CN204661589U - A kind of thick cyclobufene sultone produces the continuous production device of tetramethylene sulfone - Google Patents

A kind of thick cyclobufene sultone produces the continuous production device of tetramethylene sulfone Download PDF

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CN204661589U
CN204661589U CN201520147381.6U CN201520147381U CN204661589U CN 204661589 U CN204661589 U CN 204661589U CN 201520147381 U CN201520147381 U CN 201520147381U CN 204661589 U CN204661589 U CN 204661589U
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desulfurization
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tetramethylene sulfone
thick
tank
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王修纲
吴剑华
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Shenyang University of Chemical Technology
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Shenyang University of Chemical Technology
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Abstract

The utility model discloses the continuous production device that a kind of thick cyclobufene sultone produces tetramethylene sulfone.This device is that thick cyclobufene sultone and solvent prepare alkene sulfolane solution, and alkene sulfolane solution mixes with nitrogen through one section of desulfurization mixing tank (2), one section of desulfurization separator (3), and in alkene sulfolane solution, sulfurous gas is entrained with by nitrogen, and content is down to about 0.05%; The sulfurous gas remained in after one section of desulfurization in alkene sulfolane solution is neutralized by alkali lye in two sections of desulfurization mixing tanks (12), 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) and carry out hydrogenation reaction; Reaction product isolates unreacting hydrogen can obtain crude product tetramethylene sulfone; Carry nitrogen discharger recycling respectively after washing, separation of sulfurous gas secretly; The thick cyclobufene sultone that the utility model proposes produces the continuous production device stable production process of tetramethylene sulfone, and greatly, raw material availability is high, good product quality for throughput and turndown ratio.

Description

A kind of thick cyclobufene sultone produces the continuous production device of tetramethylene sulfone
Technical field
The utility model relates to a kind of preparation facilities of solvent, and particularly a kind of thick cyclobufene sultone produces the continuous production device 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 purpose of this utility model be to provide a kind of with thick cyclobufene sultone be desulfurization of raw material, the continuous production device of hydrogenation synthesis cyclobufene sultone.The utility model 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.
the technical solution of the utility model is as follows:
Thick cyclobufene sultone produces a continuous production device for tetramethylene sulfone, and described device 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; Solvent dispersion device is connected with one section of desulfurization mixing tank with desulfur pump, one section of desulfurization mixing tank is connected with one section of sulphur separator, desulfur pump communicates with two sections of desulfurization mixing tanks, and communicate with section desulfurization mixer entrance, the gaseous phase outlet of one section of desulfurization separator with absorb the nitrogen washings device of liquid pump and wash separating tank and be connected, washing separating tank is communicated with absorption flow container, well heater and sulfurous gas flash tank, absorb flow container through water cooler and be connected, strainer is connected with hydrogenation annular-pipe reactor, between be provided with back pressure valve.
Described a kind of thick cyclobufene sultone produces the continuous production device of tetramethylene sulfone, and hydrogenation annular-pipe reactor is provided with chuck or does not establish chuck, is blank pipe or arrange dynamic and static hybrid element in pipe.
Described a kind of thick cyclobufene sultone produces the continuous production device 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.
Described a kind of thick cyclobufene sultone produces the continuous production device of tetramethylene sulfone, and hydrogenation annular-pipe reactor is stirring tank, tower reactor.
the utility model has the advantages that:
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 (4)

1. a thick cyclobufene sultone produces the continuous production device of tetramethylene sulfone, it is characterized in that described device 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, solvent dispersion device (1) is connected with one section of desulfurization mixing tank (2) with desulfur pump (4), one section of desulfurization mixing tank (2) one sections of sulphur separators (3) are connected, desulfur pump (4) communicates with two sections of desulfurization mixing tanks (12), and communicate with section desulfurization mixing tank (2) entrance, the gaseous phase outlet of one section of desulfurization separator (3) with absorb the nitrogen washings device (5) of liquid pump (8) and wash separating tank (6) and be connected, washing separating tank (6) is communicated with absorption flow container (7), well heater (9) and sulfurous gas flash tank (10), absorb flow container (7) through water cooler (11) to be connected, strainer (13) is connected with hydrogenation annular-pipe reactor (14), between be provided with back pressure valve (15).
2. a kind of thick cyclobufene sultone according to claim 1 produces the continuous production device of tetramethylene sulfone, it is characterized in that hydrogenation annular-pipe reactor (14) is provided with chuck or does not establish 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 device 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.
4. a kind of thick cyclobufene sultone according to claim 1 produces the continuous production device of tetramethylene sulfone, it is characterized in that hydrogenation annular-pipe reactor (14) is stirring tank, tower reactor.
CN201520147381.6U 2015-03-16 2015-03-16 A kind of thick cyclobufene sultone produces the continuous production device of tetramethylene sulfone Active CN204661589U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106366066A (en) * 2016-08-24 2017-02-01 沈阳工业大学 Method of recycling SO2 through compression/condensation during production process of sulfolane
CN109833637A (en) * 2017-11-27 2019-06-04 中国石油天然气股份有限公司 Recyclable device

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106366066A (en) * 2016-08-24 2017-02-01 沈阳工业大学 Method of recycling SO2 through compression/condensation during production process of sulfolane
CN106366066B (en) * 2016-08-24 2019-07-12 沈阳工业大学 A kind of compression/condensing recovery sulfur dioxide method in sulfolane production process
CN109833637A (en) * 2017-11-27 2019-06-04 中国石油天然气股份有限公司 Recyclable device

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