CN104045590B - The thick methyl mercapto of methanthiol and acrylic aldehyde synthesis is for the process system of propionic aldehyde - Google Patents
The thick methyl mercapto of methanthiol and acrylic aldehyde synthesis is for the process system of propionic aldehyde Download PDFInfo
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- CN104045590B CN104045590B CN201410245911.0A CN201410245911A CN104045590B CN 104045590 B CN104045590 B CN 104045590B CN 201410245911 A CN201410245911 A CN 201410245911A CN 104045590 B CN104045590 B CN 104045590B
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Abstract
The thick methyl mercapto of methanthiol and acrolein reaction synthesis processes system for propionic aldehyde, including: coarse vacuum rectifying column, receive thick methyl mercapto for propionic aldehyde, from discharging heavier component at the bottom of tower and discharging light components from tower top；High vacuum rectification tower, receives the heavier component discharged at the bottom of the tower of coarse vacuum rectifying column, discharges product methyl mercapto for propionic aldehyde from tower top, and from discharging heavy component at the bottom of tower；Emulsion tank, receives the light components discharged from the tower top of coarse vacuum rectifying column and from the heavy component of discharge at the bottom of the tower of high vacuum rectification tower；And incinerator, from the emulsion tank described emulsion of reception and burn described emulsion by pipeline.Utilize the process system of the present invention to locate the thick methyl mercapto of reason methanthiol and acrolein reaction synthesis for propionic aldehyde, by being the mode of emulsion by light heavy component emulsifying, solve the difficult problem carrying light heavy component can block pipeline respectively, stop environmental protection event to produce, improve workshop and local resident's environment.
Description
To be " 201210131610.6 ", the applying date be April 28, denomination of invention in 2012 that the application is application number is the divisional application of the application for a patent for invention of " the thick methyl mercapto of methanthiol and acrylic aldehyde synthesis is for the processing method of propionic aldehyde and system ".
Technical field
The present invention relates to the thick methyl mercapto synthesized by methanthiol and acrolein reaction for the process of propionic aldehyde, be specifically related to thick methyl mercapto for the process system of by-product in propionic aldehyde.
Background technology
Methyl mercapto is the important intermediate preparing methionine for propionic aldehyde, occurs Michael addition reaction to prepare mainly by methanthiol and acrylic aldehyde under the catalysis of organic base.Utilizing the method can under comparatively gentle condition, as just prepared methyl mercapto under the normal pressure that temperature is 30-40 DEG C for propionic aldehyde, and yield be all higher than 90%.But acrolein polymer, methyl mercapto can be produced in this course of reaction for propionic aldehyde polymer, including the multiple by-product such as dimer, trimer, there is also simultaneously and do not participate in the methyl sulfide of reaction, hydrogen sulfide, water, methanol, acetic acid and unreacted methanthiol completely and acrylic aldehyde on a small quantity.Some of them Organic substance boiling point than methyl mercapto for the low light components of propionic aldehyde, such as methyl sulfide, hydrogen sulfide, methanthiol, acetic acid etc.；Other Organic substance boiling points than methyl mercapto for the high heavy component of propionic aldehyde, if acrolein polymer, methyl mercapto are for propionic aldehyde polymer, including dimer, trimer etc..Owing to methyl mercapto is higher for the boiling point of propionic aldehyde, it is generally adopted rectification under vacuum.For preventing from having aldehyde radical, the Organic substance of ethylene linkage is polymerized, the efficiency of reduction rectifying column and methyl mercapto are for propionic aldehyde product yield, it is generally adopted elder generation in coarse vacuum condition by relatively low for boiling point by-product, such as foul gass such as hydrogen sulfide, methyl sulfide, methanthiol, acrylic aldehyde from coarse vacuum rectifying column tower top through vacuum pump venting light components surge tank, then send to burning disposal.It is that major part methyl mercapto is for the higher by-product of propionic aldehyde and a small amount of boiling point at the bottom of tower, if acrolein polymer, methyl mercapto are for propionic aldehyde polymer, including dimer, trimer etc., send into high vacuum rectification tower, overhead extraction methyl mercapto is for propionic aldehyde product, at the bottom of tower, high boiling point by-products produced being pumped up, into heavy component surge tank, is re-fed into burning disposal.No matter being light components or heavy component, be mostly the Organic substance of sulfur-bearing, these Organic substances have the characteristic of essence, and adhesion is extremely strong, the concentration at air be 0.08ppb will make people feel sick feel bad.Therefore, at refining methyl mercapto in the process of propionic aldehyde, by-product must strictly control, it is impossible to is leaked in air, otherwise can cause environmental issue having a strong impact on the living environment of resident.
In actual commercial production, it is usually and light components and heavy component are sent to burning disposal respectively.But, due to heavy component very thickness, as Colophonium, go the pump both not had suitable good airproof performance in the process burned to carry this dope in conveying, also very easily block pipeline simultaneously；And once blocking pipeline, workshop continuous and stable production not only can be affected；And in the process of maintenance blocking pipeline, this heavy component can be leaked in environment, causes serious environmental pollution.
Summary of the invention
It is an object of the invention to solve above-mentioned Problems existing, it is provided that a kind of thick methyl mercapto synthesized by methanthiol and acrolein reaction, for the processing method of propionic aldehyde, carries out burning disposal again by after light heavy component mixing and emulsifying.
According to the first aspect of the invention, it is provided that the thick methyl mercapto of a kind of place reason methanthiol and acrolein reaction synthesis for the method for propionic aldehyde, including:
Thick methyl mercapto is sent into coarse vacuum rectifying column for propionic aldehyde, discharges light components from tower top and send into emulsion tank, from discharging the heavier component containing methyl mercapto for propionic aldehyde at the bottom of tower；
Contain methyl mercapto heavier component send what discharge at the bottom of the tower from coarse vacuum rectifying column into the high vacuum rectification tower for propionic aldehyde, discharge and collect product methyl mercapto from tower top for propionic aldehyde, from discharging heavy component at the bottom of tower and sending into described emulsion tank equally；
At described emulsion tank internal emulsification light components and heavy component to form uniform and stable emulsion；
Described emulsion is sent into incinerator by pipeline.
Preferably, the method for the present invention also includes: combustion-supporting gas and combustion gas are sent in incinerator to help to burn described emulsion.
Preferably, wherein said emulsion tank is provided externally with jacket heat-preservation layer, and inside is provided with agitator and controls the variator of agitator.
Preferably, wherein agitator speed is not less than 150RMP；Emulsifying temperature is not less than 60 DEG C；Emulsification times is not less than 5min.It is highly preferred that wherein agitator speed is 200RMP；Emulsifying temperature is 80 DEG C；Emulsification times is 10min.
Preferably, wherein emulsion particle diameter is 100nm.
Preferably, wherein emulsion viscosity is basically identical for propionic aldehyde viscosity with product methyl mercapto.Preferably, wherein by canned motor pump, described emulsion is sent into incinerator by pipeline.
Preferably, wherein the vacuum of coarse vacuum rectifying column is 8-20 kPa；The vacuum of high vacuum rectification tower is 1-5 kPa.
Thick methyl mercapto generally includes methyl mercapto for propionic aldehyde, hydrogen sulfide, methyl sulfide, acrylic aldehyde, acetic acid, methanol, water, hydroquinone, morpholine, acrolein polymer and methyl mercapto for propionic aldehyde polymer for propionic aldehyde.Light components generally comprises hydrogen sulfide, methyl sulfide, acrylic aldehyde, acetic acid, methanol, morpholine and water.Heavier component generally comprises methyl mercapto for propionic aldehyde, hydroquinone, acrolein polymer and methyl mercapto for propionic aldehyde polymer.Heavy component generally comprises hydroquinone, a large amount of methyl mercapto for propionic aldehyde polymer, a small amount of acrolein polymer and a small amount of methyl mercapto for propionic aldehyde.
According to the second aspect of the invention, it is provided that a kind of thick methyl mercapto synthesized by methanthiol and acrolein reaction processes system for propionic aldehyde, including:
Coarse vacuum rectifying column, receives the thick methyl mercapto that synthesized by methanthiol and acrolein reaction for propionic aldehyde, from discharging at the bottom of tower containing the methyl mercapto heavier component for propionic aldehyde and discharging light components from tower top；
High vacuum rectification tower, what receive discharge at the bottom of the tower of coarse vacuum rectifying column contains the methyl mercapto heavier component for propionic aldehyde, discharges product methyl mercapto for propionic aldehyde from tower top, and from discharging heavy component at the bottom of tower；
Emulsion tank, receives the light components discharged from the tower top of coarse vacuum rectifying column and from the heavy component of discharge at the bottom of the tower of high vacuum rectification tower, and light components and heavy component form uniform and stable emulsion at emulsion tank internal emulsification；And
Incinerator, from the emulsion tank described emulsion of reception and burns described emulsion by pipeline.
At the thick methyl mercapto of the present invention in propionic aldehyde process system, it is preferable that emulsion tank is provided externally with jacket heat-preservation layer, inside is provided with agitator and controls the variator of agitator.
The thick methyl mercapto of the present invention processes system for propionic aldehyde can also include canned motor pump, for described emulsion is sent into incinerator by pipeline from emulsion tank.
The thick methyl mercapto of place's reason methanthiol of the present invention and acrolein reaction synthesis is for the method for propionic aldehyde, by being the mode of emulsion by light heavy component emulsifying, solve the difficult problem carrying light heavy component can block pipeline respectively, stop environmental protection event to produce, improve workshop and local resident's environment.
Accompanying drawing explanation
Fig. 1 is the thick methyl mercapto exemplary process flow figure for propionic aldehyde of place's reason methanthiol of the present invention and acrolein reaction synthesis.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, present disclosure is described in detail.
Referring to the thick methyl mercapto of place's reason methanthiol of Fig. 1 and acrolein reaction synthesis for the exemplary process flow figure of propionic aldehyde.Thick methyl mercapto, for propionic aldehyde 11, mainly includes methyl mercapto for propionic aldehyde, hydrogen sulfide, methyl sulfide, acrylic aldehyde, acetic acid, methanol, water, hydroquinone, morpholine, acrolein polymer and methyl mercapto for propionic aldehyde polymer etc..Thick methyl mercapto is continuously introduced into coarse vacuum rectifying column 1 for propionic aldehyde 11 through pump, it is 8-20 kPa in vacuum, when being preferably the coarse vacuum of 15-18 kPa, boiling point is lower than the methyl mercapto light components 12 for propionic aldehyde, including hydrogen sulfide, methyl sulfide, acrylic aldehyde, acetic acid, methanol, morpholine and water, discharge from the tower top of coarse vacuum rectifying column 1, be sent directly into emulsion tank 3.Now, heavier component 13 at the bottom of the tower of coarse vacuum rectifying column 1, it is mainly methyl mercapto for propionic aldehyde, and boiling point is higher than the methyl mercapto heavy component for propionic aldehyde, including polymer etc. for propionic aldehyde of a small amount of hydroquinone, acrolein polymer and methyl mercapto, it is pumped up into high vacuum rectification tower 2, it is 1-5 kPa in vacuum, it is preferably under the high vacuum condition of 3-4 kPa, the purity product methyl mercapto more than 99.7% is discharged from the tower top of high vacuum rectification tower 2 for propionic aldehyde 14, sends into product storage tank (not shown).The heavy component 15 got at the tower bottom of high vacuum rectification tower 2 includes a large amount of methyl mercapto for propionic aldehyde polymer, a small amount of acrolein polymer etc..Due to the economy principle operated according to rectifying column principle and tower, methyl mercapto can not be distilled off from tower top completely for propionic aldehyde, therefore, possibly together with a small amount of methyl mercapto for propionic aldehyde in the heavy component at the bottom of high vacuum rectification tower 2 tower.Owing to the Organic substance in the heavy component 15 at the bottom of tower has the characteristic of essence, trace residue in the environment, also almost can be permanently present, contaminated environment.Therefore, it must be avoided to reveal in an atmosphere as far as possible.These heavy components 15 are pumped up into emulsion tank 3.Emulsion tank 3 is outside can be provided with jacket heat-preservation layer, and inside can be provided with agitator and control the buncher of agitator.
In time having heavy component 15 to send in emulsion tank 3, start mechanical agitation, regulate speed of agitator by buncher, regulate the temperature of emulsion tank simultaneously, until the liquid in emulsion tank becomes uniform and stable emulsion 16.In this process, it is crucial for forming uniform and stable emulsion, if uniform and stable emulsion can not be formed, can there is creaming of emulsion, heavy component is in lower floor, and light components, on upper strata, so goes in the process burned in conveying, the viscosity of heavy component is still very big, pipeline can be blocked, it is impossible to conveying, then in the process processing blocking pipeline, inevitably these odorants are revealed in the environment, cause serious Environment Pollution Event.In the method for the invention, it is possible to forming uniform and stable emulsion 16 by adjustment speed of agitator, temperature, emulsification times, the viscosity of this emulsion 16 is almost suitable for propionic aldehyde with product methyl mercapto, it is simple to canned motor pump is carried.Table 1 be light heavy component different temperatures, rotating speed, emulsification times emulsifying effectiveness.Test shows, in optional stirrer paddle form, rotating speed is not less than 150RMP, and emulsifying temperature is not less than 60 DEG C, when emulsification times is not less than 5min, all emulsifiable for being suitable for the emulsion transported.Wherein, it is preferred that emulsification condition is: agitator speed is 200RMP；Emulsifying temperature is 80 DEG C；Emulsification times is 10min；The emulsion particle diameter of its formation can reach 100nm.
Table 1 different temperatures, rotating speed, emulsification times emulsifying effectiveness
Emulsion 16 after emulsifying is sent into incinerator 4 by canned motor pump through pipeline.Combustion-supporting gas 18 and natural gas 19 are sent in incinerator 4 to help to burn described emulsion 16.Flue gas 17 after burning is mainly carbon dioxide, air and trace sulfur dioxide, it is possible to be directly discharged in air.
