CN111514613A - Alkali liquor separation system and cyclohexanone preparation system - Google Patents
Alkali liquor separation system and cyclohexanone preparation system Download PDFInfo
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- 239000003513 alkali Substances 0.000 title claims abstract description 93
- 238000000926 separation method Methods 0.000 title claims abstract description 55
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 150
- 239000007788 liquid Substances 0.000 claims abstract description 106
- 150000002500 ions Chemical class 0.000 claims abstract description 38
- 238000005406 washing Methods 0.000 claims abstract description 23
- 239000012071 phase Substances 0.000 claims description 119
- 238000001802 infusion Methods 0.000 claims description 26
- 239000013505 freshwater Substances 0.000 claims description 11
- 239000008346 aqueous phase Substances 0.000 claims description 7
- 239000003518 caustics Substances 0.000 claims 1
- 238000007865 diluting Methods 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract description 5
- 235000019198 oils Nutrition 0.000 description 35
- 238000000034 method Methods 0.000 description 16
- 239000000243 solution Substances 0.000 description 13
- 230000008569 process Effects 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 235000019476 oil-water mixture Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- HGCIXCUEYOPUTN-UHFFFAOYSA-N cyclohexene Chemical compound C1CCC=CC1 HGCIXCUEYOPUTN-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/12—Auxiliary equipment particularly adapted for use with liquid-separating apparatus, e.g. control circuits
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C49/00—Ketones; Ketenes; Dimeric ketenes; Ketonic chelates
- C07C49/385—Saturated compounds containing a keto group being part of a ring
- C07C49/403—Saturated compounds containing a keto group being part of a ring of a six-membered ring
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明实施例提供一种碱液分离系统及环己酮制备系统，该碱液分离系统包括第一碱液分离器、第一混合器、第二碱液分离器、第二混合器和第三碱液分离器，其中，第一碱液分离器用于对待分离液进行油水分离；第一混合器的进液口分别与第一碱液分离器的油相出口、第二碱液分离器的水相出口以及第三碱液分离器的水相出口连接；第二碱液分离器的进液口与第一混合器的出液口连接；第二混合器的进液口分别与第二碱液分离器的油相出口、第三碱液分离器的水相出口以及外部供水系统连接；第三碱液分离器的进液口与第二混合器的出液口连接。该碱液分离系统通过对洗水进行循环利用和稀释，既降低了耗水量，又使各个碱液分离器保持了较高的碱离子去除率。
The embodiment of the present invention provides a lye separation system and a cyclohexanone preparation system, the lye separation system includes a first lye separator, a first mixer, a second lye separator, a second mixer and a third lye separator A lye separator, wherein the first lye separator is used for oil-water separation of the liquid to be separated; the liquid inlet of the first mixer is respectively connected with the oil phase outlet of the first lye separator and the water of the second lye separator The phase outlet and the water phase outlet of the third lye separator are connected; the liquid inlet of the second lye separator is connected with the liquid outlet of the first mixer; the liquid inlet of the second mixer is respectively connected with the second lye liquid The oil phase outlet of the separator, the water phase outlet of the third alkaline liquid separator and the external water supply system are connected; the liquid inlet of the third alkaline liquid separator is connected with the liquid outlet of the second mixer. By recycling and diluting the washing water, the lye separation system not only reduces the water consumption, but also maintains a high alkali ion removal rate for each lye separator.
Description
技术领域technical field
本发明实施例涉及环己酮制备技术领域，尤其涉及一种碱液分离系统及环己酮制备系统。The embodiments of the present invention relate to the technical field of cyclohexanone preparation, and in particular, to a lye separation system and a cyclohexanone preparation system.
背景技术Background technique
环己酮作为一种重要的化工产品，是生产己二酸、己内酰胺的重要原料。目前世界上生产环己酮的工艺主要有苯酚法、环己烷氧化法和环己烯法三种，其中工业上70％以上的环己酮生产厂家采用的是环己烷氧化法工艺。该工艺主要包括氧化、分解、废碱分离、烷精馏、皂化、精制、脱氢及热回收等工序，其中，氧化工序会产生废碱液，如果废碱液随物料进入到烷精馏工艺，会导致再沸器的列管结垢，致使再沸器换热效率降低，环己烷回收系统动力不足，当再沸器结垢严重到一定程度时，整个环己酮生产系统就会被迫停车清洗，造成能耗升高。碱液中的碱离子，是有机物缩合的催化剂，如果物料中碱离子含量较高，在高温条件下，会促进有机物缩合反应，进而生产大量副产物，物耗也会升高。现有的废碱分离系统要么分离效率较低，要么耗水量较大。As an important chemical product, cyclohexanone is an important raw material for the production of adipic acid and caprolactam. At present, there are three main processes for producing cyclohexanone in the world: phenol method, cyclohexane oxidation method and cyclohexene method. Among them, more than 70% of cyclohexanone manufacturers in the industry use the cyclohexane oxidation method. The process mainly includes oxidation, decomposition, waste alkali separation, alkane rectification, saponification, refining, dehydrogenation and heat recovery. Among them, the oxidation process will generate waste lye, if the waste lye enters the alkane rectification process with the material , it will lead to the fouling of the reboiler tubes, resulting in the reduction of the heat exchange efficiency of the reboiler and the insufficient power of the cyclohexane recovery system. When the scale of the reboiler is serious to a certain extent, the entire cyclohexanone production system will be destroyed. Forced to stop for cleaning, resulting in increased energy consumption. The alkali ions in the lye solution are catalysts for the condensation of organic substances. If the content of alkali ions in the material is high, the condensation reaction of organic substances will be promoted under high temperature conditions, and a large number of by-products will be produced, and the material consumption will also increase. The existing spent alkali separation systems either have low separation efficiency or consume large amounts of water.
发明内容SUMMARY OF THE INVENTION
有鉴于现有技术中存在的上述问题，本发明实施例提供了一种耗水量较低且分离效率较高的碱液分离系统及应用该碱液分离系统的环己酮制备系统。In view of the above problems existing in the prior art, the embodiments of the present invention provide an alkali liquid separation system with low water consumption and high separation efficiency, and a cyclohexanone preparation system using the alkali liquid separation system.
为实现上述目的，本发明实施例一方面提供了一种碱液分离系统，其包括第一碱液分离器、第一混合器、第二碱液分离器、第二混合器和第三碱液分离器，其中：In order to achieve the above purpose, one aspect of the embodiments of the present invention provides a lye separation system, which includes a first lye separator, a first mixer, a second lye separator, a second mixer and a third lye separator, where:
所述第一碱液分离器的进液口用于接收待分离液，所述待分离液包含油相、水相及掺杂在油相和水相中的碱离子，所述第一碱液分离器用于对所述待分离液进行油水分离，并将分离获得的溶解有部分碱离子的水相从所述第一碱液分离器的水相出口排出；The liquid inlet of the first alkali liquid separator is used to receive the liquid to be separated, and the liquid to be separated includes an oil phase, a water phase and alkali ions doped in the oil phase and the water phase, and the first alkali liquid The separator is used to separate the oil and water of the liquid to be separated, and discharge the water phase obtained by the separation in which some alkali ions are dissolved from the water phase outlet of the first alkali liquid separator;
所述第一混合器的进液口分别与所述第一碱液分离器的油相出口、所述第二碱液分离器的水相出口以及所述第三碱液分离器的水相出口连接，所述第一混合器用于接收所述第一碱液分离器输出的油相、所述第二碱液分离器输出的水相以及所述第三碱液分离器输出的水相，并对三者进行混合以使油相中的碱离子溶解于水相中；The liquid inlet of the first mixer is respectively connected with the oil phase outlet of the first lye separator, the water phase outlet of the second lye separator and the water phase outlet of the third lye separator connected, the first mixer is configured to receive the oil phase output from the first lye separator, the water phase output from the second lye separator and the water phase output from the third lye separator, and The three are mixed to dissolve the alkali ions in the oil phase in the water phase;
所述第二碱液分离器的进液口与所述第一混合器的出液口连接，用于接收所述第一混合器输出的油水混合液并进行油水分离；The liquid inlet of the second lye separator is connected with the liquid outlet of the first mixer, and is used for receiving the oil-water mixed liquid output by the first mixer and performing oil-water separation;
所述第二混合器的进液口分别与所述第二碱液分离器的油相出口、所述第三碱液分离器的水相出口以及外部供水系统连接，所述第二混合器用于接收所述第二碱液分离器输出的油相、所述第三碱液分离器输出的水相以及外部供水系统输送的新鲜水，并对三者进行混合以使油相中的碱离子溶解于水相中；The liquid inlet of the second mixer is respectively connected with the oil phase outlet of the second lye separator, the water phase outlet of the third lye separator and the external water supply system, and the second mixer is used for Receive the oil phase output from the second lye separator, the water phase output from the third lye separator and the fresh water delivered by the external water supply system, and mix the three to dissolve the alkali ions in the oil phase in the water phase;
所述第三碱液分离器的进液口与所述第二混合器的出液口连接，用于接收所述第二混合器输出的油水混合液并进行油水分离，将分离后的油相从所述第三碱液分离器的油相出口排出。The liquid inlet of the third lye separator is connected with the liquid outlet of the second mixer, for receiving the oil-water mixed liquid output by the second mixer and separating oil and water, and separating the separated oil phase It is discharged from the oil phase outlet of the third lye separator.
在一些实施例中，所述碱液分离系统还包括：In some embodiments, the lye separation system further includes:
第一输液泵，其连接在所述第一混合器的进液口和所述第二碱液分离器的水相出口之间，用于将所述第二碱液分离器输出的水相输送至所述第一混合器。The first infusion pump, which is connected between the liquid inlet of the first mixer and the water phase outlet of the second lye separator, is used to transport the water phase output from the second lye separator to the first mixer.
在一些实施例中，所述第一输液泵还与外部碱液配置系统连接，以将所述第二碱液分离器输出的部分水相输送至外部碱液配置系统。In some embodiments, the first infusion pump is further connected to an external lye dispensing system to deliver part of the aqueous phase output from the second lye separator to the external lye dispensing system.
在一些实施例中，所述第一输液泵向所述第一混合器输送水相的流速为20-50m3/h；所述第一输液泵向外部碱液配置系统输送水相的流速为4-8m3/h。In some embodiments, the flow rate of the first infusion pump to deliver the water phase to the first mixer is 20-50 m 3 /h; the flow rate of the first infusion pump to deliver the water phase to the external alkali solution configuration system is 4-8m 3 /h.
在一些实施例中，所述碱液分离系统还包括：In some embodiments, the lye separation system further includes:
第二输液泵，其分别与所述第一混合器的进液口、所述第二混合器的进液口和所述第三碱液分离器的水相出口连接，用于将所述第三碱液分离器输出的水相分别输送至所述第一混合器和所述第二混合器。A second infusion pump, which is respectively connected with the liquid inlet of the first mixer, the liquid inlet of the second mixer and the water phase outlet of the third lye separator, and is used for connecting the first mixer The water phase output from the three lye separators is respectively sent to the first mixer and the second mixer.
在一些实施例中，所述第二输液泵向所述第一混合器输送水相的流速为2-6m3/h，所述第二输液泵向所述第二混合器输送水相的流速为20-50m3/h。In some embodiments, the second infusion pump delivers the water phase to the first mixer at a flow rate of 2-6 m 3 /h, and the second infusion pump delivers the water phase to the second mixer at a flow rate of 2-6
在一些实施例中，所述第一碱液分离器、所述第二碱液分离器和所述第三碱液分离器均为碱洗油水分离罐。In some embodiments, the first alkaline liquid separator, the second alkaline liquid separator and the third alkaline liquid separator are all alkaline washing oil-water separation tanks.
在一些实施例中，所述第一碱液分离器的水相出口与外部碱液配制系统连接，以将溶解有碱离子的水相输送至外部碱液配制系统。In some embodiments, the water phase outlet of the first lye separator is connected to an external lye preparation system, so as to deliver the aqueous phase in which the alkali ions are dissolved to the external lye preparation system.
在一些实施例中，所述外部供水系统向所述第二混合器输送新鲜水的流速为1-3m3/h。In some embodiments, the external water supply system delivers fresh water to the second mixer at a flow rate of 1-3 m 3 /h.
本发明实施例另一方面还提供了一种环己酮制备系统，其包括如上所述的碱液分离系统。Another aspect of the embodiments of the present invention also provides a system for preparing cyclohexanone, which includes the above-mentioned alkali liquid separation system.
与现有技术相比，本发明实施例的碱液分离系统，待分离液经第一碱液分离器进行油水分离后，水相自第一碱液分离器的水相出口排出，油相进入到第一混合器，与第二碱液分离器的洗水和第三碱液分离器的洗水混合，通过对第二碱液分离器的洗水和第三碱液分离器的洗水进行循环利用，能够节省水资源利用率，而且，由于第三碱液分离器的洗水中碱离子浓度较低，能够起到对第二碱液分离器的洗水进行稀释的作用，以使第二碱液分离器具有较高的碱离子去除率。油水混合物经第二碱液分离器进行油水分离后，水相自第二碱液分离器的水相出口排出循环利用，油相进入到第二混合器，与第三碱液分离器的洗水和外部供水系统的新鲜水混合，通过补入新鲜水，能够保证第三碱液分离器具有较高的碱离子去除率。该碱液分离系统通过对洗水进行循环利用和稀释，既降低了耗水量，又使各个碱液分离器保持了较高的碱离子去除率。Compared with the prior art, in the lye separation system of the embodiment of the present invention, after the separation liquid is separated from oil and water by the first lye separator, the water phase is discharged from the water phase outlet of the first lye separator, and the oil phase enters the first lye separator. To the first mixer, it is mixed with the washing water of the second lye separator and the washing water of the third lye separator, and is carried out by the washing water of the second lye separator and the washing water of the third lye separator. Recycling can save the utilization rate of water resources, and because the concentration of alkali ions in the washing water of the third lye separator is low, it can play the role of diluting the washing water of the second lye separator, so that the second The lye separator has a high alkali ion removal rate. After the oil-water mixture is separated from oil and water by the second lye separator, the water phase is discharged from the water phase outlet of the second lye separator for recycling, and the oil phase enters the second mixer, which is combined with the washing water of the third lye separator. It is mixed with the fresh water of the external water supply system, and by replenishing the fresh water, it can ensure that the third lye separator has a higher alkali ion removal rate. By recycling and diluting the washing water, the lye separation system not only reduces the water consumption, but also maintains a high alkali ion removal rate for each lye separator.
应当理解，前面的一般描述和以下详细描述都仅是示例性和说明性的，而不是用于限制本发明。It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not intended to limit the invention.
本发明文件提供本发明中描述的技术的各种实现或示例的概述，并不是所公开技术的全部范围或所有特征的全面公开。This disclosure document provides a summary of various implementations or examples of the technology described in this disclosure, and is not a comprehensive disclosure of the full scope or all features of the disclosed technology.
附图说明Description of drawings
在不一定按比例绘制的附图中，相同的附图标记可以在不同的视图中描述相似的部件。具有字母后缀或不同字母后缀的相同附图标记可以表示相似部件的不同实例。附图大体上通过举例而不是限制的方式示出各种实施例，并且与说明书以及权利要求书一起用于对所公开的实施例进行说明。在适当的时候，在所有附图中使用相同的附图标记指代同一或相似的部分。这样的实施例是例证性的，而并非旨在作为本装置或方法的穷尽或排他实施例。In the drawings, which are not necessarily to scale, the same reference numbers may describe similar parts in different views. The same reference number with a letter suffix or a different letter suffix may denote different instances of similar components. The drawings illustrate various embodiments generally by way of example and not limitation, and together with the specification and claims serve to explain the disclosed embodiments. Where appropriate, the same reference numbers will be used throughout the drawings to refer to the same or like parts. Such embodiments are illustrative, and are not intended to be exhaustive or exclusive embodiments of the present apparatus or method.
图1为本发明实施例的碱液分离系统的结构示意图。FIG. 1 is a schematic structural diagram of an alkali liquid separation system according to an embodiment of the present invention.
附图标记说明：Description of reference numbers:
1-第一碱液分离器；2-第一混合器；3-第二碱液分离器；4-第二混合器；5-第三碱液分离器；6-第一输液泵；7-第二输液泵。1- The first lye separator; 2- The first mixer; 3- The second lye separator; 4- The second mixer; 5- The third lye separator; 6- The first infusion pump; 7- Second infusion pump.
具体实施方式Detailed ways
为了使得本发明实施例的目的、技术方案和优点更加清楚，下面将结合本发明实施例的附图，对本发明实施例的技术方案进行清楚、完整地描述。显然，所描述的实施例是本发明的一部分实施例，而不是全部的实施例。基于所描述的本发明的实施例，本领域普通技术人员在无需创造性劳动的前提下所获得的所有其他实施例，都属于本发明保护的范围。In order to make the purposes, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be described clearly and completely below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are some, but not all, embodiments of the present invention. Based on the described embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the protection scope of the present invention.
除非另外定义，本发明使用的技术术语或者科学术语应当为本发明所属领域内具有一般技能的人士所理解的通常意义。本发明中使用的“第一”、“第二”以及类似的词语并不表示任何顺序、数量或者重要性，而只是用来区分不同的组成部分。“包括”或者“包含”等类似的词语意指出现该词前面的元件或者物件涵盖出现在该词后面列举的元件或者物件及其等同，而不排除其他元件或者物件。“连接”或者“相连”等类似的词语并非限定于物理的或者机械的连接，而是可以包括电性的连接，不管是直接的还是间接的。“上”、“下”、“左”、“右”等仅用于表示相对位置关系，当被描述对象的绝对位置改变后，则该相对位置关系也可能相应地改变。Unless otherwise defined, technical or scientific terms used in the present invention should have the ordinary meaning as understood by one of ordinary skill in the art to which the present invention belongs. The terms "first," "second," and similar terms used herein do not denote any order, quantity, or importance, but are merely used to distinguish different components. "Comprises" or "comprising" and similar words mean that the elements or things appearing before the word encompass the elements or things recited after the word and their equivalents, but do not exclude other elements or things. Words like "connected" or "connected" are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "Up", "Down", "Left", "Right", etc. are only used to represent the relative positional relationship, and when the absolute position of the described object changes, the relative positional relationship may also change accordingly.
为了保持本发明实施例的以下说明清楚且简明，本发明省略了已知功能和已知部件的详细说明。In order to keep the following description of the embodiments of the present invention clear and concise, the present invention omits detailed descriptions of well-known functions and well-known components.
图1为本发明实施例的碱液分离系统的结构示意图，参见图1所示，本发明实施例的碱液分离系统包括第一碱液分离器1、第一混合器2、第二碱液分离器3、第二混合器4和第三碱液分离器5，其中：FIG. 1 is a schematic structural diagram of an alkali liquid separation system according to an embodiment of the present invention. Referring to FIG. 1 , the alkali liquid separation system according to the embodiment of the present invention includes a first alkali liquid separator 1 , a first mixer 2 , and a second alkali liquid Separator 3, second mixer 4 and third lye separator 5, wherein:
第一碱液分离器1的进液口用于接收待分离液，待分离液包含油相、水相及掺杂在油相和水相中的碱离子。具体的，该待分离液可为环己酮生成过程中分解环节产生的料液，料液中包括环己烷等油相和碱液等水相，碱离子主要以钠离子为主，钠离子掺杂于油相和水相中，当然，该待分离液不仅限于环己酮生产过程中所产生的料液，也可为其他待分离液。第一碱液分离器1用于对待分离液进行油水分离，并将分离获得的溶解有碱离子的水相从第一碱液分离器1的水相出口排出。The liquid inlet of the first alkali liquid separator 1 is used to receive the liquid to be separated, and the liquid to be separated includes an oil phase, a water phase, and alkali ions doped in the oil phase and the water phase. Specifically, the to-be-separated liquid can be the feed liquid produced by the decomposition step in the cyclohexanone generation process. The feed liquid includes an oil phase such as cyclohexane and an aqueous phase such as alkali liquor. The alkali ions are mainly sodium ions, and the sodium ions are the main ones. Mixed in the oil phase and the water phase, of course, the liquid to be separated is not limited to the feed liquid produced in the production process of cyclohexanone, but can also be other liquids to be separated. The first alkali liquid separator 1 is used for oil-water separation of the liquid to be separated, and the water phase obtained by separation and dissolved with alkali ions is discharged from the water phase outlet of the first alkali liquid separator 1 .
第一混合器2的进液口分别与第一碱液分离器1的油相出口、第二碱液分离器3的水相出口以及第三碱液分离器5的水相出口连接，第一混合器2用于接收第一碱液分离器1输出的油相、第二碱液分离器3输出的水相以及第三碱液分离器5输出的水相，并对三者进行混合以使油相中的碱离子溶解于水相中。The liquid inlet of the first mixer 2 is respectively connected with the oil phase outlet of the first lye separator 1, the water phase outlet of the
第二碱液分离器3的进液口与第一混合器2的出液口连接，用于接收第一混合器2输出的油水混合液并进行油水分离。The liquid inlet of the
第二混合器4的进液口分别与第二碱液分离器3的油相出口、第三碱液分离器5的水相出口以及外部供水系统连接，第二混合器4用于接收第二碱液分离器3输出的油相、第三碱液分离器5输出的水相以及外部供水系统输送的新鲜水，并对三者进行混合以使油相中的碱离子溶解于水相中。The liquid inlet of the second mixer 4 is respectively connected with the oil phase outlet of the
第三碱液分离器5的进液口与第二混合器4的出液口连接，用于接收第二混合器4输出的油水混合液并进行油水分离，将分离后的油相从第三碱液分离器5的油相出口排出。在具体实施时，该第一碱液分离器1、第二碱液分离器3和第三碱液分离器5均可为碱洗油水分离罐。The liquid inlet of the third lye separator 5 is connected to the liquid outlet of the second mixer 4 for receiving the oil-water mixture output from the second mixer 4 and separating the oil and water, so as to separate the separated oil phase from the third The oil phase outlet of the lye separator 5 is discharged. In specific implementation, the first alkali liquid separator 1 , the second
采用上述结构的碱液分离系统，待分离液经第一碱液分离器1进行油水分离后，水相自第一碱液分离器1的水相出口排出，油相进入到第一混合器2，与第二碱液分离器3的洗水(也即油水分离获得的水相)和第三碱液分离器5的洗水混合，通过对第二碱液分离器3的洗水和第三碱液分离器5的洗水进行循环利用，能够节省水资源利用率，而且，由于第三碱液分离器5的洗水中碱离子浓度较低，能够起到对第二碱液分离器3的洗水进行稀释的作用，以使第二碱液分离器3具有较高的碱离子去除率。油水混合物经第二碱液分离器3进行油水分离后，水相自第二碱液分离器3的水相出口排出循环利用，油相进入到第二混合器4，与第三碱液分离器5的洗水和外部供水系统的新鲜水混合，通过补入新鲜水，能够保证第三碱液分离器5具有较高的碱离子去除率。该碱液分离系统通过对洗水进行循环利用和稀释，既降低了耗水量，又使各个碱液分离器保持了较高的碱离子去除率。With the lye separation system of the above structure, after the separation liquid is separated from oil and water by the first lye separator 1, the water phase is discharged from the water phase outlet of the first lye separator 1, and the oil phase enters the first mixer 2 , mixed with the washing water of the second lye separator 3 (that is, the water phase obtained by oil-water separation) and the washing water of the third lye separator 5, through the washing water of the
在一些实施例中，第一碱液分离器1的水相出口可与外部碱液配制系统连接，以将溶解有碱离子的水相输送至外部碱液配制系统。该外部碱液配置系统可为例如环己酮生产系统中的碱液配置系统，将溶解有碱离子的水相输送至该外部碱液配制系统，能够对水相中的碱离子回收再利用，以减少环己酮生产过程中的物耗。In some embodiments, the water phase outlet of the first lye separator 1 can be connected to an external lye preparation system, so as to deliver the aqueous phase in which the alkali ions are dissolved to the external lye preparation system. The external alkali solution preparation system can be, for example, an alkali solution preparation system in a cyclohexanone production system, and the aqueous phase in which the alkali ions are dissolved is transported to the external alkali solution preparation system, so that the alkali ions in the water phase can be recovered and reused, In order to reduce the material consumption in the production process of cyclohexanone.
在一些实施例中，碱液分离系统还包括第一输液泵6，第一输液泵6连接在第一混合器2的进液口和第二碱液分离器3的水相出口之间，用于将第二碱液分离器3输出的水相输送至第一混合器2。该第一输液泵6还可与外部碱液配置系统连接，以将第二碱液分离器3输出的部分水相输送至外部碱液配置系统，以对水相中的碱离子进行回收再利用，而且通过减少部分第二碱液分离器3输出的水相，并补入部分第三碱液分离器5输出的水相，能够很好的起到稀释洗水的目的，使第二碱液分离器3保持较高的碱离子去除率。In some embodiments, the alkali liquid separation system further includes a
在具体实施过程中，该第一输液泵6的出液口可通过例如三通阀与第一混合器2和外部碱液配置系统连接，通过该三通阀可控制流向第一混合器2的水相流速，以及流向外部碱液配置系统的水相流速，从而在保证第二碱液分离器3具有较高的碱离子去除率的同时，尽可能的减少耗水量。In the specific implementation process, the liquid outlet of the
在一个优选实施例中，第一输液泵6向第一混合器2输送水相的流速可为20-50m3/h，具体的，可为20m3/h、30m3/h或50m3/h；第一输液泵6向外部碱液配置系统输送水相的流速为4-8m3/h，具体的，可为4m3/h、6m3/h或8m3/h。In a preferred embodiment, the flow rate of the water phase delivered by the
在一些实施例中，该碱液分离系统还包括第二输液泵7，该第二输液泵7分别与第一混合器2的进液口、第二混合器4的进液口和第三碱液分离器5的水相出口连接，用于将第三碱液分离器5输出的水相分别输送至第一混合器2和第二混合器4。In some embodiments, the alkali liquid separation system further includes a second infusion pump 7, which is respectively connected with the liquid inlet of the first mixer 2, the liquid inlet of the second mixer 4 and the third alkali The water phase outlet of the liquid separator 5 is connected, and is used for sending the water phase output from the third alkali liquid separator 5 to the first mixer 2 and the second mixer 4 respectively.
在具体实施时，第二输液泵7的出液口可通过另一三通阀分别与第一混合器2和第二混合器4连接，通过该另一三通阀可控制输送至第一混合器2和第二混合器4的水相流速。In specific implementation, the liquid outlet of the second infusion pump 7 can be respectively connected to the first mixer 2 and the second mixer 4 through another three-way valve, and the other three-way valve can control the delivery to the first mixer The flow rate of the water phase in the second mixer 2 and the second mixer 4.
在一个优选实施例中，第二输液泵7向第一混合器2输送水相的流速为2-6m3/h，具体的，可为2m3/h、4m3/h或6m3/h；第二输液泵7向第二混合器4输送水相的流速为20-50m3/h，具体的，可为20m3/h、30m3/h或50m3/h。In a preferred embodiment, the flow rate at which the second infusion pump 7 delivers the water phase to the first mixer 2 is 2-6 m 3 /h, specifically, 2 m 3 /h, 4 m 3 /h or 6 m 3 /h ; The second infusion pump 7 delivers the water phase to the second mixer 4 with a flow rate of 20-50m 3 /h, specifically, 20m 3 /h, 30m 3 /h or 50m 3 /h.
在一些实施例中，外部供水系统向第二混合器4输送新鲜水的流速可为1-3m3/h，具体的，可为例如1m3/h、2m3/h或3m3/h等。经第一碱液分离器1和第二碱液分离器3分离后，第二碱液分离器3排出的油相中碱离子浓度已经很低，通过外部供水系统供给新鲜水，能够起到稀释第三碱液分离器5的洗水的目的，使洗水中碱离子也保持较低浓度，从而保证第三碱液分离器5具有较高的碱离子去除效率。In some embodiments, the flow rate of the fresh water delivered by the external water supply system to the second mixer 4 may be 1-3 m 3 /h, specifically, it may be, for example, 1 m 3 /h, 2 m 3 /h or 3 m 3 /h, etc. . After being separated by the first lye separator 1 and the
本发明实施例还提供了一种环己酮制备系统，其包括如上任一实施例所述的碱液分离系统。在具体实施时，该碱液分离系统可连接在环己酮制备系统中分解工序和精馏工序之间，分解工序产生的料液进入到碱液分离系统，去除碱离子后的油相可进入到精馏工序进行精馏。The embodiment of the present invention also provides a cyclohexanone preparation system, which includes the alkali liquid separation system described in any of the above embodiments. In specific implementation, the lye separation system can be connected between the decomposition process and the rectification process in the cyclohexanone preparation system, the feed liquid produced in the decomposition process enters the lye separation system, and the oil phase after removing alkali ions can enter the To the rectification process for rectification.
