CN112871121B - Self-suction type continuous isomerization reaction device for alkane and use method thereof - Google Patents
Self-suction type continuous isomerization reaction device for alkane and use method thereof Download PDFInfo
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- 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
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a self-priming continuous isomerization reaction device for alkane and a using method thereof. The device consists of a gas pipeline, a control system (the control system comprises a feeding system and a reaction system) and a product cooling and collecting system. The gas pipeline is connected with a gas inlet pipeline of a liquid storage tank in the feeding system, a gas outlet pipeline of the liquid storage tank of the feeding system is connected with a self-suction stirring paddle of a high-pressure reaction kettle of the reaction system, and a liquid outlet of the high-pressure kettle is connected with a product cooling and collecting system through a pipeline. The liquid storage tank of the feeding system is provided with a feeding hole for adding raw materials into the liquid storage tank so as to form a continuous feeding process; the isomerization reaction is completed in a high-pressure reaction kettle after raw materials enter the high-pressure reaction kettle of the reaction system through a feeding system and are mixed with the ionic liquid catalyst in the kettle. The invention utilizes the characteristics of low temperature, high activity and lasting stability of the ionic liquid catalyst to apply the device to self-priming continuous isomerization reaction of alkane for the first time.
Description
Technical Field
The invention belongs to the technical field of petrochemical industry, and particularly relates to a self-suction type continuous isomerization reaction device for alkane and a using method thereof.
Background
At present, the limitation degree of toxic aromatic hydrocarbon in automobile fuel is increased, and the requirement of refineries on the process capable of increasing the octane number of non-aromatic oil products is obviously increased. The isomerization of paraffins is an important process for refineries to increase the octane number of light gasoline fractions. Octane number represents the ability of an oil combusted in an engine cylinder to resist knock. With the banning of tetraethyl lead (TEL) additives in gasoline, the technology of isomerization of lower alkanes has developed rapidly. The low octane component is partially replaced by an octane enhancer such as MTBE (methyl tert-butyl ether), which is limited, however, by contamination of groundwater. Refineries prefer the isomerization of lower alkanes, an environmentally benign process (free of carcinogenic benzene and other poisons), to increase the octane number of gasoline. As a product thereof, the isomerized oil has the following characteristics: the yield is high, the sulfur content is very low, and the catalyst does not contain olefin, aromatic hydrocarbon and benzene; the octane value of the product is obviously improved; octane sensitivity is small, Research Octane Number (RON) and Motor Octane Number (MON) typically differ by only 1.5 units; can improve the front-end octane number of the gasoline, and ensure that the distillation range and the octane number of the gasoline are reasonably distributed, thereby improving the starting performance of an engine. Along with the increase of the quantity of imported crude oil in China, the sources of the low-carbon alkane are gradually increased, but the production of an isomerized product by the low-carbon alkane in a self-suction continuous device is not reported yet. Therefore, the self-absorption continuous isomerization reaction device and method for catalyzing alkane by the ionic liquid catalyst have great practical and economic significance for industrially and continuously producing the isomerized products.
In the prior art patents, the main devices for isomerization of paraffins are: continuous flow fixed bed reactors (petrochemical and chemical, 2009(2): 37-40.), small fixed bed reactors, ACE (R) units and riser catalytic cracking units (petro-leu, 2005, 20(6): 14-19.), Penex-DIH isomerization units (petroleum refining and chemical, 2020), and the like. Although these isomerization units have been used in large quantities in industry, they are complex to operate, costly and are directed to catalyst systems that are solid catalysts: such as bifunctional catalyst, acidic solid catalyst, molecular sieve, etc., and is suitable for ionic liquid catalyst and the like, and has not been reported about a self-priming continuous isomerization reaction device with self-priming function.
