Reaction device of epoxy succinic acid

Abstract

The utility model relates to the technical field of chemical engineering devices, in particular to an epoxy succinic acid reaction device. The utility model relates to a reaction device of epoxy succinic acid. The reaction device comprises a reaction kettle, a stirring mechanism and a gas circulating device, a feeding hole, an air outlet and a rotary stirring hole are formed in the top of the reaction kettle, a rotator is arranged in the reaction kettle, a rotating shaft of the rotator extends out of the reaction kettle from the rotary stirring hole, and a shell-and-tube constant-temperature heat exchanger is arranged on the outer wall of the reaction kettle; the rotator comprises a rotating pipe, a supporting rod, a scraping plate and an air outlet hole, the rotating pipe is supported and fixed on the reaction kettle and is provided with a driven gear, and transmission is carried out through a meshing motor and the rotating pipe; the gas circulation device comprises a ventilation pipeline, a high-temperature gas pump, a three-way valve, a gas inlet sealing end and a gas outlet sealing end. According to the reaction kettle, the problem of caking of maleic anhydride sodium salt on the inner wall of the reaction kettle is greatly reduced through stirring of the scraper and high-temperature circulation of gas, and the problem that maleic anhydride is sublimated and condensed on the inner wall of the reaction kettle is also solved through high-temperature circulation operation of the gas.

Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of chemical industry, especially relates to a reaction device of epoxy succinic acid. BACKGROUND

[0002] Polyepoxysuccinic acid (PESA) is an excellent circulating water scale inhibitor, which has good scale inhibition and dispersion performance for calcium carbonate, calcium sulfate, barium sulfate and other salts in water, and is environment-friendly and degradable.

[0003] The mainstream method for producing polyepoxysuccinic acid in industry is to use maleic anhydride as raw material, react with hydrogen peroxide under the condition of a catalyst to generate epoxy succinic acid, and then catalyze ring-opening polymerization to generate polyepoxysuccinic acid. In the process of generating epoxy succinic acid, two problems occur: first, due to the self characteristics and water solubility of epoxy succinic acid, it will deposit on the inner wall of the reaction kettle with liquid phase, form dense solid clumps, which are hard to remove, and in the subsequent ring-opening polymerization reaction, the epoxy succinic acid deposited on the wall will not participate in the reaction, resulting in reduced product yield and increased reactor cleaning cost; second, maleic anhydride will partially sublimate and condense on the upper part of the reactor wall during the synthesis of epoxy succinic acid, which will reduce the effective utilization rate of the raw material maleic anhydride and pollute the subsequent ring-opening polymerization product.

[0004] In order to solve the problem of clumping on the inner wall of the reaction kettle, the patent CN218281682U designs a reaction kettle that avoids residual materials on the inner wall, which can effectively inhibit the clumping on the inner wall of the reaction kettle by scraping the wall with the stirring rod and the scraping piece to scrape the adhered raw materials and products on the inner wall. However, when this reaction kettle is used in the production of epoxy succinic acid, it is found that there are still thin layers of solid clumps on the inner wall of the reaction kettle below the liquid surface, and there is condensed maleic anhydride on the inner wall of the reaction kettle above the liquid surface, which cannot meet the conversion requirements of maleic anhydride. Therefore, the present application provides a reaction device for epoxy succinic acid, which can effectively solve the above problems. SUMMARY

[0005] In order to solve the above problems, the utility model provides a reaction device for epoxy succinic acid, which can effectively solve the problem of clumping of epoxy succinic acid raw material maleic anhydride sodium salt on the inner wall of the reaction kettle, and avoid the condensation of maleic anhydride on the inner wall due to sublimation, thereby improving the utilization rate of raw materials and yield.

[0006] The specific technical scheme is as follows:

[0007] The reaction device for epoxy succinic acid of the utility model, comprising: a reaction kettle, a stirring mechanism and a gas circulation device;

[0008] The top of the reactor is provided with a feeding port, a gas outlet, a rotating stirring hole and a supporting bearing, the supporting bearing is arranged at the rotating stirring hole, the bottom is provided with supporting legs and a discharging port, the inside is provided with a rotator, the rotating shaft of the rotator extends out of the reactor from the rotating stirring hole, and the outer wall of the reactor is provided with a shell-and-tube constant-temperature heat exchanger.

