WO2015096316A1 - 异丁烷脱氢制异丁烯中异丁烯夹带的废催化剂浓缩干燥及解毒的处理方法及装置 - Google Patents

异丁烷脱氢制异丁烯中异丁烯夹带的废催化剂浓缩干燥及解毒的处理方法及装置 Download PDF

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WO2015096316A1
WO2015096316A1 PCT/CN2014/075886 CN2014075886W WO2015096316A1 WO 2015096316 A1 WO2015096316 A1 WO 2015096316A1 CN 2014075886 W CN2014075886 W CN 2014075886W WO 2015096316 A1 WO2015096316 A1 WO 2015096316A1
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catalyst
washing
isobutylene
water
micro
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PCT/CN2014/075886
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English (en)
French (fr)
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吕文杰
白兆圆
马良
汪华林
刘洪来
张艳红
隋志军
崔馨
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上海华畅环保设备发展有限公司
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Publication of WO2015096316A1 publication Critical patent/WO2015096316A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/24—Chromium, molybdenum or tungsten
    • B01J23/26—Chromium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/90—Regeneration or reactivation
    • B01J23/92—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
    • C07C5/32—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with formation of free hydrogen
    • C07C5/327—Formation of non-aromatic carbon-to-carbon double bonds only
    • C07C5/333—Catalytic processes
    • C07C5/3332—Catalytic processes with metal oxides or metal sulfides
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
    • C07C2523/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper
    • C07C2523/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups C07C2523/02 - C07C2523/36
    • C07C2523/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups C07C2523/02 - C07C2523/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • C07C2523/85—Chromium, molybdenum or tungsten
    • C07C2523/86—Chromium
    • 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
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/584—Recycling of catalysts

Definitions

  • the invention belongs to the field of chemical solid waste prevention and relates to a method for concentrated catalyst drying and detoxification treatment of isobutylene entrained by isobutane in isobutylene, and in particular, the invention relates to washing by using a washing tower for crude isobutylene products.
  • the obtained washing wastewater is subjected to micro-swirl concentration and pressure filtration, and the obtained catalyst cake is dried by using the temperature of the regeneration gas to obtain a wet catalyst cake having a lower water content, and finally the spent catalyst is detoxified in the regenerator.
  • the invention also relates to a device for deconcentrating and detoxifying a waste catalyst entrained by isobutylene in isobutane dehydrogenation. Background technique
  • Isobutane is mainly used for the following purposes: high calorific value, high performance fuel; isobutylene by alkylation to isooctane, as a gasoline octane improver; can also be used as a substitute for refrigerant; dehydrogenation to isobutylene; Acrylic acid, acetone, methanol, etc.
  • Isobutylene has gradually become another important petrochemical base material in addition to ethylene and propylene.
  • the dehydrogenation of isobutane to isobutylene is one of the main ways to utilize isobutane resources abroad.
  • the total amount of isobutylene produced by isobutane in the world reaches more than 3 million tons per year. In the United States alone, it is produced by dehydrogenation of isobutane. The isobutylene reached more than 2 million tons.
  • the main method for dehydrogenation of isobutane is catalytic cracking dehydrogenation, and the catalyst is mainly chromium oxide.
  • the reaction is an endothermic reaction.
  • increasing the temperature or lowering the pressure is beneficial to dehydrogenation.
  • the high temperature tends to cause polymerization of the olefin, causing coking on the surface of the catalyst, covering the active site of the catalyst, which results in a decrease in catalyst activity and selectivity.
  • the chromium oxide catalyst has the problems of poor low temperature activity, frequent catalyst regeneration, and easy oxidation and reduction of hexavalent chromium.
  • the hexavalent chromium has high toxicity, and can cause acute respiratory irritation, nosebleed, hoarseness after inhalation.
  • the nasal mucosa is atrophied, sometimes with asthma and purpura, and severe pneumonia can occur. Oral can stimulate and corrode the digestive tract, causing nausea, vomiting, and abdomen Pain, bloody stools, etc.; severe cases of dyspnea, purpura, shock, liver damage and acute renal failure. Therefore, it is very important to carry out regeneration and detoxification treatment of the collected catalyst.
  • reaction is accompanied by cleavage side reactions, which involve both dehydrogenation reactions, cracking, isomerization, aromatization, alkylation, polymerization, coking, etc., and dehydrogenation products except isobutylene.
  • cleavage side reactions involve both dehydrogenation reactions, cracking, isomerization, aromatization, alkylation, polymerization, coking, etc., and dehydrogenation products except isobutylene.
  • various alkanes, olefins, heavy aromatic hydrocarbons, and coke are also included, and by-products such as aldehydes, ketones, alcohols, ethers, and furans may also be formed.
  • the above impurities can be removed by elution of water to obtain a crude isobutylene product while the catalyst particles enter the washing water.
  • the accumulation of these catalyst particles in the process of recycling the washing water will block the subsequent equipment, and in severe cases, it must be shut down for cleaning, which affects the continuous and stable operation of the entire device. Therefore, it is necessary to separate and recover the catalyst in the washing water to reduce the content of the catalyst in the water to a balanced concentration that satisfies the long-term operation of the system.
  • catalyst separation There are many methods for catalyst separation, which are mainly classified according to the type of catalyst, particle size, density, service life and system. Mainly include: sedimentation method, filtration method, membrane separation, cyclone separation, etc.
  • a slurry system is provided to treat the washing water with catalyst, the reaction gas carrying the catalyst particles is washed by the washing tower, the fine powder of the catalyst enters the washing water, and part of the washing water is sent to the catalyst for precipitation.
  • the tank is settled by gravity, and the settled slurry is returned to the reactor by the slurry pump, and the slurry is dried by the high-temperature regeneration flue gas, and finally the dried catalyst is discharged; and the settled clear liquid After clarifying the water tank, it is returned to the cold water circulation line by means of a clarified water pump and then circulated in the system.
  • the sedimentation tank with gravity sedimentation has a treatment capacity of 40 m 3 /h, a land area of about 180 m 2 , and requires 1 open and 1 reserve.
  • the utility model has the advantages of large occupied area, small processing amount, poor separation effect, short operation period, and the washing tower is easy to foam.