In the prior art patents, the catalysts used for the isomerization of alkanes are mainly bifunctional catalysts. These bifunctional catalysts are mainly metal/acidic carrier bifunctional catalysts, wherein the metals are mainly noble metals such as Journal of the American Chemical Society, 136 (2014), 6830-6833, Catalysis Today, 259 (2016), 331-339, and non-noble metals such as Ni, Co, W, Mo, etc. are used in some researches to reduce the cost (CN 104289251A), and the acidic carrier is mainly metal oxide (WO 104289251A)3-ZrO2(Catalysis Today, 73 (2002): 95-103.、Molybdenum oxide (Applied Catalysis a-General, 242 (2003): 267-274., Catalysis Communications, 12 (2011): 1188-1192.), molecular sieves (Microporous and Mesoporous Materials, 164 (2012): 222-231., Journal of Catalysis, 330 (2015): 485-496.), and solid superacid SO4 2-/MxOy(ZrO2、TiO2、SiO2Etc.) (Catalysis Today, 81 (2003): 495-. However, most bifunctional catalysts are prone to carbon deposition, and are expensive, which increases the operation cost. Moreover, the isomerization reaction is exothermic reaction, and the lower reaction temperature is more favorable in thermodynamics, so that the reduction of the catalyst cost and the operation cost and the reduction of the isomerization reaction temperature are the development trends of the low-carbon alkane isomerization catalyst.
Ionic liquids have a wide range of promising applications due to their numerous enhanced properties. Lewis acidic ionic liquid is commonly used in low-carbon alkane alkylation (Fuel, 2017, (189): 203-. Therefore, the ionic liquid catalyst is applied to the alkane self-suction type continuous isomerization reaction device for the first time by utilizing the characteristics of low temperature, high activity and lasting stability of the ionic liquid catalyst, and has very important scientific research significance and practical value for the technical development of continuous production of isomeric products.
Disclosure of Invention
The invention aims to provide a self-priming continuous alkane isomerization reaction device which is low in cost and excellent in performance and aims at the catalysis of an ionic liquid catalyst, aiming at overcoming the defects in the prior art.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a self-suction type continuous isomerization reaction device for alkane mainly comprises a gas pipeline, a control system and a product cooling and collecting system, wherein the control system comprises a feeding system and a reaction system, the feeding system comprises a liquid storage tank, and the upper end of the liquid storage tank is respectively provided with a gas inlet, a feeding hole and a gas outlet; the reaction system comprises a high-pressure reaction kettle, wherein a self-suction stirring paddle is arranged in the middle of the high-pressure reaction kettle, and a discharge hole is formed in the upper right part of the high-pressure reaction kettle; one end of the gas pipeline is connected with external gas, the other end of the gas pipeline is connected with a gas inlet of a liquid storage tank in the feeding system, and a gas outlet of the liquid storage tank of the feeding system is connected with a self-suction stirring paddle of a high-pressure reaction kettle of the reaction system.
Furthermore, a self-suction stirring paddle of the high-pressure reaction kettle in the reaction system has a self-suction feeding function, a stirring shaft of the high-pressure reaction kettle is integrated with a spiral stirring paddle and is made of a hollow material, and the stirring shaft is connected with an air outlet of a liquid storage tank of the feeding system and is used for blowing a raw material into the high-pressure reaction kettle by gas so as to realize the mixing of the raw material alkane and the ionic liquid catalyst; the feed inlet of the liquid storage tank is used for adding raw material alkane into the liquid storage tank so as to realize the continuity of feeding, the liquid storage tank is made of transparent materials, a raw material detector (for detecting the residual condition of the raw material in the liquid storage tank) is not required to be arranged, and the residual quantity of the raw material is directly observed so as to add the raw material into the liquid storage tank.
Furthermore, a discharge port of a high-pressure reaction kettle in the reaction system is divided into two pipelines which are respectively connected with a product cooling and collecting system and an online real-time analysis system so as to realize continuous production or online real-time analysis of the isomerization products, the product cooling and collecting system is provided with a cooling circulating pump connected with a collecting tank, and the online real-time analysis system is connected into required analysis equipment according to specific requirements and is respectively used for continuous collection and analysis of the isomerization products of the alkanes.
Further, a thermometer is arranged at the left part of the high-pressure reaction kettle and used for monitoring the reaction temperature.
