Anhydride hydrolysis reactor, hydrolysis reaction method and application thereof
By adopting the design of a hydraulic jet reactor in the succinic anhydride hydrolysis reactor, the problems of explosive boiling of the reactor and poor equipment stability are solved, and the equipment is high stability and low cost production are achieved.
Patent Information
- Application Number
- CN202311555613.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-11-21
- Publication Date
- 2025-05-23
AI Technical Summary
The existing succinic anhydride hydrolysis reactors are prone to bumps when dealing with the acid anhydride hydrolysis reaction, and the equipment has poor sealing and stability, resulting in frequent equipment failures and affecting the continuous and stable operation of production.
A hydraulic jet reactor is adopted to set up an anhydride inlet, a circulating liquid inlet, an anhydride distributor and a circulating liquid nozzle. The reaction heat is taken away by uniform distribution of the liquid phase anhydride and the injection of the circulating liquid, preventing bumps, and simplifying the equipment structure and reducing costs.
It effectively prevents bumps in the reactor, improves the stability and sealing of the equipment, reduces the occurrence of equipment failures, reduces production costs, and simplifies the process.
Smart Images

Figure CN120022846A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the field of reactors, and in particular relates to an acid anhydride hydrolysis reactor and application thereof. Background Art
[0002] The hydrolysis equation of anhydride such as succinic anhydride is: CH 2 COOOCCH 2 +H 2 O=2(CH 2 COOH), the simple formula of anhydride is RCO-O-COR, which is an acid dehydration product. Anhydride has a strong water absorption, and it is easy to absorb water and return to the original acid form, so it is very easy to hydrolyze, and the hydrolysis process releases a large amount of heat. The water absorption process of anhydride is similar to sulfuric acid. When water is added to sulfuric acid, it will produce a boiling phenomenon, so the dilution process of sulfuric acid is to slowly drip sulfuric acid into water. To prevent boiling, the existing succinic anhydride hydrolysis reactor mainly adopts a stirring paddle reactor, and the liquid anhydride is passed into the reactor liquid phase, and the heat generated by the reaction is taken away by mechanical stirring to prevent the local temperature from being too high and boiling, and impacting the equipment. The existing stirring paddle reactor has a better mixing effect with a stirring paddle, but a complicated and expensive agitator structure must be used. The disadvantage of using a stirred reactor is that the agitator shaft must pass through the wall of the pressurized reactor, which has a high requirement for sealing. At the same time, it is affected by the rotation of the stirring shaft, and the reactor seal and the stirring paddle have a high stress effect. The stirring device is prone to equipment failure, which seriously affects the continuous and stable operation of production. Summary of the invention
[0003] In order to overcome the problems existing in the prior art, the present invention provides an anhydride hydrolysis reactor and its application. The present invention adopts a hydraulic injection reactor type and stipulates the position and nozzle type of the liquid anhydride entering the reactor, which can not only prevent the rapid reaction from boiling over, but also improve the stability of the equipment and avoid leakage problems, and greatly reduce the equipment cost and process complexity of the succinic acid device in industry.
[0004] On one hand, the present invention provides an anhydride hydrolysis reactor, on which an anhydride inlet, a circulating liquid inlet, an anhydride distributor and a circulating liquid nozzle are arranged, wherein the anhydride distributor is connected to the anhydride inlet through an anhydride introduction pipe, and the circulating liquid inlet is connected to the circulating liquid nozzle through a circulating liquid introduction pipe.
[0005] The anhydride inlet is arranged on the side of the reactor, and / or the anhydride distributor is arranged inside the reactor.
[0006] The acid anhydride distributor is in a ring-shaped, branch-shaped, square-shaped or other special-shaped structure. More preferably, a plurality of distribution holes are arranged on the acid anhydride distributor.
[0007] The distribution holes are evenly distributed at equal distances on the anhydride distributor, and are preferably arranged downward;
[0008] Preferably, the distribution holes include a connecting section, a transition section and a reinforcement section from top to bottom, the connecting section is a cylindrical barrel, the transition section is a conical boss 1 that is wide at the top and narrow at the bottom, and the reinforcement section is a conical boss 2 that is wide at the top and narrow at the bottom;
[0009] More preferably: the second conical boss is arranged to be inclined, preferably inclined toward the direction of the reactor wall.
[0010] The circulating liquid inlet is arranged at the top or upper part of the reactor, and the circulating liquid nozzle is arranged inside the reactor; preferably, the circulating liquid nozzle is arranged above the anhydride distributor.
