A reaction device for preparing rosin-based Gemini surfactant

Abstract

The invention discloses a reaction device for preparing a rosin-based Gemini surfactant. The process comprises the following steps: S1: under stirring, 50-75 parts by weight of fumaric acid rosin, 20-40 parts by weight of polyethylene glycol, 10-15 parts by weight of pentaerythritol and a catalyst are put into a reactor, first mixed evenly at 150-155° C., then heated to 180-200° C., and reacted for 0.5-1 hour; in the process for preparing the rosin-based Gemini surfactant, through a gradual heating process, a cooling process and matching corresponding raw material components, the generation of by-products such as low-boiling substances is reduced as much as possible and the purity of the final product rosin-based surfactant is improved, thereby effectively improving the comprehensive performance; in the reaction device of the invention, a stirring mechanism and a reflux mechanism that are convenient for temperature control are provided, so that the upper and lower circulations of materials can be realized, the mixing effect is greatly improved, the temperature control rate is improved, and thus the reaction rate and production efficiency are improved.

Description

Technical Field

[0001] The invention relates to the technical field of surfactant preparation, in particular to a reaction device for preparing rosin-based Gemini surfactant. Background Art

[0002] Gemini surfactants with high surface activity have been a research hotspot in the field of surfactants in recent years. The commonly studied Gemini surfactants are composed of two identical surfactant molecules connected together by a linker at or near the hydrophilic base to form a symmetrical structure, that is, Gemini surfactants with symmetrical molecular structure. Hetero-gemini surfactants with asymmetrical molecular structure have become a new type of surfactant with superior performance because they contain head groups with different chemical structures, alkane main chains of different lengths and various linker chains, and play an important role in understanding the mechanism of molecular self-organization and constructing molecular ordered aggregates with novel structures. Rosin is an abundant natural renewable resource. Its main component is resin acid, which is a monocarboxylic acid with two double bonds in a tricyclic phenanthrene skeleton. The tricyclic phenanthrene skeleton has strong hydrophobicity, and hydrophilic groups can be introduced with double bonds and carboxylic acids as reaction centers. At present, there are also reports on symmetrical rosin-based Gemini surfactants, but research on rosin-based hetero-gemini surfactants is relatively rare. Therefore, it is very necessary to develop a rosin-based Gemini surfactant that is efficient, environmentally friendly and easy to prepare. Summary of the invention

[0003] The object of the present invention is to provide a reaction device for preparing rosin-based Gemini surfactants to solve the problems raised in the above background technology.

[0004] To achieve the above object, the present invention provides the following technical scheme: A process for preparing a rosin-based Gemini surfactant, comprising the following steps: S1: Under stirring, 50-75 parts by weight of fumaric acid rosin, 20-40 parts by weight of polyethylene glycol, 10-15 parts by weight of pentaerythritol and a catalyst are placed in a reaction kettle, first mixed uniformly at 150° C.-155° C., then heated to 180° C.-200° C., reacted for 0.5 hour-1 hour, then heated to 230° C.-280° C., reacted for 2 hours-3 hours;

[0005] S2: After the previous step, 0.05-0.1 parts by weight of hydroquinone and 0.3-0.5 parts by weight of phosphorus pentoxide are added to the reaction kettle, and then the temperature is reduced to 90° C.-105° C. and the reaction is kept at this temperature for 0.2 hour-0.5 hour;

[0006] S3: After the previous step, sodium hydroxide is added to the reactor under stirring to make the pH value of the reaction material within the range of 7-8, and then the temperature is lowered to 20°C-40°C, and the reaction is kept warm for 0.5-1 hour, and the product is obtained by discharging the material.

[0007] Preferably, the catalyst is a double metal cyanide complex or 4-dimethylaminopyridine.

[0008] A reaction device for preparing rosin-based Gemini surfactants comprises a reactor body 1, wherein a plurality of electric heating tubes 22 are arranged in the reactor body 1, a feeding port 2 is arranged at the top of the reactor body 1, a driving motor 3 is installed at the center of the top surface of the reactor body 1, an output end of the driving motor 3 is connected to a central shaft 4, a stirring mechanism for facilitating temperature control is arranged on the central shaft 4, and a reflux mechanism is arranged at the bottom of the reactor body 1.

