CN206337191U - A kind of continuous device for extracting medical grade propylene glycol - Google Patents

A kind of continuous device for extracting medical grade propylene glycol Download PDF

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Publication number
CN206337191U
CN206337191U CN201621391142.6U CN201621391142U CN206337191U CN 206337191 U CN206337191 U CN 206337191U CN 201621391142 U CN201621391142 U CN 201621391142U CN 206337191 U CN206337191 U CN 206337191U
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tower
pump
stripper
rectifying column
rectifying
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CN201621391142.6U
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刘力源
梁明国
韩玉志
张海龙
王伟
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Yangquan Coal Group Qingdao Hengyuan Chemical Co Ltd
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Yangquan Coal Group Qingdao Hengyuan Chemical Co Ltd
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Abstract

The utility model discloses a kind of continuous device for extracting medical grade propylene glycol, primary rectifying column tower top is connected with the first reflux pump, first reflux pump is connected with primary rectifying column tower top and methanol rectifying tower respectively by pipeline, primary tower bottom of rectifying tower bottom is connected with the first tower reactor pump charging aperture, first tower reactor pumps out material mouth and connected with stripper top, provided with steam feed mouthful in the middle part of stripper, stripper bottom is by the second tower reactor pump with being connected in the middle part of refined rectifying column, stripper top is connected with the second reflux pump, second reflux pump is connected with stripper top and water treatment facilities respectively by pipeline, refined tower bottom of rectifying tower is connected with the 3rd tower reactor pump, refined rectifying column tower top is connected with the 3rd reflux pump, 3rd reflux pump at the top of refined rectifying column with stripper top respectively by pipeline with connecting, discharging opening is set in the middle part of refined rectifying column.Technique is simple, can not only utilize the exhaust steam of on-site, be effectively reduced energy consumption, propane diols purity reaches 99.99%, and the rate of recovery is more than 95%.

