CN108083968B - Method for strengthening separation of dimethyl ether in crude isobutene - Google Patents
Method for strengthening separation of dimethyl ether in crude isobutene Download PDFInfo
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Abstract
The invention discloses a method for strengthening separation of dimethyl ether in crude isobutene, which comprises the processes of cold separation, water absorption, drying adsorption and the like. The method is a new method for separating dimethyl ether from crude isobutene at the top of the light component removal tower in the process of producing isobutene by cracking methyl tert-butyl ether, overcomes the defects of the conventional process of returning the crude isobutene to a methyl tert-butyl ether synthesis section to separate the dimethyl ether or avoids the waste phenomenon caused by directly discharging the crude isobutene to a pipe network for combustion, and has the advantages of simple and convenient operation, low energy consumption, remarkable separation effect and the like. The method is applied to the process for producing isobutene on a large scale by cracking methyl tert-butyl ether, and has obvious economic benefit and wide application prospect.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a method for strengthening separation of dimethyl ether in crude isobutene.
Background
Isobutene, also known as 2-methyl propylene, is an important organic chemical raw material. Isobutene can be divided into low-purity isobutene and high-purity isobutene according to different product purities in industrial production. Wherein, the low-purity isobutene generally requires the mass concentration of about 98.5 percent and is widely applied to the synthesis and preparation of antioxidants, pesticides, medical intermediates and other fine chemical products; the mass concentration of the high-purity isobutene is more than 99.9 percent, and the high-purity isobutene is mainly applied to the fields of butyl rubber, polyisobutylene and other macromolecules. In recent years, with the development of petrochemical industry and the extension of fine chemical industry chain in China, the demand for high-purity isobutene is increased sharply, and higher requirements on the quality of the high-purity isobutene are provided.
At present, the industrial production approach of isobutene mainly comes from mixed carbon-four liquefied gas, and the separation and preparation methods of isobutene include a sulfuric acid extraction separation method, a direct hydration separation method, a butane isomerization dehydrogenation method, a tert-butyl alcohol dehydration method, an etherification-cracking method and the like.
The technology for preparing isobutene by cracking methyl tert-butyl ether is an important isobutene production technology developed in the end of the 70 th 20 th century, and through technical innovation and improvement for decades, the technology forms a relatively complete technological process which comprises a methyl tert-butyl ether refining and reacting unit, a gas-liquid separating unit, a water washing unit, an isobutene light-removing unit, an isobutene heavy-removing unit and a methanol recovering unit. Moreover, with the continuous extension of the industry chain downstream of oil processing, the technology is receiving increasing attention from enterprises. Nevertheless, the disadvantage of difficult separation of dimethyl ether from crude isobutene at the top of the light component removal tower in the technology has not been solved substantially for a long time.
At present, crude isobutene in the top of the lightness-removing tower is mainly utilized in two aspects, namely, the stream is returned to an MTBE synthesis stage and is merged with a C4 stream from a battery compartment, the dimethyl ether is separated in a dimethyl ether removing tower after the MTBE is synthesized, and the refined MTBE is continuously sent to a methyl tert-butyl ether cracking device to produce isobutene; and the second is directly sent to a tank field to be used as liquefied gas. Even, there are a small number of small businesses that directly send this stream to a flare for combustion. Analyzing the utilization method of crude isobutene adopted in the prior art, or having the defects of additionally increasing production energy consumption and prolonging production period, or having the phenomenon of low utilization added value of crude isobutene, which causes waste of energy and resource values to different degrees. Under the situation that petroleum resources are gradually lacking in the global scope, the goal of realizing the maximization of the utilization value of the downstream resources in petroleum processing is significant.
Based on the difficult problem of utilization of the dimethyl ether-containing crude isobutene in China at present, the key point of improving the yield of isobutene and realizing continuous production is that dimethyl ether in the crude isobutene can be effectively separated. The technology for producing isobutene by cracking methyl tert-butyl ether is mature day by day, but according to the existing reports on dimethyl ether removal, the existing research on dimethyl ether separation still has many disadvantages. In summary, on one hand, the separation process is relatively complex, and relates to the processes of multistage absorption, multiple rectification and the like, the corresponding equipment investment is large, and the production energy consumption is high; on the other hand, part of the absorbent involved in the patent cannot be directly recycled due to the dissolution of the C4 olefin raw material, and the subsequent further separation and recovery of the solvent are required, which causes the loss of the raw material, reduces the recovery rate and increases the separation load.
Disclosure of Invention
Based on the existing method for separating dimethyl ether from crude isobutene in the conventional methyl tert-butyl ether cracking production process and the problems existing in the conventional research, the invention provides an enhanced separation method for dimethyl ether from crude isobutene, which comprises the separation processes of cold separation, water absorption, drying adsorption and the like. The method obviously strengthens the separation effect of dimethyl ether in the crude isobutene, the removal rate of the dimethyl ether is more than 99.99 percent, and the recovery rate of the isobutene is between 96 and 98 percent. Meanwhile, the method has the advantages of simple and convenient operation, low energy consumption and the like, and has wide application prospect.
In order to realize the aim, the invention discloses an enhanced separation method of dimethyl ether in crude isobutene, which has the following specific technical scheme:
1) cooling and condensing: cooling and condensing the crude isobutene component containing dimethyl ether in a cooler; wherein the condensing medium is salt-containing water or low boiling point liquefied organic matter (such as liquefied ethylene, liquefied propylene, etc.); because the condensation process belongs to a shallow low-temperature condensation system, and from the viewpoint of reducing the cost, 10 to 25 mass percent of salt-containing water is preferred, and most of the salt is sodium chloride or calcium chloride.
Wherein the cooling and condensing temperature is-5 ℃ to-25 ℃, and the normal pressure operation and the pressurization operation can be carried out.
By cooling and condensing, isobutene and a very small amount of dimethyl ether are liquefied, and most of dimethyl ether still keeps a gas phase state.
2) Separation: sending the components condensed in the step 1) to a gas-liquid separation tank, realizing the separation of liquefied components and gas-phase light components in the crude isobutene by using a tower bottom liquid cutting operation mode, and sending the gas-phase components to a torch system.
3) Water absorption: delivering the liquefied component separated in the step 2) to the bottom of an absorption tower, and meanwhile, enabling absorbent water to pass through the absorption tower from top to bottom from the top of the absorption tower, and carrying out countercurrent contact and mass transfer on the absorbent water and the gasified liquefied component from the bottom of the absorption tower; wherein the operation temperature of the absorption tower is 10-20 ℃, and the operation pressure is 0.8-1.2 MPa; the mass flow of the absorbent in the absorption tower is comprehensively determined by the mass flow of the liquefied material flow separated in the step 2) and the content of dimethyl ether in the liquefied material flow, generally speaking, the higher the relative mass flow of the absorbent is, the better the absorption effect is, and in order to enhance the mass transfer effect and reduce the energy consumption as much as possible, the mass flow ratio of the absorbent to the dimethyl ether is preferably controlled to be 10: 1-100: 1. In this process, the vast majority of the dimethyl ether in the crude isobutene is dissolved in water.
4) And (3) drying: delivering the isobutene absorbed by water into a dryer, and removing trace moisture brought out in the water solution absorption process in an adsorption drying mode to reduce the water content in the isobutene to be below 5 ppm; the drying agent in the dryer is one or more of calcium chloride, soda lime, silica gel drying agent and molecular sieve drying agent, wherein the silica gel drying agent can be a commonly used 2A microporous silica gel drying agent, and the molecular sieve drying agent can be a commonly used 3A molecular sieve.
5) Desorption and circulation: and (3) conveying the absorbent material flow containing the dimethyl ether in the step 3) to a normal-pressure flash tank, wherein the dimethyl ether dissolved in water is spontaneously released by the system due to poor water solubility of the dimethyl ether under normal pressure, and the desorbed water is continuously used in the water absorption link of the step 3). No dimethyl ether is present in the desorbed water.
In actual production, the production process of the method tends to a stable state mostly, and each component in the crude isobutene can be tracked and quantitatively analyzed, the analysis process has two methods, one is the analysis of a chromatographic on-line analyzer, and the other is the gas chromatography quantitative analysis performed in a laboratory after sampling, the two methods can quickly determine the content of dimethyl ether in the crude isobutene, and simultaneously, the mass flow of each material flow in the production can be remotely sent to a DCS system through a mass flow meter and corresponding data is directly read, so that the mass flow of the dimethyl ether can be easily determined, and the mass flow of an absorbent can be further determined. Other operations in the steps of the invention, which are not described, are conventional processes, and are not described herein again.
Compared with the prior art, the invention has the following innovation points:
1. the method only relates to three separation units of cold separation, water absorption and adsorption, and has the advantages of simple process, simple and convenient operation, low energy consumption and low equipment investment and maintenance cost;
2. the cold separation process in the invention can not only separate dimethyl ether in crude isobutene by a large margin at one time, but also avoid the loss of isobutene, thus being beneficial to improving the recovery rate of isobutene;
3. in the cold separation process, salt-containing water is preferably used as a cooling medium, and compared with other common cooling agents, the method can effectively achieve the separation effect and reduce the production cost;
4. under the condition of the invention, the absorbent absorbs the dimethyl ether and releases the pressure after flowing out, the dimethyl ether dissolved in water is spontaneously and completely released, and the cyclic utilization of the water can be realized;
5. the water content in the high-purity isobutene of the final product is less than 5ppm, so that the application requirement of downstream industries can be met;
6. the dimethyl ether separation method obviously strengthens the separation effect of dimethyl ether in the crude isobutene, the removal rate of the dimethyl ether is more than 99.99 percent, and the recovery rate of the isobutene is between 96 and 98 percent.
The process of the invention fundamentally provides an effective industrialized separation method for removing the dimethyl ether, has simple process, low energy consumption, high recovery rate and high yield, can obtain high-purity isobutene and meets the general requirements of national scientific and technical development planning. The method can meet the requirement of industrial application and production and has wide application value.
Drawings
FIG. 1 is a process flow diagram of the present invention for enhanced separation of dimethyl ether from crude isobutylene by a methyl tert-butyl ether cracking process;
wherein, 1 is a cooler, 2 is a gas-liquid separation tank, 3 is an absorption tower, 4 is a flash tank, and 5 is a dryer.
Detailed Description
The following further description of the present invention is provided in connection with specific embodiments to enable those skilled in the art to further understand the present invention, and not to limit the present invention, and all techniques based on the principles described herein are within the scope of the present invention.
Example 1
1) Cooling and condensing: cooling and condensing the crude isobutene component containing 7% of dimethyl ether by using an aqueous solution containing 15% of sodium chloride, wherein the cooling temperature is-15 ℃, and the pressure is 0.1 MPa;
2) separation: sending the components condensed in the step 1) to a gas-liquid separation tank, separating liquefied isobutene in a tower bottom-cutting liquid operation mode when the liquid level of a glass metering plate of the separation tank reaches 60%, and sending the separated dimethyl ether containing trace isobutene to a flare system, wherein the dimethyl ether content in the isobutene is 0.35%;
3) water absorption: delivering the liquefied component separated in the step 2) to the bottom of an absorption tower, and meanwhile, enabling absorbent water to pass through the absorption tower from top to bottom from the top of the absorption tower, and carrying out countercurrent contact and mass transfer on the absorbent water and the liquefied component from the bottom of the absorption tower; wherein the temperature of the absorbent water is controlled to be 15-18 ℃, the operating pressure of the absorption tower is 0.8MPa, and the mass flow ratio of the absorbent to the dimethyl ether is 50: 1. The content of dimethyl ether in isobutene at the top of the tower is 5ppm and the water content is 80ppm through analysis;
4) and (3) drying: delivering the isobutene absorbed by the water into a dryer with a 3A molecular sieve, and reducing the water content in the isobutene to 1ppm in an adsorption mode to finally obtain high-quality isobutene with the mass content of more than 99.99%, wherein the recovery rate of the isobutene in the whole process is 96.8%;
5) desorption and circulation: and (3) sending the absorbent material flow containing dimethyl ether in the step 3) to a normal-pressure flash tank, spontaneously releasing dimethyl ether dissolved in the aqueous solution by the system, and continuously using the desorbed aqueous solution for circulation in the step 3).
Example 2
1) Cooling and condensing: cooling and condensing the crude isobutene component containing 7% of dimethyl ether by using an aqueous solution containing 25% of calcium chloride, wherein the cooling temperature is-5 ℃, and the pressure is 0.8 MPa;
2) separation: sending the components condensed in the step 1) to a gas-liquid separation tank, separating liquefied isobutene in a tower bottom-cutting liquid operation mode and sending the liquefied isobutene to the bottom of an absorption tower when the liquid level of a glass metering plate of the separation tank reaches 45%, and sending the separated dimethyl ether containing trace isobutene to a torch system, wherein the dimethyl ether content in the isobutene is 0.42%;
3) water absorption: and (3) delivering the liquefied component separated in the step 2) to the bottom of the absorption tower, and meanwhile, enabling absorbent water to pass through the absorption tower from top to bottom of the absorption tower, and carrying out countercurrent contact and mass transfer on the absorbent water and the liquefied component from the bottom of the absorption tower. Wherein the temperature of the absorbent water is controlled to be 15-18 ℃, the operating pressure of the absorption tower is 1.2MPa, and the mass flow ratio of the absorbent to the dimethyl ether is 80: 1. Analysis determines that the dimethyl ether content in the isobutene at the top of the tower is 4.2ppm, and the water content is 86 ppm;
4) and (3) drying: delivering the isobutene absorbed by the water into a dryer filled with anhydrous calcium chloride, and reducing the water content in the isobutene to 1ppm in an adsorption mode to finally obtain high-quality isobutene with the mass content of more than 99.99%, wherein the recovery rate of the isobutene in the whole process is 97.6%;
5) desorption and circulation: and (3) sending the absorbent material flow containing dimethyl ether in the step 3) to a normal-pressure flash tank, spontaneously releasing dimethyl ether dissolved in the aqueous solution by the system, and continuously using the desorbed aqueous solution for circulation in the step 3).
Example 3
1) Cooling and condensing: cooling and condensing the crude isobutene component containing 5.8 percent of dimethyl ether by liquefied propylene, wherein the cooling temperature is-20 ℃ and the pressure is 0.3 MPa;
2) separation: sending the components condensed in the step 1) to a gas-liquid separation tank, separating liquefied isobutene in a tower bottom-cutting liquid operation mode when the liquid level of a glass metering plate of the separation tank reaches 50%, and sending the separated dimethyl ether containing trace isobutene to a flare system, wherein the dimethyl ether content in the isobutene is 0.25%;
3) water absorption: delivering the liquefied component separated in the step 2) to the bottom of an absorption tower, and meanwhile, enabling absorbent water to pass through the absorption tower from top to bottom from the top of the absorption tower, and carrying out countercurrent contact and mass transfer on the absorbent water and the liquefied component from the bottom of the absorption tower; wherein the temperature of the absorbent water is controlled to be 12-15 ℃, the operating pressure of the absorption tower is 1.0MPa, and the mass flow ratio of the absorbent to the dimethyl ether is 15: 1. The content of dimethyl ether in isobutene at the top of the tower is 5ppm and the water content is 36ppm through analysis;
4) and (3) drying: delivering the isobutene absorbed by the water into a dryer filled with 2A microporous silica gel, reducing the water content in the isobutene to 1ppm in an adsorption mode, and finally obtaining high-quality isobutene with the mass content of more than 99.99%, wherein the recovery rate of the isobutene in the whole process is 95.8%;
5) desorption and circulation: and (3) sending the absorbent material flow containing dimethyl ether in the step 3) to a normal-pressure flash tank, spontaneously releasing dimethyl ether dissolved in the aqueous solution by the system, and continuously using the desorbed aqueous solution for circulation in the step 3).
Example 4
1) Cooling and condensing: cooling and condensing the crude isobutene component containing 4% of dimethyl ether by liquefied ethylene, wherein the cooling temperature is-25 ℃ and the pressure is 0.1 MPa;
2) separation: sending the components condensed in the step 1) to a gas-liquid separation tank, separating liquefied isobutene in a tower bottom-cutting liquid operation mode when the liquid level of a glass metering plate of the separation tank reaches 30%, and sending the separated dimethyl ether containing trace isobutene to a flare system, wherein the dimethyl ether content in the isobutene is 0.18%;
3) water absorption: delivering the liquefied component separated in the step 2) to the bottom of an absorption tower, and meanwhile, enabling absorbent water to pass through the absorption tower from top to bottom from the top of the absorption tower, and carrying out countercurrent contact and mass transfer on the absorbent water and the liquefied component from the bottom of the absorption tower; wherein the temperature of the absorbent water is controlled to be 12-15 ℃, the operating pressure of the absorption tower is 1.0MPa, and the mass flow ratio of the absorbent to the dimethyl ether is 25: 1. Analysis determines that the dimethyl ether content in the isobutene at the top of the tower is 2ppm, and the water content is 48 ppm;
4) and (3) drying: delivering the isobutene absorbed by the water into a dryer filled with soda lime, and reducing the water content in the isobutene to 1ppm in an adsorption mode to finally obtain high-quality isobutene with the mass content of 99.99%, wherein the recovery rate of the isobutene in the whole process is 97.2%;
5) desorption and circulation: and (3) sending the absorbent material flow containing dimethyl ether in the step 3) to a normal-pressure flash tank, spontaneously releasing dimethyl ether dissolved in the aqueous solution by the system, and continuously using the desorbed aqueous solution for circulation in the step 3).
Claims (6)
1. The method for intensively separating dimethyl ether from crude isobutene is characterized by comprising the following steps of:
1) cooling and condensing: cooling and condensing the crude isobutene component containing dimethyl ether;
2) separation: sending the components condensed in the step 1) to a gas-liquid separation tank, realizing the separation of liquefied components and gas-phase light components in the crude isobutene by using a tower bottom liquid cutting operation mode, and sending the gas-phase components to a torch system;
3) water absorption: delivering the liquefied component separated in the step 2) to the bottom of an absorption tower, and meanwhile, enabling absorbent water to pass through the absorption tower from top to bottom from the top of the absorption tower, and carrying out countercurrent contact and mass transfer on the absorbent water and the gasified liquefied component from the bottom of the absorption tower;
4) and (3) drying: delivering the isobutene absorbed by water into a dryer, and removing trace moisture brought out in the water solution absorption process in an adsorption drying mode to reduce the water content in the isobutene to be below 5 ppm;
5) desorption and circulation: delivering the absorbent material flow containing dimethyl ether in the step 3) to a normal-pressure flash tank, spontaneously releasing dimethyl ether dissolved in water by the system, and continuously using the desorbed water in the water absorption link of the step 3);
the temperature of the cooling and condensing in the step 1) is-5 ℃ to-25 ℃.
2. The method for enhanced separation of dimethyl ether from crude isobutylene as claimed in claim 1, wherein: the condensing medium used in the condensing process in the step 1) is salt-containing water or low-boiling-point liquefied organic matter.
3. The method for enhanced separation of dimethyl ether from crude isobutylene as claimed in claim 2, wherein: the salt-containing water is 10-25% by mass, and the salt is sodium chloride or calcium chloride.
4. The method for enhanced separation of dimethyl ether from crude isobutylene as claimed in claim 1, wherein: the operation temperature of the absorption tower in the step 3) is 10-20 ℃, and the operation pressure is 0.8-1.2 MPa.
5. The method for enhanced separation of dimethyl ether from crude isobutylene as claimed in claim 1, wherein: the mass flow ratio of the absorbent to the dimethyl ether in the step 3) is controlled to be 10: 1-100: 1.
6. The method for enhanced separation of dimethyl ether from crude isobutylene as claimed in claim 1, wherein: and the drying agent in the dryer in the step 4) is one or more of calcium chloride, soda lime, silica gel drying agent and molecular sieve drying agent.
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| US5336841A (en) * | 1993-04-05 | 1994-08-09 | Chemical Research & Licensing Company | Oxygenate removal in MTBE process |
| RU2083541C1 (en) * | 1995-08-07 | 1997-07-10 | Товарищество с ограниченной ответственностью "Научно-исследовательский центр по нефтехимическим технологиям" | Process for preparing isobutylene from methyl- or ethyl- tert-butyl ether |
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