  • the high-temperature regenerated flue gas in the reactor dries the slurry. In the process, the regeneration gas has an impact on the reactor. At this time, the obtained catalyst has a water content of 90%, and the energy consumption in the drying process is high.
  • a catalyst separation system which is a catalyst separation system for separating solid catalyst particles from hydrocarbons, the system comprising a reactor, a storage tank, a filter and a filtrate recovery device, and the filter is recovered from the storage tank to the filtrate.
  • the slurry flow path of the container is arranged in series.
  • the invention mainly focuses on the catalyst recovery part, and adopts a plurality of filters, resulting in more system equipment, a cumbersome system and a large floor space.
  • Chinese patent application CN102716605A discloses a method and a device for comprehensively utilizing quenching wastewater of isobutane dehydrogenation to isobutylene reaction product, mainly adopting multi-stage separation method for solid-liquid separation of catalyst particles entrained in quenching wastewater to ensure quenching water.
  • the water quality reaches the requirement of circulating cooling and reuse, and the spent catalyst drying is recovered in solid form.
  • the method requires three-stage cyclone separation, and the number of equipment is relatively large. Large, the biggest drawback is that the spent catalyst is in the form of powder, the drying energy is high, and the spent catalyst is easy to fly and pollute the environment.
  • the activity of the chromium-containing spent catalyst is low, and the economic value of the separate recycling is not significant.
  • the invention provides a novel method and a device for concentrating, drying and detoxifying waste catalyst entrained by isobutylene in isobutane dehydrogenation to isobutylene, which solves the problem that the equipment existing in the prior art has large land area, poor separation effect, washing
  • the solvent in the tower is easy to foam, and the activity of recovering the spent catalyst is low, which effectively prolongs the continuous operation period of the device, optimizes the overall working condition of the device, realizes the catalyst recycling and utilization, reduces energy consumption, and realizes low energy consumption production.
  • the present invention provides a process for the concentration, drying, and detoxification of spent catalyst entrained in isobutylene to isobutene in an isobutane process, the method comprising the steps of:
  • the CO gas is introduced into the regenerator to perform a redox reaction to regenerate the catalyst.
  • the isobutylene crude product has a temperature of 600 ° C
  • the circulating cooling water has a temperature of 35 ° C
  • the washing wastewater temperature is 55 ° C
  • the regenerator temperature is 200-250 ° C.
  • the spent catalyst particles containing spent catalyst have a particle size of 0.1-40 ⁇ m, and the separation particle size of the microswirl separation is not more than 2 ⁇ m and the pressure drop is not more than 0.2 MPa.
  • the water content of the spent catalyst concentrate obtained by the micro-swirl separation is 60-99%, and the moisture content of the waste catalyst cake obtained by pressure filtration is not more than 20%.
  • the filtrate has a catalyst content of not more than 20 ppm.
  • the present invention provides a treatment apparatus for concentrated catalyst drying, detoxification of isobutylene entrained in isobutane and isobutylene entrained in isobutylene, the apparatus comprising:
  • washing tower for washing high-temperature isobutylene gas generated by the isobutane cracking reaction with circulating cooling water to obtain washing wastewater containing spent catalyst
  • a micro-swirl separator connected to the washing tower for concentrating the spent catalyst particles in the obtained washing wastewater by micro-swirl separation to obtain a spent catalyst concentrate
  • a filter press connected to the micro cyclone separator for pressurizing and filtering the obtained spent catalyst concentrate to further remove free water in the concentrate to obtain a spent catalyst cake;
  • regenerator connected to the filter press for drying the obtained spent catalyst cake by using the flue gas of the regenerator in the process of dehydrogenation of isobutane to isobutene to obtain a wet catalyst cake having a low water content;
  • the temperature of the wet catalyst cake is increased by the heat of the regeneration gas; wherein the CO gas is introduced into the regenerator to perform a redox reaction to regenerate the catalyst.
  • the apparatus further includes:
  • a filter connected to the scrubber for filtering the crude isobutylene product obtained from the reactor connected thereto;
  • a clarified water tank connected to the micro-swirl separator and the filter press for further gravity clarification of the washing wastewater after the micro-swirl separation and the filtrate obtained by the pressure filtration to ensure that the washing water returned to the washing tower does not contain Solid particles;
  • a cold water circulation pump connected to the washing tower, and a clarification water pump connected to the cold water circulation pump for sending the clarified washing water to the washing tower;
  • a reflux cooler located at the top of the scrubber tower for cooling the brine.
  • the dehydrogenation reaction is carried out under the action of a catalyst in a reactor at a high temperature of 585 to 620 ° C and a low pressure of less than 0.2 MPa.
  • the apparatus when the washing waste water head of the bottom of the washing tower cannot meet the pressure drop requirement of the micro cyclone separator, the apparatus further comprises a hot water circulating pump at the bottom of the washing tower, for The washing wastewater at the bottom of the washing tower is pressurized.
  • the micro-swirl separator is composed of a single or a plurality of micro-swirl core tubes connected in parallel, and the pressure drop of the micro-swirl core tube is not more than 0.2 MPa, and the separation granularity is not More than 2 ⁇ , the separation efficiency reaches 90%.
  • the clarified water tank is selected from a gravity settling device.
  • Fig. 1 is a flow chart showing the process of concentration drying and detoxification of waste catalyst entrained in isobutylene in isobutane dehydrogenation to isobutylene according to an embodiment of the present invention. detailed description
  • micro-swirl separation technology to separate the catalyst chromium oxide entrained in the wash water can separate the catalyst particles with high precision, effectively improve the recycling of the wash water, and prolong the operation cycle.
  • the invention firstly uses the circulating water to wash the high-temperature isobutylene gas generated by the isobutane cracking reaction in the washing tower, washes the waste catalyst entrained by the isobutylene into the circulating water; and then uses the micro-swirl separator to carry out the waste catalyst in the washing circulating water.
  • the spent catalyst concentrate is obtained by cyclone concentration, and the spent catalyst concentrate is further dehydrated by a filter press to obtain a waste catalyst cake.
  • the waste catalyst cake is dried by using the exhaust gas of the regenerator to obtain a wet water having a low water content.
