CN105348041A - Method for separation of n-hexane-isopropanol constant boiling system through multilevel cross flow liquid-liquid extraction - Google Patents

Method for separation of n-hexane-isopropanol constant boiling system through multilevel cross flow liquid-liquid extraction Download PDF

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CN105348041A
CN105348041A CN201510889475.5A CN201510889475A CN105348041A CN 105348041 A CN105348041 A CN 105348041A CN 201510889475 A CN201510889475 A CN 201510889475A CN 105348041 A CN105348041 A CN 105348041A
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extraction
liquid
hexane
virahol
normal hexane
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林军
苏佳伟
汤良燕
尹小军
王文彬
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Nanjing Normal University
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    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/86—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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Abstract

本发明公开了一种多级错流液液萃取分离正己烷－异丙醇恒沸体系的方法，包括以下步骤：以水为萃取剂，对正己烷和异丙醇混合液进行多级错流液液萃取；萃余相经正己烷精制塔处理后，得到正己烷；萃取相经异丙醇精制塔处理之后，异丙醇精制塔塔顶得到异丙醇，塔底得到萃取剂水循环使用。本发明的多级错流液液萃取分离方法能够有效的分离正己烷和异丙醇混合液，经过精制后，可得到含量在99.9wt％以上的正己烷以及含量在99.5wt％以上的异丙醇，产品回收率达到97％以上；本发明方法分离产品纯度高，能耗低，整个工艺过程成本低，不会造成任何环境污染。

The invention discloses a method for multistage cross-flow liquid-liquid extraction and separation of n-hexane-isopropanol azeotropic system. Liquid-liquid extraction; after the raffinate phase is treated by a n-hexane refining tower, n-hexane is obtained; after the extract phase is treated by an isopropanol refining tower, isopropanol is obtained from the top of the isopropanol refining tower, and the extractant water is obtained from the bottom of the tower for recycling. The multi-stage cross-flow liquid-liquid extraction and separation method of the present invention can effectively separate n-hexane and isopropanol mixed liquid, and after refining, n-hexane with a content of more than 99.9 wt% and isopropanol with a content of more than 99.5 wt% can be obtained Alcohol, the product recovery rate reaches more than 97%; the method of the invention has high purity of separated products, low energy consumption, low cost of the whole process, and will not cause any environmental pollution.

Description

一种多级错流液液萃取分离正己烷－异丙醇恒沸体系的方法A method for separating n-hexane-isopropanol azeotropic system by multistage cross-flow liquid-liquid extraction

技术领域technical field

本发明涉及一种正己烷－异丙醇恒沸体系的分离方法，特别是一种多级错流液液萃取分离正己烷－异丙醇恒沸体系的方法。The invention relates to a separation method for a constant boiling system of n-hexane-isopropanol, in particular to a method for separating the constant-boiling system of n-hexane-isopropanol through multistage cross-flow liquid-liquid extraction.

背景技术Background technique

正己烷、异丙醇都是重要的化工原料，也都是性能优良、效果理想的低沸点有机溶剂，广泛用于炼油、染料、涂料、粘合剂、医药及电子等行业，应用领域十分广泛，近年来世界各国对其消费量急剧增加。Both n-hexane and isopropanol are important chemical raw materials, and they are also low-boiling organic solvents with excellent performance and ideal effects. They are widely used in oil refining, dyes, coatings, adhesives, pharmaceuticals, and electronics industries. They have a wide range of applications , In recent years, countries all over the world have sharply increased their consumption.

在大量的工业生产过程中正己烷和异丙醇都同时作为溶剂使用，不可避免会产生两者的混合废液，由于正己烷和异丙醇在常温下就会互溶，蒸馏时又形成恒沸体系(质量组成为77％正己烷、23％异丙醇)，给正己烷-异丙醇混合液的分离带来了困难，普通精馏方式难以同时得到高纯度正己烷、异丙醇产品。因此开发有效的分离工艺，不仅有利于提高产品的纯度、降低生产能耗并且能够进一步提高这类溶剂的利用效率。In a large number of industrial production processes, both n-hexane and isopropanol are used as solvents at the same time, and the mixed waste liquid of the two will inevitably be produced. Since n-hexane and isopropanol will dissolve each other at room temperature, they will form constant boiling during distillation. The system (mass composition is 77% n-hexane, 23% isopropanol) has brought difficulties to the separation of n-hexane-isopropanol mixed liquid, and it is difficult to obtain high-purity n-hexane and isopropanol products simultaneously by common rectification methods. Therefore, the development of an effective separation process is not only conducive to improving the purity of the product, reducing production energy consumption and further improving the utilization efficiency of such solvents.

