absorption flow container is entered through washing separating tank after the sulfurous gas be entrained in nitrogen is absorbed by liquid absorption; Through absorbing, liquid pump pressurizes the absorption liquid of sulphur dioxide rich, heater heats flash distillation in sulfurous gas flash tank gets back to absorption flow container through water cooler after discharging sulfurous gas; The sulfur dioxide recovery that sulfurous gas flash tank discharges utilizes;
C. the alkene sulfolane solution after one section of desulfurization and alkali lye are mixed into two sections of desulfurization mixing tanks, control flux of alkaline liquor, and sulfurous gas (inferior sulfate radical) remaining in alkene sulfolane solution is neutralized;
D. the alkene sulfolane solution after two sections of desulfurization through filter consider insolubles after to converge with hydrogen, homogeneous catalyst and enter hydrogenation annular-pipe reactor, in hydrogenation annular-pipe reactor, carry out hydrogenation reaction, back pressure valve controls hydrogenation reaction pressure; Excess hydrogen is separated and recycle through tetramethylene sulfone separating tank by reaction product, and tetramethylene sulfone separating tank gained liquid phase obtains tetramethylene sulfone through separation and purification;
Described a kind of thick cyclobufene sultone produces the continuous production method of tetramethylene sulfone, and hydrogenation annular-pipe reactor, with or without chuck, is blank pipe or arrange dynamic and static hybrid element in pipe;
Described a kind of thick cyclobufene sultone produces the continuous production method of tetramethylene sulfone, and solvent dispersion device, one section of desulfurization mixing tank, nitrogen washings device, two sections of desulfurization mixing tanks are jet mixer, stirring tank or other mixing device;
Described a kind of thick cyclobufene sultone produces the continuous production method of tetramethylene sulfone, and hydrogenation annular-pipe reactor can use stirring tank, tower reactor to replace;
Described a kind of thick cyclobufene sultone produces the continuous production method of tetramethylene sulfone, and the impellent that material flows at each equipment room is provided by pump, compressor, potential difference or pressure difference;
Described a kind of thick cyclobufene sultone produces the continuous production method of tetramethylene sulfone, and solvent is the inert solvent such as water, methyl alcohol, is preferably water;
Described a kind of thick cyclobufene sultone produces the continuous production method of tetramethylene sulfone, and absorption liquid is tetramethylene sulfone, water, alkali lye etc., preferred tetramethylene sulfone;
Described a kind of thick cyclobufene sultone produces the continuous production method of tetramethylene sulfone, and homogeneous catalyst is liquid phase, has the catalyzer of catalytic hydrogenation, preferred Ziegler-Natta type homogeneous hydrogenation catalyzer.
advantage of the present invention is:
1. can make to realize continuous prodution by thick cyclobufene sultone desulfurization and hydrogenation synthesis tetramethylene sulfone, production efficiency is high, and turndown ratio is large, raw material availability is high, non-environmental-pollution.
2. adopt annular-pipe reactor hydrogenation, heat and mass is effective, and the residence time is controlled, and turndown ratio is large.
3. adopt two sections of desulfurization of two-stage desulfurization, Automated condtrol, make desulfurization more thorough, be conducive to extending the hydrogenation catalyst life-span and improving the quality of products.
4. adopt nitrogen circulation washing, sulfur dioxide recovery utilization, unconverted raw material is maximized and reclaims, raw material availability is high, non-environmental-pollution.
Accompanying drawing explanation
Fig. 1 is production equipment and the schematic flow sheet that thick cyclobufene sultone produces the continuous production method embodiment 1 of tetramethylene sulfone.
