High-purity methylal synthesis test device

Abstract

The invention relates to the technical field of test teaching, and discloses a high-purity methylal synthesis test device, which comprises a tower kettle overflow tank, a tower kettle liquid condenser, a circulating water pump condenser, a raw material liquid tank, a tower kettle and a profile frame, and is characterized in that the tower kettle overflow tank is fixedly connected to the surface of the profile frame; the tower kettle liquid condenser is fixedly connected to a bracket on the profile frame; by means of the optimized tower body structure and filler, under specific experimental conditions, the concentration of methylal products at the top of the tower can reach 98% and is far higher than that of existing teaching devices in the market, the rectification purification teaching concept is effectively verified, continuous production is achieved, and the production efficiency is improved. The device can stably operate for a long time, provides sufficient experiment time and a stable experiment environment for teaching experiments, and is helpful for students to deeply understand and master methylal synthesis and rectification purification processes.

Description

Technical Field

[0001] The present invention relates to the technical field of experimental teaching, and specifically provides a high-purity dimethoxymethane synthesis experimental device. Background Art

[0002] Dimethoxymethane (DMM), also known as dimethoxymethane chemically, with the molecular formula C3H8O2, is a colorless, transparent, low-toxic, and volatile oxygen-containing organic compound. Its unique physical and chemical properties make it have important applications in multiple industrial fields:

[0003] 1. High-quality solvent: Dimethoxymethane has excellent solubility and low surface tension, and can replace traditional benzene solvents in the formulations of automotive paints and wood lacquers, reducing VOC emissions by more than 30%; it can also be used as an electronic component cleaner, quickly dissolving residues of soldering fluxes such as rosin; meanwhile, it is also used in the pharmaceutical industry for the crystallization and purification processes of antibiotics and vitamins.

[0004] 2. Clean fuel additive: Dimethoxymethane can be used as an oxygen-containing additive for diesel (the addition amount is 5% - 15%) to increase the cetane number, promote complete combustion, and reduce particulate matter emissions by more than 50%; in addition, it can be blended with biodiesel to improve low-temperature fluidity and alleviate the problem of engine carbon deposition.

[0005] An efficient synthesis process is the key to realizing its large-scale production. Currently, the common dimethoxymethane synthesis processes still use traditional liquid acid catalysts such as sulfuric acid, hydrochloric acid, or phosphoric acid.

[0006] For undergraduate teaching, it is necessary for students to be familiar with the production processes of common chemicals. Reactive distillation for synthesizing dimethoxymethane is often used in special distillation teaching. However, the product concentrations of the current teaching devices on the market are all lower than 95% of industrial production, and the operation concept of rectification and purification cannot be realized. Therefore, a high-purity dimethoxymethane synthesis experimental device is designed. Summary of the Invention

[0007] (1) Technical Problems to be Solved

[0008] Aiming at the deficiencies of the prior art, the present invention provides a high-purity dimethoxymethane synthesis experimental device, which solves the problems of weak rectification and purification teaching concepts and poor experimental effects of existing teaching devices.

[0009] (2) Technical Solutions

[0010] To achieve the above object, the present invention provides the following technical solution: A high-purity dimethoxymethane synthesis experimental device includes a column still overflow tank, a column still liquid condenser, a circulating water pump condenser, a raw material liquid tank, a column still, and a profile frame. The column still overflow tank is fixedly connected to the surface of the profile frame, and the column still liquid condenser is fixedly connected to the bracket on the profile frame;

[0011] The circulating water pump condenser is fixedly connected to the outer surface of the profile frame, the raw material liquid tank is fixedly connected to the bracket of the profile frame, the tower kettle is fixedly connected to the surface of the profile frame, and the tower kettle is fixedly connected to the tower kettle liquid condenser through a pipeline.

[0012] Preferably, it further includes an electric control box, a tower body, a feed pump, a controller display terminal, a product tank, a raw material tank, a tower head and a reflux ratio controller. The electric control box is fixedly connected to the outer surface of the profile frame, and the tower body is fixedly connected to the outer surface of the profile frame.