发明内容Contents of the invention

本发明的目的是提供一种多级错流液液萃取分离正己烷-异丙醇恒沸体系的方法。所述方法克服了正己烷-异丙醇混合溶液分离所存在的上述困难，原料液经液液萃取后，可一次得到99.5％以上的正己烷，同时萃取相脱水后得到99.5％以上的异丙醇。所述方法不仅产品纯度更高，同时萃取剂循环使用，有利于降低物耗能耗。The purpose of the present invention is to provide a method for multistage cross-flow liquid-liquid extraction and separation of n-hexane-isopropanol azeotropic system. The method overcomes the above-mentioned difficulties in the separation of n-hexane-isopropanol mixed solution. After liquid-liquid extraction of the raw material liquid, more than 99.5% of n-hexane can be obtained at one time, and at the same time, more than 99.5% of isopropyl alcohol can be obtained after dehydration of the extraction phase. alcohol. The method not only has higher product purity, but also recycles the extraction agent, which is beneficial to reducing material consumption and energy consumption.

完成上述发明的技术方案是：The technical scheme for accomplishing the above invention is:

一种多级错流液液萃取分离正己烷－异丙醇恒沸体系的方法，步骤如下：A method for separating n-hexane-isopropanol azeotropic system by multistage cross-flow liquid-liquid extraction, the steps are as follows:

原料为正己烷和异丙醇混合液，以水为萃取剂，对正己烷和异丙醇混合液进行多级错流液液萃取；萃余相得到正己烷，萃取相经异丙醇精制塔处理之后，异丙醇精制塔塔顶得到异丙醇，异丙醇精制塔塔底得到萃取剂水，循环使用。The raw material is a mixture of n-hexane and isopropanol, and water is used as the extractant to perform multi-stage cross-flow liquid-liquid extraction on the mixture of n-hexane and isopropanol; the raffinate phase is obtained from n-hexane, and the extraction phase is passed through an isopropanol refining tower After the treatment, isopropanol is obtained from the top of the isopropanol refining tower, and extractant water is obtained from the bottom of the isopropanol refining tower for recycling.

本发明采用液液萃取分离正己烷－异丙醇恒沸体系，需要选择一种萃取剂(S)难溶于正己烷，易溶于异丙醇，本发明的萃取剂为水。The present invention adopts liquid-liquid extraction to separate n-hexane-isopropanol azeotropic system, and it is necessary to select an extractant (S) that is hardly soluble in n-hexane and easily soluble in isopropanol, and the extractant of the present invention is water.

所述方法中，萃余相得到的正己烷含量在99.5wt％以上，萃余相经正己烷精制塔处理后，得到含量在99.9wt％以上的正己烷。In the method, the n-hexane content obtained from the raffinate phase is above 99.5 wt%, and the raffinate phase is treated in a n-hexane refining tower to obtain n-hexane with a content above 99.9 wt%.

所述方法中，原料正己烷和异丙醇混合液，可以是正己烷和异丙醇任意比例的混合溶液；特别地，推荐本发明方法用于正己烷和异丙醇的恒沸体系，其中包含77wt％的正己烷和23wt％的异丙醇。In the described method, raw material n-hexane and isopropanol mixed solution can be the mixed solution of normal hexane and isopropanol in any ratio; Especially, it is recommended that the inventive method be used for the azeotropic system of normal hexane and isopropanol, wherein Contains 77 wt% n-hexane and 23 wt% isopropanol.

本发明方法多级错流液液萃取通常可进行2-5级萃取，优选为3级错流萃取。每一级萃取操作时，常温下将原料正己烷和异丙醇混合液与萃取剂混合搅拌1h，搅拌轴转速为100转/分钟，静置1h后分层，可进行下一级处理。The multistage cross-flow liquid-liquid extraction of the method of the present invention can usually carry out 2-5 stages of extraction, preferably 3 stages of cross-flow extraction. During each stage of extraction operation, the mixture of raw materials n-hexane and isopropanol is mixed with the extractant at room temperature for 1 hour, the rotation speed of the stirring shaft is 100 rpm, and the layers are separated after standing for 1 hour, and the next stage of treatment can be carried out.

所述方法中，每一级萃取中，所述萃取剂与原料的质量比为：0.5∶1～5∶1，其中，最佳比例为1∶1。In the method, in each stage of extraction, the mass ratio of the extractant to the raw material is: 0.5:1-5:1, wherein the optimum ratio is 1:1.