  • the invention combines micro-swirl separation and pressure filtration to realize the purification of the washing water used for recycling, and reduces the waste catalyst particles in Accumulation in the scrubber, heat recovery heat exchanger and pipeline, avoiding the shutdown and maintenance caused by catalyst fouling, and prolonging the continuous stable operation cycle of the isobutane dehydrogenation isobutylene circulating water system.
  • a process for the treatment of concentration, drying and detoxification of spent catalyst entrained by isobutene in isobutane dehydrogenation to isobutylene comprising:
  • the catalyst slurry obtained by micro-swirl de-solidification is subjected to pressure filtration; at the same time, the concentrated catalyst is dried by using the flue gas from the regenerator to obtain a catalyst cake with a lower water content, and the temperature of the filter cake is increased to ensure the injection of the catalyst. Cracking the detoxification temperature in the regenerated flue gas, and additionally purifying the regeneration gas by using the filter cake structure;
  • washing water after micro-swirl de-solidification and the filtrate obtained by pressure filtration are subjected to further gravity clarification, and it is ensured that the washing water returned to the washing tower for recycling does not contain solids;
  • the dried catalyst is then driven into a regenerator, and a CO gas is introduced to carry out a high-temperature oxidation-reduction reaction to reduce the toxicity of the catalyst, and the catalyst deactivated component chromium trioxide is reduced to reduce the hexavalent chromium to trivalent chromium.
  • the temperature of the obtained crude isobutylene product is about 600 ° C, and the temperature of the circulating cooling water is about
  • the temperature of the recycled wastewater after washing is about 55 ° C.
  • the washing water is subjected to micro-swirl de-solidification using a micro-swirl separator having a separation particle size of not more than 2 ⁇ m and a pressure drop of not more than 0.2 MPa.
  • the catalyst slurry obtained by the micro-swirl dewatering has a water content of about 60-99%, and the catalyst cake obtained by pressure filtration has a water content of not more than about 20%, and the catalyst content of the obtained filtrate is obtained. Not more than about 20 ppm.
  • the detoxification temperature of the regenerator is about 200 to 250 °C.
  • a treatment apparatus for concentration drying and detoxification of a waste catalyst entrained in isobutene in isobutane dehydrogenation to isobutylene comprising:
  • regenerator for regenerating a catalyst that deactivates the coking of the reactor
  • micro-swirl separator for concentrating spent catalyst in washing wastewater of a scrubber and performing micro-swirl de-solidification
  • a filter press for performing pressure filtration on the catalyst slurry obtained by decoupling the micro-swirl; a clarified water tank for further gravity clarification of the washing water after the micro-swirl desolidation and the filtrate obtained by pressure filtration to ensure that the washing water returning to the washing tower does not contain solid particles;
  • a cold water circulation pump for pumping brine to the scrubber;
  • a clarified water pump for pumping the clarification water to the scrubber;
  • a water-washed overhead reflux cooler for cooling brine A water-washed overhead reflux cooler for cooling brine.
  • the apparatus when the washing water head of the bottom of the washing tower cannot satisfy the pressure drop requirement of the micro-swirl separator, the apparatus further includes a hot water circulation pump for pressurizing the washing water at the bottom of the washing tower.
  • the microcyclone separator utilizes cyclone centrifugation to achieve a separation efficiency of about 90%.
  • the micro-swirl separator is composed of a single or a plurality of micro-swirl core tubes connected in parallel, and the pressure drop of the micro-swirl core tube is not more than about 0.2 MPa, and the separation granularity is not more than about 2 ⁇ . .
  • the clarified water tank may be selected from a gravity settling device.
  • the chromic oxide catalyst cake produced by the filter press is dried by using the exhaust gas from the regenerator to obtain a catalyst cake having a lower water content, and at the same time, increasing the temperature of the filter cake. , to ensure that the detoxification temperature in the catalytic cracking regeneration flue gas reaches 200-250 ° C;
  • the filter cake structure is used to purify the regeneration gas.
  • the resulting higher temperature catalyst cake is returned to the regenerator for regeneration and detoxification treatment.
  • Fig. 1 is a flow chart showing a process for concentrating, drying and detoxifying a spent catalyst entrained in isobutylene in isobutane dehydrogenation to isobutylene according to an embodiment of the present invention.
  • isobutane enters the reactor 1 for reaction; the crude isobutylene obtained by the reaction is sent to the filter 3 from the top of the reactor 1 for filtration; the filtrate is discharged from the bottom of the filter 3 and discharged from the bottom of the reactor 1.
  • the live catalyst is sent to the regenerator 2 for regeneration.
  • the regenerated active catalyst is returned to the reactor 1 from the bottom of the regenerator 2, and the CO 2 is discharged from the top of the regenerator 2; the filtered high-temperature isobutylene gas is sent from the top of the filter 3 to the scrubber. 4 washing, the obtained isobutylene product is discharged and recovered, and the obtained waste catalyst-containing washing wastewater is pumped to the micro-swirl separator 6 through a hot water circulation pump for concentration separation, and the obtained spent catalyst concentrate is obtained from the bottom of the micro-swirl separator 6
  • the discharge is sent to the filter press 7, the deactivated catalyst cake is obtained, the filter cake temperature is increased by the heat of the regeneration gas, a wet catalyst cake having a lower water content is obtained, and the wet catalyst cake is sent to the regenerator to recover the catalyst;
  • the exhaust gas is discharged from the top of the filter press 7; the obtained filtrate is discharged from the top of the filter press 7, and is washed after being desolidated by the micro-swirl discharged from the top
  • the invention adopts the cyclone separation technology to separate the washing water of the washing tower, and has high separation precision, small equipment footprint (reduced by 90% compared with foreign processes), and the solvent foaming problem is suppressed to some extent, and the solution is effectively solved.
  • the clogging problem of the catalyst in the washing tower makes the continuous operation cycle of the device prolonged, and the economical operation of the device is improved.
  • the catalyst deactivation problem is considered, and the spent catalyst is detoxified by the regenerator, thereby realizing the reuse of the catalyst and reducing the catalyst input. Improve the economics of the equipment.
  • the invention adopts the use of the filter press to effectively filter the swirling underflow portion, so that the water content of the catalyst cake is significantly reduced, and the catalyst is effectively recovered; and the flue gas generated by the regenerator is introduced to the filter press.