[0009] The rotator comprises a rotating pipe, a supporting rod, a scraper and a gas outlet hole, the supporting bearing is horizontally fixed at the center position of the top of the reactor, is tightly engaged with the upper portion of the rotating pipe, and achieves the purpose of supporting and fixing the rotating pipe on the reactor, a driven gear is arranged on the rotating pipe, a motor is arranged, and a driving gear is arranged in meshing transmission with the driven gear.

[0010] The gas circulating device comprises a gas pipeline, a high-temperature gas pump, a three-way valve, a gas inlet end and a gas outlet end, the gas pipeline is a double-layer sleeve structure, the inner pipe is used for circulating gas, the heating device is arranged between the outer pipe and the inner pipe, the high-temperature gas pump and the three-way valve are inlaidly connected to the gas pipeline, and the two ends of the gas pipeline are the gas inlet end and the gas outlet end, the gas inlet end is connected with the gas outlet, and the gas outlet end is connected with the top of the rotating pipe of the rotator.

[0011] According to the reaction device for epoxy succinic acid, the feeding port is a tubular port, is communicated between the inside and outside of the kettle body, the tubular port is provided with a rotating thread, a pipeline matched with the tubular port is tightly connected through the rotating thread, a valve is arranged below the thread of the tubular port, and the gas outlet is connected with the gas circulating device.

[0012] According to the reaction device for epoxy succinic acid, the supporting legs are arranged in a group and are uniformly distributed at the bottom of the kettle body and used for supporting the kettle body.

[0013] According to the reaction device for epoxy succinic acid, the discharging port is a tubular port, is communicated between the inside and outside of the kettle body, the tubular port is provided with a rotating thread, a pipeline matched with the tubular port is tightly connected through the rotating thread, and a valve is arranged below the thread of the tubular port.

[0014] According to the reaction device for epoxy succinic acid, the lower half of the reactor is spherical, the upper half is conical, and the included angle between the conical shape and the vertical plane ranges from 30° to 45°.

[0015] According to the reaction device for epoxy succinic acid, the material of the inner wall of the reactor is enamel or polytetrafluoroethylene, the rotating pipe and the supporting rod are made of steel, and the scraper is made of steel or polytetrafluoroethylene.

[0016] According to the reaction device for epoxy succinic acid, the supporting rod is horizontally fixed on the rotating pipe, the scraper is fixedly connected with the tail ends of the plurality of supporting rods in a vertical mode, each scraper is 1-2 cm wide, surrounds the inner wall of the kettle for one round, and the distance between the tail ends of the supporting rods and the scraper and the inner wall of the kettle ranges from 1.5 cm to 2.5 cm.

[0017] According to the reaction device of the epoxy succinic acid, the number of the scrapers on the rotator is 2-4, which are uniformly distributed around the rotating tube and fixed at the tail end of the support rod.

[0018] According to the reaction device of the epoxy succinic acid, the rotating tube and the support rod are cylindrical, and the inside is provided with a gas pipeline with an inner diameter of 1-2 cm; the port of the support rod is provided with an air outlet hole, which is a circular hole with an inner diameter of 0.5-1 cm; the air outlet hole is close to the inner wall of the reaction kettle; and a one-way valve is arranged at the air outlet hole to prevent the liquid in the kettle from flowing into the air pipeline.

[0019] According to the reaction device of the epoxy succinic acid, the upper end of the shell-and-tube constant-temperature heat exchanger is provided with a heat exchange outlet, and the bottom end is provided with a heat exchange inlet; the heat exchange inlet is connected with a circulating hot water supply pipeline through a pipeline and is connected with a valve and a transmission pump in series; and the heat exchange outlet is connected with a circulating hot water recovery pipeline through a pipeline and is connected with a one-way valve in series.

[0020] The reaction device of the epoxy succinic acid has the following beneficial effects:

[0021] The reaction device of the epoxy succinic acid provided by the utility model greatly reduces the caking problem of maleic anhydride sodium salt on the inner wall of the reaction kettle through scraper stirring and high-temperature circulation of the gas; the high-temperature circulation operation of the gas also solves the problem that maleic anhydride is condensed on the inner wall of the reaction kettle due to sublimation; the solving of the two problems greatly improves the raw material conversion rate and utilization rate, reduces the product maleic anhydride content, improves the product stability and quality, and is beneficial to industrial production. BRIEF DESCRIPTION OF DRAWINGS

[0022] Figure 1 It is a perspective view of the utility model,

[0023] Figure 2 It is a sectional view of the utility model,

[0024] Figure 3 It is a perspective view of the rotator structure,

[0025] Reference signs:

[0026] The reaction kettle, 11, the feed inlet, 12, the air outlet, 13, the support bearing, 14, the support leg, 15, the discharge port, 16, the rotator, 161, the rotating tube, 162, the support rod, 163, the scraper, 164, the air outlet hole, 17, the shell-and-tube constant-temperature heat exchanger, 171, the heat exchange outlet, 172, the heat exchange inlet, 18, the driven gear, 19, the motor, 2, the gas circulation device, 21, the air pipeline, 22, the high-temperature gas pump, 23, the three-way valve, 24, the air inlet end, 25, the air outlet end. DETAILED DESCRIPTION

[0027] The specific content of the utility model will be further described below:

[0028] The utility model discloses an epoxy succinic acid's reaction device, including reation kettle 1, stirring mechanism and gas circulation device 2,

[0029] The top of reation kettle 1 is equipped with feed inlet 11, gas outlet 12, rotary stirring hole and support bearing 13, support bearing 13 is arranged at rotary stirring hole, the bottom is equipped with support leg 14 and discharge port 15, and the inside is equipped with rotator 16, and the rotation axis of rotator 16 extends from rotary stirring hole and stretches out reation kettle, and the outer wall of reation kettle is equipped with shell and tube type constant temperature heat exchanger 17;

[0030] Rotator 16 includes rotary tube 161, support rod 162, scraper 163 and gas outlet hole 164, support bearing 13 is horizontally fixed at the center position of the top of reation kettle 1, is tightly engaged with the upper portion of rotary tube 161, reaches the purpose that rotary tube 161 is supported and fixed on reation kettle 1, is equipped with driven gear 18 on the upper surface of support bearing 13, is equipped with motor 19 and is equipped with driving gear and driven gear 18 meshing transmission.

[0031] The utility model discloses a gas circulation device 2 including air pipe 21, high temperature gas pump 22, three way valve 23, gas inlet end 24 and gas outlet end 25, air pipe 21 is double layer sleeve pipe structure, and the inner tube is ventilated, is used for gas circulation, and heating device is installed between the outer tube and the inner tube, high temperature gas pump 22 and three way valve 23 are embeddedly connected on air pipe 21, and the both ends of air pipe are gas inlet end 24 and gas outlet end 25, gas inlet end 24 is connected with gas outlet 12, and the top of the rotary tube 161 of rotator is connected with gas outlet end 25.

[0032] Feed inlet 11 is tubular mouth, and the inside and outside of kettle body are communicated, and the tubular mouth is equipped with rotary thread, and is closely connected with the matched pipeline through screw, and the valve is arranged below the thread of tubular mouth, and gas outlet 12 is connected with gas circulation device 2. Support leg 143 or 4 groups are evenly distributed at the bottom of kettle body and are used to support kettle body.

[0033] Discharge port 15 is tubular mouth, and the inside and outside of kettle body are communicated, and the tubular mouth is equipped with rotary thread, and is closely connected with the matched pipeline through screw, and the valve is arranged below the thread of tubular mouth. The lower half of reation kettle 1 is spherical, and the upper half is conical, and the included angle between the conical and the vertical surface is 30 ° ~ 45 °.

[0034] The inner wall material of reation kettle 1 is enamel or polytetrafluoroethylene, the rotary tube 161 and support rod 162 are steel materials, and the scraper 163 is steel material or polytetrafluoroethylene.

[0035] Supporting rods 162 are horizontally fixed on the rotating tube 161, and the scraper 163 is vertically fixed with the tail end of the plurality of supporting rods. Each scraper is 1-2 cm wide, and surrounds the inner wall of the reactor. The distance between the tail end of the supporting rod and the inner wall of the reactor is 1.5-2.5 cm. The number of scrapers 163 on the rotator 16 is 2-4, which are evenly distributed around the rotating tube 161 and fixed on the tail end of the supporting rod 162.

[0036] Specifically, the rotating tube 161 and the supporting rod 162 are cylindrical, and the inside is provided with a gas pipeline with an inner diameter of 1-2 cm. The port of the supporting rod is provided with a gas outlet hole 164, which is a circular hole with an inner diameter of 0.5-1 cm. The gas outlet hole 164 is close to the inner wall of the reactor. A one-way valve is arranged at the gas outlet hole 164 to prevent the liquid in the reactor from flowing into the air pipeline.

[0037] The upper end of the shell-and-tube constant-temperature heat exchanger 17 in the device is provided with a heat exchange outlet 171, and the bottom end is provided with a heat exchange inlet 172. The heat exchange inlet 172 is connected to the circulating hot water supply pipeline through a pipeline and is connected in series with a valve and a transmission pump. The heat exchange outlet 171 is connected to the circulating hot water recovery pipeline through a pipeline and is connected in series with a one-way valve.

[0038] The utility model will be further described in detail below in combination with the drawings and specific embodiments.

[0039] Main raw material equipment specifications: the widest inner diameter of the reactor is 2 m, the upper part is conical with an inclination angle of 4°, the number of scraper of the rotator is 2, which is equally divided around the rotating tube 4, and the width of the scraper is 1 cm; the hydrogen peroxide is an industrial grade with a concentration of 27.5%, the maleic anhydride is an industrial grade, and the sodium hydroxide aqueous solution is a self-produced product of the company with a mass fraction of 32%.

[0040] The embodiments of using the device are as follows:

[0041] Step 1: 200 kg of maleic anhydride and 300 kg of water are sequentially added to the reactor 1 from the feed inlet 11, then the sodium hydroxide aqueous solution is added dropwise, the pH of the system is adjusted to 5-6, the rotator 16 is started, the rotating speed is 10 r / min, the corresponding valve is opened, the shell-and-tube constant-temperature heat exchanger 17 is started, the hot water with a temperature of 50±2℃ is controlled to flow into the inlet 172 and flow out of the outlet 172, the medium in the interlayer of the heating air pipeline 201 is heated, the temperature is controlled to be 100-105℃, the high-temperature gas pump 22 is started, and the gas sequentially passes through the gas pipeline in the rotating rod 161 and the supporting rod 162 from the gas outlet hole 164 into the inside of the reactor 1, and then returns to the gas circulation device 2 from the gas outlet 12 of the reactor, thereby completing the circulation of the gas.

[0042] Step 2: Start to add 350 kg of mass fraction 27.5% hydrogen peroxide into the reaction kettle 1, 2 h drop is completed, heat preservation 1 h, the reaction process uses liquid alkali to control the kettle pH at 5~6, the heat preservation process is controlled by the three-way valve 203, part of the air is added into the gas circulation system, after heat preservation, the high temperature gas pump 202 and the corresponding valve are closed, the gas circulation is stopped, the cooling is started, after cooling to room temperature, the product epoxy succinic acid aqueous solution 1129.4 kg is obtained by filtration.

[0043] Through detection, the content of maleic anhydride in the product is 0.02%, the content of epoxy succinic acid is 23.24%, and the yield (calculated from maleic anhydride) is 97.45%.

[0044] Through the scraper stirring and the high-temperature circulation of the gas, the caking problem of maleic anhydride sodium salt on the inner wall of the reaction kettle is greatly reduced, and the high-temperature circulation operation of the gas also solves the problem that maleic anhydride is condensed on the inner wall of the reaction kettle due to sublimation, and the solution of the two problems greatly improves the conversion rate and utilization rate of the raw materials, and reduces the content of maleic anhydride in the product. For ordinary skilled persons in the art, according to the teaching of the present application, the changes, modifications, replacements and modifications of the embodiments without departing from the principles and spirits of the present application still fall within the protection scope of the present application.

Claims

1. An apparatus for the reaction of epoxy succinic acid, characterized by, Include: The reaction kettle (1), stirring mechanism and gas circulation device (2); The reaction kettle (1) top is equipped with feed inlet (11), gas outlet (12), rotating stirring hole and support bearing (13), support bearing (13) is arranged at rotating stirring hole, bottom is equipped with support leg (14) and discharge port (15), inside is equipped with rotator (16), the rotation axis of rotator (16) from rotating stirring hole stretches out the reaction kettle, the outer wall of reaction kettle is equipped with shell and tube type constant temperature heat exchanger (17); The rotator (16) includes rotating tube (161), support rod (162), scraper (163) and gas outlet hole (164), the support bearing (13) is horizontally fixed at the center position of the top of the reaction kettle (1), is closely engaged with the upper portion of rotating tube (161), reaches the purpose of supporting and fixing rotating tube (161) on the reaction kettle (1), is equipped with driven gear (18) on rotating tube (161), is equipped with motor (19) and is equipped with driving gear and driven gear (18) meshing transmission; The gas circulation device (2) includes vent pipe (21), high-temperature gas pump (22), three-way valve (23), gas inlet end (24) and gas outlet end (25), the vent pipe (21) is double-layered sleeve structure, the inner tube is vented, is used for gas circulation, heating device is installed between the outer tube and the inner tube, the high-temperature gas pump (22) and three-way valve (23) are connected on the vent pipe (21), and the vent pipe two ends are gas inlet end (24) and gas outlet end (25), the gas inlet end (24) is connected with the gas outlet (12), and the gas outlet end (25) is connected with the top of the rotating tube (161) of the rotator.

2. The reaction apparatus for epoxy succinic acid according to claim 1, characterized by, The feed inlet (11) is a tubular port, which is connected inside and outside the kettle body, and the tubular port is provided with a rotating thread, which is tightly connected with a matched pipeline through screwing, and a valve is arranged below the thread of the tubular port, and the gas outlet (12) is connected with the gas circulation device (2).

3. The reaction apparatus for epoxy succinic acid according to claim 1, characterized by, The support leg (14) is 3 or 4 in a group, and is evenly distributed at the bottom of the kettle body, and is used for supporting the kettle body.

4. The reaction apparatus for epoxy succinic acid according to claim 1, characterized by, The discharge port (15) is a tubular port, which is connected inside and outside the kettle body, and the tubular port is provided with a rotating thread, which is tightly connected with a matched pipeline through screwing, and a valve is arranged below the thread of the tubular port.

5. The reaction apparatus for epoxy succinic acid according to claim 1, characterized by, The lower half of the reaction kettle (1) is spherical, and the upper half is conical, and the included angle between the conical shape and the vertical plane is in the range of 30°-45°.

6. The reaction apparatus for epoxy succinic acid according to claim 1, characterized by, The inner wall material of the reaction kettle (1) is enamel or polytetrafluoroethylene, the rotating tube (161) and the support rod (162) are steel materials, and the scraper (163) is steel or polytetrafluoroethylene.

7. The reaction apparatus for epoxy succinic acid according to claim 1, characterized by The support rod (162) is horizontally fixed on the rotating tube (161), and the scraper (163) is fixedly connected with the tail ends of the plurality of support rods perpendicularly, each scraper is 1-2 cm wide, surrounds the inner wall of the kettle, and the distance between the tail ends of the support rods and the scraper and the inner wall of the kettle is 1.5-2.5 cm.

8. The reaction apparatus for epoxy succinic acid according to claim 7, characterized by, The number of scrapers (163) on the rotator (16) is 2-4, which are evenly distributed around the rotating tube (161) and fixed at the tail ends of the support rods (162).

9. The reaction apparatus for epoxy succinic acid according to claim 7, characterized by, The rotating tube (161) and the supporting rod (162) are cylindrical, and the inside is provided with a gas pipeline with an inner diameter of 1-2 cm. The port of the supporting rod is provided with an air outlet hole (164), which is a circular hole with an inner diameter of 0.5-1 cm. The air outlet hole (164) is close to the inner wall of the reaction kettle, and a one-way valve is arranged at the air outlet hole (164) to prevent the liquid in the kettle from flowing into the air pipeline.

10. The reaction apparatus for epoxy succinic acid according to claim 7, characterized by, The upper end of the shell-and-tube constant-temperature heat exchanger (17) is provided with a heat exchange outlet (171), and the bottom end is provided with a heat exchange inlet (172). The heat exchange inlet (172) is connected to the circulating hot water supply pipeline through a pipeline and is connected in series with a valve and a transmission pump. The heat exchange outlet (171) is connected to the circulating hot water recovery pipeline through a pipeline and is connected in series with a one-way valve.

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