所述方法中，正己烷和异丙醇混合液经多级错流液液萃取，萃余相为含量≥99.5wt％的正己烷，萃余相经正己烷精制塔处理后，得到含量在99.9wt％以上的正己烷，回收率达到97％以上；萃取相为水和异丙醇的混合物，经异丙醇精制塔处理之后，异丙醇精制塔塔顶得到含量在99.5wt％以上的异丙醇，异丙醇精制塔塔底得到萃取剂水，循环利用。In the method, the mixture of n-hexane and isopropanol is subjected to multistage cross-flow liquid-liquid extraction, the raffinate phase is n-hexane with a content ≥ 99.5 wt%, and the raffinate phase is treated with a n-hexane refining tower to obtain a content of 99.9% Wt% or more normal hexane, the recovery rate reaches more than 97%; the extraction phase is a mixture of water and isopropanol, after being treated in the isopropanol refining tower, the isopropanol refining tower top obtains isopropanol with a content of more than 99.5wt%. Propanol and isopropanol are purified at the bottom of the tower to obtain extractant water for recycling.

本发明的优点：本发明方法采用图1所示工艺流程和优化的工艺参数，以水为萃取剂，原料正己烷和异丙醇混合液经多级错流液液萃取，萃余相经正己烷精制塔处理后，得到纯度在99.9wt％以上的正己烷；萃取相经异丙醇精制塔处理之后，异丙醇精制塔塔顶得到纯度在99.5wt％以上的异丙醇，异丙醇精制塔塔底得到萃取剂水循环利用。本发明的分离方法与现有技术中的普通蒸馏、共沸精馏等方法相比，分离效果更加明显，分离得到的正己烷、异丙醇产品纯度更高，回收率更高(＞97％)，能耗更低。整个分离工艺过程以水为萃取溶剂，成本较低，而且不会造成环境污染。Advantages of the present invention: the method of the present invention adopts the process flow shown in Figure 1 and the optimized process parameters, water is used as the extraction agent, the raw material n-hexane and isopropanol mixture is subjected to multi-stage cross-flow liquid-liquid extraction, and the raffinate is extracted by n-hexane After the alkane refining tower is processed, obtain the normal hexane that purity is more than 99.9wt%; The extraction agent water is recycled from the bottom of the refining tower. Compared with methods such as ordinary distillation and azeotropic distillation in the prior art, the separation method of the present invention has more obvious separation effects, and the normal hexane and Virahol products obtained by separation have higher purity and higher recovery (>97%) ), lower energy consumption. The whole separation process uses water as the extraction solvent, which has low cost and will not cause environmental pollution.

附图说明Description of drawings

图1为多级错流液液萃取分离方法的工艺流程图。Figure 1 is a process flow diagram of a multistage cross-flow liquid-liquid extraction separation method.

具体实施方式detailed description

本发明所述的一种多级错流液液萃取分离正己烷－异丙醇恒沸体系的方法，采用多级错流萃取与精制塔相结合的处理工艺，工艺流程图如图1所示，其中Ⅰ为萃取釜Ⅰ，Ⅱ为萃取釜Ⅱ，Ⅲ为萃取釜Ⅲ，Ⅳ为正己烷精制塔，Ⅴ为异丙醇精制塔；以F表示原料，S表示萃取剂，R表示萃余相，E表示萃取相，工艺流程中涉及的主要流股包括，S为萃取剂水，①为原料，②为萃取釜Ⅰ萃余相，③为萃取釜Ⅱ萃余相，④为萃取釜Ⅲ萃余相，⑤为萃取釜Ⅰ萃取相，⑥为萃取釜Ⅱ萃取相，⑦为萃取釜Ⅲ萃取相，⑧为正己烷精制塔Ⅳ塔顶出料，⑨为正己烷精制塔Ⅳ塔釜出料，⑩为异丙醇精制塔Ⅴ塔顶出料，为异丙醇精制塔Ⅴ塔釜出料。A method for separating n-hexane-isopropanol azeotropic system by multi-stage cross-flow liquid-liquid extraction according to the present invention adopts a treatment process combining multi-stage cross-flow extraction and refining tower, and the process flow chart is shown in Figure 1 , where I is the extraction tank I, II is the extraction tank II, III is the extraction tank III, IV is the n-hexane refining tower, and V is the isopropanol refining tower; F represents the raw material, S represents the extraction agent, and R represents the raffinate phase , E represents the extraction phase, the main streams involved in the process flow include, S is the extraction agent water, ① is the raw material, ② is the raffinate phase of the extraction tank I, ③ is the raffinate phase of the extraction tank II, and ④ is the extraction phase of the extraction tank III The remaining phase, ⑤ is the extraction phase of the extraction tank I, ⑥ is the extraction phase of the extraction tank II, ⑦ is the extraction phase of the extraction tank III, ⑧ is the output from the top of the n-hexane refining tower IV, and ⑨ is the output from the bottom of the n-hexane refining tower IV , ⑩ is the top discharge of isopropanol refining tower V, It is the output from the bottom of the isopropanol refining tower V.

