WO2020083118A1 - 一种加压酯化合成后快速提取精纯醋酸乙酯的系统及工艺 - Google Patents

一种加压酯化合成后快速提取精纯醋酸乙酯的系统及工艺 Download PDF

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WO2020083118A1
WO2020083118A1 PCT/CN2019/112044 CN2019112044W WO2020083118A1 WO 2020083118 A1 WO2020083118 A1 WO 2020083118A1 CN 2019112044 W CN2019112044 W CN 2019112044W WO 2020083118 A1 WO2020083118 A1 WO 2020083118A1
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WIPO (PCT)
Prior art keywords
tower
refining
ethyl acetate
layerer
reaction rectification
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PCT/CN2019/112044
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English (en)
French (fr)
Chinese (zh)
Inventor
刘强
李志远
郭向东
张玉娟
于超
包磊磊
张宇
陈明
梁群
刘成刚
杨文攀
常亮
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兖矿鲁南化工有限公司
兖矿集团有限公司
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Priority to KR1020217002172A priority Critical patent/KR102484021B1/ko
Publication of WO2020083118A1 publication Critical patent/WO2020083118A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/48—Separation; Purification; Stabilisation; Use of additives
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
    • C07C69/02—Esters of acyclic saturated monocarboxylic acids having the carboxyl group bound to an acyclic carbon atom or to hydrogen
    • C07C69/12—Acetic acid esters
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Definitions

