CN209338421U - The preparation facilities of propylene glycol methyl ether acetate - Google Patents
The preparation facilities of propylene glycol methyl ether acetate Download PDFInfo
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- CN209338421U CN209338421U CN201821969062.3U CN201821969062U CN209338421U CN 209338421 U CN209338421 U CN 209338421U CN 201821969062 U CN201821969062 U CN 201821969062U CN 209338421 U CN209338421 U CN 209338421U
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- propylene glycol
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- acetate
- methyl ether
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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Abstract
The utility model belongs to chemical reagent preparation technical field, is related to a kind of preparation facilities of propylene glycol methyl ether acetate.The preparation facilities of the propylene glycol methyl ether acetate, including propylene glycol monomethyl ether Material supply system, methyl acetate Material supply system, reaction unit, propylene glycol methyl ether acetate products pot and methanol product tank；Reaction unit is provided with basic catalyst；Propylene glycol monomethyl ether Material supply system and methyl acetate Material supply system are connect with the feed inlet of reaction unit respectively, and propylene glycol methyl ether acetate products pot and methanol product tank are connect with the discharge port of reaction unit respectively.The utility model improves reaction conversion ratio and yield, the phenomenon that alleviating equipment seriously corroded, extend the service life of equipment, the recyclable recycling of catalyst, reduce production cost, the solution route of a low cost, high efficiency, clean and environmental protection, high income, application easy to spread are provided to the production of propylene glycol methyl ether acetate.
Description
Technical field
The utility model belongs to chemical reagent preparation technical field, in particular to a kind of propylene glycol methyl ether acetate
Preparation facilities.
Background technique
Propylene glycol methyl ether acetate (abbreviation PMA) is a kind of important low toxicity, advanced industrial solvent, has unique molecule
Structure is that one kind has multi-functional non-public hazards solvent, existing nonpolar moiety in same molecule, and polarized polarity portion
Point, this two-part functional group, which not only mutually restricts, to be repelled, but also respectively plays its intrinsic effect, therefore it is to polarity and nonpolarity
Substance has preferable solvability, and solubility property is much higher than common solvent and propylene glycol ethers and gylcol ether is molten
Agent.Since propylene glycol methyl ether acetate has excellent performance, it is widely used in paint, ink, coating, detergent, printing and dyeing, spinning
Knit, sense organ material, pesticide and pluronic polymer etc. it is industrial, it can also be used to the cleaning agent in production of liquid crystal displays.
Currently, the synthetic method of propylene glycol methyl ether acetate mainly has direct esterification, ester-interchange method or by propylene oxide
With methyl acetate one-step synthesis.Wherein direct esterification is raw material through esterification system third using propylene glycol monomethyl ether and acetic acid
Glycol methyl ether acetate is the highly developed industrial method of current technology, is more general technology path.Produced in conventional processes
PMA is usually using inorganic acid as catalyst, and pollution, seriously corroded can not be reused, and be not readily separated.Generally speaking,
Existing PMA production technology or system are primarily present following problems: (1) using acetic acid as raw material, with for phosphoric acid, hydrochloric acid, the concentrated sulfuric acid,
The acid such as chlorosulfonic acid, oxalic acid, citric acid, methanesulfonic acid or p-methyl benzenesulfonic acid is used as catalyst, and equipment etching problem is serious, maintenance of equipment
High expensive；(2), it is usually simple tank reactor, carries out rectifying again after the reaction was completed, reaction conversion ratio is low, yield is not high,
Conversion ratio is generally 40%~50%；(3) catalyst amount cannot recycle 1% or so and lead to not reuse, and waste is big,
Cause production cost higher.
It is more more and more urgent to the clean manufacturing demand of PMA with the raising that Environmental Protection in China requires, it needs to traditional production
System improves, and develops a kind of efficient, clean and environmental protection PMA production technology, improves product yield and conversion ratio, alleviate corrosion
Seriously, the higher problem of material loss, popularization production, market efficiency and enterprise to PMA and society all have and its important
Meaning.
In consideration of it, special propose the utility model.
Summary of the invention
The purpose of this utility model is to provide a kind of preparation facilities of propylene glycol methyl ether acetate, can overcome above-mentioned ask
Inscribe or at least be partially solved above-mentioned technical problem.
To achieve the above object, the technical solution adopted in the utility model are as follows:
A kind of preparation facilities of propylene glycol methyl ether acetate, including propylene glycol monomethyl ether Material supply system, methyl acetate are former
Expect supply system, reaction unit, propylene glycol methyl ether acetate products pot and methanol product tank；
The reaction unit is provided with basic catalyst；
The propylene glycol monomethyl ether Material supply system and the methyl acetate Material supply system react dress with described respectively
The feed inlet connection set, the propylene glycol methyl ether acetate products pot and the discharging with the reaction unit respectively of methanol product tank
Mouth connection.
As further preferred technical solution, the reaction unit is reactive distillation column, the tower top of the reactive distillation column
It is connect with methanol product tank, the tower bottom of the reactive distillation column is connect with propylene glycol methyl ether acetate products pot.
As further preferred technical solution, the propylene glycol monomethyl ether Material supply system and methyl acetate raw material supply system
System respectively includes propylene glycol monomethyl ether storage tank and methyl acetate storage tank, the feed inlet of the reaction unit respectively with the propylene glycol first
Ether storage tank is connected with methyl acetate storage tank.
It further include methyl acetate and methanol separator and propylene glycol monomethyl ether-the third two as further preferred technical solution
Alcohol methyl ether acetate-catalyst separation device.
As further preferred technical solution, the methyl acetate and methanol separator includes dealcoholysis tower and recovery tower, institute
The tower top for stating reactive distillation column is successively connect with dealcoholysis tower and recovery tower, the MA discharge port and methyl acetate raw material of the dealcoholysis tower
Supply system is connected and/or is connect with reaction unit, and the discharge port of the recovery tower is connect with methanol product tank.
As further preferred technical solution, the dealcoholysis tower is Salt Addition Extraction Refinery Tower.
