CN207227307U - A kind of device of continuous production hexylene glycol - Google Patents

A kind of device of continuous production hexylene glycol Download PDF

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Publication number
CN207227307U
CN207227307U CN201721093595.5U CN201721093595U CN207227307U CN 207227307 U CN207227307 U CN 207227307U CN 201721093595 U CN201721093595 U CN 201721093595U CN 207227307 U CN207227307 U CN 207227307U
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via pipeline
hexylene glycol
partition plate
dimethyl adipate
tower
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CN201721093595.5U
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邬慧雄
屈艳莉
赵秋松
吴莹莹
骆彩萍
张旭
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Hualu Engineering and Technology Co Ltd
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Hualu Engineering and Technology Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals

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Abstract

The utility model discloses a kind of device of continuous production hexylene glycol, particularly obtains dimethyl adipate via adipic acid and methanol esterification, then the continuous production device of hexylene glycol is produced via hydrogenation.A kind of device of continuous production hexylene glycol, it is characterised in that:Mainly include reactive distillation column, dimethyl adipate recovery tower, around heat exchange of heat pipe, feed heater, hydrogenation reactor, recycle gas compressor, three phase extraction separator, pressure reducing valve, methanol distillation column, pump and hexylene glycol product tower.Wherein, three phase extraction separator includes three-phase extractor, partition plate, condenser, return tank, reflux pump, part vaporizer.The utility model can realize the production technology of continuous feed reaction and the coupling of product transport disengaging height at the same time, it can effectively ensure that the conversion ratio of reaction raw materials adipic acid, and the selectivity to product hexylene glycol, significantly reduce energy consumption and the investment of device, it is and easy to operate, stable, good product quality, environmental protection and safety coefficient are high, with good economic efficiency.

