Fluidized bed reactor and method for producing nitrile compounds

Abstract

The application discloses a fluidized bed reaction device and method for producing nitrile compounds, and the fluidized bed reaction device comprises a feeding unit, a fluidized bed reactor and a filtering unit which are sequentially connected; wherein the feeding unit is located at one side of the fluidized bed reactor and is connected with a feeding port of the fluidized bed reactor, and is used for input of reaction raw materials; the feeding unit comprises a solid feeding unit and / or a liquid feeding unit. The reaction device and method of the application are aimed at a reaction process for preparing nitrile compounds by means of ammoniation dehydration of carboxylic acid and carboxylic acid ester or dehydration of amide; by means of internal structure design of the core fluidized bed reactor, high-boiling-point raw materials such as carboxylic acid, carboxylic acid ester and amide are directly introduced into the reactor without heating, so that particle heating, thermal collapse and gasification of the raw materials are orderly carried out, and therefore the catalytic conversion reaction interface is improved, the residence time of the raw materials is increased, and the conversion rate and selectivity are greatly improved.

Description

Technical Field

[0001] This invention relates to the field of heterogeneous catalytic reaction technology, and in particular to a fluidized bed reactor and method for producing nitrile compounds. Background Technology

[0002] Nitriles are important chemical raw materials and synthetic intermediates. They typically possess unique chemical structures and physical properties, and have wide applications in chemical fields such as synthetic materials, resins, pesticides, adhesives, and specialty solvents. Furthermore, they are also intermediates in the chemical synthesis of pharmaceuticals, dyes, vitamins, and plastics.

[0003] Amination dehydration of carboxylic acids (esters) and direct dehydration of amides are important methods for preparing nitrile compounds. Commonly used dehydrating agents include phosphorus pentoxide, phosphorus oxychloride, thionyl chloride, or highly toxic chemicals such as phosgene and triphosgene. The use of phosphorus-containing dehydrating agents generates large amounts of phosphorus-containing wastewater, which is difficult to treat environmentally. Phosgene-based chemicals are toxic and hazardous chemicals, and the reaction process is highly exothermic, resulting in poor process safety and the generation of large amounts of acidic wastewater.

[0004] CN112645840A achieves continuous production of salicylnitrile by passing salicylamide dissolved in an organic solvent and ammonia together into a fixed-bed reactor packed with a catalyst. CN115160182A synthesizes salicylnitrile by catalytic synthesis of methyl salicylate and ammonia preheated and mixed in a fixed-bed catalyst reactor. CN111848447A synthesizes adiponitrile by mixing adipic acid gasified with ammonia and passing the mixture through a fixed-bed or fluidized-bed catalytic reactor. All of these processes successfully avoid the use of traditional dehydrating agents and achieve continuous production of nitrile compounds. However, high-boiling-point raw materials such as carboxylic acids, carboxylic esters, and amides often need to be dissolved in organic solvents or gasified at high temperatures before being fed into the fixed-bed reactor. Therefore, it is necessary to add many auxiliary equipment for organic solvent recovery or raw material preheating and gasification, resulting in significant energy consumption. Furthermore, dehydration catalysts are prone to carbon buildup and deactivation, often requiring two fixed-bed reactors to alternate between reaction and catalyst regeneration to ensure continuous and stable production, resulting in substantial equipment investment.

[0005] Therefore, developing fluidized bed catalytic reactors with direct solid or liquid phase feed to achieve rapid catalytic dehydration and rapid catalyst regeneration is of great significance for the dehydration to nitrile production process. Summary of the Invention

[0006] In view of the problems existing in the prior art, the present invention provides a fluidized bed reactor and method for preparing nitrile compounds. The apparatus is provided with an air inlet and a feed inlet. The raw material enters the reactor and rapidly exchanges heat with the catalyst in a fluidized state, directly gasifies and catalytically converts it, and quickly forms the target nitrile compound. This fluidized bed apparatus has simple feeding, large processing capacity, high conversion rate and few by-products.

[0007] One object of the present invention is to provide a fluidized bed reactor for preparing nitrile compounds.

[0008] A fluidized bed reactor for producing nitrile compounds includes a feed unit, a fluidized bed reactor, and a filtration unit connected in sequence.

[0009] The feeding unit is located on one side of the fluidized bed reactor and is connected to the feed inlet of the fluidized bed reactor. It is used to input the reaction raw materials, which can be solid or liquid.

[0010] The fluidized bed reactor has a three-section structure: an upper cylindrical structure, a middle inverted conical structure, and a lower cylindrical structure. The diameter of the upper cylindrical structure is larger than that of the lower cylindrical structure, forming an enlarged section. The diameter ratio of the upper and lower sections is 1.1:1 to 4:1. They are connected by the middle inverted conical structure to form a whole. The angle between the cone surface of the middle inverted conical structure and the vertical direction is 15°-45°. The lower cylindrical structure is the main reaction zone. In a relatively small space, by controlling process conditions such as gas distribution, air velocity, and heat exchange, the reactants and catalyst are brought into full contact to achieve the reaction conditions, thus enabling a rapid reaction. The main purposes of the upper cylindrical structure are: firstly, to reduce the gas velocity to achieve gas-solid phase separation; and secondly, to provide sufficient space for auxiliary components such as feeding or exhaust devices. The middle inverted conical structure connects the upper and lower structures and promotes the return of materials or catalysts to the lower reaction zone of the fluidized bed. This is specifically controlled by the cone angle, fluidizing gas velocity, and catalyst particle size.

[0011] The fluidized bed reactor has at least one feed inlet; the lower cylindrical structure, which serves as the main reaction zone, is equipped with single or multiple horizontal distribution plates to carry the catalyst and distribute the gas, while dividing the reaction process into several corresponding reaction zones. The catalysts packed on each distribution plate can be the same or different; the bottom of the fluidized bed reactor is provided with an air inlet for introducing carrier gas or a mixture of carrier gas and NH3. The carrier gas is usually an inert gas, such as nitrogen. The carrier gas and NH3 together serve as fluidizing gas to fluidize the catalyst, with some NH3 participating in the reaction.

[0012] The filtration unit is located on the other side of the fluidized bed reactor and is connected to the outlet of the fluidized bed reactor. It is used to filter out solid materials or catalyst particles entrained in the gas-phase mixture.

[0013] Preferably, the feed inlet of the fluidized bed reactor is located at one or more positions on the top of the upper cylindrical structure, the side wall of the upper cylindrical structure, the upper part of the side wall of the lower cylindrical structure, or the side wall of the reaction zone between the various levels of horizontal distribution plates of the lower cylindrical structure. The feed is selected from different feed inlets according to the properties, phase, and reaction conditions of the reactants.

[0014] Preferably, when the reactant is a solid phase, the feeding unit includes a hopper and a feeder;

[0015] Furthermore, when the reactant is a solid phase, the feeder includes, but is not limited to, a screw feeder or a star feeder, and the feeder is directly connected to the feed inlet of the fluidized bed reactor;

[0016] Preferably, for the fluidized bed reactor containing a single-stage distribution plate, when the reactant is a solid phase, the fluidized bed reactor further includes a vertical baffle. The vertical baffle has a three-section structure: an upper inverted trapezoidal structure, a middle rectangular structure, and a lower flow-guiding structure inclined to one side. The shape of the inverted trapezoidal structure is consistent with the cross-section of the middle inverted cone structure of the fluidized bed reactor, and the middle rectangular structure is consistent with the cross-section of the lower cylindrical structure of the fluidized bed reactor. The vertical baffle is vertically arranged in the middle inverted cone structure and the lower cylindrical structure of the fluidized bed reactor, dividing the space into two parts with unequal volumes: a preheating fluidized zone and a reaction fluidized zone, with a volume ratio of 1:4 to 1:2. The lower flow-guiding structure of the vertical baffle is located above the horizontal distribution plate, and the flow-guiding structure does not contact the horizontal distribution plate, forming a gap.

[0017] Preferably, the portion of the single-stage distribution plate corresponding to the preheating fluidized zone side is not provided with pores, so there is no bottom-up fluidizing air on the preheating fluidized zone side. The portion of the single-stage distribution plate corresponding to the reaction fluidized zone side is provided with pores, so the fluidizing air enters the reaction fluidized zone through the pores.

[0018] Preferably, the sidewall of the preheating fluidized zone is provided with a push air vent, a loosening air vent, and a blowing air vent from top to bottom; wherein the push air vent promotes the downward movement of the material; wherein the loosening air vent loosens the material to prevent it from accumulating at corners; wherein the blowing air vent blows the material in the preheating fluidized zone to the reaction zone through the inclined flow guiding structure at the lower part of the vertical partition.

[0019] Preferably, when the reactant is a liquid phase, the feeder includes a storage tank and a feed pump;

[0020] Furthermore, when the reactant is a liquid phase, a liquid distributor is also provided in the upper cylindrical structure of the fluidized bed reactor. The liquid distributor includes, but is not limited to, a liquid distribution plate and an atomizing nozzle. The feed pump of the feeding unit is connected to the feed inlet of the fluidized bed reactor through a pipeline and transports the reactant to the liquid distributor.

[0021] Preferably, the discharge port is located at the top of the fluidized bed reactor for discharging a gaseous mixture, including the generated gaseous products, carrier gas, and NH3 (NH3 may be absent when the feedstock is amide).

[0022] Preferably, the horizontal distribution plate is, but is not limited to, a sieve plate, a sintering plate, or a bubble cap plate;

[0023] Preferably, the number of horizontal distribution plates is 1 to 10;

[0024] Preferably, catalyst discharge ports are provided near the reactor wall above each horizontal distribution plate in the fluidized bed reactor to facilitate catalyst discharge. The catalyst can be loaded through the manhole or handhole of the fluidized bed reactor, or it can be added through the feed inlet.

[0025] Preferably, when a solid-phase amination agent is used, it can be pre-mixed with the reaction raw materials and added to the fluidized bed reactor through the feeding unit; or an additional feeding unit can be added, and the feed port can be selected according to the specific reaction conditions.

[0026] Preferably, an auxiliary heat exchanger may be provided on the outer wall of the reaction zone of the lower cylindrical structure of the fluidized bed reactor. The auxiliary heat exchanger includes, but is not limited to, a heat tracing cable, a heat exchange coil, a heat exchange jacket, and ceramic heating elements.

[0027] Preferably, the filter of the filtration unit may include, but is not limited to, a screen with a corresponding aperture, a cyclone separator, etc.

[0028] According to another aspect of the present invention, another object of the present invention is to provide a method for producing nitrile compounds, comprising the following steps:

[0029] 1) Weigh out each section of catalyst according to the specified weight, and then fill the catalyst into the corresponding horizontal distribution plate through the manhole, handhole or corresponding feed port of each section of the fluidized bed reactor. Then seal the entire reaction device and check the airtightness.

[0030] 2) Carrier gas is introduced into the reactor through the air inlet of the fluidized bed reactor to replace the system. After the oxygen content in the entire reaction device system is lower than 0.1%, the temperature is prepared to be increased.

[0031] 3) Start the auxiliary heat exchanger, and at the same time, the preheated carrier gas nitrogen is continuously introduced into the fluidized bed reactor to fluidize and heat the catalyst in each section of the reactor. The carrier gas flows out of the fluidized bed reactor through the gas phase outlet and continues to enter the subsequent filtration unit to heat the filtration unit together. Then it flows out of the entire reaction device. The heating process continues until the fluidized bed reactor is heated to the specified temperature.

[0032] When the raw material is amide, proceed directly to step 5);

[0033] 4) After the fluidized bed reactor is normally fluidized and reaches the specified temperature, NH3 is gradually mixed into the carrier gas in proportion and preheated together to the specified temperature before being introduced into the reactor until the reactor is stably fluidized under mixed gas conditions and reaches the reaction temperature.

[0034] 5) After the fluidized bed reactor has been fluidized at the set temperature for a period of time (not less than 2 hours), start the feeding unit and gradually adjust the feeder speed or the opening of the feed pump valve to control the feeding rate, and feed the reaction raw materials into the fluidized bed reactor; control the feeding rate so that the mass ratio of the feed to the catalyst in the reactor per unit time is between 0.1:1 and 3:1, and adjust the carrier gas and the heat exchange of the reactor accordingly with the change of the feed rate to maintain a suitable reaction temperature and fluidization rate;

[0035] 6) The raw materials and catalyst are mixed and fluidized together in the fluidized bed reactor, and are simultaneously catalytically converted into gaseous products;

[0036] 7) Adjust the feed rate, inlet gas temperature, and reactor temperature respectively, and simultaneously sample and monitor the composition of gaseous products to stabilize and optimize the reaction process;

[0037] 8) The obtained gaseous product flows out of the fluidized bed reactor from the top gas outlet along with the carrier gas nitrogen and unreacted NH3 (mainly the carrier gas when the raw material is amide). After the small amount of fine catalyst powder entrained is removed by the filtration unit, it flows out of the reaction device for collection.

[0038] Preferably, the amination dehydration or dehydration reaction temperature is 280℃-450℃, and the reaction pressure is 0.1-1MPa.

[0039] Preferably, when the fluidized bed reactor performs a catalytic ammoniation dehydration reaction, the ammonifying agent is NH3, or any one or a combination of urea, ammonium bicarbonate, ammonium carbonate, melamine, or ammonium chloride.

[0040] Preferably, the catalyst in step 1) is a mixture of metal oxides, including but not limited to metals such as iron, calcium, magnesium, aluminum, and copper, and the mass ratio of each catalyst section is 1:1 or the mass is reduced by 1 to 8% from bottom to top.

[0041] Preferably, in step 3), the temperature of each catalyst section is raised to 280–450°C, and the heating rate is less than 5°C / min; the specified temperature is 280–450°C.

[0042] Preferably, in step 4), the specified temperature is 100–280°C, the molar ratio of ammonia to material is 1:1–15:1, and the reaction temperature is 280–450°C.

[0043] Preferably, the raw materials in step 6) include carboxylic acid, ester, and amide compounds, wherein the carboxylic acid and ester compounds require the addition of an amination agent during the reaction;

[0044] Preferably, in step 6), the carboxylic acid raw material is selected from one or more of salicylic acid, phthalic acid, terephthalic acid, glutaric acid, adipic acid, 1,4-cyclohexanedicarboxylic acid, 1,3-cyclohexanedicarboxylic acid, isophthalic acid, methacrylic acid, n-valeric acid, and n-hexanoic acid, wherein methacrylic acid, n-valeric acid, and n-hexanoic acid are liquid raw materials, and the others are solid raw materials;

[0045] Preferably, in step 6), the ester raw materials are selected from methyl salicylate, dimethyl phthalate, dimethyl terephthalate, methyl glutarate, methyl adipate, dimethyl 1,4-cyclohexanedicarboxylate, dimethyl 1,3-cyclohexanedicarboxylate, dimethyl isophthalate, and methacrylates; wherein methyl salicylate, dimethyl phthalate, dimethyl glutarate, dimethyl adipate, dimethyl 1,4-cyclohexanedicarboxylate, dimethyl 1,3-cyclohexanedicarboxylate, and methyl methacrylate are liquid raw materials, and the others are solid raw materials;

[0046] Preferably, the amide compound raw material in step 6) is selected from one or more of salicylamide, phthalamide, terephthalamide, glutaramide, adipamide, 1,4-cyclohexanedicarboxamide, 1,3-cyclohexanedicarboxamide, and methacrylamide, and all are solid raw materials;

[0047] Preferably, in step 7), the mass ratio of raw material to catalyst in the reactor is 0.1:1 to 3:1, the inlet temperature is 100 to 280°C, and the reactor temperature is 280 to 450°C.

[0048] Preferably, the specific reaction process of step 5) is as follows:

[0049] 51) Solid raw materials with a particle size of 0.1–2 mm are introduced from above or the side of the preheated fluidized zone;

[0050] 52) Mix with the catalyst overflowing from the reaction fluidization zone and heat up, controlling the upper limit of the temperature rise not to exceed the liquefaction or sublimation temperature of the raw material;

[0051] 53) The catalyst overflow rate is controlled by the blowing air velocity and the fluidizing air velocity. The blowing air velocity is 0.1 to 3 m / s and the fluidizing air velocity is 0.1 to 1.2 m / s. The mixing ratio of the material and the catalyst is controlled to be 1:0.5 to 1:6 by the above two air velocities. The temperature range of the preheating fluidization zone is 100 to 280℃.

[0052] 54) In the preheating fluidized zone, the raw materials and catalyst are mixed and reach the bottom of the preheating fluidized zone from top to bottom, and finally sent into the reaction fluidized zone by blowing air through the inclined guide plate;

[0053] 55) The particles entering the reaction fluidization zone continue to undergo rapid heating and thermal collapse into fine powder with a particle size of less than 100 μm, and then rapidly change phase to gaseous state, and are fully converted under the action of catalyst.

[0054] Beneficial effects

[0055] The reaction apparatus and method of this invention are designed for the amination and dehydration of carboxylic acids and carboxylic esters or the dehydration of amides to prepare nitrile compounds. Through the internal structural design of the core fluidized bed reactor, high-boiling-point carboxylic acids, carboxylic esters, and amides are directly introduced into the reactor without heating. By controlling particle movement through process design, direct carry-over within the fluidized bed is reduced or largely avoided, achieving orderly heating, thermal collapse, and gasification of the raw material particles. This improves the catalytic conversion reaction interface, increases the residence time of the raw materials, and significantly enhances the conversion rate and selectivity. Furthermore, this method does not use any organic solvents or toxic traditional dehydrating agents, resulting in minimal waste, safety, and reliability; it is a continuous, efficient, and green reaction apparatus. Attached Figure Description

[0056] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0057] Figure 1a A schematic diagram of a fluidized bed reactor for producing nitrile compounds according to the present invention, when the raw material is in a solid phase.

[0058] Figure 1b A schematic diagram of a fluidized bed reactor for producing nitrile compounds according to the present invention, when the raw material is in the liquid phase;

[0059] Figure 2 This is a schematic diagram of a fluidized bed reactor for producing nitrile compounds according to the present invention, wherein vertical baffles are provided.

[0060] Figure 3 a is a front view of the vertical partition of a fluidized bed reactor for producing nitrile compounds according to the present invention;

[0061] Figure 3 b is based on Figure 2 The cross-sectional view at the position indicated by the dashed line AA shows the relative position of the vertical partition to the fluidized bed reactor.

[0062] Figure 4 This is a top view based on the horizontal distribution plate;

[0063] In the diagram: 1a Solid feed unit; 11a Hopper; 12a Feeder; 1b Liquid feed unit; 11b Storage tank; 12b Feed pump;

[0064] 2 Fluidized bed reactor; 21-1 First feed inlet, 21-2 Second feed inlet, 21-3 Third feed inlet, 21-4 Fourth feed inlet, 22 Liquid distributor; 23 Air inlet; 24 Distribution plate; 25 Discharge outlet; 26 Catalyst discharge outlet; 27 Auxiliary heat exchanger; 28-1 Push air outlet; 28-2 Loose air outlet; 28-3 Blowing air outlet; 29 Vertical partition, 29-1 Inverted trapezoidal structure, 29-2 Rectangular structure, 29-3 Flow guiding structure; 3 Filter unit; 31 Filter. Detailed Implementation

[0065] The present invention will now be described in detail. Before proceeding with the description, it should be understood that the terminology used in this specification and the appended claims should not be construed as limited to its general or dictionary meaning, but rather should be interpreted according to the meaning and concept corresponding to the technical aspects of the invention, based on the principle that the inventors are allowed to appropriately define the terms for the best interpretation. Therefore, the description presented herein is merely a preferred example for illustrative purposes and is not intended to limit the scope of the invention. It should be understood that other equivalents or modifications can be obtained from it without departing from the spirit and scope of the invention.

[0066] The following embodiments are merely examples illustrating implementations of the present invention and do not constitute any limitation on the present invention. Those skilled in the art will understand that modifications made without departing from the spirit and concept of the present invention fall within the protection scope of the present invention. Unless otherwise specified, the reagents and instruments used in the following embodiments are commercially available products.

[0067] Preferred embodiments of the present disclosure will be described in detail below with reference to the accompanying drawings. Before description, it should be understood that the terminology used in the specification and appended claims should not be construed as limited to its general and dictionary meaning, but rather should be interpreted based on the principle of allowing the inventors to appropriately define the terminology for the best interpretation, and based on its meaning and concept corresponding to the technical level of the invention. Therefore, the description herein is merely a preferred example for illustrative purposes and is not intended to limit the scope of the invention; thus, it should be understood that other equivalent implementations and modifications can be made without departing from the spirit and scope of the invention.

[0068] In this document, the terms “comprising,” “including,” “having,” “containing,” or any other similar terms are open-ended conjunctions intended to cover non-exclusive inclusions. For example, a composition or article containing a plurality of elements is not limited to those listed herein, but may also include other elements not explicitly listed but typically inherent to the composition or article. Furthermore, unless explicitly stated to the contrary, the term “or” is inclusive, not exclusive. For example, the condition “A or B” is satisfied in any of the following cases: A is true (or exists) and B is false (or does not exist); A is false (or does not exist) and B is true (or exists); A and B are both true (or exist). Moreover, in this document, the terms “comprising,” “including,” “having,” and “containing” should be interpreted as specifically disclosed and simultaneously cover closed or semi-closed conjunctions such as “composed of” and “substantially composed of.”

[0069] In this document, all features or conditions defined in the form of numerical ranges or percentage ranges are for the sake of brevity and convenience only. Accordingly, descriptions of numerical ranges or percentage ranges should be considered as covering and specifically disclosing all possible secondary ranges and individual values ​​within those ranges, particularly integer values. For example, a range description of "1 to 8" should be considered as specifically disclosing all secondary ranges such as 1 to 7, 2 to 8, 2 to 6, 3 to 6, 4 to 8, 3 to 8, etc., particularly secondary ranges defined by all integer values, and should be considered as specifically disclosing individual values ​​within those ranges such as 1, 2, 3, 4, 5, 6, 7, 8, etc. Unless otherwise specified, the foregoing interpretation applies to all content throughout this invention, regardless of its scope.

[0070] If a quantity or other numerical value or parameter is expressed as a range, a preferred range, or a series of upper and lower limits, it should be understood that this document has specifically disclosed all ranges consisting of any upper or preferred value of that range and the lower or preferred value of that range, regardless of whether such ranges are separately disclosed. Furthermore, when a range of numerical values ​​is mentioned herein, unless otherwise stated, the range shall include its endpoints and all integers and fractions within the range.

[0071] In this document, numerical values ​​are to be understood as having a precision with significant digits, provided that the purpose of the invention can be achieved. For example, the number 40.0 should be understood to cover a range from 39.50 to 40.49.

[0072] To clarify the invention, parts irrelevant to the description have been omitted from the drawings, and throughout the specification, the same or similar parts are indicated by the same reference numerals.

[0073] Furthermore, for ease of explanation, the dimensions and thicknesses of each component shown in the accompanying drawings are arbitrarily illustrated; therefore, the invention is not necessarily limited to those shown in the drawings.

[0074] Throughout the specification, when it is said that an element is "connected" to another element, it includes not only "direct connection" but also "indirect connection" between other components. Furthermore, when it is said that an element "comprises" a part, it means that the element may further include other parts rather than exclude them, unless otherwise explicitly stated.

[0075] The terms “first”, “second”, etc., used in this article are used to explain various constituent elements, and they are only used for the purpose of distinguishing one constituent element from another.

[0076] Furthermore, the terminology used herein is for the purpose of explaining exemplary embodiments only and is not intended to limit the invention. Singular expressions also include their plural expressions unless otherwise expressly indicated in the context. Terms such as “comprising,” “equipped with,” or “having” as used herein are used to specify the presence of a practical characteristic, number, step, constituent element, or combination thereof, and should be understood to not exclude the possibility of the addition or presence of one or more other characteristics, numbers, steps, constituent elements, or combinations thereof.

[0077] Furthermore, if a layer or element is referred to as being formed "above" or "on top of" a "layer" or "element", it means that each layer or element is formed directly on that layer or element, or that other layers or elements may be formed between layers, bodies, or substrates.

[0078] In addition, unless otherwise stated, the reagents and solvents disclosed below were purchased from Sinopharm Chemical Reagent Co., Ltd. Salicylic acid amide was purchased from Shandong Longxin Chemical Co., Ltd. HPLC detection was performed using a Shimadzu LC-20A HPLC system equipped with a UV detector.

[0079] The detection method is as follows:

[0080] Mobile phase: acetonitrile + 50 mM sodium dihydrogen phosphate buffer; flow rate: 1.0 ml / min; column: ODS-C18: 4.6 mm × 250 mm × 5 μm; column temperature: 30 ℃; detection wavelength: 275 nm;

[0081] Injection volume: 10 μl;

[0082]

[0083]

[0084] Gas chromatography detection was performed using a Shimadzu GC-2010plus, equipped with an FID detector.

[0085] The detection method is as follows:

[0086] Mobile phase: high-purity nitrogen; vaporization chamber conditions: 280℃;

[0087] Chromatographic column: DB-5, 30m*0.25mm*0.25um; column temperature: initial temperature 50℃, increased to 160℃ at 20℃ / min, then increased to 220℃ at 2℃ / min; column flow rate 0.91ml / min; split ratio 5; detector conditions: 300℃; injection volume: 1μl.

[0088]

[0089]

[0090]

[0091]

[0092] The flow rate of the raw material is expressed in g / min, and the amount of catalyst is expressed in g.

[0093] The structure of the device of the present invention will be described in detail below with reference to Figures 1-4:

[0094] A fluidized bed reactor for producing nitrile compounds includes a feed unit 1, a fluidized bed reactor 2, and a filtration unit 3 connected in sequence.

[0095] The feeding unit 1 is located on one side of the fluidized bed reactor 2 and is connected to the feed inlet of the fluidized bed reactor 2. It is used for the input of reaction raw materials, which can be solid or liquid.

[0096] The fluidized bed reactor 2 has a three-section structure: an upper cylindrical structure, a middle inverted conical structure, and a lower cylindrical structure. The diameter of the upper cylindrical structure is larger than that of the lower cylindrical structure, forming an enlarged section. The diameter ratio of the upper and lower sections is 1.1:1 to 4:1. They are connected by the middle inverted conical structure to form a whole. The angle between the cone surface of the middle inverted conical structure and the vertical direction is 15°-45°. The lower cylindrical structure is the main reaction zone. In a relatively small space, by controlling process conditions such as gas distribution, air velocity, and heat exchange, the reactants and catalyst are brought into full contact to achieve the reaction conditions, thereby achieving a rapid reaction. The main purposes of the upper cylindrical structure are: firstly, to reduce the gas velocity to achieve gas-solid phase separation; and secondly, to provide sufficient space for auxiliary components such as feeding or exhaust devices. The middle inverted conical structure connects the upper and lower structures and promotes the return of materials or catalysts to the lower reaction zone of the fluidized bed. This is specifically controlled by the cone angle, fluidizing gas velocity, and catalyst particle size.

[0097] The fluidized bed reactor 2 has at least one feed inlet; the lower cylindrical structure, which serves as the main reaction zone, is equipped with single-stage or multi-stage horizontal distribution plates 24 for carrying the catalyst and distributing the gas, while dividing the reaction process into several corresponding reaction zones. The catalysts packed on each distribution plate can be the same or different; the bottom of the fluidized bed reactor is provided with an air inlet 23 for introducing carrier gas or a mixture of carrier gas and NH3. The carrier gas is usually an inert gas, such as nitrogen. The carrier gas and NH3 together serve as fluidizing gas to fluidize the catalyst, with some NH3 participating in the reaction.

[0098] The filtration unit 3 is located on the other side of the fluidized bed reactor 2 and is connected to the outlet 25 of the fluidized bed reactor 2. It is used to filter and remove solid materials or catalyst particles entrained in the gas phase mixture.