As further preferred technical solution, the propylene glycol monomethyl ether-propylene glycol methyl ether acetate-catalyst separation device
Including ether-ether knockout tower and evaporation equipment, the tower bottom of the reactive distillation column is successively connect with ether-ether knockout tower and evaporation equipment,
The PM discharge port of the ether-ether knockout tower connect with propylene glycol monomethyl ether Material supply system and/or connect with reaction unit, described
The discharge port of evaporation equipment is connect with propylene glycol methyl ether acetate products pot.
As further preferred technical solution, the ether-ether knockout tower is vacuum rectification tower.
As further preferred technical solution, the evaporation equipment is scraper evaporator.
It further include propylene glycol monomethyl ether preheater and methyl acetate preheater as further preferred technical solution, described third
Glycol methyl ether Material supply system is connected by the feed inlet of propylene glycol monomethyl ether preheater and reaction unit, and the methyl acetate is former
Expect that supply system is connected by the feed inlet of methyl acetate preheater and reaction unit.
Compared with prior art, the utility model has the beneficial effects that:
The utility model uses basic catalyst as catalyst, carries out using propylene glycol monomethyl ether and methyl acetate as raw material
The phenomenon that ester exchange reaction improves reaction conversion ratio and yield, alleviates equipment seriously corroded, extend equipment uses year
Limit, the recyclable recycling of catalyst, reduces production cost, to the production of propylene glycol methyl ether acetate provide one it is low at
The solution route of sheet, high efficiency, clean and environmental protection, high income can reduce cost, economize on resources, reduce environmental pollution, green ring
It protects, creates good economic benefit and environmental benefit, improve the market competitiveness of propylene glycol methyl ether acetate, it is easy to spread
Using.
Utility model device is structurally reasonable, equipment operational safety, reliable and stable, sets without complicated, expensive
It is standby, it can satisfy the demand of Vehicles Collected from Market, it is easy to accomplish large-scale production.
Detailed description of the invention
It, below will be right in order to illustrate more clearly of specific embodiment of the present invention or technical solution in the prior art
Specific embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, it is described below
In attached drawing be that some embodiments of the utility model are not paying creativeness for those of ordinary skill in the art
Under the premise of labour, it is also possible to obtain other drawings based on these drawings.
Fig. 1 is the preparation facilities structural schematic diagram of propylene glycol methyl ether acetate provided by the embodiment of the utility model；
Fig. 2 is the preparation method flow diagram of propylene glycol methyl ether acetate provided by the embodiment of the utility model.
Icon: 1- reactive distillation column；2- dealcoholysis tower；3- recovery tower；4- ether-ether knockout tower；5- scraper evaporator；6- the third two
Alcohol methyl ether storage tank；7- methyl acetate storage tank；8- methanol product tank；9- propylene glycol methyl ether acetate products pot；101,102,103,
104,105- condensed in two stages device.
Specific embodiment
The technical solution of the utility model is clearly and completely described below, it is clear that described embodiment is this
Utility model a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the utility model protection
Range.
It is in the description of the present invention, it should be noted that term " center ", "upper", "lower", "left", "right", " perpendicular
Directly ", the orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, and is only
For ease of description the utility model and simplify description, rather than the device or element of indication or suggestion meaning must have it is specific
Orientation, be constructed and operated in a specific orientation, therefore should not be understood as limiting the present invention.In addition, term " the
One ", " second ", " third " are used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " is pacified
Dress ", " connected ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or integrally
Connection；It can be mechanical connection, be also possible to be electrically connected；Can be directly connected, can also indirectly connected through an intermediary,
It can be the connection inside two elements.For the ordinary skill in the art, above-mentioned art can be understood with concrete condition
The concrete meaning of language in the present invention.
It should be understood that
In the utility model, if without particularly illustrating, all embodiments mentioned in this article and preferred implementation
Method can be combined with each other to form new technical solution.
In the utility model, if without particularly illustrating, all technical characteristics and preferred feature mentioned in this article
It can be combined with each other to form new technical solution.
In the utility model, unless otherwise indicated, each reaction or operating procedure can be carried out sequentially, can not also be according to
Sequence carries out.Preferably, operating method herein is that sequence carries out.
A kind of preparation facilities of propylene glycol methyl ether acetate, including propylene glycol monomethyl ether original are provided at least one embodiment
Expect supply system, methyl acetate Material supply system, reaction unit, propylene glycol methyl ether acetate products pot and methanol product tank；
The reaction unit is provided with basic catalyst；
The propylene glycol monomethyl ether Material supply system and the methyl acetate Material supply system react dress with described respectively
The feed inlet connection set, the propylene glycol methyl ether acetate products pot and the discharging with the reaction unit respectively of methanol product tank
Mouth connection.
It should be understood that the preparation method of the propylene glycol methyl ether acetate, comprising: with propylene glycol monomethyl ether and methyl acetate
Propylene glycol methyl ether acetate and methanol are obtained by reaction in the presence of basic catalyst for raw material.
In view of existing propylene glycol methyl ether acetate (PMA) production technology there are equipment seriously corroded, catalyst repeat
The problems such as, high production cost not high using difficult, reaction conversion ratio and product yield, the utility model breaks those skilled in the art
The confinement of conventional thought provides a kind of PMA synthetic technology of novel green chemical technology, reduces investment, maintenance cost to reach,
Reaction conversion ratio and product yield, safety and environmental protection, the purpose for avoiding equipment corrosion phenomenon are improved, and has found and realizes the purpose
Particular technique means greatly improve reaction conversion ratio and product yield with these technological means, reduce the corrosivity to equipment,
The costs such as investment, operation, maintenance are reduced, and recycling for catalyst may be implemented, further increase the market competition of PMA
Power.
Further speaking, the preparation method of the utility model belongs to green chemistry process, is the skill by improving chemistry
Art and method reduce the chemical industry product even completely eliminated to human health, the harmful effect of ecological environment, while promoting chemistry
The realization of industrial energy saving target.The exploitation of green chemistry process is chemically reacted in line with the principle of zero-emission, clean manufacturing
Beginning is set about, and then effectively prevent and control the generation of pollution.