[0009] Preferably, a plurality of supporting legs are arranged on the bottom surface of the reactor body 1, and fixing holes are provided on the supporting legs.

[0010] Preferably, the stirring mechanism includes an array of stirring rods 5 installed on the central axis 4, a sleeve ring fixed on the central axis 4 is provided in the middle of the stirring rod 5, a plurality of side blades 6 are provided on the stirring rod 5, an internal flow channel 7 is provided inside the side blades 6, a channel connected to the internal flow channel 7 is provided inside the stirring rod 5, an outer ring 8 is connected to the end of the stirring rod 5, a flange 9 is provided on the side wall of the outer ring 8, and a liquid inlet hole 10 and a liquid outlet hole 11 are opened above and below the flange 9.

[0011] Preferably, an annular groove 12 is provided on the side wall of the reactor body 1, the outer ring 8 is slidably embedded in the annular groove 12, the convex edge 9 divides the annular groove 12 into an upper chamber 13 and a lower chamber 14, and an injection port 15 and a discharge port 16 are provided on the outer wall of the annular groove 12, the injection port 15 is connected to the upper chamber 13, and the discharge port 16 is connected to the lower chamber 14.

[0012] Preferably, the side leaves 6 are symmetrically distributed vertically.

[0013] Preferably, a dynamic sealing structure is provided at the connection between the annular groove 12 and the outer ring 8.

[0014] Preferably, the reflux mechanism includes several reflux pipes 17, one end of the reflux pipe 17 is connected to the bottom surface of the reactor body 1 and a first solenoid valve 18 is provided at this end, the other end of the reflux pipe 17 is connected to the upper side wall of the reactor body 1, and a reflux pump 19 is provided on the reflux pipe 17.

[0015] Preferably, a discharge pipe 20 is provided on one of the return pipes 17 , and a second solenoid valve 21 is provided at the connection between the return pipe 17 and the discharge pipe 20 .

[0016] Compared with the prior art, the present invention has the following beneficial effects:

[0017] 1. The present invention provides a reaction device for preparing a rosin-based Gemini surfactant. In the process of preparing a rosin-based Gemini surfactant, the generation of by-products such as low-boiling substances is reduced as much as possible, and the purity of the final product rosin-based surfactant is improved through a gradual heating process, a cooling process and matching corresponding raw material components, thereby effectively improving its comprehensive performance;

[0018] 2. The reaction device of the present invention is provided with a stirring mechanism and a reflux mechanism for convenient temperature control. When the material is in the reactor body 1, the driving motor 3 is started to drive the central shaft 4 to rotate, so that the stirring rod 5 stirs and mixes the material. At the same time, the multiple sets of side blades 6 can also stir the material to improve the stirring effect. At the same time, the reflux pump 19 is started to transport the material at the bottom to the top of the reactor body 1 through the reflux pipe 17, so that the upper and lower circulation of the material can be realized, which greatly improves the mixing effect, thereby improving the reaction rate and production efficiency. During the process, the reaction temperature needs to be increased and decreased many times. Multiple electric heating tubes 22 can greatly improve the heating effect. When cooling, coolant is injected into the interior through the injection port 15, and then the coolant enters the upper chamber 13 and enters the inner flow channel 7 of the upper side leaf 6 through the liquid inlet hole 10, and then enters the inner flow channel 7 of the lower side leaf 6 through the other end and returns to the lower chamber 14 through the liquid outlet 11, and then is discharged through the drain port 16. The side leaf 6 can achieve cooling from various positions inside the material when stirring the material, thereby improving the temperature control rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a schematic diagram of the structure of the device of the present invention.

[0020] Figure 2 for Figure 1 Enlarged view of point A in the middle.

[0021] Figure 3 It is a structural diagram of the stirring mechanism of the present invention.

[0022] In the figure: reactor body 1, feeding port 2, driving motor 3, central axis 4, stirring rod 5, side blades 6, inner flow channel 7, outer ring 8, flange 9, liquid inlet 10, liquid outlet 11, annular groove 12, upper chamber 13, lower chamber 14, liquid injection port 15, liquid discharge port 16, reflux pipe 17, first solenoid valve 18, reflux pump 19, discharge pipe 20, second solenoid valve 21, electric heating pipe 22. DETAILED DESCRIPTION

[0023] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] See also Figures 1 to 3 The present invention provides a technical solution: a rosin-based Gemini surfactant preparation process, comprising the following steps: S1: under stirring, 50-75 parts by weight of fumaric acid rosin, 20-40 parts by weight of polyethylene glycol, 10-15 parts by weight of pentaerythritol and a catalyst are placed in a reaction kettle, first mixed uniformly at 150°C-155°C, then heated to 180°C-200°C, reacted for 0.5 hour-1 hour, then heated to 230°C-280°C, reacted for 2 hours-3 hours;

[0025] S2: After the previous step, 0.05-0.1 parts by weight of hydroquinone and 0.3-0.5 parts by weight of phosphorus pentoxide are added to the reaction kettle, and then the temperature is reduced to 90° C.-105° C. and the reaction is kept at this temperature for 0.2 hour-0.5 hour;

[0026] S3: After the previous step, sodium hydroxide is added to the reactor under stirring to make the pH value of the reaction material within the range of 7-8, and then the temperature is lowered to 20°C-40°C, and the reaction is kept warm for 0.5-1 hour, and the product is obtained by discharging the material.

[0027] The catalyst is a double metal cyanide complex or 4-dimethylaminopyridine.

[0028] Embodiment 1:

[0029] S1: Under stirring, 50 kg of fumaric acid rosin, 20 kg of polyethylene glycol, 10 kg of pentaerythritol and a catalyst were placed in a reactor, first mixed evenly at 150°C, then heated to 180°C, reacted for 0.5 hours, and then heated to 230°C, reacted for 2 hours;

[0030] S2: After the previous step, 0.05 kg of hydroquinone and 0.3 kg of phosphorus pentoxide are added to the reactor, and then the temperature is lowered to 90° C. and kept at this temperature for 0.2 hours;

[0031] S3: After the previous step, sodium hydroxide is added to the reactor under stirring to make the pH value of the reaction material 7, and then the temperature is lowered to 20° C. and the reaction is kept at this temperature for 0.5 hours. The product is obtained by discharging the material.

[0032] Embodiment 2:

[0033] S1: Under stirring, 65 kg of fumaric acid rosin, 30 kg of polyethylene glycol, 12 kg of pentaerythritol and a catalyst were placed in a reactor, first mixed evenly at 150°C, then heated to 190°C, reacted for 1 hour, and then heated to 250°C, reacted for 2.5 hours;

[0034] S2: After the previous step, 0.75 kg of hydroquinone and 0.4 kg of phosphorus pentoxide are added to the reactor, and then the temperature is lowered to 100° C. and the reaction is kept at this temperature for 0.5 hours;

[0035] S3: After the previous step, sodium hydroxide is added to the reactor under stirring to make the pH value of the reaction material 7, and then the temperature is lowered to 30° C., and the reaction is kept at this temperature for 1 hour, and the product is obtained by discharging the material.

[0036] Embodiment 3:

[0037] S1: Under stirring, 75 kg of fumaric acid rosin, 40 kg of polyethylene glycol, 15 kg of pentaerythritol and a catalyst were placed in a reactor, first mixed evenly at 155°C, then heated to 200°C, reacted for 1 hour, and then heated to 280°C, reacted for 3 hours;

[0038] S2: After the previous step, 0.1 kg of hydroquinone and 0.5 kg of phosphorus pentoxide are added to the reactor, and then the temperature is lowered to 105° C. and kept at this temperature for 0.5 hours;

[0039] S3: After the previous step, sodium hydroxide is added to the reactor under stirring to make the pH value of the reaction material 8, and then the temperature is lowered to 40° C., and the reaction is kept at this temperature for 1 hour, and the material is discharged to obtain the product.