由于该碱液分离系统具有较高的碱离子去除效率，且耗水量较低，所以应用该碱液分离系统的环己酮制备系统同样具有耗水量低的优点，而且由于碱离子去除的较为彻底，不容易导致再沸器的列管结垢，能够延长再沸器的检修间隔，并且能够使环己酮生产系统保持较低能耗水平，另外，也不会引起有机物锁合反应，副产物产生较小，物耗较低。Because the alkali liquor separation system has high alkali ion removal efficiency and low water consumption, the cyclohexanone preparation system using the alkali liquor separation system also has the advantages of low water consumption, and because the alkali ion removal is relatively thorough , it is not easy to cause fouling of the reboiler tubes, can prolong the maintenance interval of the reboiler, and can keep the energy consumption of the cyclohexanone production system at a low level. The production is small and the material consumption is low.
以上描述旨在是说明性的而不是限制性的。例如，上述示例(或其一个或更多方案)可以彼此组合使用。例如本领域普通技术人员在阅读上述描述时可以使用其它实施例。另外，在上述具体实施方式中，各种特征可以被分组在一起以简单化本发明。这不应解释为一种不要求保护的公开的特征对于任一权利要求是必要的意图。相反，本发明的主题可以少于特定的公开的实施例的全部特征。从而，以下权利要求书作为示例或实施例在此并入具体实施方式中，其中每个权利要求独立地作为单独的实施例，并且考虑这些实施例可以以各种组合或排列彼此组合。本发明的范围应参照所附权利要求以及这些权利要求赋权的等同形式的全部范围来确定。The above description is intended to be illustrative and not restrictive. For example, the above examples (or one or more of them) may be used in combination with each other. For example, other embodiments may be utilized by those of ordinary skill in the art upon reading the above description. Additionally, in the above Detailed Description, various features may be grouped together to simplify the present invention. This should not be construed as an intention that an unclaimed disclosed feature is essential to any claim. Rather, inventive subject matter may lie in less than all features of a particular disclosed embodiment. Thus, the following claims are hereby incorporated into the Detailed Description by way of example or embodiment, with each claim standing on its own as a separate embodiment, and it is contemplated that these embodiments may be combined with each other in various combinations or permutations. The scope of the invention should be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled.
以上实施例仅为本发明的示例性实施例，不用于限制本发明，本发明的保护范围由权利要求书限定。本领域技术人员可以在本发明的实质和保护范围内，对本发明做出各种修改或等同替换，这种修改或等同替换也应视为落在本发明的保护范围内。The above embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and the protection scope of the present invention is defined by the claims. Those skilled in the art can make various modifications or equivalent replacements to the present invention within the spirit and protection scope of the present invention, and such modifications or equivalent replacements should also be regarded as falling within the protection scope of the present invention.
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| US20100126938A1 (en) * | 2008-11-27 | 2010-05-27 | Zhishan Bai | Process and apparatus for separating and recovering waste alkali from cyclohexane oxidation solution |
| CN102302868A (en) * | 2011-07-13 | 2012-01-04 | 化学工业第二设计院宁波工程有限公司 | Alkali waste separating device and method in process of preparing cyclohexanone and cyclohexanol by oxidization of cyclohexane |
| CN107433052A (en) * | 2017-08-01 | 2017-12-05 | 湖北兴达石化设备有限公司 | A kind of salkali waste piece-rate system prepared in cyclohexanone technique |
| CN212282983U (en) * | 2020-06-05 | 2021-01-05 | 山东方明化工股份有限公司 | Alkali liquor separation system and cyclohexanone preparation system |
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| US20100126938A1 (en) * | 2008-11-27 | 2010-05-27 | Zhishan Bai | Process and apparatus for separating and recovering waste alkali from cyclohexane oxidation solution |
| CN102302868A (en) * | 2011-07-13 | 2012-01-04 | 化学工业第二设计院宁波工程有限公司 | Alkali waste separating device and method in process of preparing cyclohexanone and cyclohexanol by oxidization of cyclohexane |
| CN107433052A (en) * | 2017-08-01 | 2017-12-05 | 湖北兴达石化设备有限公司 | A kind of salkali waste piece-rate system prepared in cyclohexanone technique |
| CN212282983U (en) * | 2020-06-05 | 2021-01-05 | 山东方明化工股份有限公司 | Alkali liquor separation system and cyclohexanone preparation system |
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