  • the chromium oxide catalyst cake is dried to obtain a catalyst cake with a lower water content.
  • the filter cake layer is dried by using the heat of the regeneration gas, and the temperature of the filter cake is increased to ensure the injection into the catalytic cracking regeneration flue gas.
  • the initial temperature ensures the detoxification temperature of the catalyst in the regenerator, which effectively reduces the heat loss and reduces the energy consumption.
  • the filter cake layer is used to purify and filter the regeneration gas, and the catalyst entrained by the regeneration gas is recovered, and the material is reduced. Loss.
  • the washing wastewater is separated by a combination of a micro-swirl separator and a filter press, and the specific operation process and effects are described as follows:
  • the high-temperature isobutylene gas generated by the isobutane cracking reaction is washed by circulating cooling water to obtain washing wastewater containing spent catalyst; the obtained washing wastewater is subjected to micro-swirl separation method to concentrate the spent catalyst particles to obtain a waste catalyst concentration.
  • the obtained spent catalyst concentrate is subjected to pressure filtration to further remove free water in the concentrate to obtain a spent catalyst cake; the flue gas of the regenerator in the process of dehydrogenation of isobutane to isobutene is under pressure filtration
  • the above-mentioned spent catalyst cake is dried in the machine to obtain a wet catalyst cake with a lower water content; at the same time, the temperature of the catalyst cake is increased by using the heat of the regeneration gas to ensure that the detoxification reaction temperature of the catalyst regenerator reaches the regenerator requirement.
  • the resulting three stocks include: purified wash water, filter cake, and regeneration gas.
  • the inlet, overflow and underflow solids obtained from the microcyclone separator are as follows: Serial number average solid content
  • the solid content and water content of the filtrate and filter cake obtained by the filter press are as follows:
  • the device of the present invention covers only 1/10 of the original production process, which effectively reduces the funds used for equipment construction and prolongs the operation cycle.

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  • Chemical Kinetics & Catalysis (AREA)
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Abstract

