WO2021017620A1 - 一种丁烯酮的连续萃取干燥装置和方法 - Google Patents

一种丁烯酮的连续萃取干燥装置和方法 Download PDF

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WO2021017620A1
WO2021017620A1 PCT/CN2020/093915 CN2020093915W WO2021017620A1 WO 2021017620 A1 WO2021017620 A1 WO 2021017620A1 CN 2020093915 W CN2020093915 W CN 2020093915W WO 2021017620 A1 WO2021017620 A1 WO 2021017620A1
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butenone
tower
water
extraction
extractant
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PCT/CN2020/093915
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English (en)
French (fr)
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王浩亮
刘智强
潘必文
苏珍莹
陈林锋
陈旭泽
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厦门金达威维生素有限公司
厦门金达威集团股份有限公司
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Publication of WO2021017620A1 publication Critical patent/WO2021017620A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78—Separation; Purification; Stabilisation; Use of additives
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78—Separation; Purification; Stabilisation; Use of additives
    • C07C45/80—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment

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  • the invention belongs to the field of drying, and specifically relates to a continuous extraction and drying device and method for water-containing butenone.
  • the traditional drying method of water-containing butenone is to use anhydrous calcium chloride, magnesium sulfate, magnesium carbonate, etc. as a desiccant, and achieve the purpose of drying by reversibly combining with water to form a hydrate.
  • a desiccant When the water-containing butenone flows through the filter, the moisture is adsorbed on the desiccant, which is suitable for the drying of trace moisture butenone;
  • One is to put the desiccant into the reaction kettle, stir and let it stand fully, extract the upper oil layer, and recycle the lower salt organic layer.
  • the traditional water-containing butenone drying process has the following problems: (1) solid waste or high-salt, high-COD wastewater is generated; (2) automatic control is not easy to achieve, and the operation is cumbersome; (3) there are many supporting equipment and the equipment is relatively large Large, low butenone recovery rate and low equipment utilization; (4) Strong labor and poor operating environment.
  • the purpose of the present invention is to overcome the defects in the prior art that using a desiccant to dry water-containing butenone has low butenone recovery rate and also produces solid waste or high-salt, high-COD wastewater, and to provide a butene A continuous extraction and drying device and method with high ketone recovery rate and no solid waste or high-salt, high-COD waste water in the whole process.
  • the present invention provides a continuous extraction and drying device for butenone, wherein the continuous extraction and drying device includes an extraction tower, a rectification tower, a condenser, a water separator, a reboiler, and an oil layer receiving tank;
  • the extraction column from top to bottom includes three parts: an oil layer standing section, a mixing section, and a water layer standing section, and the mixing section is provided with an upper feed port and a lower feed port, respectively, the rectification
  • the column from top to bottom includes two parts with water section and stripping section.
  • the outlet of the oil layer standing section of the extraction tower is connected with the material inlet of the rectification tower, and the top outlet of the rectification tower is connected with The material inlet of the condenser is in communication, the material outlet of the condenser is in communication with the material inlet of the water separation tank, the outlet of the bottom of the rectification tower is in cyclic communication with the reboiler and the other is in communication with the reboiler.
  • the oil layer is connected by the tank; or,
  • the extraction tower from top to bottom includes three parts: a water layer standing section, a mixing section, and an oil layer standing section, and the mixing section is provided with an upper feed port and a lower feed port, respectively, the rectification
  • the column from top to bottom includes two parts with water section and stripping section.
  • the outlet of the oil layer standing section of the extraction tower is connected with the material inlet of the rectification tower, and the top outlet of the rectification tower is connected with The material inlet of the condenser is in communication, the material outlet of the condenser material is in communication with the material inlet of the water separation tank, the outlet of the bottom of the rectification tower is in cyclic communication with the reboiler and the other
  • the oil layer is connected by the tank.
  • the extraction tower is a spray tower, a packed tower, a sieve tray or a rotating disk extraction tower.
  • the stationary section of the water layer of the extraction tower is controlled by an interface controller.
  • the rectification tower is a packed tower or a sieve tray.
  • the condenser is a shell-and-tube condenser, a winding condenser or a plate condenser.
  • the water separation tank is a standing tank with an interface controller.
  • the reboiler is a thermosiphon reboiler or a falling film reboiler.
  • the continuous extraction and drying device for butenone further includes an extraction oil layer receiving tank and an oil layer inlet on the communication pipeline between the oil layer standing section outlet of the extraction tower and the material inlet of the rectifying tower.
  • the oil layer receiving tank is used to buffer the organic oil layer from the extraction tower, and the oil layer feed pump is used to transport materials.
  • the present invention also provides a continuous extraction and drying method for butenone, wherein the method includes:
  • the continuous extraction and drying method is performed in the above-mentioned (i) continuous extraction and drying device and includes: And extractant are added into the extraction tower from the upper feed port and the lower feed port respectively for mixing and extraction, the waste water obtained at the bottom of the extraction tower is discharged and the organic oil layer containing the extractant obtained at the top of the tower is discharged from the The exit of the standing section of the oil layer is led out and enters the rectification tower for rectification. The extractant containing water and a small amount of butenone obtained at the top of the rectification tower enters the condenser for condensation, and the condensed product enters the distillation tower. Water is separated in the water separation tank to obtain extractant and waste water, and the dewatered butenone obtained from the bottom of the rectification tower is introduced into the oil layer receiving tank;
  • the continuous extraction and drying method is carried out in the above-mentioned (ii) continuous extraction and drying device and includes: And the extractant are added to the extraction tower from the lower feed port and the upper feed port respectively for mixing and extraction, the waste water obtained at the top of the extraction tower is discharged and the organic oil layer containing the extractant obtained at the bottom of the tower is discharged from the The exit of the standing section of the oil layer is led out and enters the rectification tower for rectification.
  • the extractant containing water and a small amount of butenone obtained at the top of the rectification tower enters the condenser for condensation, and the condensed product enters the distillation tower.
