Device for preparing acetone glycerol acetal and method for preparing acetone glycerol acetal using the device

Abstract

The invention discloses a device for preparing acetone glycerol acetal and a method for preparing acetone glycerol acetal by using the device. The method comprises the following steps: a. loading an acid catalyst into a reactor, setting a certain temperature of a jacket heat transfer oil and putting it into use; b. continuously feeding glycerol and acetone in a specific proportion into a tubular reactor through a metering pump, with materials entering from the bottom and exiting from the top; c. performing process sampling and monitoring, collecting materials at the reactor outlet into a collecting bottle for standby use; d. collecting a certain amount of reaction liquid and transferring it into a three-necked flask; e. controlling the top temperature to be greater than 100 DEG C, stirring the solution in the three-necked flask by using the device for preparing acetone glycerol acetal, and removing unreacted acetone, water and other impurities; f. collecting products, and stopping extraction when the kettle temperature is higher than 160 DEG C. The application can improve the conversion rate of the reaction and reduce equipment investment.

Description

Technical Field

[0001] The invention belongs to the technical field of energy recycling, and in particular relates to a device for preparing acetone glycerol acetal and a method for preparing acetone glycerol acetal by using the device. Background Art

[0002] Acetone glycerol acetal is an important organic synthesis intermediate, which can be used as a solvent, plasticizer, pharmaceutical excipient, etc. Acetone glycerol acetal is prepared by condensation reaction of acetone and glycerol under the action of an acidic catalyst. In addition to traditional inorganic acids, there are also a large number of literature reports on the catalysts for the condensation reaction of acetone and glycerol, such as p-toluenesulfonic acid, aminosulfonic acid, molecular sieves, heteropoly acids, precious metals and other solid catalysts, which are basically produced in an intermittent manner. The condensation reaction of acetone and glycerol is a reversible reaction. The water generated during the reaction is not conducive to the right shift of the reaction, and at the same time reduces the catalytic activity of the catalyst, which is not conducive to the improvement of the conversion rate. In the reaction, water separation reagents are mostly used to remove the water generated by the reaction from the reaction system; however, the boiling point of acetone is low, and acetone is also removed from the reaction system while separating water. The low single-pass conversion rate, high equipment investment, cumbersome product post-processing process, and high energy consumption have become the biggest obstacles to the production of this product. Summary of the invention

[0003] The content of this application is used to introduce concepts in a brief form, which will be described in detail in the detailed implementation section below. The content of this application is not intended to identify the key features or essential features of the technical solution claimed for protection, nor is it intended to limit the scope of the technical solution claimed for protection.

[0004] In order to overcome the deficiencies of the prior art, the present invention provides a device for preparing acetone glycerol acetal and a method for preparing acetone glycerol acetal using the device.

[0005] In order to achieve the above-mentioned purpose, the present invention adopts the following technical scheme: a device for preparing acetone glycerol acetal, comprising: a base, placed on a table; a support rod, arranged on the base; a mounting block, arranged on the support rod; a motor, arranged on the mounting block; a stirring rod, connected to the output shaft of the motor; a receiving groove is provided on the stirring rod, a movable rod is provided in the receiving groove, one end of the movable rod is rotatably connected to the receiving groove; the motor can drive the movable rod to flip out of the receiving groove or flip into the receiving groove.

[0006] Furthermore, the stirring rod includes a first rod body and a second rod body, the first rod body is provided with a first movable groove, one end of the second rod body is inserted into the first movable groove, and the accommodating groove is provided on the second push rod.

[0007] Furthermore, the second rod body is provided with a first through cavity communicated with the accommodating groove, a rotating shaft is provided in the first through cavity, a first connecting rod is provided at the bottom of the rotating shaft, a baffle is provided at the bottom of the first connecting rod, a connecting rope is wound around the first connecting rod, one end of the connecting rope is fixedly connected to the movable rod; an arc-shaped spring sheet is provided on the inner wall of the accommodating groove.

[0008] Furthermore, a second through cavity is provided on the top of the first movable groove, a transmission shaft is provided in the second through cavity, an movable cavity is provided on the side wall of the second through cavity, a limit plate is provided on the transmission shaft, a first support spring is provided at the bottom of the movable cavity, a plurality of first ribs are provided on the top, and a first groove corresponding to the first rib is provided on the limit plate.

