A polycarboxylate water reducer synthesis reactor
By adopting an arc-shaped drop distributor and a three-layer stirring blade structure in the polycarboxylate water-reducing agent synthesis reactor, combined with intelligent control technology, the problem of gel polymer production in traditional stirring and drop addition methods is solved, achieving a more efficient and safe production process and high-quality product performance.
Patent Information
- Application Number
- CN202211211150.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-09-30
- Publication Date
- 2025-09-26
- Estimated Expiration
- 2042-09-30
AI Technical Summary
Traditional stirring and dripping methods cannot meet the requirements of polycarboxylic acid water-reducing agent mother liquor synthesis, resulting in the production of gel polymer substances, affecting product performance and reducing production efficiency, while also posing safety and environmental risks.
A polycarboxylate superplasticizer synthesis reactor is designed. It adopts an arc-shaped drop distributor and a three-layer stirring blade structure. Combined with intelligent control technology, it ensures uniform distribution of the added material and avoids polymerization reaction. The telescopic movement of the upper stirring blade is controlled by a liquid level detector to achieve sufficient stirring.
The production efficiency and product performance of polycarboxylate water-reducing agent mother liquor are improved, safety and environmental protection risks are reduced, and a safer and more efficient production process is achieved.
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Figure CN115779824B_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of building material production processes and equipment, and relates to a stirring and dripping device for a polycarboxylate water-reducing agent mother liquor synthesis process. More specifically, the present invention relates to a polycarboxylate water-reducing agent synthesis reactor. Background Art
[0002] As the latest generation of chemical admixtures for concrete, polycarboxylate water reducer features low dosage, high water reduction rate, minimal collapse, excellent durability, and extremely low content of harmful substances. It possesses comprehensive technical performance advantages and environmentally friendly features that meet the requirements of modern construction projects. It not only greatly improves the mechanical properties of high-strength concrete, but also simplifies and facilitates construction processes. It has become one of the important products for commercial concrete and new building materials both domestically and internationally.
[0003] Due to the excellent application performance and molecular designability of polycarboxylate superplasticizers, the preparation and synthesis process utilizes macromolecular compounds with sulfonic acid, carboxyl, amino, and polyoxyethylene side chains. These compounds are synthesized via free radical copolymerization in aqueous solution or in a melt, creating a high-molecular-weight surfactant with a comb-like structure. The chemical substances used all possess high activity and high valence unsaturation. During the mother liquor synthesis process for polycarboxylate superplasticizers, primers, work units, redox systems, and chain transfer agents are typically designed and added individually, either dropwise or in a controlled manner, to effectively control the polymerization rate and molecular weight, thereby achieving the desired performance of the polycarboxylate superplasticizer.
[0004] However, with the in-depth research on the synthesis technology and application performance of polycarboxylate water-reducing agent mother liquor, the selection of polyether monomers, functional monomers and catalytic reducing agents has become more extensive, the activity is higher, and the catalytic reaction is faster. While improving production efficiency and reducing production costs, further improving the actual application performance of polycarboxylate water-reducing agent mother liquor is the core of competition. The reaction temperature system of polycarboxylate water-reducing agent mother liquor synthesis has evolved from high temperature to room temperature and then to the current low temperature.
[0005] Traditional stirring and dripping methods cannot meet the needs, resulting in the appearance of a large amount of gel polymer substances during the stirring and dripping process, which not only affects product performance but also reduces the production efficiency of the reactor; and the gel polymer substances need to be manually cleaned, so there is a greater safety and environmental risk.
[0006] During the synthesis of the polycarboxylate water-reducing agent mother liquor, the chemical synthesis reaction is carried out in a reactor with an internal double coil. The stirring method is a three-layer fixed paddle stirring method. The small reaction materials are added dropwise using three (A, B, and C material dropping ports). Usually, the three dropping ports are designed in a single-tube design side by side on the top of the reactor.