Description

A kind of continuous device for extracting medical grade propylene glycol
Technical field:
The utility model belongs to compound purification technique field, is related to a kind of continuous dress for extracting medical grade propylene glycol Put, and in particular to a kind of using primary rectifying, air lift and the part of refined rectifying three obtains high-purity, the propane diols of high-recovery is carried Pure device.
Background technology:
In dimethyl carbonate and propane diols joint process, the first step is first synthesized using expoxy propane and carbon dioxide effect Propene carbonate, second step carbonate synthesis again in the presence of methylate salt catalyst by raw material of propene carbonate and methanol Dimethyl ester and propane diols, then obtain product by last handling process, and last handling process is specially:Pass through extractive distillation column first Prepared calcium carbonate dimethyl ester, then reclaims methanol by methanol rectifying tower, then removes methylate salt by the desalination that is carbonized, filtering, Finally give propane diols crude product.The propylene glycol product that above-mentioned aftertreatment technology is obtained exist easily discoloration, penetrating odor it is big, The problems such as inferior quality, it is impossible to reach the requirement of medical grade propylene glycol, it is impossible to be applied to medicine, food, essence, spices, cosmetic In the high added value industry such as product.The impurity in propylene glycol product is typically now further removed using 3-4 rectifying column, but should Purifying technique tedious process, high cost, the propane diols rate of recovery can only achieve 20-30%.Chinese invention patent CN2016103426310 discloses a kind of processing method of the medical grade propylene glycol of ester-interchange method generation dimethyl carbonate by-product, first Methanol is first isolated using method separation tower, then material enters in thin film evaporator, be -85~95Kpa, steam temperature in pressure Under conditions of 105~108 DEG C of degree, thin film evaporator top material travels further into propylene glycol product tower rectifying, and to obtain pharmaceutical grade pure Contain catalyst feed and be delivered to hydrolysis carbonization kettle processing in the propylene glycol product of degree, thin film evaporator bottom.
The content of the invention:
The purpose of this utility model is to overcome the shortcoming of prior art there is provided a kind of side of continuous raw medical grade propylene glycol Method, it is cumbersome to solve existing propane diols purifying technique, high cost, the problem of propane diols rate of recovery is low.
To achieve these goals, the method for the medical grade propylene glycol of continuous extraction that the utility model is related to, is specifically included Three below step:
(1) the just rectifying of grade propylene glycol:The propane diols crude product that the desalination that is carbonized is obtained enters primary rectifying column, primary essence It is -80~-90Kpa to evaporate tower in negative pressure, and tower top temperature is 90~100 DEG C, and bottom temperature is smart under conditions of controlling 145~155 DEG C The light component water evaporated in processing, propane diols crude product is flowed out with methanol by primary rectifying column tower top, travels further into methanol rectifying tower Reclaimed;
(2) the first stripping of grade propylene glycol:By primary tower bottom of rectifying tower heavy constituent from stripper overhead is added to stripper, 100~130 DEG C of steam are entered by stripper bottom, and it is -85~-90Kpa, stripper overhead outflow to control stripper internal pressure Thing is focused on into sewage-treatment plant;
(3) medical grade propylene glycol is refined:Stripper tower reactor heavy constituent enters refined rectifying column by middle part, refines rectifying column Negative pressure is -80~-90Kpa, and tower top temperature is 120~130 DEG C, and bottom temperature is rectification process under conditions of 135~140 DEG C, It is 99.99% pharmaceutical grade propylene glycol product to finally give from the purity of the middle part discharging of refined treating column, refines treating column tower reactor In kettle raffinate it is periodically outer arrange, the light component propane diols and moisture in refined column overhead are from top return to step (2) Stripper circular treatment.
The primary rectifying tower internals that the utility model is related to use structured packing or high-efficient tower plate, or structured packing and height It is dimethyl carbonate and propane diols coproduction last handling process to imitate the methanol rectifying tower in tower tray mixing column inner parts structure, step (1) Middle methanol rectifying tower;Steam in step (2) adds thermogenetic steam for deionized water.
The method of the medical grade propylene glycol of continuous production that the utility model is related to uses propylene glycol continuous production device, and the third two Alcohol continuous production device specifically includes primary rectifying column, stripper, refined rectifying column, the first reflux pump, the first tower reactor pump, second Reflux pump, the second tower reactor pump, the 3rd reflux pump, product storage tank, product send pump and the 3rd tower reactor pump outside, primary rectifying column tower top with First reflux pump is connected, and the first reflux pump is connected with primary rectifying column tower top and methanol rectifying tower respectively by pipeline, primary essence Evaporate tower tower reactor bottom to connect with the first tower reactor pump charging aperture, the first tower reactor pumps out material mouth and connected with stripper top, in stripper Portion is connected provided with steam feed mouthful, stripper bottom by the second tower reactor pump and refined rectifying column middle part, stripper top and the Two reflux pumps are connected, and the second reflux pump is connected with stripper top and water treatment facilities respectively by pipeline, refine rectifying tower Kettle is connected with the 3rd tower reactor pump, and refined rectifying column tower top is connected with the 3rd reflux pump, and the 3rd reflux pump passes through pipeline and essence respectively Connected at the top of rectifying column processed with stripper top, refine and discharging opening is set in the middle part of rectifying column, discharging opening is stored up by pipeline and product Tank is connected, and product storage tank is sent pump outside with product and connected.
The method for the continuous raw medical grade propylene glycol that the utility model is related to, compared with prior art, has the advantage that: (1) technique is simple;(2) traditional distillation process is replaced using stripping, can not only utilizes the exhaust steam of on-site, stripping is replaced Rectifying can be effectively reduced energy consumption, and effectively remove the impurity in propane diols;(3) propane diols purity reaches 99.99%, returns Yield is more than 95%;(4) production process of serialization, improves the yield of propane diols, is easy to industrial application.
Brief description of the drawings:
The continuous production pharmacopeia grade propylene glycol structure drawing of device that Fig. 1 is related to for the utility model.
Embodiment:
Below in conjunction with the accompanying drawings and the utility model is described in further detail by specific embodiment.
Embodiment 1:
To achieve these goals, the method for the medical grade propylene glycol of the present embodiment is related to continuous extraction, specifically include with Lower three steps:
(1) the just rectifying of grade propylene glycol:The propane diols crude product that the desalination that is carbonized is obtained enters primary rectifying column 1, primary Rectifying column 1 is -80~-90Kpa in negative pressure, and tower top temperature is 90~100 DEG C, and bottom temperature is controlled under conditions of 145~155 DEG C Light component water in rectification process, propane diols crude product is flowed out with methanol by the primary tower top of rectifying column 1, travels further into methanol rectification Tower is reclaimed;
(2) the first stripping of grade propylene glycol:The primary tower reactor heavy constituent of rectifying column 1 is added to stripper 2 from the tower top of stripper 2 In, 100~130 DEG C of steam are entered by the bottom of stripper 2, controls the internal pressure of stripper 2 for -85~-90Kpa, and then by third Allyl alcohol, propylene glycol monomethyl ether, 2- methoxy-1-propanols, pyruvic alcohol in glycol crude product, methyl n-heptyl ketone, dipropylene glycol list first The impurity such as ether and 2,3-butanediol is discharged from the tower top of stripper 2, and the tower top effluent of stripper 2 is collected into sewage-treatment plant Middle processing, arranges or goes to sewage treatment plant outside after processing is qualified and be uniformly processed;
(3) medical grade propylene glycol is refined:The tower reactor heavy constituent of stripper 2 enters refined rectifying column 3 by middle part, refines rectifying The negative pressure of tower 3 is -80~-90Kpa, and tower top temperature is 120~130 DEG C, and bottom temperature is under conditions of 135~140 DEG C at rectifying Reason, it is 99.99% pharmaceutical grade propylene glycol product to finally give from the purity of the middle part discharging of refined treating column 3, refines treating column 3 Kettle raffinate in tower reactor is periodically outer to be arranged, and refines light component propane diols and moisture in the tower top for the treatment of column 3 from top return to step (2) In the circular treatment of stripper 2, and in whole process propane diols the rate of recovery more than 95%.
The primary rectifying tower internals that the present embodiment is related to use structured packing or high-efficient tower plate, or structured packing with efficiently Methanol rectifying tower in tower tray mixing column inner parts structure, step (1) is in dimethyl carbonate and propane diols coproduction last handling process Methanol rectifying tower;Steam in step (2) adds thermogenetic steam for deionized water.
The method for the medical grade propylene glycol of continuous production that the present embodiment is related to uses propylene glycol continuous production device, propane diols Continuous production device specifically include primary rectifying column 1, stripper 2, refined rectifying column 3, the first reflux pump 4, the first tower reactor pump 5, Second reflux pump 6, the second tower reactor pump 7, the 3rd reflux pump 8, product storage tank 9, product send the tower reactor pump 11 of pump 10 and the 3rd outside, primary The tower top of rectifying column 1 is connected with the first reflux pump 4, and the first reflux pump 4 is smart with the primary tower top of rectifying column 1 and methanol respectively by pipeline Tower connection is evaporated, realizes that another part material is transported to methanol rectification by the backflow of a part of material of the primary tower top of rectifying column 1 simultaneously In tower, the primary tower reactor bottom of rectifying column 1 is connected with the charging aperture of the first tower reactor pump 5, and the discharging opening of the first tower reactor pump 5 is pushed up with stripper 2 Portion is connected, and the middle part of stripper 2 enters stripper 2, stripper provided with steam feed mouthful, 100~130 DEG C of steam from steam feed mouthful 2 bottoms are connected by the second tower reactor pump 7 with the refined middle part of rectifying column 3, and the top of stripper 2 is connected with the second reflux pump 6, second time Stream pump 6 is connected with the top of stripper 2 and water treatment facilities respectively by pipeline, realizes that a part of top light component of stripper 2 is returned The top light component of another part stripper 2 is transported to water treatment facilities to stream simultaneously, refines the tower reactor of rectifying column 3 and the 3rd tower reactor pump 11 The regular outer row of the refined tower reactor heavy constituent of rectifying column 3 is realized in connection, and the refined tower top of rectifying column 3 is connected with the 3rd reflux pump 8, the 3rd Reflux pump 8 is connected by pipeline with the refined top of rectifying column 3 and the top of stripper 2 respectively, by tower top one in refined rectifying column 3 Another part component is simultaneously pipelined to the top of stripper 2 by point component backflow, is refined the middle part of rectifying column 3 and is set discharging Mouthful, discharging opening is connected by pipeline with product storage tank 9, and product storage tank 9 sends pump 10 outside with product and connects that the propane diols refined is defeated It is sent to outside.