本发明涉及异丁烷脱氢制异丁烯中异丁烯夹带的废催化剂浓缩干燥及解毒的处理方法及装置，该方法包括以下步骤：（a）利用循环冷却水对异丁烷裂解反应生成的高温异丁烯气体进行洗涤，得到含废催化剂的洗涤废水；（b）采用微旋流分离对所得的洗涤废水中的废催化剂微粒进行浓缩，得到废催化剂浓缩液；（c）对所得的废催化剂浓缩液进行加压过滤，以进一步脱除浓缩液中的游离水，获得废催化剂滤饼；（d）采用异丁烷脱氢制异丁烯过程中再生器的外排烟气对所得的废催化剂滤饼进行烘干，获得含水量低的湿催化剂滤饼；同时利用再生气热量提高湿催化剂滤饼温度；以及（e）再生器内通入CO气体，进行氧化还原反应以再生催化剂。

Description

异丁烷脱氢制异丁烯中异丁烯夹带的废催化剂
浓缩干燥及解毒的处理方法及装置 技术领域
本发明属于化工固体废弃物防治领域， 涉及一种异丁烷脱氢制异丁烯中异丁 烯夹带的废催化剂浓缩干燥及解毒处理的方法， 具体地说， 本发明涉及通过将异 丁烯粗产品利用洗涤塔洗涤， 对所得洗涤废水进行微旋流浓缩和压滤， 同时利用 再生气温度对所得催化剂滤饼烘干， 得到含水量较低的湿催化剂滤饼， 最后在再 生器中对废催化剂进行解毒处理， 得到活性较高的催化剂的方法。 本发明还涉及 一种异丁烷脱氢制异丁烯中异丁烯夹带的废催化剂浓缩干燥及解毒处理的装置。 背景技术
随着原油处理量的增加以及石油加工方法的改进， 在我国石油炼制行业中的 异丁烷资源愈加丰富， 主要来源于催化裂化石油气、 天然气和 c4馏分。 异丁烷主 要有以下用途： 高热值、 高性能的燃料； 异丁烯经烃化制异辛烷， 作为汽油辛烷 值改进剂； 也可用做替代冷冻剂； 脱氢至异丁烯； 还可制甲基丙烯酸、 丙酮和甲 醇等。 异丁烯逐渐成为除乙烯、 丙烯以外又一重要的石油化工基础原料， 主要用 于制取甲基叔丁基醚、 生产丁基橡胶及聚异丁烯。 以异丁烯为资源的精细化工工 业发展迅速， 需求量增长很快， 而我国的异丁烯资源稀缺， 因此， 异丁烷催化脱 氢制异丁烯成为解决异丁烯短缺的主要方法之一。
异丁烷脱氢制异丁烯是国外利用异丁烷资源的主要途径之一， 全世界由异丁 烷生产的异丁烯总量每年达到 300多万吨， 仅在美国， 由异丁烷脱氢生产的异丁 烯就达到 200多万吨。
异丁烷脱氢的主要方法是催化裂化脱氢， 催化剂采用的主要是三氧化二铬。 该反应属于吸热反应， 根据化学热力学平衡分析， 提高温度或者降低压力有利于 脱氢。 但高温容易引起烯烃聚合， 造成催化剂表面结焦， 覆盖催化剂活性中心， 其结果降低了催化剂活性和选择性。 同时三氧化二铬催化剂存在低温活性较差， 催化剂再生频繁的问题， 且易于氧化还原六价铬， 六价铬具有较高毒性， 吸入后 可引起急性呼吸道剌激症状、 鼻出血、 声音嘶哑、 鼻粘膜萎缩， 有时出现哮喘和 紫绀， 重者可发生化学性肺炎。 口服可剌激和腐蚀消化道， 引起恶心、 呕吐、 腹 痛、 血便等； 重者出现呼吸困难、 紫绀、 休克、 肝损害及急性肾功能衰竭等。 因 此， 对收集的催化剂进行再生降毒处理十分重要。 此外， 该反应还伴有裂解副反 应发生， 过程中既有脱氢反应， 又有裂解、 异构化、 芳构化、 烷基化、 聚合、 结 焦等各种副反应， 脱氢产物除异丁烯外， 还包括各种烷烃、 烯烃、 重芳烃及焦炭 等， 亦有可能会有醛、 酮、 醇、 醚、 呋喃等副产物生成。
可通过升压水洗脱除以上杂质， 获得异丁烯粗产品， 同时催化剂颗粒进入洗 涤水中。 这些催化剂颗粒在洗涤水循环利用的过程中不断累积会堵塞后续设备， 严重时须停工清洗， 影响整个装置的连续稳定运转。 因此有必要对洗涤水中的催 化剂进行分离回收， 以降低水中催化剂的含量， 使其达到满足系统长周期运转的 平衡浓度。
催化剂分离方法有很多种， 主要根据催化剂的类型、 粒径、 密度、 使用寿命 和体系的不同而分类。 主要有： 沉降法、 过滤法、 膜分离、 旋流分离等。 目前俄 罗斯异丁烷脱氢制异丁烯工艺中， 设有渣浆系统来处理带催化剂的洗涤水， 通过 洗涤塔将携带催化剂颗粒的反应气洗涤， 催化剂微粉进入洗涤水中， 部分洗涤水 送至催化剂沉淀罐利用重力进行沉降处理， 进而利用渣浆泵将沉降后的渣浆打回 到反应器， 通过高温再生烟气进行渣浆的干燥， 最后将干燥后的催化剂外排； 而 沉降后的澄清液至澄清水罐， 后利用澄清水泵将其打回冷水循环管线， 然后在系 统循环。 采用重力沉降的沉淀罐处理量为 40m3/h， 占地面积约为 180m2， 且需 1 开 1备。 占地面积大， 处理量小， 分离效果差， 运行周期短， 且洗涤塔容易发泡。 另外， 反应器内高温再生烟气对渣浆进行干燥， 此过程中再生气对反应器有冲击， 此时所得催化剂含水率达 90%， 对其干燥过程中的能耗高。
中国专利申请 CN102165042A公开了一种催化剂分离系统， 即将固体催化剂 粒子从烃中分离的催化剂分离系统， 该系统包括反应器、 贮存罐、 过滤器及滤液 回收器， 且过滤器在贮存罐到滤液回收容器的浆料流路上串联配置， 该发明主要 侧重于催化剂回收部分， 采用多个过滤器， 造成系统设备较多， 系统较为繁琐， 占地面积大。
中国专利申请 CN102716605A公开了一种异丁烷脱氢制异丁烯反应产物急冷 废水综合化利用的方法与装置， 主要采用多级分离的方法对急冷废水夹带的催化 剂颗粒进行固液分离， 保证急冷水的水质到达循环冷却回用的要求， 废催化剂干 燥以固态形式回收。 该方法需采用三级旋流分离， 设备数量较多占地面积相对较 大， 最大的缺陷是废催化剂呈粉末状， 干燥能耗高， 容易使废催化剂飞扬并污染 环境， 另一方面含铬废催化剂的活性较低， 单独回收利用的经济价值不显著。
因此， 对于异丁烷脱氢制异丁烯废催化剂， 本领域亟需开发出成本低且效果 好的处理回收方法与装置。 发明内容