Description

A kind of device of continuous production hexylene glycol
Technical field
A kind of device of continuous production hexylene glycol is the utility model is related to, is particularly obtained via adipic acid and methanol esterification Dimethyl adipate, then the continuous production device for producing hexylene glycol via being hydrogenated with.
Background technology
Hexylene glycol is a kind of important organic compound, is mainly used for improving the mechanical strength of product, improves product water resistant The performances such as solution, heat-resisting, chemical-resistant reagent, its purposes is very extensive, particularly coil coating, polyurethane, polyester, plasticizer, The fields such as the fields such as pesticide, medicine, dyestuff, photocuring, it is in an increasingly wide range of applications.Currently, with polyurethane, volume The development of material, paint industry, the global hexylene glycol market demand are increasing rapidly.
The production technology of hexylene glycol is mainly grasped by a few countries such as Germany, Japan.German BASF uses epoxy fourth Diene prepares hexylene glycol, but epoxy butadiene selling at exorbitant prices;Mitsubishi Chemical, Yu Buxingchan companies and the Asahi Kasei Corporation of Japan Using adipic acid without over-churning, direct hydrogenation prepares hexylene glycol, but never realizes industrialized production.
At present, commonly used is to use technology of the dimethyl adipate Hydrogenation for hexylene glycol, but its esterification is general All over using batch tank esterifier, a large amount of acid waste waters, seriously polluted, product separating energy consumption height are produced, and produce It is unstable, it is difficult to realize continuous operation.Meanwhile the raw material of the hydrogenation reaction dewatered dimethyl adipate of Seeking Truth again, this On the one hand separated energy consumption is big, on the other hand can not also utilize work(of the water to the timely extract and separate of hydrogenation reaction product hexylene glycol Can, cause hydrogenation reaction conversion ratio and selectivity can not all be improved.
Utility model content
For problems of the prior art, the purpose of this utility model is to provide a kind of continuous production hexylene glycol Device, can realize the production technology of continuous feed reaction and the separated height coupling of product at the same time, can effectively ensure that anti- The conversion ratio of raw material adipic acid and the selectivity to product hexylene glycol are answered, and the energy consumption of device and investment are low.Meanwhile operate letter Single, stable, good product quality is with good economic efficiency.
Technical solution is as follows used by the utility model:A kind of device of continuous production hexylene glycol, it is characterised in that:It is main To include reactive distillation column, dimethyl adipate recovery tower, around heat exchange of heat pipe, feed heater, hydrogenation reactor, circulation air pressure Contracting machine, three phase extraction separator, pressure reducing valve, methanol distillation column, hexylene glycol product tower and pump.Three phase extraction separator includes two Partition plate, condenser, return tank, reflux pump, part vaporizer.
According to a concrete scheme of the utility model, the top charging of the reactive distillation includes coming via pipeline connection The catalyst and adipic acid liquid for coming from No. two pumps are connected with via pipeline from outside battery limit (BL), lower part charging includes connecting via pipeline Fetch the methanol liquid for coming from reactive distillation tower top and No. four pumps from outside battery limit (BL), via pipeline connection.
According to a concrete scheme of the utility model, in the reactive distillation column, under the action of catalyst part oneself Diacid and part methanol react generation dimethyl adipate and water, wherein it is low-boiling without the methanol reacted from tower top Discharged via pipeline, it is high boiling without the adipic acid reacted, catalyst and reaction product dimethyl adipate, water from bottom of towe Discharge, and dimethyl adipate recovery tower is connected to via pipeline, in dimethyl adipate recovery tower, high boiling catalyst Discharged with solution of adipic acid from bottom of towe, low-boiling dimethyl adipate and water are discharged from tower top.
According to a concrete scheme of the utility model, the adipic acid diformazan that No. three pumps are come from via pipeline connection The mixing liquid of ester and water does not separate, and is directly connected to via pipeline around heat exchange of heat pipe, in heat exchange of heat pipe, by via pipeline After connection comes from the high-temp liquid heating of three phase extraction separator bottom water phase, then converge via pipeline connection and come from circulation The circulating hydrogen of air compressor, the fresh hydrogen for coming from battery limit (BL) and the dimethyl adipate liquid for coming from No. five pumps, mixing Material afterwards, feed heater is connected to via pipeline, after being heated to the temperature of hydrogenation reaction needs, then is connected to via pipeline Hydrogenation reactor.
According to a concrete scheme of the utility model, in the hydrogenation reactor, part dimethyl adipate and hydrogen Reaction generation hexylene glycol and methanol, connects via pipeline and the water for coming from hexylene glycol product column overhead is connected with via pipeline converges Afterwards, then via pipeline three phase extraction separator is connected to, in three phase extraction separator, charging initially enters bottom No.1 partition plate Leftward space, then partial gasification device is connected to from its bottom via pipeline, then connect via pipeline, into bottom one, two The intermediate space of partition plate, wherein vapour phase are discharged by the top of three phase extraction separator, and liquid phase is from the centre of one, No. two partition plate in bottom Space, is sequentially connected to condenser, return tank and reflux pump, the circulating hydrogen at the top of return tank is arranged via pipeline via pipeline Go out, bottom liquid then pressurizes via reflux pump and returns to the top of three phase extraction separator, while the centre of one, No. two partition plate in bottom The water of the bottom in space is mutually connected to around heat exchange of heat pipe via pipeline, then is connected to pressure reducing valve through pipeline, after decompression, is connected through pipeline Be connected to methanol distillation column, then No. two partition plates are crossed in overflow to the oil phase at the top of it, into the rightward space of No. two partition plates in bottom, then from its Bottom connects via pipeline and discharges, the wherein liquid level on the left of the No.1 partition plate of three phase extraction separator bottom, higher than one, No. two every Plate intermediate space, and the liquid level of one, No. two partition plate intermediate space is higher than No. two partition plate rightward spaces.
According to a concrete scheme of the utility model, the water phase for coming from three phase extraction separator bottom, via Pipeline is connected to methanol distillation column, and in methanol distillation column, low-boiling methanol is discharged from tower top via pipeline, it is high boiling oneself Two alcohol and waters are discharged from bottom of towe, and are connected to hexylene glycol product tower via pipeline, in hexylene glycol product tower, it is high boiling oneself Glycol connects discharge battery limit (BL) from bottom of towe via pipeline, and low-boiling water is discharged via pipeline from tower top, partly connected via pipeline In three phase extraction separator, partly discharge battery limit (BL) is connected via pipeline.
