CN106187765B - Acetone, water separation equipment in a kind of two tower of rectifying removing vinyl acetate - Google Patents

Acetone, water separation equipment in a kind of two tower of rectifying removing vinyl acetate Download PDF

Info

Publication number
CN106187765B
CN106187765B CN201610553472.9A CN201610553472A CN106187765B CN 106187765 B CN106187765 B CN 106187765B CN 201610553472 A CN201610553472 A CN 201610553472A CN 106187765 B CN106187765 B CN 106187765B
Authority
CN
China
Prior art keywords
slot
water
tower
vinyl acetate
rectifying
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
Application number
CN201610553472.9A
Other languages
Chinese (zh)
Other versions
CN106187765A (en
Inventor
张仁文
刘永旺
徐小明
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sinopec Great Wall Energy Chemical Ningxia Co Ltd
Original Assignee
Sinopec Great Wall Energy Chemical Ningxia Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Sinopec Great Wall Energy Chemical Ningxia Co Ltd filed Critical Sinopec Great Wall Energy Chemical Ningxia Co Ltd
Priority to CN201610553472.9A priority Critical patent/CN106187765B/en
Publication of CN106187765A publication Critical patent/CN106187765A/en
Application granted granted Critical
Publication of CN106187765B publication Critical patent/CN106187765B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/141Fractional distillation or use of a fractionation or rectification column where at least one distillation column contains at least one dividing wall
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

A kind of removing of two tower of vinyl acetate rectifying acetone, water separation equipment, belong to the separating-purifying apparatus field of vinyl acetate, the equipment includes Second distillation column, segregator, complete condenser and cooler, slot is distillated using hierarchical design, the tower top of two tower of vinyl acetate rectifying must have the condenser of enough heat exchange areas to provide refrigeration duty, exhaust temperature is controlled, while ensuring that enough regurgitant volumes control the acetic acid content distillated.Tower top, which distillates slot, must enough residence times, guarantee the layering of vinyl acetate and water, and the water content in reflux is allowed to control below 1%.Lower aqueous by distillating slot drains to control the layering interfaces for distillating slot.The present invention solves the problems, such as that vinyl acetate product Zhong Shui and total aldehyde are exceeded in traditional handicraft, make vinyl acetate product reach domestic and international advanced level, have widened the application range of product.