[0009] Furthermore, an installation cavity is provided on the installation block, and an installation tube is provided in the installation cavity. The installation tube passes through the installation cavity, and the first rod body is inserted in the installation tube. A support plate is provided in the installation tube, and one end of the first rod body is against the support plate. A second movable groove is provided on the first rod body, and a first fixed block is provided in the second movable groove. A connecting spring is provided on the first fixed block, and a fixing groove corresponding to the first fixed block is provided on the installation tube.

[0010] Furthermore, a first transmission wheel is provided on the mounting tube, a movable frame is provided in the mounting cavity, the movable frame is connected to the output shaft of the motor, and a second transmission wheel is provided on the movable frame for transmission cooperation with the first transmission wheel; a convex rod is also provided on the movable frame, and a transmission groove is provided on the convex rod for transmission cooperation with the transmission shaft.

[0011] Furthermore, the acetone glycerol preparation device also includes: a sleeve, which is sleeved on the support rod; a second connecting rod, which is arranged on the sleeve; a fixed plate, which is arranged in the sleeve; a third movable groove is provided on the inner wall of the sleeve, and the fixed plate is located in the third movable groove; and rubber pads are respectively provided on the top and bottom of the sleeve.

[0012] Furthermore, the acetone glycerol preparation device also includes: a ring, which is sleeved on the support rod; a first movable ring and a second movable ring, which are rotatably connected to the ring; a first clamping rod, which is arranged on the first movable ring; a second clamping rod, which is arranged on the second movable ring; the second movable ring is located below the first movable ring, and the first rod body is clamped between the first clamping rod and the second clamping rod.

[0013] Furthermore, the acetone glycerol preparation device also includes: a baffle rod, used to connect the first clamp rod and the second clamp rod; a first latch, used to connect the baffle rod and the first clamp rod; a second latch, used to connect the baffle rod and the second clamp rod; the first clamp rod is provided with a first connecting hole corresponding to the first latch, and the second clamp rod is provided with a second connecting hole corresponding to the second latch.

[0014] As another aspect of the present application, a method for preparing glycerol acetone acetal using the glycerol acetone acetal preparation device as described above is also disclosed, comprising the following steps:

[0015] a. The reactor is loaded with acidic catalyst, the jacket heat transfer oil is set to a certain temperature and put into use;

[0016] b. Glycerol and acetone in a specific ratio are continuously fed into the tubular reactor via a metering pump, with the materials entering from the bottom and exiting from the top;

[0017] c. Process sampling and monitoring, the materials at the reactor outlet are collected into a collection bottle for standby use;

[0018] d. Collect a certain amount of the reaction solution and transfer it into a three-necked flask;

[0019] e. Control the top temperature to be greater than 100°C, and use the acetone glycerol preparation device to stir the solution in the three-necked flask to remove unreacted acetone, water and other impurities;

[0020] f. Collect the product and stop collecting when the kettle temperature is higher than 160℃.

[0021] The invention is beneficial in that it provides a device for preparing acetone glycerol acetal, which improves the conversion rate of the reaction and reduces the equipment investment, and a method for preparing acetone glycerol acetal by using the device. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] The drawings constituting a part of this application are used to provide a further understanding of this application, so that other features, purposes and advantages of this application become more obvious. The illustrative embodiment drawings and their descriptions of this application are used to explain this application and do not constitute an improper limitation on this application.

[0023] In addition, throughout the drawings, the same or similar reference numerals represent the same or similar elements. It should be understood that the drawings are schematic and that the components and elements are not necessarily drawn to scale.

[0024] In the attached picture:

[0025] Figure 1 The figure is a schematic diagram of the structure of a device for preparing acetone glycerol in one embodiment of the present invention.

[0026] Figure 2 for Figure 1 A cross-sectional view of a stirring rod of the device for preparing glycerol acetone in the illustrated embodiment.

[0027] Figure 3 for Figure 2 Enlarged view of point A in .

[0028] Figure 4 for Figure 2 Enlarged view of point B in .

[0029] Figure 5 for Figure 2 Enlarged view of point C in the figure.

[0030] Figure 6 for Figure 2 Enlarged view of point D in .

[0031] Figure 7 for Figure 2 Enlarged view of point E in FIG.

[0032] Figure 8 for Figure 1 A cross-sectional view of a fixing rod of the device for producing solketal in the illustrated embodiment.

[0033] Fig. 9 for Figure 8 Enlarged view of point F in FIG.

[0034] Fig.10 for Figure 1 A cross-sectional view of a protrusion of the device for preparing glycerol acetone in the illustrated embodiment.

[0035] Fig.11 for Fig.10 Enlarged view of point G in .

[0036] Fig.12 for Figure 1 A cross-sectional view of a first latch of the apparatus for preparing glycerol acetone in the illustrated embodiment.

[0037] Fig.13 for Fig.12 Enlarged view of point H in the figure.

[0038] The meanings of the reference numerals in the figures are as follows:

[0039] 101, base; 102, support rod; 103, mounting block; 104, first rod body; 105, second rod body; 106, movable rod; 107, connecting rope; 108, sleeve; 1081, convex block; 109, push rod; 110, second connecting rod; 111, sleeve; 112, third connecting rod; 113, first movable ring; 114, second movable ring; 115, first clamping rod; 1151, first convex ring; 116, second clamping rod; 117, motor; 118, rotating shaft; 119, first connecting rod; 120, baffle; 121, arc-shaped spring piece; 122, support block; 123, support rod; 124, transmission shaft; 1241, limit plate; 125 , stop rod; 126, second latch; 127, first support spring; 128, mounting tube; 1281, first transmission wheel; 129, first fixing block; 1291, connecting spring; 130, movable frame; 1301, extension portion; 1302, second transmission wheel; 1303, convex rod; 131, East second support spring; 132, electromagnet; 133, fixing rod; 1331, second convex rib; 1332, extension rod; 134, third support spring; 135, fixing plate; 136, first threaded rod; 137, rubber pad; 138, connecting plate; 139, second threaded rod; 140, second fixing block; 141, first latch; 1411, third convex ring. DETAILED DESCRIPTION

[0040] Embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. Although certain embodiments of the present disclosure are shown in the accompanying drawings, it should be understood that the present disclosure can be implemented in various forms and should not be construed as being limited to the embodiments set forth herein. On the contrary, these embodiments are provided to provide a more thorough and complete understanding of the present disclosure. It should be understood that the drawings and embodiments of the present disclosure are only for exemplary purposes and are not intended to limit the scope of protection of the present disclosure.

[0041] It should also be noted that, for ease of description, only the parts related to the invention are shown in the drawings. In the absence of conflict, the embodiments and features in the embodiments of the present disclosure can be combined with each other.

[0042] It should be noted that the concepts such as "first" and "second" mentioned in the present disclosure are only used to distinguish different devices, modules or units, and are not used to limit the order or interdependence of the functions performed by these devices, modules or units.

[0043] It should be noted that the modifications of "one" and "plurality" mentioned in the present disclosure are illustrative rather than restrictive, and those skilled in the art should understand that unless otherwise clearly indicated in the context, it should be understood as "one or more".

[0044] The names of the messages or information exchanged between multiple devices in the embodiments of the present disclosure are only used for illustrative purposes and are not used to limit the scope of these messages or information.

[0045] The present disclosure will be described in detail below with reference to the accompanying drawings and in conjunction with embodiments.

[0046] like Figure 1-13 As shown, a device for preparing acetone glycerol acetal includes a base 101, a support rod 102, a mounting block 103, a motor 117 and a stirring rod; the base 101 is placed on a desktop; the support rod 102 is arranged on the base 101; the mounting block 103 is arranged on the support rod 102; the motor 117 is arranged on the mounting block 103; the stirring rod is connected to the output shaft of the motor 117; a receiving groove is provided on the stirring rod, and a movable rod 106 is provided in the receiving groove, and one end of the movable rod 106 is rotatably connected to the receiving groove; the motor 117 can drive the movable rod 106 to flip out of the receiving groove or flip into the receiving groove.

[0047] By storing the movable rod 106 in the receiving groove, the diameter of the stirring rod is reduced, so that the stirring rod can be easily inserted into the flask, avoiding the stirring rod from colliding with the inner wall of the flask mouth, and protecting the flask. The stirring rod can adapt to a variety of small-caliber vessels; after the stirring rod is inserted into the flask, the motor 117 drives the movable rod 106 to flip out of the receiving groove, and the movable rod 106 protrudes from the side wall of the stirring rod. When the motor 117 drives the stirring to rotate, the movable rod 106 stirs the solution, thereby improving the stirring effect of the stirring rod on the solution.

[0048] Specifically, the stirring rod includes a first rod body 104 and a second rod body 105. The first rod body 104 is provided with a first movable groove. One end of the second rod body 105 is inserted into the first movable groove. The receiving groove is provided on the second push rod 109. The second rod body 105 can move relative to the first rod body 104 to adjust the overall length of the stirring rod to adapt to vessels of different heights and improve the practicality of the device.

[0049] The second rod body 105 is provided with a first through cavity which is communicated with the accommodating groove, a rotating shaft 118 is provided in the first through cavity, a first connecting rod 119 is provided at the bottom of the rotating shaft 118, a baffle 120 is provided at the bottom of the first connecting rod 119, a connecting rope 107 is wound around the first connecting rod 119, one end of the connecting rope 107 is fixedly connected to the movable rod 106; an arc-shaped spring piece 121 is provided on the inner wall of the accommodating groove, and the arc-shaped spring piece 121 is located at the top of the side wall of the accommodating groove.

[0050] A second through cavity is provided on the top of the first movable groove, and a transmission shaft 124 is provided in the second through cavity. The rotating shaft 118 is a tubular structure, and one end of the transmission shaft 124 is inserted in the rotating shaft 118, and the transmission shaft 124 cooperates with the rotating shaft 118 in transmission. An movable cavity is provided on the side wall of the second through cavity, and a limit plate 1241 is provided on the transmission shaft 124. A first supporting spring 127 is provided at the bottom of the movable cavity, and a plurality of first ribs are provided on the top. A first groove corresponding to the first rib is provided on the limit plate 1241; the first supporting spring 127 pushes the limit plate 1241 against the top surface of the movable cavity, and the first rib is embedded in the first groove so that the limit plate 1241 is fixedly connected to the movable cavity, and the rotating shaft 118 is fixed by fixing the transmission shaft 124.

[0051] The mounting block 103 is provided with a mounting cavity, in which a mounting tube 128 is provided, and the mounting tube 128 passes through the mounting cavity. The first rod body 104 is inserted in the mounting tube 128, and a support plate is provided in the mounting tube 128. A through hole is provided on the support plate for the transmission shaft 124 to pass through. One end of the first rod body 104 is against the support plate, and a second movable groove is provided on the first rod body 104. A first fixing block 129 is provided in the second movable groove. A connecting spring 1291 is provided on the first fixing block 129, and one end of the connecting spring 1291 is fixedly connected to the inner wall of the second movable groove. There is a fixing groove corresponding to the first fixing block 129, and the first fixing block 129 is provided with an inclined surface. When installing the stirring rod, the stirring rod is directly inserted into the mounting tube 128, the first fixing block 129 is aligned with the fixing groove, the first fixing block 129 is inserted into the fixing groove, and the first fixing block 129 and the support plate cooperate with each other to fix the stirring rod on the mounting tube 128; when replacing the stirring rod, the first fixing block 129 is pushed into the second movable groove, and the stirring rod is removed from the mounting tube 128 after the first fixing block 129 is moved out of the fixing groove, and the stirring rod is quickly replaced.

[0052] A first transmission wheel 1281 is provided on the mounting tube 128, and a movable frame 130 is provided in the mounting cavity. The movable frame 130 is a disc-shaped structure. The movable frame 130 is connected to the output shaft of the motor 117. An extension portion 1301 is provided at the bottom of the movable frame 130, and a second transmission wheel 1302 that cooperates with the first transmission wheel 1281 is provided on the extension portion 1301; the movable frame 130 is also provided with a convex rod 1303, and the convex rod 1303 is provided with a transmission groove that cooperates with the transmission shaft 124; a second supporting spring and an electromagnet 132 are provided at the bottom of the movable cavity, and the top of the second supporting spring is against the movable frame 130, and the movable frame 130 is made of iron alloy.

[0053] A support block 122 is provided in the receiving groove, and the movable rod 106 rests on the support block 122 after being flipped out of the receiving groove, and the movable rod 106 can only be flipped to a horizontal state by means of the support block 122; a storage groove is provided on the movable rod 106, and a plurality of support rods 123 are provided in the storage groove, and one end of the support rod 123 is rotatably connected to the storage groove; when the movable rod 106 is in the receiving groove, the support rod 123 is stored in the storage groove under the action of gravity; after the movable rod 106 is flipped out of the receiving groove, the support rod 123 is flipped out of the storage groove under the action of gravity, and the support rod 123 is used to increase the stirring area of ​​the movable rod 106, thereby further improving the stirring effect of the stirring rod on the solution.

[0054] Before the stirring rod is inserted into the flask, the movable rod 106 is in the receiving groove, the connecting rope 107 is in a tightened state, and the stirring rod is only a rod body, which can be easily inserted into the flask to avoid collision with the inner wall of the bottle mouth when the stirring rod is inserted into the flask; after the stirring rod is inserted into the flask, the electromagnet 132 is energized to attract the movable frame 130 to move downward, and the second transmission wheel 1302 is staggered with the first transmission wheel 1281 when the movable frame 130 moves, and the transmission groove is sleeved on the transmission shaft 124 when the movable frame 130 moves, and the top surface of the transmission groove is against the top of the transmission shaft 124 to push the transmission The movable shaft 124 moves toward the second rod body 105, and the limit plate 1241 moves to the middle position of the movable cavity. When the motor 117 drives the movable frame 130 to rotate, the transmission shaft 124 is driven to rotate, and the transmission shaft 124 drives the rotating shaft 118 to rotate. The connecting rope 107 is rotated out of the first connecting rod 119, and the arc-shaped spring piece 121 pushes the movable rod 106 out of the receiving groove. The movable rod 106 is turned out of the receiving groove to stir the solution; the movable rod 106 is turned to a horizontal state and abuts against the support block 122, and the support rod 123 is rotated out of the receiving groove, and the electromagnet 132 When the power is off, the second supporting spring pushes the movable frame 130 to move back and reset, the second transmission wheel 1302 moves to the first transmission wheel 1281 to form a transmission match with the first transmission wheel 1281, the transmission groove is disengaged from the transmission shaft 124, the first supporting spring 127 pushes the limit plate 1241 to move to the top of the movable cavity, the first convex rib is embedded in the first groove to fix the transmission shaft 124, the motor 117 drives the movable frame 130 to rotate, the second transmission wheel 1302 drives the first transmission wheel 1281 to rotate, the mounting tube 128 drives the stirring rod to rotate, and the movable rod 106 and The support rod 123 cooperates to stir the solution; after the solution treatment is completed, the electromagnet 132 is energized again so that the motor 117 drives the transmission shaft 124 to rotate, and the connecting rope 107 is wound around the first connecting rod 119. The connecting rope 107 pulls the top of the movable rod 106 to move upward, and the movable rod 106 flips into the receiving groove. After the movable rod 106 enters the receiving groove, the electromagnet 132 is powered off, and the limit plate 1241 is fixed on the top surface of the movable cavity. The movable rod 106 is received in the receiving groove, and the support rod 123 is in the receiving groove, so the stirring rod can be conveniently taken out of the flask.

[0055] Furthermore, the acetone glycerol preparation device also includes a sleeve 108 and a second connecting rod 110, the sleeve 108 is sleeved on the support rod 102; the second connecting rod 110 is arranged on the sleeve 108; a third movable groove is provided on the inner wall of the sleeve 108, a fixing plate 135 is provided in the third movable groove, a first threaded rod 136 is rotatably connected to the fixing plate 135, a first threaded hole is provided on the side wall of the third movable groove, and the first threaded rod 136 passes through the first threaded hole; rubber pads 137 are respectively provided on the top and bottom of the sleeve 108, and the rubber pad 137 at the top of the sleeve 108 and the rubber pad 137 at the bottom are arranged oppositely, that is, the rubber pad 137 at the top of the sleeve 108 and the rubber pad 137 at the bottom are respectively located on both sides of the inner wall of the sleeve 108.