  • Water is separated in the water separation tank to obtain extractant and waste water, and the dewatered butenone obtained from the bottom of the rectification tower is introduced into the oil layer receiving tank;
  • the boiling point is lower than the normal pressure boiling point of butenone, and the difference is more than 10°C.
  • the moisture content in the hydrous butenone is 0.1 to 23 wt%.
  • the difference between the boiling point of the extractant and the boiling point of the hydrous butenone is 15-50°C.
  • the extraction agent is selected from at least one of dichloromethane, chloroform, n-hexane, petroleum ether, diethyl ether, methyl tert-butyl ether and isopropyl ether.
  • the feed volume ratio of the aqueous butenone to the extractant is 1:(1-5), preferably 1:(1.5-4), more preferably 1:(1.5-3.0).
  • the bottom of the rectification tower is heated by steam and the temperature of the bottom is controlled at 40-80°C, preferably at 45-75°C; the reflux ratio is controlled at 0.25-10, preferably at 0.5-5.
  • an extractant that is difficult to dissolve or insoluble in water and has good miscibility with water-containing butenone is used to extract butenone, followed by rectification with water, and a tower kettle to obtain butenone with extremely low water content.
  • the recovery rate of butenone is high, and the whole process will not produce solid waste or high-salt, high-COD wastewater, which is green and environmentally friendly.
  • the continuous extraction and drying device provided by the present invention is environmentally friendly, efficient, and convenient for automatic control, can realize continuous operation, has high production efficiency and equipment utilization, and has a friendly operating environment.
  • Figure 1 is a schematic diagram of a connection of a continuous extraction drying device provided by the present invention.
  • Figure 2 is a schematic diagram of another connection of the continuous extraction drying device provided by the present invention.
  • 1-extraction tower 2-extraction oil layer receiving tank, 3-oil layer feed pump, 4-rectification tower, 5-condenser, 6-water separator, 7-reboiler, 8-oil layer receiving tank.
  • the continuous extraction and drying device includes an extraction tower 1, a rectification tower 4, a condenser 5, a water separator 6, and a reboiler 7. And the oil layer receiving tank 8; the extraction tower 1 includes three parts, from top to bottom, an oil layer standing section, a mixing section and a water layer standing section, and the mixing section is provided with an upper feed port and a lower feed port, respectively,
  • the rectification tower 4 includes two parts, a water section and a stripping section, from top to bottom.
  • the outlet of the oil layer stationary section of the extraction tower 1 is connected to the material inlet of the rectification tower 4,
  • the top outlet of the distillation column 4 is in communication with the material inlet of the condenser 5, the material outlet of the condenser 5 is in communication with the material inlet of the water separation tank 6, and the bottom outlet of the rectification tower 4 is connected all the way with
  • the reboiler 7 is in cyclic communication and the other path is in communication with the oil layer receiving tank 8.
  • the continuous extraction and drying device includes an extraction tower 1, a rectification tower 4, a condenser 5, a water separator 6, and a reboiler 7 and the oil layer receiving tank 8;
  • the extraction tower 1 includes three parts from top to bottom: a water layer standing section, a mixing section and an oil layer standing section, and the mixing section is provided with an upper feed port and a lower feed port respectively
  • the rectification tower 4 includes two parts, from top to bottom, a rectification zone with water and a stripping section.
  • the outlet of the oil layer stationary section of the extraction tower 1 is in communication with the material inlet of the rectification tower 4.
  • the top outlet of the rectification tower 4 communicates with the material inlet of the condenser 5, the material outlet of the condenser 5 communicates with the material inlet of the water separation tank 6, and the bottom outlet of the rectification tower 4 It is in cyclic communication with the reboiler 7 and the other path is in communication with the oil reservoir 8.
  • the extraction tower 1 is used to extract butenone from water-containing butenone. Since the extractant has good solubility with butenone and the extractant is hardly soluble in water, it can achieve water and Separation of butenone.
  • the extraction tower 1 may specifically adopt a spray tower, a packed tower, a sieve tray or a rotating disk extraction tower. When working, the aqueous butenone and the extractant are in countercurrent contact in the extraction tower 1, and the feed positions of the two in the extraction tower 1 (upper and lower feed ports) depend on the density.
  • the two are mixed countercurrently in the mixing section of the extraction tower 1, resulting in a light weight extractant containing
  • the organic oil layer enters the standing section of the oil layer at the top of the tower, and the resulting heavy wastewater enters the standing section of the water layer at the bottom of the tower; when the density of the aqueous butenone is less than the density of the extractant, it should be in the above paragraph (ii)
  • Continuous extraction and drying are carried out in a continuous extraction drying device.
  • the aqueous butenone enters from the lower inlet of the extraction tower 1, and the extractant enters from the upper inlet of the extraction tower 1. Due to gravity, the aqueous butenone moves upward.
  • the extractant moves downwards, and the two are mixed countercurrently in the mixing section of the extraction tower 1, the obtained light wastewater enters the standing section of the water layer at the top of the tower, and the obtained heavy organic oil layer containing the extractant enters the bottom of the tower.
  • the stationary section of the water layer of the extraction tower 1 is preferably controlled by an interface controller, which can stabilize the extraction process and reduce entrainment, thereby ensuring the extraction effect.
  • the rectification tower 4 is used to separate the extractant and the butenone, and at the same time, a small amount of water in the organic oil layer containing the extractant derived from the extraction tower 1 is removed by evaporation of water. It can be a packed tower or a sieve tray.
  • the rectification tower 4 from top to bottom includes two parts, a rectification zone with water and a stripping zone. The role of the rectification zone with water is to realize the separation of butenone and extractant while entraining the oil layer. The role of the stripping section is to heat and evaporate the oil layer extractant and a small amount of water.
  • the material inlet of the rectification tower 4 is located in the stripping section.
  • the organic oil layer containing the extractant drawn from the exit of the oil layer static section of the extraction tower 1 enters the stripping section of the rectification tower 4 for evaporation.
  • the butenone and the extractant are separated in the water section of the rectification.
  • a small amount of water contained in it is also taken out with the extractant and enters the condenser 5 for condensation, and the obtained butenone with water removed is drawn from the bottom of the rectification tower 4.