Description

Acetone, water separation equipment in a kind of two tower of rectifying removing vinyl acetate
Technical field
The technology of the present invention belongs to a kind of removing vinegar of two tower of purification technique field more particularly to rectifying of vinyl acetate Acetone, water separation equipment in sour ethylene.
Background technique
Vinyl acetate (VAC) is a kind of common chemical intermediate, can manufacture adhesive, cream by solution or emulsion polymerization Agent, coating, cement additive, food product packing film, cosmetic additive agent, chewing gum base etc..Contain ethylene in its molecule Base, may be polymerized reaction, and polymerizate polyvinyl acetate (PVAC) is the raw material for preparing polyvinyl alcohol (PVA).Acetic acid second A large amount of impurity can be generated in alkene production process, such as acetaldehyde, acetone, crotonaldehyde, water will affect polymerization reaction, also will affect The degree of staining of finished product.The impurity content exceeding indexs such as acetaldehyde, acetone in vinyl acetate, directly affect product food product packing film, The purposes of cosmetics, chewing gum base etc. is promoted.
The existing thick vinyl acetate of synthesis is in rectification and purification to product vinyl acetate, because two tower of rectifying distillates slot water segregator The reasons such as smaller and segregator heat exchange area deficiency remove acetaldehyde list impurity composition when causing two tower of rectifying that can only meet underload Ability, cannot achieve removing acetone and water purpose.When production, the material water content that two tower reactor of rectifying goes out is up to 1.2%, always Aldehyde (including acetaldehyde, acetone, crotonaldehyde) content is up to 0.031%.The thick vinyl acetate of high impurity enters rear system, influences acetic acid The quality of ethylene product, is unable to meet production requirement and the market demand.
Summary of the invention
In order to reduce the impurity content in product, it is necessary to increase the ability of the removing water and total aldehyde impurity of two tower of rectifying, control The water content of tower reactor processed is 0.2% hereinafter, total aldehyde content is less than 0.02%.
The purpose of the present invention is for the thick vinyl acetate of existing synthesis existing for the rectification and purification to product vinyl acetate not Foot place provides a kind of removing of two tower of rectifying acetone, water separation equipment, the light component in the charging of smart vinyl acetate is isolated It goes, can prepare that impurity content is few using this method, and the VAC product of purity is high.
Realize that the technical solution of the object of the invention is such that acetone, water in a kind of removing vinyl acetate of two tower of rectifying Separation equipment.The equipment includes Second distillation column, segregator, complete condenser, cooler, distillates slot and tower reactor heater, above-mentioned each Equipment is connected.Segregator, complete condenser and cooler combined operating distillate slot using hierarchical design, and tower top distillates slot in lower liquid pipe The partition that height is 0.7 meter is provided between outlet tube, upper oil phase flows back by partition as two tower of rectifying, and water phase is concentrated In distillating slot water collector, by extraction pipe extraction, achieve the purpose that water removal.It synthesizes thick vinyl acetate and gives rectifying two towers from feed inlet Charging, for two tower of rectifying using 0.6mpa steam and bottom heater as heat source, top gaseous phase passes through segregator, complete condenser and cooling After device is cooling, acetaldehyde, acetone, water impurity are produced from light component extraction pipe, liquid, which enters, after segregator and complete condenser cooling distillates Slot is distillating the layering passed through partition in slot and distillate slot water collector realization vinyl acetate and water, and vinyl acetate is as rectifying two The reflux of tower, the extraction part water management for distillating slot water collector distillate the layering interfaces of slot.
The tower top of two tower of vinyl acetate rectifying must have the condenser of enough heat exchange areas to provide refrigeration duty, control tail Temperature degree ensures that enough regurgitant volumes control the acetic acid content distillated at 62.5 ± 1 DEG C.Tower top, which distillates slot, to be had Enough residence times guarantee the layering of vinyl acetate and water, and the water content in reflux is allowed to control below 1%.By distillating slot Lower aqueous drain to control the layering interfaces for distillating slot.
The heat exchange area of two column overhead segregator of rectifying is increased to 811.9 ㎡, while segregator by 133.2 ㎡ by the present invention Cooling water pipe diameter increases to DN350 by DN150, to greatly improve the heat transfer effect of segregator.Simultaneously by water segregator Length increases to 2.5 meters, and the above structure transformation for distillating slot increases the stratification time of vinyl acetate and water, can will flow back In water be removed to 1% or less.It can guarantee tower reactor by increasing the quantity of steam of tower reactor heater by above-mentioned two tower of variation rectifying Water content control is 0.2% hereinafter, two column overhead of rectifying distillates slot control tower with what is be transformed by the segregator of enough heat exchange areas The total aldehyde content of kettle is less than 0.02%.
The present invention has following remarkable result: after applying the present invention, the water outlet of two tower reactor of rectifying and total aldehyde content are lower, acetic acid Ethylene product water content and light component content reach high-class product index, produce good economic benefit, have widened product Application range opens market for the sale of product.
Detailed description of the invention
Fig. 1 is present device and components installation, attachment structure schematic diagram.
In figure: 1- Second distillation column, 2- segregator, 3- complete condenser, 4- cooler, 5- distillate slot, 6- tower reactor heater, 7- Feed inlet, 8- partition, 9- light component extraction pipe, 10- extraction pipe, 11- condenser lower night, 12- distillate slot oil phase, and 13- distillates slot Water collector, bis- tower reactor of 14- go out.
Specific embodiment
A specific embodiment of the invention combination attached drawing is illustrated, but the description of the invention is not limited to that.
A kind of removing of two tower of rectifying acetone, water separation equipment, which includes Second distillation column 1, segregator 2, complete condenser 3, cooler 4, distillate slot 5 and tower reactor heater 6, above-mentioned each equipment is connected.Segregator 2, complete condenser 3 combine fortune with cooler 4 Row distillates slot 5 using hierarchical design, and tower top distillates slot and is provided with the partition that height is 0.7 meter between lower liquid pipe and outlet tube 8, upper oil phase flows back by partition 8 as two tower of rectifying, and water phase, which concentrates on, distillates slot water collector 13, adopts by producing pipe 10 Out, achieve the purpose that water removal.Tower top light component (acetaldehyde, acetone) etc. is distillated by light component extraction pipe 9, realizes the de- of light component It removes.
Synthesize thick vinyl acetate (vinyl acetate 39%-42%, acetic acid 58%-61%, acetaldehyde 1.04%, acetone 0.02%) from into Material mouth 7 is fed to two tower of rectifying, and two tower of rectifying is using 0.6mpa steam and bottom heater 6 as heat source, and top gaseous phase is through excessive After condenser 2, complete condenser 3 and cooler 4 are cooling, from impurity such as cooler outlet extraction acetaldehyde, acetone, water.Segregator 2 is coagulated with complete Liquid, which enters, after device 3 is cooling distillates slot 5, distillates slot water collector by the partition 8 of height 0.7m and 2.5m long distillating in slot 5 13 realize that the layering of vinyl acetate and water, reflux of the vinyl acetate as two tower of rectifying distillate the extraction part of slot water collector 13 Water management distillates the layering interfaces of slot 5.Two tower reactor of rectifying goes out 14 extraction water contents lower than 0.2%, and total aldehyde is lower than 0.02% acetic acid Ethylene raw is used for downstream purified product vinyl acetate, guarantees that the water content of product vinyl acetate and total aldehyde content reach excellent Product requirement, to meet the market demand.

