A reaction device for producing ultra-pure hydroxylamine solution

Abstract

The utility model relates to the technical field of ultrapure hydroxylamine solution production, specifically to a reaction unit for ultrapure hydroxylamine solution production, which comprises a reaction kettle, a feed inlet is formed in the top of the reaction kettle, a discharge port is formed in the bottom of the reaction kettle, a jacket is installed on the outer wall of the reaction kettle, a cold and hot exchange port is formed in the outer wall of the jacket, a motor is fixedly installed on the top of the reaction kettle, and a rotating rod is fixedly installed at the output end of the motor. The utility model is provided with a large scraper, which can scrape off the residual materials on the inner wall of the reaction kettle. After the contact rod moves downward and the spring plate resets upward, axial upward and downward movement is formed, the residual materials on the kettle wall are completely scraped off, the uniformity of material mixing is further ensured, contamination in the kettle is prevented, the risk of cross contamination caused by material retention is avoided from the root, the equipment cleaning process is simplified, and the production continuity and product batch consistency are improved.

Description

Technical Field

[0001] This utility model relates to the field of ultrapure hydroxylamine solution production technology, specifically a reaction device for the production of ultrapure hydroxylamine solution. Background Technology

[0002] Ultrapure hydroxylamine solution is a key material in the fields of electronics and semiconductor manufacturing, widely used in applications such as chip photoresist stripping and semiconductor device cleaning. Its purity directly affects the performance and reliability of the final product, typically requiring impurity content below ppm, with high-end applications requiring ppb. The reaction vessel is the core equipment for the production of ultrapure hydroxylamine solution, responsible for supporting the synthesis reaction, controlling reaction conditions, and ensuring product purity. It is a crucial carrier for achieving raw material conversion, suppressing side reactions, and preventing the introduction of impurities.

[0003] However, existing reactors used for the production of ultrapure hydroxylamine solutions have several problems in practical applications: the raw materials contain both solid and powdered components, and clumping occurs when these three components are mixed. Furthermore, the stirring device inside the reactor lacks an effective internal cleaning and scraping structure, leading to easy material adhesion and residue buildup, making cleaning difficult and increasing the risk of batch-to-batch cross-contamination. Therefore, we propose a reactor for the production of ultrapure hydroxylamine solutions. Utility Model Content

[0004] The purpose of this invention is to solve the problem of adhesion to the inner wall and to provide a reaction device for the production of ultrapure hydroxylamine solution.

[0005] To achieve the above objectives, this utility model provides the following technical solution:

[0006] A reaction apparatus for producing ultrapure hydroxylamine solution includes a reaction vessel with a feed inlet at the top and a discharge outlet at the bottom. A jacket is installed on the outer wall of the reaction vessel, and a heat exchange port is provided on the outer wall of the jacket. A motor is fixedly installed on the top of the reaction vessel, and a rotating rod is fixedly installed on the output end of the motor. A large stirring rod and a small stirring rod are respectively fixedly installed on the outer wall of the bottom and middle ends of the rotating rod. A drain outlet is provided on the outer wall of the discharge outlet. The outer walls of both sides of the large stirring rod parallel to the inner wall of the reaction vessel are... The reactor has a chute. A flow-slowing plate is fixedly installed on the top surface of the inner wall of the reactor. A rotating rod is installed through and rotatably on the top of the flow-slowing plate. A contact rod is slidably installed through the top surfaces of the large and small stirring rods. A sliding rod is slidably installed on the inner wall of the chute. A connecting block is fixedly installed on the outer wall of the sliding rod. A large scraper is fixedly installed on the outer wall of the connecting block near the inner wall of the reactor. A spring is provided between the bottom end of the chute and the sliding rod. Several arc-shaped blocks are fixedly installed on the outer side of the bottom surface of the flow-slowing plate. A small scraper is fixedly installed on the bottom end of the large stirring rod.

[0007] Preferably, the flow-slowing plate is tapered, the top of the abutment rod is an isosceles triangle, the sliding rod is fixedly connected to the bottom of the abutment rod, the number of connecting blocks is several, and three connecting blocks form a group. Each group of connecting blocks is slidably installed on the outer wall of one end of the large stirring rod parallel to the inner wall of the reactor. The radius of the arc surface of the arc block is adapted to the radius of the movement trajectory of the triangular end of the abutment rod.

[0008] Preferably, the large scraper and the small scraper are in contact with the inner side wall and the inner bottom wall of the reactor, respectively, and the large scraper and the small scraper are adapted to the inner side wall and the inner bottom wall of the reactor.

[0009] Preferably, the discharge port is fixedly connected to an external ultrapure leak-free shut-off valve, and the discharge port has a flow channel inside that connects the drain port and the cavity of the jacket.

[0010] Preferably, the components inside the reactor that directly or indirectly contact the raw materials or the crude hydroxylamine solution produced after the reaction include a rotating rod, a large stirring rod, a small stirring rod, a flow buffer, a contact rod, a sliding rod, a connecting block, a large scraper, a spring, an arc-shaped block, and a small scraper. The main body material of the above components is TA pure titanium or PFA material, and the purity is ≥99.95%. The scraping surfaces of the large scraper and the small scraper and the end faces that contact the material are all coated with perfluoroethylene propylene coating, and the coating is free of pinholes and cracks.

[0011] By employing the above technical solution, this utility model provides a reaction apparatus for the production of ultrapure hydroxylamine solution. Its beneficial effects are: The large scraper removes residual material from the inner wall of the reactor. Furthermore, the downward movement of the contact rod and the upward repositioning of the spring plate create axial up-and-down movement, thoroughly scraping away residual material from the reactor wall. This further ensures the uniformity of material mixing, prevents contamination inside the reactor, and fundamentally avoids the risk of cross-contamination caused by material retention. It also simplifies the equipment cleaning process and improves production continuity and batch consistency. Attached Figure Description

[0012] The accompanying drawings, which are included to provide a further understanding of the present invention, form part of this application:

[0013] Figure 1 This is a front view schematic diagram of the overall structure of this utility model;

[0014] Figure 2 This is a bottom view of the overall structure of this utility model;

[0015] Figure 3 This is a cross-sectional view of Embodiment 1;

[0016] Figure 4 This is an enlarged schematic diagram of point A in this embodiment.

[0017] In the diagram: 1. Reactor; 2. Inlet; 3. Outlet; 4. Jacket; 401. Heat exchange port; 402. Drain port; 5. Motor; 6. Rotary rod; 7. Large stirring rod; 71. Slide chute; 8. Small stirring rod; 9. Flow buffer; 10. Abutment rod; 11. Slide rod; 12. Connecting block; 13. Large scraper; 14. Spring; 15. Arc-shaped block; 16. Small scraper. Detailed Implementation

[0018] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0019] Example 1

[0020] A reaction apparatus for the production of ultrapure hydroxylamine solution, such as Figures 1-4 As shown, the reactor includes a reactor 1, with a feed inlet 2 at the top and a discharge outlet 3 at the bottom. A jacket 4 is installed on the outer wall of the reactor 1, and a heat exchange port 401 is located on the outer wall of the jacket 4. A motor 5 is fixedly installed on the top of the reactor 1, and a rotating rod 6 is fixedly installed at the output end of the motor 5. A large stirring rod 7 and a small stirring rod 8 are fixedly installed on the outer wall of the bottom and middle ends of the rotating rod 6, respectively. A drain outlet 402 is located on the outer wall of the discharge outlet 3. Sliding grooves 71 are located on both sides of the outer wall of the large stirring rod 7, which is parallel to the inner wall of the reactor 1. A flow-retarding plate 9 is fixedly installed on the top surface of the reactor 1, and a rotating rod 6 is installed through and rotatably on the top of the flow-retarding plate 9. A contact rod 10 is slidably installed through the top surfaces of the large stirring rod 7 and the small stirring rod 8. A sliding rod 11 is slidably installed on the inner wall of the trough 71. A connecting block 12 is fixedly installed on the outer wall of the sliding rod 11. A large scraper 13 is fixedly installed on the outer wall of the connecting block 12 near the inner wall of the reactor 1. A spring piece 14 is provided between the bottom end of the trough 71 and the sliding rod 11. Several arc-shaped blocks 15 are fixedly installed on the outer side of the bottom surface of the flow-retarding plate 9. A small scraper 16 is fixedly installed on the bottom end of the large stirring rod 7.

[0021] The flow-slowing plate 9 is tapered, the top of the contact rod 10 is an isosceles triangle, the slide rod 11 is fixedly connected to the bottom of the contact rod 10, there are several connecting blocks 12, and three connecting blocks 12 form a group. Each group of connecting blocks 12 is slidably installed on the outer wall of one end of the large stirring rod 7 parallel to the inner wall of the reactor 1. The radius of the arc surface of the arc block 15 is adapted to the radius of the movement trajectory of the triangular end of the contact rod 10.

[0022] The large scraper 13 and the small scraper 16 are in contact with the inner side wall and the inner bottom wall of the reactor 1, respectively, and the large scraper 13 and the small scraper 16 are adapted to the inner side wall and the inner bottom wall of the reactor 1.

[0023] The discharge port 3 is fixedly connected to an external ultrapure leak-free shut-off valve, and the discharge port 3 has a flow channel inside that connects the cavity of the drain port 402 and the jacket 4.

[0024] The components inside the reactor 1 that directly or indirectly contact the raw materials or the crude hydroxylamine solution produced after the reaction include a rotating rod 6, a large stirring rod 7, a small stirring rod 8, a flow-retarding plate 9, a contact rod 10, a sliding rod 11, a connecting block 12, a large scraper 13, a spring sheet 14, an arc-shaped block 15, and a small scraper 16. The main body material of the above components is TA2 pure titanium or PFA material, and the purity is ≥99.95%. The scraping surfaces of the large scraper 13 and the end faces that contact the material are all coated with perfluoroethylene propylene coating, and the coating is free of pinholes and cracks.

[0025] This invention relates to a reaction apparatus for producing ultrapure hydroxylamine solution. In operation, high-purity ketones, solid hydroxylamine salts, ultrapure water, and catalysts are added through inlet 2. The flow-damping plate 9 prevents liquid raw materials from impacting the bottom of the vessel and damaging the inner wall. After the raw materials are added, heat transfer oil (for heating) or chilled brine (for cooling) is introduced through the heat exchange port 401 of the jacket 4. The medium forms a covering cooling effect within the annular chamber of the jacket 4, and then is discharged through the drain port 402, achieving precise temperature control within the vessel.

[0026] When it is necessary to mix the raw materials, the motor 5 is turned on. The output end of the motor 5 drives the rotating rod 6 to rotate. The rotating rod 6 drives the large stirring rod 7 and the small stirring rod 8 to rotate in a circle, and the large stirring rod 7 and the small stirring rod 8 mix the raw materials. When the large stirring rod 7 rotates, it will drive the sliding rod 11, the contact rod 10 and the small scraper 16 at the bottom of the sliding groove 71 to rotate. The sliding rod 11 drives the connecting block 12 to rotate, which in turn causes the large scraper 13 to rotate along the inner wall of the pot. The isosceles triangle on the contact rod 10 will contact the arc-shaped block 15 at the bottom of the flow buffer 9 on the path of rotation. The isosceles triangle on the contact rod 10 will move downward along the arc surface of the arc block 15. The downward movement of the contact rod 10 will drive the slide rod 11 to move downward. The slide rod 11 will drive the connecting block 12 to move downward. At the same time, the slide rod 11 will compress the bottom spring piece 14 downward. The connecting block 12 will drive the large scraper 13 to move downward. After the isosceles triangle on the contact rod 10 passes the vertex of the arc surface of the arc block 15, the elasticity of the bottom spring piece 14 will cause the slide rod 11 to return to its original position. The large scraper 13 will also slide upward. By using the large scraper 13, residual materials on the inner wall of the reactor 1 are scraped off. The downward movement of the contact rod 10 and the upward reset of the spring 14 create an axial up-and-down movement, thoroughly scraping off residual materials from the reactor wall. This further ensures the uniformity of material mixing, prevents contamination inside the reactor, and avoids the risk of cross-contamination caused by material retention at the source. It also simplifies the equipment cleaning process and improves production continuity and product batch consistency.

[0027] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0028] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A reaction apparatus for producing ultrapure hydroxylamine solution, comprising a reaction vessel (1), wherein a feed inlet (2) is provided at the top of the reaction vessel (1), a discharge outlet (3) is provided at the bottom of the reaction vessel (1), a jacket (4) is installed on the outer wall of the reaction vessel (1), a heat exchange port (401) is provided on the outer wall of the jacket (4), a motor (5) is fixedly installed at the top of the reaction vessel (1), a rotating rod (6) is fixedly installed at the output end of the motor (5), and a large stirring rod (7) and a small stirring rod (8) are fixedly installed on the outer wall of the bottom and middle ends of the rotating rod (6), respectively, characterized in that: The outer wall of the discharge port (3) is provided with a drain port (402). The outer walls of both sides of the large stirring rod (7) parallel to the inner wall of the reactor (1) are provided with sliding grooves (71). The top surface of the inner wall of the reactor (1) is fixedly installed with a flow-slowing plate (9), and the rotating rod (6) is installed through and rotatably on the top of the flow-slowing plate (9). The top surfaces of the large stirring rod (7) and the small stirring rod (8) are slidably installed with abutment rods (10). The inner surface of the sliding groove (71) is provided with a drain port (402). A sliding rod (11) is slidably installed on the wall. A connecting block (12) is fixedly installed on the outer wall of the sliding rod (11). A large scraper (13) is fixedly installed on the outer wall of the connecting block (12) near the inner wall of the reactor (1). A spring piece (14) is provided between the bottom end of the sliding groove (71) and the sliding rod (11). Several arc-shaped blocks (15) are fixedly installed on the outer side of the bottom surface of the slow flow plate (9). A small scraper (16) is fixedly installed on the bottom end of the large stirring rod (7).

2. The reaction apparatus for producing ultrapure hydroxylamine solution according to claim 1, characterized in that: The slow-flow plate (9) is tapered, the top of the contact rod (10) is an isosceles triangle, the slide rod (11) is fixedly connected to the bottom of the contact rod (10), the number of connecting blocks (12) is several, and three connecting blocks (12) form a group. Each group of connecting blocks (12) is slidably installed on the outer wall of one end of the large stirring rod (7) parallel to the inner wall of the reactor (1). The radius of the arc surface of the arc block (15) is adapted to the radius of the movement trajectory of the triangular end of the contact rod (10).

3. The reaction apparatus for producing ultrapure hydroxylamine solution according to claim 1, characterized in that: The large scraper (13) and the small scraper (16) are in contact with the inner side wall and the inner bottom wall of the reactor (1), respectively, and the large scraper (13) and the small scraper (16) are adapted to the inner side wall and the inner bottom wall of the reactor (1).

4. The reaction apparatus for producing ultrapure hydroxylamine solution according to claim 1, characterized in that: The discharge port (3) is fixedly connected to an external ultrapure leak-free shut-off valve. The discharge port (3) has a flow channel inside that connects the drain port (402) and the jacket (4).

5. The reaction apparatus for producing ultrapure hydroxylamine solution according to claim 4, characterized in that: The components inside the reactor (1) that directly or indirectly contact the raw materials or the crude hydroxylamine solution produced after the reaction include a rotating rod (6), a large stirring rod (7), a small stirring rod (8), a slowing plate (9), a contact rod (10), a sliding rod (11), a connecting block (12), a large scraper (13), a spring (14), an arc block (15), and a small scraper (16). The main body material of the above components is TA2 pure titanium or PFA material, and the purity is ≥99.95%. The scraping surface of the large scraper (13) and the end face that contacts the material are covered with perfluoroethylene propylene coating, and the coating is free of pinholes and cracks.

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