  • the condenser 5 is used to condense the extractant containing water and a small amount of butenone from the top of the rectification tower 4, and may be a shell-and-tube condenser, a spiral condenser, or a plate condenser.
  • the water separation tank 6 is used to separate the separated water in the condensed product from the condenser 5 to obtain the extractant and waste water, and the extractant can be recycled.
  • the water diversion tank 6 may specifically be a standing tank with an interface controller.
  • the reboiler 7 is used to provide the rectification tower 4 with the rising steam flow and the energy required in the separation process, and specifically may be a thermosyphon reboiler or a falling film reboiler.
  • the continuous extraction and drying device further includes materials arranged in sequence at the outlet of the oil layer static section of the extraction tower 1 and the rectification tower 4
  • the continuous extraction drying method provided by the present invention includes:
  • the continuous extraction and drying method is carried out in the above-mentioned (i) continuous extraction and drying device and includes: separate the water-containing butenone and the extractant From the upper feed port and the lower feed port, it is added to the extraction tower 1 for mixing and extraction.
  • the waste water obtained at the bottom of the extraction tower 1 is discharged and the organic oil layer containing the extractant obtained at the top of the tower is statically removed from the oil layer.
  • the outlet of the set section is led out and enters the rectification tower 4 for rectification (evaporates with water), and the extractant containing water and a small amount of butenone obtained at the top of the rectification tower 4 enters the condenser 5 for condensation,
  • the condensed product enters the water separation tank 6 for water separation to obtain an extractant and waste water, and the dewatered butenone obtained from the 4 rectification tower still is introduced into the oil layer receiving tank 8;
  • the continuous extraction and drying method is carried out in the above-mentioned (ii) continuous extraction and drying device and includes: And the extractant are added to the extraction tower 1 from the lower feed port and the upper feed port respectively for mixing and extraction.
  • the waste water obtained at the top of the extraction tower 1 is discharged and the organic oil layer containing the extractant obtained at the bottom of the tower is discharged from The exit of the oil layer standing section is led out and enters the rectification tower 4 for rectification (evaporates with water), and the extractant containing water and a small amount of butenone obtained at the top of the rectification tower 4 enters the condenser 5.
  • the condensed product enters the water separation tank 6 for water separation to obtain extractant and waste water.
  • the dewatered butenone obtained in the rectification tower 4 tower is introduced into the oil layer receiving tank 8.
  • the continuous extraction drying device and method provided by the present invention are not only suitable for drying butenone with a small amount of moisture, but also particularly suitable for drying butenone with higher water content, and has wide universality.
  • the moisture content in the hydrous butenone may be 0.1 to 23 wt%.
  • the water-carrying effect is good, whether it is azeotropic water-carrying or entraining water, it needs to have a good water-carrying effect to reduce the amount of extractant used;
  • the boiling point is lower than the normal pressure boiling point of butenone, and the difference between the two is more than 10°C, preferably 15-50°C, to facilitate subsequent separation.
  • the extractant may be selected from at least one of dichloromethane, chloroform, n-hexane, petroleum ether, diethyl ether, methyl tert-butyl ether and isopropyl ether.
  • the feed volume ratio of the aqueous butenone to the extractant is preferably 1:(1 to 5), preferably 1:(1.5 to 4), more preferably 1:(1.5 to 3.0).
  • the bottom of the rectification tower 4 is heated by steam and the temperature of the bottom is preferably controlled at 40-80°C, more preferably controlled at 45-75°C; reflux ratio is preferably controlled at 0.25-10, more preferably controlled In 0.5 ⁇ 5.
  • the continuous extraction and drying device shown in Figure 1 is used to process it, specifically: an aqueous solution of butenone with a water content of 23 wt% at a flow rate of 0.5 m 3 /h and the extractant ether at a rate of 0.7 m 3 /h
  • the flow rates are fed from the upper and lower inlets of the extraction tower 1, after thorough mixing and extraction, the tower kettle obtains wastewater with a residual butenone content of 0.3wt%.
  • the COD value of the wastewater is 3000mg /L
  • the butenone-containing ether oil layer obtained from the top of the tower is pumped into the rectification tower 4 through the oil layer feed pump 3
  • the bottom of the rectification tower 4 is heated by steam and the temperature of the bottom is controlled at 50°C and the reflux ratio Controlled at 1
  • the ether solution containing water and a small amount of butenone obtained at the top of the rectifying tower 4 is condensed to 20°C by the condenser 5 and then introduced into the water separator 6 to stand still to separate the bottom water to obtain the extractant ether and waste water.
  • the ether is recycled, and the butenone with a moisture content of 0.05% by weight obtained from the four stills of the rectification tower is introduced into the oil reservoir 8, and the butenone recovery rate is 97.5%.
  • the whole process does not produce high COD wastewater, can realize continuous operation, and is environmentally friendly.
  • the continuous extraction and drying device shown in FIG. 1 is used to process the butenone aqueous solution, specifically: the butenone aqueous solution with a water content of 23% by weight is used at a flow rate of 0.5 m 3 /h and the extractant is n-hexane at a rate of 0.9 m
  • the flow rate of 3 /h is fed from the upper and lower feed ports of the extraction tower 1, after thorough mixing and extraction, the tower kettle obtains waste water with a residual butenone content of 0.4 wt%.
  • the COD value is 4000 mg/L.
  • the n-hexane oil layer containing butenone obtained at the top of the tower is pumped into the rectification tower 4 through the oil layer feed pump 3, and the bottom of the rectification tower 4 is heated by steam and the temperature of the bottom is controlled at 72°C, reflux ratio is controlled at 1.5, the n-hexane solution containing water and a small amount of butenone obtained at the top of the rectification tower 4 is condensed to 30°C by condenser 5, and then introduced into the water separator 6 to stand still to separate the bottom moisture. The n-hexane and waste water are extracted and the n-hexane is recycled.
  • the butenone with a moisture content of 0.03 wt% obtained from the four rectification tower stills is introduced into the oil reservoir 8 and the butenone recovery rate is 97.0%.