Claims (2)

1. a kind of two tower of rectifying removes acetone, water separation equipment, it is characterised in that the equipment includes Second distillation column (1), fractional condensation Device (2), cooler (4), distillates slot (5) and tower reactor heater (6) at complete condenser (3), and above-mentioned each equipment is connected, segregator (2), Complete condenser (3) and cooler (4) combined operating distillate slot (5) using hierarchical design, distillate slot (5) in lower liquid pipe and outlet tube Between to be provided with height be 0.7 meter of partition (8), upper oil phase as the reflux of two tower of rectifying, is removed by partition (8) in order to reach The purpose of water, water phase, which concentrates on, distillates slot water collector (13) by extraction pipe (10) extraction;Thick vinyl acetate is synthesized from feed inlet (7) it is fed to two tower of rectifying, two tower of rectifying is using 0.6mpa steam and bottom heater (6) as heat source, and top gaseous phase is through excessive After condenser (2), complete condenser (3) and cooler (4) are cooling, pipe (9) is produced from light component and produces acetaldehyde, acetone, water impurity, fractional condensation Liquid, which enters, after device (2) and complete condenser (3) are cooling distillates slot (5), catchments distillating to pass through partition (8) in slot (5) and distillate slot Device (13) realizes that the layering of vinyl acetate and water, reflux of the vinyl acetate as two tower of rectifying distillate adopting for slot water collector (13) Part water management distillates the layering interfaces of slot (5) out;The heat exchange area of two column overhead segregator (2) of rectifying increases to 811.9 ㎡, while segregator cooling water pipe diameter increases to DN350.
2. removing acetone according to claim 1, water separation equipment, which is characterized in that described distillates slot water collector (13) length is 2.5m.
CN201610553472.9A 2016-07-14 2016-07-14 Acetone, water separation equipment in a kind of two tower of rectifying removing vinyl acetate Active CN106187765B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610553472.9A CN106187765B (en) 2016-07-14 2016-07-14 Acetone, water separation equipment in a kind of two tower of rectifying removing vinyl acetate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610553472.9A CN106187765B (en) 2016-07-14 2016-07-14 Acetone, water separation equipment in a kind of two tower of rectifying removing vinyl acetate