Brief description of the drawings
Fig. 1 is a kind of schematic diagram of the device of continuous production hexylene glycol.
1 is reactive distillation column, and 2,3,5,8,10,15 and 17 be respectively one to No. seven pump, and 4 recycle for dimethyl adipate Tower, 6 be that 7 be feed heater, and 9 be pressure reducing valve, and 11 be recycle gas compressor, and 12 be hydrogenation reactor, and 13 are around heat exchange of heat pipe Three phase extraction separator, 14 be methanol distillation column, and 16 be hexylene glycol product tower, and 30-55 and 71,72 are pipeline.
Fig. 2 is the schematic diagram of three phase extraction separator.
21 be part vaporizer, and 22 be reflux pump, and 23 be condenser, and 24 be return tank, and 25 be No.1 partition plate, and 26 be No. two Partition plate, 59-68 are pipeline.
Embodiment
With reference to the accompanying drawings, the utility model is further described.
Referring to attached Fig. 1 and 2, a kind of device of continuous production hexylene glycol, mainly includes reactive distillation column 1, adipic acid diformazan Ester recovery tower 4, around heat exchange of heat pipe 6, feed heater 7, hydrogenation reactor 12, recycle gas compressor 11, three phase extraction separator 13rd, pressure reducing valve 9, methanol distillation column 14, hexylene glycol product tower 16 and pump.Three phase extraction separator 13 includes two 25 Hes of partition plate 26th, condenser 23, return tank 24, reflux pump 22, part vaporizer 21.
Being connected via the catalyst of the connection of pipeline 30 and the mixed solution of adipic acid and via pipeline 33 outside battery limit (BL) The catalyst come from after 3 pressurization of the pump of 4 bottom of towe of dimethyl adipate recovery tower two and adipic acid liquid hybrid solution converge Afterwards, the top of reactive distillation column 1 is continuously entered;Outside battery limit (BL) via pipeline 31 connect methanol liquid, via pipeline 32 Connection come from 1 tower top of reactive distillation column methanol liquid and via pipeline 34 connection come from and 14 tower top of methanol distillation column Via the methanol liquids of No. 4 pump pressurizations of pipeline connection, jointly via pipeline 31, the lower part of reactive distillation column 1 is continuously entered, Two bursts charging between, under the action of catalyst part adipic acid and part methanol react generation dimethyl adipate and Water.
It is low-boiling without the methanol reacted in reactive distillation column 1, discharged from tower top via pipeline 32, higher boiling Then discharged without the adipic acid, catalyst and reaction product dimethyl adipate, water reacted from bottom of towe, and via pipeline 2 No.1 pump 2 is connected to, after pressurization, dimethyl adipate recovery tower 4 is connected to via pipeline 2, in dimethyl adipate recovery tower 4 Interior, high boiling catalyst and solution of adipic acid are discharged via pipeline 35 from bottom of towe, low-boiling dimethyl adipate and water from Tower top, is discharged via pipeline 37.
The mixing liquid of the dimethyl ester and water that come from 4 tower top of dimethyl adipate recovery tower does not separate, directly via pipe Road connects No. three pumps 5, after pressurization, is connected to via pipeline 38 around heat exchange of heat pipe 6, in heat exchange of heat pipe 6, by via pipeline 39 After connection comes from the high temperature aqueous phase liquid heating of 13 bottom of three phase extraction separator, then converge via the connection of pipeline 40 and come from Circulating hydrogen in the recycle gas compressor 11 connected via pipeline 43, the fresh hydrogen for coming from the battery limit (BL) connected via pipeline 71 Gas and the dimethyl adipate liquid for coming from No. five pumps 10 in 13 bottom of three phase extraction separator connected via pipeline 42, mixing Material afterwards, feed heater 7 is connected to via pipeline 40, after being heated to the temperature of hydrogenation reaction needs, then via pipeline 41 It is connected to hydrogenation reactor 12.In hydrogenation reactor 12, part dimethyl adipate and hydrogen partial reaction generation hexylene glycol And methanol, connected via pipeline connection 46 and via pipeline 54 come from 16 tower top of hexylene glycol product tower water converge after, then pass through Three phase extraction separation 13 is connected to by pipeline 72.
In three phase extraction separator 13, charging enters the leftward space of bottom No.1 partition plate 25 via pipeline 72 first, Partial gasification device 21 is connected to from its bottom via pipeline 66 again, in partial gasification device 21, is connected via pipeline 67 and 68 Steam heating and partization after, connected via pipeline 65, the intermediate space between the partition plate 25 and 26 of bottom one, two, Its vapour phase is discharged from the top of three phase extraction separator 13, is connected to condenser 59 via pipeline 62, in condenser 59, is passed through After the circulating cooling water cooling connected by pipeline 60 and 61, connected via pipeline 59, into return tank 24, the recycle hydrogen at the top of it Gas is connected to recycle gas compressor 11 via pipeline 47, its bottom liquid, and reflux pump 22 is connected to via pipeline 63, after pressurization, The top of three phase extraction separator 13 is connected to via pipeline 64 again.And the partition plate of the bottom of three phase extraction separator 13 one, two The top of intermediate space between 25 and 26, then No. two partition plates 26 are crossed in overflow to oil phase liquid, into the right side of No. 2 partition plates 26 in bottom Space, then connect and discharge via pipeline 48 from its bottom.
Meanwhile the bottom of the intermediate space between the partition plate 25 and 26 of the bottom of three phase extraction separator 13 one, two, water Phase liquid, then be connected to around heat exchange of heat pipe 6 via pipeline 39, and in heat exchange of heat pipe 6, its heat is absorbed, and temperature reduces, then Pressure reducing valve 9 is connected to via pipeline 44, after pressure reduces, methanol distillation column 14 is connected to via pipeline 45, in methanol distillation column In 14, low-boiling methanol is connected to No. four pumps 8 from tower top via pipeline 49, and high boiling hexylene glycol and water are discharged from bottom of towe, And be connected to No. six pumps 15 via pipeline 50, after being pressurized, then via pipeline 51 be connected to hexylene glycol product tower 16, oneself two In alcohol product tower 16, high boiling hexylene glycol from bottom of towe via pipeline 52 connect discharge battery limit (BL), low-boiling water from tower top via Pipeline 53 is discharged, and after being partly connected to No. seven pressurizations of pump 17 via pipeline 54, then is connected to three phase extraction via pipeline 55 and is separated Device 13, partly connects discharge battery limit (BL) via pipeline 53.
In addition, the liquid level of 25 leftward space of No.1 partition plate of 13 bottom of three phase extraction separator, one, No. two higher than bottom Intermediate space between partition plate 25 and 26, and the space on higher than No. two right sides of partition plate 26 of the liquid level of intermediate space.