实施例1：Example 1:

参照图1所示工艺流程和表1所示工艺参数，采用3级错流液液萃取分离正己烷与异丙醇的混合液F(流股①)，其中正己烷与异丙醇的质量含量分别为77％、23％，以水为萃取剂，其中每一级萃取剂与原料的质量比均为1:1。原料正己烷与异丙醇混合液F(流股①)，以流量为5Kg/h，进入萃取釜Ⅰ，同时将萃取剂水S以流量5Kg/h加入萃取釜Ⅰ，经搅拌1小时(搅拌轴转速100转/分钟)、静置1小时后得到的萃余相R1(流股②)；将萃取釜Ⅰ得到的萃余相R1(流股②)以流量为3.9Kg/h加入萃取釜Ⅱ，同时加入的还有萃取剂水S，流量为3.9Kg/h，经搅拌1小时(搅拌轴转速100转/分钟)、静置1小时后得到的萃余相R2(流股③)；将萃取釜Ⅱ得到的萃余相R2(流股③)以流量为3.8Kg/h加入萃取釜Ⅲ，同时加入的还有萃取剂水S，流量为3.8Kg/h，经搅拌1小时(搅拌轴转速100转/分钟)、静置1小时后得到的萃余相R3(流股④)；将萃取釜Ⅲ得到的萃余相R3(流股④)以流量为3.7Kg/h加入正己烷精制塔Ⅳ，正己烷精制塔Ⅳ塔顶出料⑧为含量在99.9wt％以上的正己烷，其流量为3.5Kg/h，正己烷精制塔Ⅳ塔釜出料⑨为含量在98.9wt％以上的正己烷，其流量为0.2Kg/h，可回收利用。萃取釜Ⅰ、Ⅱ、Ⅲ中得到的萃取相分别为E1(流股⑤、流量为6.1Kg/h)、E2(流股⑥、流量为4.0Kg/h)、E3(流股⑦、流量为3.9Kg/h)，合并后进入异丙醇精制塔Ⅴ，异丙醇精制塔Ⅴ塔顶出料⑩为含量在99.9wt％以上的异丙醇，其流量为1.3Kg/h，异丙醇精制塔Ⅴ塔釜出料为含量在99.5wt％以上的萃取剂水，其流量为12.7Kg/h，萃取剂水可循环使用。正己烷和异丙醇的回收率可以达到97％以上。With reference to the process flow shown in Figure 1 and the process parameters shown in Table 1, adopt 3 stages of cross-flow liquid-liquid extraction to separate the mixed solution F (stream ①) of n-hexane and Virahol, wherein the mass content of n-hexane and Virahol 77% and 23% respectively, water is used as the extractant, and the mass ratio of each stage of extractant to raw material is 1:1. The raw material n-hexane and isopropanol mixed liquid F (stream ①) enters the extraction kettle I at a flow rate of 5Kg/h, and simultaneously adds the extractant water S into the extraction kettle I at a flow rate of 5Kg/h, and stirs for 1 hour (stirring shaft speed 100 rev/min), the raffinate phase R 1 (stream ②) obtained after standing for 1 hour; the raffinate phase R 1 (stream ②) obtained by the extraction kettle Ⅰ was added with a flow rate of 3.9Kg/h Extraction kettle II also added extractant water S at the same time, and the flow rate was 3.9Kg/h. The raffinate phase R obtained after stirring for 1 hour (stirrer shaft speed 100 rpm) and standing for 1 hour (stream ③); the raffinate phase R2 ( stream ③) obtained by the extraction kettle II is added to the extraction kettle III at a flow rate of 3.8Kg/h, and the extraction agent water S is also added at the same time, and the flow rate is 3.8Kg/h. After stirring 1 hour (stirrer shaft speed 100 rev/min), the raffinate phase R obtained after standing for 1 hour 3 (stream ④); Kg/h is added to n-hexane refining tower IV, and the output ⑧ from the top of n-hexane refining tower IV is normal hexane with a content of more than 99.9 wt%, and its flow rate is 3.5Kg/h, and the output ⑨ from the bottom of n-hexane refining tower IV is The flow rate of n-hexane with a content of more than 98.9 wt% is 0.2Kg/h, which can be recycled. The extraction phases obtained in extraction kettles I, II, and III are respectively E 1 (stream ⑤, flow rate is 6.1Kg/h), E 2 (stream stream ⑥, flow rate is 4.0Kg/h), E 3 (stream stream ⑦ , flow rate is 3.9Kg/h), enters Virahol refining tower Ⅴ after merging, and Virahol refining tower Ⅴ tower top discharge ⑩ is the Virahol that content is more than 99.9wt%, and its flow rate is 1.3Kg/h, Discharge of isopropanol refining tower V tower kettle It is the extractant water whose content is more than 99.5wt%, its flow rate is 12.7Kg/h, and the extractant water can be recycled. The recovery rate of n-hexane and isopropanol can reach more than 97%.