Publications (2)

Publication Number Publication Date
CN106187765A CN106187765A (en) 2016-12-07
CN106187765B true CN106187765B (en) 2019-01-11

Family

ID=57476190

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610553472.9A Active CN106187765B (en) 2016-07-14 2016-07-14 Acetone, water separation equipment in a kind of two tower of rectifying removing vinyl acetate

Country Status (1)

Country Link
CN (1) CN106187765B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108958026B (en) * 2017-05-27 2021-07-27 蓝星(北京)技术中心有限公司 Optimized control method and system for heavy component separation system in chemical production

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1699326A (en) * 2004-05-20 2005-11-23 中国石化上海石油化工股份有限公司 Process for refining vinyl acetate crude products
CN104030921A (en) * 2013-07-05 2014-09-10 中石化上海工程有限公司 Method for separating vinyl acetate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1699326A (en) * 2004-05-20 2005-11-23 中国石化上海石油化工股份有限公司 Process for refining vinyl acetate crude products
CN104030921A (en) * 2013-07-05 2014-09-10 中石化上海工程有限公司 Method for separating vinyl acetate

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
改进精馏NQ206冷凝器;夏世伟 等;《设备管理与维修》;20131231(第7期);第67页

Also Published As

Publication number Publication date
CN106187765A (en) 2016-12-07

Similar Documents

Publication Publication Date Title
CN101153257B (en) Five-tower two-grade difference pressure distillation equipment for senior edible ethanol and technique thereof
CN105348098B (en) Method for rectifying and separating methyl formate, methanol and water by intermittent reaction
CN105344124B (en) Double smart tower quadruple effect top grade alcohol distillation method and apparatus for producing alcohol
CN106187765B (en) Acetone, water separation equipment in a kind of two tower of rectifying removing vinyl acetate
CN105396315A (en) Ethyl vanillin rectification device
CN203200253U (en) System used for brandy or fruit wine forced reflux distillation
CN101391153A (en) Double-kettle batch extraction rectification device and method for separating ethanol-water azeotropic system
CN110724025B (en) Device and method for preparing styrene by dehydrating phenethyl alcohol
CN212655719U (en) N-propyl acetate production system capable of recycling in grading manner
CN204303239U (en) A kind ofly promote the chemical experiment device that Synthesis Diethyl ether reaction forward is carried out
CN105272815A (en) Method for extracting methylnaphthalene in C10 aromatics
CN104447267B (en) A kind of Separation of Benzene ethyl ketone, method of alpha-phenyl ethyl alcohol from 1-Phenylethanone. and alpha-phenyl ethyl alcohol mixture
CN103706136A (en) Double-rectifying-tower series separation and purification method for recovery of methyl tert-butyl ether-tetrahydrofuran in waste liquid in statins synthesis process
CN107162909B (en) A kind of thermal coupling methods and device that vinyl acetate is refined
CN206621817U (en) A kind of energy-conserving and environment-protective chlorophenesic acid continuous rectification system
CN203754414U (en) System for producing hydrogen chloride gas by hydrochloric acid analysis
CN113233982B (en) Device and method for obtaining high-purity methyl salicylate through continuous rectification purification
CN205576087U (en) Cooling device in wine processing
CN104803828B (en) Device and method for improving 1,4-butanediol yield
CN204840984U (en) Rectifying device
CN106316793A (en) Alcohol preparing device and method based on the double rectification column and six-column and four-effect distillation
CN103755532B (en) Chloromethyl ether continuous production system and production process utilizing same
CN208287511U (en) A kind of N- acryloyl morpholine purifying plant
CN111807959A (en) Energy-saving process and process equipment for n-propyl acetate
CN206940766U (en) The production equipment of methyl chloroacetate

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant