CN116020175A - Method for treating two or more raw materials by liquid phase simulated moving bed reactor - Google Patents
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Abstract
The invention provides a method for treating two or more raw materials by a liquid-phase simulated moving bed reactor, which comprises the following steps: injecting the supplementary raw material into the region between the injection point of the initial raw material and the withdrawal point of the raffinate in each step of the continuous repeated injection cycle, and the injection point of the supplementary raw material and the initial raw material F 1 The distance between the injection points of the supplementary material is smaller than the distance between the injection point of the supplementary material and the extraction point of the raffinate, the content of the target product in the supplementary material is low, and the target product in the supplementary material does not reach thermodynamic equilibrium. The initial raw materials are mainly used for separating target products; the supplementary material injected into the simulated moving bed reactor is mainly used for strengthening the reaction process of the adsorption zone, producing and separating target products. By introducing the supplementary material which does not reach thermodynamic equilibrium at the position of the adsorption zone close to the initial material injection point, the reaction process in the adsorption zone is strengthened, the yield is further improved, the yield of the target product is increased, the separation purity of the target product is ensured, and the downstream purification is simplified.
Description
Technical Field
The invention relates to the technical field of adsorption separation, in particular to a method for treating two or more raw materials by a liquid-phase simulated moving bed reactor.
Background
A liquid phase simulated moving bed reactor is a device for liquid separation operation by utilizing the adsorption principle. The material inlet and outlet positions of the liquid-phase simulated moving bed reactor are periodically changed in a countercurrent continuous operation mode, so that the position of a solid medium is unchanged, and the materials are separated by countercurrent contact of liquid phases and solid phases which continuously move relatively.
The separation of isomers with small boiling point differences or components with different structural features in simulated moving bed reactors is currently a more efficient process in the art. However, in the prior art, the yield of the obtained target product is smaller during adsorption separation.
Disclosure of Invention
Aiming at the technical problem of smaller yield of target products in the prior art, the invention provides a method for treating two or more raw materials by using a liquid phase simulated moving bed reactor.
In order to achieve the above object, the method for processing two or more raw materials by using the liquid phase simulated moving bed reactor provided by the invention comprises the following steps: passing the raw material containing the isomer through the liquid phase simulated moving bed reactor for adsorption separation and conversion,to extract the target product A 1 The raw materials comprise initial raw material F 1 And supplementing raw materials;
wherein the material entering the liquid phase simulated moving bed reactor at least comprises initial raw material F 1 The material extracted from the liquid phase simulated moving bed reactor at least comprises extract liquid and raffinate, and the extract liquid contains target product A 1 ；
Wherein the initial raw material F 1 The region between the injection point of the raffinate and the extraction point of the desorbent is an adsorption zone, the region between the extraction point of the raffinate and the injection point of the desorbent is an isolation zone, the region between the injection point of the desorbent and the extraction point of the extract is a desorption zone, and the extraction point of the extract is a desorption zone 1 The region between the injection points of (a) is a purification region;
wherein the initial raw material F 1 Comprising component A 1 、……、A n N is an integer greater than 2;
the injection point of the supplementary raw material is positioned in the adsorption zone and is equal to the initial raw material F 1 The distance between the injection points of the supplementary material and the extraction point of the raffinate is smaller than the distance between the injection points of the supplementary material, the target product A in the supplementary material 1 Is less than the initial raw material F 1 Target product A of (a) 1 And the content of the target product A in the supplementary raw material 1 Thermodynamic equilibrium is not reached.
Further, the injection point of the supplementary raw material is equal to the initial raw material F 1 The number of the adsorption beds at intervals between the injection points of (1) to (q/2-0.5), q being the initial raw material F 1 Is separated from the raffinate withdrawal point.
Further, the injection point of the supplementary raw material is equal to the initial raw material F 1 The number of adsorbent beds spaced between injection points is between 1 and 14.
Further, the injection point of the supplementary raw material is equal to the initial raw material F 1 The number of adsorbent beds spaced between injection points is between 2 and 7.
Further, the initial raw material F 1 Target product A of (a) 1 Reach thermodynamic equilibrium and target product A 1 Has a higher adsorption capacity than component A 2 To A n Adsorption capacity of any one of the components.
Further, the injected supplemental feedstock includes one or more strands.
Further, the injected supplemental feedstock comprises F 2 、……、F m Multistrand, m is an integer greater than 2, and m is less than or equal to n.
Further, F 2 、……、F m The injection points of the multiple supplemental feeds may be the same or different.
Further, F 2 、……、F m Multiple strands of supplementary raw materials with different injection points (m-1) Is located at the injection point of the supplementary raw material F (m-2) Is added with supplementary material F m Is filled with raw material F (m-2) Is added with the raw material F (m-1) Is added with supplementary material F m Is continuous with the injection point of the (c).
Further, initial raw material F 1 Is positioned at the extraction point of the extracted liquid and the supplementary raw material F 2 Between the injection points of (a) and (b) the extraction point of the extraction liquid and the initial raw material F 1 Is added to the feed point and the supplementary raw material F 2 Is continuous with the injection point of the (c).
Through the technical scheme provided by the invention, the invention has at least the following technical effects:
the method for treating two or more raw materials by a liquid-phase simulated moving bed reactor of the present invention comprises injecting a supplementary raw material into an adsorption zone between an injection point of an initial raw material and a withdrawal point of a raffinate in each step of a continuous repeated injection cycle, and injecting the supplementary raw material into the adsorption zone between the injection point of the initial raw material and the withdrawal point of the initial raw material F 1 The distance between the injection points of the supplementary material is smaller than the distance between the injection point of the supplementary material and the extraction point of the raffinate, the content of the target product in the supplementary material is lower, and the target product in the supplementary material does not reach thermodynamic equilibrium. Initial raw materialsThe method is mainly used for separating target products; the supplementary material injected into the simulated moving bed reactor is mainly used for strengthening the reaction process of the adsorption zone, producing and separating target products. By introducing the supplementary material which does not reach thermodynamic equilibrium at the position of the adsorption zone close to the initial material injection point, the reaction process in the adsorption zone is strengthened, the yield is further improved, the yield of the target product is increased, the separation purity of the target product is ensured, and the downstream purification is simplified.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings are included to provide a further understanding of embodiments 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, without limitation, the embodiments of the invention. In the drawings:
FIG. 1 is a schematic diagram of the injection points of additional feedstock in a method for treating two or more feedstocks in a liquid phase simulated moving bed reactor according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of injection points of different supplemental feedstock in a method for treating two or more feedstocks in a liquid phase simulated moving bed reactor according to an embodiment of the present invention;
FIG. 3 is a schematic diagram showing concentration distribution of each adsorption bed layer of the liquid-phase simulated moving bed reactor in the method for treating two or more raw materials by the liquid-phase simulated moving bed reactor according to the embodiment of the invention.
Detailed Description
The following describes the detailed implementation of the embodiments of the present invention with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
In the present invention, unless otherwise indicated, terms of orientation such as "upper, lower, top, bottom" are used generally with respect to the orientation shown in the drawings or with respect to the positional relationship of the various components with respect to one another in the vertical, vertical or gravitational directions.
The invention will be described in detail below with reference to the drawings in connection with embodiments.
Referring to fig. 1, an embodiment of the present invention provides a method for processing two or more raw materials in a liquid-phase simulated moving bed reactor, the liquid-phase simulated moving bed reactor includes p adsorption beds containing solid media, fluid collection distributors are disposed between two adjacent adsorption beds, and material inlet and outlet lines of the adsorption beds are disposed on each fluid collection distributor, the method includes:
subjecting a raw material containing isomers to adsorption separation and conversion by the liquid phase simulated moving bed reactor to extract a target product A 1 The raw materials comprise initial raw material F 1 And supplementing raw materials;
wherein the material entering the liquid phase simulated moving bed reactor at least comprises initial raw material F 1 Supplementing raw materials and desorbing agents, wherein the materials extracted from the liquid-phase simulated moving bed reactor at least comprise extract liquid and raffinate liquid; the extracted liquid contains a target product A 1 ；
Wherein the initial raw material F 1 The region between the injection point of the raffinate and the extraction point of the desorbent is an adsorption zone, the region between the extraction point of the raffinate and the injection point of the desorbent is an isolation zone, the region between the injection point of the desorbent and the extraction point of the extract is a desorption zone, and the extraction point of the extract is a desorption zone 1 The region between the injection points of (a) is a purification region;
wherein the initial raw material F 1 Comprising component A 1 、……、A n N is an integer greater than 2;
the injection point of the supplementary raw material is positioned in the adsorption zone and is equal to the initial raw material F 1 The distance between the injection points of the supplementary material and the extraction point of the raffinate is smaller than the distance between the injection points of the supplementary material, the target product A in the supplementary material 1 Is less than the initial contentRaw material F 1 Target product A of (a) 1 And the content of the target product A in the supplementary raw material 1 Thermodynamic equilibrium is not reached.
Specifically, in the embodiment of the invention, the liquid-phase simulated moving bed reactor comprises p adsorption beds containing solid media, the adsorption beds are interconnected in an annular conformation, a fluid collecting distributor is arranged between two adjacent adsorption beds, a material inlet and outlet pipeline of the adsorption bed is arranged on each fluid collecting distributor, the material from the previous adsorption bed can be uniformly mixed with a material flow from the previous adsorption bed, and part of the material flow from the previous adsorption bed is led out. When the liquid phase simulated moving bed reactor is used, the continuous countercurrent movement of the liquid phase and the stationary phase is simulated by periodically and synchronously switching the positions of the material inlet and the material outlet, so that the strong adsorption component is adsorbed on the stationary phase medium, and the weak adsorption component is left in the liquid phase to move in the opposite direction, thereby achieving the purpose of separation. Switching from one adsorbent bed to another adsorbent bed, switching injection and withdrawal points may use valves (e.g., rotary valves or two-position or multi-position valve networks) that work in conjunction with inlet and outlet lines of multiple adsorbent beds.
In the present application, the liquid-phase simulated moving bed reactor comprises at least three feeds, and the adsorption raw material F 1 Supplementing the raw materials and desorbing agents; at least two discharges, a raffinate and a raffinate. Initial raw material F 1 The region between the injection point of the raffinate and the extraction point of the raffinate is an adsorption region, the region between the extraction point of the raffinate and the injection point of the desorbent is an isolation region, the region between the injection point of the desorbent and the extraction point of the extract is a desorption region, the extraction point of the extract and the initial raw material F 1 The region between the injection points of (a) is the purification region.
In a liquid phase simulated moving bed reactor, the purification zone and adsorption zone are used to allow the fast and slow components to move more apart, while the separation zone and desorption zone are used to prevent the slow components from lagging too far and the fast components from advancing too far, respectively. Each zone is allowed to have a different flow rate and the amount of injected material is fixed.
Initial raw material F 1 Comprising component A 1 、……、A n N is an integer greater than 2, initial raw material F 1 The method is mainly used for separating target products. The extracted liquid comprises a slow elution fraction, the raffinate comprises a fast elution fraction, and the target product A 1 Can be extracted from the effluent of the liquid phase simulated moving bed reactor.
The injection point of the supplementary raw material is located at the initial raw material F 1 An adsorption zone between the injection point of the feed and the withdrawal point of the raffinate, and make-up the injection point of the feed and the initial feed F 1 The distance between the injection point of the make-up feed and the withdrawal point of the raffinate is smaller than the distance between the injection point of the make-up feed and the withdrawal point of the raffinate. The supplementary material is injected into the region and can be fully contacted with the solid medium in the adsorption bed layer to react to produce the target product A 1 The product purity of the liquid phase simulated moving bed reactor is not reduced. Supplementing the target product A in the raw materials 1 Is small or approximately zero, and supplements the target product A in the raw materials 1 Thermodynamic equilibrium is not reached. Under the influence of thermodynamic equilibrium, the target product A is removed from the supplementary raw materials 1 Other substances are converted into the target product A 1 The supplementary material is mainly used for strengthening the reaction process of the adsorption zone to produce and separate target products. The solid medium can be used for separating reactants from target products and also can be used as other substances to react respectively to generate the target product A 1 Is a catalyst of (a).
Further, the injection point of the supplementary raw material is equal to the initial raw material F 1 The number of the adsorption beds at intervals between the injection points of (1) to (q/2-0.5), q being the initial raw material F 1 Is separated from the raffinate withdrawal point.
Specifically, in the embodiment of the present invention, the injection point of the supplementary raw material is equal to the initial raw material F 1 At least one adsorption bed is arranged between the injection points of the supplementary raw material and the initial raw material F 1 The spacing between the injection points of (a) is less than half the length of the adsorption zone.
Further, the injection point of the supplementary raw material is equal to the initial raw material F 1 Is to be injected into (a)The number of adsorbent beds spaced between the inlet points is between 1 and 14.
Further, the injection point of the supplementary raw material is equal to the initial raw material F 1 The number of adsorbent beds spaced between injection points is between 2 and 7.
Further, the initial raw material F 1 Target product A of (a) 1 Reach thermodynamic equilibrium and target product A 1 Has a higher adsorption capacity than component A 2 To A n Adsorption capacity of any one of the components.
Specifically, in embodiments of the present invention, initial raw material F 1 Target product A of (a) 1 To thermodynamic equilibrium, initial charge F 1 Each component has obvious adsorption difference, and the target product A 1 Has a higher adsorption capacity than component A 2 To A n Adsorption capacity of any one of the components.
Further, the injected supplemental feedstock includes one or more strands.
Further, the injected supplemental feedstock comprises F 2 、……、F m Multistrand, m is an integer greater than 2, and m is less than or equal to n.
Further, F 2 、……、F m The injection points of the multiple supplemental feeds may be the same or different.
Specifically, referring to fig. 2, in the embodiment of the present invention, the injection points of the multiple supplementary raw materials may be the same or different.
Further, the arrangement positions of the material injection points and the material extraction points of the liquid-phase simulated moving bed reactor are as follows:
F 2 、……、F m multiple strands of supplementary raw materials with different injection points (m-1) Is located at the injection point of the supplementary raw material F (m-2) Is added with supplementary material F m Is filled with raw material F (m-2) Is added with the raw material F (m-1) Is added with supplementary material F m The injection points of the three are continuous;
initial raw material F 1 Is positioned at the extraction point of the extracted liquid and the supplementary raw material F 2 Between the injection points of (a) and (b) the extraction point of the extraction liquid and the initial raw material F 1 Is added to the feed point and the supplementary raw material F 2 The injection points of the three are continuous;
supplementary raw material F m Is located at the injection point of the supplementary raw material F (m-1) Between the injection point of the extraction liquid and the extraction point of the extraction liquid, the raw material F is supplemented m Is added with the raw material F (m-1) The injection point of the extraction liquid and the extraction point of the extraction liquid are continuous;
the injection point of the desorbent is positioned between the extraction point of the raffinate and the extraction point of the extract, and the extraction point of the raffinate, the injection point of the desorbent and the extraction point of the extract are continuous;
the extraction point of the extraction liquid is positioned at the injection point of the desorbent and the raw material F 1 Between the injection points of the raw material F 1 The injection point of the extraction liquid, the extraction point of the desorbent are continuous;
supplementary raw material F m Is located at the injection point of the supplementary raw material F (m-1) Between the injection point of the extraction liquid and the extraction point of the extraction liquid, the raw material F is supplemented m Is added with the raw material F (m-1) The injection point of the extraction liquid is continuous;
the point of withdrawal of the raffinate is located at the make-up feed F m Between the injection point of the desorbent and the injection point of the supplemental feedstock F m The injection point of the raffinate, the extraction point of the raffinate, and the injection point of the desorbent 3 are continuous.
Further, n is between 2 and 6, and further preferably, n is 3 or 4.
Further, p is between 12 and 36, and more preferably, p is between 16 and 36.
The operating conditions of the liquid phase simulated moving bed reactor will depend on the solid medium in the adsorbent bed. The predetermined temperature of the reaction in the liquid phase simulated moving bed reactor is typically between 170 ℃ and 300 ℃. The pressure of the reaction in the liquid phase simulated moving bed reactor is typically between 2000KPa and 3000 KPa. Other predetermined temperatures and pressures are possible depending on the reaction.
The method can be applied to liquid phase isomerization reversible reaction, and can increase the yield of the paraxylene in the carbon octaaromatic hydrocarbon mixture.
The method of the invention can also be applied to other fields, such as medicine, food and the like, such as increasing the yield of D-psicose in the mixture of D-fructose and D-psicose; and increasing the yield of fructose, fructose in a glucose mixture, and the like.
The process of the present invention can be carried out using many different types of catalysts and separation media (solid media) for the mixing reaction and separation. It is also possible to use a single solid as both catalyst and separation medium. Solid media include, but are not limited to, polymeric resins, molecular sieves, or others.
Example 1
In this example, taking n=3 and m=2 as examples, the material entering the liquid phase simulated moving bed reactor comprises: initial raw material F 1 Comprises A 1 、A 2 And A 3 Component A 1 Reaching thermodynamic equilibrium; supplementary raw material F 2 Not containing A 1 Comprises only A 2 And A 3 Component A 1 Thermodynamic equilibrium is not reached; desorbent D. The material withdrawn from the liquid phase simulated moving bed reactor comprises a withdrawn liquid E and a raffinate R. The contents used below are all mass percentages.
This example allows the purification of para-xylene from a C8 aromatic hydrocarbon feedstock blend. Initial raw material F 1 The contents of each group are as follows: 27.4% of para-xylene (PX), 57.8% of meta-xylene (MX) and 14.8% of ortho-xylene (OX). Supplementary raw material F 2 The contents of each group are as follows: 79.6% of meta-xylene (MX) and 20.4% of ortho-xylene (OX). Content of adsorbent in solid medium: 95% of zeolite (BaX) and 5% of kaolin. The catalyst in the solid medium is beta molecular sieve. The adsorbent accounts for 87.6% of the total amount of the adsorbent and the catalyst. Desorbent D is toluene. One step time of periodically and synchronously switching the positions of the material inlet and the material outlet is 39.2 seconds, and the temperature of the liquid phase simulated moving bed reactor is 256 ℃ and the pressure is 2100KPa. Initial raw material F 1 The feeding temperature is 150 ℃, and the raw material F is supplemented 2 The feed temperature was 150 ℃.
The liquid phase simulated moving bed reactor has 24 adsorption beds with a length of 1.14 m and a diameter of 4.12 m. Each adsorbent bed was assigned as follows:
desorption zone: comprises 4 adsorption beds;
purification zone: comprises 3 adsorption beds;
adsorption zone: comprises 15 adsorption beds, and supplementary material F is injected between the 4 th adsorption bed layer and the 5 th adsorption bed layer of the adsorption zone 2 ；
Isolation region: comprising 2 adsorbent beds.
The flow rates of the materials are as follows: raw material F 1 :56926.46kg/h; supplementary raw material F 2 :10000.00kg/h; desorbent D:294556.20kg/h; and (3) extracting a liquid E:279839.20kg/h; raffinate R:81643.52kg/h.
And finally purifying to obtain the paraxylene with the purity of 70%, the yield of the paraxylene of 84.1kg/h and the yield of the paraxylene of 119.91%, wherein the concentration distribution of each adsorption bed layer in the liquid-phase simulated moving bed reactor is shown in figure 3.
By the method provided by the invention, the supplementary raw materials which do not reach thermodynamic equilibrium are introduced at the position of the adsorption zone close to the initial raw material injection point, the reaction process in the adsorption zone is strengthened, the yield is further improved, the yield of the target product is increased, the separation purity of the target product is ensured, and the downstream purification is simplified.
The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (10)
1. A method for processing two or more raw materials by a liquid-phase simulated moving bed reactor, the liquid-phase simulated moving bed reactor comprises p adsorption beds containing solid media, a fluid collection distributor is arranged between two adjacent adsorption beds, and a material inlet and outlet pipeline of the adsorption beds is arranged on each fluid collection distributor, and the method is characterized by comprising the following steps:
subjecting a raw material containing isomers to adsorption separation and conversion by the liquid phase simulated moving bed reactor to extract a target product A 1 The raw materials comprise initial raw material F 1 And supplementing raw materials;
wherein the material entering the liquid phase simulated moving bed reactor at least comprises initial raw material F 1 The material extracted from the liquid phase simulated moving bed reactor at least comprises extract liquid and raffinate, and the extract liquid contains target product A 1 ；
Wherein the initial raw material F 1 The region between the injection point of the raffinate and the extraction point of the desorbent is an adsorption zone, the region between the extraction point of the raffinate and the injection point of the desorbent is an isolation zone, the region between the injection point of the desorbent and the extraction point of the extract is a desorption zone, and the extraction point of the extract is a desorption zone 1 The region between the injection points of (a) is a purification region;
wherein the initial raw material F 1 Comprising component A 1 、……、A n N is an integer greater than 2;
the injection point of the supplementary raw material is positioned in the adsorption zone and is equal to the initial raw material F 1 The distance between the injection points of the supplementary material and the extraction point of the raffinate is smaller than the distance between the injection points of the supplementary material, the target product A in the supplementary material 1 Is less than the initial raw material F 1 Target product A of (a) 1 And the content of the target product A in the supplementary raw material 1 Thermodynamic equilibrium is not reached.
2. The liquid phase simulated moving bed reactor according to claim 1A method for treating two or more raw materials by a reactor, characterized in that the injection point of the supplementary raw material is equal to that of the initial raw material F 1 The number of the adsorption beds at intervals between the injection points of (1) to (q/2-0.5), q being the initial raw material F 1 Is separated from the raffinate withdrawal point.
3. A method for treating two or more feedstocks in a liquid-phase simulated moving bed reactor according to claim 1, wherein the injection point of the supplemental feedstock is the same as the initial feedstock F 1 The number of adsorbent beds spaced between injection points is between 1 and 14.
4. A method for treating two or more feedstocks in a liquid phase simulated moving bed reactor according to claim 3, wherein the injection point of the supplemental feedstock is the same as the initial feedstock F 1 The number of adsorbent beds spaced between injection points is between 2 and 7.
5. A method for treating two or more feedstocks in a liquid-phase simulated moving bed reactor according to claim 1, wherein the initial feedstock F 1 Target product A of (a) 1 Reach thermodynamic equilibrium and target product A 1 Has a higher adsorption capacity than component A 2 To A n Adsorption capacity of any one of the components.
6. A method for treating two or more feeds in a liquid phase simulated moving bed reactor according to claim 5, wherein the injected supplemental feed comprises one or more feeds.
7. A method for treating two or more feedstocks in a liquid phase simulated moving bed reactor according to claim 6, wherein said injected supplemental feedstock comprises F 2 、……、F m Multistrand, m is an integer greater than 2, and m is less than or equal to n.
8. According to claimA method for treating two or more materials in a liquid-phase simulated moving bed reactor according to 7, characterized by comprising F 2 、……、F m The injection points of the multiple supplemental feeds may be the same or different.
9. A method for treating two or more materials in a liquid-phase simulated moving bed reactor according to claim 8, wherein F 2 、……、F m Multiple strands of supplementary raw materials with different injection points (m-1) Is located at the injection point of the supplementary raw material F (m-2) Is added with supplementary material F m Is filled with raw material F (m-2) Is added with the raw material F (m-1) Is added with supplementary material F m Is continuous with the injection point of the (c).
10. A method for treating two or more feeds in a liquid-phase simulated moving bed reactor according to claim 9, wherein the initial feed F 1 Is positioned at the extraction point of the extracted liquid and the supplementary raw material F 2 Between the injection points of (a) and (b) the extraction point of the extraction liquid and the initial raw material F 1 Is added to the feed point and the supplementary raw material F 2 Is continuous with the injection point of the (c).
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