CN110787476A - High-efficient reaction rectifier unit of n butyl acetate - Google Patents

High-efficient reaction rectifier unit of n butyl acetate Download PDF

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Publication number
CN110787476A
CN110787476A CN201911099811.0A CN201911099811A CN110787476A CN 110787476 A CN110787476 A CN 110787476A CN 201911099811 A CN201911099811 A CN 201911099811A CN 110787476 A CN110787476 A CN 110787476A
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CN
China
Prior art keywords
tower
pipeline
phase
butyl acetate
plate
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.)
Pending
Application number
CN201911099811.0A
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Chinese (zh)
Inventor
张超
何晓芳
李祥建
杜树旺
吴艳
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LINYI JINXIMENG BIOLOGICAL TECHNOLOGY Co Ltd
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LINYI JINXIMENG BIOLOGICAL TECHNOLOGY Co Ltd
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Publication date
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Priority to CN201911099811.0A priority Critical patent/CN110787476A/en
Publication of CN110787476A publication Critical patent/CN110787476A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/32Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/08Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/48Separation; Purification; Stabilisation; Use of additives
    • C07C67/52Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C67/54Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

Abstract

The invention discloses a n-butyl acetate high-efficiency reaction rectifying device which comprises a plate tower, an esterification kettle, a reboiler, a condenser, a cooler and a phase separator, wherein the esterification kettle and the reboiler are connected with each other through a pipeline and a pipe fitting and are connected with the plate tower; the condenser is connected to the top of the plate tower through a pipeline; the phase separator is connected with a plate tower through a pipeline and a reflux pump, a reaction liquid circulating feed inlet is arranged on the plate tower and is connected with the esterification kettle through the pipeline and a reaction liquid circulating pump, and a tower middle extraction outlet and a reflux port are also arranged on the plate tower and are connected with a tower middle cooler through the pipeline. The device can effectively separate byproducts in the production process, reduces the alcohol content in the reactants at the top of the tower to the minimum, and reduces the separation load of a subsequent system; the material circulation amount in the production process can be reduced, so that the purposes of saving energy, reducing consumption and increasing productivity are achieved.