[0007] When synthesizing the polycarboxylate water-reducing agent mother liquor, open the internal and external circulation coils to increase or decrease the temperature; start the stirring equipment to stir; polyoxyethylene polyether and the like are dissolved and configured to form a bottom material that reaches about 2 / 3 of the volume in the kettle (without touching the upper stirring blades); after the temperature reaches the control requirement, start the fixed-frequency dropwise addition of the three materials A, B, and C at the same time.
[0008] Among them, the dropwise added material A is a solution containing a highly active double bond mixture (such as acrylic acid, hydroxyethyl acrylate, etc.), B is a chain transfer agent solution, and material C is a reducing agent solution (such as VC, etc.).
[0009] During the dropwise addition process for a period of time (1-2 hours), since the A, B, and C dropping ports are placed side by side and concentrated, under the action of the airflow in the kettle, the A, B, and C materials partially come into contact and undergo polymerization reaction;
[0010] On the other hand, because the upper stirring blades are not covered by the bottom material, materials A, B, and C will drip onto the rotating stirring blades or be scattered onto the coils in the kettle, where polymerization reactions will also occur. They will not enter the bottom material to participate in effective reactions with polyoxyethylene polyether, etc., resulting in the materials failing to reach the designed reaction ratio of the product, and further resulting in poor performance of the synthesized polycarboxylic acid water-reducing agent mother liquor. Moreover, because the polymerization product of materials A, B, and C is a high-molecular gel substance with high viscosity and insoluble in water, it is easy for residues to accumulate on the stirring blades, inner coils, and kettle walls in the reactor, requiring manual cleaning for a period of time, posing a greater safety and environmental risk. Summary of the Invention
[0011] The invention provides a polycarboxylate water-reducing agent synthesis reactor, which aims to promote more complete reaction and improve production efficiency and product performance.
[0012] In order to achieve the above object, the technical solution adopted by the present invention is:
[0013] The polycarboxylate water-reducing agent synthesis reactor of the present invention comprises a dripping structure arranged on the top of the reactor and a stirring mechanism arranged inside the reactor; the dripping structure comprises a dripping port for material A, a dripping port for material B, and a dripping port for material C; the stirring mechanism comprises a variable frequency motor and a stirring reducer arranged at the center of the top of the reactor, wherein the output shaft of the stirring reducer is coaxially fixedly connected to the stirring shaft of the stirrer; on the horizontal projection plane of the reactor, the dripping port for material A, the dripping port for material B, and the dripping port for material C are distributed along an arc with the center of the reactor as the center.
[0014] The stirring mechanism is provided with three layers of stirring blades, namely an upper stirring blade, a middle stirring blade and a lower stirring blade.
[0015] The material A dropping port, material B dropping port and material C dropping port are respectively extended into the reactor through vertical dropping pipes; at the lower end of the dropping pipe, an arc-shaped dropping distributor for material A, an arc-shaped dropping distributor for material B and an arc-shaped dropping distributor for material C are respectively provided.
[0016] The arc-shaped drop-adding distributors for material A, material B and material C are distributed on the same plane, with their arc centers coinciding with the axis of the reactor; multiple arc-shaped drop-adding distribution holes are evenly distributed on each distributor.
[0017] A liquid level detector is provided on the upper portion of the inner wall of the reactor.
[0018] The upper stirring blade is connected to the stirring shaft of the stirrer through the upper stirring fixed blade; an upper stirring telescopic blade is arranged on the upper stirring fixed blade; the upper stirring telescopic blade performs telescopic movement along the double-groove track on the upper stirring fixed blade; an electric push-pull device is arranged on the upper stirring fixed blade to drive the telescopic movement of the upper stirring telescopic blade.
[0019] The upper stirring blade is tilted 45 degrees in the opposite direction of the rotation direction of the stirring shaft of the vertical stirrer, and the tilting direction is such that the liquid is pushed downward after the blade rotates.
[0020] The installation height of the liquid level detector is 8 cm higher than the upper stirring blade.
[0021] The lower stirring blade adopts a flat anchor frame fixed paddle structure, the upper part of the flat anchor frame fixed paddle structure is perpendicular to the horizontal blade of the agitator stirring shaft, and the horizontal blade is inclined 45° along the rotation direction of the vertical agitator stirring shaft, and the inclination direction is such that the liquid is pushed upward after the blade rotates.
[0022] The materials of the dropping material pipe and the dropping distributor are stainless steel pipe or polytetrafluoroethylene.
[0023] The material A is a solution containing a highly active double bond mixture; the material B is a chain transfer agent solution; and the material C is a reducing agent solution.
[0024] The number of the arc-shaped dripping distribution holes on each dripping distributor is 8; and the hole spacing between adjacent arc-shaped dripping distribution holes is 10 cm.
[0025] The present invention adopts the above technical solution, adopts intelligent control means, and combines the principles of dropwise addition and stirring to prevent functional monomers and reducing components from polymerizing and gelling during the dropwise addition process. Its reasonable structural design can overcome the gelation and performance problems during the synthesis of polycarboxylate water-reducing agent mother liquor, not only improving work efficiency and product performance, but also being safer and more environmentally friendly. BRIEF DESCRIPTION OF THE DRAWINGS
[0026] The contents shown in the accompanying drawings and the symbols in the drawings are briefly described as follows:
[0027] Figure 1 This is a schematic diagram of the internal structure of the polycarboxylate water-reducing agent mother liquor process synthesis reactor;
[0028] Figure 2 This is a top view schematic diagram of the reactor top structure of the polycarboxylate superplasticizer mother liquor synthesis reactor;
[0029] Figure 3 This is a schematic diagram of the structure of an arc-shaped (closed at both ends) drop distributor device;
[0030] Figure 4 Schematic diagram of the stirring paddle and stirring blade structure;
[0031] Figure 5 For Figure 4 Schematic diagram of the agitator agitator shaft rotated 90°;
[0032] Figure 6 Schematic diagram of the structure of the upper stirring blade.
[0033] The following are marked in the figure:
[0034] 1. Reactor, 2. Reactor cover, 3. Oxidant inlet, 4. Liquid alkali inlet, 5. Stirring reducer, 6. Frequency conversion motor, 7. Drop-feed port for material A, 8. Drop-feed port for material B, 9. Drop-feed port for material C, 10. Polyether inlet, 11. Desalted water inlet, 12. Exhaust hole, 13. Arc-shaped drop-feed distributor for material A, 14. Arc-shaped drop-feed distributor for material B, 15. Arc-shaped drop-feed distributor for material C, 16. Liquid level detector, 17. Upper stirring retractable blade, 18. Electric push-pull device, 19. Middle stirring blade, 20. Double inner coils inside the reactor, 21. Single coil outside the reactor, 22. Lower stirring blade, 23. Stirring shaft of agitator, 24. Discharge port, 25. Arc-shaped drop-feed distribution hole, 26. Upper stirring fixed blade, 27. Double-slot track. DETAILED DESCRIPTION
[0035] The specific implementation methods of the present invention will be further explained in detail below by describing the embodiments with reference to the accompanying drawings, so as to help those skilled in the art to have a more complete, accurate and in-depth understanding of the inventive concept and technical solution of the present invention.
[0036] like Figures 1 to 6 The structure of the present invention is a polycarboxylate water-reducing agent synthesis reactor 1, a reactor cover 2 and a vent 12 are provided on the top; and a discharge port 24 is provided in the middle of the bottom of the reactor 1.
[0037] The top of the reactor 1 is provided with an oxidant inlet 3, a liquid alkali inlet 4, a polyether inlet 10 and a desalted water inlet 11. The main material for the polycarboxylate water reducer is added to the reactor 1 through stirring.
[0038] The reactor 1 includes a dropping structure arranged on the top of the reactor 1 and a stirring mechanism arranged inside the reactor 1; the dropping structure also includes a dropping port 7 for material A, a dropping port 8 for material B and a dropping port 9 for material C; the stirring mechanism includes a variable frequency motor 6 and a stirring reducer 5 arranged at the center of the top of the reactor 1, and the output shaft of the stirring reducer 5 is coaxially fixedly connected to the stirring shaft 23 of the stirrer.
[0039] In order to ensure that the reaction conditions are met and the effective area of mass and heat transfer in the reactor 1 is realized, the reactor 1 adopts a heat exchange structure design of double coils 20 inside the reactor and a single coil 21 outside the reactor.
[0040] 1. Setting of the dropping port for dropping material:
[0041] In order to solve the problems existing in the prior art and overcome its defects, and to achieve the invention objectives of promoting a more complete reaction, improving production efficiency and product performance, the technical solution adopted by the present invention is as follows:
[0042] like Figures 1 to 3 As shown, in the polycarboxylate water-reducing agent synthesis reactor of the present invention, on the horizontal projection plane of the reactor 1, the material A drop-in port 7, the material B drop-in port 8 and the material C drop-in port 9 are distributed along an arc with the center of the reactor 1 as the center.
[0043] The present invention aims at solving the existing stirring and dripping defects, mainly improving the dripping method and stirring blades of functional small materials and catalytic reduction, and designing the position and method of dripping functional small materials (A, B, C material dripping ports).
[0044] The dropwise addition material A is a solution containing a highly active double bond mixture, such as acrylic acid, hydroxyethyl acrylate, etc.; the dropwise addition material B is a chain transfer agent solution; and the dropwise addition material C is a reducing agent solution, such as VC, etc.
[0045] like Figure 2 As shown, the chemically active single small material drop-in port is designed and fixed according to the position of A material inlet 7, B material inlet 8, and C material inlet 9; after the A, B, and C drop-in positions are selected, the arc-shaped drop-in distributor is manufactured and installed; the corresponding arc-shaped drop-in distributor is installed according to Figure 3 Design and follow Figure 2 The positions of the arc-shaped drop-adding distributor 13 for material A, the arc-shaped drop-adding distributor 14 for material B, and the arc-shaped drop-adding distributor 15 for material C are installed and fixed.
[0046] The material A drop-feeding port 7, the material B drop-feeding port 8 and the material C drop-feeding port 9 are respectively extended into the reactor 1 through vertical drop-feeding pipes; at the lower ends of the drop-feeding pipes, arc-shaped drop-feeding distributors 13, 14 and 15 for material A, B and C are respectively provided.
[0047] The arc-shaped drop-adding distributor 13 for material A, the arc-shaped drop-adding distributor 14 for material B and the arc-shaped drop-adding distributor 15 for material C are distributed on the same plane, and the center of the arc coincides with the axis of the reactor 1; multiple arc-shaped drop-adding distribution holes 25 are evenly distributed on each distributor.
[0048] Each drip distributor has eight arc-shaped drip distribution holes 25, with a spacing of 10 cm between adjacent arc-shaped drip distribution holes 25. Each drip tube in the kettle is arc-shaped (closed at both ends) for drip distribution, and each arc-shaped tube has eight holes, with each hole approximately 10 cm apart.
[0049] The material of the drop feeding pipe and the drop feeding distributor is a stainless tube or polytetrafluoroethylene. The stainless tube or polytetrafluoroethylene (PTFE) is used to evenly distribute holes on the top of the reactor 1.
[0050] 2. Setting of stirring mechanism:
[0051] like Figure 1 、 Figure 4 As shown, the upper, middle, and lower layers of stirring paddles are arranged parallel to each other, with the middle layer of stirring blades 19 fixed vertically. The stirring mechanism comprises three layers of stirring blades: upper stirring blades, middle stirring blades 19, and lower stirring blades 22. This three-layer stirring design provides sufficient rotary stirring and up-and-down tumbling, resolving the gelling problem during the synthesis of the polycarboxylate superplasticizer mother liquor and promoting a more complete reaction, thereby improving production efficiency and product performance.
[0052] 1. Upper stirring blade:
[0053] like Figure 1 As shown, a liquid level detector 16 is provided on the upper portion of the inner wall of the reactor 1. The liquid level detector 16 is used to realize the intelligent control interlocking telescopic movement with the upper stirring blade.
[0054] like Figure 1 、 Figure 4-Figure 6 As shown, the upper stirring blade is connected to the agitator stirring shaft 23 through the upper stirring fixed blade 26; an upper stirring telescopic blade 17 is provided on the upper stirring fixed blade 26; the upper stirring telescopic blade 17 performs telescopic movement along the double-groove track 27 on the upper stirring fixed blade 26; an electric push-pull device 18 is provided on the upper stirring fixed blade 26 to drive the telescopic movement of the upper stirring telescopic blade 17.
[0055] The upper stirring paddles utilize a liquid level positioning system and an electric push-pull system to create a retractable blade. This allows the electric pusher to retract before the bottom material reaches the upper stirring blades, preventing the A, B, and C droplets from being hit and splashed by the upper paddles. When the liquid level detector 16 measures the liquid level at the set point, the electric pusher 18 pushes the upper retractable paddles 17 to straighten, achieving a downward pressure on the liquid during stirring.
[0056] The upper stirring blades are tilted 45° in the reverse direction of the rotation of the vertical stirrer stirring shaft 23, and the tilting direction is such that the liquid is pushed downward after the blades rotate. Figure 5 As shown, the upper stirring fixed blade 26 is designed and fixed at a 45-degree tilt in the opposite direction of the vertical stirring shaft rotation direction; the upper stirring blade adopts a combination of fixed blade and movable telescopic blade, and is designed according to the length of the movable telescopic blade 17 being 1 / 3 of the fixed blade 26, so that the liquid being stirred produces a downward movement while rotating, thereby increasing the mixing effect of the liquid.
[0057] The liquid level detector 16 is installed 8 cm higher than the upper stirring blades. That is, the probe of the liquid level detector 16 is 8 cm away from the horizontal plane of the upper stirring blades. This ensures that the liquid level surface completely submerges the upper stirring blades, allowing the upper retractable stirring blades 17 to extend and begin stirring.
[0058] 2. Lower stirring blade:
[0059] like Figure 4 、 Figure 5 As shown, the lower stirring blade 22 adopts a flat anchor frame fixed paddle structure, the upper part of the flat anchor frame fixed paddle structure is perpendicular to the horizontal blade of the agitator stirring shaft 23, and the horizontal blade is inclined 45° along the rotation direction of the vertical agitator stirring shaft 23, and the inclination direction is such that the liquid is pushed upward after the blade rotates.
[0060] The lower stirring blade adopts a flat anchor frame fixed blade 22, and the anchor flat blade is tilted 45 degrees along the vertical stirring shaft rotation direction, so that the lower blade rotates to press the liquid upward, so that the stirring liquid produces an upward movement while rotating, thereby increasing the mixing effect of the liquid.
[0061] During the stirring process, the liquid is subjected to an upward thrust, while the blades are subjected to a downward reaction force, causing both ends to bend and deform. In order to overcome this problem, the lower stirring blades adopt a lower frame structure to support both ends of the lower stirring blades and prevent them from deforming downward.
[0062] 3. Middle stirring blade:
[0063] like Figure 1and Figure 4 As shown, the middle stirring blade 19 is designed so that the longitudinal direction of the blade is perpendicular to the longitudinal direction of the stirring shaft 23 of the stirrer, and the plane of the blade coincides with the stirring shaft 23 of the stirrer to achieve a dispersing stirring effect.
[0064] III. Summary of Invention and Creativity:
[0065] The present invention provides a polycarboxylate superplasticizer mother liquor synthesis stirring and dripping device, comprising a dripping position, an arc-shaped dripping distributor, a reaction stirring paddle with independently designed blades, a liquid level positioner, and a stainless steel insulated electric push-pull mechanism. Its rational structural design overcomes gelation and performance issues during polycarboxylate superplasticizer mother liquor synthesis, meeting the requirements of modern polycarboxylate superplasticizer mother liquor synthesis processes. It prevents functional monomers and reducing components from polymerizing and gelling during the dripping process. By combining the dripping and stirring principles and employing intelligent control technology to control the extension and retraction of the upper paddle, it not only improves work efficiency and product performance, but also enhances safety and environmental friendliness.
[0066] The present invention is described above by way of example in conjunction with the accompanying drawings. It is obvious that the specific implementation of the present invention is not limited to the above-mentioned method. As long as various non-substantial improvements are made using the method concept and technical solution of the present invention, or the concept and technical solution of the present invention are directly applied to other occasions without improvement, they are all within the scope of protection of the present invention.
Claims
1. A polycarboxylate water-reducing agent synthesis reactor, comprising a dripping structure arranged on the top of the reactor (1) and a stirring mechanism arranged in the reactor (1); the dripping structure comprises a material A dripping port (7), a material B dripping port (8) and a material C dripping port (9); the stirring mechanism comprises a variable frequency motor (6) and a stirring reducer (5) arranged at the center of the top of the reactor (1); the output shaft of the stirring reducer (5) is coaxially fixedly connected to the stirring shaft (23) of the stirrer; Its characteristics are: The material A is a solution containing a highly active double bond mixture; the material B is a chain transfer agent solution; and the material C is a reducing agent solution. On the horizontal projection surface of the reactor (1), the material A drop-feeding port (7), the material B drop-feeding port (8), and the material C drop-feeding port (9) are distributed along an arc with the center of the reactor (1) as the center; The stirring mechanism is provided with three layers of stirring blades, namely an upper stirring blade, a middle stirring blade (19) and a lower stirring blade (22); The material A drop-feeding port (7), the material B drop-feeding port (8), and the material C drop-feeding port (9) are respectively extended into the reactor (1) through vertical drop-feeding pipes; at the lower ends of the drop-feeding pipes, an arc-shaped drop-feeding distributor (13) for material A, an arc-shaped drop-feeding distributor (14) for material B, and an arc-shaped drop-feeding distributor (15) for material C are respectively provided; The arc-shaped drop-adding distributor (13) for material A, the arc-shaped drop-adding distributor (14) for material B, and the arc-shaped drop-adding distributor (15) for material C are distributed on the same plane, and the centers of the arcs coincide with the axis of the reactor (1); a plurality of arc-shaped drop-adding distribution holes (25) are evenly distributed on each distributor; A liquid level detector (16) is provided on the upper portion of the inner wall of the reactor (1); The upper stirring blade is connected to the stirring shaft (23) of the stirrer through the upper stirring fixed blade (26); an upper stirring telescopic blade (17) is provided on the upper stirring fixed blade (26); the upper stirring telescopic blade (17) performs telescopic movement along the double-grooved track (27) on the upper stirring fixed blade (26); an electric push-pull device (18) is provided on the upper stirring fixed blade (26) to drive the telescopic movement of the upper stirring telescopic blade (17); The upper stirring blade is tilted 45 degrees in the opposite direction of the rotation direction of the vertical stirrer stirring shaft (23), and the tilt direction is such that the liquid is pushed downward after the blade rotates; The installation height of the liquid level detector (16) is 8 cm higher than the upper stirring blade; The lower stirring blade (22) adopts a flat anchor frame fixed blade structure, the upper part of the flat anchor frame fixed blade structure is perpendicular to the horizontal blade of the stirrer stirring shaft (23), and the horizontal blade is inclined 45 degrees along the rotation direction of the vertical stirrer stirring shaft (23), and the inclination direction is such that the liquid is pushed upward after the blade rotates; The material of the dropping pipe and the dropping distributor is stainless steel pipe or polytetrafluoroethylene; The number of the arc-shaped dripping distribution holes (25) on each dripping distributor is 8; and the hole spacing between adjacent arc-shaped dripping distribution holes (25) is 10 cm.
Citation Information
Patent Citations
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