表1：萃取釜工艺条件Table 1: Extraction kettle process conditions

工艺参数Process parameters 萃取釜ⅠExtraction kettle Ⅰ 萃取釜ⅡExtraction kettle Ⅱ 萃取釜ⅢExtraction kettle Ⅲ 搅拌时间Stiring time 1小时1 hour 1小时1 hour 1小时1 hour 静止时间still time 1小时1 hour 1小时1 hour 1小时1 hour 搅拌轴转速Stirring shaft speed 100转/分钟100 rpm 100转/分钟100 rpm 100转/分钟100 rpm 操作温度operating temperature 常温room temperature 常温room temperature 常温room temperature

表2：错流液液萃取分离结果Table 2: Separation results of cross-flow liquid-liquid extraction

实施例2Example 2

与实施例1基本相同，不同之处在于，任意一级萃取中，萃取剂与原料质量比为2：1。It is basically the same as Example 1, except that in any stage of extraction, the mass ratio of extractant to raw material is 2:1.

实施例3Example 3

与实施例1基本相同，不同之处在于，任意一级萃取中，萃取剂与原料质量比为3：1。It is basically the same as Example 1, except that in any stage of extraction, the mass ratio of extractant to raw material is 3:1.

实施例4Example 4

与实施例1基本相同，不同之处在于萃取级数为4级。It is basically the same as Example 1, except that the number of extraction stages is 4.

Claims (6)

1. multistage cross flow liquid-liquid extraction is separated a method for normal hexane-Virahol azeotropic system, and step is as follows: raw material is normal hexane and Virahol mixed solution, take water as extraction agent, carries out multistage cross flow liquid-liquid extraction to normal hexane and Virahol mixed solution; Extracting phase obtains normal hexane; Extraction phase is after the process of Virahol treating tower, and Virahol treating tower tower top obtains Virahol, is extracted agent water, recycles at the bottom of Virahol treating tower tower.
2. a kind of multistage cross flow liquid-liquid extraction according to claim 1 is separated the method for normal hexane-Virahol azeotropic system, it is characterized in that, the normal hexane content that described extracting phase obtains is at more than 99.5wt%, extracting phase, after the process of normal hexane treating tower, obtains the normal hexane of content at more than 99.9wt%.
3. a kind of multistage cross flow liquid-liquid extraction according to claim 1 is separated the method for normal hexane-Virahol azeotropic system, and it is characterized in that, described raw material is the azeotrope of normal hexane and Virahol, the normal hexane containing 77wt% and the Virahol of 23wt%.
4. a kind of multistage cross flow liquid-liquid extraction according to claim 1 is separated the method for normal hexane-Virahol azeotropic system, and it is characterized in that, the extraction of 2-5 level is carried out in described multistage cross flow liquid-liquid extraction.
5. a kind of multistage cross flow liquid-liquid extraction according to claim 1 is separated the method for normal hexane-Virahol azeotropic system, it is characterized in that, the processing condition of any one-level extraction of described multistage cross flow liquid-liquid extraction are, by raw material normal hexane and Virahol mixed solution and extraction agent mix and blend 1h, agitator shaft speed is 100 revs/min, layering after standing 1h.
6. a kind of multistage cross flow liquid-liquid extraction according to claim 1 is separated the method for normal hexane-Virahol azeotropic system, it is characterized in that, in any one-level extraction, the mass ratio of described extraction agent and raw material is: 0.5 ~ 5: 1.
CN201510889475.5A 2015-12-07 2015-12-07 Method for separation of n-hexane-isopropanol constant boiling system through multilevel cross flow liquid-liquid extraction Pending CN105348041A (en)

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