Description

High-efficient reaction rectifier unit of n butyl acetate
Technical Field
The invention relates to the technical field of chemical equipment, in particular to an efficient reaction and rectification device for n-butyl acetate.
Background
In chemical production, n-butyl acetate is usually produced by a continuous esterification method, namely raw materials of acetic acid and n-butyl alcohol are subjected to esterification reaction in a strong acid homogeneous catalyst at a certain temperature and under a certain pressure, a reaction product is primarily separated by an esterification tower to obtain a crude ester semi-finished product, and the crude ester semi-finished product is separated by a dehydration tower to obtain an n-butyl acetate product. The traditional esterification method production device adopts a ceramic packed tower as an esterification tower, so that the reaction system has the following problems: 1. as strong acid is used as a catalyst in the esterification reaction, the strong oxidizing property of the strong acid is easy to cause side reactions such as sulfonation, carbonization and the like, so that the pollution of a reaction system in chemical production is fast, the cleaning period is frequent, and the ceramic filler is washed and corroded, so that the rectification effect is easily reduced; 2. in the traditional esterification reaction-rectification process using a ceramic packed tower as an esterification tower, because the conversion rate of n-butanol is low, the alcohol content at the top of the ceramic packed tower is high, so that the n-butanol which is not completely reacted is brought into a subsequent separation system, and the alcohol which is not completely reacted needs to be separated and then enters a reaction system again to participate in the esterification reaction, thus increasing the energy consumption of the reaction and separation system in the esterification reaction process. 3. The reflux amount of the ortho-esterification system is large, so that the energy consumption is high.
Disclosure of Invention
The invention aims to provide an efficient reaction rectifying device for n-butyl acetate, which is used for solving the problems of serious equipment corrosion, poor rectifying effect, larger reflux, low n-butyl alcohol conversion rate and high energy consumption in the device for synthesizing the n-butyl acetate by an esterification method.
The invention provides the following technical scheme:
an efficient reaction rectifying device for n-butyl acetate comprises a plate tower, an esterification kettle, a reboiler, a condenser, a cooler and a phase separator, wherein the esterification kettle and the reboiler are connected with each other through a pipeline and a pipe fitting and are connected with the plate tower, and the condenser, the cooler and the phase separator are sequentially connected through the pipeline and the pipe fitting; the condenser is connected to the top of the plate tower through a pipeline; the phase separator is connected with a plate tower through a pipeline and a reflux pump, a reaction liquid circulating feed inlet is arranged on the plate tower and is connected with the esterification kettle through the pipeline and a reaction liquid circulating pump, and a tower middle extraction outlet and a reflux port are also arranged on the plate tower and are connected with a tower middle cooler through the pipeline.
The preferred scheme of the high-efficiency reaction rectifying device for the n-butyl acetate is that the reaction liquid circulating feed inlet is positioned at the middle lower part of the plate tower.
A preferred scheme of the n-butyl acetate efficient reaction rectifying device is that a middle extraction opening of a tower is positioned in the middle of a plate tower, so that liquid in the tower is extracted, cooled by a cooler, passes through a potential difference, naturally overflows and then returns to two layers of tower plates below the middle extraction opening of the tower.
The preferred scheme of the high-efficiency reaction rectifying device for the n-butyl acetate is that the phase separator is connected with a water phase extraction tank and an ester phase reflux tank through pipelines.
A high-efficiency reaction rectifying device for n-butyl acetate is characterized in that materials at the top of a tower are subjected to phase separation by a phase separator, and a bottom water phase enters a water phase extraction tank and then is extracted to a waste water tank; the upper ester phase enters an ester phase reflux tank, then partially reflows through a reflux pump, and part of the ester phase is taken as crude ester to be extracted.
The invention has the beneficial effects that:
(1) the device provided by the invention can effectively separate byproducts in the production process, reduce the alcohol content in the reactants at the top of the tower to the minimum and reduce the separation load of a subsequent system;
(2) the invention can reduce the material circulation in the production process, thereby achieving the purposes of saving energy, reducing consumption and increasing productivity;
(3) the invention can effectively reduce the cleaning frequency of the reaction system, and the pollution of the reaction system is slow;
(4) the invention can effectively reduce the reflux ratio of the tower top.
Drawings
The above and other features, properties and advantages of the present invention will become more apparent from the following description of the embodiments with reference to the accompanying drawings in which like reference numerals denote like features throughout the several views, wherein:
FIG. 1 is a schematic diagram of a high efficiency reactive distillation apparatus of the present invention.
FIG. 2 is a partially enlarged schematic view of a catalytic distillation apparatus according to the present invention.
In the figure: 1. an esterification kettle; 2. a reboiler; 3. a condenser; 4. a cooler; 5. a phase splitter; 6. a cooler in the column; 7. a reflux pump; 8. a reaction liquid circulating pump; 9. a plate column.
Detailed Description
The technical solutions described in the present application are further described below with reference to the accompanying drawings and embodiments. It should be noted that the following paragraphs may refer to terms of orientation including, but not limited to, "upper, lower, left, right, front, rear", etc., which are based on the orientation shown in the drawings corresponding to the specification, and should not be construed as limiting the scope or technical solutions of the present application, but merely as facilitating better understanding of the technical solutions described in the present application by those skilled in the art.
Embodiment 1 referring to fig. 1 and 2, an n-butyl acetate high-efficiency reactive distillation device comprises a tray column 9, an esterification kettle 1, a reboiler 2, a condenser 3, a cooler 4 and a phase separator 5, wherein the esterification kettle 1 and the reboiler 2 are connected with each other through a pipeline and a pipe fitting and are connected with the tray column 9, and the condenser 3, the cooler 4 and the phase separator 5 are sequentially connected through a pipeline and a pipe fitting; the condenser 3 is connected to the top of the plate tower 9 through a pipeline; the phase separator 5 is connected with a plate tower 9 through a pipeline and a reflux pump 7, a reaction liquid circulating feed inlet is arranged on the plate tower 9 and is connected with the esterification kettle 1 through a pipeline and a reaction liquid circulating pump 8, and a tower middle extraction outlet and a reflux opening are also arranged on the plate tower 9 and are connected with a tower middle cooler 6 through a pipeline.
Specifically, the reaction liquid circulation feed inlet is positioned at the middle lower part of the plate tower 9. The extraction outlet in the tower is positioned in the middle of the plate tower 9, so that liquid in the tower is extracted, cooled by the cooler 6 in the tower, and naturally overflows through the potential difference and then returns to two layers of tower plates below the extraction outlet in the tower.
Wherein, the phase separator 5 is connected with a water phase extraction tank and an ester phase reflux tank through pipelines; after the materials at the top of the tower are subjected to phase splitting by the phase splitter 5, the bottom water phase enters a water phase extraction tank and then is extracted to a wastewater tank; the upper ester phase enters an ester phase reflux tank, then partially reflows through a reflux pump 7, and part of the ester phase is taken as crude ester to be extracted.
When the invention is used, raw materials of acetic acid and n-butanol are added into a reaction kettle according to a certain proportion, and the reaction is carried out in the reaction kettle under the condition of steam heating, and the generated products are n-butyl acetate and water; ester, water and alcohol ternary azeotrope or ester and water binary azeotrope is rectified in a plate tower 9 to obtain a crude ester semi-finished product with low water, alcohol and acid content from the top of the plate tower 9. The reaction liquid circulating feed inlet positioned at the middle lower part of the plate tower 9 enables the catalyst in the reaction liquid to enter the middle lower part of the plate tower and reversely contact with n-butyl alcohol and acetic acid which are not completely reacted, further reaction enables the alcohol content in the n-butyl acetate reaction product to be reduced to the minimum, the reaction conversion rate is improved, the effect is improved, the separation burden of a system is reduced, the material circulating amount in the production process is reduced, and the purposes of saving energy, reducing consumption and improving productivity are achieved.
When the invention is used, liquid materials in a production pipe in the tower are introduced to a cooler 6 in the tower for cooling, and the cooled materials naturally overflow through the potential difference and then return to the lower two layers of tower plates at a production port in the tower. The purpose of reducing the reflux quantity at the top of the tower and improving the productivity is achieved.
After the invention is used, the alcohol content in the crude ester semi-finished product generated at the top of the plate tower is lower than 1 percent, and the using time and the maintenance period of the equipment are obviously improved compared with the prior traditional equipment, thereby reducing the production cost and improving the production efficiency.
It should be noted that the above-mentioned embodiments are only some of the preferred modes for implementing the invention, and not all of them. Obviously, all other embodiments obtained by persons of ordinary skill in the art based on the above-mentioned embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.