[0099] Preferably, the feed inlet of the fluidized bed reactor 2 is located at one or more positions on the top of the upper cylindrical structure, the side wall of the upper cylindrical structure, the upper part of the side wall of the lower cylindrical structure, or the side wall of the reaction zone between the various levels of horizontal distribution plates 24 of the lower cylindrical structure. The feed inlet is selected from different locations based on the properties, phase, and reaction conditions of the reactants. (Reference) Figure 1a and Figure 1bThe fluidized bed reactor 2 may include one or more of inlets 21-1, 21-2, 21-3, and 21-4, wherein inlet 21-4 is located at the top of the upper cylindrical structure near the cylinder wall, inlet 21-1 is located on the side wall of the upper cylindrical structure, inlet 21-2 is located at the upper part of the side wall of the lower cylindrical structure of the fluidized bed reactor 2, and inlet 21-3 is located near the middle of the side wall of the lower cylindrical structure of the fluidized bed reactor 2. Different inlets can be selected to add raw materials according to the material condition, reaction conditions, etc., and the raw materials can be solid or liquid.

[0100] Preferably, refer to Figure 1a When the reactant is a solid phase, the feeding unit 1a includes a hopper 11a and a feeder 12a;

[0101] Furthermore, refer to Figure 1a When the reactant is a solid phase, the feeder 12a includes, but is not limited to, a screw feeder or a star feeder, and the feeder is directly connected to the feed inlet of the fluidized bed reactor 2.

[0102] Preferably, refer to Figure 3 For the fluidized bed reactor 2 containing a single-stage distribution plate, when the reactant is a solid phase, the fluidized bed reactor 2 further includes a vertical baffle 29. The vertical baffle 29 has a three-section structure: an inverted trapezoidal structure 29-1 at the top, a rectangular structure 29-2 in the middle, and a flow-guiding structure 29-3 inclined to one side at the bottom. The shape of the inverted trapezoidal structure 29-1 is consistent with the cross-section of the inverted conical structure in the middle of the fluidized bed reactor 2. The rectangular structure 29-2 in the middle is consistent with the cross-section of the fluidized bed reactor. The cross-section of the lower cylindrical structure of the fluidized bed reactor 2 remains consistent. The vertical baffle 29 is vertically arranged in the middle inverted cone structure and the lower cylindrical structure of the fluidized bed reactor 2, dividing the space into two parts with different volumes: a preheating fluidized zone and a reaction fluidized zone, with a volume ratio between the two parts being 1:4 and 1:2. The lower flow guiding structure 29-3 of the vertical baffle 29 is located above the horizontal distribution plate 24, and the flow guiding structure 29-3 does not contact the horizontal distribution plate 24, forming a gap.

[0103] Further reference Figure 2 The feed inlets 21-1 to 21-4 are arranged to correspond to the preheating fluidized zone separated by the vertical partition 29. When raw materials are added, they first fall into the preheating fluidized zone for preheating, and then fall naturally to the vicinity of the flow guide structure 29-3 of the vertical partition 29. The airflow blown by the blower 28-3 enters the reaction fluidized zone through the gap between the flow guide structure 29-3 and the horizontal distribution plate 24 for reaction, which helps to repeat the reaction.

[0104] Preferably, refer to Figure 4 The portion of the single-stage horizontal distribution plate 24 corresponding to the preheating fluidized zone side is not provided with pores, so there is no fluidizing air on the preheating fluidized zone side. The portion of the single-stage distribution plate 24 corresponding to the reaction fluidized zone side is provided with pores, so the fluidizing air enters the reaction fluidized zone through the pores, promoting the reaction.

[0105] Preferably, the sidewall of the preheating fluidized zone is provided with a push air vent 28-1, a loosening air vent 28-2, and a blowing air vent 28-3 from top to bottom; wherein the push air vent 28-1 promotes the downward flow of materials; wherein the loosening air vent 28-2 loosens materials to prevent them from accumulating at corners; wherein the blowing air vent 28-3 blows the materials in the preheating fluidized zone to the reaction zone through the inclined flow guiding structure at the lower part of the vertical partition.

[0106] Preferably, refer to Figure 1b When the reaction raw material is liquid, the feeder 1b includes a storage tank 11b and a feed pump 12b;

[0107] Furthermore, refer to Figure 1b When the reactant is a liquid phase, a liquid distributor 22 is also provided in the upper cylindrical structure of the fluidized bed reactor 2. The liquid distributor 22 includes, but is not limited to, a liquid distribution plate and an atomizing nozzle. The feed pump 12b of the feed unit 1b is connected to the feed inlet 21-1 of the fluidized bed reactor 2 through a pipeline and transports the reactant to the liquid distributor 22.

[0108] Preferably, the discharge port 25 is located at the top of the fluidized bed reactor 2 and is used to discharge the gas phase mixture, including the generated gas phase products, carrier gas and NH3 (NH3 may not be present when the raw material is amide);

[0109] Preferably, the horizontal distribution plate 24 is, but is not limited to, a sieve plate, a sintering plate, or a bubble cap plate;

[0110] Preferably, the number of the horizontal distribution plates 24 is 1 to 10;

[0111] Preferably, catalyst discharge ports 26 are provided near the reactor wall above each horizontal distribution plate 24 in the fluidized bed reactor 2 to facilitate catalyst discharge. The catalyst can be loaded through the manhole or handhole of the fluidized bed reactor, or it can be added through the feed port.

[0112] Preferably, when a solid-phase ammoniating agent is used, it can be pre-mixed with the reaction raw materials and added to the fluidized bed reactor 2 through the feed unit 1a; or an additional set of the feed unit 1a can be added, and the feed port can be selected according to the specific reaction conditions.

[0113] Preferably, an auxiliary heat exchanger 27 may be provided on the outer wall of the reaction zone of the lower cylindrical structure of the fluidized bed reactor 2. The auxiliary heat exchanger 27 includes, but is not limited to, a heat tracing cable, a heat exchange coil, a heat exchange jacket, and ceramic heating elements.

[0114] Preferably, the filter 31 of the filtration unit 3 may include, but is not limited to, a screen with a corresponding aperture, a cyclone separator, etc.

[0115] Example 1:

[0116] refer to Figure 1a The structure of the fluidized bed is as follows: reaction section Φ40mm, single-layer horizontal distribution plate without vertical partition 29, upper expansion section Φ100mm, total length about 400mm, and about 300g of catalyst is loaded.

[0117] 1) After the system is purged with nitrogen, nitrogen carrier gas is introduced into the fluidized bed reactor 2 through the air inlet 23. The flow meter controls the nitrogen flow rate to be about 5 L / min, so as to fluidize the catalyst in the fluidized bed reactor 2.

[0118] 2) Turn on the auxiliary heat exchanger 27, and at the same time, preheated carrier gas nitrogen is continuously introduced into the fluidized bed reactor 2 to heat the reactor until the fluidized bed reactor 2 is heated to about 350°C and stabilized in fluidization.

[0119] 3) The raw material is solid salicylamide. Start the feeding unit 1 and gradually adjust the speed of the feeder 12 to control the feeding rate, and send the reaction raw material into the fluidized bed reactor 2.