Embodiment
Embodiment 1
Production equipment comprises: solvent dispersion device 1, one section of desulfurization mixing tank 2, one section of desulfurization separator 3, desulfur pump 4, nitrogen washings device 5, washing separating tank 6, absorption flow container 7, absorption liquid pump 8, well heater 9, sulfurous gas flash tank 10, water cooler 11, two sections of desulfurization mixing tanks 12, strainer 13, hydrogenation annular-pipe reactor 14, back pressure valve 15, tetramethylene sulfone separating tank 16, equipment room connection line, control instruments and annexes; Solvent dispersion device 1 is continuous stirred tank, and one section of desulfurization mixing tank 2, nitrogen washings device 5, two sections of desulfurization mixing tanks 12 are injector; Hydrogenation annular-pipe reactor 15 is the turbulent element of band enhancement of heat transfer in chuck, installs the annular-pipe reactor of static mixing element in pipe; Working method comprises following 4 operations: 1) liquid thick cyclobufene sultone and solvent enter solvent dispersion device 1 in proportion and prepare alkene sulfolane solution; The alkene sulfolane solution that alkene sulfolane solution and desulfur pump 4 return and nitrogen converge and enter one section of desulfurization mixing tank 2 and fully mix, and make the sulfurous gas in alkene sulfolane solution transfer in nitrogen; The material going out one section of desulfurization mixing tank 2 carries out two-phase laminated flow in one section of desulfurization separator 3, and liquid phase enters two sections of desulfurization mixing tanks 12 through a part of extraction of desulfur pump 4 and continues desulfurization, and another part is circulated to one section of desulfurization mixing tank 2 entrance; In liquid phase (alkene sulfolane solution), the content of sulfurous gas is by-extraction ratio the control that circulates, and circulation-extraction is than larger, and content of sulfur dioxide is lower; Through one section of desulfurization, content of sulfur dioxide in alkene sulfolane solution is down to about 0.05%(massfraction); 2) nitrogen carrying sulfurous gas secretly is fully mixed through nitrogen washings device 5 by the gaseous phase outlet discharge of one section of desulfurization separator 3 with from the absorption liquid absorbing liquid pump 8, washs, discharge in washing separating tank 6 gaseous phase outlet, the nitrogen after washing can emptying also reusable edible; Enter through washing separating tank 6 after the sulfurous gas be entrained in nitrogen is absorbed by liquid absorption and absorb flow container 7; Through absorbing, liquid pump 8 pressurizes the absorption liquid of sulphur dioxide rich, well heater 9 calorifies after flash distillation in sulfurous gas flash tank 10 discharges sulfurous gas and gets back to absorption flow container 7 through water cooler 11; The sulfur dioxide recovery that sulfurous gas flash tank 10 discharges utilizes; 3) the alkene sulfolane solution after one section of desulfurization and alkali lye are mixed into two sections of desulfurization mixing tanks 12, control flux of alkaline liquor, and sulfurous gas (inferior sulfate radical) remaining in alkene sulfolane solution is neutralized; 4) the alkene sulfolane solution after two sections of desulfurization through filter 13 consider insolubles after to converge with hydrogen, homogeneous catalyst and enter hydrogenation annular-pipe reactor 14, in hydrogenation annular-pipe reactor 14, carry out hydrogenation reaction, back pressure valve 15 controls hydrogenation reaction pressure; Excess hydrogen is separated and recycle through tetramethylene sulfone separating tank 16 by reaction product, and tetramethylene sulfone separating tank 16 gained liquid phase can obtain tetramethylene sulfone through separation and purification; Embodiment 1 as shown in Figure 1.
Embodiment 2
Embodiment 2 is substantially the same manner as Example 1, and difference is that hydrogenation annular-pipe reactor 14 is for chuck band enhancement of heat transfer turbulent element, is the annular-pipe reactor of blank pipe in pipe;
Embodiment 3
Embodiment 3 is substantially the same manner as Example 1, the tube mixer that difference is one section of desulfurization mixing tank 2, nitrogen washings device 5, two sections of desulfurization mixing tanks 12 are built-in turbulent element.
