CN205821214U - A kind of production technology device of high-purity methyl acetate - Google Patents
A kind of production technology device of high-purity methyl acetate Download PDFInfo
- Publication number
- CN205821214U CN205821214U CN201620700649.9U CN201620700649U CN205821214U CN 205821214 U CN205821214 U CN 205821214U CN 201620700649 U CN201620700649 U CN 201620700649U CN 205821214 U CN205821214 U CN 205821214U
- Authority
- CN
- China
- Prior art keywords
- section
- methyl acetate
- methanol
- distillation column
- production technology
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses the production technology device of a kind of high-purity methyl acetate, including reactive distillation column and multiple external hanging type reactor, described reactive distillation column is divided into separating methanol section, reactive multilayer section, extraction section and rectifying section from bottom to up, described reactive multilayer section is plate column plate structure, and the conversion zone of every layer of column plate is connected with corresponding external hanging type reactor cycles by pipeline；Described extraction section connects with reactive multilayer section, and is provided with acetic acid entrance；The top of described rectifying section is also associated with condenser and return tank；Described segregation section is provided with methanol inlet, and the bottom cycle connection of segregation section has reboiler.Reaction and separation are organically combined by this utility model, thus improve reaction rate, inhibit again the generation of back reaction, it is effectively improved conversion ratio, it is achieved thereby that the lifting of methyl acetate product quality concentration, can be used for producing high-purity (more than 97%) methyl acetate product, there is the features such as simple, efficient, remarkable in economical benefits.
Description
Technical field
This utility model belongs to derived energy chemical technical field, particularly relates to process units and the process of methyl acetate.
Background technology
Methyl acetate is a kind of important solvent and Organic Chemicals, is used for replacing acetone, butanone, ethyl acetate, ring
Pentanes etc., are mainly used for the quick-drying solvent as NC Nitroncellulose and cellulose acetate, as paint, artificial leather and
Raw material that spice manufactures and be used as oil extraction agent etc.；Meanwhile, high-purity methyl acetate can be used for synthesize acetic acid, acetic anhydride, third
E pioic acid methyl ester, vinyl acetate and acetamide etc..Along with the development of C1 chemical industry, the demand that methyl acetate is applied as the raw material of industry
Increase further.The methyl acetate concentration of market sale is mostly 90%～95%(mass fraction, lower same), high-purity tumer
The market price of ester (more than 97%) costly, has the biggest economic worth.Methanol and acetic acid are under acidic catalyst effect
Can generate methyl acetate, the condition of reaction is gentleer, but owing to binary or ternary can be formed between methyl acetate, methanol, water
Azeotrope, so being difficult to prepare highly purified methyl acetate by conventional method.Industrial conventional production high-purity methyl acetate
Need to use 1 reactor and 9 rectifying columns.The major defect of common process is:
L the synthesis of () methyl acetate is reversible reaction, by Equilibrium limit, reaction conversion ratio is low.
(2) methyl acetate and water, tumer is cruel and methanol, and methyl acetate, methanol, water three are formed and methyl acetate respectively
The azeotropic mixture that boiling point is close, it is difficult to separating, product purification system is sufficiently complex.
(3) having a large amount of unreacted methanol and acetic acid to need circulation in system, separation process is complicated, and equipment investment is big, energy consumption
High.
For solving the problem of above-mentioned existence, research uses the technology generations of reaction rectification technique synthesis methyl acetate for traditional
Technique will have great meaning.
Summary of the invention
Goal of the invention: for the problem and shortage of above-mentioned existing existence, the purpose of this utility model is to provide a kind of high-purity
The production technology apparatus and method of degree methyl acetate, can obtain the methyl acetate product of 97% concentrations above, have conversion ratio high,
Separation efficiency is high, the features such as investment of production equipment is little, and production cost is low.
Technical scheme: in order to solve above-mentioned technical problem, this utility model by the following technical solutions: a kind of high-purity vinegar
The production technology device of acid methyl ester, including reactive distillation column and multiple external hanging type reactor, described reactive distillation column is from bottom to up
Being divided into separating methanol section, reactive multilayer section, extraction section and rectifying section, described reactive multilayer section is plate column plate structure, every layer of tower
By tedge UNICOM between plate, the conversion zone of every layer of column plate is connected with corresponding external hanging type reactor cycles by pipeline；Institute
State extraction section to connect with reactive multilayer section, and be provided with acetic acid entrance；The top of described rectifying section is also associated with condenser and backflow
Tank；Described segregation section is provided with methanol inlet, and the bottom cycle connection of segregation section has reboiler.
As preferably, the bottom of described reactive distillation column is also associated with methanol distillation column.
As preferably, described methanol inlet is connected with the conversion zone entrance of the bottom.
Beneficial effect: compared with prior art, this utility model mainly uses reactive distillation by course of reaction and to separate
Journey organically combines, and reactant separates with product while reaction.By improving reactant concentration in the reactor,
Thus improve reaction rate, make product leave reactor in time again and inhibit the generation of back reaction, be effectively improved acetic acid
The conversion ratio of methyl ester synthetic reaction, it is achieved thereby that the lifting of methyl acetate product quality concentration.This utility model can be used for giving birth to
Production of high purity (more than 97%) methyl acetate product, the method has the features such as simple, efficient, remarkable in economical benefits.