  • the continuous extraction and drying device shown in FIG. 2 is used to process the butenone aqueous solution, specifically: the butenone aqueous solution with a water content of 23% by weight is used at a flow rate of 0.5 m 3 /h and the extractant dichloromethane is 1.0
  • the flow rate of m 3 /h is fed from the lower feed port and the upper feed port of the extraction tower 1, after thorough mixing and extraction, the top of the tower obtains waste water with a residual butenone content of 0.1 wt%.
  • the waste water The COD value is 2000mg/L, and the methylene chloride oil layer containing butenone obtained from the bottom of the column is pumped into the rectification tower 4 through the oil layer feed pump 3.
  • the bottom of the rectification tower 4 is heated by steam and the temperature of the bottom is The temperature is controlled at 51°C and the reflux ratio is controlled at 1.0.
  • the dichloromethane solution containing water and a small amount of butenone obtained at the top of the rectification tower 4 is condensed to 25°C by the condenser 5 and then introduced into the water separator 6 to stand for separation.
  • the water at the bottom obtains the extractant dichloromethane and waste water, and the dichloromethane is recycled and reused.
  • the butenone with a moisture content of 0.02wt% from the bottom of the rectifying tower 4 is introduced into the oil reservoir 8 and the butenone recovery rate is 98.1% .
  • the continuous extraction and drying device shown in Figure 2 is used to process the butenone aqueous solution, specifically: the butenone aqueous solution with a water content of 23% by weight is used at a flow rate of 0.5 m 3 /h and the extractant chloroform is at 1.2 The flow rate of m 3 /h is fed from the lower feed port and the upper feed port of the extraction tower 1. After thorough mixing and extraction, the top of the tower obtains waste water with a residual butenone content of 0.05 wt%.
  • the waste water The COD value is 2000mg/L
  • the butenone-containing chloroform oil layer obtained from the bottom of the column is pumped into the rectification tower 4 through the oil layer feed pump 3, and the bottom of the rectification tower 4 is heated by steam and the temperature of the bottom is The temperature is controlled at 68°C and the reflux ratio is controlled at 1.3.
  • the chloroform solution containing water and a small amount of butenone obtained at the top of the rectification tower 4 is condensed to 28°C by the condenser 5 and then introduced into the water separator 6 to stand for separation.