The use method for the alkane self-suction type continuous isomerization reaction device comprises the steps of respectively placing alkane and the ionic liquid catalyst in a liquid storage tank in a feeding system and a high-pressure reaction kettle in a reaction system, blowing alkane in the liquid storage tank into the high-pressure reaction kettle in the reaction system through nitrogen or inert gas to be mixed with the ionic liquid catalyst; the reaction is started after the reaction temperature, the purging flow and the stirring speed are set on a panel of the control system, reaction products enter a product cooling and collecting system through a gas outlet of the high-pressure reaction kettle to be collected or enter an online real-time analysis system to be analyzed, the whole process realizes the continuity of raw material feeding and the continuity of product discharging, and the continuous isomerization reaction of alkane catalyzed by the ionic liquid catalyst is realized.
Further, synthesis of ionic liquid catalyst: the specific synthesis method of the invention is as follows: in the step, the ionic liquid catalyst is imidazole, pyridine, quaternary ammonium type or quaternary phosphine type plasma liquid and is a compound represented by the following specific structure:
wherein X-Is AlCl4 -, Al2Cl7 -, CuAlCl5 -, AlBr4 -One or more metal halide anions; r is C1-C8Any one of the linear alkyl groups of (a); r' is other than C1-C8Any one of linear alkyl or-COOH, -SO3H, etc.; n = 1-6.
The ionic liquid catalyst used in the present invention can be prepared by the known prior art methods known to those skilled in the art
a. Synthesizing an ionic liquid precursor: accurately weighing a certain amount of A in a three-neck flask, adding a certain amount of organic solvent, fully stirring and dissolving, dropwise adding equimolar amount of B dissolved in the organic solvent under a protective atmosphere, and raising the temperature of the system to 70-120 ℃ after uniformly stirringoC, reacting for 12-36 h, cooling the system after the reaction is finished, removing the organic solvent, and separating unreacted raw materials from the product by a centrifugal separation method to obtain an ionic liquid precursor C;
b. synthesis of ionic liquid catalyst: accurately weighing a certain amount of ionic liquid precursor C in a three-neck bottle, adding dried D with a certain molar ratio in batches under a protective atmosphere, and after uniformly stirring, raising the temperature of the system to 70-120 DEGoC, reacting for 12-36 h, and finallyObtaining the ionic liquid catalyst.
Wherein said compound a: imidazole, pyridine, quaternary ammonium type, quaternary phosphonium type;
the compound B: one of 1, 3-propane sultone, 1, 4-butane sultone and propenyl-1, 3-sultone;
the compound C: is determined by the structures of A and B together;
the compound D: one or more of anhydrous aluminum trichloride, anhydrous zinc chloride, anhydrous copper bromide and anhydrous copper chloride;
the protective gas: nitrogen or other inert gas.
Further, the starting alkane: c4-C12Preferably C6-C10An alkane of (a); nitrogen or inert gas purge pressure: 0.1-5 MPa, preferably 0.5-2 MPa; temperature of catalytic reaction: 0-150 ℃, preferably 20-100 ℃; catalytic reaction time: 1-30d, preferably 2-20 d.
The invention has the advantages that:
(1) the self-suction stirring paddle has the advantages that: the stirring paddle of the high-pressure reaction kettle is used for adding raw materials into the high-pressure reaction kettle to be mixed with the ionic liquid catalyst, the raw materials directly enter the interior of the catalyst to be in full contact reaction with the catalyst, the reacted alkane isomerization product is gasified at the reaction temperature and rises to the top of the kettle, and then the reacted alkane isomerization product enters an air outlet pipeline of the high-pressure reaction kettle and passes through a cooling and collecting system or an online real-time analysis system;
(2) advantages of alkane separation from ionic liquid catalyst: alkane slowly enters the reaction kettle through bubbling, and the alkane slowly enters the high-pressure reaction kettle to be contacted with the ionic liquid catalyst, so that the contact area and the contact duration of the alkane and the active site of the ionic liquid catalyst are ensured, the reaction rate can be improved, and the reaction energy consumption can be reduced;
(3) the advantages of ionic liquid serialization are: the existing reaction device for catalyzing the ionic liquid catalyst does not relate to serialization, and the reaction system for catalyzing the ionic liquid catalyst is used in the serialization device, so that the research on the service life of the catalyst and various performance analyses are facilitated.