本发明提供了一种新颖的异丁烷脱氢制异丁烯中异丁烯夹带的废催化剂浓 缩干燥及解毒的处理方法及装置， 解决了现有技术中存在的设备占地面积大， 分 离效果差， 洗涤塔内溶剂易发泡， 回收废催化剂活性较低等问题， 有效地延长了 装置连续运行周期， 优化了装置整体工况， 实现了催化剂降毒回收利用， 同时降 低能量消耗， 实现低能耗生产。
一方面，本发明提供了一种异丁烷脱氢制异丁烯中异丁烯夹带的废催化剂浓缩 干燥及解毒的处理方法， 该方法包括以下步骤：
( a)利用循环冷却水对异丁烷裂解反应生成的高温异丁烯气体进行洗涤， 得 到含废催化剂的洗涤废水；
(b)采用微旋流分离对所得的洗涤废水中的废催化剂微粒进行浓缩， 得到废 催化剂浓缩液；
( c)对所得的废催化剂浓缩液进行加压过滤， 以进一步脱除浓缩液中的游离 水， 获得废催化剂滤饼；
( d)采用异丁烷脱氢制异丁烯过程中再生器的外排烟气对所得的废催化剂滤 饼进行烘干， 获得含水量低的湿催化剂滤饼； 同时利用再生气热量提高湿催化剂 滤饼温度； 以及
( e) 再生器内通入 CO气体， 进行氧化还原反应以再生催化剂。
在一个优选的实施方式中， 异丁烯粗产品的温度为 600°C， 循环冷却水的温 度为 35°C， 洗涤废水的温度为 55°C， 再生器内的温度为 200-250°C。
在另一个优选的实施方式中， 含废催化剂的洗涤废水所携带的废催化剂微粒 的粒径为 0.1-40μπι， 微旋流分离的分离粒度不大于 2μπι、 压力降不大于 0.2MPa。
在另一个优选的实施方式中， 所述微旋流分离所得的废催化剂浓缩液的含水 率为 60-99%， 经过加压过滤所得的废催化剂滤饼的含水率不高于 20%， 所得的滤 液的催化剂含量不大于 20ppm。 另一方面，本发明提供了一种异丁烷脱氢制异丁烯中异丁烯夹带的废催化剂浓 缩干燥及解毒的处理装置， 该装置包括：
洗涤塔， 用于利用循环冷却水对异丁烷裂解反应生成的高温异丁烯气体进行 洗涤， 得到含废催化剂的洗涤废水；
与洗涤塔连接的微旋流分离器， 用于采用微旋流分离对所得的洗涤废水中的 废催化剂微粒进行浓缩， 得到废催化剂浓缩液；
与微旋流分离器连接的压滤机，用于对所得的废催化剂浓缩液进行加压过滤， 以进一步脱除浓缩液中的游离水， 获得废催化剂滤饼；
与压滤机连接的再生器， 用于采用异丁烷脱氢制异丁烯过程中再生器的外排 烟气对所得的废催化剂滤饼进行烘干， 获得含水量低的湿催化剂滤饼； 同时利用 再生气热量提高湿催化剂滤饼温度； 其中， 再生器内通入 CO气体， 进行氧化还 原反应以再生催化剂。
在一个优选的实施方式中， 该装置还包括：
与洗涤塔连接的过滤器， 用于对与其连接的反应器得到的异丁烯粗产品进行 过滤；
与微旋流分离器和压滤机连接的澄清水罐， 用于对微旋流分离后的洗涤废水 和加压过滤所得的滤液进行进一步的重力澄清， 以保证返回洗涤塔的洗涤水不含 固体颗粒；
与洗涤塔连接的冷水循环泵， 与冷水循环泵连接的澄清水泵， 用于将澄清的 洗涤水送至洗涤塔；
位于洗涤塔塔顶的回流冷却器， 用于将含盐水冷却。
在另一个优选的实施方式中，在反应器内，在 585-620°C的高温和小于 0.2MPa 的低压下， 在催化剂作用下进行脱氢反应。
在另一个优选的实施方式中， 当洗涤塔塔底的洗涤废水压头不能满足微旋流 分离器的压力降要求时， 该装置还包括位于洗涤塔塔底的热水循环泵， 用于对洗 涤塔塔底的洗涤废水进行增压。
在另一个优选的实施方式中， 所述微旋流分离器是由单根或多根微旋流芯管 并联组成的， 所述微旋流芯管的压力降不大于 0.2MPa、 分离粒度不大于 2μπι、 分 离效率达到 90%。
在另一个优选的实施方式中， 所述澄清水罐选自重力沉降设备。 附图说明
根据结合附图进行的如下详细说明， 本发明的目的和特征将变得更加明显， 附图中：
图 1是根据本发明一个实施方式的异丁烷脱氢制异丁烯中异丁烯夹带的废催 化剂浓缩干燥及解毒的处理工艺流程图。 具体实施方式
本申请的发明人在经过了广泛而深入的研究之后发现， 利用微旋流分离技术 分离洗涤水夹带的催化剂氧化铬， 可以高精度地分离催化剂颗粒， 有效提高洗涤 水的循环利用， 延长运行周期， 降低经济损耗， 同时在一定程度上抑制发泡； 另 夕卜， 利用压滤机对旋流底流压滤， 同时引入装置再生气反吹， 对滤饼进行烘干， 有效利用了再生气余热， 同时净化了再生气， 有效减少了能热量损失， 且有效回 收了催化剂， 节能降耗， 绿色生产； 同时将压滤得到的失活的催化剂返回再生器 进行再生降毒处理， 重复利用了催化剂， 安全生产。 基于上述发现， 本发明得以 完成。
本发明的技术构思如下：
在烷烃催化裂化脱氢过程中， 在催化剂的作用下不止生成了烯烃， 还生成了 醛、 酮等副产物， 通过升压水洗脱除这些杂质， 可以获得烯烃粗产品， 而同时催 化剂颗粒进入洗涤水中； 这些催化剂颗粒在洗涤水循环利用的过程中不断累积会 堵塞后续设备， 严重时须停工清洗， 且失活的催化剂具有较高的毒性， 容易造成 清洗过程中危险事故产生， 进而影响整个装置的连续稳定运转； 因此， 必须对洗 涤水中的催化剂进行分离、 降毒处理；
本发明首先利用循环水在洗涤塔中对异丁烷裂解反应生成的高温异丁烯气 体进行洗涤， 将异丁烯夹带的废催化剂洗涤到循环水中； 然后采用微旋流分离器 对洗涤循环水中的废催化剂进行旋流浓缩得到废催化剂浓缩液， 废催化剂浓缩液 采用压滤机进一步脱水得到废催化剂滤饼， 同时采用再生器的外排烟气对废催化 剂滤饼进行烘干， 获得含水量较低的湿催化剂滤饼； 最后将湿催化剂滤饼送入再 生器中进行高温降毒， 将六价铬转化为三价铬， 回收催化剂。 本发明通过微旋流 分离与压力过滤组合， 实现对循环使用的洗涤水的净化， 减少了废催化剂颗粒在 洗涤塔、 余热回收的换热器及管线中的累积， 避免催化剂积垢导致的停工检修， 延长了异丁烷脱氢制异丁烯循环水系统的连续稳定运转周期。
在本发明的第一方面， 提供了一种异丁烷脱氢制异丁烯中异丁烯夹带的废催 化剂浓缩干燥及解毒的处理方法， 该方法包括：
利用洗涤塔对异丁烷裂解反应生成的高温异丁烯气体进行洗涤；