[0040] A reaction device for preparing rosin-based Gemini surfactants, comprising a reactor body 1, a plurality of support legs are arranged on the bottom surface of the reactor body 1, and fixing holes are provided on the support legs, and the device can be fixed to the ground by bolts, a plurality of electric heating tubes 22 are arranged in the reactor body 1, and the electric heating tubes 22 are divided into multiple layers, and a plurality of tubes in each layer are evenly distributed in the inner wall of the reactor body 1, so as to effectively improve the heating efficiency, a feeding port 2 is arranged on the top of the reactor body 1, a driving motor 3 is installed at the center of the top surface of the reactor body 1, and a central shaft 4 is connected to the output end of the driving motor 3, and a stirring mechanism for facilitating temperature control is arranged on the central shaft 4, and the stirring mechanism comprises an array of stirring rods 5 installed on the central shaft 4, a sleeve ring fixed on the central shaft 4 is arranged in the middle of the stirring rod 5, a plurality of side blades 6 are arranged on the stirring rod 5, and the side blades 6 are symmetrically distributed up and down, and an inner flow channel 7 is arranged inside the side blades 6, and the inner part of the stirring rod 5 A channel connected to the inner flow channel 7 is provided, and a channel is also provided in the sleeve ring to connect the inner flow channels 7 on both sides. At the rightmost end of the stirring rod 5, the upper and lower channels are connected, so that the upper and lower inner flow channels 7 are connected. The end of the stirring rod 5 is connected to an outer ring 8, and a convex edge 9 is provided on the side wall of the outer ring 8. A liquid inlet hole 10 and a liquid outlet hole 11 are opened above and below the convex edge 9; an annular groove 12 is provided on the side wall of the reactor body 1, and the outer ring 8 is slidably embedded in the annular groove 12 In the figure, a dynamic sealing structure is arranged at the connection between the annular groove 12 and the outer ring 8, so that no material can enter the annular groove 12, and the convex edge 9 divides the annular groove 12 into an upper chamber 13 and a lower chamber 14. An injection port 15 and a discharge port 16 are arranged on the outer wall of the annular groove 12. The injection port 15 is connected to the upper chamber 13, and the discharge port 16 is connected to the lower chamber 14. The injection port 15 and the discharge port 16 need to be connected to external pipes respectively, which are used to inject coolant and absorb coolant respectively.

[0041] A reflux mechanism is provided at the bottom of the reactor body 1, and the reflux mechanism includes several reflux pipes 17, one end of the reflux pipe 17 is connected to the bottom surface of the reactor body 1 and a first solenoid valve 18 is provided at this end, the other end of the reflux pipe 17 is connected to the upper end side wall of the reactor body 1, a reflux pump 19 is provided on the reflux pipe 17, one of the reflux pipes 17 is provided with a discharge pipe 20, and a third solenoid valve is provided on the reflux pipe 17, and a valve 19 is provided at the connection between the reflux pipe 17 and the discharge pipe 20. The second solenoid valve 21, when stirring, the first solenoid valve 18 is opened and the second solenoid valve 21 is closed, and the reflux pump 19 is started to transport the material at the bottom to the top of the reactor body 1 through the reflux pipe 17, so as to realize the upper and lower circulation of the material, which greatly improves the mixing effect. When discharging, it is only necessary to open the first solenoid valve 18 and the second solenoid valve 21 at the end of the reflux pipe 17 connected to the discharge pipe 20, close the third solenoid valve, and start the reflux pump 19 to discharge the material from the discharge pipe 20.

[0042] In actual use, the reaction device for preparing rosin-based Gemini surfactant proposed in the present invention reduces the generation of by-products such as low-boiling substances as much as possible and improves the purity of the final product rosin-based surfactant through a gradual heating process, a cooling process and matching corresponding raw material components in the process of preparing the rosin-based Gemini surfactant, thereby effectively improving its comprehensive performance.