[0013] Preferably, the tower body is fixedly connected to the tower kettle, both feed pumps are fixedly connected to the surface of the profile frame, the controller display terminal is fixedly connected to the outer surface of the profile frame, and the controller display terminal is electrically connected to the electric control box;

[0014] Among them, the product tank is fixedly connected to the outer surface of the profile frame, and the raw material tank is fixedly connected to the outer surface of the profile frame.

[0015] Preferably, the tower head is fixedly connected to the outer surface of the profile frame, the reflux ratio controller is fixedly connected to the outer surface of the profile frame, the tower head is fixedly connected to the tower body, the reflux ratio controller is fixedly connected to the tower head and the tower body, and the tower body of the distillation column has 8 measuring ports for temperature measurement or adjusting the feed position. The measuring port numbers are sequentially 1 - 8 from top to bottom of the distillation column;

[0016] Among them, the input end of one feed pump is fixedly communicated with the raw material liquid tank, and the output end of one feed pump is fixedly communicated with the tower body.

[0017] Preferably, the input end of the other feed pump is fixedly communicated with the raw material tank, and the output end of the other feed pump is fixedly communicated with the tower body. One feed pump can pump the raw material in the raw material liquid tank into the tower body, and the other feed pump can pump the raw material in the raw material tank into the tower body.

[0018] Preferably, the electric control box is electrically connected to the two feed pumps, the product tank is connected to the tower head through a hose, and the reflux ratio controller is connected to the tower head.

[0019] A high - purity methylal synthesis test device, characterized in that:

[0020] First, meet the following conditions:

[0021] Tower kettle liquid preparation: Prepare 300 ml of 16.67% methanol solution (including 250 ml of water and 50 ml of methanol);

[0022] Continuous feeding: The raw material liquid tank contains a mixture of 19% formaldehyde solution and 2% concentrated sulfuric acid catalyst, and the raw material tank contains 99.5% methanol. The feeding flow rates are controlled at 3.2 ml / min for formaldehyde and 2.2 ml / min for methanol. The feeding positions are such that the formaldehyde solution enters the tower body at position 4, and the methanol solution enters the tower body at position 7.

[0023] (III) Beneficial effects

[0024] Compared with the prior art, the present invention provides a high-purity methylal synthesis test device, which has the following beneficial effects:

[0025] 1. For this high-purity methylal synthesis test device, through the optimized tower body structure and packing, under specific experimental conditions, the concentration of methylal product at the top of the tower can reach 98%, far exceeding the existing teaching devices in the market, effectively verifying the teaching concept of rectification and purification. For continuous production, it can operate stably for a long time, providing sufficient experimental time and a stable experimental environment for teaching experiments, and helping students to deeply understand and master the methylal synthesis and rectification and purification processes.

[0026] 2. For this high-purity methylal synthesis test device, the materials selected for each component are appropriate. For example, the high-temperature resistant borosilicate glass tower body is convenient for students to observe the experimental process; the profile frame is equipped with universal wheels, facilitating the movement of the device; the electric control box integrates the electric control device, and the control and display terminals are convenient to operate, improving the convenience and controllability of the experimental operation. Description of the drawings

[0027] Figure 1 It is a schematic structural diagram of the high-purity methylal synthesis test device of the present invention;

[0028] Figure 2 It is a schematic structural diagram of the tower body of the high-purity methylal synthesis test device of the present invention;

[0029] Figure 3 It is a schematic structural diagram of the tower kettle of the high-purity methylal synthesis test device of the present invention;

[0030] Figure 4 It is a schematic structural diagram of the raw material tank of the high-purity methylal synthesis test device of the present invention;

[0031] Figure 5 It is a schematic diagram of the results of Example 1 of the high-purity methylal synthesis test device of the present invention;

[0032] Figure 6 It is a schematic diagram of the results of Example 2 of the high-purity methylal synthesis test device of the present invention;

[0033] Figure 7 It is a schematic diagram of the results of Example 3 of the high-purity methylal synthesis test device of the present invention.

[0034] In the figure: 1. Bottom kettle overflow tank; 2. Bottom kettle liquid condenser; 3. Circulating water pump condenser; 4. Raw material liquid tank; 5. Bottom kettle; 6. Profile frame; 7. Electric control box; 8. Tower body; 9. Feed pump; 10. Controller display terminal; 11. Product tank; 12. Raw material tank; 13. Tower head; 14. Reflux ratio controller. Detailed implementation manners

[0035] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0036] Please refer to Figure 1-7 , the present invention provides a new technical solution: a high-purity methylal synthesis test device, including a bottom kettle overflow tank 1, a bottom kettle liquid condenser 2, a circulating water pump condenser 3, a raw material liquid tank 4, a bottom kettle 5 and a profile frame 6. The bottom kettle overflow tank 1 is fixedly connected to the surface of the profile frame 6. The bottom kettle liquid condenser 2 is fixedly connected to the bracket on the profile frame 6. The circulating water pump condenser 3 is fixedly connected to the outer surface of the profile frame 6. The raw material liquid tank 4 is fixedly connected to the bracket on the profile frame 6. The bottom kettle 5 is fixedly connected to the surface of the profile frame 6. The bottom kettle 5 is fixedly connected to the bottom kettle liquid condenser 2 through a pipeline.

[0037] Furthermore, it further includes an electric control box 7, a tower body 8, a feed pump 9, a controller display terminal 10, a product tank 11, a raw material tank 12, a tower head 13 and a reflux ratio controller 14. The electric control box 7 is fixedly connected to the outer surface of the profile frame 6. The tower body 8 is fixedly connected to the outer surface of the profile frame 6. The tower body 8 is fixedly connected to the bottom kettle 5. Both feed pumps 9 are fixedly connected to the surface of the profile frame 6. The controller display terminal 10 is fixedly connected to the outer surface of the profile frame 6. The controller display terminal 10 is electrically connected to the electric control box;

[0038] Among them, the product tank 11 is fixedly connected to the outer surface of the profile frame 6. The raw material tank 12 is fixedly connected to the outer surface of the profile frame 6. The tower head 13 is fixedly connected to the outer surface of the profile frame 6. The reflux ratio controller 14 is fixedly connected to the outer surface of the profile frame 6. The tower head 13 is fixedly connected to the tower body 8. The reflux ratio controller is fixedly connected to the tower head 13 and the tower body 8;

[0039] Among them, the input end of one feed pump 9 is fixedly connected to the raw material liquid tank 4, the output end of one feed pump 9 is fixedly connected to the tower body 8, the input end of another feed pump 9 is fixedly connected to the raw material tank 12, and the output end of another feed pump 9 is fixedly connected to the tower body 8. One feed pump 9 can pump the raw material in the raw material liquid tank 4 into the tower body 8, and the other feed pump 9 can pump the raw material in the raw material tank 12 into the tower body 8. The electrical control box 7 is electrically connected to the two feed pumps 9, the product tank 11 is connected to the tower head 13 through a hose, and the reflux ratio controller 14 is connected to the tower head 13.

[0040] Furthermore, the various components of the device are made of suitable materials. For example, the high-temperature resistant high-borosilicate glass tower body 8 is convenient for students to observe the experimental process; the profile frame 6 has universal wheels to facilitate the movement of the device; the electric control box integrates the electric control device, and the control and display terminals are easy to operate, thereby improving the convenience and controllability of the experimental operation.

[0041] Furthermore, when using the device, the following conditions are first met:

[0042] Bottom liquid ingredients: prepare 300 ml of 16.67% methanol solution (including 250 ml of water and 50 ml of methanol);

[0043] Continuous feeding: raw material liquid tank 4 is a mixture of 19% formaldehyde solution and 2% concentrated sulfuric acid catalyst, raw material tank 12 is 99.5% methanol, feed flow rate is controlled to formaldehyde 3.2ml / min, methanol 2.2ml / min; the feeding position is formaldehyde solution entering tower body 8 from position 4, methanol solution entering tower body 8 from position 7.