Claims (1)

1. a kind of continuous device for extracting medical grade propylene glycol, it is characterised in that propylene glycol continuous production device is specifically included just Level rectifying column, stripper, refined rectifying column, the first reflux pump, the first tower reactor pump, the second reflux pump, the second tower reactor pump, the 3rd time Stream pump, product storage tank, product send pump and the 3rd tower reactor pump outside, and primary rectifying column tower top is connected with the first reflux pump, the first backflow Pump is connected with primary rectifying column tower top and methanol rectifying tower respectively by pipeline, primary tower bottom of rectifying tower bottom and the first tower reactor pump Charging aperture is connected, and the first tower reactor pumps out material mouth and connected with stripper top, provided with steam feed mouthful, stripping tower bottom in the middle part of stripper Portion in the middle part of refined rectifying column by the second tower reactor pump with being connected, and stripper top is connected with the second reflux pump, and the second reflux pump leads to Piping is connected with stripper top and water treatment facilities respectively, and refined tower bottom of rectifying tower is connected with the 3rd tower reactor pump, refines essence Evaporate column overhead to connect with the 3rd reflux pump, the 3rd reflux pump at the top of pipeline and refined rectifying column with stripper top respectively by connecting It is logical, refine and discharging opening is set in the middle part of rectifying column, discharging opening is connected by pipeline with product storage tank, product storage tank sends pump outside with product Connection.
CN201621391142.6U 2016-12-16 2016-12-16 A kind of continuous device for extracting medical grade propylene glycol Active CN206337191U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115636730A (en) * 2021-07-20 2023-01-24 中国石油天然气股份有限公司 Method for purifying and decoloring 1, 3-propylene glycol crude product

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115636730A (en) * 2021-07-20 2023-01-24 中国石油天然气股份有限公司 Method for purifying and decoloring 1, 3-propylene glycol crude product

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