CN105439853A - Ethyl acetate continuous esterification apparatus - Google Patents

Ethyl acetate continuous esterification apparatus Download PDF

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Publication number
CN105439853A
CN105439853A CN201610017503.9A CN201610017503A CN105439853A CN 105439853 A CN105439853 A CN 105439853A CN 201610017503 A CN201610017503 A CN 201610017503A CN 105439853 A CN105439853 A CN 105439853A
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CN
China
Prior art keywords
tower
esterification
ethyl acetate
column
equipment
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
CN201610017503.9A
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Chinese (zh)
Inventor
徐大鹏
冯英
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GUANGXI XINTIANDE ENERGY CO Ltd
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GUANGXI XINTIANDE ENERGY 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 GUANGXI XINTIANDE ENERGY CO Ltd filed Critical GUANGXI XINTIANDE ENERGY CO Ltd
Priority to CN201610017503.9A priority Critical patent/CN105439853A/en
Publication of CN105439853A publication Critical patent/CN105439853A/en
Pending legal-status Critical Current

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Classifications

    • 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

Abstract

The invention belongs to the field of chemosynthesis apparatuses and more particularly relates to an ethyl acetate continuous esterification apparatus. The apparatus is formed by sequentially connecting a raw material mixer 1, a preheater 2, an esterification column 3, a separating column 4, a proportioning mixer 5, a decanter 7 and a drying column 6 through a pipeline, wherein the bottom of the raw material mixer 1 is connected with the middle part of the esterification column 3 through the preheater 2; the top of the esterification column 3 is connected with the middle part of the separating column 4 through the decanter 7; the top of the separating column 4 is connected with the top of the proportioning mixer 5; the bottom of the proportioning mixer 5 is connected with the middle part of the drying column 6 through the decanter 7. The apparatus disclosed by the invention is used for a continuous reaction for preparing ethyl acetate, the product conversion rate can be increased to 93% to 99%, the energy consumption is greatly reduced, and the performance indexes of the ethyl acetate product are improved.

Description

Ethyl acetate continuous esterification equipment
Technical field
The invention belongs to chemosynthesis apparatus field, be specifically related to ethyl acetate continuous esterification equipment.
Background technology
Ethyl acetate (ethylacetat), has another name called vinyl acetic monomer, and outward appearance is the fruity colourless transparent liquid of tool, is one of most widely used fatty acid ester, has excellent solubility property, is a kind of volatile, industrial solvent that solvability is fabulous.Be widely used in chemistry, food medicine, weaving and automotive industry,
Industrial ethyl acetate main production process has following several in the world at present: acid esterification method, acetaldehyde condensation method, Addition on ethylene method and alcohol dehydrogenase method etc.But at present esterification process comparative maturity, reliable, production cost is relatively low, but the nitration mixture formed due to catalyzer and acetic acid to equipment corrosion seriously, and therefore maintenance cost is higher.It is few that acetaldehyde condensation method has raw material consumption, and technological process is simple, the advantage little to equipment corrosion, energy consumption is low, " three wastes " quantity discharged is few, but its throughput is not as esterification process, is therefore difficult to scale operation.Utilize ethene direct addition method product yield and selectivity all higher, but investment also higher.Ethanol with one-step method is the novel process that development in recent years is got up, and use this handicraft product yield high, little to equipment corrosion, advantage of lower cost, does not produce acid-bearing wastewater, and is conducive to scale operation.
Summary of the invention
The present invention is by research continuous esterification technology and technique, improve the transformation efficiency of the reactant such as ethanol, acetic acid, improve the quality of products and yield, the defects such as the side reaction brought is many, acid solution quantity discharged is large, equipment is perishable, energy consumption is high are reacted for traditional direct esterification, a kind of ethyl acetate continuous esterification equipment is provided, alleviates the manipulation strength of the processes such as later separation concentrate, refining, low vinegar recovery, waste water reclamation.
The solution of the present invention is by realizing like this: a kind of ethyl acetate continuous esterification equipment, this equipment is connected to form by pipeline successively by material mixer 1, preheater 2, esterification column 3, knockout tower 4, proportioning mixing tank 5, decanting vessel 7, drying tower 6, be connected by preheater 2 with in the middle part of esterification column 3 bottom material mixer 1, esterification column 3 tower top is connected by decanting vessel 7 with in the middle part of knockout tower 4, knockout tower 4 top is connected with proportioning mixing tank 5 top, is connected bottom proportioning mixing tank 5 with in the middle part of drying tower 6 by decanting vessel 7.
As further restriction of the present invention, in this equipment at the bottom of knockout tower 4 tower with at the bottom of esterification column 3 tower between have to reflux and be connected.
As further restriction of the present invention, in this equipment at the bottom of proportioning mixing tank 5 tower with at the bottom of knockout tower 3 tower between have to reflux and be connected.
As further restriction of the present invention, bottom esterification column 3, be provided with heavy constituent refuse discharge port.
The technical process that the present invention realizes is: continuous esterification method adopts acetic acid, the ethanol of 95% and the sulfuric acid of a small amount of 96% to mix in material mixer, after preheater preheats, enters esterification column and carries out esterification.The temperature of esterification tower top is 80 DEG C.Heavy constituent refuse in reaction mixture refluxes out bottom esterification column, and a part of distillate enters knockout tower from esterification column, distillate consist of 70% ethanol, 20% ester and 10% water.Knockout tower part distillate is back to esterification column from bottom, and tower top ternary azeotrope (83% ethyl acetate, 9% ethanol, 8% water) out enters proportioning mixing tank from knockout tower, after mixing, enters in decanting vessel and carries out layering in proportioning mixing tank with the water of equivalent.Be aqueous phase bottom decanting vessel between proportioning mixing tank and knockout tower, containing a small amount of alcohol and ester, be sent back to the bottom of knockout tower; Decanting vessel top between proportioning mixing tank and knockout tower is the ethyl acetate containing 93%, also containing the water of 5% and the alcohol mixture of 2%.Decanting vessel tower top material between proportioning mixing tank and knockout tower is sent to drying tower, and in drying tower, moisture is distilled out, and alcohol continues to be sent to esterification column and reacts.Drying tower bottoms material is the ethyl acetate of content 95% ~ 99%.Materials at bottom of tower can obtain more highly purified product as product stock or further refining.
The present invention possesses following good result: ethyl acetate serialization equipment is the upgrading of system thermal comprehensive utilization technique under novel process, adopt serialization equipment of the present invention to prepare ethyl acetate and can improve conversion rate of products to 93 ~ 99%, reduce significantly energy consumption, improve the performance index of ethyl acetate product, product purity >=99.8% obtained, acid content≤0.003%, water-content≤0.04%, is better than GB/T3728-2007 premium grads.
Figure of description
Fig. 1. ethyl acetate continuous esterification equipment of the present invention.Identify in figure: 1-material mixer, 2-preheater, 3-esterification column, 4-knockout tower, 5-proportioning mixing tank, 6-drying tower, 7-decanting vessel.
Embodiment
Describe ethyl acetate continuous esterification equipment of the present invention below in conjunction with embodiment and accompanying drawing, these descriptions are not be further limited content of the present invention.
Embodiment
As shown in Figure 1, ethyl acetate continuous esterification equipment of the present invention is connected to form by pipeline successively by material mixer 1, preheater 2, esterification column 3, knockout tower 4, proportioning mixing tank 5, decanting vessel 7, drying tower 6, be connected by preheater 2 with in the middle part of esterification column 3 bottom material mixer 1, esterification column 3 tower top is connected by decanting vessel 7 with in the middle part of knockout tower 4, knockout tower 4 top is connected with proportioning mixing tank 5 top, is connected bottom proportioning mixing tank 5 with in the middle part of drying tower 6 by decanting vessel 7.In this equipment at the bottom of knockout tower 4 tower with at the bottom of esterification column 3 tower between have to reflux and be connected.In this equipment at the bottom of proportioning mixing tank 5 tower with at the bottom of knockout tower 3 tower between have to reflux and be connected.Heavy constituent refuse discharge port is provided with bottom esterification column 3.
Use procedure, adopts acetic acid, the ethanol of 95% and the sulfuric acid of a small amount of 96% to mix in material mixer, after preheater preheats, enters esterification column and carry out esterification.The temperature of esterification tower top is 80 DEG C.Heavy constituent refuse in reaction mixture refluxes out bottom esterification column, and a part of distillate enters knockout tower from esterification column, distillate consist of 70% ethanol, 20% ester and 10% water.Knockout tower part distillate is back to esterification column from bottom, and tower top ternary azeotrope (83% ethyl acetate, 9% ethanol, 8% water) out enters proportioning mixing tank from knockout tower, after mixing, enters in decanting vessel and carries out layering in proportioning mixing tank with the water of equivalent.Be aqueous phase bottom decanting vessel between proportioning mixing tank and knockout tower, containing a small amount of alcohol and ester, be sent back to the bottom of knockout tower; Decanting vessel top between proportioning mixing tank and knockout tower is the ethyl acetate containing 93%, also containing the water of 5% and the alcohol mixture of 2%.Decanting vessel tower top material between proportioning mixing tank and knockout tower is sent to drying tower, and in drying tower, moisture is distilled out, and alcohol continues to be sent to esterification column and reacts.Drying tower bottoms material is the ethyl acetate of content 95% ~ 99%.Materials at bottom of tower can obtain more highly purified product as product stock or further refining.
Adopt serialization equipment of the present invention to prepare ethyl acetate and can improve conversion rate of products to 93 ~ 99%, reduce significantly energy consumption, improve the performance index of ethyl acetate product, product purity >=99.8% obtained, acid content≤0.003%, water-content≤0.04%, is better than GB/T3728-2007 premium grads.
The above embodiment of the present invention scheme is only can not limit the present invention to explanation of the present invention, indicate in claim that present device is formed and mode of connection, and the scope of parameter of the present invention is not pointed out in above-mentioned explanation, therefore, any change in the implication suitable with claims of the present invention and scope, is all considered to be and is included in the scope of claims.

Claims (4)

1. an ethyl acetate continuous esterification equipment, it is characterized in that, this equipment is by material mixer (1), preheater (2), esterification column (3), knockout tower (4), proportioning mixing tank (5), decanting vessel (7), drying tower (6) is connected to form successively by pipeline, material mixer (1) bottom is connected by preheater (2) with esterification column (3) middle part, esterification column (3) tower top is connected by decanting vessel (7) with knockout tower (4) middle part, knockout tower (4) top is connected with proportioning mixing tank (5) top, proportioning mixing tank (5) bottom is connected by decanting vessel (7) with drying tower (6) middle part.
2. ethyl acetate continuous esterification equipment according to claim 1, is characterized in that, in this equipment at the bottom of knockout tower (4) tower with at the bottom of esterification column (3) tower between have to reflux and be connected.
3. ethyl acetate continuous esterification equipment according to claim 1, is characterized in that, in this equipment at the bottom of proportioning mixing tank (5) tower with at the bottom of knockout tower (3) tower between have to reflux and be connected.
4. ethyl acetate continuous esterification equipment according to claim 1, is characterized in that, esterification column (3) bottom is provided with heavy constituent refuse discharge port.
CN201610017503.9A 2016-01-12 2016-01-12 Ethyl acetate continuous esterification apparatus Pending CN105439853A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610017503.9A CN105439853A (en) 2016-01-12 2016-01-12 Ethyl acetate continuous esterification apparatus

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610017503.9A CN105439853A (en) 2016-01-12 2016-01-12 Ethyl acetate continuous esterification apparatus

Publications (1)

Publication Number Publication Date
CN105439853A true CN105439853A (en) 2016-03-30

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Application Number Title Priority Date Filing Date
CN201610017503.9A Pending CN105439853A (en) 2016-01-12 2016-01-12 Ethyl acetate continuous esterification apparatus

Country Status (1)

Country Link
CN (1) CN105439853A (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1827581A (en) * 2006-04-07 2006-09-06 华南理工大学 Process and equipment for preparing ethyl acetate and butyl acetate
CN101486641A (en) * 2009-02-16 2009-07-22 江门谦信化工发展有限公司 Industrialized production method of ethyl acetate and production apparatus thereof
CN101735045A (en) * 2009-12-18 2010-06-16 中山大学 Method for producing ethyl acetate by using entrainer

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1827581A (en) * 2006-04-07 2006-09-06 华南理工大学 Process and equipment for preparing ethyl acetate and butyl acetate
CN101486641A (en) * 2009-02-16 2009-07-22 江门谦信化工发展有限公司 Industrialized production method of ethyl acetate and production apparatus thereof
CN101735045A (en) * 2009-12-18 2010-06-16 中山大学 Method for producing ethyl acetate by using entrainer

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
梅允福等: "乙酸乙酯合成技术进展", 《广州化工》 *

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Application publication date: 20160330