Claims (8)
1. thick cyclobufene sultone produces a continuous production method for tetramethylene sulfone, it is characterized in that described technique comprises following production equipment and working method:
Production equipment comprises: solvent dispersion device (1), one section of desulfurization mixing tank (2), one section of desulfurization separator (3), desulfur pump (4), nitrogen washings device (5), washing separating tank (6), absorb flow container (7), absorb liquid pump (8), well heater (9), sulfurous gas flash tank (10), water cooler (11), two sections of desulfurization mixing tanks (12), strainer (13), hydrogenation annular-pipe reactor (14), back pressure valve (15), tetramethylene sulfone separating tank (16), equipment room connection line, control instruments and annex,
Working method comprises:
Liquid thick cyclobufene sultone and solvent enter solvent dispersion device (1) in proportion and prepare alkene sulfolane solution; The alkene sulfolane solution that alkene sulfolane solution and desulfur pump (4) return and nitrogen converge and enter one section of desulfurization mixing tank (2) and fully mix, and make the sulfurous gas in alkene sulfolane solution transfer in nitrogen; The material going out one section of desulfurization mixing tank (2) carries out two-phase laminated flow in one section of desulfurization separator (3), liquid phase enters two sections of desulfurization mixing tanks (12) through desulfur pump (4) a part of extraction and continues desulfurization, and another part is circulated to one section of desulfurization mixing tank (2) entrance; In liquid phase (alkene sulfolane solution), the content of sulfurous gas is by-extraction ratio the control that circulates, and circulation-extraction is than larger, and content of sulfur dioxide is lower; Through one section of desulfurization, content of sulfur dioxide in alkene sulfolane solution is down to about 0.05%(massfraction);
The nitrogen carrying sulfurous gas secretly is fully mixed, washs with from the absorption liquid absorbing liquid pump (8) through nitrogen washings device (5) by the gaseous phase outlet discharge of one section of desulfurization separator (3), discharge in washing separating tank (6) gaseous phase outlet, the nitrogen after washing can emptying also reusable edible; Enter through washing separating tank (6) after the sulfurous gas be entrained in nitrogen is absorbed by liquid absorption and absorb flow container (7); Through absorbing, liquid pump (8) pressurizes the absorption liquid of sulphur dioxide rich, well heater (9) calorifies after flash distillation discharges sulfurous gas in sulfurous gas flash tank (10) and gets back to absorption flow container (7) through water cooler (11); The sulfur dioxide recovery that sulfurous gas flash tank (10) discharges utilizes;
Alkene sulfolane solution after one section of desulfurization and alkali lye are mixed into two sections of desulfurization mixing tanks (12), control flux of alkaline liquor, and sulfurous gas (inferior sulfate radical) remaining in alkene sulfolane solution is neutralized;
Alkene sulfolane solution after two sections of desulfurization through filter (13) consider insolubles after to converge with hydrogen, homogeneous catalyst and enter hydrogenation annular-pipe reactor (14), in hydrogenation annular-pipe reactor (14), carry out hydrogenation reaction, back pressure valve (15) controls hydrogenation reaction pressure; Excess hydrogen is separated and recycle through tetramethylene sulfone separating tank (16) by reaction product, and tetramethylene sulfone separating tank (16) gained liquid phase obtains tetramethylene sulfone through separation and purification.
2. a kind of thick cyclobufene sultone according to claim 1 produces the continuous production method of tetramethylene sulfone, it is characterized in that hydrogenation annular-pipe reactor (14) is with or without chuck, is blank pipe or arrange dynamic and static hybrid element in pipe.
3. a kind of thick cyclobufene sultone according to claim 1 produces the continuous production method of tetramethylene sulfone, it is characterized in that solvent dispersion device (1), one section of desulfurization mixing tank (2), nitrogen washings device (5), two sections of desulfurization mixing tanks (12) be jet mixer, stirring tank or other mixing device.
4. a kind of thick cyclobufene sultone according to claim 1 produces the continuous production method of tetramethylene sulfone, it is characterized in that hydrogenation annular-pipe reactor (14) available stirring tank, tower reactor replace.
5. a kind of thick cyclobufene sultone according to claim 1 produces the continuous production method of tetramethylene sulfone, it is characterized in that the impellent that material flows at each equipment room is provided by pump, compressor, potential difference or pressure difference.
6. a kind of thick cyclobufene sultone according to claim 1 produces the continuous production method of tetramethylene sulfone, it is characterized in that solvent is the inert solvent such as water, methyl alcohol, is preferably water.