  • the invention relates to the field of acetic acid synthesis, in particular to a system and process for rapid extraction of pure ethyl acetate after pressure esterification synthesis.
  • Ethyl acetate also known as ethyl acetate, is an important downstream product of acetic acid, with excellent solubility and fast drying. In the industry, it is mainly used as a solvent for the production of paints (paints, nuclear enamels), binders, ethyl cellulose, artificial leather, linoleum colorants, and artificial fibers. It can also be used as a binder for the production of printing inks, artificial pearls, etc. . It is used as an extractant in the production of medicines, organic acid products, etc. In addition, it can also be used as a raw material for the production of pineapple, banana, strawberry and other fruit flavor nuclear whiskey, cream and other spices. Ethyl acetate has excellent dissolving power, can be used as a quick-drying solvent, and is widely used in the chemical industry and the pharmaceutical industry.
  • Acetic acid esterification is the most common production method of ethyl acetate. In the presence of a catalyst, acetic acid and ethanol undergo an esterification reaction to produce ethyl acetate.
  • the ethyl acetate in China is mainly produced by the acetate esterification method, and most of the five towers are used.
  • the rectification process has many equipments and high energy consumption; some ethyl acetate production processes use excessive ethanol to make the acetic acid react as completely as possible to omit the deacidification tower, but the crude ester prepared by this method contains a large amount of The low content of ethanol and ethyl acetate leads to a low purification efficiency of ethyl acetate, resulting in the problem of long production cycle of ethyl acetate.
  • the production process of ethyl acetate is to mix acetic acid, ethanol and catalyst to react in the esterification kettle, and then send the reacted materials to a rectification tower for rectification.
  • the object of the present invention is to provide a system and process for rapid extraction of pure ethyl acetate after pressure esterification synthesis.
  • a system for rapid extraction of pure ethyl acetate after pressurized esterification synthesis including a reactive rectification tower, a purification tower, a deacidification tower and a recovery tower, wherein the middle of the reactive rectification tower is connected to an acetic acid source and an ethanol source,
  • the top of the reaction rectification tower is connected to the inlet of the first collection tank through a cooler, and the first collection tank is also in communication with the first stratifier.
  • the top of the first stratifier is connected to the top of the reaction rectification tower and the The middle part of the refining tower is connected; the first layerer is connected with the desalinated water storage device, and the desalinated water is added to the first layerer;
  • the top of the refining tower is connected to the inlet of the cooler, the outlet of the cooler is connected to the second collection tank; the middle of the refining tower is connected to the inlet of the second layerer, and the outlet of the organic phase of the second layerer is connected to the refining tower, The bottom of the second layerer communicates with the recovery tower; the tower kettle of the refining tower communicates with the inlet of the deacidification tower;
  • the top of the deacidification tower is connected to the inlet of the third cooler, the outlet of the third cooler is connected to the third collection tank, and the third collection tank is connected to the finished product tank; the tower kettle of the deacidification tower is connected to the reaction rectification tower Connected.
  • desalinated water is water that removes or reduces the strong electrolyte that is easily removed to a certain degree, and the remaining salt content in the desalted water should be between 1-5mg / L
  • the substance can be used as an extractant to extract impurities such as light components and reaction by-products in the crude ester, and can also accelerate the replacement speed of the acetic acid content in the crude ester and increase the initial product qualification rate of the ethyl acetate unit during the initial operation.
  • the reactor of the reaction rectification tower is connected to the middle of the reaction rectification tower through a pump and a heat exchanger.
  • the acetic acid conveyed to the reaction rectification tower generally accumulates in the reactor of the reaction rectification tower.
  • the pump can transfer the acetic acid accumulated in the tower kettle to the reaction section of the reaction rectification tower after heating.
  • the acetic acid can be added again. Ensure the concentration of acetic acid in the reaction system, promote the conversion rate of ethanol, and increase the content of ethyl acetate.
  • repeated addition of acetic acid can ensure the utilization of acetic acid, prevent the waste of acetic acid, and further simplify the subsequent purification of ethyl acetate Process.
  • a fourth collection tank is connected to the top of the recovery tower.
  • the top of the recovery tower is connected to the reaction rectification tower through a cooler.
  • a process for rapid extraction of pure ethyl acetate after pressure esterification synthesis includes the following steps:
  • the preparation and purification process of ethyl acetate includes the steps of esterification-refining-deacidification-wastewater recovery. After the esterification is completed, the overhead material is cooled and sent to the first layerer for layering, which is added in the first layerer Demineralized water to extract impurities in the crude ester and promote the replacement rate of acetic acid in ethyl acetate.
  • the esterification specifically includes the following steps: after the ethanol and acetic acid are mixed, they enter the reaction rectification tower from the middle; Re-participate in the reaction; the azeotrope of ethyl acetate and water and part of the alcohol are distilled from the top of the reaction rectification tower, after cooling, they are transported by the pump to the first layerer, and the organic phase is collected from the top of the first layerer
  • the water is partly refluxed to the rectification tower, and the rest is heated and transported to the refining tower; the water phase is withdrawn from the bottom of the first layerer and transported to the recovery tower.
  • the working pressure in the reactive distillation column is 0.15-0.2 MPa, and the working temperature is 120-150 ° C.
  • the flow ratio of the material refluxed to the rectification tower and the material transported to the purification tower is 1.5-2.0: 1.
  • the molar ratio of ethanol to acetic acid during the esterification is 0.85-0.97: 1.
  • the refining specifically includes the following steps: the material from the esterification process enters the refining tower from the middle, the light components accumulate in the refining tower and distill out from the top of the tower, and the top-recovered materials are condensed and returned to the top of the refining tower;
  • the ethyl acetate is purified from the refining tower and transferred to the deacidification tower from the refining tower;
  • ethyl acetate is produced as an intermediate product from the bottom of the refining tower and sent to the deacidification tower. In order to further reduce system consumption and avoid material loss, it is collected from the middle of the refining tower. Part of the side-mining material is discharged into the second layerer for layering, the water phase sinks in the second layerer, and after preheating it is recovered to the recovery tower, and the organic phase is recycled to the refining tower.
  • the working pressure in the refining step is 0.15-0.23 MPa, and the working temperature is 110-116 ° C.
  • the working pressure of the deacidification step is 0.1-0.15 MPa, and the working temperature is 100-115 ° C.
  • the wastewater recovery step is 0.1-0.15 MPa, and the working temperature is 110-126 ° C.
  • the invention can rapidly improve the purity of ethyl acetate products, greatly shorten the driving time of the ethyl acetate device, and the driving time can be shortened by at least 8-10 hours at a time.
  • the acid content in ethyl acetate products can be reduced to below 30ppm, and the product purity can be stably controlled at above 99.9%.
  • the invention can be applied to most ethyl acetate production processes with pressure distillation.
  • FIG. 1 is a schematic structural diagram of the system of the present invention.
  • Reaction rectification tower 2. First layerer, 3. First collection tank, 4. Refining tower, 5. Second collection tank, 6. Second layerer, 7. Deacidification tower, 8. Third collection tank, 9. Recovery tower, 10. Fourth collection tank.
  • a system for rapid extraction of pure ethyl acetate after pressurized esterification synthesis includes a reaction rectification tower 1, a purification tower 4, a deacidification tower 7, and a recovery tower 9, wherein the reaction rectification tower
  • the middle part of 1 is connected with an acetic acid source and an ethanol source
  • the top of the reactive distillation column 1 is connected with the inlet of the first collection tank 3 through the first cooler
  • the first collection tank 3 is communicated with the first layerer 2
  • the top of the layer 2 is communicated with the top of the reaction rectification tower 1 and the middle of the refining tower 4 respectively
  • the column kettle of the reaction rectification tower 1 is connected to the middle of the reaction rectification tower 1 through a pump and a heat exchanger.
  • the top of the refining tower 4 is connected to the inlet of the second cooler, the outlet of the second cooler is connected to the second collecting tank 5, the second collecting pipe 5 communicates with the refining tower 4; the middle of the refining tower 4 is connected to the second layer
  • the inlet of the separator 6 is connected, the organic phase outlet of the second layerer 6 is connected to the refining tower 4, the bottom of the second layerer 6 is connected to the recovery tower 9; the tower kettle of the refining tower 4 and the deacidification tower 7 The entrance of is connected;
  • the top of the deacidification tower 7 is connected to the inlet of the third cooler, the outlet of the third cooler is connected to the third collection tank 8, and the third collection tank 8 is connected to the finished product tank;
  • the reactive distillation column 1 is in communication.
  • a fourth collection tank 10 is connected to the top of the recovery tower 9.
  • This set of ethyl acetate device adopts the production process of four-tower rectification.
  • the "esterification-refining-deacidification-wastewater recovery" esterification method produces the four-tower rectification process of ethyl acetate.
  • the whole process consists of reactive rectification process and refining process It consists of deacidification process and recovery process, with simple process and low energy consumption.
  • the new ethyl acetate production process can quickly improve product purity, reduce the content of acetic acid in the product, improve the market competitiveness of ethyl acetate products, and lay the foundation for other downstream products of acetic acid.
  • the reactive rectification process mainly includes: reactive rectification tower, reboiler, cooler, collection tank, delaminator, and reflux pump. After the ethanol and acetic acid are mixed, they enter the reaction rectification tower from the middle, and an equilibrium reaction occurs in the reaction rectification tower. The gaseous material enters the distillation section of the reaction rectification tower, and excess acetic acid accumulates at the bottom of the reaction rectification tower to participate in the reaction again.
  • the azeotrope of ethyl acetate and water and part of the alcohol are distilled from the top of the reaction rectification tower, and after cooling, they are transported by the pump to the rectification tower layerer.
  • the organic phase is taken from the top of the stratification device of the rectification tower, and part of it is refluxed to the rectification tower, and the rest is heated and sent to the refining tower, and the materials sent to the refining tower, ethyl acetate, ethanol and water each account for the mass percentage
  • the content is: ethyl acetate 85% ⁇ 92%, ethanol 2% ⁇ 5%, water 6% ⁇ 10%.
  • the aqueous phase is withdrawn from the bottom of the rectifier column layerer and sent to the recovery tower.
  • additional demineralized water is added in the first layer 2 of the rectification tower. This substance can be used as an extractant to extract the light components in the crude ester and the reaction vice Impurities such as products can accelerate the replacement rate of acetic acid in crude esters and increase the qualified rate of the initial product of the ethyl acetate unit.
  • the mass percentage of ethyl acetate in crude esters is increased from 87 to 91% to 89% ⁇ 93%, the purity of the obtained ethyl acetate product is above 99.9%, and the use of desalinated water can shorten the qualification rate of ethyl acetate products by 8 to 10 hours.
  • the mass percentage of acetic acid in the top of the reactive distillation column is 0.5% to 1.0%, and the content of acetic acid in the finished product of ethyl acetate requires 0.004% or less. Therefore, the repeated distillation replacement of the reactive distillation system is required.
  • the content of acetic acid in the overhead distillate drops to less than 0.01%, and then enters the refining tower as crude ester for refining. Therefore, the initial product qualification is slow.
  • the amount of desalinated water added at the initial start-up is 2 to 6 t / h, and the flow rate ratio to the top distillate is 0.1 to 0.3: 1.
  • Working pressure of reactive distillation tower 0.15 ⁇ 0.2MPa; operating temperature of reactive distillation tower: 120 ⁇ 150 °C.
  • the refining process mainly includes: refining tower, reboiler, cooler, collecting tank, layerer, and pump.
  • the material from the reactive distillation process enters the refining tower from the middle, and the light components accumulate in the refining tower and distill out from the top of the tower.
  • the top mining material is condensed and used as the reflux of the refining tower.
  • some light components can be taken out intermittently.
  • Ethyl acetate is purified in the stripping section of the refining tower and sent to the deacidification tower as an intermediate product from the tower kettle.
  • a part of the side mining material is taken from the middle of the tower and enters the refining tower layerer.
  • the water phase sinks and separates in the layerer of the refining tower, and enters the recovery tower through the feed preheater of the recovery tower.
  • the organic phase is recycled to the refinery column feed upstream of the condenser of the rectification column.
  • Working pressure of refining tower 0.15 ⁇ 0.23MPa; operating temperature of refining tower: 110 ⁇ 116 °C
  • Deacidification equipment including deacidification tower, reboiler, cooler, collection tank, production pump. After removing some light components and other impurities through the refining tower, the crude ester enters the deacidification tower. After being heated by the reboiler, the ethyl acetate product is taken from the top of the tower, cooled by the top cooler and sent to the finished tank area. The products at the bottom of the tower are pumped into the reaction rectification tower for recycling.
  • the working pressure of deacidification tower is 0.1 ⁇ 0.15MPa; the temperature of sensitive board of deacidification tower is 100 ⁇ 115 °C.
  • the recovery process mainly includes: recovery tower, reboiler, cooler, collection tank, and production pump.
  • the water containing organic matter from the rectifying tower layerer and the refining tower layerer enters the recovery tower. Ethanol and ethyl acetate are concentrated at the top of the tower. After cooling the overhead material, part of the material is sent to the reaction rectification tower for reaction. Qualified waste water after purification is taken from the recovery tower tower kettle and sent to sewage treatment.
  • Working pressure of recovery tower 0.1 ⁇ 0.15MPa; operation temperature of recovery tower: 110 ⁇ 126 °C
  • the tower described in the present invention is a rectification tower commonly used in the chemical industry.
  • the pump used in the present invention is a pump in a general sense, and it is a device for transferring liquid.
  • the reboiler used in the present invention is a device that uses saturated steam as a heating medium to heat materials.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
PCT/CN2019/112044 2018-10-25 2019-10-18 一种加压酯化合成后快速提取精纯醋酸乙酯的系统及工艺 WO2020083118A1 (zh)

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CN114163320A (zh) * 2021-12-17 2022-03-11 福建南平龙晟香精香料有限公司 一种龙涎酮中间体制备方法及其装置
CN115317949A (zh) * 2022-08-22 2022-11-11 宁波王龙科技股份有限公司 一种节能环保的稀醋酸提浓系统
CN115624778A (zh) * 2022-10-21 2023-01-20 泰兴金江化学工业有限公司 一种带有回收处理装置的醋酸乙酯蒸馏装置及其蒸馏方法
CN115845421A (zh) * 2022-12-19 2023-03-28 滨州黄海科学技术研究院有限公司 一种连续化分离全氟己酮的系统及方法

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CN109534997B (zh) * 2018-10-25 2019-08-30 兖矿鲁南化工有限公司 一种加压酯化合成后快速提取精纯醋酸乙酯的系统及工艺
CN114100176B (zh) * 2021-12-09 2022-12-09 江苏恒兴新材料科技股份有限公司 一种复合丁酸乙酯提纯塔和分离精制系统及其分离工艺

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Publication number Priority date Publication date Assignee Title
CN114163320A (zh) * 2021-12-17 2022-03-11 福建南平龙晟香精香料有限公司 一种龙涎酮中间体制备方法及其装置
CN114163320B (zh) * 2021-12-17 2023-12-12 福建南平龙晟香精香料有限公司 一种龙涎酮中间体制备方法及其装置
CN115317949A (zh) * 2022-08-22 2022-11-11 宁波王龙科技股份有限公司 一种节能环保的稀醋酸提浓系统
CN115317949B (zh) * 2022-08-22 2024-01-30 宁波王龙科技股份有限公司 一种节能环保的稀醋酸提浓系统
CN115624778A (zh) * 2022-10-21 2023-01-20 泰兴金江化学工业有限公司 一种带有回收处理装置的醋酸乙酯蒸馏装置及其蒸馏方法
CN115845421A (zh) * 2022-12-19 2023-03-28 滨州黄海科学技术研究院有限公司 一种连续化分离全氟己酮的系统及方法
CN115845421B (zh) * 2022-12-19 2023-06-30 滨州黄海科学技术研究院有限公司 一种连续化分离全氟己酮的系统及方法

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