Accompanying drawing explanation
Fig. 1 is the production technology apparatus structure schematic diagram of methyl acetate described in the utility model.
Wherein, reactive distillation column 1, reboiler 2, condenser 3, return tank 4, external hanging type reactor 5, methanol distillation column 6.
Detailed description of the invention
Below in conjunction with the accompanying drawings and specific embodiment, it is further elucidated with this utility model, it should be understood that these embodiments are only used for
This utility model is described rather than limits scope of the present utility model, after having read this utility model, art technology
Personnel all fall within the application claims limited range to the amendment of the various equivalent form of values of the present utility model.
Shown in Fig. 1, the manufacturing technique method of high-purity methyl acetate of the present utility model, by course of reaction and separation process
Organically combining, reactant separates with product while reaction.This had both improve reactant concentration in the reactor,
Thus improve reaction rate, make product leave reactor in time again and inhibit the generation of back reaction, effectively carry tumer
The conversion ratio of ester synthesis reaction, it is achieved thereby that the lifting of methyl acetate product quality concentration.Specific embodiment is as follows
(1) reaction raw materials acetic acid autoreaction rectifying column middle and upper part enters, and methanol enters from middle and lower part, and feeding temperature is 40 DEG C
Left and right.Employing strongly acidic cation-exchange is catalyst.
(2) middle and upper part of reactive distillation column is extraction section, and the methyl acetate come from conversion zone top and azeotropic mixture thereof enter
Extraction section, acetic acid extraction section be reactant be also extractant, react with methanol as reactant acetic acid, generate tumer
Ester.
(3) the middle part methanol of reactive distillation column and the acetic acid from extraction section are mainly through row esterification.Owing to esterification is anti-
Should be to carry out in the liquid phase.Therefore external hanging type reactor is devised to obtain high liquid holdup.Under the effect of catalyst, instead
Answer through row esterification in the plug-in reactor of tower, generate water and methyl acetate.
(4) the main separating reaction in the bottom of reactive distillation column generates water and unreacting material methanol and mixture, through gas
After proposing separation, water is discharged from the bottom of tower, and methanol is upwardly into conversion zone, continues to participate in esterification, thus is effectively improved raw material first
The conversion ratio of alcohol.
Reactive distillation column bottom is substantially carried out methanol and separates with water generation reaction, by reboiler methanol steam constantly on
Rise and participate in esterification；And tower reactor drop temperature is about 100 DEG C, entering methanol distillation column, methanol loop uses, and waste water is arranged
Go out.
At rectifying section, primarily discrete methyl acetate and raw material acetic acid, the acetic acid obtaining purity is worth, and drop temperature is 56
About DEG C.An innovative point of the present utility model is: the middle part of reactive distillation section is reactive multilayer section, and every layer of column plate is instead
Answer layer, and connected with corresponding plug-in reactor cycles by pipeline, by the reaction liquid phase of conversion zone is sent into plug-in reaction
Reacting in device, maintain the liquid hold-up of esterification, the liquid phase after esterification returns to react anti-during column plate
Should be while the temperature that controls conversion zone makes acetic acid product methyl ester take the lead in from liquid-phase reaction system separates gasification and enter upper strata
Column plate, in such liquid phase, the concentration of methyl acetate is less than equilibrium composition, thus has broken the restriction of chemical equilibrium.Make esterification
React the direction to generating methyl acetate to carry out.Meanwhile, owing to acetic acid is to enter from conversion zone top, the acetic acid on upper strata contains
Amount is relatively big, is also extractant while participating in esterification, and the dissolubility in acetic acid is than its dissolving in methyl acetate
Degree is bigger, and the H2O in such MeOAc/H2O is preferentially dissolved in acetic acid, has broken azeotropic composition so that complicated azeotropic mixture obtains
To efficiently separating.
The generation place that plug-in reactor is esterification of this utility model design, due to the boiling point of acetic acid product methyl ester
Less than material benzenemethanol and acetic acid, the methyl acetate of generation takes the lead in separating from the liquid-phase reaction system of column plate, and gasification enters
Upper strata column plate, in such liquid phase, the concentration of methyl acetate is less than equilibrium composition, thus has broken the restriction of chemical equilibrium.Make
Esterification is carried out to the direction generating methyl acetate.
Preferably, the input concentration of material benzenemethanol is more than 99%, wt%.Preferred feedstock concentration is 99%, 99.2%,
99.5%、99.7%；The charge ratio of material benzenemethanol and acetic acid is (1.2～1.6): 1, preferably 1.2:1,1.3:1,1.4:1,1.5:
1、1.6:1；Final tower top methyl acetate product quality mark is more than 97%, up to 97.5%, 98%, 98.5%, 99%, 99.5.