7. a kind of thick cyclobufene sultone according to claim 1 produces the continuous production method of tetramethylene sulfone, it is characterized in that absorption liquid is tetramethylene sulfone, water, alkali lye etc., preferred tetramethylene sulfone.
8. a kind of thick cyclobufene sultone according to claim 1 produces the continuous production method of tetramethylene sulfone, it is characterized in that homogeneous catalyst is liquid phase, has the catalyzer of catalytic hydrogenation, preferred Ziegler-Natta type homogeneous hydrogenation catalyzer.
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| CN201510113499.1A CN104788422B (en) | 2015-03-16 | 2015-03-16 | Continuous production method for preparing sulfolane from crude butadiene sulfone |
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| CN201510113499.1A CN104788422B (en) | 2015-03-16 | 2015-03-16 | Continuous production method for preparing sulfolane from crude butadiene sulfone |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109111424A (en) * | 2017-06-26 | 2019-01-01 | 中国石油天然气股份有限公司 | Method for recovering sulfolene crystallization wastewater |
| CN109232522A (en) * | 2018-09-30 | 2019-01-18 | 辽阳辽东精细化工有限公司 | Sulfolane continuous process system and technique |
| CN109761955A (en) * | 2017-11-09 | 2019-05-17 | 中国石油天然气股份有限公司 | Preparation method of sulfolene |
| CN109833637A (en) * | 2017-11-27 | 2019-06-04 | 中国石油天然气股份有限公司 | Recovery device |
| CN112239454A (en) * | 2019-07-17 | 2021-01-19 | 中国石油天然气股份有限公司 | System and method for producing sulfolane |
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| US3622598A (en) * | 1966-11-21 | 1971-11-23 | Phillips Petroleum Co | Production of sulfolane |
| US5030737A (en) * | 1990-02-12 | 1991-07-09 | Phillips Petroleum Company | Use of a solvent for hydrogenation of sulfolene to sulfolane |
| CN102020632A (en) * | 2009-09-16 | 2011-04-20 | 辽阳辽东精细化工有限公司 | Method and device for producing sulfolane |
| CN102407025A (en) * | 2010-09-20 | 2012-04-11 | 光华化工(营口)有限公司 | Method for recycling sulfur dioxide and butadiene |
-
2015
- 2015-03-16 CN CN201510113499.1A patent/CN104788422B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US3622598A (en) * | 1966-11-21 | 1971-11-23 | Phillips Petroleum Co | Production of sulfolane |
| US5030737A (en) * | 1990-02-12 | 1991-07-09 | Phillips Petroleum Company | Use of a solvent for hydrogenation of sulfolene to sulfolane |
| CN102020632A (en) * | 2009-09-16 | 2011-04-20 | 辽阳辽东精细化工有限公司 | Method and device for producing sulfolane |
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Non-Patent Citations (1)
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109111424A (en) * | 2017-06-26 | 2019-01-01 | 中国石油天然气股份有限公司 | Method for recovering sulfolene crystallization wastewater |
| CN109111424B (en) * | 2017-06-26 | 2020-10-09 | 中国石油天然气股份有限公司 | Method for recovering sulfolene crystallization wastewater |
| CN109761955A (en) * | 2017-11-09 | 2019-05-17 | 中国石油天然气股份有限公司 | Preparation method of sulfolene |
| CN109833637A (en) * | 2017-11-27 | 2019-06-04 | 中国石油天然气股份有限公司 | Recovery device |
| CN109232522A (en) * | 2018-09-30 | 2019-01-18 | 辽阳辽东精细化工有限公司 | Sulfolane continuous process system and technique |
| CN109232522B (en) * | 2018-09-30 | 2023-09-26 | 辽阳辽东精细化工有限公司 | Sulfolane continuous production system and process |
| CN112239454A (en) * | 2019-07-17 | 2021-01-19 | 中国石油天然气股份有限公司 | System and method for producing sulfolane |
| CN112239454B (en) * | 2019-07-17 | 2022-08-05 | 中国石油天然气股份有限公司 | System and method for producing sulfolane |
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