As can be seen here, will from the coarse vacuum rectifying column 1 isolated light components of tower top 12 and feeding emulsion tank 3 together with heavy component 15 isolated at the bottom of high vacuum rectification tower 2 tower, by controlling emulsification condition, all can prepare viscosity suitable for propionic aldehyde with methyl mercapto, uniform and stable, it is simple to the emulsion of transport pump, solve conveying weight component respectively and can block a difficult problem for pipeline, stop environmental protection event to produce, improve workshop and local resident's environment.
It will be appreciated by those skilled in the art that above-described embodiment is only for explaining that the present invention makes any restriction not for it.
Claims (1)
1. the thick methyl mercapto synthesized by methanthiol and acrolein reaction processes a system for propionic aldehyde, including:
Coarse vacuum rectifying column, receives the thick methyl mercapto synthesized by methanthiol and acrolein reaction for propionic aldehyde, contains methyl mercapto for the heavier component of propionic aldehyde and from tower top discharge light components from discharging at the bottom of tower, and during work, the vacuum of coarse vacuum rectifying column is 8-20 kPa；
High vacuum rectification tower, what receive discharge at the bottom of the tower of coarse vacuum rectifying column contains the methyl mercapto heavier component for propionic aldehyde, discharges product methyl mercapto for propionic aldehyde from tower top, and from discharging heavy component at the bottom of tower, during work, the vacuum of high vacuum rectification tower is 1-5 kPa；
Emulsion tank, receives the light components discharged from the tower top of coarse vacuum rectifying column and from the heavy component of discharge at the bottom of the tower of high vacuum rectification tower, and light components and heavy component form uniform and stable emulsion at emulsion tank internal emulsification；Wherein emulsion tank is provided externally with jacket heat-preservation layer, and inside is provided with agitator and controls the variator of agitator；During work, rotating speed is not less than 150RPM, and emulsifying temperature is not less than 60 DEG C, and emulsification times is not less than 5min；
Incinerator, from the emulsion tank described emulsion of reception and burns described emulsion by pipeline, and incinerator also receives combustion-supporting gas and natural gas to help to burn described emulsion；And
Canned motor pump, for sending into incinerator by pipeline from emulsion tank by described emulsion.
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| CN201410245911.0A CN104045590B (en) | 2012-04-28 | 2012-04-28 | The thick methyl mercapto of methanthiol and acrylic aldehyde synthesis is for the process system of propionic aldehyde |
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| CN201410245911.0A CN104045590B (en) | 2012-04-28 | 2012-04-28 | The thick methyl mercapto of methanthiol and acrylic aldehyde synthesis is for the process system of propionic aldehyde |
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| CN201210131610.6A Division CN102633698B (en) | 2012-04-28 | 2012-04-28 | Treating method and system for crude methylthiopropanal synthesized of methyl mercaptan and acraldehyde |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4319047A (en) * | 1979-07-10 | 1982-03-09 | Rhone-Poulenc Industries | Preparation of beta-methylthiopropionaldehyde |
| CN1188470A (en) * | 1995-06-22 | 1998-07-22 | 诺沃斯国际公司 | Process for preparation of 3-(methylthion) propanal |
| US6057481A (en) * | 1996-04-01 | 2000-05-02 | Union Carbide Chemicals & Plastics Technology Corporation | Processes for the manufacture of methylmercaptopropanal |
| CN102282119A (en) * | 2008-11-20 | 2011-12-14 | 阿肯马法国公司 | Method for manufacturing methylmercaptopropionaldehyde and methionine using renewable raw materials |
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2012
- 2012-04-28 CN CN201410245911.0A patent/CN104045590B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4319047A (en) * | 1979-07-10 | 1982-03-09 | Rhone-Poulenc Industries | Preparation of beta-methylthiopropionaldehyde |
| CN1188470A (en) * | 1995-06-22 | 1998-07-22 | 诺沃斯国际公司 | Process for preparation of 3-(methylthion) propanal |
| US6057481A (en) * | 1996-04-01 | 2000-05-02 | Union Carbide Chemicals & Plastics Technology Corporation | Processes for the manufacture of methylmercaptopropanal |
| CN102282119A (en) * | 2008-11-20 | 2011-12-14 | 阿肯马法国公司 | Method for manufacturing methylmercaptopropionaldehyde and methionine using renewable raw materials |
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Effective date of registration: 20160527 Address after: 755000 the Ningxia Hui Autonomous Region central defence industrial park Applicant after: NINGXIA ZIGUANG TIANHUA METHIONINE CO., LTD. Address before: 408200, Chongqing County, Zhenjiang Town, Fengdu village Xiangjiaba Applicant before: Chongqing Unisplendour Tianhua Methionine Co., Ltd. |
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