[0120] 4) When the salicylamide falls into the reaction zone of the fluidized bed reactor 2, it is rapidly mixed and fluidized with the catalyst therein, and heat and mass transfer occur simultaneously. The salicylamide is heated and vaporized, and then catalytically dehydrated to generate gaseous salicylic nitrile products.

[0121] 5) Adjust the feed rate, air temperature and other process conditions respectively to control the conversion rate of salicylamide and the amount of by-product phenol generated;

[0122] 6) The obtained salicylnitrile, phenol and unreacted salicylamide, etc., flow out of the fluidized bed reactor 2 from the gas phase outlet 25 at the top with nitrogen gas. After the small amount of fine catalyst powder entrained is removed by the filter unit 3, they flow out of the reaction device for cooling and collection.

[0123] The above-mentioned salicylamide dehydration reaction was carried out using three different catalysts, with a space velocity of 0.3 h⁻¹ for each catalyst. -1 When the reaction temperature is 330℃, the following results are obtained:

[0124]

[0125] Example 2:

[0126] refer to Figure 1b The structure of the fluidized bed is as follows: reaction section Φ40mm, single-layer horizontal distribution plate without vertical partition 29, upper expansion section Φ100mm, total length about 400mm, and filled with a mixture of 100g Al2O3 and 200g Fe3O4 catalyst.

[0127] 1) After the system is purged with nitrogen, nitrogen carrier gas is introduced into the fluidized bed reactor 2 through the air inlet 23. The flow meter controls the nitrogen flow rate to be about 5 L / min, so as to fluidize the catalyst in the fluidized bed reactor 2.

[0128] 2) Turn on the auxiliary heat exchanger 27, and at the same time, preheated carrier gas nitrogen is continuously introduced into the fluidized bed reactor 2 to heat the reactor.

[0129] 3) When the fluidized bed reactor 2 is normally fluidized and reaches about 330°C, NH3 is gradually mixed into nitrogen gas in proportion, and the mixture is preheated to 300°C-350°C and then introduced into the reactor until the reactor is stably fluidized under mixed gas conditions and reaches the specified temperature of 330°C-350°C.

[0130] 4) The raw materials are methyl salicylate, dimethyl phthalate, and dimethyl terephthalate, wherein methyl salicylate and dimethyl phthalate are liquid raw materials, and dimethyl terephthalate is preheated to liquid. The feeding unit 1 is turned on, and the opening of the valve of the feed pump 12 is gradually adjusted to control the feeding rate, so as to send the reaction raw materials into the fluidized bed reactor 2.

[0131] 5) After the raw material is atomized, it falls into the reaction zone of the fluidized bed reactor 2 and mixes rapidly with the catalyst therein, resulting in heat and mass transfer. The raw material is heated and vaporized, and at the same time, it undergoes catalytic dehydration on the catalyst surface to generate the corresponding gaseous nitriles.

[0132] 6) Adjust the feed rate, air temperature and other process conditions respectively to control the conversion rate of raw materials and the amount of by-products generated;

[0133] 7) The obtained gaseous products, etc., flow out of the fluidized bed reactor 2 from the gaseous outlet 25 at the top with nitrogen gas. After the small amount of fine catalyst powder entrained is removed by the filter unit 3, the products flow out of the reaction device for cooling and collection.

[0134] The above-mentioned amination and dehydration reaction process was carried out on three raw materials: methyl salicylate, dimethyl phthalate, and dimethyl terephthalate, with a molar ratio of NH3 to raw materials of 10:1. The results are as follows:

[0135] Methyl salicylate: space velocity 0.2h -1At a temperature of 350℃, the conversion rate was 99.2%, and the selectivity for salicylate was 91%.

[0136] Dimethyl phthalate: space velocity 0.3h -1 At a temperature of 330℃, the conversion rate was 99.2%, and the selectivity for phthalic acid dicarboxylate was 91%.

[0137] Dimethyl terephthalate: space velocity 0.3h -1 At a temperature of 330℃, the conversion rate was 99.5%, and the selectivity for dimethyl terephthalate was 92%.

[0138] Example 3

[0139] refer to Figure 1b The structure of the fluidized bed is as follows: reaction section Φ40mm, single-layer horizontal distribution plate without vertical partition 29, upper expansion section Φ100mm, total length about 400mm, and about 300g of a mixture of 150g Al2O3, 50g CaO and 100g Fe3O4 catalyst.

[0140] 1) After the system is purged with nitrogen, nitrogen carrier gas is introduced into the fluidized bed reactor 2 through the air inlet 23. The flow meter controls the nitrogen flow rate to be about 5 L / min, so as to fluidize the catalyst in the fluidized bed reactor 2.

[0141] 2) Turn on the auxiliary heat exchanger 27, and at the same time, preheat the carrier gas nitrogen and continuously introduce it into the fluidized bed reactor 2 to heat the reactor until the fluidized bed reactor 2 is normally fluidized and reaches 300℃-330℃;

[0142] 3) The raw materials are valeric acid and hexanoic acid, and the ammonia source is urea. The two are mixed in advance according to the ratio. The feeding unit 1 is turned on and the feed rate is controlled by gradually adjusting the speed of the feeder 12 to send the reaction raw materials into the fluidized bed reactor 2.

[0143] 4) The raw materials and catalyst are mixed and fluidized in the fluidized bed reactor 2. The raw materials are heated and gasified while being catalytically dehydrated to generate the corresponding gaseous nitriles.

[0144] 5) Adjust the feed rate, air temperature and other process conditions respectively to control the conversion rate of raw materials and the amount of by-products generated;

[0145] 6) The obtained gaseous products, etc., flow out of the fluidized bed reactor 2 from the gaseous outlet 25 at the top with nitrogen gas. After the small amount of fine catalyst powder entrained is removed by the filter unit 3, the products flow out of the reaction device for cooling and collection.

[0146] The raw materials were valeric acid and hexanoic acid, with urea as the ammonia source. The above-mentioned ammoniation and dehydration reaction processes were carried out separately, and the results are as follows:

[0147] Valeric acid: The molar ratio of valeric acid to urea is 5:1, and the space velocity is 0.2 h⁻¹. -1 At a temperature of 300℃, the conversion rate was 100%, and the selectivity for n-valeronitrile was 96%.

[0148] Hexanoic acid: The molar ratio of hexanoic acid to urea is 6:1, and the space velocity is 0.2 h⁻¹. -1 At a temperature of 300℃, the conversion rate was 100%, and the selectivity for n-hexanonitrile was 97%.

[0149] Example 4

[0150] refer to Figure 1a The structure uses a fluidized bed with the following dimensions: a reaction section of Φ400mm, a single-layer horizontal distribution plate with vertical baffles 29, an upper expansion section of Φ1000mm, a total height of approximately 4000mm, and is filled with a mixture of 100kg Al2O3, 100kg Fe3O4, and approximately 200kg of fluidized bed.

[0151] 1) After the system is purged with nitrogen, nitrogen carrier gas is introduced into the fluidized bed reactor 2 through the air inlet 23. The flow meter controls the nitrogen flow rate to be about 500 L / min, so as to fluidize the catalyst in the fluidized bed reactor 2.

[0152] 2) Turn on the auxiliary heat exchanger 27, and simultaneously, continuously introduce preheated carrier gas nitrogen into the fluidized bed reactor 2 to heat the reactor until the fluidized bed reactor 2 is normally fluidized and reaches approximately 300℃-380℃.

[0153] 3) The raw material is solid salicylamide. Start the feeding unit 1 and gradually adjust the speed of the feeder 12 to control the feeding rate to 60 kg / h, and send the reaction raw material into the fluidized bed reactor 2.

[0154] 4) When the salicylamide and the catalyst are mixed downward in the preheating zone of the fluidized bed reactor 2 and reach the bottom of the fluidized bed, they are sent into the fluidized reaction zone by blowing air. After the salicylamide is further heated, it undergoes thermal collapse and vaporization in sequence, and catalytic dehydration on the catalyst surface to generate gaseous salicylic nitrile products.

[0155] 5) Adjust the feed rate, air temperature and other process conditions respectively to control the conversion rate of salicylamide and the amount of by-product phenol generated;

[0156] 6) The obtained salicylnitrile, phenol and unreacted salicylamide, etc., flow out of the fluidized bed reactor 2 from the gas phase outlet 25 at the top with nitrogen gas. After the small amount of fine catalyst powder entrained is removed by the filter unit 3, they flow out of the reaction device for cooling and collection.

[0157] The reaction results are as follows:

[0158] Temperature 370℃, air velocity 0.6h -1Salicylic amide conversion rate 99.5%, salicylic nitrile selectivity 92%, phenol selectivity 5%;

[0159] Temperature 350℃, air velocity 0.4h -1 Salicylic amide conversion rate 99.5%, salicylic nitrile selectivity 94%, phenol selectivity 4%.

[0160] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A fluidized bed reactor for producing nitrile compounds, characterized in that, It includes a feeding unit, a fluidized bed reactor, and a filtration unit connected in sequence; The feeding unit is located on one side of the fluidized bed reactor and is connected to the feed inlet of the fluidized bed reactor. It is used to input the reaction raw materials, which are solid raw materials. The fluidized bed reactor has a three-section structure: an upper cylindrical structure, a middle inverted conical structure, and a lower cylindrical structure. The diameter of the upper cylindrical structure is larger than that of the lower cylindrical structure, forming an enlarged section. The diameter ratio of the upper and lower sections is 1.1:1 to 4:

1. They are connected by the middle inverted conical structure to form a whole. The angle between the conical surface of the middle inverted conical structure and the vertical direction is 15° to 45°. The fluidized bed reactor has at least one feed inlet; the lower cylindrical structure, which serves as the main reaction zone, is equipped with single or multiple horizontal distribution plates to carry the catalyst and distribute the gas, while dividing the reaction process into several corresponding reaction zones. The catalysts packed on each distribution plate may be the same or different; the bottom of the fluidized bed reactor is provided with an air inlet for introducing carrier gas or a mixture of carrier gas and NH3. The filtration unit is located on the other side of the fluidized bed reactor and is connected to the outlet of the fluidized bed reactor. It is used to filter out solid materials or catalyst particles entrained in the gas-phase mixture. When the reactants are in a solid phase, the feeding unit includes a hopper and a feeder; When the reactant is a solid phase, the feeder includes a screw feeder or a star feeder, and the feeder is directly connected to the feed inlet of the fluidized bed reactor. For the fluidized bed reactor containing a single-stage distribution plate, when the reactant is a solid phase, the fluidized bed reactor further includes a vertical baffle. The vertical baffle has a three-section structure: an inverted trapezoidal structure at the top, a rectangular structure in the middle, and a flow-guiding structure inclined to one side at the bottom. The shape of the inverted trapezoidal structure is consistent with the cross-section of the inverted conical structure in the middle of the fluidized bed reactor, and the rectangular structure is consistent with the cross-section of the lower cylindrical structure in the fluidized bed reactor. The vertical baffle is vertically arranged in the inverted conical structure in the middle and the lower cylindrical structure of the fluidized bed reactor, dividing the space into two parts with unequal volumes: a preheating fluidized zone and a reaction fluidized zone, with a volume ratio of 1:4 to 1:

2. The lower flow-guiding structure of the vertical baffle is located above the horizontal distribution plate, and the flow-guiding structure does not contact the horizontal distribution plate, forming a gap. The portion of the single-stage distribution plate corresponding to the preheating fluidized zone side is not provided with pores, so there is no bottom-up fluidizing air on the preheating fluidized zone side. The portion of the single-stage distribution plate corresponding to the reaction fluidized zone side is provided with pores, so the fluidizing air enters the reaction fluidized zone through the pores. The preheating fluidized zone sidewall is provided with push air vents, loosening air vents, and blowing air vents in sequence from top to bottom; wherein the push air vents are used to promote the downward movement of materials; wherein the loosening air vents are used to loosen materials to prevent them from accumulating at corners; wherein the blowing air vents are used to blow materials from the preheating fluidized zone to the reaction zone through the inclined flow guiding structure at the lower part of the vertical partition. The fluidized bed reactor is used for the reaction of preparing nitrile compounds by amination and dehydration of carboxylic acids, carboxylic esters, or amides. The solid raw material has a particle size of 0.1-2 mm. The raw material undergoes heating and thermal avalanche in the reactor to become fine powder with a particle size of less than 100 μm and then gasification.

2. The fluidized bed reactor for producing nitrile compounds according to claim 1, characterized in that, The feed inlet of the fluidized bed reactor is located at one or more positions on the top of the upper cylindrical structure, the side wall of the upper cylindrical structure, the upper part of the side wall of the lower cylindrical structure, or the side wall of the reaction zone between the horizontal distribution plates of the lower cylindrical structure. The feed is selected from different feed inlets according to the properties, phases, and reaction conditions of the reactants.

3. The fluidized bed reactor for producing nitrile compounds according to claim 1, characterized in that, When the reactants are in the liquid phase, the feeder includes a storage tank and a feed pump; When the reactant is a liquid phase, a liquid distributor is also provided in the upper cylindrical structure of the fluidized bed reactor. The liquid distributor includes a liquid distribution plate and an atomizing nozzle. The feed pump of the feeding unit is connected to the feed inlet of the fluidized bed reactor through a pipeline and transports the reactant to the liquid distributor.

4. The fluidized bed reactor for producing nitrile compounds according to claim 1, characterized in that, The discharge port is located at the top of the fluidized bed reactor and is used to discharge the gas phase mixture, which includes the generated gas phase products, carrier gas and NH3. When the raw material is amide, it may or may not contain NH3.

5. A fluidized bed reactor for producing nitrile compounds according to claim 4, characterized in that, The horizontal distribution plate may include a sieve plate, a sintered plate, or a bubble cap plate.

6. A fluidized bed reactor for producing nitrile compounds according to claim 4, characterized in that, The number of horizontal distribution plates is 1 to 10.

7. A fluidized bed reactor for producing nitrile compounds according to claim 4, characterized in that, Catalyst discharge ports are provided near the reactor wall above each horizontal distribution plate in the fluidized bed reactor to facilitate catalyst discharge. Catalyst loading is completed through the manhole or handhole of the fluidized bed reactor or added through the feed port.