Drawings
FIG. 1 is an overall view of a self-priming continuous isomerization reaction apparatus for alkane according to the present invention;
FIG. 2 is a view showing an internal structure of a control system in the apparatus of the present invention;
in the figure: 1-air inlet, 2-feed inlet, 3-air outlet, 4-liquid storage tank, 5-thermometer, 6-high pressure reactor, 7-self-suction stirring paddle and 8-discharge outlet.
Detailed Description
The following examples further illustrate the practice of the present invention in detail, but should not be construed as limiting the scope of the invention.
Example 1
Referring to fig. 1 and 2, a self-priming continuous isomerization reaction device for alkane mainly comprises a gas pipeline, a control system and a product cooling and collecting system, wherein the control system comprises a feeding system and a reaction system, the feeding system comprises a liquid storage tank, and the upper end of the liquid storage tank is respectively provided with a gas inlet 1, a feeding port 2 and a gas outlet 3; the reaction system comprises a high-pressure reaction kettle 6, wherein a self-suction stirring paddle 7 is arranged in the middle of the high-pressure reaction kettle, and a discharge hole 8 is formed in the right upper part of the high-pressure reaction kettle 6; one end of the gas pipeline is connected with external gas, the other end of the gas pipeline is connected with a gas inlet 1 of a liquid storage tank 4 in the feeding system, and a gas outlet 3 of the liquid storage tank 4 of the feeding system is connected with a self-suction stirring paddle 7 of a high-pressure reaction kettle 6 of the reaction system.
In the embodiment, the self-suction type stirring paddle 7 of the high-pressure reaction kettle 6 in the reaction system has a self-suction feeding function, the stirring shaft of the self-suction type stirring paddle is integrated with the spiral stirring paddle and is made of a hollow material, and the stirring shaft is connected with the air outlet 3 of the liquid storage tank 4 of the feeding system and is used for blowing a raw material into the high-pressure reaction kettle 6 by gas so as to realize the mixing of the alkane and the ionic liquid catalyst; the feed inlet 2 of the liquid storage tank 4 is used for adding raw material alkane into the liquid storage tank 4 to realize the continuity of feeding, the liquid storage tank 4 is made of transparent materials, a raw material detector (for detecting the residual condition of the raw material in the liquid storage tank) is not needed, and the residual quantity of the raw material is directly observed so as to add the raw material into the liquid storage tank 4.
In this embodiment, the discharge port 8 of the high pressure reactor 6 in the reaction system is divided into two pipelines, which are respectively connected with the product cooling and collecting system and the online real-time analysis system to realize the continuous production or online real-time analysis of the isomerization products, the product cooling and collecting system is equipped with a cooling circulation pump connected with a collecting tank, and the online real-time analysis system is connected to the required analysis equipment according to specific requirements, and is respectively used for the continuous collection and analysis of the isomerization products of alkanes.
In this embodiment, a thermometer 5 is disposed at the left portion of the high pressure reactor 6 for monitoring the reaction temperature.
In the use method of the self-priming continuous alkane isomerization reaction device in the embodiment, alkane and an ionic liquid catalyst are respectively placed in a liquid storage tank 4 in a feeding system and a high-pressure reaction kettle 6 in a reaction system, and alkane in the liquid storage tank 4 is blown into the high-pressure reaction kettle 6 in the reaction system by nitrogen or inert gas to be mixed with the ionic liquid catalyst; the reaction is started after the reaction temperature, the purging flow and the stirring speed are set on a panel of the control system, reaction products enter a product cooling and collecting system through an air outlet 8 of the high-pressure reaction kettle 6 to be collected or enter an online real-time analysis system to be analyzed, the raw material feeding continuity and the product discharging continuity are realized in the whole process, and the continuous isomerization reaction of alkane catalyzed by the ionic liquid catalyst is realized.
In this example, the ionic liquid was an imidazole type ionic liquid, X-Is AlCl4 -. Raw material alkane: C5-C10 alkane; nitrogen or inert gas purge pressure: 0.1 MPa; temperature of catalytic reaction: 100 ℃; catalytic reaction time: 1 d. The conversion rates of the reactions were 95% (corresponding to C5 for the starting material), 98% (corresponding to C6), 97% (corresponding to C7), 99% (corresponding to C8), 95% (corresponding to C9) and 96% (corresponding to C10), respectively.
Although the present invention has been described in connection with the accompanying drawings, the present invention is not limited to the above-described embodiments, which are only illustrative and not restrictive, and many modifications may be made by those skilled in the art without departing from the spirit of the present invention, within the scope of the present invention.
Claims (5)
1. A is used for self-priming continuous isomerization reaction unit of alkane which characterized in that: the device mainly comprises a gas pipeline, a control system and a product cooling and collecting system, wherein the control system comprises a feeding system and a reaction system, the feeding system comprises a liquid storage tank, and the upper end of the liquid storage tank is respectively provided with a gas inlet, a feed inlet and a gas outlet; the reaction system comprises a high-pressure reaction kettle, wherein a self-suction stirring paddle is arranged in the middle of the high-pressure reaction kettle, and a discharge hole is formed in the upper right part of the high-pressure reaction kettle; one end of the gas pipeline is connected with external gas, the other end of the gas pipeline is connected with a gas inlet of a liquid storage tank in the feeding system, and a gas outlet of the liquid storage tank of the feeding system is connected with a self-suction stirring paddle of a high-pressure reaction kettle of the reaction system;
the self-suction type stirring paddle of the high-pressure reaction kettle in the reaction system has a self-suction feeding function, a stirring shaft of the reaction system is integrated with the spiral stirring paddle and is made of a hollow material and is connected with an air outlet of a liquid storage tank of the feeding system, and a feeding port in the liquid storage tank is used for introducing alkane;
a discharge port of a high-pressure reaction kettle in the reaction system is divided into two pipelines which are respectively connected with a product cooling and collecting system and an online real-time analysis system, so that the continuous production or online real-time analysis of heterogeneous products is realized;
the use method for the alkane self-suction type continuous isomerization reaction device comprises the steps of respectively placing alkane and the ionic liquid catalyst in a liquid storage tank in a feeding system and a high-pressure reaction kettle in a reaction system, blowing alkane in the liquid storage tank into the high-pressure reaction kettle in the reaction system through nitrogen or inert gas to be mixed with the ionic liquid catalyst; the reaction is started after the reaction temperature, the purging flow and the stirring speed are set on a panel of the control system, reaction products enter a product cooling and collecting system through a gas outlet of the high-pressure reaction kettle to be collected or enter an online real-time analysis system to be analyzed, the whole process realizes the continuity of raw material feeding and the continuity of product discharging, and the continuous isomerization reaction of alkane catalyzed by the ionic liquid catalyst is realized.
2. The self-priming continuous isomerization reactor for alkanes of claim 1, wherein: and a thermometer is arranged at the left part of the high-pressure reaction kettle and used for monitoring the reaction temperature.
3. The self-priming continuous isomerization reactor for alkanes of claim 1, wherein: the alkane is C4-C12The ionic liquid comprises imidazole, pyridine, quaternary ammonium type or quaternary phosphonium type ionic liquid.
4. The self-priming continuous isomerization reactor for alkanes of claim 1, wherein: the blowing pressure of the nitrogen or the inert gas is 0.1-5 MPa.
5. The self-priming continuous isomerization reactor for alkanes of claim 1, wherein: the catalytic reaction temperature is 0-150 ℃, and the reaction time is 1-30 d.
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| CN1291954C (en) * | 2004-01-19 | 2006-12-27 | 中国石油化工股份有限公司 | Akylation reaction method for solid acid catalyzed isomeric paraffine and olefins |
| CN203408682U (en) * | 2013-06-26 | 2014-01-29 | 沈阳化工大学 | Double-analysis high-pressure micro-reaction pilot plant |
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