  • the water at the bottom obtains the extractant chloroform and waste water, and the chloroform is recycled.
  • the butenone with a moisture content of 0.03wt% obtained from the four rectification towers is introduced into the oil reservoir 8 and the butenone recovery rate is 98.7% .

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Abstract

本发明属于丁烯酮干燥领域，公开了一种连续萃取干燥丁烯酮的装置和方法。所述连续萃取干燥方法包括：将含水丁烯酮和萃取剂引入萃取塔中进行混合、萃取，萃取塔所得废水外排且所得含萃取剂的有机油层从油层静置段出口引出并进入精馏塔中进行蒸发带水，精馏塔塔顶所得含水和少量丁烯酮的萃取剂进入冷凝器中进行冷凝，经冷凝的产物进入分水罐中进行分水，精馏塔塔釜得到含水量极低的丁烯酮。本发明由于采用难溶或不溶于水且与含水丁烯酮有较好互溶性的萃取剂来萃取含水丁烯酮，后续通过精馏带水，塔釜得到含水量极低的丁烯酮，丁烯酮的回收率高，且整个过程不会产生固废或高盐、高COD的废水，绿色环保。

Description

一种丁烯酮的连续萃取干燥装置和方法 技术领域
本发明属于干燥领域，具体涉及一种含水丁烯酮的连续萃取干燥装置和方法。
背景技术
含水丁烯酮的传统干燥方式是采用无水氯化钙、硫酸镁、碳酸镁等作为干燥剂，通过与水可逆结合形成水合物而达到干燥目的。常见的使用方式有两种：一种是将干燥剂填充在过滤器当中，当含水丁烯酮流经过滤器时，水分被吸附在干燥剂上，这种适合微量水分丁烯酮的干燥；另一种是将干燥剂投入反应釜当中，搅拌，充分静置，抽取上层油层，下层含盐有机物层回收套用。
然而，传统的含水丁烯酮干燥工艺存在以下问题：(1)会产生固废或高盐、高COD废水；(2)不易实现自动化控制，操作繁琐；(3)配套设备多，设备体积较大，丁烯酮回收率低且设备利用率低；(4)劳动强大，操作环境差。
发明内容
本发明的目的是为了克服现有技术采用干燥剂对含水丁烯酮进行干燥存在丁烯酮回收率低且还会产生固废或高盐、高COD的废水的缺陷，而提供一种丁烯酮回收率高且整个过程不会产生固废或高盐、高COD的废水的连续萃取干燥装置和方法。
具体地，本发明提供了一种丁烯酮的连续萃取干燥装置，其中，所述连续萃取干燥装置包括萃取塔、精馏塔、冷凝器、分水罐、再沸器和油层受罐；
(i)所述萃取塔由上而下包括油层静置段、混合段和水层静置段三个部分且所述混合段分别设置有上部进料口和下部进料口，所述精馏塔由上而下包括精馏带水段和提馏段两个部分，所述萃取塔的油层静置段出口与所述精馏塔的物料入口连通，所述精馏塔的塔顶出口与所述冷凝器的物料入口连通，所述冷凝器的物料出口与所述分水罐的物料入口连通，所述精馏塔的塔釜出口一路与所述再沸器循环连通且另一路与所述油层受罐连通；或者，
(ii)所述萃取塔由上而下包括水层静置段、混合段和油层静置段三个部分且所述混合段分别设置有上部进料口和下部进料口，所述精馏塔由上而下包括精馏带水段和提馏段两个部分，所述萃取塔的油层静置段出口与所述精馏塔的物料入口连通，所述精馏塔的塔顶 出口与所述冷凝器的物料入口连通，所述冷凝器物料的物料出口与所述分水罐的物料入口连通，所述精馏塔的塔釜出口一路与所述再沸器循环连通且另一路与所述油层受罐连通。
进一步的，所述萃取塔为喷洒塔、填料塔、筛板塔或转盘萃取塔。
进一步的，所述萃取塔的水层静置段采用界面控制仪控制。
进一步的，所述精馏塔为填料塔或筛板塔。
进一步的，所述冷凝器为管壳式冷凝器、缠绕式冷凝器或板式冷凝器。
进一步的，所述分水罐为带界面控制仪的静置罐。
进一步的，所述再沸器为热虹吸式再沸器或降膜式再沸器。
进一步的，所述丁烯酮的连续萃取干燥装置还包括依次设置在所述萃取塔的油层静置段出口与所述精馏塔的物料入口之间连通管路上的萃取油层受罐和油层进料泵，所述萃取油层受罐用于对源自所述萃取塔的有机油层进行缓存，所述油层进料泵用于输送物料。
本发明还提供了一种丁烯酮的连续萃取干燥方法，其中，该方法包括：
(i)当待萃取干燥的含水丁烯酮的密度大于萃取剂的密度时，所述连续萃取干燥方法在上述第(i)种连续萃取干燥装置中进行且包括：将所述含水丁烯酮和萃取剂分别从所述上部进料口和下部进料口加入所述萃取塔中进行混合、萃取，所述萃取塔塔底所得废水外排且塔顶所得含萃取剂的有机油层从所述油层静置段出口引出并进入所述精馏塔中进行精馏，所述精馏塔塔顶所得含水和少量丁烯酮的萃取剂进入所述冷凝器中进行冷凝，经冷凝的产物进入所述分水罐中进行分水得到萃取剂和废水，所述精馏塔塔釜所得除水的丁烯酮引入所述油层受罐中；
(ii)当待萃取干燥的含水丁烯酮的密度小于萃取剂的密度时，所述连续萃取干燥方法在上述第(ii)种连续萃取干燥装置中进行且包括：将所述含水丁烯酮和萃取剂分别从所述下部进料口和上部进料口加入所述萃取塔中进行混合、萃取，所述萃取塔塔顶所得废水外排且塔底所得含萃取剂的有机油层从所述油层静置段出口引出并进入所述精馏塔中进行精馏，所述精馏塔塔顶所得含水和少量丁烯酮的萃取剂进入所述冷凝器中进行冷凝，经冷凝的产物进入所述分水罐中进行分水得到萃取剂和废水，所述精馏塔塔釜所得除水的丁烯酮引入所述油层受罐中；
(i)和(ii)中所述萃取剂均应该满足以下三个条件：
a、难溶或不溶于水，与所述丁烯酮互溶性好且不发生反应；
b、带水效果好；
c、沸点小于丁烯酮的常压沸点，且相差10℃以上。