[0056] A connecting groove is provided on the mounting block 103, and the second connecting rod 110 is inserted into the connecting groove. The mounting block 103 can move relative to the second connecting rod 110, but the second connecting rod 110 cannot escape from the connecting groove. A fourth movable groove is provided at the bottom of the connecting groove, and a fixing rod 133 is provided in the fourth movable groove. A plurality of second ribs 1331 are provided on the fixing rod 133, and a plurality of second grooves corresponding to the second ribs 1331 are provided at the bottom of the second connecting rod 110; a third supporting spring 134 is provided at the bottom of the fixing rod 133, and the third supporting spring 134 rests on the bottom surface of the fourth movable groove, and an extension rod 1332 is provided at the top, and the extension rod 1332 passes through the top of the fourth movable groove, and a push rod 109 is provided on the extension rod 1332.

[0057] The mounting block 103 can be moved relative to the sleeve 108 to adjust the position of the stirring rod. At the same time, the sleeve 108 can slide along the support rod 102 to adjust the height of the mounting block 103. When moving the mounting block 103, the push rod 109 is pushed in the direction of the mounting block 103, and the push rod 109 drives the fixing rod 133 to move to the bottom of the fourth movable groove, and the fixing rod 133 is disengaged from the second connecting rod 110, which can conveniently move the position of the mounting block 103. After releasing the push rod 109, the third supporting spring 134 pushes the fixing rod 133 to move upward so that the fixing rod 133 is against the bottom surface of the second connecting rod 110, and the second rib 1331 is embedded in the second groove so that the mounting block 103 is fixed on the second connecting rod 110, completing the adjustment of the stirring rod position; when adjusting the height of the mounting block 103, the first threaded rod 136 is rotated, and the fixing plate 135 moves to the third movable groove. After the fixing plate 135 is against the support rod 102, the fixing plate 135 squeezes the side wall of the support rod 102 so that the inner wall of the sleeve 108 also presses against the support rod 102, thereby fixing the sleeve 108 on the support rod 102.

[0058] Furthermore, the acetone glycerol preparation device also includes a sleeve 111, a first movable ring 113, a second movable ring 114, a first clamping rod 115 and a second clamping rod 116; the sleeve 111 is sleeved on the support rod 102; the first movable ring 113 and the second movable ring 114 are rotatably connected to the sleeve 111; the first clamping rod 115 is arranged on the first movable ring 113; the second clamping rod 116 is arranged on the second movable ring 114; the second movable ring 114 is located below the first movable ring 113, and the first rod body 104 is clamped between the first clamping rod 115 and the second clamping rod 116.

[0059] A third connecting rod 112 is provided on the ring 111, a third through cavity is provided on the sleeve 108, the third connecting rod 112 is inserted in the third through cavity, a protrusion 1081 is provided on the sleeve 108, a cavity communicating with the third through cavity is provided on the protrusion 1081, a second fixing block 140 is provided in the cavity, a connecting plate 138 is provided on the second fixing block 140, a second threaded rod 139 is rotatably connected to the connecting plate 138, a second threaded hole is provided on the side wall of the cavity, and the second threaded rod 139 is passed through the second threaded hole.

[0060] The acetone glycerol preparation device also includes a blocking rod 125, a first latch 141 and a second latch 126; the blocking rod 125 is used to connect the first clamping rod 115 and the second clamping rod 116; the first latch 141 is used to connect the blocking rod 125 and the first clamping rod 115; the second latch 126 is used to connect the blocking rod 125 and the second clamping rod 116; the first clamping rod 115 is provided with a first connecting hole corresponding to a plurality of first latches 141, the second clamping rod 116 is provided with a plurality of second connecting holes corresponding to the second latches 126, a first convex ring 1151 is provided on the inner wall of the first connecting hole, a second convex ring is provided on the inner wall of the second connecting hole, a third convex ring 1411 is provided on the first latch 141, and a fourth convex ring is provided on the second latch 126, and the first latch 141 and the second latch 126 can be conveniently fixed in the first connecting hole and the second connecting hole by cooperation between the convex rings.

[0061] There are two blocking rods 125. When the first clamping rod 115 and the second clamping rod 116 are parallel, the two blocking rods 125 are connected to the first clamping rod 115 and the second clamping rod 116 to form a quadrilateral structure to position the first rod body 104; when the first clamping rod 115 and the second clamping rod 116 are obliquely intersected, only one blocking rod 125 is required to connect the first clamping rod 115 and the second clamping rod 116, and the blocking rod 125, the first clamping rod 115 and the second clamping rod 116 form a triangular structure to position the first rod body 104.

[0062] The second fixing block 140 can be controlled to move by rotating the second threaded rod 139, so that the ring 111 can move relative to the sleeve 108, ensuring that the first clamping rod 115 and the second clamping rod 116 are both on the side of the first rod body 104; the third connecting rod 112 is used to fix the relative positions of the sleeve 108 and the ring 111, and the ring 111 moves with the sleeve 108; after the stirring rod is inserted into the flask, the first movable ring 113 and the second movable ring 114 are relatively rotated, so that the first clamping rod 115 and the second clamping rod 116 are clamped on the first rod body 104, and then the blocking rod 125 is connected to the first clamping rod 115 and the second clamping rod 116, and the first rod body 104 is positioned by the clamping rod and the blocking rod 125, so as to reduce the shaking of the stirring rod when it rotates, avoid the collision of the stirring rod with the inner wall of the bottle mouth of the flask when it is working, and protect the flask.

[0063] As another aspect of the present application, a method for preparing glycerol acetone acetal using the glycerol acetone acetal preparation device as described above is also disclosed, comprising the following steps:

[0064] a. The reactor is loaded with acidic catalyst, the jacket heat transfer oil is set to a certain temperature and put into use;

[0065] b. Glycerol and acetone in a specific ratio are continuously fed into the tubular reactor via a metering pump, with the materials entering from the bottom and exiting from the top;

[0066] c. Process sampling and monitoring, the materials at the reactor outlet are collected into a collection bottle for standby use;

[0067] d. Collect a certain amount of the reaction solution and transfer it into a three-necked flask;

[0068] e. Control the top temperature to be greater than 100°C, and use the acetone glycerol preparation device to stir the solution in the three-necked flask to remove unreacted acetone, water and other impurities;

[0069] f. Collect the product and stop collecting when the kettle temperature is higher than 160℃.

[0070] The experimental results using this method are shown in the following table:

[0071]

[0072] The method adopts the method of continuous feeding of excess glycerol, thereby improving the conversion rate of the reaction and the production capacity of the device.

[0073] The fixed bed method is adopted, no water separation agent is required, the process is simple, the energy consumption is low, the subsequent separation trouble is reduced, and the equipment investment is reduced.

[0074] The above descriptions are only some preferred embodiments of the present disclosure and an explanation of the technical principles used. Those skilled in the art should understand that the scope of the invention involved in the embodiments of the present disclosure is not limited to the technical solutions formed by a specific combination of the above-mentioned technical features, but should also cover other technical solutions formed by any combination of the above-mentioned technical features or their equivalent features without departing from the above-mentioned inventive concept. For example, the above-mentioned features are replaced with the technical features with similar functions disclosed in the embodiments of the present disclosure (but not limited to) and the technical solutions formed.

Claims

1. A device for preparing glycerol acetone acetal, comprising: Base, placed on the table; A support rod, arranged on the base; A mounting block, disposed on the support rod; A motor, arranged on the mounting block; A stirring rod connected to the output shaft of the motor; Features: The stirring rod is provided with a receiving groove, and a movable rod is provided in the receiving groove. One end of the movable rod is rotatably connected to the receiving groove; the motor can drive the movable rod to flip out of the receiving groove or flip into the receiving groove.

2. The device for preparing glycerol acetone acetal according to claim 1, characterized in that: The stirring rod comprises a first rod body and a second rod body, the first rod body is provided with a first movable groove, one end of the second rod body is inserted into the first movable groove, and the accommodating groove is provided on the second push rod.

3. The device for preparing glycerol acetone acetal according to claim 2, characterized in that: The second rod body is provided with a first through cavity which is communicated with the accommodating groove, a rotating shaft is provided in the first through cavity, a first connecting rod is provided at the bottom of the rotating shaft, a baffle is provided at the bottom of the first connecting rod, a connecting rope is wound around the first connecting rod, one end of the connecting rope is fixedly connected to the movable rod; an arc-shaped spring sheet is provided on the inner wall of the accommodating groove.

4. The device for preparing glycerol acetone acetal according to claim 3, characterized in that: A second through cavity is provided on the top of the first movable groove, a transmission shaft is provided in the second through cavity, an movable cavity is provided on the side wall of the second through cavity, a limiting plate is provided on the transmission shaft, a first supporting spring is provided at the bottom of the movable cavity, a plurality of first ribs are provided on the top, and a first groove corresponding to the first rib is provided on the limiting plate.

5. The device for preparing glycerol acetone acetal according to claim 4, characterized in that: The mounting block is provided with a mounting cavity, a mounting tube is provided in the mounting cavity, the mounting tube passes through the mounting cavity, the first rod body is inserted in the mounting tube, a support plate is provided in the mounting tube, one end of the first rod body is against the support plate, a second movable groove is provided on the first rod body, a first fixed block is provided in the second movable groove, a connecting spring is provided on the first fixed block, and a fixing groove corresponding to the first fixed block is provided on the mounting tube.

6. The device for preparing glycerol acetone acetal according to claim 5, characterized in that: A first transmission wheel is provided on the mounting tube, a movable frame is provided in the mounting cavity, the movable frame is connected to the output shaft of the motor, and a second transmission wheel is provided on the movable frame for transmission cooperation with the first transmission wheel; a convex rod is also provided on the movable frame, and a transmission groove is provided on the convex rod for transmission cooperation with the transmission shaft.

7. The device for preparing glycerol acetone acetal according to claim 2, characterized in that: Also includes: A sleeve, sleeved on the support rod; A second connecting rod, disposed on the sleeve; A fixing plate, arranged in the sleeve; A third movable groove is arranged on the inner wall of the sleeve, and the fixing plate is located in the third movable groove; and rubber pads are respectively arranged on the top and bottom of the sleeve.

8. The device for preparing glycerol acetone acetal according to claim 7, characterized in that: Also includes: A collar, sleeved on the support rod; A first movable ring and a second movable ring are rotatably connected to the sleeve ring; A first clamping rod, disposed on the first movable ring; A second clamping rod, disposed on the second movable ring; The second movable ring is located below the first movable ring, and the first rod body is clamped between the first clamping rod and the second clamping rod.

9. The device for preparing glycerol acetone acetal according to claim 8, characterized in that: Also includes: A blocking rod, used to connect the first clamping rod and the second clamping rod; A first latch, used to connect the blocking rod and the first clamping rod; A second latch, used to connect the blocking rod and the second clamping rod; The first clamping rod is provided with a first connecting hole corresponding to the first latch pin, and the second clamping rod is provided with a second connecting hole corresponding to the second latch pin.

10. A method for preparing glycerol acetone acetal using the glycerol acetone acetal preparation device as claimed in any one of claims 1 to 9, characterized in that: The following steps are involved: a. The reactor is loaded with acidic catalyst, the jacket heat transfer oil is set to a certain temperature and put into use; b. Glycerol and acetone in a specific ratio are continuously fed into the tubular reactor via a metering pump, with the materials entering from the bottom and exiting from the top; c. Process sampling and monitoring, the materials at the reactor outlet are collected into a collection bottle for standby use; d. Collect a certain amount of the reaction solution and transfer it into a three-necked flask; e. Controlling the top temperature to be greater than 100° C., stirring the solution in the three-necked flask using the acetone glycerol preparation device to remove unreacted acetone, water and other impurities; f. Collect the product and stop collecting when the kettle temperature is higher than 160℃.

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