On the one hand, the selection of raw material is the source of production of chemicals, meanwhile, also decide different chemical production process and
Technique.The exploitation primary goal of green chemistry process is without using poisonous and hazardous raw material.In order to prevent chemical dirt from source
The principle of dye, green chemistry process exploitation is to try to that reproducible natural material is selected to make raw material.Such as sawdust, branch etc. are wild
The waste of the agricultural and sideline products such as fibre plant and bagasse, wheat straw, straw is furfural and alcohol, ketone, acids as Raw material processing
Chemicals generates hydrogen etc. with gasification of biomass, is all the typical example of green material application.On the other hand, using nontoxic nothing
Very important part in harmful chemical catalyst and green chemistry process.Currently, about 90% or more chemical reaction is real
Existing industrialized production needs to improve its reaction rate using catalyst；Thus, developing new and effective, nontoxic catalyst is
One of direction of green chemistry process.
Based on this, principle of the utility model based on Green Chemistry, provide it is a kind of with propylene glycol monomethyl ether (abbreviation PM) and
Methyl acetate (also at methyl acetate, abbreviation MA) is raw material, uses basic catalyst as catalyst, carries out ester exchange reaction,
The method for synthesizing PMA, not only increases the conversion ratio of reaction and the yield of product, and harm to the human body is small, simple process,
Easily operated, highly-safe, used raw material and catalyst safety, environmental protection are small to equipment corrosion, reduce equipment investment
And maintenance maintenance cost, the service life of equipment is extended, meanwhile, basic catalyst can be recycled and be recycled, and be reduced
The loss of resource, avoids waste, greatly reduces production cost.
In a preferred embodiment, it the described method comprises the following steps:
It,, will using reactive distillation column as reaction unit using alkali as catalyst using propylene glycol monomethyl ether and methyl acetate as raw material
Propylene glycol monomethyl ether, methyl acetate and basic catalyst are added from the identical or different position of reactive distillation column respectively, are reacted；
The tower bottom of reactive distillation column produces the mixture of propylene glycol monomethyl ether, propylene glycol methyl ether acetate and basic catalyst,
Propylene glycol methyl ether acetate product is obtained after separation；
The overhead extraction methyl acetate of reactive distillation column and the mixture of methanol obtain methanol after separation and can return
It is back to the methyl acetate that circular response is carried out in reactive distillation column.
According to the utility model, raw material PM and MA and basic catalyst can add from the different parts of rectifying column respectively
Enter, such as the middle and upper part from tower, middle part, middle and lower part or lower part enter, and can also be added from the same section of tower, such as three is equal
It is added from tower reactor.It is understood that different reactive modes, feeding manner is different, such as when continuous reaction rectification, PM, MA
It can be added from the middle and upper part of rectifying column, middle part and middle and lower part with basic catalyst, when batch reactive distillation, then can select respectively
It selects and is added to three together in the tower reactor of reactive distillation column.
It, can be with it should be noted that the utility model is not particularly limited the specific constructive form of reactive distillation column
For packed tower or plate column, the specific theoretical cam curve of rectifying column is also that those skilled in the art can be according to specific
Actual process demand is calculated, and the utility model is not described in detail herein.
The utility model utilizes the rectificating method of reactive distillation, promotes to react with rectifying, i.e., is constantly removed instead by rectifying
The product answered, to improve reaction conversion ratio and product yield.It is demonstrated experimentally that the reaction conversion ratio of the utility model method is reachable
To 70% or more, product yield can reach 95% or more, compared with existing PMA synthetic method, reaction conversion ratio and product yield
All it is largely increased.
Optionally, PM, MA and basic catalyst are proportionally added into the tower reactor of rectifying column；
Alternatively, PM, MA and basic catalyst can also be proportionally added into pre-reactor, it is performed under heating conditions
Then initial reaction enters back into reaction kettle.In this way, helping to further increase reaction conversion ratio, accelerate reaction speed.
In a preferred embodiment, the reaction includes that continuous rectification reaction or batch fractionating react, preferably
Batch fractionating reaction.
It should be understood that the reaction can be reacted using continuous rectification, can also be reacted using batch fractionating, it is preferred to use
Batch fractionating reaction.The features such as batch fractionating operation has operation relatively easy, and flexible and changeable, opposite continuous rectification, interval
Rectifying can a kettle one charging, batch fractionating is more energy efficient when treating capacity is fewer.In addition, when containing in raw material compared with multicomponent
Batch fractionating is preferably used, a set of equipment can separate each component, save equipment investment.
In a preferred embodiment, the basic catalyst includes the alkyl oxide and/or alkalinity of alkali metal
Resin catalyst；
Preferably, the alkyl oxide of the alkali metal includes sodium methoxide, potassium methoxide, sodium ethoxide, potassium ethoxide, sodium tert-butoxide
At least one of with potassium tert-butoxide, preferably sodium methoxide.
The utility model replaces acetic acid as raw material using MA, using acidic catalysts such as the basic catalyst substitution concentrated sulfuric acids
Agent can greatly reduce the corrosivity to equipment, extend the service life of equipment, reduce maintenance maintenance cost.Meanwhile the alkalinity is urged
Agent can be can be avoided the waste to resource, further be saved cost with recycling and reusing.
It should be understood that the utility model is not particularly limited the concrete type of basic catalyst, as long as not right
The purpose of this utility model generates limitation.
Preferably, using the alkyl oxide of alkali metal as catalyst, such as sodium methoxide, sodium ethoxide, potassium methoxide etc.；More
Good, using sodium methoxide as catalyst, have source wide, at low cost, the more preferable feature of application effect.