将高温异丁烯夹带的废催化剂洗涤下来， 并对洗涤塔底含有的废催化剂颗粒 的洗涤水实施微旋流脱固， 实现洗涤水中催化剂颗粒的脱除；
对微旋流脱固所得的催化剂浆料实施压力过滤； 同时采用再生器外排烟气对 浓缩催化剂进行烘干， 得到含水量较低的催化剂滤饼， 并提高滤饼温度， 保证喷 入催化裂化再生烟气中的解毒温度， 另外利用滤饼结构净化再生气；
对微旋流脱固后的洗涤水和压力过滤得到的滤液进行进一步的重力澄清， 保 证返回洗涤塔循环使用的洗涤水不含固体；
烘干后的催化剂再打入再生器中， 通入 CO气体， 进行高温氧化还原反应， 以降低催化剂毒性， 还原催化剂失活组分三氧化铬， 使得六价铬还原为三价铬。
在本发明中， 所得异丁烯粗产品的温度约为 600°C， 循环冷却水的温度约为
35°C， 洗涤后的循环废水的温度约为 55°C。
在本发明中， 采用分离粒度不大于 2μπι、 压力降不大于 0.2MPa的微旋流分 离器对所述洗涤水实施微旋流脱固。
在本发明中， 所述微旋流脱固所得的催化剂浆料的含水率约为 60-99%， 经过 压力过滤所得的催化剂滤饼的含水率不高于约 20%， 所得滤液的催化剂含量不大 于约 20ppm。
在本发明中， 所述再生器的解毒温度约为 200-250°C。
在本发明的第二方面， 提供了一种异丁烷脱氢制异丁烯中异丁烯夹带的废催 化剂浓缩干燥及解毒的处理装置， 该装置包括：
用于对反应器得到的异丁烯粗产品进行过滤的过滤器；
用于对反应器的结焦失活的催化剂进行再生处理的再生器；
用于对高温异丁烯粗产品进行急冷洗涤的洗涤塔；
用于对洗涤塔的洗涤废水中的废催化剂进行浓缩并进行微旋流脱固的微旋 流分离器；
用于对所述微旋流脱固所得的催化剂浆料实施压力过滤的压滤机； 用于对微旋流脱固后的洗涤水和压力过滤所得的滤液进行进一步重力澄清 的澄清水罐， 以保证返回洗涤塔的洗涤水不含固体颗粒；
用于将含盐水泵送至洗涤塔的冷水循环泵； 用于将澄清水泵送至洗涤塔的澄 清水泵；
用于将含盐水冷却的水洗塔顶回流冷却器。
在本发明中， 当洗涤塔塔底的洗涤水压头不能满足微旋流分离器的压力降要 求时， 所述装置还包括对洗涤塔塔底的洗涤水进行增压的热水循环泵。
在本发明中， 微旋液分离器利用旋流离心作用， 分离效率可达到约 90%。 在本发明中， 所述微旋流分离器是由单根或若干根微旋流芯管并联组成的， 所述微旋流芯管的压力降不大于约 0.2MPa、 分离粒度不大于约 2μπι。
在本发明中， 所述澄清水罐可以选自重力沉降设备。
在本发明中， 在所述压滤机内， 采用再生器外排烟气对压滤机产生的氧化铬 催化剂滤饼进行烘干， 得到含水量较低的催化剂滤饼， 同时提高滤饼温度， 保证 喷入催化裂化再生烟气中的解毒温度达到 200-250°C ; 另外， 利用滤饼结构净化 再生气。
在本发明中， 所得的较高温度的催化剂滤饼返回再生器进行再生降毒处理。 以下根据附图详细说明本发明的装置结构及方法。
图 1是根据本发明一个实施方式的异丁烷脱氢制异丁烯中异丁烯夹带的废催 化剂浓缩干燥及解毒的处理工艺流程图。 如图 1所示， 异丁烷进入反应器 1进行 反应； 反应所得的异丁烯粗产品由反应器 1顶部送入过滤器 3进行过滤； 滤液由 过滤器 3底部与由反应器 1底部排出的失活催化剂一同送入再生器 2再生， 再生 得到的活性催化剂由再生器 2底部返回反应器 1使用， CO2由再生器 2顶部排出； 经过滤的高温异丁烯气体由过滤器 3顶部送入洗涤塔 4洗涤， 得到的异丁烯产品 排出回收， 得到的含废催化剂的洗涤废水经热水循环泵泵送至微旋流分离器 6进 行浓缩分离， 得到的废催化剂浓缩液由微旋流分离器 6底部排出送入压滤机 7， 得到失活催化剂滤饼， 利用再生气热量提高滤饼温度， 获得含水量较低的湿催化 剂滤饼， 并将湿催化剂滤饼送入再生器中回收催化剂； 所得的乏气由压滤机 7顶 部排出； 所得的滤液由压滤机 7顶部排出， 与由微旋流分离器 6顶部排出的微旋 流脱固后的洗涤水一同送入澄清水罐 8， 进行进一步的重力澄清， 所得的澄清水 经由澄清水泵 10， 连同经由冷水循环泵 9泵送的含盐水一同经回流冷却器 11冷 却后送入洗涤塔。 本发明的主要优点在于：
本发明采用旋流分离技术对洗涤塔洗涤水进行分离， 其分离精度高， 设备占地 面积小（与国外工艺相比减少了 90%) ， 且一定程度上抑制了溶剂发泡问题， 有效解 决了洗涤塔催化剂堵塞问题， 使得装置连续运行周期延长， 装置运行经济性提高； 同 时考虑了催化剂失活问题， 采用再生器对废催化剂进行解毒处理， 实现了催化剂的重 复利用， 降低了催化剂投入， 提高了设备的经济性。
另外， 本发明通过压滤机的使用， 对旋流底流部分进行了有效的压滤， 使得催 化剂滤饼含水量明显降低， 有效回收催化剂； 同时引入再生器外排烟气对压滤机产生 的氧化铬催化剂滤饼进行烘干， 得到含水量较低的催化剂滤饼， 一方面利用了再生气 热量对滤饼层进行烘干，并提高滤饼温度，保证喷入催化裂化再生烟气中的初始温度， 保障催化剂在再生器中的解毒温度， 有效降低了热量损失， 减少了能量的消耗， 另一 方面利用滤饼层对再生气进行净化过滤， 回收了再生气夹带的催化剂， 减少了物料的 损耗。 实施例
下面结合具体的实施例进一步阐述本发明。 但是， 应该明白， 这些实施例仅用 于说明本发明而不构成对本发明范围的限制。下列实施例中未注明具体条件的试验方 法， 通常按照常规条件， 或按照制造厂商所建议的条件。 除非另有说明， 所有的百分 比和份数按重量计。 实施例 1 :
在一个 10万吨 /年异丁烷脱氢制异丁烯装置中， 按照本发明的方法， 采用微 旋流分离器与压滤机组合对洗涤废水进行分离处理， 其具体运作过程及效果描述 如下：
1. 异丁烷脱氢制异丁烯装置去催化剂沉淀罐洗涤水物性参数，系统采用的负 载三氧化二铬的颗粒作为催化剂， 主要活性组分为 Cr2O3。 介质名称 水、 催化剂