进一步的，所述含水丁烯酮中的水分含量为0.1～23wt％。
进一步的，所述萃取剂的沸点与所述含水丁烯酮的沸点之差为15～50℃。
进一步的，所述萃取剂选自二氯甲烷、三氯甲烷、正己烷、石油醚、乙醚、甲基叔丁基醚和异丙醚中的至少一种。
进一步的，所述含水丁烯酮与萃取剂的进料体积比为1:(1～5)，优选为1:(1.5～4)，更优选为1:(1.5～3.0)。
进一步的，所述精馏塔的塔釜采用蒸汽加热且塔釜温度控制在40～80℃，优选控制在45～75℃；回流比控制在0.25～10，优选控制在0.5～5。
与传统的脱水干燥工艺相比，本发明的有益效果如下：
本发明巧妙地采用难溶或不溶于水且与含水丁烯酮有较好互溶性的萃取剂来萃取丁烯酮，后续通过精馏带水，塔釜得到含水量极低的丁烯酮，丁烯酮的回收率高，并且整个过程不会产生固废或高盐、高COD的废水，绿色环保。此外，本发明提供的连续萃取干燥装置环保、高效、便于自动化控制，可实现连续操作，生产效率和设备利用率高，操作环境友好。
附图说明
图1为本发明提供的连续萃取干燥装置的一种连接示意图；
图2为本发明提供的连续萃取干燥装置的另一种连接示意图。
附图标记说明
1-萃取塔，2-萃取油层受罐，3-油层进料泵，4-精馏塔，5-冷凝器，6-分水罐，7-再沸器，8-油层受罐。
具体实施方式
根据本发明的一种具体实施方式(记为i)，如图1所示，所述连续萃取干燥装置包括萃取塔1、精馏塔4、冷凝器5、分水罐6、再沸器7和油层受罐8；所述萃取塔1由上而下包括油层静置段、混合段和水层静置段三个部分且所述混合段分别设置有上部进料口和下部进料口，所述精馏塔4由上而下包括精馏带水段和提馏段两个部分，所述萃取塔1的油层静置段出口与所述精馏塔4的物料入口连通，所述精馏塔4的塔顶出口与所述冷凝器5的物料入口连通，所述冷凝器5的物料出口与所述分水罐6的物料入口连通，所述精馏塔4的塔釜出口一路与所述再沸器7循环连通且另一路与所述油层受罐8连通。
根据本发明的另一种具体实施方式(记为ii)，如图2所示，所述连续萃取干燥装置 包括萃取塔1、精馏塔4、冷凝器5、分水罐6、再沸器7和油层受罐8；所述萃取塔1由上而下包括水层静置段、混合段和油层静置段三个部分且所述混合段分别设置有上部进料口和下部进料口，所述精馏塔4由上而下包括精馏带水段和提馏段两个部分，所述萃取塔1的油层静置段出口与所述精馏塔4的物料入口连通，所述精馏塔4的塔顶出口与所述冷凝器5的物料入口连通，所述冷凝器5的物料出口与所述分水罐6的物料入口连通，所述精馏塔4的塔釜出口一路与所述再沸器7循环连通且另一路与所述油层受罐8连通。
在本发明中，所述萃取塔1用于从含水丁烯酮中萃取丁烯酮，由于萃取剂与丁烯酮有很好的溶解性而萃取剂又难溶于水，故可以实现水与丁烯酮的分离。所述萃取塔1具体可以采用喷洒塔、填料塔、筛板塔或转盘萃取塔。当工作时，含水丁烯酮与萃取剂在萃取塔1中逆流接触，两者在萃取塔1中的进料位置(上部进料口和下部进料口)视密度而定。具体地，当含水丁烯酮的密度大于萃取剂的密度时，应在上述第(i)种连续萃取干燥装置中进行连续萃取干燥，含水丁烯酮从萃取塔1的上部进料口进入，萃取剂从萃取塔1的下部进料口进入，由于重力作用，含水丁烯酮往下运动，萃取剂往上运动，两者在萃取塔1的混合段逆流混合，所得质轻的含萃取剂的有机油层进入位于塔顶的油层静置段，所得质重的废水进入位于塔釜的水层静置段；当含水丁烯酮的密度小于萃取剂的密度时，应在上述第(ii)种连续萃取干燥装置中进行连续萃取干燥，含水丁烯酮从萃取塔1的下部进料口进入，萃取剂从萃取塔1的上部进料口进入，由于重力作用，含水丁烯酮往上运动，萃取剂往下运动，两者在萃取塔1的混合段逆流混合，所得质轻的废水进入位于塔顶的水层静置段，所得质重的含萃取剂的有机油层进入位于塔釜的油层静置段。此外，所述萃取塔1的水层静置段优选采用界面控制仪控制，这样能够使得萃取过程稳定，减少夹带，从而保证了萃取效果。
在本发明中，所述精馏塔4用于萃取剂与丁烯酮的分离，同时通过蒸发带水以将源自所述萃取塔1的含萃取剂的有机油层中的少量水分去除，具体可以为填料塔或筛板塔。所述精馏塔4由上而下包括精馏带水段和提馏段两个部分，其中，精馏带水段所起的作用为实现丁烯酮与萃取剂的分离，同时夹带出油层中的少量水份，提馏段所起的作用为加热蒸发油层萃取剂和少量水份。所述精馏塔4的物料入口位于所述提馏段。从所述萃取塔1的油层静置段出口引出的含萃取剂的有机油层进入精馏塔4的提馏段进行蒸发，在精馏带水段实现丁烯酮与萃取剂的分离，同时物料中所含少量水也随萃取剂带出，进入冷凝器5中进行冷凝，所得除水的丁烯酮从精馏塔4的塔釜引出。
在本发明中，所述冷凝器5用于对源自精馏塔4塔顶的含水和少量丁烯酮的萃取剂进行冷凝，具体可以为管壳式、缠绕式或板式等冷凝器。
在本发明中，所述分水罐6用于对源自冷凝器5的冷凝产物中的分水进行分离，以得 到萃取剂和废水，萃取剂可循环套用。所述分水罐6具体可以为带界面控制仪的静置罐。
在本发明中，所述再沸器7用于为精馏塔4提供上升蒸汽流及分离过程中所需的能量，具体可以为热虹吸式再沸器或降膜式再沸器。
根据本发明的一种具体实施方式，如图1和图2所示，所述连续萃取干燥装置还包括依次设置在所述萃取塔1的油层静置段出口与所述精馏塔4的物料入口之间连通管路上的萃取油层受罐2和油层进料泵3，所述萃取油层受罐2用于对源自所述萃取塔1的有机油层进行缓存，所述油层进料泵3用于输送物料。
本发明提供的连续萃取干燥方法包括：
(i)当含水丁烯酮的密度大于萃取剂的密度时，所述连续萃取干燥方法在上述第(i)种连续萃取干燥装置中进行且包括：将所述含水丁烯酮和萃取剂分别从所述上部进料口和下部进料口加入所述萃取塔1中进行混合、萃取，所述萃取塔1塔底所得废水外排且塔顶所得含萃取剂的有机油层从所述油层静置段出口引出并进入所述精馏塔4中进行精馏(蒸发带水)，所述精馏塔4塔顶所得含水和少量丁烯酮的萃取剂进入所述冷凝器5中进行冷凝，经冷凝的产物进入所述分水罐6中进行分水得到萃取剂和废水，所述精馏塔4塔釜所得除水的丁烯酮引入所述油层受罐8中；
