A method for preparing polyether macromonomer for polycarboxylate water reducer

Abstract

The present application discloses a method for preparing a polyether macromonomer for polycarboxylic acid water-reducing agent, which comprises the following steps: S1, preparing methallyl oligomers; S2, generating methallyl random polyethers; a monitoring mechanism for monitoring the temperature at different positions is provided in the reactor; in both S1 and S2, the reaction temperature needs to be controlled by a cooling device, the cooling device comprising a cooling jacket fixed outside the reactor, a water supply mechanism for introducing cooling water into the cooling jacket, a cooling mechanism for rapid cooling, and a heating mechanism for preheating the cooling water, the cooling jacket cover is provided on the outer wall of the reactor, the cooling jacket is also provided with a plurality of temperature regulating chambers, the temperature regulating chambers are used for the cooling mechanism or the heating mechanism to work, and a temperature regulating sensor is provided in the cooling jacket. The present application has the effect of improving the efficiency of controlling the temperature rise and cooling in the reactor.

Description

Technical Field

[0001] The present application relates to the technical field of organic compound synthesis, and in particular to a method for preparing a polyether macromonomer for a polycarboxylic acid water reducer. Background Art

[0002] At present, HPEG and TPEG are the new generation of monomers after APEG and MPEG. Although APEG has a simple synthesis process, its performance is low. MPEG has excellent performance, but the synthesis process is complicated, the esterification process is difficult to control, and the esterification product has a great influence on the performance of the polymerization reaction and the final product. Both have gradually withdrawn from the market, replaced by HPEG and TPEG. Both products have excellent performance, high water reduction rate, good slump retention, simple production process, low energy consumption, no three wastes discharge, and certain market competitiveness, which is conducive to large-scale production and application. For example: HPEG2400 and TPEG2400. However, with the improvement of concrete engineering requirements, the contradiction between the higher durability index requirements of high-performance concrete (HPC) and the deterioration of sand and gravel mixing materials has become increasingly acute. The existing polycarboxylic acid water reducer has exposed the performance defects of low water reduction rate and weak slump retention. High molecular weight polyether macromonomers can form large steric hindrance in polycarboxylic acid water reducers, increase water reduction rate and slump retention, and the highest number average molecular weight commonly seen on the market does not exceed 3000. On the one hand, it is technically difficult to produce under the action of alkaline catalysts, and on the other hand, the unsaturation will decrease after the number average molecular weight increases, and the polyethylene glycol content will be too high, which will affect the performance of the water reducer synthesized later. Synthesizing high molecular weight polyether water reducer macromonomers with high unsaturation and low polyethylene glycol content can greatly improve the performance of water reducers and has great industrial value.

[0003] In the related art, a Chinese patent with a patent publication number of CN107936240A proposes a method for preparing a polyether macromonomer for polycarboxylic acid water reducer, comprising the following steps: (1) taking part of methyl allyl alcohol and reacting it with catalyst one, then putting the product after the reaction into the remaining methyl allyl alcohol, and introducing ethylene oxide and propylene oxide to react; (2) reacting the above methyl allyl random oligomer with catalyst two and catalyst three, and then introducing ethylene oxide and propylene oxide to react; the catalyst one is one or more of sodium, potassium, and sodium hydride; the catalyst two is one or more of 18-crown-6 and 15-crown-5; the catalyst three is hexachlorocyclotriphosphazene. Compared with the prior art, the method for synthesizing a methyl allyl random polyether obtained by using the present invention has the advantages of high effective content, low by-product content, narrow molecular weight distribution, high double bond retention rate, etc., the molecular weight distribution coefficient is less than 1.05, and the double bond retention rate is greater than 98.0%.

[0004] With respect to the above-mentioned related technologies, the inventors believe that the following defects exist: in the process of preparing methallyl oligomers and methallyl random polyethers using a reactor, the reactor needs to be cooled. Currently, cooling water is used in the reactor for cooling. However, during the cooling process, if the cooling is only performed by controlling the cooling water flow rate, the working efficiency is low and the thermal insulation effect is poor. Therefore, it is necessary to solve the above-mentioned problems of poor cooling and thermal insulation effects. Summary of the invention

[0005] In order to improve the problem of low cooling efficiency, the present application provides a method for preparing a polyether macromonomer for a polycarboxylate water-reducing agent.

[0006] The present application provides a method for preparing a polyether macromonomer for a polycarboxylate water-reducing agent using the following technical solution:

[0007] A method for preparing a polyether macromonomer for a polycarboxylate water-reducing agent comprises the following steps:

[0008] S1. Preparation of methallyl oligomer: methallyl alcohol and sodium metal catalyst are added to a reactor. After the reaction is completed, the product is added to methallyl alcohol, replaced with nitrogen, heated to 70° C., ethylene oxide and propylene oxide are introduced, the reaction temperature is controlled to be 70-95° C., and the reaction time is 3.0-4.0 hours; after the reaction is completed, the temperature is lowered to 70° C. and the methallyl oligomer with a molecular weight of 300 is obtained;

[0009] S2, generating methallyl random polyether: adding the methallyl oligomer obtained in step S1 into a reaction kettle, adding catalysts 18-crown-6 and hexachlorocyclotriphosphazene, controlling the reaction temperature to 30-50°C, and the reaction time to 0.5-1.0 hour; after the reaction, nitrogen replacement is performed, the temperature is raised to 80°C, ethylene oxide and propylene oxide are introduced, the reaction temperature is controlled to 80-100°C, and the reaction time is 4.0-5.0 hours; after the reaction, the temperature is lowered to 80°C, and degassing is performed for 10-30 minutes to obtain methallyl random polyether with a molecular weight of 1000;

[0010] A monitoring mechanism for monitoring the temperature at different positions is provided in the reactor;

[0011] In both S1 and S2, the reaction temperature needs to be controlled by a cooling device, and the cooling device includes a cooling jacket fixed outside the reactor, a water supply mechanism for introducing cooling water into the cooling jacket, a cooling mechanism for rapid cooling, and a heating mechanism for preheating the cooling water. The cooling jacket cover is arranged on the outer wall of the reactor. The cooling jacket is also provided with a plurality of temperature regulating chambers, and the temperature regulating chambers are used for the cooling mechanism or the heating mechanism to work. A temperature regulating sensor is arranged in the cooling jacket.

[0012] Optionally, the heating mechanism includes a heating rack that is lifted and lowered below the cooling jacket, a plurality of phase change tubes fixed in the heating rack, a power part for lifting and lowering the heating rack, and an auxiliary component for assisting the heating of the phase change tubes. The phase change tubes are filled with phase change materials for absorbing and releasing heat. The cooling jacket is also provided with a regulating mechanism in the temperature control cavity for controlling whether water enters. The phase change tubes are plugged into the temperature control cavity.

[0013] Optionally, the adjustment mechanism includes an adjustment plate, an abutment block, and a transmission part for ensuring that the adjustment plate can only move upward and the abutment block can only move downward. The inner wall of the temperature adjustment chamber is provided with a water inlet connected to the cooling jacket. The adjustment plate slides on the outer wall of the temperature adjustment chamber and slides in contact with the water inlet, and the abutment block slides on the adjustment plate toward the side wall of the temperature adjustment chamber.

[0014] Optionally, the transmission part includes an upper block, a lower block, an upper spring and a lower spring, the side wall of the abutment block is fixedly connected to the lower block, the adjustment plate is provided with a lower groove for sliding of the lower block, both ends of the lower groove are closed, both ends of the lower spring are respectively fixedly connected to the upper end of the lower block and the upper end of the lower groove, and the initial position of the lower block is located at the top end of the lower groove;

[0015] The upper block is fixedly connected to the side wall of the upper end of the adjustment plate, the cooling sleeve is provided with two upper grooves on the outer wall of the temperature adjustment chamber for sliding of the upper block, the two ends of the upper spring are fixedly connected to the lower end of the upper block and the lower end of the upper groove, respectively, and the initial position of the upper block is located at the bottom end of the upper groove;

[0016] The upper block, the inner wall of the upper groove, the lower block and the inner wall of the lower groove are all configured in a T-shape in horizontal cross-section.

[0017] Optionally, the auxiliary component includes a heating tube detachably connected to the phase change tube, a heating element arranged in the heating tube, and a fixing portion for fixing the heating tube in the temperature control chamber. The heating tube and the phase change tube are adsorbed and connected by a first electromagnet. The heating tube is located at the top of the phase change tube, and the heating tube is slidingly adapted to the temperature control chamber.

[0018] Optionally, the fixed part includes two plug-in blocks and a second electromagnet, the heating tube is provided with two slide grooves close to the bottom wall, the plug-in block is elastically arranged in the slide grooves, the bottom side wall of the temperature control chamber is provided with two plug-in holes, the plug-in block is plugged into the plug-in holes, and an adsorption hole connected to both the slide grooves is provided at the center of the bottom of the heating tube, the second electromagnet is installed in the adsorption hole, and the ends of the two plug-in blocks are adsorbed by the second electromagnet.

[0019] Optionally, the cooling mechanism includes a cooling frame that is lifted and lowered at the upper end of the cooling sleeve, a reciprocating part for realizing the lifting and lowering of the cooling frame, a rotating ring rotatably arranged on the cooling frame, a driving component for driving the rotating ring to rotate, a plurality of cooling tubes fixed on the rotating frame, an ice-making component for making ice for water in the cooling tubes, a circulation component for providing hot water to the cooling tubes, and a detection component for detecting whether ice making in the plurality of cooling tubes is completed, the plurality of cooling tubes are respectively plugged and adapted with the plurality of temperature regulating chambers, and the top end of the cooling tube is opened.

[0020] Optionally, the ice-making assembly includes a nozzle fixed on the cooling rack and a storage tank for storing liquid nitrogen, the storage tank is placed on the external environment, and the nozzle is facing the top opening of the cooling tube, the driving assembly causes the rotating ring to rotate intermittently and the angle of each rotation of the rotating ring causes the corresponding top opening of the cooling tube to face the nozzle.

[0021] Optionally, the detection assembly includes a detection needle elastically arranged on the cooling rack, a handle fixedly connected to the top of the detection needle, a resetting part for resetting the detection needle, a third electromagnet, a trigger member for intermittently pushing the third electromagnet to move toward one end of the handle, and a proximity switch, the third electromagnet moves in a horizontal direction toward the end of the handle, the proximity switch is electrically connected to the trigger member, and the proximity switch and the third electromagnet are respectively located on both sides of the detection needle.

[0022] Optionally, the monitoring mechanism includes a monitoring frame, a first temperature sensor and a second temperature sensor which are lifted and lowered in the reactor, the first temperature sensor and the second temperature sensor are both fixed on the monitoring frame, and the first temperature sensor is close to the side wall of the reactor, and the second temperature sensor is close to the center of the reactor.

[0023] In summary, the present application includes at least one of the following beneficial technical effects:

[0024] 1. After heat exchange between the cooling tube and the solution in the reactor, the temperature is quickly reduced to the set temperature or close to the set temperature, and then the cooling tube is removed; and at this time, the cooling tube will only push the abutment block to move on the adjustment plate, and the adjustment plate will not move, so as to prevent the cold water from directly contacting the cooling tube and affecting the cooling speed of the cooling tube; when the phase change tube and the heating tube are both inserted into the temperature adjustment chamber, the abutment block will not move, and the adjustment plate will be pushed upward, and the phase change tube is located at the water inlet. At this time, the cooling water in the cooling jacket can be preheated and heated by the phase change tube. When the phase change tube slides out of the temperature adjustment chamber, the heating tube is located in the temperature adjustment chamber and needs to be kept at the water inlet. The cooling water still does not enter the temperature adjustment chamber, and the heating tube begins to heat the cooling water. A temperature adjustment sensor is installed in the cooling jacket, and the temperature adjustment sensor is used to control the temperature of the cooling water in the cooling jacket;

[0025] 2. When the heating tube moves toward the water inlet, one end of the plug-in block facing the plug-in hole is located in the slide groove, and the limiting spring is stretched and deformed. When the plug-in block moves to the position of the plug-in hole, the second electromagnet is powered off and demagnetized. Under the elastic force of the limiting spring, the plug-in block is plugged into the plug-in hole, and the other end of the plug-in block is still located in the adsorption hole. Therefore, it is only necessary to energize the second electromagnet and adsorb the plug-in block, and then the plug-in block can be pulled out of the plug-in hole; when the heating tube is fixed in the temperature adjustment chamber, the first electromagnet is powered off, and the heating tube is separated from the phase change tube, so that the heating tube can better heat the cooling water to prevent the phase change tube from absorbing the heat of the heating tube, and then the constant temperature state of the cooling water can be achieved with the help of the control of the temperature adjustment sensor;

[0026] 3. When the temperature in the reactor begins to rise, the heating rack moves upward, the phase change tube is plugged into the corresponding temperature control cavity, and no cooling water is introduced into the cooling jacket. During the temperature rise of the phase change tube in the reactor, the phase change material in the phase change tube absorbs heat. After the heating work is completed, the phase change tube is pulled out of the temperature control cavity. When the temperature in the reactor needs to be cooled down, when the temperature in the reactor begins to rise, the heating rack moves upward, the phase change tube is plugged into the corresponding temperature control cavity, and no cooling water is introduced into the cooling jacket. During the temperature rise of the phase change tube in the reactor, the phase change material in the phase change tube absorbs heat. After the heating work is completed, the phase change tube is pulled out of the temperature control cavity. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 is a process flow chart of an embodiment of the present application;

[0028] Figure 2 It is a schematic diagram of the overall structure of an embodiment of the present application;

[0029] Figure 3 is a schematic diagram of a cooling mechanism in an embodiment of the present application;

[0030] Figure 4 yes Figure 2 A magnified schematic diagram of part A;

[0031] Figure 5 yes Figure 2 Schematic diagram of the enlarged portion B.

[0032] Figure numerals: 1, reactor; 2, cooling jacket; 3, temperature adjustment chamber; 4, temperature adjustment sensor; 5, heating rack; 6, phase change tube; 7, power part; 8, adjustment plate; 9, abutment block; 10, water inlet; 11, upper block; 12, upper groove; 13, lower block; 14, lower groove; 15, upper spring; 16, lower spring; 17, heating tube; 18, heating element; 19, first electromagnet; 20, plug-in block; 21, plug-in hole; 22, slide groove; 23, second electromagnet; 24, adsorption hole; 25, cooling rack; 26 , reciprocating part; 27, rotating ring; 28, cooling pipe; 29, driving motor; 30, gear; 31, ring gear; 32, storage tank; 33, nozzle; 34, circulation pump; 35, water nozzle; 36, circulation pipe; 37, water supply tank; 38, water supply pump; 39, water supply pipe; 40, handle; 41, detection needle; 42, reset part; 43, reset electromagnet; 44, third electromagnet; 45, trigger part; 46, proximity switch; 47, monitoring frame; 48, first temperature sensor; 49, second temperature sensor. DETAILED DESCRIPTION

[0033] The following is combined with Figure 1-5 This application is described in further detail.

[0034] The present application discloses a method for preparing a polyether macromonomer for a polycarboxylate water reducer. Figure 1 A method for preparing a polyether macromonomer for a polycarboxylate water-reducing agent comprises the following steps:

[0035] S1, preparation of methallyl oligomer: 28.8 parts of methallyl alcohol and 2.4 parts of catalyst metal sodium were added to reactor 1, and after the reaction, the product was added to 259.2 parts of methallyl alcohol, nitrogen was replaced, the temperature was raised to 70°C, 638.4 parts of ethylene oxide and 273.6 parts of propylene oxide were introduced, the reaction temperature was controlled to be 70-95°C, and the reaction time was 3.0-4.0 hours; after the reaction, the temperature was lowered to 70°C and the methallyl oligomer with a molecular weight of 300 was obtained;

[0036] S2, generating methallyl random polyether: adding 540 parts of methallyl oligomer obtained in step S1 into reactor 1, adding 0.3 parts of 18-crown-6 and hexachlorocyclotriphosphazene as catalysts, controlling the reaction temperature to 30-50°C, and the reaction time to 0.5-1.0 hour; after the reaction, nitrogen replacement is performed, the temperature is raised to 80°C, 882 parts of ethylene oxide and 378 parts of propylene oxide are introduced, the reaction temperature is controlled to 80-100°C, and the reaction time is 4.0-5.0 hours; after the reaction, the temperature is lowered to 80°C, and degassing is performed for 10-30 minutes to obtain methallyl random polyether with a molecular weight of 1000.

[0037] Reference Figure 2 and Figure 3 The reactor 1 is provided with a monitoring mechanism for monitoring the temperature at different positions, the monitoring mechanism comprising a monitoring frame 47, a first temperature sensor 48 and a second temperature sensor 49 which are lifted and lowered in the reactor 1. The lifting and lowering of the monitoring frame 47 is realized by an electric push rod or a cylinder, and the electric push rod or the cylinder is located outside the reactor 1, and the monitoring frame 47 is located on one side of the stirring rod in the reactor 1. When monitoring the temperature, the present embodiment preferably starts monitoring after the stirring work is completed. The first temperature sensor 48 and the second temperature sensor 49 are both fixed on the monitoring frame 47, and the first temperature sensor 48 is close to the side wall of the reactor 1, and the second temperature sensor 49 is fixed to the monitoring frame 47. The first temperature sensor 49 is close to the center of the reactor 1, and the second temperature sensor 49 avoids the position of the stirring blade on the stirring rod. When heating, the temperatures of the first temperature sensor 48 and the second temperature sensor 49 need to be kept consistent to prove that the temperature of the solution in the reactor 1 is uniform. In the cooling process, when the first temperature sensor 48 detects that the temperature at the side wall of the reactor 1 is close to or lower than the set temperature, the cooling water needs to be heated and the temperature of the cooling water is kept consistent with the set temperature, so as to ensure that the temperatures of the first temperature sensor 48 and the second temperature sensor 49 are consistent, which also proves that the cooling work in the reactor 1 is completed.

[0038] Reference Figure 2 and Figure 3In both S1 and S2, the reaction temperature needs to be controlled by a cooling device. The cooling device includes a cooling jacket 2 fixed outside the reactor 1, a water supply mechanism for introducing cooling water into the cooling jacket 2, a cooling mechanism for rapid cooling, and a heating mechanism for preheating the cooling water. The water supply mechanism includes a water supply tank 37, a water supply pump 38, and a water supply pipe 39. The water supply tank 37 is arranged in the external environment, the water supply pump 38 is installed in the water supply tank 37, the water supply pipe 39 is connected to the output end of the water supply pump 38, and the other end of the water supply pipe 39 is connected to the cooling jacket 2. In this embodiment, a downpipe can also be installed at the bottom of the cooling jacket 2, and the downpipe guides water into the water supply tank 37, thereby achieving a cooling water circulation effect. The cooling jacket 2 is covered on the outer wall of the reactor 1. A plurality of temperature regulating chambers 3 are arranged near the outer wall of the reactor 1 on the cooling jacket 2. The plurality of temperature regulating chambers 3 are arranged on the cooling jacket 2 at equal intervals. Both ends of the temperature regulating chambers 3 are opened. The temperature regulating chambers 3 are used for the operation of the cooling mechanism or the heating mechanism. In the cooling process of this embodiment, the temperature is firstly quickly reduced to a set temperature or close to a set temperature after heat exchange with the solution in the reactor 1 through the cooling mechanism. Then, the cooling mechanism is removed and the cooling water is heated by the heating mechanism. Thus, the solution in the reactor 1 can achieve a water bath effect. Thus, while completing the cooling work, it is also convenient to keep the temperature of the solution in the reactor 1 uniform.

[0039] Reference Figure 2 and Figure 4 The heating mechanism includes a heating frame 5 which is lifted and arranged below the cooling jacket 2, a plurality of phase change tubes 6 fixed in the heating frame 5, a power part 7 for lifting and lowering the heating frame 5, and an auxiliary component for assisting the heating of the phase change tube 6. The phase change tube 6 is filled with a phase change material for absorbing and releasing heat. The power part 7 in this embodiment can be an electric push rod or a cylinder. The power part 7 is installed on the cooling jacket 2, the heating frame 5 is located below the cooling jacket 2, and the heating frame 5 is arranged in a ring shape. A plurality of phase change tubes 6 are fixed on the heating frame 5 at equal intervals, and the phase change tube 6 is aligned with the temperature regulating chamber 3. When the temperature in the reactor 1 begins to rise, the heating rack 5 moves upward, the phase change tube 6 is inserted into the corresponding temperature control chamber 3, and no cooling water is introduced into the cooling jacket 2. During the temperature rise process of the phase change tube 6 in the reactor 1, the phase change material in the phase change tube 6 absorbs heat. After the heating work is completed, the phase change tube 6 is pulled out of the temperature control chamber 3. In this embodiment, the temperature in the air has little effect on the phase change tube 6, and will not cause excessive heat loss in the phase change tube 6 in the air. Of course, the phase change tube 6 can also be placed in the air and a thermal insulation material can be arranged outside the phase change tube 6.

[0040] Reference Figure 2 and Figure 4The adjusting mechanism includes an adjusting plate 8, an abutting block 9, and a transmission part for realizing that the adjusting plate 8 can only move upward and the abutting block 9 can only move downward. The inner wall of the temperature regulating chamber 3 is provided with a water inlet 10 connected to the inside of the cooling jacket 2. The adjusting plate 8 slides on the outer wall of the temperature regulating chamber 3 and slides in contact with the water inlet 10. The abutting block 9 slides on the side wall of the adjusting plate 8 toward the temperature regulating chamber 3. The transmission part includes an upper block 11, a lower block 13, an upper spring 15 and a lower spring 16. The side wall of the abutting block 9 is fixedly connected to the lower block 13. The adjusting plate 8 is provided with a The lower groove 14 in which the lower block 13 slides is vertically arranged and both ends are closed. The two ends of the lower spring 16 are fixedly connected to the upper end of the lower block 13 and the upper end of the lower groove 14 respectively. The initial position of the lower block 13 is located at the top of the lower groove 14. The horizontal cross-section of the lower block 13 and the inner wall of the lower groove 14 is set to be T-shaped, that is, the lower block 13 can move in the lower groove 14 along its length direction. At this time, the lower block 13 cannot fall off from the lower groove 14, that is, the abutment block 9 can only move downward and cannot move upward.

[0041] The upper block 11 is fixedly connected to the side wall of the upper end of the adjusting plate 8, and the cooling sleeve 2 is provided with an upper groove 12 for sliding the upper block 11 on the outer wall of the temperature regulating chamber 3. The upper groove 12 is vertically arranged and both ends are also closed. The horizontal cross-section of the upper block 11 and the inner wall of the upper groove 12 is set in a T-shape. The upper block 11 can only move along the length direction of the upper groove 12, and the upper block 11 will not fall off from the upper groove 12; the two ends of the upper spring 15 are respectively fixedly connected to the lower block 13 of the upper block 11 and the lower end of the upper groove 12, and the initial position of the upper block 11 is located at the bottom of the upper groove 12. The adjusting plate 8 fits the outer wall of the temperature regulating chamber 3 and can also be installed with a sealing ring. The adjusting plate 8 just blocks the water inlet 10, that is, the adjusting plate 8 can only move upward and cannot move downward. In this embodiment, the movement of the abutment block 9 will not allow cooling water to enter the temperature regulating chamber 3. Only when the adjusting plate 8 moves upward can the water inlet 10 be opened, and the cooling water enters the temperature regulating chamber 3 from the water inlet 10.

[0042] Reference Figure 2 and Figure 5The auxiliary component includes a heating tube 17 detachably connected to the phase change tube 6, a heating element 18 arranged in the heating tube 17, and a fixing portion for fixing the heating tube 17 in the temperature control chamber 3. The heating tube 17 and the phase change tube 6 are adsorbed and connected by a first electromagnet 19. The heating tube 17 is located at the top of the phase change tube 6. The heating tube 17 is slidingly adapted to the temperature control chamber 3. In this embodiment, the length of the phase change tube 6 is smaller than the length of the temperature control chamber 3. Therefore, when the phase change tube 6 and the heating tube 17 are both inserted into the temperature control chamber 3, the phase change tube 6 is located at the position of the water inlet 10. If the abutment block 9 is fully adapted to the regulating port and the temperature control chamber 3, part of the cooling water will also enter the temperature control chamber 3. In this embodiment, it does not matter whether the cold air water enters the temperature control chamber 3. The heating tube 17 and the phase change tube 6 block the lower end of the temperature control chamber 3, while the upper end of the temperature control chamber 3 has little effect on the cooling water temperature. The upper end of the temperature regulating chamber 3 is set to be open without affecting the temperature of the cooling water. At this time, the cooling water in the cooling jacket 2 can be preheated and heated by the phase change tube 6. The heating element 18 can be set as an electric heating wire in this embodiment. The cooling water can be heated after the electric heating wire is energized. When the phase change tube 6 slides out of the temperature regulating chamber 3, the heating tube 17 is located in the temperature regulating chamber 3 and the heating tube 17 needs to be kept at the water inlet 10. The cooling water still does not enter the temperature regulating chamber 3, and the heating tube 17 starts to heat the cooling water. A temperature regulating sensor 4 is installed in the cooling jacket 2. The temperature regulating sensor 4 is used to control the temperature of the cooling water in the cooling jacket 2. The temperature regulating sensor 4 and the heating element 18 are connected through the control of the PLC controller, thereby ensuring that the water in the cooling jacket 2 is kept at a constant temperature. During the heating process of the cooling water in the cooling jacket 2, the cooling water in the cooling jacket 2 does not need to be circulated.

[0043] In order to make the heating tube 17 heat the cooling water better and prevent the phase change tube 6 from absorbing the heat of the heating tube 17, the fixed part includes two plug-in blocks 20 and a second electromagnet 23. Two plug-in holes 21 are provided on the bottom side wall of the temperature adjustment chamber 3. The plug-in block 20 is plugged into the plug-in hole 21. Two slide grooves 22 are provided near the bottom of the heating tube 17. The plug-in block 20 is elastically arranged in the slide groove 22. A limiting block is fixedly connected to the side wall of the plug-in block 20. A limiting groove for sliding the limiting block is provided on the side wall of the slide groove 22. Both ends of the limiting groove are closed. Both ends of the limiting spring are fixedly connected to either end of the limiting block and the corresponding end of the limiting groove. An adsorption hole 24 is provided at the bottom center of the heating tube 17. The adsorption hole 24 is connected to the ends of the two slide grooves 22. The second electromagnet 23 is installed in the adsorption hole 24, and the position of the first electromagnet 19 is staggered with the position of the second electromagnet 23 to avoid mutual interference. In the initial state, one end of the plug-in block 20 facing the plug-in hole 21 is located in the slide groove 22, and the limiting spring is stretched and deformed. When the plug-in block 20 moves to the position of the plug-in hole 21, the second electromagnet 23 is powered off and demagnetized. Under the elastic force of the limiting spring, the plug-in block 20 is plugged into the plug-in hole 21, and the other end of the plug-in block 20 is still located in the adsorption hole 24. Therefore, it is only necessary to energize the second electromagnet 23 and adsorb the plug-in block 20, and then the plug-in block 20 can be pulled out of the plug-in hole 21; when the heating tube 17 is fixed in the temperature control chamber 3, the first electromagnet 19 is powered off, and the heating tube 17 is separated from the phase change tube 6.

[0044] Reference Figure 2 and Figure 3 The cooling mechanism includes a cooling frame 25 which is lifted and lowered on the upper end of the cooling jacket 2, a reciprocating member 26 for realizing the lifting of the cooling frame 25, a rotating ring 27 which is rotatably arranged on the cooling frame 25, a driving component for driving the rotating ring 27 to rotate, a plurality of cooling pipes 28 fixed on the rotating frame, an ice-making component for making ice for water in the cooling pipes 28, a circulation component for providing hot water to the cooling pipes 28, and a detection component for detecting whether ice making in the plurality of cooling pipes 28 is completed. The plurality of cooling pipes 28 are respectively plugged and adapted with the plurality of temperature regulating chambers 3, and the top of the cooling pipe 28 is an opening. The reciprocating member 26 can be an electric push rod or a cylinder. The reciprocating member 26 is installed at the upper end of the cooling jacket 2. The rotating ring 27 is rotatably connected to the cooling frame 25 through a bearing. The length of the rotating ring 27 is greater than the thickness of the cooling frame 25. The driving assembly includes a gear 30, a driving motor 29 and a ring gear 31. The ring gear 31 is fixed to the outer wall of the rotating ring 27. The gear 30 is rotatably connected to the cooling frame 25. The driving motor 29 is installed on the cooling frame 25 and is used to drive the gear 30 to rotate. The gear 30 is meshed with the ring gear 31. The driving motor 29 intermittently drives the rotating ring 27 to rotate.

[0045] Reference Figure 2 and Figure 3The circulation component includes a water nozzle 35, a circulation box, a circulation pump 34 and a circulation pipe 36. The cooling jacket 2 is provided with a circulation water inlet at the bottom, and the circulation water inlet is connected to the circulation box. The circulation box is a closed setting. The circulation pump 34 is installed in the circulation box. The circulation box is installed in the external environment and the circulation box is located below the cooling jacket 2. One end of the circulation pipe 36 is connected to the output end of the circulation pump 34, and the other end is connected to the water nozzle 35. The water nozzle 35 is tilted and the water nozzle 35 is directly facing the opening of the cooling pipe 28. The water nozzle 35 is fixed on the cooling rack 25. When the cooling water insulation work in the cooling pipe is completed, the circulation water inlet is installed with a solenoid valve to start the circulation water inlet. The cooling water used for insulation enters the circulation box from the circulation water inlet. When ice making is needed, the water in the circulation box can be pumped to the water nozzle 35, and the water nozzle 35 sprays the cooling book into the cooling pipe 28. Since the speed at which hot water freezes after encountering liquid nitrogen is faster than the speed at which cooling water at normal temperature freezes.

[0046] The ice-making assembly includes a nozzle 33 fixed on the cooling frame 25 and a storage tank 32 for storing liquid nitrogen. The storage tank 32 is placed in an external environment. The nozzle 33 is directly opposite to the top opening of the cooling tube 28, and the nozzle 33 is also tilted. In this embodiment, the nozzle 33 is also tilted, and the positions of the nozzle 33 and the water nozzle 35 are staggered to avoid mutual influence. During the intermittent movement of the gear 30 controlled by the driving motor 29, the rotating ring 27 also rotates intermittently, and the angle of each rotation of the rotating ring 27 makes the top opening of the corresponding cooling tube 28 directly opposite to the nozzle 33; in this embodiment, when ice is needed, water is first sprayed into the cooling tube 28 through the water nozzle 35, and then the nozzle 33 is controlled to spray liquid nitrogen into the cooling tube 28. Since the cooling tube 28 is hot water or warm water, the speed of ice formation is accelerated. At this time, it is necessary to control the rotating ring 27 to rotate, and the next cooling tube 28 is rotated to the bottom of the nozzle 33 after the water nozzle 35, and the ice making operation is continued. The ice making work of all cooling tubes 28 is completed by analogy.

[0047] Reference Figure 2 and Figure 3The detection assembly includes a detection needle 41 elastically arranged on the cooling rack 25, a handle 40 fixedly connected to the top of the detection needle 41, a reset part for resetting the detection needle 41, a third electromagnet 44, a trigger 45 for intermittently pushing the third electromagnet 44 to move toward one end of the handle 40, and a proximity switch 46. The handle 40 is arranged perpendicular to the length direction of the detection needle 41. The detection needle 41 is provided with a detection spring on its outer sleeve. The two ends of the detection spring are fixedly connected to the handle 40 and the wall of the cooling rack 25 respectively. The reset part includes a The reset member 42 and the reset electromagnet 43 for adsorbing the handle 40, the reset member 42 is an electric push rod, the reset electromagnet 43 is fixed to the output end of the reset member 42, the reset electromagnet 43 is energized to adsorb the handle 40, the third electromagnet 44 is fixedly connected to the end of the handle 40 in the horizontal direction, the trigger member 45 is set to an electric push rod, the trigger member 45 is installed on the cooling frame 25, the proximity switch 46 is fixed on the cooling frame 25, and the proximity switch 46 and the third electromagnet 44 are respectively located at two points of the detection needle 41, and the proximity switch 46 is fixed at the third electromagnet 44. The third electromagnet 44 is located at the bottom of the cooling tube 28, and the proximity switch 46 corresponds to the end of the handle 40 away from the third electromagnet 44. Only when ice making in the cooling tube 28 is not completed or the detection needle 41 can move in the cooling tube 28, when the detection needle 41 moves to the bottom, the proximity switch 46 contacts the corresponding end of the handle 40. When the handle 40 is at the highest position, that is, the initial position, if the third electromagnet 44 moves to the end position of the handle 40, the third electromagnet 44 can adsorb the handle 40 and stop the detection work. In this embodiment, it is configured to perform random inspections on multiple cooling tubes 28, for example The two cooling tubes 28 are randomly inspected. If both cooling tubes 28 have completed ice making, it is assumed that the ice making work of all cooling tubes 28 is completed, and the trigger member 45 is set such that when the trigger member 45 pushes the third electromagnet 44 to move twice, the third electromagnet 44 can be pushed from the initial position to the position at the end of the handle 40, and it can be proved that ice making is completed. If after the random inspection of the two cooling tubes 28, the third electromagnet 44 is not adsorbed with the handle 40, and the detection needle 41 continues to perform the detection work, the cooling tubes 28 that need multiple ice making work need to be re-inspected and the ice making work needs to be re-performed.

[0048] The implementation principle of the method for preparing a polyether macromonomer for a polycarboxylic acid water-reducing agent according to the embodiment of the present application is as follows: when the temperature in the reactor 1 starts to rise, the heating rack 5 moves upward, the phase change tube 6 is plugged into the corresponding temperature control chamber 3, and no cooling water is introduced into the cooling jacket 2. During the temperature rise of the phase change tube 6 in the reactor 1, the phase change material in the phase change tube 6 absorbs heat. After the heating work is completed, the phase change tube 6 is pulled out from the temperature control chamber 3. When it is necessary to cool down the temperature in the reactor 1, when the temperature in the reactor 1 starts to rise, the heating rack 5 moves upward, the phase change tube 6 is plugged into the corresponding temperature control chamber 3, and no cooling water is introduced into the cooling jacket 2. During the temperature rise of the phase change tube 6 in the reactor 1, the phase change material in the phase change tube 6 absorbs heat. After the heating work is completed, the phase change tube 6 is pulled out from the temperature control chamber 3.

[0049] The two cooling tubes 28 are randomly inspected. If both cooling tubes 28 have completed ice making, it is assumed that the ice making work of all cooling tubes 28 is completed, and the trigger member 45 is set such that when the trigger member 45 pushes the third electromagnet 44 to move twice, the third electromagnet 44 can be pushed from the initial position to the position at the end of the handle 40, and it can be proved that ice making is completed. If after the random inspection of the two cooling tubes 28, the third electromagnet 44 is not adsorbed with the handle 40, and the detection needle 41 continues to perform the detection work, the cooling tubes 28 that need multiple ice making work need to be re-inspected and the ice making work needs to be re-performed.

[0050] After the cooling tube 28 performs heat exchange with the solution in the reactor 1, the temperature is quickly reduced to the set temperature or close to the set temperature, and then the cooling tube 28 is removed; and at this time, the cooling tube 28 will only push the abutment block 9 to move on the adjustment plate 8, and the adjustment plate 8 will not move, so as to prevent the cold water from directly contacting the cooling tube 28 and affecting the cooling speed of the cooling tube 28; when the phase change tube 6 and the heating tube 17 are both inserted into the temperature adjustment chamber 3, the abutment block 9 will not move, and the adjustment plate 8 will be pushed upward. Movement, the phase change tube 6 is located at the position of the water inlet 10, at this time the cooling water in the cooling jacket 2 can be preheated and heated by the phase change tube 6, when the phase change tube 6 slides out of the temperature adjustment chamber 3, the heating tube 17 is located in the temperature adjustment chamber 3 and the heating tube 17 needs to be kept at the water inlet 10, the cooling water still does not enter the temperature adjustment chamber 3, and the heating tube 17 starts to heat the cooling water, and a temperature adjustment sensor 4 is installed in the cooling jacket 2, and the temperature adjustment sensor 4 is used to control the temperature of the cooling water in the cooling jacket 2.

[0051] During the movement of the heating tube 17 toward the water inlet 10, one end of the plug block 20 facing the plug hole 21 is located in the slide groove 22, and the limiting spring is stretched and deformed. When the plug block 20 moves to the position of the plug hole 21, the second electromagnet 23 is powered off and demagnetized. Under the elastic force of the limiting spring, the plug block 20 is plugged into the plug hole 21, and the other end of the plug block 20 is still located in the adsorption hole 24. Therefore, it is only necessary to energize the second electromagnet 23 and adsorb the plug block 20, and then the plug block 20 can be pulled out of the plug hole 21; when the heating tube 17 is fixed in the temperature adjustment chamber 3, the first electromagnet 19 is powered off, and the heating tube 17 is separated from the phase change tube 6, so that the heating tube 17 can better heat the cooling water to prevent the phase change tube 6 from absorbing the heat of the heating tube 17, and then with the help of the control of the adjusting temperature sensor 4, the constant temperature state of the cooling water can be achieved.

[0052] The above are all preferred embodiments of the present application, and the protection scope of the present application is not limited thereto. Therefore, any equivalent changes made according to the structure, shape, and principle of the present application should be included in the protection scope of the present application.

Claims

1. A method for preparing a polyether macromonomer for a polycarboxylate water-reducing agent, characterized in that: The steps include: S1. Preparation of methyl allyl oligomer: 28.8 parts of methyl allyl alcohol and 2.4 parts of catalyst metal sodium were added to a reaction kettle (1). After the reaction, the product was added to 259.2 parts of methyl allyl alcohol, replaced with nitrogen, heated to 70°C, and 638.4 parts of ethylene oxide and 273.6 parts of propylene oxide were introduced. The reaction temperature was controlled to be 70-95°C, and the reaction time was 3.0-4.0 hours. After the reaction, the temperature was lowered to 70°C and the product was discharged to obtain a methyl allyl oligomer with a molecular weight of 300. S2, generating methallyl random polyether: adding 540 parts of methallyl oligomer obtained in step S1 into a reaction kettle (1), adding 0.3 parts of 18-crown-6 and hexachlorocyclotriphosphazene as catalysts, controlling the reaction temperature to 30-50°C, and the reaction time to 0.5-1.0 hour; after the reaction, nitrogen replacement is performed, the temperature is raised to 80°C, 882 parts of ethylene oxide and 378 parts of propylene oxide are introduced, the reaction temperature is controlled to 80-100°C, and the reaction time is 4.0-5.0 hours; after the reaction, the temperature is lowered to 80°C, and degassing is performed for 10-30 minutes to obtain methallyl random polyether with a molecular weight of 1000; A monitoring mechanism for monitoring the temperature at different positions is provided in the reactor (1); In both S1 and S2, the reaction temperature needs to be controlled by a cooling device, the cooling device comprising a cooling jacket (2) fixed outside the reactor (1), a water supply mechanism for introducing cooling water into the cooling jacket (2), a cooling mechanism for rapid cooling, and a heating mechanism for preheating the cooling water, the cooling jacket (2) being covered on the outer wall of the reactor (1), the cooling jacket (2) being further provided with a plurality of temperature adjustment chambers (3), the temperature adjustment chambers (3) being used for the operation of the cooling mechanism or the heating mechanism, and a temperature adjustment sensor (4) being provided in the cooling jacket (2); The heating mechanism comprises a heating frame (5) which is lifted and arranged below the cooling jacket (2), a plurality of phase change tubes (6) fixed in the heating frame (5), a power part (7) for lifting and lowering the heating frame (5), and an auxiliary component for assisting the heating of the phase change tube (6); the phase change tube (6) is filled with a phase change material for absorbing and releasing heat; the cooling jacket (2) is also provided with a regulating mechanism in the temperature regulating chamber (3) for controlling whether water enters; the phase change tube (6) is plugged into the temperature regulating chamber (3); the regulating mechanism comprises a regulating plate (8), an abutment block (9), and a transmission part for realizing that the regulating plate (8) can only move upward and the abutment block (9) can only move downward; the inner wall of the temperature regulating chamber (3) is provided with an inlet port which is connected to the cooling jacket (2). The water inlet (10) is provided with a regulating plate (8) which slides on the outer wall of the temperature regulating chamber (3) and slides in contact with the water inlet (10); the abutting block (9) slides on the side wall of the regulating plate (8) facing the temperature regulating chamber (3); the transmission part comprises an upper block (11), a lower block (13), an upper spring (15) and a lower spring (16); the side wall of the abutting block (9) is fixedly connected to the lower block (13); the regulating plate (8) is provided with a lower groove (14) for sliding the lower block (13); both ends of the lower groove (14) are closed; both ends of the lower spring (16) are fixedly connected to the upper end of the lower block (13) and the upper end of the lower groove (14) respectively; and the initial position of the lower block (13) is located at the top of the lower groove (14); The upper block (11) is fixedly connected to the side wall of the upper end of the adjustment plate (8); the cooling jacket (2) is provided with two upper grooves (12) on the outer wall of the temperature adjustment chamber (3) for the upper block (11) to slide; the two ends of the upper spring (15) are fixedly connected to the lower end of the upper block (11) and the lower end of the upper groove (12), respectively; the initial position of the upper block (11) is located at the bottom end of the upper groove (12); The upper block (11), the inner wall of the upper groove (12), the lower block (13) and the inner wall of the lower groove (14) are all arranged in a T-shape in horizontal cross-section; The auxiliary component comprises a heating tube (17) detachably connected to the phase change tube (6), a heating element (18) arranged in the heating tube (17), and a fixing portion for fixing the heating tube (17) in the temperature adjustment chamber (3); the heating tube (17) and the phase change tube (6) are adsorbed and connected via a first electromagnet (19); the heating tube (17) is located at the top end of the phase change tube (6); the heating tube (17) and the temperature adjustment chamber (3) are slidably adapted; the cooling mechanism comprises a cooling frame (25) arranged at the upper end of the cooling jacket (2) and a cooling element (25) for realizing the cooling; A reciprocating member (26) for lifting and lowering the temperature rack (25), a rotating ring (27) rotatably arranged on the temperature-reducing rack (25), a driving assembly for driving the rotating ring (27) to rotate, a plurality of temperature-reducing pipes (28) fixed on the rotating rack, an ice-making assembly for making ice for water in the temperature-reducing pipes (28), a circulation assembly for providing hot water to the temperature-reducing pipes (28), and a detection assembly for detecting whether ice making in the plurality of temperature-reducing pipes (28) is completed, the plurality of temperature-reducing pipes (28) are respectively plugged and adapted with the plurality of temperature-adjusting chambers (3), and the top end of the temperature-reducing pipes (28) is open; The ice-making assembly comprises a nozzle (33) fixed on the cooling rack (25) and a storage tank (32) for storing liquid nitrogen, the storage tank (32) being placed on the external environment, and the nozzle (33) facing the top opening of the cooling tube (28), the driving assembly causing the rotating ring (27) to rotate intermittently, and the angle of each rotation of the rotating ring (27) causing the top opening of the corresponding cooling tube (28) to face the nozzle (33).

2. The method for preparing a polyether macromonomer for polycarboxylate water-reducing agent according to claim 1, characterized in that: The fixing part comprises two plug-in blocks (20) and a second electromagnet (23); the heating tube (17) is provided with two slide grooves (22) near the bottom wall; the plug-in block (20) is elastically arranged in the slide grooves (22); the bottom side wall of the temperature regulating chamber (3) is provided with two plug-in holes (21); the plug-in block (20) is plugged into the plug-in holes (21); the bottom center of the heating tube (17) is provided with an adsorption hole (24) which is connected to both the slide grooves (22); the second electromagnet (23) is installed in the adsorption hole (24); and the ends of the two plug-in blocks (20) are adsorbed by the second electromagnet (23).

3. The method for preparing a polyether macromonomer for polycarboxylate water-reducing agent according to claim 2, characterized in that: The detection assembly comprises a detection needle (41) elastically arranged on the cooling rack (25), a handle (40) fixedly connected to the top of the detection needle (41), a reset portion for resetting the detection needle (41), a third electromagnet (44), a trigger member (45) for intermittently pushing the third electromagnet (44) to move toward one end of the handle (40), and a proximity switch (46), wherein the third electromagnet (44) moves toward the end of the handle (40) along a horizontal direction, the proximity switch (46) is electrically connected to the trigger member (45), and the proximity switch (46) and the third electromagnet (44) are respectively located on both sides of the detection needle (41).

4. The method for preparing a polyether macromonomer for polycarboxylate water-reducing agent according to claim 3, characterized in that: The monitoring mechanism comprises a monitoring frame (47) which is lifted and disposed in the reactor (1), a first temperature sensor (48) and a second temperature sensor (49); the first temperature sensor (48) and the second temperature sensor (49) are both fixed on the monitoring frame (47); the first temperature sensor (48) is close to the side wall of the reactor (1), and the second temperature sensor (49) is close to the center of the reactor (1).

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