[0043] The reaction device of the present invention is provided with a stirring mechanism and a reflux mechanism for convenient temperature control. When the material is in the reactor body 1, the driving motor 3 is started to drive the central shaft 4 to rotate, so that the stirring rod 5 stirs and mixes the material. At the same time, the multiple groups of side blades 6 can also stir the material to improve the stirring effect. At the same time, the reflux pump 19 is started to transport the material at the bottom to the top of the reactor body 1 through the reflux pipe 17, so as to realize the upper and lower circulation of the material, greatly improving the mixing effect, thereby improving the reaction rate and production efficiency. , the reaction temperature needs to be increased and decreased multiple times, and multiple electric heating tubes 22 can greatly improve the heating effect. When cooling, coolant is injected into the interior through the injection port 15, and then the coolant enters the upper chamber 13 and enters the inner flow channel 7 of the upper side leaf 6 through the liquid inlet hole 10, and then enters the inner flow channel 7 of the lower side leaf 6 through the other end and returns to the lower chamber 14 through the liquid outlet 11, and then is discharged through the drain port 16. When the side leaf 6 stirs the material, it can achieve cooling from various positions inside the material, which greatly improves the cooling rate.

[0044] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A reaction device for preparing rosin-based Gemini surfactant, characterized in that: The invention comprises a reactor body (1), wherein a plurality of electric heating tubes (22) are arranged in the reactor body (1), a feeding port (2) is arranged at the top of the reactor body (1), a driving motor (3) is installed at the center of the top surface of the reactor body (1), an output end of the driving motor (3) is connected to a central shaft (4), a stirring mechanism for facilitating temperature control is arranged on the central shaft (4), the stirring mechanism comprises an array of stirring rods (5) installed on the central shaft (4), a sleeve ring fixed on the central shaft (4) is arranged in the middle of the stirring rod (5), a plurality of side blades (6) are arranged on the stirring rod (5), an inner flow channel (7) is arranged inside the side blades (6), and the stirring mechanism A channel communicating with the inner flow channel (7) is provided inside the rod (5); an outer ring (8) is connected to the end of the stirring rod (5); a convex edge (9) is provided on the side wall of the outer ring (8); a liquid inlet (10) and a liquid outlet (11) are provided above and below the convex edge (9); an annular groove (12) is provided on the side wall of the reactor body (1); the outer ring (8) is slidably embedded in the annular groove (12); the convex edge (9) divides the annular groove (12) into an upper chamber (13) and a lower chamber (14); an injection port (15) and a liquid discharge port (16) are provided on the outer wall of the annular groove (12); the injection port (15) is connected to the upper chamber (13); and the liquid discharge port (16) is connected to the lower chamber (14); A reflux mechanism is provided at the bottom of the reactor body (1), the reflux mechanism comprising a plurality of reflux pipes (17), one end of the reflux pipe (17) being connected to the bottom surface of the reactor body (1) and a first solenoid valve (18) being provided at this end, the other end of the reflux pipe (17) being connected to the upper side wall of the reactor body (1), and a reflux pump (19) being provided on the reflux pipe (17).

2. A reaction device for preparing rosin-based Gemini surfactant according to claim 1, characterized in that: A plurality of supporting legs are arranged on the bottom surface of the reactor body (1), and fixing holes are provided on the supporting legs.

3. A reaction device for preparing rosin-based Gemini surfactant according to claim 1, characterized in that: The side leaves (6) are symmetrically distributed up and down.

4. A reaction device for preparing rosin-based Gemini surfactant according to claim 1, characterized in that: A dynamic sealing structure is provided at the connection between the annular groove (12) and the outer ring (8).

5. A reaction device for preparing rosin-based Gemini surfactant according to claim 1, characterized in that: A discharge pipe (20) is provided on one of the return pipes (17), and a second solenoid valve (21) is provided at the connection between the return pipe (17) and the discharge pipe (20).

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