[0011] A circulating liquid outlet is provided at the bottom or lower part of the reactor; preferably, the circulating liquid outlet is connected to the circulating liquid inlet via an external circulation pipeline on the outside of the reactor.
[0012] The circulating liquid nozzle is arranged below the liquid level of the reactor; preferably, the ratio of the distance between the circulating liquid nozzle and the top of the reactor to the inner diameter of the reactor is 0.4 to 0.75, preferably 0.45 to 0.6.
[0013] Assuming that the distance between the circulating liquid nozzle and the anhydride distributor is h, and the maximum width of the anhydride distributor is d, then h:d = α / e*(3π+1); wherein the circulation ratio α is the ratio of the volume of the external circulating reaction liquid to the volume of the reactor liquid phase per unit time, e≈2.7.
[0014] The circulating liquid nozzle is a cylinder with a hollow structure, which includes a connecting part, a flow guiding part and a spraying part from top to bottom.
[0015] The connecting part is in the shape of a hollow cylinder, wherein the hollow cavity is in the shape of a cylinder, and preferably a slot is provided on the outer side of the connecting part;
[0016] The diversion part is in the shape of a hollow cylinder, and a concave spiral line is arranged on the inner wall of the diversion part, and the end surface of the concave spiral line is in the shape of a curved triangle;
[0017] The injection part is hollow cylindrical, and the hollow cavity of the injection part is a deformed cylinder. The cross section of the upper end of the injection part is circular, and the cross section of the lower end is a curved triangle I (or Reuleaux triangle), and the upper end and the lower end are connected by a curved transition; further, the cross section at the middle position of the injection part is a curved triangle II. Preferably, the vertex side of the curved triangle I corresponds to the curve side of the curved triangle II.
[0018] Among them, this structure of the injection part can enhance the fine-scale mixing of the liquid outlet and reduce the large-scale regular flow. Therefore, this design can increase the jet Reynolds number and make the circulating liquid have a larger volume mass transfer coefficient when it is sprayed out. The rounded corner design of the Reuleaux triangle avoids the impact on the nozzle and prolongs the service life. It can also form a large shear surface to provide higher mass transfer efficiency for the mixing of circulating liquid and anhydride.
[0019] The second aspect of the present invention provides an anhydride hydrolysis reaction method, which is carried out using the anhydride hydrolysis reactor described in the first aspect of the present invention.
[0020] The third aspect of the present invention provides the use of the anhydride hydrolysis reactor described in the first aspect of the present invention in acid anhydride hydrolysis, especially in succinic anhydride hydrolysis.
[0021] The endpoints and any values of the scope disclosed in the present invention are not limited to the precise scope or value, and these scopes or values should be understood to include values close to these scopes or values. For numerical ranges, the endpoint values of each scope, the endpoint values of each scope and the individual point values, and the individual point values can be combined with each other to obtain one or more new numerical ranges, which should be regarded as specifically disclosed in this article. Hereinafter, in principle, each technical solution can be combined with each other to obtain a new technical solution, which should also be regarded as specifically disclosed in this article.
[0022] Compared with the prior art, the present invention has the following beneficial effects:
[0023] (1) The acid anhydride hydrolysis reactor of the present invention has a simple structure, does not require any moving equipment such as a stirring paddle, and can be processed using corrosion-resistant metals such as pickaxes and titanium;
[0024] (2) The anhydride hydrolysis reactor of the present invention limits the position and nozzle type of the liquid anhydride entering the reactor, which can not only prevent rapid boiling of the reaction, but also improve the stability of the equipment, avoid leakage problems, and greatly reduce the equipment cost and process complexity of the succinic acid device in industry. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] Figure 1 A schematic structural diagram of the anhydride hydrolysis reactor of the present invention is shown.
[0026] Figure 2 Show Figure 1 Schematic diagram of the cross section at AA in the middle.
[0027] Figure 3 Show Figure 2 The structural schematic diagram of the BB in the middle (i.e. the structural schematic diagram of the distribution holes).
[0028] Figure 4 A schematic axial cross-sectional view of an embodiment of the circulating fluid nozzle is shown.
[0029] Figure 5 A structural diagram showing an embodiment of the hollow cavity of the injection portion of the circulating liquid nozzle.
[0030] Figure 6 A cross-sectional view showing the upper, middle and lower ends of the spraying portion of the circulating liquid nozzle.
[0031] 1-circulating liquid inlet, 2-circulating liquid nozzle, 21-connecting part, 211-slot, 22-guiding part, 221, concave spiral line, 23-injection part, 3-anhydride inlet, 4-anhydride distributor, 41-connecting section, 42-transition section, 43-reinforcement section, 5-circulating liquid outlet, 6-liquid level in the reactor, H-distance between the upper and lower heads of the reactor tangent (TL), D-inner diameter of the reactor, d-maximum width of the anhydride distributor, l-distance between the circulating liquid nozzle and the top of the reactor, h-distance between the circulating liquid nozzle and the anhydride distributor. An external circulation pipeline connection is provided between the circulating liquid outlet 5 and the circulating liquid inlet 1 (not shown in the figure), and a circulating liquid introduction pipe (not shown in the figure) is provided between the circulating liquid inlet 1 and the circulating liquid nozzle 2.
[0032] In the reactor, the aspect ratio of the reactor is 1 to 1.8, preferably 1.1 to 1.45.
[0033] The anhydride inlet is arranged on the upper side or the upper middle side of the reactor, and the anhydride distributor is arranged inside the reactor at the same level as the anhydride inlet. Figure 2 The anhydride distributor is annular, branched, square or other special-shaped structures, and the ratio of the maximum width of the anhydride distributor to the inner diameter of the reactor is 0.2 to 0.8, preferably 0.33 to 0.67. The anhydride distributor is provided with 50 to 500, preferably 100 to 350 distribution holes, and the distribution holes (such as Figure 3 As shown) are evenly and equidistantly distributed on the anhydride distributor.
[0034] The inlet of the circulating liquid is arranged at the top or upper part of the reactor, and the circulating liquid nozzle is arranged inside the reactor and preferably above the anhydride distributor. A circulating liquid outlet is arranged at the bottom or lower part of the reactor, and the circulating liquid outlet is connected to the circulating liquid inlet through an external circulation pipeline. The circulating liquid nozzle is arranged below the liquid level of the reactor. The ratio of the distance (l) between the circulating liquid nozzle and the top of the reactor to the inner diameter (D) of the reactor is 0.4 to 0.75, preferably 0.45 to 0.6. Let the distance between the circulating liquid nozzle and the anhydride distributor be h, and the maximum width of the anhydride distributor be d, then h:d = α / e*(3π + 1); wherein, the circulation ratio α is the ratio of the volume of the external circulating reaction liquid to the volume of the liquid phase in the reactor per unit time.
[0035] The circulating liquid nozzle (as Figures 4-5 shown) includes a connecting part, a guiding part, and a spraying part. The circulating liquid nozzle is manufactured by machining a high-nickel chromium molybdenum-based alloy. The connecting part and the circulating liquid inlet pipe are double-connected by interference fitting and a clamping groove method; the hollow cavity of the connecting part is cylindrical; spiral lines are recessed on the inner wall of the guiding part, and the end face of the recessed spiral line is a curved-edge triangle (the cut part when looking at the cross-section is a curved-edge triangle), for example, it is obtained by machining the spiral line in the way of an end-face curved-edge triangle. The spraying part is a hollow cylinder, the cross-section of the upper end of the spraying part is circular, the cross-section of the lower end is a curved-surface triangle I (or Reuleaux triangle), and the upper end and the lower end are connected by a curved surface; further, the cross-section at the middle position of the spraying part is a curved-surface triangle II. Preferably, the vertex side of the curved-surface triangle I corresponds to the curved side of the curved-surface triangle II. Detailed implementation mode
[0036] The present invention will be described in detail below, and the features and advantages of the present invention will become clearer and more definite with these descriptions.
[0037] One of the purposes of the present invention is to provide an anhydride hydrolysis reactor, on which an anhydride inlet, a circulating liquid inlet, an anhydride distributor, and a circulating liquid nozzle are arranged. Among them, the anhydride distributor is connected to the anhydride inlet through an anhydride inlet pipe, and the circulating liquid inlet is connected to the circulating liquid nozzle through a circulating liquid inlet pipe.
[0038] The hydraulic jet reactor adopted by the present invention has a simple structure, no dynamic equipment such as stirring paddles, can be processed by corrosion-resistant metals such as zirconium materials and titanium materials, and the nozzle type can be a simple reduced-diameter pipe or other nozzle types that can endow the initial flow pattern to enhance the stirring effect.
[0039] In a preferred embodiment, the reactor has an aspect ratio of 1 to 1.8, preferably 1.1 to 1.45, for example 1, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7 or 1.8.
[0040] Among them, the "aspect ratio" of the present invention refers to Figure 1 The value of H / D in .
[0041] In a preferred embodiment, the anhydride inlet is arranged on the side (preferably the upper part or the upper middle part) of the reactor, and the anhydride distributor is arranged inside the reactor.
[0042] In a further preferred embodiment, the acid anhydride distributor is in a ring-shaped, branch-shaped, square-shaped or other special-shaped structure. Preferably, a plurality of distribution holes are provided on the acid anhydride distributor.
[0043] In a further preferred embodiment, the ratio of the maximum width of the anhydride distributor to the inner diameter of the reactor is 0.2 to 0.8, preferably 0.33 to 0.67, for example 0.2, 0.3, 0.4, 0.5, 0.6, 0.7 or 0.8.
[0044] Among them, when the acid anhydride distributor is ring-shaped, its maximum width refers to the diameter of the ring; when the acid anhydride distributor is square-shaped, its maximum width refers to the length of the diagonal of the square; when the acid anhydride distributor is branched or other special-shaped structures, its maximum width is the maximum distance from any end to any other end.
[0045] After a large number of experiments, the inventors found that if the maximum width of the anhydride distributor is too small, the number of openings will be reduced and the anhydride liquid phase feed amount will be too low; if the maximum width of the anhydride distributor is too large, the feed will be close to the reactor wall, the flow rate of the mixed liquid will be too slow, and the reaction heat cannot be quickly taken away, resulting in boiling.
[0046] In a preferred embodiment, the anhydride distributor is provided with 50 to 500 distribution holes, preferably 100 to 350 distribution holes, for example 50, 100, 150, 200, 250, 300, 350, 400, 450 or 500.
[0047] In a further preferred embodiment, the distribution holes are evenly distributed at equal intervals on the anhydride distributor, and are preferably arranged downward.
[0048] In a preferred embodiment, the distribution holes include a connecting section, a transition section and a reinforcement section from top to bottom, the connecting section is a cylindrical barrel, the transition section is a conical boss 1 that is wide at the top and narrow at the bottom, and the reinforcement section is a conical boss 2 that is wide at the top and narrow at the bottom.
[0049] In a further preferred embodiment, the semi-apex angle of the conical boss 1 is 10° to 20° (e.g., 10°, 12°, 14°, 16°, 18° or 20°), and / or the conical boss 2 is inclined, preferably inclined toward the direction of the reactor wall or inclined outward, more preferably inclined by 10° to 80° (e.g., Figure 3 The value θ shown can be any point value among 10°, 20°, 30°, 40°, 50°, 60°, 70°, 80°, or a range consisting of any two point values).
[0050] Here, θ also refers to the angle between the central axis of the second conical boss and the vertical direction. The first conical boss serves as a connecting transition, which can effectively compensate the opening equal area strength of the structure at the nozzle opening, and at the same time, can guide the distribution of the liquid anhydride.
[0051] In a preferred embodiment, the circulating liquid inlet is arranged at the top or upper part of the reactor, and the circulating liquid nozzle is arranged inside the reactor.
[0052] In a further preferred embodiment, the circulating liquid nozzle is arranged above the anhydride distributor.
[0053] In a preferred embodiment, a circulating liquid outlet is provided at the bottom or lower portion of the reactor.
[0054] In a further preferred embodiment, outside the reactor, the circulating liquid outlet and the circulating liquid inlet are connected via an external circulation pipeline.
[0055] In a preferred embodiment, the circulating liquid nozzle is disposed below the liquid level of the reactor.
[0056] Wherein, the circulating liquid nozzle is arranged below the liquid surface, and the reaction occurs in the liquid phase, which is conducive to heat removal and prevention of violent boiling.
[0057] In a further preferred embodiment, the ratio of the distance (l) between the circulating liquid nozzle and the top of the reactor to the inner diameter (D) of the reactor is 0.4 to 0.75, preferably 0.45 to 0.6, for example 0.4, 0.5, 0.6, 0.7 or 0.75.
[0058] The inventors found during a large number of experiments that a nozzle outlet position that is too high or too low cannot form a good stirring effect. The vortex formed at the nozzle outlet cannot suck in and drive the liquid in the entire reactor to form turbulence, which easily forms a dead zone.
[0059] In a preferred embodiment, assuming that the distance between the circulating liquid nozzle and the anhydride distributor is h, and the maximum width of the anhydride distributor is d, then h:d=α / e*(3π+1); wherein the circulation ratio α is the ratio of the volume of the external circulating reaction liquid to the volume of the reactor liquid phase per unit time.
[0060] In a preferred embodiment, the circulating liquid nozzle is a hollow structure, which includes a connection part (which can be as follows) from top to bottom. Figure 4 Structure shown), guide part and injection part.
[0061] In a further preferred embodiment, the connecting portion is in the shape of a hollow cylinder, and a slot is preferably provided on the outer side of the cylinder, wherein the connecting portion is connected by interference fit or by a slot, or is doubly connected by interference fit and a slot.
[0062] The circulating fluid nozzle is made of nickel-based alloy (nickel-based alloy includes stainless steel, nickel-chromium-molybdenum alloy, nickel-copper alloy, etc.), and is connected to the circulating fluid inlet pipe by interference fit or slot, or double connection by interference fit and slot, such as Figure 4 As shown, the left and right grooves of the connecting component are slot-fitted and overall interference-fitted.
[0063] In the present invention, the connection part of the circulating liquid nozzle is finely processed by a CNC machine tool (for example, a five-axis CNC machine tool). Before assembling the connection part, the connection part should be cooled by a low-temperature liquid nitrogen spray for a specified time (cooling time is 40 to 60 seconds), and the gap between the nozzle connection part and the circulating liquid inlet pipe should be adjusted to a degree that can be assembled, and then the rotation and locking are completed along the alignment to the card slot, and finally slowly restored to room temperature at a specified heating rate (preferably not more than 20 degrees Celsius per minute) to ensure the connection reliability of the connection part. This connection method can effectively reduce the thermal stress and deformation problems during welding connection, and improves the firmness and reliability of the connection compared to traditional threaded connections.
[0064] In a further preferred embodiment, the diversion part is in the shape of a hollow cylinder, and a recessed spiral line is arranged on the inner side of the cylinder, and the end face of the recessed spiral line is a curved triangle (the cut-off part when looking at the cross section is a curved triangle), for example, it is obtained by processing the spiral line with the end face curved triangle.
[0065] The curved triangle is also an arc triangle or a Reuleaux triangle. The spiral line of the inner wall of the nozzle used in the present invention plays an effective role in guiding the feed liquid. The spiral line processed on the inner wall can assist in guiding the liquid to generate a swirl flow, effectively overcome the viscosity caused by the surface tension of the liquid, and enable the liquid to reach the injection forming part of the nozzle with low resistance and high swirl flow.
[0066] In a further preferred embodiment, the injection part is hollow cylindrical, the cross section of the upper end of the injection part is circular, the cross section of the lower end is curved triangle I (or Reuleaux triangle), and the upper end and the lower end are connected by a curved transition. Further, the cross section at the middle position of the injection part is curved triangle II. Preferably, the vertex side of the curved triangle I corresponds to the curve side of the curved triangle II.
[0067] Wherein, the structure of the inner cavity of the injection part is as follows Figure 5 The cross section of the upper end, the middle part and the lower end of the injection part are shown in FIG. Figure 6 shown.
[0068] The acid anhydride hydrolysis reactor of the present invention has a simple structure. After the liquid acid anhydride enters the circulation flow field, the reaction heat can be quickly taken away, which reduces the risk of boiling, eliminates equipment damage caused by vibration, and ensures the smooth and continuous progress of the hydrolysis reaction.
[0069] In a preferred embodiment, an impact baffle is arranged below the interior of the reactor.
[0070] The second object of the present invention is to provide an acid anhydride hydrolysis reaction method, which is carried out using the acid anhydride hydrolysis reactor described in one of the objects of the present invention.
[0071] Among them, the use of it for anhydride hydrolysis reaction increases the reaction volume, realizes full liquid-liquid mixing in the reactor, eliminates the unstable factors caused by mechanical stirring, reduces the dead zone in the reactor, increases the effective reaction volume of the reactor, and has a simple structure and is safe and reliable. The application of this reactor in engineering can greatly reduce the cost of the reactor, increase the continuous operation time of the reactor, expand the volume of a single reactor, and provide the possibility for scale expansion.
[0072] The third object of the present invention is to provide the use of the reactor described in the first object of the present invention in the hydrolysis of succinic anhydride.
[0073] Among them, the use of the reactor for succinic acid hydrolysis reaction increases the reaction volume, realizes sufficient liquid-liquid mixing in the reactor, eliminates the unstable factors caused by mechanical stirring, reduces the dead zone in the reactor, increases the effective reaction volume of the reactor, and has a simple structure and is safe and reliable. The application of this reactor in engineering can greatly reduce the cost of the reactor, increase the continuous operation time of the reactor, expand the volume of a single reactor, and provide the possibility for scale expansion.
[0074] Example
[0075] The present invention is described in detail below in conjunction with specific embodiments. It is necessary to point out that the following embodiments are only used to further illustrate the present invention and cannot be understood as limiting the scope of protection of the present invention. Some non-essential improvements and adjustments made to the present invention by those skilled in the art based on the contents of the present invention still fall within the scope of protection of the present invention.
[0076] It should also be noted that the various specific technical features described in the following specific embodiments can be combined in any suitable manner without contradiction. To avoid unnecessary repetition, the present invention will not further describe various possible combinations.
[0077] In addition, the various embodiments of the present invention may be arbitrarily combined as long as they do not violate the concept of the present invention. The technical solutions thus formed belong to part of the original disclosure of this specification and also fall within the protection scope of the present invention.
[0078] The raw materials used in the examples and comparative examples, unless otherwise specified, are disclosed in the prior art, for example, they can be directly purchased or prepared according to the preparation methods disclosed in the prior art.
[0079] [Example 1]
[0080] use Figure 1 The reactor shown uses Figures 2-3 The anhydride distributor and Figures 4 to 6 The circulating liquid nozzle shown is used for hydrolysis of succinic anhydride.
[0081] In the reactor, the distance H between tangent lines (TL) of the reactor was 5000 mm, and the inner diameter D was 4000 mm.
[0082] The anhydride inlet is arranged on the upper side of the reactor, and the anhydride distributor is arranged inside the reactor at the same level as the anhydride inlet. The anhydride distributor is annular, and the ratio of the diameter of the annular to the inner diameter of the reactor is 0.5. The anhydride distributor is provided with 200 distribution holes, and the distribution holes are evenly distributed at equal intervals on the anhydride distributor. The distribution holes on the anhydride distributor are arranged downward, and the distribution holes include a connecting section, a transition section and a reinforcement section from top to bottom. The connecting section is a cylindrical barrel, the transition section is a conical boss 1 that is wide at the top and narrow at the bottom, and the reinforcement section is a conical boss 2 that is wide at the top and narrow at the bottom; the semi-apex angle of the conical boss 1 is 10°, and the conical boss 2 is inclined outward, and the inclination angle θ is 30°.
[0083] The circulating liquid inlet is arranged at the top of the reactor, and the circulating liquid nozzle is arranged inside the reactor and above the anhydride distributor. A circulating liquid outlet is arranged at the bottom of the reactor, and the circulating liquid outlet is connected to the circulating liquid inlet through an external circulation pipeline. The circulating liquid nozzle is arranged below the liquid level of the reactor. The distance l between the circulating liquid nozzle and the top of the reactor is 2000 mm, the distance h between the circulating liquid nozzle and the anhydride distributor is 700 mm, and the circulation ratio α≈10.
[0084] The circulating liquid nozzle includes a connecting part, a guide part, and an injection part. The circulating liquid nozzle is made of high nickel-chromium-molybdenum-based alloy, and is doubly connected to the preceding nozzle by interference fitting and slotting. The guide part is a spiral structure, and the end face of the spiral structure is a curved triangle (the part cut off when looking at the cross section is a curved triangle). It is obtained by processing the spiral with the end face curved triangle. The injection part is a hollow cylinder, and the cross-section of the upper end of the injection part is circular, and the cross-section of the lower end is a curved triangle I (or Reuleaux triangle), and the upper end and the lower end are connected by a curved transition; further, the cross-section at the middle position of the injection part is a curved triangle II. Preferably, the vertex side of the curved triangle I corresponds to the curve side of the curved triangle II.
[0085] The reactor is used in the hydrolysis of acid anhydride: the molar ratio of succinic anhydride liquid to water (added in the circulating liquid) is 1:3, with water in excess. The reaction is carried out at 60°C and normal pressure to hydrolyze to generate succinic acid. The succinic anhydride conversion rate is 100% when the reactor is used for the reaction. The reaction heat is removed by the external circulation of the circulating liquid. No bumping occurs at the inlet of the liquid succinic anhydride, and the expected effect can be achieved.
[0086] [Example 2]
[0087] use Figure 1 The reactor shown uses Figure 2 The anhydride distributor shown is used to hydrolyze succinic anhydride.
[0088] In the reactor, the height H of the reactor is 6000 mm and the inner diameter D is 4500 mm.
[0089] The anhydride inlet is arranged on the upper side of the reactor, and the anhydride distributor is arranged inside the reactor at the same level as the anhydride inlet. The anhydride distributor is annular, and the ratio of the diameter of the annular to the inner diameter of the reactor is 0.6. The anhydride distributor is provided with 350 distribution holes, and the distribution holes are evenly distributed at equal intervals on the anhydride distributor. The distribution holes on the anhydride distributor are arranged downward, and the distribution holes include a connecting section, a transition section and a reinforcement section from top to bottom. The connecting section is a cylindrical barrel, the transition section is a conical boss 1 that is wide at the top and narrow at the bottom, and the reinforcement section is a conical boss 2 that is wide at the top and narrow at the bottom; the semi-apex angle of the conical boss 1 is 18°, and the conical boss 2 is inclined outward, and the inclination angle θ is 60°.
[0090] The circulating liquid inlet is arranged at the top of the reactor, and the circulating liquid nozzle is arranged inside the reactor and above the anhydride distributor. A circulating liquid outlet is arranged at the bottom of the reactor, and the circulating liquid outlet is connected to the circulating liquid inlet through an external circulation pipeline. The circulating liquid nozzle is arranged below the liquid level of the reactor. The distance l between the circulating liquid nozzle and the top of the reactor is 2700 mm, the distance h between the circulating liquid nozzle and the anhydride distributor is 950 mm, and the circulation ratio α≈10.
[0091] The circulating liquid nozzle includes a connecting part, a guide part, and an injection part. The circulating liquid nozzle is made of high nickel-chromium-molybdenum-based alloy, and is doubly connected to the preceding nozzle by interference fitting and slotting. The guide part is a spiral structure, and the end face of the spiral structure is a curved triangle (the part cut off when looking at the cross section is a curved triangle). It is obtained by processing the spiral with the end face curved triangle. The injection part is a hollow cylinder, and the cross-section of the upper end of the injection part is circular, and the cross-section of the lower end is a curved triangle I (or Reuleaux triangle), and the upper end and the lower end are connected by a curved transition; further, the cross-section at the middle position of the injection part is a curved triangle II. Preferably, the vertex side of the curved triangle I corresponds to the curve side of the curved triangle II.
[0092] The reactor is used in the hydrolysis of acid anhydride: the molar ratio of succinic anhydride liquid to water (added in the circulating liquid) is 1:3, with water in excess. The reaction is carried out at 60°C and normal pressure to hydrolyze to generate succinic acid. The succinic anhydride conversion rate is 100% when the reactor is used for the reaction. The reaction heat is removed by the external circulation of the circulating liquid. No bumping occurs at the inlet of the liquid succinic anhydride, and the expected effect can be achieved.
[0093] [Example 3]
[0094] use Figure 1 The reactor shown uses Figure 2 The anhydride distributor shown is used to hydrolyze succinic anhydride.
[0095] In the reactor, the height H of the reactor is 4500 mm and the inner diameter D is 4000 mm.
[0096] The anhydride inlet is arranged on the upper side of the reactor, and the anhydride distributor is arranged inside the reactor at the same level as the anhydride inlet. The anhydride distributor is annular, and the ratio of the diameter of the annular to the inner diameter of the reactor is 0.4. The anhydride distributor is provided with 150 distribution holes, and the distribution holes are evenly distributed at equal intervals on the anhydride distributor. The distribution holes on the anhydride distributor are arranged downward, and the distribution holes include a connecting section, a transition section and a reinforcement section from top to bottom. The connecting section is a cylindrical barrel, the transition section is a conical boss 1 that is wide at the top and narrow at the bottom, and the reinforcement section is a conical boss 2 that is wide at the top and narrow at the bottom; the semi-apex angle of the conical boss 1 is 15°, and the conical boss 2 is inclined outward, and the inclination angle θ is 40°.
[0097] The circulating liquid inlet is arranged at the top of the reactor, and the circulating liquid nozzle is arranged inside the reactor and above the anhydride distributor. A circulating liquid outlet is arranged at the bottom of the reactor, and the circulating liquid outlet is connected to the circulating liquid inlet through an external circulation pipeline. The circulating liquid nozzle is arranged below the liquid level of the reactor. The distance l between the circulating liquid nozzle and the top of the reactor is 1800 mm, the distance h between the circulating liquid nozzle and the anhydride distributor is 550 mm, and the circulation ratio α≈10.
[0098] The circulating liquid nozzle includes a connecting part, a guide part, and an injection part. The circulating liquid nozzle is made of high nickel-chromium-molybdenum-based alloy, and is doubly connected to the preceding nozzle by interference fitting and slotting. The guide part is a spiral structure, and the end face of the spiral structure is a curved triangle (the part cut off when looking at the cross section is a curved triangle). It is obtained by processing the spiral with the end face curved triangle. The injection part is a hollow cylinder, and the cross-section of the upper end of the injection part is circular, and the cross-section of the lower end is a curved triangle I (or Reuleaux triangle), and the upper end and the lower end are connected by a curved transition; further, the cross-section at the middle position of the injection part is a curved triangle II. Preferably, the vertex side of the curved triangle I corresponds to the curve side of the curved triangle II.
[0099] The reactor is used in the hydrolysis of acid anhydride: the molar ratio of succinic anhydride liquid to water (added in the circulating liquid) is 1:3, with water in excess. The reaction is carried out at 60°C and normal pressure to hydrolyze to generate succinic acid. The succinic anhydride conversion rate is 100% when the reactor is used for the reaction. The reaction heat is removed by the external circulation of the circulating liquid. No bumping occurs at the inlet of the liquid succinic anhydride, and the expected effect can be achieved.
[0100] The present invention has been described in detail above in conjunction with specific implementations and exemplary examples, but these descriptions cannot be understood as limiting the present invention. Those skilled in the art understand that, without departing from the spirit and scope of the present invention, a variety of equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its implementation methods, all of which fall within the scope of the present invention. The scope of protection of the present invention shall be subject to the attached claims.
Claims
1. An anhydride hydrolysis reactor, wherein an anhydride inlet, a circulating liquid inlet, an anhydride distributor and a circulating liquid nozzle are provided on the reactor, in, The acid anhydride distributor is connected to the acid anhydride inlet through an acid anhydride introduction pipe, and the circulating liquid inlet is connected to the circulating liquid nozzle through a circulating liquid introduction pipe.
2. The anhydride hydrolysis reactor according to claim 1, It is characterized in that The anhydride inlet is arranged on the side of the reactor, and / or the anhydride distributor is arranged inside the reactor.
3. The anhydride hydrolysis reactor according to claim 2, It is characterized in that Preferably, the acid anhydride distributor is in a ring-shaped, branched, square or other special-shaped structure. More preferably, a plurality of distribution holes are provided on the acid anhydride distributor.
4. The anhydride hydrolysis reactor according to claim 3, It is characterized in that The distribution holes are evenly distributed at equal distances on the anhydride distributor, and are preferably arranged downward; Preferably, the distribution holes include a connecting section, a transition section and a reinforcement section from top to bottom, the connecting section is a cylindrical barrel, the transition section is a conical boss 1 that is wide at the top and narrow at the bottom, and the reinforcement section is a conical boss 2 that is wide at the top and narrow at the bottom; More preferably: the second conical boss is tilted, preferably tilted toward the reactor wall.
5. The anhydride hydrolysis reactor according to claim 1, It is characterized in that The circulating liquid inlet is arranged at the top or upper part of the reactor, and the circulating liquid nozzle is arranged inside the reactor; preferably, the circulating liquid nozzle is arranged above the anhydride distributor.
6. The anhydride hydrolysis reactor according to claim 1, It is characterized in that A circulating liquid outlet is provided at the bottom or lower part of the reactor; preferably, the circulating liquid outlet is connected to the circulating liquid inlet via an external circulation pipeline on the outside of the reactor.
7. The anhydride hydrolysis reactor according to claim 1, It is characterized in that The circulating liquid nozzle is arranged below the liquid level of the reactor; preferably, the ratio of the distance between the circulating liquid nozzle and the top of the reactor to the inner diameter of the reactor is 0.4 to 0.75, preferably 0.45 to 0.
6.
8. The anhydride hydrolysis reactor according to claim 1, It is characterized in that Assuming that the distance between the circulating liquid nozzle and the anhydride distributor is h, and the maximum width of the anhydride distributor is d, then h:d=α / e*(3π+1); wherein the circulation ratio α is the ratio of the volume of the external circulating reaction liquid to the volume of the reactor liquid phase per unit time.
9. The anhydride hydrolysis reactor according to any one of claims 1 to 8, It is characterized in that The circulating liquid nozzle is a cylinder with a hollow structure, which includes a connecting part, a flow guiding part and a spraying part from top to bottom.
10. The anhydride hydrolysis reactor according to claim 9, It is characterized in that The connecting portion is in the shape of a hollow cylinder, and preferably a slot is provided on the outer side of the cylinder; and / or, The diversion part is in the shape of a hollow cylinder, a concave spiral line is arranged on the inner side of the cylinder, and the end surface of the concave spiral line is in the shape of a curved triangle; and / or, The injection part is in the shape of a hollow cylinder, the cross section of the upper end of the injection part is circular, the cross section of the lower end is a curved triangle I, and the upper end and the lower end are connected by a curved transition.
11. A method for anhydride hydrolysis reaction, which is carried out using the anhydride hydrolysis reactor according to any one of claims 1 to 10.
12. Use of the reactor according to any one of claims 1 to 10 in the hydrolysis of succinic anhydride.