Claims (4)

  1. A kind of 1. device of continuous production hexylene glycol, it is characterised in that:Recycled including reactive distillation column (1), dimethyl adipate Tower (4), around heat exchange of heat pipe (6), feed heater (7), hydrogenation reactor (12), recycle gas compressor (11), three phase extraction point From device (13), methanol distillation column (14), hexylene glycol product tower (16) and various pumps, wherein three phase extraction separator (13) includes one Number partition plate (25), No. two partition plates (26), condenser (23), return tank (24), reflux pump (22), part vaporizer (21).
  2. 2. the device of continuous production hexylene glycol according to claim 1, it is characterised in that:The reactive distillation column (1) Top charging include connect with via pipeline outside the battery limit (BL) via pipeline connection the catalyst for coming from No. two pumps (3) with oneself two Acid solution body, lower part charging include coming from reactive distillation tower top and four outside battery limit (BL), via pipeline connection via pipeline connection Number pump Liquid Phase Methanol.
  3. 3. the device of continuous production hexylene glycol according to claim 1, it is characterised in that:In the reactive distillation column (1), Adipic acid and methanol, which react, under the action of catalyst generates dimethyl adipate and water, and low-boiling methanol is passed through from tower top To be discharged by pipeline, high boiling adipic acid, catalyst and reaction product dimethyl adipate, water are discharged from bottom of towe, and via pipe Road is connected to dimethyl adipate recovery tower (4), in the dimethyl adipate recovery tower (4), high boiling catalyst and oneself two Acid solution body is discharged from bottom of towe, and low-boiling dimethyl adipate and water are discharged from tower top.
  4. 4. the device of continuous production hexylene glycol according to claim 1, it is characterised in that:The three phase extraction separator (13) in, charging initially enters the leftward space of bottom No.1 partition plate (25), then is connected to partial gasification device (21) via pipeline, Connected again via pipeline, into bottom No.1 partition plate (25), the intermediate space of No. two partition plates (26), wherein vapour phase is from three phase extraction Discharge, condenser (23), return tank (24) and reflux pump (22), return tank are sequentially connected to via pipeline at the top of separator (13) (24) circulating hydrogen at the top of is discharged via pipeline, and bottom liquid pressurizes via reflux pump (22) and returns to three phase extraction separator (13) top, while the water of the bottom of bottom No.1 partition plate (25), No. two partition plate (26) intermediate spaces is mutually connected via pipeline Discharge, No. two partition plates (26) are crossed in the oil phase overflow at the top of it, into the rightward space of No. two partition plates (26) in bottom, then from its bottom Connecting and discharge via pipeline, the wherein liquid level on the left of No.1 partition plate (25) is higher than the space among one, No. two partition plate, and one, two The liquid level in the space among number partition plate is higher than No. two partition plate (26) rightward spaces again.
CN201721093595.5U 2017-08-29 2017-08-29 A kind of device of continuous production hexylene glycol Active CN207227307U (en)

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CN201721093595.5U CN207227307U (en) 2017-08-29 2017-08-29 A kind of device of continuous production hexylene glycol

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Application Number Priority Date Filing Date Title
CN201721093595.5U CN207227307U (en) 2017-08-29 2017-08-29 A kind of device of continuous production hexylene glycol

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CN207227307U true CN207227307U (en) 2018-04-13

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