CN111807959A - Energy-saving process and process equipment for n-propyl acetate - Google Patents

Energy-saving process and process equipment for n-propyl acetate Download PDF

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Publication number
CN111807959A
CN111807959A CN202010703617.5A CN202010703617A CN111807959A CN 111807959 A CN111807959 A CN 111807959A CN 202010703617 A CN202010703617 A CN 202010703617A CN 111807959 A CN111807959 A CN 111807959A
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China
Prior art keywords
finished product
propyl acetate
phase
energy
rectifying tower
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CN202010703617.5A
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Chinese (zh)
Inventor
冯烈
吴方丽
陈云斌
李东
张华建
谈敦玲
王爱艳
刘小兵
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ZHEJIANG JIANYE CHEMICAL CO Ltd
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ZHEJIANG JIANYE CHEMICAL CO Ltd
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Priority to CN202010703617.5A priority Critical patent/CN111807959A/en
Publication of CN111807959A publication Critical patent/CN111807959A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/48Separation; Purification; Stabilisation; Use of additives
    • 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
    • B01D3/007Energy recuperation; Heat pumps
    • 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
    • B01D3/14Fractional 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
    • 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
    • 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
    • Y02P20/50Improvements relating to the production of bulk chemicals

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention provides an energy-saving process and process equipment for n-propyl acetate, which comprise a rectifying tower, wherein a liquid phase outlet of the rectifying tower is connected with a finished product extraction pump, the finished product extraction pump is connected with a finished product groove, a gas phase outlet of the rectifying tower is connected with a tower top condenser, the tower top condenser is connected with a phase splitter, and a split phase outlet of the phase splitter is connected with external extraction equipment and a reflux port of the rectifying tower. The gas-phase extraction of the finished ester is improved into liquid-phase extraction, so that the latent heat of vaporization of the finished ester is saved; the finished ester exchanges heat with the reflux component which flows back to the rectifying tower from the phase separator and then is conveyed to a finished product tank, so that the sensible heat of the finished ester is fully utilized, the energy is effectively saved, and the consumption is reduced.