[0044] Embodiment 1:

[0045] Step 1: Injection: At 2024-09-28 12:09:01, the sample was injected into the detection instrument; the 19% formaldehyde solution in the raw material tank 4 was mixed with the 2% concentrated sulfuric acid catalyst and the 99.5% methanol in the raw material tank 12, and entered the reaction distillation tower from position 4 (formaldehyde solution) and position 7 (methanol solution) at flow rates of 3.2 ml / min (formaldehyde solution) and 2.2 ml / min (methanol solution), respectively;

[0046] Step 2: Acquisition, with a slope / peak width of 1000.0 / 1.0, and an acquisition time of 15.82 min;

[0047] The temperature sensor, pressure sensor and flow sensor provided by the device were used to collect the temperature, pressure, flow and other parameters of the tower top and tower bottom. The collection time was 15.82 minutes, starting from the injection time 2024-09-28 12:09:01, and the slope / peak width was set to 1000.0 / 1.0;

[0048] Step 3: Results. After analysis, methanol and formaldehyde react to form methylal under the action of a catalyst. After detection, the peak area content of methylal is 98.2489%. The peak area contents of other components are as follows: the component with a retention time of 2.233 min accounts for 1.5402%, the component with a retention time of 3.035 min accounts for 0.0232%, the component with a retention time of 4.581 min accounts for 0.1875%, and the component with a retention time of 12.231 min accounts for 0.0002%.

[0049] Example 2:

[0050] Step 1: Sampling. The sample was injected at 13:42:40 on September 28, 2024;

[0051] Similarly, according to the feeding requirements of the raw material liquid tank 4 and the raw material tank 12, that is, a 19% formaldehyde solution is mixed with a catalyst and 99.5% methanol, and the formaldehyde solution is fed at a flow rate of 3.2 ml / min and the methanol solution is fed at a flow rate of 2.2 ml / min. The formaldehyde solution is fed from the 4th position and the methanol solution is fed from the 7th position into the reactive distillation column;

[0052] Step 2: Collection. The collection was carried out at a slope / peak width of 1000.0 / 1.0 for a collection duration of 20.32 min;

[0053] Starting from the injection at 13:42:40 on September 28, 2024, the collection was carried out at a slope / peak width of 1000.0 / 1.0 for a collection duration of 20.32 min, and the temperature, pressure, flow rate and other parameters of the top and bottom of the column were collected;

[0054] Step 3: Results. Methylal was formed by reaction. The peak area content of methylal is 98.0928%. In addition, the peak area content of formaldehyde with a retention time of 2.686 min is 1.6953%, the peak area content of the component with a retention time of 5.002 min is 0.2118%, and the peak area content of the component with a retention time of 12.190 min is 0.0001%.

[0055] Example 3:

[0056] Step 1: Sampling. The sample was injected at 13:54:42 on September 29, 2024;

[0057] Keep the feeding composition, flow rate and feeding position of the raw material liquid tank 4 and the raw material tank 12 unchanged, and let the raw materials enter the reactive distillation column;

[0058] Step 2: Collection. The collection was carried out at a slope / peak width of 1000.0 / 1.0 for a collection duration of 16.90 min;

[0059] After injecting the sample at 13:54:42 on September 29, 2024, data such as the temperature, pressure, and flow rate at the top and bottom of the tower were collected with a slope / peak width of 1000.0 / 1.0 and a collection duration of 16.90 min.

[0060] Step 3: Results. Methylal was generated. The peak area content of methylal was 98.1093%, the peak area content of the component with a retention time of 2.387 min was 1.6875%, the peak area content of the component with a retention time of 4.735 min was 0.1897%, the peak area content of the component with a retention time of 7.106 min was 0.0136%, and the peak area content of the component with a retention time of 12.188 min was 0.0000%.