According to the utility model, the distillation of batch reactive distillation tower is added with methyl acetate according to a certain ratio for propylene glycol monomethyl ether
In kettle (tower reactor), and a certain amount of basic catalyst sodium methoxide being added, starting, which stirs and opens steam valve, begins to warm up reaction,
The methanol steam generated in reaction process with methyl acetate after overhead condenser condenses formed azeotropic mixture head fraction first from
Overhead extraction, the methyl acetate and carbinol mixture of extraction promote the progress of propylene glycol monomethyl ether ester exchange reaction, help to mention
High reaction conversion ratio.The azeotropic mixture is sent to dealcoholysis tower and recovery tower carries out methanol and (can be used with separating for methyl acetate and add salt
The mode of extracting rectifying is separated), obtained methanol can be used as product sale, and methyl acetate can then be back to reactive distillation
It is recycled in tower.Secondly the methyl acetate (interim fraction) of extraction can also return again to after overhead condenser condenses to reaction
It is recycled in rectifying column.After reaction, propylene glycol monomethyl ether, propylene glycol methyl ether acetate and methanol are mainly contained in distillation still
Sodium, the kettle liquid are sent into ether-ether batch fractionating tower and carry out rectifying, successively isolate propylene glycol monomethyl ether, propylene glycol monomethyl ether and propylene glycol first
Ether acetate mixture, propylene glycol methyl ether acetate (product).Wherein, propylene glycol monomethyl ether can import head tank, continue
Reaction.Propylene glycol monomethyl ether can also be used as raw material and return in rectifying column with propylene glycol methyl ether acetate mixture to be continued to react
Rectifying.Residual kettle is propylene glycol methyl ether acetate and sodium methoxide mixed liquor, and the kettle is residual to be scraped by evaporation equipment such as scraper evaporator
Except sodium methoxide (recycles), product propylene glycol methyl ether acetate is obtained, can be further improved product yield.
In a preferred embodiment, by the mixed of propylene glycol monomethyl ether, propylene glycol methyl ether acetate and basic catalyst
It closes in object feeding ether-ether knockout tower and carries out rectifying, successively isolate propylene glycol monomethyl ether, propylene glycol monomethyl ether and propylene glycol monomethyl ether acetic acid
The mixture and propylene glycol methyl ether acetate of ester, wherein propylene glycol monomethyl ether is back in head tank and is recycled, and/
Or, the mixture of propylene glycol monomethyl ether and propylene glycol methyl ether acetate is back in head tank and is recycled；
Preferably, the mixture of propylene glycol monomethyl ether, propylene glycol methyl ether acetate and basic catalyst is sent into ether-ether separation
Rectifying is carried out in tower, obtains the mixed liquor that kettle liquid is propylene glycol methyl ether acetate and basic catalyst, the mixed liquor is sent into
It is separated in evaporation equipment, obtains propylene glycol methyl ether acetate product；
Preferably, the evaporation equipment is scraper evaporator.
The utility model process matching scraper evaporator can carry out recycling and reusing to catalyst, reduce the wave of resource
Take, reduces cost.
It should be noted that reactive distillation column tower bottom extraction propylene glycol monomethyl ether, propylene glycol methyl ether acetate and base catalysis
The mixture of agent is sent into ether-ether knockout tower and scraper evaporator, is separated, further increases the yield of product, so that catalysis
Agent can recycle.Special limit is not done for concrete operations condition the utility model of ether-ether knockout tower and scraper evaporator
System, can be regulated and controled by those skilled in the art according to actual process demand.
It is understood that batch fractionating is nonstationary state process, feed liquid is added portionwise to the distillation operation carried out in tower reactor.
Device therefor is with continuous rectification equipment the difference is that bottom is equipped with the biggish tower reactor of volume, and tower body is without stripping section.It is produced from tower reactor
Raw steam rises along tower, after phegma contact mass transfer, into condenser.A part of condensate liquid is made as product, a part
Tower top is returned for reflux.Since the concentration of volatile components in overhead product is high, under the concentration of volatile components is continuous in kettle liquid
Drop.It when being reduced to normal concentration, stops operation, kettle liquid is once discharged.If being maintained the reflux in operation than constant, distillate
Composition will decline therewith；Conversely, should then continue to increase reflux ratio in distillation process to remain unchanged distillate composition.For
Reach scheduled requirement, practical operation can be versatile and flexible.
Intermittent rectification under vacuum can be used in the mixture (ether-ether mixture) of the reactive distillation column tower reactor extraction of the utility model
Mode of operation, decompression realize negative-pressure operation by vacuum pump, and saturated vapor or other heating methods can be used in heating.
The mixed material of propylene glycol monomethyl ether, propylene glycol methyl ether acetate and basic catalyst that reactive distillation column tower reactor produces
After liquid reaches certain liquid level pumped to ether-ether knockout tower tower reactor, ether-ether kettle type reboiler is passed through steam, and ether-ether knockout tower boils again
Device vaporizes material in tower reactor constantly, and gas-liquid contact is carried out in tower with liquid phase in tower, after infinite reflux is stablized, is formed in tower
Substantially invariable concentration gradient and temperature gradient, material steam after condenser condenses and after trap trapping, lead to from tower top
Cross reflux ratio controller, a part is back to tower top, remaining condensate liquid by reactor product cooler, successively produce interim fraction,
Propylene glycol monomethyl ether, propylene glycol methyl ether acetate, and sequentially enter correspondingly received tank.Situations such as considering sticky material and temperature-sensitive, tower
Kettle material carries out forced circulation through falling liquid film circulating pump and the falling film evaporator of outfit, shortens the residence time in kettle, increases evaporation
Rate.
It can also be sent to scraper plate thin film evaporation workshop section by falling liquid film circulating pump when kettle liquid processing is to certain liquid level, steamed
Hair.Light phase is sent into storage tank after being condensed by the condenser, the heavy phase barrelling being scraped off.
In a preferred embodiment, the overhead extraction of reactive distillation column includes the mixture of methyl acetate and methanol
And methyl acetate, methyl acetate, which is back in reactive distillation column after overhead condenser condenses, carries out circular response；
Preferably, the mixture of methyl acetate and methanol is separated in the way of extractive distillation with salt；
Preferably, extractant used by extractive distillation with salt is acetic acid aqueous solutions of potassium.
Extracting rectifying is that third component is added into material liquid, is reached with changing the relative volatility between original component point
From desired special extract rectification method.It requires the boiling point of extractant much higher compared with the boiling point of each component in material liquid, and not with group
Divide and form azeotropic liquid, is easy recycling.Extracting rectifying is usually used in separating the solution of each component volatility difference very little.Saline extraction benefit
It is that (in the aqueous solution of weak electrolyte, refractory tungsten alloys and non-electrolyte, the inorganic salts of non-same ion, energy is added in salt effect
The activity coefficient for changing solution, to change the degree of dissociation or solubility) principle, salt good separating effect in dissolved salt rectifying improves
The separating effect of solvent, reduces solvent ratio in extracting rectifying.Extractive distillation with salt is by dissolved salt rectifying and extracting rectifying
The method that advantage is integrated in one uses salt+solvent for the technical process of mixed extractant.It is waved opposite giving full play to salt
While hair degree influences, overcomes solid salt in dissolved salt rectifying and is not easy to convey, recycle and disadvantage that extraction distillation solvent dosage is big,
The effect for improving extractant, reduces energy consumption.This particular advantages and effect that the technique has, keep its more economical, are easier to
It is industrialized in realizing.
The utility model preferably uses the aqueous solution of potassium acetate as extractant, in this way can preferably by methyl acetate and
Separating methanol, and potassium acetate is more suitable for the preparation method of the utility model, it is easy to operate, it is easy to control, it can be better
Reuse methyl acetate.
It should be noted that the methyl acetate of reactive distillation column overhead extraction and the azeotropic mixture of methanol enter dealcoholysis tower and return
It receives in tower, is separated by the way of extractive distillation with salt, for the dealcoholysis tower and the concrete operations condition of recovery tower this reality
It does not do specifically limited with novel, can be regulated and controled by those skilled in the art according to actual process demand.
Optionally, the mixture of methyl acetate and methanol enters from the lower part of dealcoholysis tower, and extractant is from the middle part of dealcoholysis tower
Or top enters, the inlet amount ratio (mass ratio) of mixture and extractant is 1:0.5~5, preferably 1:1~3.
Optionally, the mass percentage of salt is 2~20%, preferably 5~15% in extractant.
Further, according to the utility model, point of methyl acetate and methanol is carried out using dealcoholysis tower and solvent recovery tower
From, separate foundation: using the aqueous solution containing potassium acetate as extractant, eliminate methyl acetate and methanol between azeotropic, increase component between
Relative volatility, reach separation purpose.The mixed material of methyl acetate and methanol is from dealcoholysis tower (can also claim extractive distillation column)
The aqueous solution of lower part charging, extractant potassium acetate is fed from dealcoholysis tower top, and vapour-liquid mass, the vapour that tower top rises are carried out in tower
Mutually enter return tank, the predominantly higher methyl acetate of purity after overhead condenser condenses, the material is after tower top return pump
Partial reflux partially enters and produces dealcoholysis tower as product, and tower reactor is then that the aqueous solution containing methanol, potassium acetate enters solvent recovery
Tower carries out extractant recycling.
Material from dealcoholysis tower tower reactor enters solvent recovery tower, and (middle and upper part carries out atmospheric distillation, the gas phase that tower top rises
Through overhead condenser) enter return tank, the predominantly mixture containing a small amount of methyl acetate, water and a large amount of methanol, the object after condensation
Material partial reflux after tower top return pump, part produce；Tower reactor is that the aqueous solution of potassium acetate returns after tower reactor cooler is cooling
Dealcoholysis tower uses.
The utility model Dichlorodiphenyl Acetate methyl esters and methanol in the way of extractive distillation with salt are separated, and vinegar is not only realized
Sour methyl esters recycles, and methanol can be used as product sale, and extractant acetic acid aqueous solutions of potassium is also achieved and recycled, and is kept away
The waste for having exempted from resource, further reduces costs, and improves the economic value of product.
In a preferred embodiment, the mass ratio of methyl acetate, propylene glycol monomethyl ether and basic catalyst is (100
~150): (50~65): (0.8~1.2), preferably (120~130): (55~60): 1.
According to the utility model, in the ester exchange reaction of methyl acetate and propylene glycol monomethyl ether, excessive tumer joined
Ester can promote the conversion ratio of propylene glycol monomethyl ether, and excessive methyl acetate can be repeated and be utilized.Methyl acetate and third
The mass ratio (100~150) of glycol methyl ether: (50~65), preferably (120~130): (55~60), it is typical but unrestricted
Such as can be 120:55,122:56,122:57,125:57,126:58,128:58,130:60,100:50,110:52,115:
54,140:62,145:65 or 150:150.
The additional amount of basic catalyst can be on the basis of the gross mass of methyl acetate and propylene glycol monomethyl ether, it can be seen that
The additional amount of the catalyst of the utility model is less, and the additional amount of catalyst accounts for methyl acetate and propylene glycol monomethyl ether gross mass
0.5% or so, such as 0.3%~0.8% or 0.4%~0.6%, can react fully progress in this way, reach preferable catalysis
Effect, and help to reduce the energy consumption of later period separation.
In a preferred embodiment, reaction temperature is 100~115 DEG C, preferably 105~110 DEG C；
And/or the reaction time is 4~10h, preferably 5~8h.
It is understood that she reacts using batch reactive distillation, which refers to a batch of reaction
Time, reaction temperature are the temperature of tower bottom of rectifying tower.Operating pressure is normal pressure, that is, common rectifying column can be used and reacted.
According to the utility model, reaction temperature is 100~115 DEG C, preferably 105~110 DEG C, typical but non-limiting
It such as can be 100 DEG C, 102 DEG C, 104 DEG C, 105 DEG C, 106 DEG C, 107 DEG C, 108 DEG C, 109 DEG C, 110 DEG C, 112 DEG C or 115 DEG C；
Reaction time be 4~10h in the reaction time, preferably 5~8h, it is typical but unrestricted for example can for 4h, 5h, 6h, 7h,
8h, 9h or 10h.