Description

Energy-saving process and process equipment for n-propyl acetate
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to an energy-saving process and process equipment for n-propyl acetate.
Background
N-propyl acetate, also known as n-propyl acetate, is a commonly used fine chemical raw material, has good dissolving capacity for various synthetic resins, and is an excellent solvent for various synthetic resins such as ethyl cellulose, nitrocellulose, polymethacrylate and the like.
The production process of the n-propyl acetate comprises the steps of adding acetic acid and n-propyl alcohol into an esterification kettle, generating the n-propyl acetate under the action of a sulfuric acid catalyst, and finally obtaining reaction liquid containing the n-propyl acetate, the acetic acid, the n-propyl alcohol and water, so that the reaction liquid needs to be purified. The boiling points of the n-propanol, water and n-propyl acetate are close, and the molecular weight size relationship is as follows: the prior art utilizes the relationship of approximate boiling points and molecular weights of the three components, adopts a gas phase extraction mode of finished products at the bottom of a rectifying tower to extract the n-propyl acetate, and the extracted n-propyl acetate is conveyed to a condenser to be condensed and finally conveyed to a finished product tank.
As the industry competition increases, n-propyl acetate vapor consumption and finished product purity become the focus of the acetate industry competition. The rectification mode needs to consume more heat and has no competitive advantage in the aspect of steam consumption. Therefore, in order to overcome the defects of the prior art, it is necessary to develop a process method which can reduce energy consumption and heat consumption.
Disclosure of Invention
The invention aims to solve the problems and provide an energy-saving process for n-propyl acetate;
the invention also aims to solve the problems and provide process equipment for the energy-saving process of the n-propyl acetate.
In order to achieve the purpose, the invention adopts the following technical scheme:
the utility model provides a process equipment of energy-conserving technology of n-propyl acetate, includes the rectifying column, the liquid phase exit linkage of rectifying column has finished product extraction pump, finished product extraction pump connect in the finished product groove, the gaseous phase exit linkage of rectifying column is in overhead condenser, overhead condenser connect in the phase splitter, just the phase splitter's phase splitting exit linkage is in the backward flow mouth of outside extraction equipment and rectifying column.
In the process equipment of the n-propyl acetate energy-saving process, a heat exchanger is connected between the finished product extraction pump and the finished product tank, and the heat exchanger is simultaneously positioned between the phase separator and the rectifying tower and used for heat exchange between the finished ester and the reflux component.
In the process equipment for the n-propyl acetate energy-saving process, a finished product condenser is connected between the heat exchanger and the finished product tank, and the heat exchanger is positioned between the finished product extraction pump and the finished product condenser.
In the process equipment of the energy-saving process for the n-propyl acetate, the liquid phase outlet of the rectifying tower is simultaneously connected with a rectifying reboiler.
An energy-saving process for preparing n-propyl acetate includes such steps as controlling the rectifying temp in rectifying tower to make the water and n-propanol in raw ester be gas phase and n-propyl acetate be liquid phase, delivering the gas phase from gas outlet of rectifying tower to tower top condenser, phase-splitting the condensed mixture in phase splitter, collecting part of the condensed mixture, reflux of part of the condensed mixture to rectifying tower, and delivering the liquid phase from liquid outlet of rectifying tower to finished product tank via finished product pump.
In the n-propyl acetate energy-saving process, the liquid phase is extracted to the heat exchanger through the finished product extraction pump and then enters the finished product tank, and the mixed liquid flows back to the reflux component of the rectifying tower to exchange heat with the liquid phase in the heat exchanger and then flows back to the rectifying tower.
In the n-propyl acetate energy-saving process, the liquid phase after heat exchange is further condensed by a finished product condenser and then conveyed to a finished product tank.
In the energy-saving process for the n-propyl acetate, the rectification temperature of the rectification tower is controlled between 100 ℃ and 101 ℃ in the rectification process.
In the energy-saving process for the n-propyl acetate, the liquid phase outlet is positioned at the bottom of the rectifying tower, the gas phase outlet is positioned at the top of the rectifying tower, and before the finished ester is extracted, the gas phase outlet flows back to the rectifying reboiler to provide vaporization heat by the rectifying reboiler.
In the energy-saving process of the n-propyl acetate, the upper-layer components in the phase separator flow back to the rectifying tower, and the lower-layer components are extracted; or the upper layer component reflows to the rectifying tower, and the lower layer component is partially extracted and partially reflows.
The invention has the advantages that the gas phase extraction of the finished ester is improved into liquid phase extraction, thereby saving the latent heat of vaporization of the finished product; the finished ester exchanges heat with the reflux component which flows back to the rectifying tower from the phase separator and then is conveyed to a finished product tank, so that the sensible heat of the finished ester is fully utilized, the energy is effectively saved, and the consumption is reduced; the extraction of the finished ester adopts a pump as conveying power, so that the flow and the speed of the extraction can be controlled, and the extracted liquid-phase finished ester and reflux components which reflux to the rectifying tower from the phase separator can fully exchange heat.
Drawings
FIG. 1 is a process flow diagram of an energy-saving process for n-propyl acetate according to the present invention.
Reference numerals: a rectifier reboiler E1; a rectification column T1; a finished product take-off pump P1; heat exchanger E3; a finished condenser E4; finished product tanks V1, V2; overhead condenser E2; phase separator V3.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
As shown in fig. 1, the present embodiment discloses a process and an apparatus for an energy-saving process of n-propyl acetate, the apparatus mainly includes a rectification reboiler E1 and a rectification column T1, a liquid phase outlet at the bottom of the rectification column T1 is connected to a finished product extraction pump P1 for extracting finished ester from a liquid phase at the bottom of the column, and the finished product extraction pump P1 is connected to finished product tanks V1 and V2 through a heat exchanger E3 and a finished product condenser E4 in sequence; the gas phase outlet at the top of the rectifying tower T1 is connected with a tower top condenser E2, the tower top condenser E2 is connected with a phase separation inlet at the top of the phase separator V3, the phase separation outlet at the bottom of the phase separator V3 is connected with external extraction equipment, and meanwhile, the gas phase outlet is connected with the top reflux port of the rectifying tower T1 through a heat exchanger E3.
The extraction pump P1 provides power, and the finished product ester is conveyed to the heat exchanger E3 to exchange heat with the reflux component which flows back to the rectifying tower T1 from the phase separator V3, and then enters the finished product condenser E4 to further reduce the temperature of the finished product ester, and then is extracted to the finished product tank V1 or V2. The extraction pump P1 is used for providing conveying power, so that the extraction flow rate is controllable, and the heat exchange with the reflux component can be fully realized.
Further, the liquid phase outlet at the bottom of the rectification column T1 is simultaneously connected to the inlet of the rectification reboiler E1, and the heat of vaporization is provided by the rectification reboiler E1 before the production of the finished ester.
Specifically, the energy-saving process flow of the n-propyl acetate comprises the following steps: the distillation temperature is controlled in the distillation column T1, so that the water and the n-propanol in the crude ester are in a gas phase, the n-propyl acetate is in a liquid phase, and the distillation temperature is controlled between 100 ℃ and 101 ℃ in the embodiment. The traditional gas phase extraction mode needs to enable the rectification temperature to be higher than the vaporization temperature of the n-propyl acetate, and the liquid phase extraction mode is adopted in the embodiment, so that the rectification temperature can be lower than the vaporization temperature of the n-propyl acetate, the latent heat of vaporization of finished products can be saved, the production energy is effectively saved, and the consumption is reduced.
Specifically, the gas phase is sent from the gas phase outlet of the rectifying tower T1 to the overhead condenser E2, the condensed mixed liquid is separated into phases in the phase separator V3, and a part of the phase separator V3 is refluxed to the rectifying tower T1, and a part is extracted. The reflux extraction ratio is determined according to specific conditions, and can be 1:1, 1:2 and the like. The upper layer component is refluxed and the lower layer component is extracted by taking the component layering as a boundary, or the upper layer component is refluxed and the lower layer component is partially refluxed and partially extracted.
The liquid phase is extracted from a liquid phase outlet of the rectifying tower T1 to a heat exchanger E3 through a finished product extraction pump P1, then is further condensed by a finished product condenser E4 and then is conveyed to finished product tanks V1 and V2; the reflux component of the mixed liquid refluxed to the rectifying tower T1 exchanges heat with the liquid phase in the heat exchanger E3, and then refluxed to the rectifying tower T1. The extracted finished ester and the reflux component in the phase separator V3 are sent out after heat exchange, the sensible heat of the finished ester is fully utilized, and the consumption is reduced.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Although rectifier reboiler E1 is used more herein; a rectification column T1; a finished product take-off pump P1; heat exchanger E3; a finished condenser E4; finished product tanks V1, V2; overhead condenser E2; phase separator V3, etc., but does not exclude the possibility of using other terms. These terms are used merely to more conveniently describe and explain the nature of the present invention; they are to be construed as being without limitation to any additional limitations that may be imposed by the spirit of the present invention.

Claims (10)

1. The utility model provides a process equipment of energy-conserving technology of n-propyl acetate, includes rectifying column (T1), its characterized in that, the liquid phase exit linkage of rectifying column (T1) has finished product to extract pump (P1), finished product extract pump (P1) connect in finished product groove (V1, V2), the gaseous phase exit linkage of rectifying column (T1) is in overhead condenser (E2), overhead condenser (E2) connect in phase splitter (V3), just the phase splitting exit linkage of phase splitter (V3) is in the reflux mouth of outside extraction equipment and rectifying column (T1).
2. The process equipment for the energy-saving process of n-propyl acetate according to claim 1, wherein a heat exchanger (E3) is connected between the finished product extraction pump (P1) and the finished product tank (V1, V2), and the heat exchanger (E3) is simultaneously positioned between the phase separator (V3) and the rectifying tower (T1) for heat exchange between the finished ester and the reflux component.
3. The process equipment for n-propyl acetate energy-saving process according to claim 2, characterized in that a finished product condenser (E4) is connected between the heat exchanger (E3) and the finished product tank (V1, V2), and the heat exchanger (E3) is located between the finished product extraction pump (P1) and the finished product condenser (E4).
4. The n-propyl acetate energy saving process equipment according to claim 3, wherein the liquid phase outlet of the rectification column (T1) is simultaneously connected to a rectification reboiler (E1).
5. An energy-saving process for n-propyl acetate is characterized in that the rectification temperature is controlled in a rectifying tower (T1), so that water and n-propanol in crude ester are in a gas phase, n-propyl acetate is in a liquid phase, the gas phase is conveyed to a tower top condenser (E2) from a gas phase outlet of the rectifying tower (T1), a part of condensed mixed solution is extracted after phase separation in a phase separator (V3), a part of condensed mixed solution is refluxed to the rectifying tower (T1), and the liquid phase is conveyed to finished product tanks (V1 and V2) from a liquid phase outlet of the rectifying tower (T1) through a finished product extraction pump (P1).
6. The energy-saving process of n-propyl acetate according to claim 5, wherein the liquid phase is extracted to the heat exchanger (E3) by a finished product extraction pump (P1) and then enters the finished product tanks (V1, V2), and the reflux component of the mixed liquid which is refluxed to the rectifying tower (T1) and the liquid phase are refluxed to the rectifying tower (T1) after exchanging heat in the heat exchanger (E3).
7. The energy-saving process for n-propyl acetate according to claim 6, wherein the liquid phase after heat exchange is further condensed by a finished product condenser (E4) and then sent to a finished product tank (V1, V2).
8. The energy-saving process for n-propyl acetate as claimed in claim 7, wherein the rectification temperature of the rectification column (T1) is controlled to be between 100 ℃ and 101 ℃ during the rectification.
9. The energy-saving process for n-propyl acetate according to claim 8, wherein the liquid phase outlet is located at the bottom of the rectification column (T1) and the gas phase outlet is located at the top of the rectification column (T1) during the rectification, and before the finished ester is extracted, the liquid phase outlet flows back to the rectification reboiler (E1) to provide vaporization heat from the rectification reboiler (E1).
10. The energy-saving process of n-propyl acetate according to claim 9, wherein the upper components in the phase separator (V3) are refluxed to the rectifying column (T1), and the lower components are extracted; or the upper layer component is refluxed to the rectifying tower (T1), and the lower layer component is partially extracted and partially refluxed.
CN202010703617.5A 2020-07-21 2020-07-21 Energy-saving process and process equipment for n-propyl acetate Pending CN111807959A (en)

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CN202010703617.5A CN111807959A (en) 2020-07-21 2020-07-21 Energy-saving process and process equipment for n-propyl acetate

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112374967A (en) * 2020-11-06 2021-02-19 杭州新德环保科技有限公司 System and method for recovering ethanol from organic waste liquid

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CN101362692A (en) * 2008-09-24 2009-02-11 中国石油大学(华东) Technology method for producing isopropyl trifluoroacetate and apparatus
CN103214367A (en) * 2013-05-09 2013-07-24 江苏瑞佳化学有限公司 Continuous production device and method for isopropyl acetate
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Publication number Priority date Publication date Assignee Title
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Application publication date: 20201023