Claims (5)

1. A high-efficiency reaction rectifying device for n-butyl acetate comprises a plate tower, an esterification kettle, a reboiler, a condenser, a cooler and a phase separator, and is characterized in that the esterification kettle and the reboiler are connected with each other through a pipeline and a pipe fitting and are connected with the plate tower, and the condenser, the cooler and the phase separator are sequentially connected through a pipeline and a pipe fitting; the condenser is connected to the top of the plate tower through a pipeline; the phase separator is connected with a plate tower through a pipeline and a reflux pump, a reaction liquid circulating feed inlet is arranged on the plate tower and is connected with the esterification kettle through the pipeline and a reaction liquid circulating pump, and a tower middle extraction outlet and a reflux port are also arranged on the plate tower and are connected with a tower middle cooler through the pipeline.
2. The efficient reaction rectifying device for n-butyl acetate according to claim 1, wherein the circulating feed inlet of the reaction liquid is positioned at the middle lower part of the plate tower.
3. The efficient reaction and rectification device for n-butyl acetate as claimed in claim 1, wherein the extraction port in the tower is located in the middle of the plate-type tower, so that liquid in the tower is extracted, cooled by a cooler, and naturally overflows through a head and then returns to two layers of tower plates below the extraction port in the tower.
4. The efficient reaction rectifying device for n-butyl acetate according to claim 1, wherein the phase separator is connected with the aqueous phase extraction tank and the ester phase reflux tank through pipelines.
5. The efficient reaction and rectification device for n-butyl acetate as claimed in claim 4, wherein after the phase separation of the material at the top of the column by the phase separator, the bottom aqueous phase enters the aqueous phase extraction tank and is extracted into the wastewater tank; the upper ester phase enters an ester phase reflux tank, then partially reflows through a reflux pump, and part of the ester phase is taken as crude ester to be extracted.
CN201911099811.0A 2019-11-12 2019-11-12 High-efficient reaction rectifier unit of n butyl acetate Pending CN110787476A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911099811.0A CN110787476A (en) 2019-11-12 2019-11-12 High-efficient reaction rectifier unit of n butyl acetate

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Application Number Priority Date Filing Date Title
CN201911099811.0A CN110787476A (en) 2019-11-12 2019-11-12 High-efficient reaction rectifier unit of n butyl acetate

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111848399A (en) * 2020-07-14 2020-10-30 上海交通大学 Method for separating dimethyl oxalate and dimethyl carbonate with low energy consumption

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111848399A (en) * 2020-07-14 2020-10-30 上海交通大学 Method for separating dimethyl oxalate and dimethyl carbonate with low energy consumption

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