It should be noted that the utility model is not particularly limited remaining operating condition of the reactive distillation column,
It can be regulated and controled according to the actual situation by those skilled in the art, such as reflux ratio can be 1~10 perhaps 2~8 or 2
~6 etc..
It should be understood that the content being not described in detail in the explanation of above-mentioned preparation method, is those skilled in the art
The Common Parameters being readily apparent that, therefore can be omitted detailed description thereof.
The preparation facilities of propylene glycol methyl ether acetate provided by the utility model can be used for realizing above-mentioned propylene glycol monomethyl ether
The preparation method of acetate.The device can be improved the conversion ratio and product yield of reaction, obtain the propylene glycol monomethyl ether of high-purity
Acetate product, stability is good, reduces to the corrosivity of equipment, extends service life of equipment；And apparatus structure is simple, if
It sets rationally, it is equipment operational safety, reliable and stable, reduce operating cost and investment cost, it can be achieved that making full use of for resource,
It can satisfy the demand of Vehicles Collected from Market, it is easy to accomplish large-scale industrial production.
It is understood that propylene glycol monomethyl ether Material supply system and methyl acetate Material supply system respectively include the third two
Alcohol methyl ether storage tank and methyl acetate storage tank, the feed inlet of reaction unit connect with propylene glycol monomethyl ether storage tank and methyl acetate storage tank respectively
Connect, and for other devices involved in propylene glycol monomethyl ether Material supply system and methyl acetate Material supply system, equipment or
Connection relationship the utility model do not do it is specifically limited, can refer to propylene glycol monomethyl ether or methyl acetate in the prior art production dress
It sets, commercially available propylene glycol monomethyl ether and acetate also can be directly used, and deposited with propylene glycol monomethyl ether storage tank and methyl acetate storage tank
Storage.
In a preferred embodiment, the reaction unit is reactive distillation column, the tower top of the reactive distillation column
It is connect with methanol product tank, the tower bottom of the reactive distillation column is connect with propylene glycol methyl ether acetate products pot.
Further, which is batch reactive distillation tower.
Optionally, reactive distillation column is one or more, and multiple reactive distillation columns are connected in series.Reactive distillation tower is
When multiple, a variety of connection types can be used, such as reactive distillation column includes the first reactive distillation column and the second reactive distillation
When tower, the tower bottom discharge port of the first reactive distillation column is successively connect with ether-ether knockout tower and scraper evaporator, ether-ether knockout tower
Secondary condenser is arranged in tower top, and the outlet of secondary condenser is connect with the feed inlet of the second reactive distillation column；Second reactive distillation
The feed inlet of tower also connect with methyl acetate Material supply system or connect with the MA discharge port of dealcoholysis tower.
Optionally, condensed in two stages device, including concatenated first condenser and the second condensation is arranged in the tower top of reactive distillation column
The outlet of device, the outlet of the first condenser or the second condenser is connected by the refluxing opening of reflux pipeline and reactive distillation column, the
The outlet of two condensers is connect with the feed inlet of dealcoholysis tower.
Optionally, temperature control valve (TCV) is installed on reflux pipeline；And/or the tower bottom of reactive distillation column and ether-ether knockout tower
Temperature control valve (TCV) is provided on the pipeline of connection；And/or it is provided on the pipeline that is connect with dealcoholysis tower of the tower top of reactive distillation column
Temperature control valve (TCV) is provided in the connecting pipeline of the feed inlet of temperature control valve (TCV), the i.e. outlet of the second condenser and dealcoholysis tower.?
Temperature control valve (TCV) is arranged on each feeding line or reflux pipeline can be convenient the control to temperature, is preferably reacted or is divided
From.
It optionally, further include propylene glycol monomethyl ether preheater and methyl acetate preheater, propylene glycol monomethyl ether Material supply system
It is connected by the feed inlet of propylene glycol monomethyl ether preheater and reactive distillation column, methyl acetate Material supply system passes through methyl acetate
The connection of the feed inlet of preheater and reactive distillation column.It further, further include static mixer, propylene glycol monomethyl ether preheater and vinegar
The outlet of sour methyl esters preheater is connected by the feed inlet of static mixer and reactive distillation column respectively.Entering reactive distillation column
It is preheated or is mixed before, the conversion ratio of reaction can be improved, accelerate the progress of reaction, reaction effect is more preferable.
It in a preferred embodiment, further include methyl acetate and methanol separator and propylene glycol monomethyl ether-the third two
Alcohol methyl ether acetate-catalyst separation device；
Preferably, the methyl acetate and methanol separator includes dealcoholysis tower and recovery tower, the tower of the reactive distillation column
Top successively connect with dealcoholysis tower and recovery tower, the MA discharge port of the dealcoholysis tower connect with methyl acetate Material supply system and/
Or connect with reactive distillation column, the discharge port of the recovery tower is connect with methanol product tank；
Preferably, the dealcoholysis tower is Salt Addition Extraction Refinery Tower；
Preferably, the propylene glycol monomethyl ether-propylene glycol methyl ether acetate-catalyst separation device include ether-ether knockout tower and
Evaporation equipment, the tower bottom of the reactive distillation column are successively connect with ether-ether knockout tower and evaporation equipment, the ether-ether knockout tower
PM discharge port connect with propylene glycol monomethyl ether Material supply system and/or connect with reactive distillation column, the discharging of the evaporation equipment
Mouth is connect with propylene glycol methyl ether acetate products pot；
Preferably, the ether-ether knockout tower is vacuum rectification tower；
Preferably, the evaporation equipment is scraper evaporator.
It should be noted that the MA discharge port of dealcoholysis tower refers to the methyl acetate discharge port of dealcoholysis tower；Ether-ether knockout tower
PM discharge port refer to the propylene glycol monomethyl ether discharge port of ether-ether knockout tower.
Optionally, the tower top of the tower top of ether-ether knockout tower, the tower top of scraper evaporator, the tower top of dealcoholysis tower and/or recovery tower
It is provided with condensed in two stages device, including concatenated first condenser and the second condenser.
It should be understood that the content being not described in detail in the explanation of above-mentioned preparation facilities, is those skilled in the art
The commonly used equipment or structure being readily apparent that, therefore can be omitted detailed description thereof.
Combined with specific embodiments below and attached drawing, the utility model is described in further detail.
Embodiment 1
As shown in Figure 1, the present embodiment provides a kind of preparation facilities of propylene glycol methyl ether acetate, including propylene glycol monomethyl ether is former
Expect supply system, methyl acetate Material supply system, reaction unit, methyl acetate and methanol separator, propylene glycol monomethyl ether-the third
Glycol methyl ether acetate-catalyst separation device, propylene glycol methyl ether acetate products pot 9 and methanol product tank 8；In reaction unit
Equipped with basic catalyst；Basic catalyst is the alkyl oxide of alkali metal, including sodium methoxide, potassium methoxide, sodium ethoxide, ethyl alcohol
At least one of potassium, sodium tert-butoxide and potassium tert-butoxide, preferably sodium methoxide.
Wherein, reaction unit is reactive distillation column 1；Methyl acetate and methanol separator includes dealcoholysis tower 2 and recovery tower 3,
Dealcoholysis tower 2 is Salt Addition Extraction Refinery Tower；Propylene glycol monomethyl ether-propylene glycol methyl ether acetate-catalyst separation device includes ether-ether point
From tower 4 and evaporation equipment, ether-ether knockout tower 4 is vacuum rectification tower, and evaporation equipment is scraper evaporator 5.Propylene glycol monomethyl ether raw material
Supply system and methyl acetate Material supply system respectively include propylene glycol monomethyl ether storage tank 6 and methyl acetate storage tank 7.
The connection relationship of each device is as follows:
Propylene glycol monomethyl ether storage tank 6 and methyl acetate storage tank 7 are connect with the feed inlet of reactive distillation column 1 respectively, reactive distillation
Condensed in two stages device 101, including concatenated first condenser and the second condenser, the outlet of the first condenser is arranged in the tower top of tower 1
Or second the outlet of condenser connect with the refluxing opening of reactive distillation column 1 by reflux pipeline, the outlet of the second condenser with take off
The feed inlet of alcohol tower 2 connects, and the tower top of dealcoholysis tower 2 is provided with condensed in two stages device 102, the MA discharge port of condensed in two stages device 102 with
Methyl acetate storage tank 7 is connected and/or is connect with reactive distillation column 1, and dealcoholysis tower 2 is also connect with recovery tower 3, and 3 tower top of recovery tower is set
Condensed in two stages device 103 is set, the discharge port of condensed in two stages device 103 is connect with methanol product tank 8；
The tower bottom of reactive distillation column 1 is connect with ether-ether knockout tower 4, and the tower top of ether-ether knockout tower 4 is provided with condensed in two stages device
104, the discharge port of the condensed in two stages device 104 connect with propylene glycol monomethyl ether storage tank 6 and/or connect with reactive distillation column 1, and two-stage is cold
The discharge port of condenser 104 is also connect with propylene glycol methyl ether acetate products pot 9, and ether-ether knockout tower 4 also connects with scraper evaporator 5
It connects, the tower top of scraper evaporator 5 is provided with condensed in two stages device 105, the discharge port and propylene glycol monomethyl ether vinegar of the condensed in two stages device 105
Acid ester product tank 9 connects.
Further, temperature control valve (TCV) is installed on reflux pipeline；And/or the tower bottom of reactive distillation column 1 is separated with ether-ether
Temperature control valve (TCV) is provided on the pipeline that tower 4 connects；And/or second condenser outlet and dealcoholysis tower 2 feed inlet connection
Temperature control valve (TCV) (not shown) is provided on pipeline.
Embodiment 2
As shown in Fig. 2, the present embodiment provides a kind of preparation methods of propylene glycol methyl ether acetate, comprising the following steps:
Propylene glycol monomethyl ether and methyl acetate are added according to a certain ratio in the distillation still of batch reactive distillation tower, and are added certain
The catalyst sodium methoxide of amount, wherein the mass ratio of methyl acetate, propylene glycol monomethyl ether and basic catalyst is 126:58:1；
Starting, which stirs and opens steam valve, begins to warm up reaction, and reaction temperature is 107 DEG C, is reacted 5 hours, reaction process
The methanol steam of middle generation is forming azeotropic mixture head fraction first from overhead extraction with methyl acetate after overhead condenser condenses,
The methyl acetate and carbinol mixture of extraction promote the progress of propylene glycol monomethyl ether ester exchange reaction, 57 DEG C of tower top temperature at this time
Left and right.The azeotropic mixture is sent to dealcoholysis tower and recovery tower and carries out separating for methanol and methyl acetate；Methanol can be used as product sale,
Methyl acetate recycles.Secondly the methyl acetate (interim fraction) of extraction can recycle after overhead condenser condenses,
57.8 DEG C of tower top temperature or so at this time.
After reaction, propylene glycol monomethyl ether, propylene glycol methyl ether acetate and sodium methoxide are mainly contained in distillation still, the kettle liquid
It is sent into ether-ether batch fractionating tower and carries out rectifying, successively isolate propylene glycol monomethyl ether, propylene glycol monomethyl ether and propylene glycol methyl ether acetate
Mixture, propylene glycol methyl ether acetate.Wherein, propylene glycol monomethyl ether can import head tank, continue to react.Propylene glycol monomethyl ether
It also can be used as raw material with propylene glycol methyl ether acetate mixture and be back in reactive distillation column and continue reactive distillation.Kettle is residual to be
Propylene glycol methyl ether acetate and sodium methoxide mixed liquor, the kettle is residual to strike off sodium methoxide by scraper evaporator, the methanol struck off
Sodium is can be recycled, and obtains product propylene glycol methyl ether acetate, so further, to improve product yield.
A collection of secondary response 5 hours, non-cutting time 2 hours, add up to 7 hours.
In the present embodiment, the conversion ratio of reaction (propylene glycol monomethyl ether) is 75.2%, the yield of product propylene glycol methyl ether acetate
It is 96.5%.
Embodiment 3
A kind of preparation method of propylene glycol methyl ether acetate, the difference from example 2 is that:
The mass ratio of methyl acetate, propylene glycol monomethyl ether and basic catalyst is 120:55:1；
Reaction temperature is 110 DEG C.
In the present embodiment, the conversion ratio of reaction (propylene glycol monomethyl ether) is 73.6%, the yield of product propylene glycol methyl ether acetate
It is 95.8%.
Embodiment 4
A kind of preparation method of propylene glycol methyl ether acetate, the difference from example 2 is that:
The mass ratio of methyl acetate, propylene glycol monomethyl ether and basic catalyst is 148:65:1.2；
Reaction temperature is 104 DEG C.
In the present embodiment, the conversion ratio of reaction (propylene glycol monomethyl ether) is 70.3%, the yield of product propylene glycol methyl ether acetate
It is 95%.
Finally, it should be noted that the above various embodiments is only to illustrate the technical solution of the utility model, rather than it is limited
System；Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should
Understand: it is still possible to modify the technical solutions described in the foregoing embodiments, or to some or all of
Technical characteristic is equivalently replaced；And these are modified or replaceed, it does not separate the essence of the corresponding technical solution, and this is practical new
The range of each embodiment technical solution of type.
Claims (10)
1. a kind of preparation facilities of propylene glycol methyl ether acetate, which is characterized in that including propylene glycol monomethyl ether Material supply system, vinegar
Sour methyl ester feedstocks supply system, reaction unit, propylene glycol methyl ether acetate products pot and methanol product tank；
The reaction unit is provided with basic catalyst；
The propylene glycol monomethyl ether Material supply system and the methyl acetate Material supply system respectively with the reaction unit
Feed inlet connection, the propylene glycol methyl ether acetate products pot and methanol product tank connect with the discharge port of the reaction unit respectively
It connects.
2. the preparation facilities of propylene glycol methyl ether acetate according to claim 1, which is characterized in that the reaction unit is
The tower top of reactive distillation column, the reactive distillation column is connect with methanol product tank, the tower bottom and propylene glycol of the reactive distillation column
The connection of methyl ether acetate products pot.
3. the preparation facilities of propylene glycol methyl ether acetate according to claim 1, which is characterized in that the propylene glycol monomethyl ether
Material supply system and methyl acetate Material supply system respectively include propylene glycol monomethyl ether storage tank and methyl acetate storage tank, described anti-
The feed inlet of device is answered to connect respectively with the propylene glycol monomethyl ether storage tank and methyl acetate storage tank.
4. the preparation facilities of propylene glycol methyl ether acetate according to claim 2, which is characterized in that further include tumer
Ester-equipment for separating methanol and propylene glycol monomethyl ether-propylene glycol methyl ether acetate-catalyst separation device.
5. the preparation facilities of propylene glycol methyl ether acetate according to claim 4, which is characterized in that the methyl acetate-
Equipment for separating methanol includes dealcoholysis tower and recovery tower, and the tower top of the reactive distillation column is successively connect with dealcoholysis tower and recovery tower,
The MA discharge port of the dealcoholysis tower connect with methyl acetate Material supply system and/or connect with reaction unit, the recovery tower
Discharge port connect with methanol product tank.
6. the preparation facilities of propylene glycol methyl ether acetate according to claim 5, which is characterized in that the dealcoholysis tower is to add
Salt extraction rectifying column.
7. the preparation facilities of propylene glycol methyl ether acetate according to claim 4, which is characterized in that the propylene glycol first
Ether-propylene glycol methyl ether acetate-catalyst separation device includes ether-ether knockout tower and evaporation equipment, the tower of the reactive distillation column
Bottom is successively connect with ether-ether knockout tower and evaporation equipment, the PM discharge port of the ether-ether knockout tower and propylene glycol monomethyl ether raw material supply
System is connected and/or is connect with reaction unit, and the discharge port of the evaporation equipment is connect with propylene glycol methyl ether acetate products pot.
8. the preparation facilities of propylene glycol methyl ether acetate according to claim 7, which is characterized in that the ether-ether knockout tower
For vacuum rectification tower.
9. the preparation facilities of propylene glycol methyl ether acetate according to claim 7, which is characterized in that the evaporation equipment is
Scraper evaporator.
10. the preparation facilities of described in any item propylene glycol methyl ether acetates according to claim 1~3, which is characterized in that also wrap
Propylene glycol monomethyl ether preheater and methyl acetate preheater are included, the propylene glycol monomethyl ether Material supply system is pre- by propylene glycol monomethyl ether
The feed inlet of hot device and reaction unit connection, the methyl acetate Material supply system by methyl acetate preheater with react fill
The feed inlet connection set.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201821969062.3U CN209338421U (en) | 2018-11-28 | 2018-11-28 | The preparation facilities of propylene glycol methyl ether acetate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445824A (en) * | 2017-06-22 | 2017-12-08 | 江门谦信化工发展有限公司 | A kind of alcohol solvent of ether ester type energy-efficient reaction process and its reaction system |
| CN113979861A (en) * | 2021-11-29 | 2022-01-28 | 河北工业大学 | Method for preparing propylene glycol monomethyl ether acetate by catalytic distillation |
-
2018
- 2018-11-28 CN CN201821969062.3U patent/CN209338421U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445824A (en) * | 2017-06-22 | 2017-12-08 | 江门谦信化工发展有限公司 | A kind of alcohol solvent of ether ester type energy-efficient reaction process and its reaction system |
| CN113979861A (en) * | 2021-11-29 | 2022-01-28 | 河北工业大学 | Method for preparing propylene glycol monomethyl ether acetate by catalytic distillation |
| CN113979861B (en) * | 2021-11-29 | 2023-12-22 | 河北工业大学 | Method for preparing propylene glycol methyl ether acetate by catalytic rectification |
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