Embodiment: the feedstock quality flow of methanol is 2135.6kg/hr, the feedstock quality flow of acetic acid is 3364.9kg/
Hr, using BHS II type high efficiency packing and strongly acidic cation-exchange is catalyst, by calculating and commercial Application practice
Recurrence, obtaining T1 tower tower diameter is 1.2m, by carrying out esterification, the acetic acid of generation in the plug-in reactor of reactive distillation column
Methyl ester takes the lead in separating from the liquid-phase reaction system of column plate, and gasification enters upper strata column plate, by the concentration of extraction section with point
From, break azeotropic system so that molecular balance is constantly carried out towards the direction of methyl acetate, the tumer of the continuous extraction of tower top simultaneously
Ester product, its mass fraction reaches more than 99%, wt%.
Claims (3)
1. the production technology device of a high-purity methyl acetate, it is characterised in that: include reactive distillation column and multiple external hanging type
Reactor, described reactive distillation column is divided into separating methanol section, reactive multilayer section, extraction section and rectifying section from bottom to up, described many
Layer conversion zone is plate column plate structure, by tedge UNICOM between every layer of column plate, the conversion zone of every layer of column plate by pipeline with
Corresponding external hanging type reactor cycles connects；Described extraction section connects with reactive multilayer section, and is provided with acetic acid entrance；Described rectification
The top of section is also associated with condenser and return tank；Described segregation section is provided with methanol inlet, and the bottom cycle of segregation section connects
There is reboiler.
The production technology device of high-purity methyl acetate the most according to claim 1, it is characterised in that: described reactive distillation column
Bottom be also associated with methanol distillation column.
The production technology device of high-purity methyl acetate the most according to claim 2, it is characterised in that: described methanol inlet with
The conversion zone entrance of the bottom connects.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620700649.9U CN205821214U (en) | 2016-07-06 | 2016-07-06 | A kind of production technology device of high-purity methyl acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620700649.9U CN205821214U (en) | 2016-07-06 | 2016-07-06 | A kind of production technology device of high-purity methyl acetate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN205821214U true CN205821214U (en) | 2016-12-21 |
Family
ID=57563994
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201620700649.9U Active CN205821214U (en) | 2016-07-06 | 2016-07-06 | A kind of production technology device of high-purity methyl acetate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN205821214U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112480064A (en) * | 2020-12-21 | 2021-03-12 | 天津科技大学 | Method for synthesizing lactide through back-pack type continuous rectification |
| CN114014755A (en) * | 2021-12-07 | 2022-02-08 | 江苏省瑞丰高分子材料有限公司 | Organic chemical methyl acetate and production process thereof |
-
2016
- 2016-07-06 CN CN201620700649.9U patent/CN205821214U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112480064A (en) * | 2020-12-21 | 2021-03-12 | 天津科技大学 | Method for synthesizing lactide through back-pack type continuous rectification |
| CN114014755A (en) * | 2021-12-07 | 2022-02-08 | 江苏省瑞丰高分子材料有限公司 | Organic chemical methyl acetate and production process thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103333047B (en) | Preparation method of dichloropropanol | |
| CN101475472B (en) | Method for preparing oxalate by coupling reaction of CO in gaseous phase | |
| CN103012062A (en) | Process for indirectly producing alcohol with synthetic gas and application of process | |
| CN104761429A (en) | Dimethyl carbonate and ethylene glycol production process | |
| CN101830807B (en) | Synthesizing device and process for alkyl nitrite | |
| CN102816061A (en) | Method for simultaneously preparing pyromellitic acid and terephthalic acid with coal serving as raw material | |
| CN203033918U (en) | Process system for indirectly producing ethanol by using synthesis gases | |
| CN104529763A (en) | Process and device for synthesizing ethyl formate with reactive distillation dividing wall column | |
| Zheng et al. | Simulation study of direct hydration of cyclohexene to cyclohexanol using isophorone as cosolvent | |
| CN102134191B (en) | Process method for producing ethyl acetate by catalytic rectification | |
| CN105801408B (en) | A kind of reaction and rectification device producing high purity acrylic acid N-butyl and method | |
| CN104151164A (en) | Method for preparing methyl chloroacetate | |
| Souza et al. | Glycerol esterification with acetic acid by reactive distillation using hexane as an entrainer | |
| CN205821214U (en) | A kind of production technology device of high-purity methyl acetate | |
| CN205347278U (en) | Synthetic methyl nitrite's device | |
| CN105968007A (en) | High-purity methyl acetate production process device and method | |
| CN102234224A (en) | Method for catalytic synthesis of dichloropropanol by hydrogen chloride-containing industrial waste gas and glycerol | |
| CN109134198A (en) | A kind of method of separation of extractive distillation tetrafluoropropanol and water azeotropic mixture | |
| CN112851507A (en) | Process for synthesizing methyl methacrylate by ethanol | |
| CN101979365A (en) | Method for continuously preparing dichlorohydrin | |
| CN103772185A (en) | Device and method for removing moisture and heteroacids in acetic acid | |
| CN101367733B (en) | Heat pump distillation apparatus and process for diethyl carbonate | |
| CN103387495A (en) | Method for the continuous production of carboxylic acid esters | |
| CN208166890U (en) | Interval catalytic reaction rectification prepares the device of dibutyl phthalate | |
| CN109646977B (en) | Reactive distillation coupling tower and application thereof in preparation of formic acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |