CN107879876B - Method and device for producing ethylene and propylene from light hydrocarbon raw material - Google Patents
Method and device for producing ethylene and propylene from light hydrocarbon raw material Download PDFInfo
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Abstract
The invention relates to the field of ethylene and propylene production from light hydrocarbon raw materials, and discloses a method and a device for producing ethylene and propylene from light hydrocarbon raw materials. The method comprises the following steps: (1) cracking light hydrocarbon raw materials to obtain cracked gas; (2) contacting the pyrolysis gas with maleic anhydride, wherein C in the pyrolysis gas4Carrying out copolymerization reaction on terminal olefin and maleic anhydride; (3) carrying out gas-liquid separation on the product obtained by the copolymerization reaction to obtain a gas-phase product and a liquid-solid mixture; (4) carrying out gas phase separation on the gas phase product to obtain ethylene, propylene, ethane and propane, and simultaneously obtaining ethane and propane as cycle materials; (5) separating the liquid-solid mixture to obtain C in the pyrolysis gas4Copolymers of terminal olefins with maleic anhydride; wherein the pyrolysis gas contains 0.1-10 wt% of C4A terminal olefin. Can effectively utilize light hydrocarbon raw materials to produce ethylene and propylene, produce cross-linked copolymer and reduce the energy consumption in the cracking separation process.
Description
Technical Field
The invention relates to the field of ethylene and propylene production from light hydrocarbon raw materials, in particular to a method and a device for producing ethylene and propylene from light hydrocarbon raw materials.
Background
Ethylene and propylene are important basic organic chemical raw materials, and products and derivative products thereof relate to various fields of national economy.
At present, the industrial process for producing ethylene and propylene mainly adopts a petrochemical production process, the adopted main production process is a steam cracking process, and the used raw material is naphtha; and a catalytic cracking process, wherein the raw material mainly comprises hydrocarbon oil capable of catalytic cracking.
The steam cracking process is the most mature technology and the most widely applied. However, in the current steam cracking process, cracking products such as ethylene and propylene are obtained by separating and purifying the cracking products, and the separation process has the problem of high energy consumption.
At present, on one hand, the industry has a strong demand on raw materials for producing ethylene and propylene, but the energy consumption of the separation process of the steam cracking process is high; on the other hand, in the petrochemical production process, a large amount of light hydrocarbon raw materials, such as light hydrocarbon raw materials, are also produced, and are mainly treated in a combustion mode at present and cannot be well utilized.
CN101781387A discloses a method for copolymerization of maleic anhydride/conjugated diene.
CN102212166B discloses a copolymerization reaction method of dicyclopentadiene and maleic anhydride, which has the advantages of simple reaction system, easy product separation, clean surface of the prepared polymer microsphere, uniform particle size, controllable morphology and good dispersibility under the condition of not increasing a stabilizer and a co-stabilizer.
CN102690393A discloses a copolymer containing functional groups, which is prepared from C5 mixed-maleic anhydride. The C5 mixture and maleic anhydride are copolymerized alternately to prepare the highly crosslinked copolymer containing functional groups in one step, thereby fully utilizing the olefin and the diene in the C5 mixture, and not concerning the condition of the low-carbon olefin below C5.
Therefore, the problems of high energy consumption in the separation process of steam cracking and processing and utilization of light hydrocarbon raw materials need to be solved.
Disclosure of Invention
The invention aims to solve the problems of processing and utilizing light hydrocarbon raw materials and reducing high energy consumption in the steam cracking separation process, and provides a processing method and a device for producing ethylene and propylene from the light hydrocarbon raw materials. The method can realize the production of ethylene and propylene products from light hydrocarbon raw materials, and in the process, the pyrolysis gas is subjected to copolymerization reaction firstly, so that the terminal olefin in the pyrolysis gas is separated and polymerized to prepare the cross-linked polymer containing the maleic anhydride functional group, the raw material which can be used as a functional material is provided, the pyrolysis gas reduces the terminal olefin component and then is separated to obtain ethylene and propylene, and the energy consumption in the separation process can be reduced.
In order to achieve the above object, the present invention provides a method for producing ethylene and propylene from light hydrocarbon raw materials, comprising the steps of: (1) under the condition of steam cracking, carrying out cracking reaction on a light hydrocarbon raw material, and carrying out gas-liquid separation on a cracking reaction product to obtain cracking gas; (2) in the presence of an initiator and an organic solvent, the pyrolysis gas is contacted with maleic anhydride, and C in the pyrolysis gas4Partially or totally copolymerizing the terminal olefin with maleic anhydride; (3) carrying out gas-liquid separation on the product obtained in the step (2) to obtain a gas-phase product and a liquid-solid mixture; c in the gas-phase product based on the total weight of the gas-phase product4The content of terminal olefin is 1 wt% or less; (4) carrying out gas phase separation on the gas phase product obtained in the step (3) to obtain ethylene, propylene, ethane and propane, and adding the ethane and the propane serving as circulating materials into the light hydrocarbon raw material obtained in the step (1); (5) separating the liquid-solid mixture obtained in the step (3) to obtain a solid product and a liquid, wherein the solid product is a polymer containing a maleic anhydride functional group; the liquid is returned to the step (2)In the above-mentioned organic solvent; wherein the pyrolysis gas contains 0.1-10 wt% of C4A terminal olefin; the light hydrocarbon raw material is one or more of ethane, propane and liquefied petroleum gas.
The invention also provides a device for producing ethylene and propylene by using the light hydrocarbon raw material, which comprises: cracking equipment, polymerization equipment, a gas-liquid separator, gas-phase separation equipment and a liquid-solid separator; wherein the content of the first and second substances,
the cracking equipment is used for introducing light hydrocarbon raw materials to carry out cracking reaction; the polymerization equipment is communicated with the cracking equipment and is used for carrying out copolymerization reaction on the cracked gas discharged by the cracking equipment and maleic anhydride;
the gas-liquid separator is communicated with the polymerization equipment and is used for carrying out gas-liquid separation on a product obtained by the copolymerization reaction and discharged by the polymerization equipment to obtain a gas-phase product and a liquid-solid mixture;
the gas phase separation equipment is communicated with the gas-liquid separator and is used for separating the gas phase product to obtain ethylene, propylene, ethane and propane;
said vapor phase separation apparatus being in communication with said cracking apparatus for recycling ethane and propane back to said cracking apparatus;
the liquid-solid separator is communicated with the gas-liquid separator and is used for separating the liquid-solid mixture to obtain a polymer containing maleic anhydride functional groups; the liquid-solid separator is in communication with the polymerization apparatus to return separated liquid.
According to the technical scheme, the light hydrocarbon raw materials are subjected to steam cracking, copolymerization reaction, gas-liquid separation, gas-phase separation and liquid-solid separation in sequence, so that the light hydrocarbon raw materials can be effectively processed and utilized to produce ethylene and propylene, and the yield of the ethylene and the propylene can reach 20-37%. In the copolymerization, C in the cracking gas4The copolymerization conversion rate of the terminal olefin can reach 85-90%, the gel content in the obtained cross-linked copolymer reaches more than 85 wt%, and the cross-linked copolymer can be used as a raw material for producing functional materials.
In the invention, on one hand, the production of light hydrocarbon raw materials can be realized to obtain ethylene and propylene products, and on the other hand, the cross-linked copolymer containing a maleic anhydride structure can be obtained and can be further used as a raw material for producing functional materials. Meanwhile, the components in the cracking gas are separated through copolymerization reaction, so that the energy consumption is saved in the separation process of obtaining ethylene and propylene products compared with the separation process of cracking gas in the prior art.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic diagram of a process flow for producing ethylene and propylene from a light hydrocarbon feedstock provided by the present invention.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for producing ethylene and propylene by using light hydrocarbon raw materials, which comprises the following steps: (1) under the condition of steam cracking, carrying out cracking reaction on a light hydrocarbon raw material, and carrying out gas-liquid separation on a cracking reaction product to obtain cracking gas; (2) in the presence of an initiator and an organic solvent, the pyrolysis gas is contacted with maleic anhydride, and C in the pyrolysis gas4Partially or totally copolymerizing the terminal olefin with maleic anhydride; (3) carrying out gas-liquid separation on the product obtained in the step (2) to obtainA gas phase product and a liquid-solid mixture; c in the gas-phase product based on the total weight of the gas-phase product4The content of terminal olefin is 1 wt% or less; (4) carrying out gas phase separation on the gas phase product obtained in the step (3) to obtain ethylene, propylene, ethane and propane, and adding the ethane and the propane serving as circulating materials into the light hydrocarbon raw material obtained in the step (1); (5) separating the liquid-solid mixture obtained in the step (3) to obtain a solid product and a liquid, wherein the solid product is a polymer containing a maleic anhydride functional group; the liquid is returned to the organic solvent in the step (2); wherein the pyrolysis gas contains 0.1-10 wt% of C4A terminal olefin; the light hydrocarbon raw material is one or more of ethane, propane and liquefied petroleum gas.
In the present invention, the liquefied petroleum gas is not particularly limited, and preferably the liquefied petroleum gas may contain 1 to 5 wt% of ethane, 0 to 4 wt% of ethylene, 16 to 60 wt% of propane, 0 to 16 wt% of propylene, 20 to 46 wt% of butane, 0.1 to 6 wt% of butene, and may further contain methane, hydrogen, and the like. Specifically, for example, hydrogen 0.2 wt%, methane 0.07 wt%, ethane 2.36 wt%, propane 55.9 wt%, propylene 0.57 wt%, butane 22.89 wt%, butene 0.56 wt%, C5Component 2.9 wt%.
The process flow diagram of the method provided by the invention is shown in figure 1.
Steam cracking
According to the invention, the steam cracking reaction of step (1) is used for converting light hydrocarbon feedstock into olefin-containing feedstock. C in the resulting cracked gas4The terminal olefin can be separated from the cracked gas by subsequent copolymerization reaction and utilized. C in cracking gas4The terminal olefins may include 1, 3-butadiene, isobutylene, 1-butene. In addition, the composition of the cracking gas can also contain normal butane, isobutane, ethylene, propylene, ethane, propane, methane and hydrogen. Preferably, the cracked gas may further contain 1 to 30% by weight of ethane, 20 to 60% by weight of ethylene, 0.1 to 10% by weight of propylene, and 0.1 to 35% by weight of propane. The composition of the cracking gas can be determined by gas chromatography using an alcoholAnalysis was performed by a Torrent 7890A Gas Chromatograph (GC).
According to the invention, the cracking reaction can convert light hydrocarbon raw materials into cracking gas containing ethylene and propylene, and then the cracking gas is further processed and utilized. Preferably, in the cracking reaction, the temperature of the cracking reaction is 800-880 ℃.
Preferably, the cracking reaction pressure is 0.15-0.25 MPa.
In the invention, the cracking reaction can be carried out in a steam cracking furnace which is conventionally used in the field, for example, a CB L-R type cracking furnace can be adopted, and the cracking reaction temperature, namely the furnace tube outlet temperature of the steam cracking furnace, is preferably 800-840 ℃.
According to the invention, in the cracking reaction, the weight ratio of the light hydrocarbon raw material to the water vapor is 1: (0.3-0.65). When the light hydrocarbon raw material is a mixture of a plurality of light hydrocarbon compounds, the weight ratio of each light hydrocarbon compound to the water vapor is 1: (0.3-0.65). For example, when the light hydrocarbon raw material is a mixture of ethane, propane and liquefied petroleum gas, the weight ratio of ethane to water vapor is 1: (0.3-0.65), wherein the weight ratio of propane to water vapor is 1: (0.3-0.65), wherein the weight ratio of the liquefied petroleum gas to the water vapor is 1: (0.3-0.65).
In the present invention, the cracked gas obtained in step (1) may be further cooled, for example, the cracked gas may be introduced into a water scrubber to be cooled, and the cracked gas having a reduced temperature may be discharged from the top of the tower. The temperature of the pyrolysis gas can reach 300-650 ℃ when the pyrolysis gas leaves the steam cracking furnace, the pyrolysis gas is further cooled in a washing tower, and the temperature of the top of the washing tower can be 35-90 ℃.
Copolymerization reaction
According to the invention, the step (2) is used for carrying out copolymerization reaction on the pyrolysis gas obtained in the step (1), and C in the pyrolysis gas can be used4The terminal olefin component and the maleic anhydride are subjected to copolymerization reaction to obtain the crosslinked copolymer for utilization, and the energy consumption of the separation process can be reduced when ethylene and propylene products are separated from pyrolysis gas. Although conventional separation means are still used to separate the ethylene and propylene products, due to C4The terminal olefin component has passedThe copolymerization reaction is separated from the cracked gas, so that the raw materials entering the separation of ethylene and propylene are reduced, and the energy consumption requirement in the separation process can be reduced. Preferably, in the step (2), the weight ratio of the pyrolysis gas to the maleic anhydride is 0.3: 1 or more, preferably the weight ratio of the pyrolysis gas to the maleic anhydride is (0.3-3): 1, more preferably, the weight ratio of the pyrolysis gas to the maleic anhydride is (0.8-3): 1. can realize more effective copolymerization reaction and more effective separation of C in the pyrolysis gas4A terminal olefin component.
In order to achieve more efficient copolymerization according to the present invention, it is preferable that the initiator is used in an amount of 0.01 to 30 mol% based on maleic anhydride.
According to the present invention, it is preferable that the initiator allows the pyrolysis gas to more efficiently undergo a copolymerization reaction with maleic anhydride, and it is preferable that the initiator is a thermal decomposition type initiator, and it is preferable that the initiator is at least one selected from the group consisting of dibenzoyl peroxide, dicumyl peroxide, di-t-butyl peroxide, lauroyl peroxide, t-butyl peroxybenzoate, diisopropyl peroxydicarbonate, dicyclohexyl peroxydicarbonate, azobisisobutyronitrile, and azobisisoheptonitrile. More preferably, the initiator is selected from azobisisobutyronitrile and/or dibenzoyl peroxide.
According to the invention, the organic solvent is added in an amount sufficient to dissolve the initiator and the maleic anhydride, and preferably, in the step (2), the amount of the maleic anhydride is less than 30 wt% of the organic solvent; the maleic anhydride is preferably used in an amount of 5 to 25 wt%, more preferably 10 to 20 wt% based on the organic solvent.
According to the invention, the organic solvent may be used to dissolve the initiator and maleic anhydride, preferably, in step (2), the organic solvent is selected from alkanes, aromatic hydrocarbons and compounds of formula R1-COO-R2At least one of organic acid alkyl esters of (1), wherein R1And R2Is C1～C5Alkyl group of (1).
In the present invention, the organic acid alkyl ester is selected from at least one of but not limited to methyl formate, ethyl formate, methyl propyl ester, methyl butyl ester, methyl isobutyl ester, amyl formate, methyl acetate, ethyl ester, propylene acetate, butyl acetate, isobutyl acetate, sec-butyl acetate, amyl acetate, isoamyl acetate, benzyl acetate, methyl propionate, ethyl propionate, butyl propionate, methyl butyrate, ethyl butyrate, butyl butyrate, isobutyl butyrate, isoamyl isovalerate, methyl benzoate, ethyl benzoate, propyl benzoate, butyl benzoate, isoamyl benzoate, methyl phenylacetate and ethyl phenylacetate. More preferably, the organic acid alkyl ester is isoamyl acetate.
In the present invention, the alkane is selected from, but not limited to, at least one of propane, n-butane, isobutane, pentane, isopentane, n-hexane, isohexane, cyclohexane, n-heptane, n-octane, and isooctane.
In the present invention, the aromatic hydrocarbon is selected from, but not limited to, at least one of benzene, toluene, xylene, chlorobenzene, and bromobenzene.
According to the invention, the copolymerization reaction can realize the selective utilization of C in the pyrolysis gas4The terminal olefin component and maleic anhydride are subjected to copolymerization reaction to obtain a raw material which can be further used as a functional material, and C is separated from the components of the pyrolysis gas4The olefin is terminated, so that the ethylene and propylene products obtained from the residual components are more convenient, and the energy consumption for separating the ethylene and the propylene is reduced compared with the conventional cracking gas. Preferably, in the step (2), the copolymerization reaction temperature is 50-90 ℃, the copolymerization reaction pressure is 0-0.25 MPa, and the copolymerization reaction time is 0.5-12 h. The copolymerization pressure is preferably 0.1 to 0.2MPa, and more preferably 0.12 to 0.15 MPa. The preferable copolymerization reaction time is 4-12 h.
According to the invention, it is particularly preferred that the copolymerization is a free radical polymerization. The 1, 3-butadiene in the pyrolysis gas is polymerized mainly in a 1,2 mode, and the side chain of the polymer chain segment contains double bonds (double bonds on 3 and 4 positions) to further react to form a cross-linking structure.
In a preferred embodiment, the copolymerization is carried out in a process comprising: and mixing the organic solvent, maleic anhydride and the initiator to form organic reaction liquid, and then adding the pyrolysis gas into the organic reaction liquid to carry out copolymerization reaction.
In the present invention, the polymerization reactor for carrying out the copolymerization reaction may be a pressure-resistant reaction vessel with a stirrer and a jacket or a tubular reactor. The medium in the jacket is used for removing reaction heat and controlling the reaction temperature.
Separation of
In the present invention, after the copolymerization reaction is completed, the copolymerization reaction product needs to be separated to obtain ethylene and propylene products and a polymer product. Two-stage separation can be adopted: the first stage is gas-liquid separation to obtain gas phase product and liquid-solid mixture; the second stage comprises two processes, wherein one process is to carry out gas phase separation on the gas phase product to obtain ethylene and propylene; another process is that the liquid-solid mixture is separated into the polymer containing the maleic anhydride functional group and the liquid through liquid-solid separation.
First, gas-liquid separation
According to the present invention, the step (3) is for gas-liquid separating the product of the copolymerization reaction of the step (2).
In the invention, after the copolymerization reaction is finished, the copolymerization reaction product is subjected to gas-liquid separation and liquid-solid separation in sequence, and the obtained solid product is washed and dried to obtain the crosslinked copolymer with the particle size range of 150-2000 nm.
In the present invention, the gas-liquid separation method may be flash separation. Preferably, the flash separation conditions are: reducing the pressure of a product subjected to the copolymerization reaction to be less than 0MPa at the temperature of more than 20 ℃, preferably 20-40 ℃, wherein C in the product4The following hydrocarbon compounds were discharged to obtain the gas phase product.
In the present invention, the terminal olefin content in the gas product can be measured by gas chromatography using agilent 7890A Gas Chromatograph (GC). Wherein, C4The content of terminal olefin is 1 wt% or less.
In the invention, the flash separator can be a simple container with a jacket for controlling temperature, various internal components which are commonly known in the field and used for fully increasing the surface area of materials can be provided, and hot special material flow can be introduced from the bottom of the device to fully increase the heat exchange quantity.
Second, gas phase separation and liquid-solid separation
1. Gas phase separation
According to the invention, step (4) is used to subject the gas-phase product to a gas-phase separation from which ethylene and propylene products are separated.
The gas phase separation can be carried out by conventional separation techniques for cracked gas in existing steam cracking processes, for example, the gas phase product can be cooled first and then separated by a front-end depropanization separation technique, for example, further separation and purification, to obtain ethylene, propylene, ethane and propane. Specifically, in the invention, for example, the gas-phase product is cooled to about 40 ℃, and then sent to a separation device such as a compressor for separation and purification, so that ethane and propane are obtained and returned to the light hydrocarbon raw material as circulating materials. Conventional separation techniques for cracked gas are not described herein in detail as long as separation of ethylene, propylene, ethane, and propane is achieved.
2. Liquid-solid separation
And carrying out liquid-solid separation on the liquid-solid mixture to obtain a polymer product.
In the present invention, the method of liquid-solid separation may be centrifugal separation under the following conditions: under the condition that the centrifugal rotating speed is more than 4000rpm, the centrifugal separation time is more than 5min, for example, the centrifugal rotating speed is 4000-16000 rpm, the centrifugal separation time is 5-20 min, and the liquid-solid mixed liquid is separated into supernatant liquid and lower-layer solid; the clear solution is an organic solvent and is removed and returned for the copolymerization reaction.
In the present invention, the centrifugal separator may be of any type, horizontal or vertical.
According to the invention, the solid product obtained by the liquid-solid separation is a polymer containing maleic anhydride functional groups, preferably the polymer is C in the pyrolysis gas4A crosslinked copolymer of a terminal olefin and maleic anhydride; preferably, the content of the maleic anhydride structural unit in the polymer is 48 to52 mol% and the gel content of the polymer is 85 to 92 wt%. Preferably, the maleic anhydride structural unit contained in the polymer can be in a main chain, a side chain or a terminal group. The content of the maleic anhydride structural unit can be determined by elemental analysis.
Preferably, the polymer may further contain a structural unit formed from at least one of 1-butene, 1, 3-butadiene and isobutylene.
Preferably, the polymer is a powder solid substance, and the average diameter of the particles can be 0.2-250 μm. The average diameter of the polymer particles can be measured by scanning electron microscopy.
In the present invention, the polymer may be a crosslinked copolymer, for example, a crosslinked structure may be formed between different polymer segments by a vinyl group introduced by a 1, 3-butadiene monomer. The gel content of the polymer can be determined by acetone extraction, reflecting the degree of crosslinking in the polymer, i.e. the degree of crosslinking of the polymer. Putting a certain amount of polymer in a Soxhlet extractor, extracting soluble components in the Soxhlet extractor to constant weight by using boiling acetone reflux, and measuring the proportion of the non-extractable part in the original polymer, namely the crosslinking degree.
The reaction conversion rate of the copolymerization reaction can be determined by weighing the weight of the polymer obtained after the reaction.
The invention selectively converts C in the cracked gas4The terminal olefin and maleic anhydride are preferably converted into a polymer containing maleic anhydride functional groups through radical copolymerization, and the polymer can be used as a raw material of a functional material and can be further prepared into other high molecular materials.
Further, the present invention can preferably perform the following steps for producing ethylene and propylene from light hydrocarbon feedstock:
(a) carrying out steam cracking on a light hydrocarbon raw material, and carrying out cracking reaction to obtain cracked gas; cooling the cracked gas by a water washing tower, and discharging the cooled cracked gas;
(b) carrying out copolymerization reaction on the pyrolysis gas and maleic anhydride, and carrying out gas-liquid separation on the obtained product to obtain a gas-phase product and a liquid-solid mixture;
(c) carrying out gas phase separation on the gas phase product to obtain ethylene, propylene, ethane and propane; ethane and propane are returned to the light hydrocarbon feedstock;
(d) and carrying out liquid-solid separation on the liquid-solid mixture to obtain the crosslinked copolymer.
The pressures involved in the present invention are gauge pressures.
Fig. 1 is a schematic diagram of a preferred embodiment of the present invention, and the working process can be briefly described as follows:
continuously introducing a light hydrocarbon raw material into a cracking device for steam cracking, introducing the obtained cracking gas into a polymerization reactor added with maleic anhydride, an initiator and an organic solvent, carrying out copolymerization reaction at a certain temperature, pressure and retention time, and introducing the obtained product into a gas-liquid separator for gas-liquid separation to obtain a gas-phase product and a liquid-solid mixture; introducing the gas-phase product into a gas-phase separation device to separate ethylene and propylene as products, and returning the separated ethane and propane to a cracking device; and (3) sending the liquid-solid mixture into a liquid-solid separator for liquid-solid separation to obtain a solid component, namely the polymer, and obtain liquid, namely the organic solvent, for recycling the copolymerization reaction.
The invention also provides a device for producing ethylene and propylene by using the light hydrocarbon raw material, which comprises: cracking equipment, polymerization equipment, a gas-liquid separator, gas-phase separation equipment and a liquid-solid separator; wherein the content of the first and second substances,
the cracking equipment is used for introducing light hydrocarbon raw materials to carry out cracking reaction; the polymerization equipment is communicated with the cracking equipment and is used for carrying out copolymerization reaction on the cracked gas discharged by the cracking equipment and maleic anhydride;
the gas-liquid separator is communicated with the polymerization equipment and is used for carrying out gas-liquid separation on a product obtained by the copolymerization reaction and discharged by the polymerization equipment to obtain a gas-phase product and a liquid-solid mixture;
the gas phase separation equipment is communicated with the gas-liquid separator and is used for separating the gas phase product to obtain ethylene, propylene, ethane and propane; said vapor phase separation apparatus being in communication with said cracking apparatus for recycling ethane and propane back to said cracking apparatus;
the liquid-solid separator is communicated with the gas-liquid separator and is used for separating the liquid-solid mixture to obtain a polymer containing maleic anhydride functional groups; the liquid-solid separator is in communication with the polymerization apparatus to return separated liquid.
In the device provided by the invention, the cracking equipment can be a CB L-R type cracking furnace, and a plurality of cracking equipments can be provided.
In the device provided by the invention, the polymerization equipment can be a pressure-resistant reaction kettle or a tubular reactor with a stirring sleeve, and is used for carrying out copolymerization reaction on a light hydrocarbon raw material and maleic anhydride in the presence of an initiator and an organic solvent to form a copolymer of terminal olefin and maleic anhydride, and the copolymer can be used as a raw material of a functional material.
In the device provided by the invention, the gas-liquid separator can be a flash separator. For separating the product of the polymerization reaction to obtain a gas phase product and a liquid-solid mixture.
In the apparatus provided by the present invention, the gas phase separation device may adopt a device for separating cracked gas in the existing steam cracking process, for example, may adopt a device for front depropanization separation technology, wherein the device may include a compressor, etc., and reference may be made to the existing device for separating cracked gas, which is not described herein again.
The device provided by the invention is characterized in that the liquid-solid separator is a centrifugal separator which can be in any horizontal or vertical form and is used for separating the liquid-solid mixture to obtain a solid copolymer product in the liquid-solid mixture.
The present invention will be described in detail below by way of examples.
In the following examples, the cracking furnace was a CB L-R type cracking furnace, and the separation system used a front depropanization separation technique;
the component analysis of the cracked gas is carried out by gas chromatography, using an Agilent 7890A Gas Chromatograph (GC);
c in the gas-phase product4The terminal olefin content was determined by gas chromatography using an agilent 7890A Gas Chromatograph (GC);
the content of the maleic anhydride structural unit in the obtained polymer was determined by elemental analysis;
the average diameter of the obtained polymer particles was measured by scanning electron microscopy;
measuring the gel content of the obtained crosslinked copolymer by an acetone extraction method in a Soxhlet extractor;
the reaction conversion of the copolymerization reaction was determined by weighing the polymer after the reaction by calculating from the following formula:
reaction conversion (%) of copolymerization reaction [ (% of C in pyrolysis gas)4Weight-polymerization of terminal olefins C in gas phase product4Weight of terminal olefin)/C in cracked gas4Weight of terminal olefin]×100％。
The ethylene and propylene yields were calculated by the following formula:
ethylene yield (%) — × 100% (weight of ethylene in cracked gas ÷ total weight of cracked gas);
the propylene yield (%) was × 100% (weight of propylene in the cracked gas ÷ total weight of the cracked gas).
Comparative example 1
This comparative example illustrates ethane cracking and the production of ethylene and propylene using conventional separation methods.
(1) Cracking reaction, namely performing cracking reaction in 11 CB L-R cracking furnaces, wherein 10 ethane furnaces and one standby furnace are used, the light hydrocarbon raw material is ethane, the outlet temperature of a furnace tube at the radiation section of the cracking furnace is 865 ℃, the weight ratio of water vapor to ethane is 0.3, the outlet pressure of the radiation section of the cracking furnace is 0.17MPa, and the ethane feeding amount of each ethane furnace is 28 tons/hour to obtain cracked gas;
the pyrolysis gas is cooled to 360 ℃ in a quenching boiler and then enters a water washing tower, and the composition of the pyrolysis gas entering the water washing tower is detailed in table 1. The cracked gas discharged from the top of the water scrubber at a temperature of 38 ℃ was further cooled in the water scrubber.
(2) And (3) separation of pyrolysis gas: and (3) introducing the cracked gas into a separation system adopting a front-end depropanization separation technology, and sending the cracked gas into a compressor and the like for separation and purification to obtain ethylene, propylene, ethane and propane.
The ethylene yield was 52.84% and the propylene yield was 1.01%. The ethane and propane (ethane content 99.57 wt%, propane content 0.43 wt%) were returned to the cracking furnace.
The gas flow into the compressor was about 270.4 tons/h.
Example 1
This example illustrates the production of ethylene and propylene from a light hydrocarbon feedstock in accordance with the present invention.
(1) Cracking reaction, namely, performing cracking reaction in 11 CB L-R cracking furnaces, wherein 10 ethane furnaces and one standby furnace are used, and the light hydrocarbon raw material is ethane.
The outlet temperature of a radiant section furnace tube of the cracking furnace is 865 ℃, the weight ratio of water vapor to ethane is 0.3, the outlet pressure of the radiant section of the cracking furnace is 0.17MPa, and the ethane feeding amount of each ethane furnace is 28 tons/hour to obtain cracked gas;
the pyrolysis gas is cooled to 360 ℃ in a quenching boiler and then enters a water washing tower, and the composition of the pyrolysis gas entering the water washing tower is detailed in table 1. The cracked gas discharged from the top of the water scrubber at a temperature of 38 ℃ was further cooled in the water scrubber.
(2) A step of copolymerization, in which pyrolysis gas obtained from the top of a water washing tower is introduced into 1000ml of isoamyl acetate organic reaction liquid containing 0.1 kg/L of maleic anhydride and 0.01 kg/L of azobisisobutyronitrile, the weight ratio of the pyrolysis gas to the maleic anhydride is 1: 4, and the copolymerization reaction is carried out for 12 hours under the copolymerization reaction pressure of 0.13MPa and the temperature of 60 ℃;
(3) separation: introducing the copolymerization reaction product into a flash separator for gas-liquid separation at 25 ℃ and 0MPa to obtain a gas-phase product and a liquid-solid mixture;
the resulting liquid-solid mixture was further subjected to liquid-solid separation in a centrifugal separator (model TG18G, Ware scientific instruments, Beijing) at 4000rpm for 20 minutes to obtain 3.15g of solid copolymer particles.
The gel content in the solid copolymer particles was determined to be 90% by weight, the maleic anhydride structure content was determined to be about 50 mol%, and the average diameter of the particles was 20 μm.
The conversion of the polymerization reaction was 100%.
The gas product was analyzed by gas chromatography and the composition is given in table 2.
And cooling the gas-phase product to 40 ℃, then feeding the gas-phase product into a separation system of a front depropanization separation technology, and feeding the gas-phase product into a compressor and the like for separation and purification to obtain ethylene, propylene, ethane and propane.
The ethylene yield was 55.51% and the propylene yield was 1.06%. Ethane and propane (ethane content 99.57 wt%, propane content 0.43 wt%) were returned to the cracking furnace.
The gas flow into the compressor was about 266.7 tons/h.
Compared with the comparative example 1, the gas flow entering the compressor is relatively reduced by 1.38 percent, and the energy consumption of the cracking device is reduced under the condition of ensuring that the yield of the ethylene and the propylene is basically unchanged.
Comparative example 2
This comparative example illustrates the cracking of ethane and propane and the production of ethylene and propylene using conventional separation methods.
(1) Cracking reaction, namely, performing cracking reaction in 11 CB L-R cracking furnaces, wherein 6 ethane furnaces, 4 propane furnaces and a standby furnace are used, and light hydrocarbon raw materials are ethane and propane.
The outlet temperature of the radiant section furnace tube of the ethane cracking furnace is 865 ℃, and the weight ratio of the water vapor to the ethane is 0.3; the outlet temperature of a radiant section furnace tube of the propane cracking furnace is 855 ℃, and the weight ratio of the water vapor to the propane is 0.4; the outlet pressure of the radiation section of the cracking furnace is 0.17MPa, and the feeding amount of each single ethane and propane cracking furnace is 28 tons/hour, so as to obtain cracking gas;
the pyrolysis gas is cooled to 360 ℃ in a quenching boiler and then enters a water washing tower, and the composition of the pyrolysis gas entering the water washing tower is detailed in table 1. Further cooling the cracked gas discharged from the top of the water scrubber at a temperature of 40 ℃ in the water scrubber.
(2) And (3) separation of pyrolysis gas: cooling the cracked gas to 40 ℃, then entering a separation system adopting a front-end depropanization separation technology, and sending the cracked gas into a compressor and the like for separation and purification to obtain ethylene, propylene, ethane and propane.
The ethylene yield was 46.82% and the propylene yield was 4.71%. The ethane and propane (ethane content 99.57 wt%, propane content 0.43 wt%) were returned to the cracking furnace.
The gas flow into the compressor was about 250.9 tons/h.
Example 2
This example illustrates the production of ethylene and propylene from a light hydrocarbon feedstock in accordance with the present invention.
(1) Cracking reaction, namely, performing cracking reaction in 11 CB L-R cracking furnaces, wherein 6 ethane furnaces, 4 propane furnaces and a standby furnace are used, and light hydrocarbon raw materials, namely ethane and propane, are respectively fed for cracking reaction.
The outlet temperature of the radiant section furnace tube of the ethane cracking furnace is 865 ℃, and the weight ratio of the water vapor to the ethane is 0.3; the outlet temperature of a radiant section furnace tube of the propane cracking furnace is 855 ℃, and the weight ratio of the water vapor to the propane is 0.4; the outlet pressure of the radiation section of the cracking furnace is 0.17MPa, and the feeding amount of each single ethane and propane cracking furnace is 28 tons/hour, so as to obtain cracking gas;
the pyrolysis gas is cooled to 360 ℃ in a quenching boiler and then enters a water washing tower, and the composition of the pyrolysis gas entering the water washing tower is detailed in table 1. Further cooling the cracked gas discharged from the top of the water scrubber at a temperature of 40 ℃ in the water scrubber.
(2) A copolymerization reaction, namely introducing pyrolysis gas obtained from the top of a water washing tower into an organic reaction solution containing 0.1 kg/L of maleic anhydride, 0.015 kg/L of dibenzoyl peroxide and 1000ml of n-hexane, wherein the weight ratio of the pyrolysis gas to the maleic anhydride is 1: 2, and the copolymerization reaction is carried out for 8 hours under the copolymerization reaction pressure of 0.12MPa and the temperature of 75 ℃;
(3) separation: introducing the copolymerization reaction product into a flash separator for gas-liquid separation at 30 ℃ and 0MPa, and continuously performing liquid-solid separation on the obtained liquid-solid mixture in a centrifugal separator at 4000rpm for 20min by centrifugal separation to obtain 6.18g of solid copolymer particles.
The gel content in the solid copolymer particles was determined to be 92% by weight, the maleic anhydride structure content was determined to be about 48 mol%, and the average diameter of the particles was 250. mu.m.
The conversion of the polymerization reaction was 100%.
The gas product was analyzed by gas chromatography and the composition is given in table 2.
And cooling the gas-phase product to 40 ℃, then feeding the gas-phase product into a separation system adopting a front-end depropanization separation technology, and feeding the gas-phase product into a compressor and the like for separation and purification to obtain ethylene, propylene, ethane and propane.
The ethylene yield was 51.03% and the propylene yield was 5.13%. The ethane and propane are returned to the cracker.
The gas flow into the compressor was about 243.3 tons/h.
Compared with the comparative example 2, the gas flow entering the compressor is relatively reduced by 3.02 percent, and the energy consumption of the cracking device is reduced under the condition of ensuring that the yield of the ethylene and the propylene is basically unchanged.
Comparative example 3
This comparative example illustrates the cracking of ethane, propane and liquefied gases and the production of ethylene and propylene using conventional separation methods.
(1) Cracking reaction, namely, performing cracking reaction in 11 CB L-R cracking furnaces, wherein 6 ethane furnaces, 2 propane furnaces, 2 liquefied petroleum gas furnaces and a standby furnace are used, and light hydrocarbon raw materials comprise ethane, propane and liquefied gas.
The outlet temperature of the radiant section furnace tube of the ethane cracking furnace is 865 ℃, and the weight ratio of the water vapor to the ethane is 0.3; the outlet temperature of a radiant section furnace tube of the propane cracking furnace is 855 ℃, and the weight ratio of the water vapor to the propane is 0.4; the outlet temperature of a radiation section furnace tube of the liquefied petroleum gas cracking furnace is 840 ℃, and the weight ratio of the water vapor to the liquefied petroleum gas is 0.65; the outlet pressure of the radiation section of the cracking furnace is 0.17MPa, and the feeding amount of each of the ethane, propane and liquefied petroleum gas cracking furnaces is 28 tons/hour; obtaining pyrolysis gas;
the cracked gas is cooled to 360 ℃ in a quenching boiler and then enters a water washing tower, and the composition of the cracked gas entering the water washing tower is detailed in table 1. And further cooling the cracked gas with the temperature of 40 ℃ discharged from the top of the water washing tower in the water washing tower, then feeding the cracked gas into a separation system adopting a front depropanization separation technology, and feeding the cracked gas into a compressor and the like for separation and purification to obtain ethylene, propylene, ethane and propane.
The ethylene yield was 44.97% and the propylene yield was 6.32%. The ethane and propane (ethane content 99.57 wt%, propane content 0.43 wt%) were returned to the cracking furnace.
The gas flow into the compressor was about 263.03 tons/h.
Example 3
This example illustrates the production of ethylene and propylene from a light hydrocarbon feedstock in accordance with the present invention.
(1) Cracking reaction, namely, performing cracking reaction in 11 CB L-R cracking furnaces, wherein 6 ethane furnaces, 2 propane furnaces, 2 liquefied petroleum gas furnaces and a standby furnace are used, and light hydrocarbon raw materials, namely ethane, propane and liquefied petroleum gas, are respectively fed for cracking reaction.
The outlet temperature of the radiant section furnace tube of the ethane cracking furnace is 865 ℃, and the weight ratio of the water vapor to the ethane is 0.3; the outlet temperature of a radiant section furnace tube of the propane cracking furnace is 855 ℃, and the weight ratio of the water vapor to the propane is 0.4; the outlet temperature of a radiation section furnace tube of the liquefied petroleum gas cracking furnace is 840 ℃, and the weight ratio of the water vapor to the liquefied petroleum gas is 0.65; the outlet pressure of the radiation section of the cracking furnace is 0.17MPa, and the feeding amount of each of the ethane, propane and liquefied petroleum gas cracking furnaces is 28 tons/hour; obtaining pyrolysis gas;
the cracked gas is cooled to 360 ℃ in a quenching boiler and then enters a water washing tower, and the composition of the cracked gas entering the water washing tower is detailed in table 1. The cracked gas discharged from the top of the water scrubber at a temperature of 55 ℃ was further cooled in the water scrubber.
(2) A step of copolymerization, in which pyrolysis gas obtained from the top of a water washing tower is introduced into an organic reaction solution containing 0.1 kg/L of maleic anhydride, 0.02 kg/L of azobisisobutyronitrile and 1000ml of toluene, the weight ratio of the pyrolysis gas to the maleic anhydride is 1: 1, and the copolymerization is carried out for 5 hours under the copolymerization pressure of 0.125MPa and the temperature of 85 ℃;
(3) separation: introducing the copolymerization reaction product into a flash separator for gas-liquid separation at 27 ℃ and 0MPa, and continuously performing liquid-solid separation on the obtained liquid-solid mixture in a centrifugal separator at 4000rpm for 20min by centrifugal separation to obtain 6.48g of solid copolymer particles.
The gel content in the solid copolymer particles was determined to be 88% by weight, the maleic anhydride structure content was determined to be 52 mol%, and the average diameter of the particles was determined to be 200. mu.m.
The conversion of the polymerization reaction was 100%.
The gas product was analyzed by gas chromatography and the composition is given in table 2.
And cooling the gas-phase product to 40 ℃, then feeding the gas-phase product into a separation system adopting a front-end depropanization separation technology, and feeding the gas-phase product into a compressor and the like for separation and purification to obtain ethylene, propylene, ethane and propane.
The ethylene yield was 49.22%, and the propylene yield was 6.92%. The ethane and propane are returned to the cracker.
The gas flow into the compressor was about 247.96 tons/h.
Compared with the comparative example 1, the gas flow entering the compressor is relatively reduced by 5.73 percent, and the energy consumption of the cracking device is reduced under the condition of ensuring that the yield of the ethylene and the propylene is basically unchanged.
TABLE 1
TABLE 2
It can be seen from the above examples that the method of the present invention can realize the production of ethylene and propylene from light hydrocarbon raw materials, and can obtain a crosslinked copolymer containing a maleic anhydride structure without adding a coupling agent to the copolymerization reaction, has a crosslinking degree of 80% or more (gel content of 80% by weight or more), and can be used as a raw material for functional materials. Meanwhile, the method can also reduce the energy consumption of the subsequent separation process of the cracking device.
Claims (11)
1. A method for producing ethylene and propylene from light hydrocarbon raw materials comprises the following steps:
(1) carrying out cracking reaction on a light hydrocarbon raw material under a steam cracking condition to obtain cracked gas;
(2) in the presence of an initiator and an organic solvent, the cracking gas is mixed with maleicAcid anhydride phase, C in the cracking gas4Partially or totally copolymerizing the terminal olefin with maleic anhydride;
(3) carrying out gas-liquid separation on the product obtained in the step (2) to obtain a gas-phase product and a liquid-solid mixture; c in the gas-phase product based on the total weight of the gas-phase product4The content of terminal olefin is 1 wt% or less;
(4) carrying out gas phase separation on the gas phase product obtained in the step (3) to obtain ethylene, propylene, ethane and propane, and adding the separated ethane and propane serving as circulating materials into the light hydrocarbon raw material obtained in the step (1);
(5) separating the liquid-solid mixture obtained in the step (3) to obtain a solid product and a liquid, wherein the solid product is a polymer containing a maleic anhydride functional group; the liquid is returned to the organic solvent in the step (2);
wherein the pyrolysis gas contains 0.1-10 wt% of C4A terminal olefin; the light hydrocarbon raw material is one or more of ethane, propane and liquefied petroleum gas; in the cracking reaction, the cracking reaction temperature is 800-880 ℃, and the weight ratio of the light hydrocarbon raw material to the water vapor is 1: (0.3-0.65);
in the step (2), the weight ratio of the pyrolysis gas to the maleic anhydride is 0.3: 1 or more; the copolymerization temperature is 50-90 ℃, the copolymerization pressure is 0-0.25 MPa, and the copolymerization time is 0.5-12 h; the amount of the initiator is 0.01-30 mol% of maleic anhydride; the initiator is an azo compound or an organic peroxide; the amount of maleic anhydride used is 30% by weight or less of the organic solvent.
2. The method of claim 1, wherein the initiator is selected from at least one of dibenzoyl peroxide, dicumyl peroxide, di-t-butyl peroxide, lauroyl peroxide, t-butyl peroxybenzoate, diisopropyl peroxydicarbonate, dicyclohexyl peroxydicarbonate, azobisisobutyronitrile, and azobisisoheptonitrile.
3. The method according to claim 1, wherein, in the step (2), the maleic anhydride is used in an amount of 5 to 25 wt% based on the organic solvent.
4. The method according to claim 3, wherein, in the step (2), the maleic anhydride is used in an amount of 10 to 20 wt% based on the organic solvent.
5. The method according to claim 1, wherein the weight ratio of the pyrolysis gas to the maleic anhydride is (0.3-3): 1.
6. the method according to claim 5, wherein the weight ratio of the pyrolysis gas to the maleic anhydride is (0.8-3): 1.
7. the method as claimed in claim 1, wherein, in the step (2), the organic solvent is selected from alkanes, aromatic hydrocarbons and compounds of formula R1-COO-R2At least one of organic acid alkyl esters of (1), wherein R1And R2Is C1～C5Alkyl group of (1).
8. The process of any one of claims 1-7, wherein the copolymerization is a free radical polymerization.
9. The method of claim 8, wherein the copolymerization reaction is carried out by a method comprising: and mixing the organic solvent, maleic anhydride and the initiator to form organic reaction liquid, and then adding the pyrolysis gas into the organic reaction liquid to carry out copolymerization reaction.
10. The method of any one of claims 1-7, wherein the polymer is C in the pyrolysis gas4A crosslinked copolymer of a terminal olefin and maleic anhydride; the content of the maleic anhydride structural unit in the polymer is 48-52 mol%, and the gel content of the polymer is 85-92 wt%.
11. An apparatus for producing ethylene and propylene from a light hydrocarbon feedstock according to any one of claims 1 to 10, comprising: cracking equipment, polymerization equipment, a gas-liquid separator, gas-phase separation equipment and a liquid-solid separator; wherein the content of the first and second substances,
the cracking equipment is used for introducing light hydrocarbon raw materials to carry out cracking reaction;
the polymerization equipment is communicated with the cracking equipment and is used for carrying out copolymerization reaction on the cracked gas discharged by the cracking equipment and maleic anhydride;
the gas-liquid separator is communicated with the polymerization equipment and is used for carrying out gas-liquid separation on a product obtained by the copolymerization reaction and discharged by the polymerization equipment to obtain a gas-phase product and a liquid-solid mixture;
the gas phase separation equipment is communicated with the gas-liquid separator and is used for separating the gas phase product to obtain ethylene, propylene, ethane and propane;
said vapor phase separation apparatus being in communication with said cracking apparatus for recycling ethane and propane back to said cracking apparatus;
the liquid-solid separator is communicated with the gas-liquid separator and is used for separating the liquid-solid mixture to obtain a polymer containing maleic anhydride functional groups; the liquid-solid separator is in communication with the polymerization apparatus to return separated liquid.
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| CN101338008A (en) * | 2008-08-19 | 2009-01-07 | 北京化工大学 | Process for preparing cross-linking maleic anhydride-styrene copolymer |
| CN102690393A (en) * | 2012-05-04 | 2012-09-26 | 北京化工大学 | Copolymer containing functional group and prepared by C5 mixture and maleic anhydride, and preparation of copolymer |
| CN102746873A (en) * | 2011-04-20 | 2012-10-24 | 中国石油化工股份有限公司 | Method for preparing ethylene and propylene through catalytic cracking of light hydrocarbons |
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| CN101205162A (en) * | 2006-12-21 | 2008-06-25 | 中国石油化工股份有限公司 | Combined technique for preparing olefins by using refinery C4 |
| CN101338008A (en) * | 2008-08-19 | 2009-01-07 | 北京化工大学 | Process for preparing cross-linking maleic anhydride-styrene copolymer |
| CN102746873A (en) * | 2011-04-20 | 2012-10-24 | 中国石油化工股份有限公司 | Method for preparing ethylene and propylene through catalytic cracking of light hydrocarbons |
| CN102690393A (en) * | 2012-05-04 | 2012-09-26 | 北京化工大学 | Copolymer containing functional group and prepared by C5 mixture and maleic anhydride, and preparation of copolymer |
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