8. A fluidized bed reactor for producing nitrile compounds according to claim 4, characterized in that, When a solid-phase ammoniating agent is used, it is pre-mixed with the reaction raw materials and added to the fluidized bed reactor through the feeding unit; or an additional feeding unit is added, and the feed port is selected according to the specific reaction conditions.

9. A fluidized bed reactor for producing nitrile compounds according to claim 1, characterized in that, An auxiliary heat exchanger is provided on the outer wall of the reaction zone of the lower cylindrical structure of the fluidized bed reactor. The auxiliary heat exchanger includes a heat tracing cable, a heat exchange coil, a heat exchange jacket, or a ceramic heating plate.

10. A fluidized bed reactor for producing nitrile compounds according to claim 9, characterized in that, The filter unit includes a screen with a corresponding aperture and a cyclone separator.

11. A method for producing nitrile compounds using a fluidized bed reactor according to any one of claims 1-10, characterized in that, Includes the following steps: 1) Weigh out each section of catalyst according to the specified weight, and then fill the catalyst into the corresponding horizontal distribution plate through the manhole, handhole or corresponding feed port of each section of the fluidized bed reactor. Then seal the entire reaction device and check the airtightness. 2) Carrier gas is introduced into the reactor through the air inlet of the fluidized bed reactor to replace the system. After the oxygen content in the entire reaction device system is lower than 0.1%, the temperature is prepared to be increased. 3) Start the auxiliary heat exchanger, and at the same time, the preheated carrier gas nitrogen is continuously introduced into the fluidized bed reactor to fluidize and heat the catalyst in each section of the reactor. The carrier gas flows out of the fluidized bed reactor through the gas phase outlet and continues to enter the subsequent filtration unit to heat the filtration unit together. Then it flows out of the entire reaction device. The heating process continues until the fluidized bed reactor is heated to the specified temperature. When the raw material is amide, proceed directly to step 5); 4) After the fluidized bed reactor is normally fluidized and reaches the specified temperature, NH3 is gradually mixed into the carrier gas in proportion and preheated together to the specified temperature before being introduced into the reactor until the reactor is stably fluidized under mixed gas conditions and reaches the reaction temperature. 5) After the fluidized bed reactor has been fluidized at the set temperature for a period of time, the feeding unit is turned on, and the feeder speed or the opening of the feed pump valve is gradually adjusted to control the feed rate, so as to send the reaction raw materials into the fluidized bed reactor; the feed rate is controlled so that the mass ratio of the feed to the catalyst in the reactor per unit time is 0.1:1 to 3:1, and the carrier gas and the heat exchange of the reactor are adjusted accordingly with the change of the feed rate to maintain a suitable reaction temperature and fluidization rate; 6) The raw materials and catalyst are mixed and fluidized together in the fluidized bed reactor, and are simultaneously catalytically converted into gaseous products; 7) Adjust the feed rate, inlet gas temperature, and reactor temperature respectively, and simultaneously sample and monitor the composition of gaseous products to stabilize and optimize the reaction process; 8) The obtained gaseous product flows out of the fluidized bed reactor from the top gas phase outlet along with the carrier gas nitrogen and unreacted NH3. After the small amount of fine catalyst powder entrained is removed by the filtration unit, it flows out of the reaction device for collection.

12. The method for producing nitrile compounds according to claim 11, characterized in that, Includes at least one of the following features (a) to (j): (a) The temperature of the ammoniation dehydration or dehydration reaction is 280℃-450℃, and the reaction pressure is 0.1-1 MPa; (b) When the fluidized bed reactor carries out the catalytic ammoniation dehydration reaction, the ammonifying agent is any one or a combination of more than one of NH3, urea, ammonium bicarbonate, ammonium carbonate, melamine or ammonium chloride; (c) The catalyst in step 1) is a mixture of metal oxides, including metal oxides of iron, calcium, magnesium, aluminum or copper, and the mass ratio of each catalyst section is 1:1 or the mass is reduced by 1-8% from bottom to top; (d) In step 3), the temperature of each catalyst section is raised to 280~450℃, and the heating rate is less than 5℃ / min; the specified temperature is 280~450℃. (e) The specified temperature in step 4) is 100~280℃, the molar ratio of ammonia to material is 1:1~15:1, and the reaction temperature is 280~450℃; (f) The raw materials in step 6) include carboxylic acid, ester or amide compounds, wherein carboxylic acid and ester compounds require the addition of an amination agent during the reaction; (g) In step 6), the carboxylic acid raw materials are selected from one or more of salicylic acid, phthalic acid, terephthalic acid, glutaric acid, adipic acid, 1,4-cyclohexanedicarboxylic acid, 1,3-cyclohexanedicarboxylic acid, isophthalic acid, methacrylic acid, n-valeric acid, or n-hexanoic acid, wherein methacrylic acid, n-valeric acid, and n-hexanoic acid are liquid raw materials, and the others are solid raw materials; (h) In step 6), the ester raw materials are selected from methyl salicylate, dimethyl phthalate, dimethyl terephthalate, methyl glutarate, methyl adipate, dimethyl 1,4-cyclohexanedicarboxylate, dimethyl 1,3-cyclohexanedicarboxylate, dimethyl isophthalate, and methacrylate; among which methyl salicylate, dimethyl phthalate, dimethyl glutarate, dimethyl adipate, dimethyl 1,4-cyclohexanedicarboxylate, dimethyl 1,3-cyclohexanedicarboxylate, and methyl methacrylate are liquid raw materials, and the others are solid raw materials; (i) The amide compound raw material in step 6) is selected from one or more of salicylamide, phthalamide, terephthalamide, glutaramide, adipamide, 1,4-cyclohexanedicarboxamide, 1,3-cyclohexanedicarboxamide or methacrylamide, and all of them are solid raw materials; (j) In step 7), the mass ratio of raw material to catalyst in the reactor is 0.1:1 to 3:1, the inlet temperature is 100 to 280°C, and the reactor temperature is 280 to 450°C.

13. The method for producing nitrile compounds according to claim 11, characterized in that, The specific reaction process in step 5) is as follows: 51) Solid raw materials with a particle size of 0.1~2mm are introduced from above or the side of the preheated fluidized zone; 52) Mix with the catalyst overflowing from the reaction fluidization zone and heat up, controlling the upper limit of the temperature rise not to exceed the liquefaction or sublimation temperature of the raw material; 53) The catalyst overflow rate is controlled by the blowing air velocity and the fluidizing air velocity, with the blowing air velocity being 0.1~3m / s and the fluidizing air velocity being 0.1~1.2m / s; the mixing ratio of material and catalyst is controlled within the range of 1:0.5~1:6 by the above blowing air velocity and fluidizing air velocity, and the temperature range of the preheating fluidization zone is 100~280℃. 54) In the preheating fluidized zone, the raw materials and catalyst are mixed and reach the bottom of the preheating fluidized zone from top to bottom, and finally sent into the reaction fluidized zone by blowing air through the inclined guide plate; 55) The particles entering the reaction fluidization zone continue to undergo rapid heating and thermal collapse into fine powder with a particle size of less than 100 μm, and then rapidly change phase to gaseous state, and are fully converted under the action of catalyst.

Images