流量， kg/h 30000
温度， 72
压力，
1.68
kg/cm2(a)
0-2 μπι 10%
2-4 μπι 8%
4-8 μπι 9%
8-12 μπι 10%
入口废催化剂
12~20μπι 35%
的粒度分布
20-30 μπι 22%
30~40μπι 5%
>40μπι 1 %
心 ±t、 100%
2. 工艺流程：
如图 1所示。
利用循环冷却水对异丁烷裂解反应生成的高温异丁烯气体进行洗涤， 得到含 废催化剂的洗涤废水； 对获得的洗涤废水， 采用微旋流分离的方法对废催化剂微 粒进行浓缩， 得到废催化剂浓缩液； 对所得的废催化剂浓缩液进行加压过滤， 进 一步脱除浓缩液中的游离水， 获得废催化剂滤饼； 采用异丁烷脱氢制异丁烯过程 中再生器的外排烟气在压滤机中对上述含废催化剂滤饼进行烘干， 获得含水量较 低的湿催化剂滤饼； 同时利用再生气热量提高催化剂滤饼温度， 保证催化剂再生 器的解毒反应温度达到再生器要求。
3. 结果分析：
使用本发明的方法与装置后， 最终所得为三股物料， 包括： 净化洗涤水、 滤 饼、 再生气。
微旋液分离器所得的进口、 溢流及底流含固量如下： 序号 名称 平均固含量
mg/L
1 进口 522
2 溢流 51
3 底流 4761
压滤机所得的滤液与滤饼含固量及含水率如下:
Figure imgf000012_0001
同时，再生气的热量得到有效利用，且有效脱除再生气所夹带的催化剂颗粒。 此外， 本发明的装置占地面积仅为原生产工艺的 1/10， 有效减小了设备建设 所用资金， 且延长了运行周期。 在本发明提及的所有文献都在本申请中引用作为参考， 就如同每一篇文献被 单独引用作为参考那样。 此外应理解， 在阅读了本发明的上述讲授内容之后， 本 领域技术人员可以对本发明作各种改动或修改， 这些等价形式同样落于本申请所 附权利要求书所限定的范围。

Claims

^
1. 一种异丁烷脱氢制异丁烯中异丁烯夹带的废催化剂浓缩干燥及解毒的处 理方法， 该方法包括以下步骤：
( a)利用循环冷却水对异丁烷裂解反应生成的高温异丁烯气体进行洗涤， 得 到含废催化剂的洗涤废水；
(b)采用微旋流分离对所得的洗涤废水中的废催化剂微粒进行浓缩， 得到废 催化剂浓缩液；
( c)对所得的废催化剂浓缩液进行加压过滤， 以进一步脱除浓缩液中的游离 水， 获得废催化剂滤饼；
( d)采用异丁烷脱氢制异丁烯过程中再生器的外排烟气对所得的废催化剂滤 饼进行烘干， 获得含水量低的湿催化剂滤饼； 同时利用再生气热量提高湿催化剂 滤饼温度； 以及
( e) 再生器内通入 CO气体， 进行氧化还原反应以再生催化剂。
2. 如权利要求 1所述的方法， 其特征在于， 异丁烯粗产品的温度为 600°C， 循环冷却水的温度为 35。C ， 洗涤废水的温度为 55 °C， 再生器内的温度为 200-250 °C。
3. 如权利要求 1所述的方法， 其特征在于， 含废催化剂的洗涤废水所携带的 废催化剂微粒的粒径为 0.1-40μπι， 微旋流分离的分离粒度不大于 2μπι、 压力降不 大于 0.2MPa。
4. 如权利要求 1所述的方法， 其特征在于， 所述微旋流分离所得的废催化剂 浓缩液的含水率为 60-99%， 经过加压过滤所得的废催化剂滤饼的含水率不高于 20% , 所得的滤液的催化剂含量不大于 20ppm。
5. 一种异丁烷脱氢制异丁烯中异丁烯夹带的废催化剂浓缩干燥及解毒的处 理装置， 该装置包括：
洗涤塔（4) ， 用于利用循环冷却水对异丁烷裂解反应生成的高温异丁烯气体 进行洗涤， 得到含废催化剂的洗涤废水；
与洗涤塔 （4) 连接的微旋流分离器 （6) ， 用于采用微旋流分离对所得的洗 涤废水中的废催化剂微粒进行浓缩， 得到废催化剂浓缩液；
与微旋流分离器 （6 ) 连接的压滤机 （7 ) ， 用于对所得的废催化剂浓缩液进 行加压过滤， 以进一步脱除浓缩液中的游离水， 获得废催化剂滤饼； 与压滤机 （7 ) 连接的再生器 （2) ， 用于采用异丁烷脱氢制异丁烯过程中再 生器的外排烟气对所得的废催化剂滤饼进行烘干，获得含水量低的湿催化剂滤饼; 同时利用再生气热量提高湿催化剂滤饼温度； 其中， 再生器内通入 CO气体， 进 行氧化还原反应以再生催化剂。
6. 如权利要求 5所述的装置， 其特征在于， 该装置还包括：
与洗涤塔 （4) 连接的过滤器 （3 ) ， 用于对与其连接的反应器 （1 ) 得到的异 丁烯粗产品进行过滤；
与微旋流分离器 （6) 和压滤机 （7 ) 连接的澄清水罐 （8 ) ， 用于对微旋流分 离后的洗涤废水和加压过滤所得的滤液进行进一步的重力澄清， 以保证返回洗涤 塔 （4) 的洗涤水不含固体颗粒；
与洗涤塔 （4) 连接的冷水循环泵 （9) ， 与冷水循环泵 （9) 连接的澄清水泵 ( 10) ， 用于将澄清的洗涤水送至洗涤塔 （4) ；
位于洗涤塔 （4) 塔顶的回流冷却器 （11 ) ， 用于将含盐水冷却。
7. 如权利要求 6所述的装置， 其特征在于， 在反应器 （1 ) 内， 在 585-620°C 的高温和小于 0.2MPa的低压下， 在催化剂作用下进行脱氢反应。
8. 如权利要求 5或 6所述的装置， 其特征在于， 当洗涤塔 （4) 塔底的洗涤 废水压头不能满足微旋流分离器（6) 的压力降要求时， 该装置还包括位于洗涤塔 ( 4) 塔底的热水循环泵 （5 ) ， 用于对洗涤塔 （4) 塔底的洗涤废水进行增压。
9. 如权利要求 5或 6所述的装置， 其特征在于， 所述微旋流分离器 （6) 是 由单根或多根微旋流芯管并联组成的， 所述微旋流芯管的压力降不大于 0.2MPa、 分离粒度不大于 2μπι、 分离效率达到 90%。
10. 如权利要求 5或 6所述的装置， 其特征在于， 所述澄清水罐 （8 ) 选自重 力沉降设备。
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