(ii)当待萃取干燥的含水丁烯酮的密度小于萃取剂的密度时，所述连续萃取干燥方法在上述第(ii)种连续萃取干燥装置中进行且包括：将所述含水丁烯酮和萃取剂分别从所述下部进料口和上部进料口加入所述萃取塔1中进行混合、萃取，所述萃取塔1塔顶所得废水外排且塔底所得含萃取剂的有机油层从所述油层静置段出口引出并进入所述精馏塔4中进行精馏(蒸发带水)，所述精馏塔4塔顶所得含水和少量丁烯酮的萃取剂进入所述冷凝器5中进行冷凝，经冷凝的产物进入所述分水罐6中进行分水得到萃取剂和废水，所述精馏塔4塔釜所得除水的丁烯酮引入所述油层受罐8中。
本发明提供的连续萃取干燥装置和方法不仅适用于含少量水分的丁烯酮的干燥，而且还特别适应于含水较高的丁烯酮的干燥，具有广泛的普适性。具体地，所述含水丁烯酮中的水分含量可以为0.1～23wt％。
在本发明中，所述萃取剂的选择需要遵循以下几个原则：
a、难溶或不溶于水，与所述含水丁烯酮互溶性好且不发生反应；
b、带水效果好，无论是共沸带水还是夹带带水，均需要有好的带水效果，以减少萃取剂的使用量；
c、沸点小于丁烯酮的常压沸点，且两者之差为10℃以上，优选为15～50℃，以便于后续分离。
具体地，所述萃取剂可以选自二氯甲烷、三氯甲烷、正己烷、石油醚、乙醚、甲基叔丁基醚和异丙醚中的至少一种。此外，所述含水丁烯酮与萃取剂的进料体积比优选为1:(1～5)，优选为1:(1.5～4)，更优选为1:(1.5～3.0)。
在本发明中，所述精馏塔4的塔釜采用蒸汽加热且塔釜温度优选控制在40～80℃，更优选控制在45～75℃；回流比优选控制在0.25～10，更优选控制在0.5～5。
下面详细描述本发明的实施例，所述实施例的示例旨在用于解释本发明，而不能理解为对本发明的限制。实施例中未注明具体技术或条件者，按照本领域内的文献所描述的技术或条件或者按照产品说明书进行。所用试剂或仪器未注明生产厂商者，均为可以通过市购获得的常规产品。
实施例1
对于含水量23wt％的丁烯酮水溶液的干燥，工业上一般采用加固体无水氯化钙进行盐析、干燥的方式进行除水，丁烯酮回收率一般不高于95％，并且在除水过程所产生的高盐废水的COD一般在80000mg/L左右。
本实施例采用图1所示的连续萃取干燥装置对其进行处理，具体地：将含水量23wt％的丁烯酮水溶液以0.5m 3/h的流速且萃取剂乙醚以0.7m 3/h的流速分别从萃取塔1的上部进料口和下部进料口进料，经充分混合、萃取，塔釜得到丁烯酮残留量为0.3wt％的废水，经检测，该废水的COD值为3000mg/L，塔顶所得含丁烯酮的乙醚油层通过油层进料泵3泵入精馏塔4中，所述精馏塔4的塔釜采用蒸汽加热且塔釜温度控制在50℃、回流比控制在1，所述精馏塔4塔顶所得含水和少量丁烯酮的乙醚溶液经冷凝器5冷凝至20℃之后引入分水罐6中静置分去底部水分得到萃取剂乙醚和废水，乙醚循环套用，所述精馏塔4塔釜所得水分含量0.05wt％的丁烯酮引入油层受罐8中，丁烯酮回收率为97.5％。整个过程不产生高COD废水，可实现连续化操作，环境友好。
实施例2
本实施例采用图1所示的连续萃取干燥装置对丁烯酮水溶液进行处理，具体地：将含水量23wt％的丁烯酮水溶液以0.5m 3/h的流速且萃取剂正己烷以0.9m 3/h的流速分别从萃取塔1的上部进料口和下部进料口进料，经充分混合、萃取，塔釜得到丁烯酮残留量为0.4wt％的废水，经检测，该废水的COD值为4000mg/L，塔顶所得含丁烯酮的正己烷油层通过油层进料泵3泵入精馏塔4中，所述精馏塔4的塔釜采用蒸汽加热且塔釜温度控制在72℃、回流比控制在1.5，所述精馏塔4塔顶所得含水和少量丁烯酮的正己烷溶液经冷凝器5冷凝 至30℃之后引入分水罐6中静置分去底部水分得到萃取正己烷和废水，正己烷循环套用，所述精馏塔4塔釜所得水分含量0.03wt％的丁烯酮引入油层受罐8中，丁烯酮回收率为97.0％。
实施例3
本实施例采用图2所示的连续萃取干燥装置对丁烯酮水溶液进行处理，具体地：将含水量23wt％的丁烯酮水溶液以0.5m 3/h的流速且萃取剂二氯甲烷以1.0m 3/h的流速分别从萃取塔1的下部进料口和上部进料口进料，经充分混合、萃取，塔顶得到丁烯酮残留量为0.1wt％的废水，经检测，该废水的COD值为2000mg/L，塔釜所得含丁烯酮的二氯甲烷油层通过油层进料泵3泵入精馏塔4中，所述精馏塔4的塔釜采用蒸汽加热且塔釜温度控制在51℃、回流比控制在1.0，所述精馏塔4塔顶所得含水和少量丁烯酮的二氯甲烷溶液经冷凝器5冷凝至25℃之后引入分水罐6中静置分去底部水分得到萃取剂二氯甲烷和废水，二氯甲烷循环套用，所述精馏塔4塔釜所得水分含量0.02wt％的丁烯酮引入油层受罐8中，丁烯酮回收率为98.1％。
实施例4
本实施例采用图2所示的连续萃取干燥装置对丁烯酮水溶液进行处理，具体地：将含水量23wt％的丁烯酮水溶液以0.5m 3/h的流速且萃取剂三氯甲烷以1.2m 3/h的流速分别从萃取塔1的下部进料口和上部进料口进料，经充分混合、萃取，塔顶得到丁烯酮残留量为0.05wt％的废水，经检测，该废水的COD值为2000mg/L，塔釜所得含丁烯酮的三氯甲烷油层通过油层进料泵3泵入精馏塔4中，所述精馏塔4的塔釜采用蒸汽加热且塔釜温度控制在68℃、回流比控制在1.3，所述精馏塔4塔顶所得含水和少量丁烯酮的三氯甲烷溶液经冷凝器5冷凝至28℃之后引入分水罐6中静置分去底部水分得到萃取剂三氯甲烷和废水，三氯甲烷循环套用，所述精馏塔4塔釜所得水分含量0.03wt％的丁烯酮引入油层受罐8中，丁烯酮回收率为98.7％。
尽管上面已经示出和描述了本发明的实施例，可以理解的是，上述实施例是示例性的，不能理解为对本发明的限制，本领域的普通技术人员在不脱离本发明的原理和宗旨的情况下在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。

Claims (17)

  1. 一种丁烯酮的连续萃取干燥装置，其特征在于，所述连续萃取干燥装置包括萃取塔(1)、精馏塔(4)、冷凝器(5)、分水罐(6)、再沸器(7)和油层受罐(8)；
    (i)所述萃取塔(1)由上而下包括油层静置段、混合段和水层静置段三个部分且所述混合段分别设置有上部进料口和下部进料口，所述精馏塔(4)由上而下包括精馏带水段和提馏段两个部分，所述萃取塔(1)的油层静置段出口与所述精馏塔(4)的物料入口连通，所述精馏塔(4)的塔顶出口与所述冷凝器(5)的物料入口连通，所述冷凝器(5)的物料出口与所述分水罐(6)的物料入口连通，所述精馏塔(4)的塔釜出口一路与所述再沸器(7)循环连通且另一路与所述油层受罐(8)连通；或者，
    (ii)所述萃取塔(1)由上而下包括水层静置段、混合段和油层静置段三个部分且所述混合段分别设置有上部进料口和下部进料口，所述精馏塔(4)由上而下包括精馏带水段和提馏段两个部分，所述萃取塔(1)的油层静置段出口与所述精馏塔(4)的物料入口连通，所述精馏塔(4)的塔顶出口与所述冷凝器(5)的物料入口连通，所述冷凝器(5)的物料出口与所述分水罐(6)的物料入口连通，所述精馏塔(4)的塔釜出口一路与所述再沸器(7)循环连通且另一路与所述油层受罐(8)连通。
  2. 根据权利要求1所述的丁烯酮的连续萃取干燥装置，其特征在于，所述萃取塔(1)为喷洒塔、填料塔、筛板塔或转盘萃取塔。
  3. 根据权利要求1所述的丁烯酮的连续萃取干燥装置，其特征在于，所述萃取塔(1)的水层静置段采用界面控制仪控制。
  4. 根据权利要求1所述的丁烯酮的连续萃取干燥装置，其特征在于，所述精馏塔(4)为填料塔或筛板塔。
  5. 根据权利要求1所述的丁烯酮的连续萃取干燥装置，其特征在于，所述冷凝器(5)为管壳式冷凝器、缠绕式冷凝器或板式冷凝器。
  6. 根据权利要求1所述的丁烯酮的连续萃取干燥装置，其特征在于，所述分水罐(6)为带界面控制仪的静置罐。
  7. 根据权利要求1所述的丁烯酮的连续萃取干燥装置，其特征在于，所述再沸器(7)为热虹吸式再沸器或降膜式再沸器。
  8. 根据权利要求1～7中任意一项所述的丁烯酮的连续萃取干燥装置，其特征在于，所述连续萃取干燥装置还包括依次设置在所述萃取塔(1)的油层静置段出口与所述精馏塔(4)的物料入口之间连通管路上的萃取油层受罐(2)和油层进料泵(3)，所述萃取油层受罐 (2)用于对源自所述萃取塔(1)的有机油层进行缓存，所述油层进料泵(3)用于输送物料。
  9. 一种丁烯酮的连续萃取干燥方法，其特征在于，该方法包括：
    (i)当待萃取干燥的含水丁烯酮的密度大于萃取剂的密度时，所述连续萃取干燥方法在权利要求1～8中任意一项中第(i)种连续萃取干燥装置中进行且包括：将所述含水丁烯酮和萃取剂分别从所述上部进料口和下部进料口加入所述萃取塔(1)中进行混合、萃取，所述萃取塔(1)塔底所得废水外排且塔顶所得含萃取剂的有机油层从所述油层静置段出口引出并进入所述精馏塔(4)中进行精馏，所述精馏塔(4)塔顶所得含水和少量丁烯酮的萃取剂进入所述冷凝器(5)中进行冷凝，经冷凝的产物进入所述分水罐(6)中进行分水得到萃取剂和废水，所述精馏塔(4)塔釜所得除水的丁烯酮引入所述油层受罐(8)中；
    (ii)当待萃取干燥的含水丁烯酮的密度小于萃取剂的密度时，所述连续萃取干燥方法在权利要求1～8中任意一项中第(ii)种连续萃取干燥装置中进行且包括：将所述含水丁烯酮和萃取剂分别从所述下部进料口和上部进料口加入所述萃取塔(1)中进行混合、萃取，所述萃取塔(1)塔顶所得废水外排且塔底所得含萃取剂的有机油层从所述油层静置段出口引出并进入所述精馏塔(4)中进行精馏，所述精馏塔(4)塔顶所得含水和少量丁烯酮的萃取剂进入所述冷凝器(5)中进行冷凝，经冷凝的产物进入所述分水罐(6)中进行分水得到萃取剂和废水，所述精馏塔(4)塔釜所得除水的丁烯酮引入所述油层受罐(8)中；
    (i)和(ii)中所述萃取剂均应该满足以下三个条件：
    a、难溶或不溶于水，与所述含水丁烯酮互溶性好且不发生反应；
    b、带水效果好；
    c、沸点小于丁烯酮的常压沸点，且相差10℃以上。
  10. 根据权利要求9所述的丁烯酮的连续萃取干燥方法，其特征在于，所述含水丁烯酮中的水分含量为0.1～23wt％。
  11. 根据权利要求9所述的丁烯酮的连续萃取干燥方法，其特征在于，所述萃取剂的沸点与所述含水丁烯酮的沸点之差为15～50℃。
  12. 根据权利要求9所述的丁烯酮连续萃取干燥方法，其特征在于，所述萃取剂选自二氯甲烷、三氯甲烷、正己烷、石油醚、乙醚、甲基叔丁基醚和异丙醚中的至少一种。
  13. 根据权利要求9～12中任意一项所述的丁烯酮的连续萃取干燥方法，其特征在于，所述含水丁烯酮与萃取剂的进料体积比为1:(1～5)，优选为1:(1.5～4)，更优选为1:(1.5～3.0)。
  14. 根据权利要求9～12中任意一项所述的丁烯酮的连续萃取干燥方法，其特征在于，所述精馏塔(4)的塔釜采用蒸汽加热且塔釜温度控制在40～80℃。
  15. 根据权利要求14所述的丁烯酮的连续萃取干燥方法，其特征在于，所述精馏塔(4)的塔釜温度控制在45～75℃。
  16. 根据权利要求9～12中任意一项所述的丁烯酮的连续萃取干燥方法，其特征在于，所述精馏塔(4)的回流比控制在0.25～10。
  17. 根据权利要求16所述的丁烯酮的连续萃取干燥方法，其特征在于，所述精馏塔(4)的回流比控制在0.5～5。
PCT/CN2020/093915 2019-07-26 2020-06-02 一种丁烯酮的连续萃取干燥装置和方法 WO2021017620A1 (zh)

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