[0061] Furthermore, through the optimized tower body structure and packing, under specific experimental conditions, the concentration of methylal product at the top of the tower can reach 98%, far exceeding the existing teaching devices in the market, effectively verifying the teaching concept of rectification and purification. Now, continuous production can be carried out, and it can operate stably for a long time, providing sufficient experimental time and a stable experimental environment for teaching experiments, which helps students deeply understand and master the synthesis and rectification and purification process of methylal.

[0062] Structural description:

[0063] Bottom overflow tank 1: Made of glass, connected to the bottom of the tower 5 by a hose, used to receive the overflow product from the bottom of the tower 5.

[0064] Bottom liquid condenser 2: Made of glass, connected to the vent of the bottom of the tower 5 by a hose, used to condense the residual liquid at the bottom of the tower, or to condense the sampled product during sample collection.

[0065] Circulating water pump condenser 3: Connected to the top condenser and the bottom liquid condenser 2 by hoses.

[0066] Raw material liquid tank 4: Connected to the feed pump 9 by a hose, and the raw material liquid is pumped into the tower body 8 through a peristaltic pump.

[0067] Bottom of the tower 5: Made of glass, used to hold the material that enters the bottom of the tower 5 after the reaction. The bottom of the tower 5 is equipped with a heating component, which is an existing device and is used for reboiling the bottom liquid. The bottom of the tower 5 is equipped with a drain port for draining the bottom liquid. The top of the bottom of the tower 5 is equipped with a chuck interface and is connected to the tower body 8 through a detachable connector.

[0068] Profile frame 6: Made of high-quality European standard aluminum profile frame, with universal wheels on the frame, which is convenient to move.

[0069] Electric control box 7: Used to install electronic control devices such as boards, signal receivers, electric heating controllers, and processors required for the device.

[0070] Tower body 8: The tower body 8 is made of high-temperature resistant borosilicate glass, with a diameter of 25 mm and a tower height of 2050 mm. The tower body of the tower body 8 has 8 measuring ports for temperature measurement or adjusting the feeding position (the measuring port numbers are sequentially 1-8 from top to bottom of the rectifying tower). Both the upper and lower parts of the tower body are equipped with chuck interfaces and are connected to the tower head 13 and the tower kettle 5 through detachable connectors.

[0071] Feed pump 9: The feed pump 9 is a peristaltic pump. The feed pump 9 uses a peristaltic pump or other transfer pumps to transport the raw materials in the raw material tank 12 into the tower body 8.

[0072] Controller display terminal 10: The controller display terminal 10 uses an industrial all-in-one computer and is fixed with a height-adjustable integrated bracket.

[0073] Product tank 11: Made of glass, the top product tank 11 is connected to the top drain port of the tower through a hose, and the bottom of the product tank 11 is provided with a drain port.

[0074] Raw material tank 12: It is connected to the feed pump 9 through a hose, and the raw material liquid is pumped into the tower body 8 through the feed pump 9.

[0075] Tower head 13: Made of glass, the tower head is equipped with a condenser for condensing the purified product flowing out. The bottom of the tower head is provided with a chuck interface and is connected to the tower body through a detachable connector.

[0076] Reflux ratio controller 14: Used to control the reflux ratio of the top reflux liquid.

[0077] Although the embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. An experimental device for synthesizing high-purity methylal, comprising a bottom kettle overflow tank (1), a bottom kettle liquid condenser (2), a circulating water pump condenser (3), a raw material liquid tank (4), a bottom kettle (5) and a profile frame (6), characterized in that: The bottom kettle overflow tank (1) is fixedly connected to the surface of the profile frame (6), and the bottom kettle liquid condenser (2) is fixedly connected to the bracket on the profile frame (6); The circulating water pump condenser (3) is fixedly connected to the outer surface of the profile frame (6), the raw material liquid tank (4) is fixedly connected to the bracket of the profile frame (6), the bottom kettle (5) is fixedly connected to the surface of the profile frame (6), and the bottom kettle (5) is fixedly connected to the bottom kettle liquid condenser (2) through a pipeline.

2. The high-purity methylal synthesis test device according to claim 1, wherein: It further includes an electric control box (7), a tower body (8), a feed pump (9), a controller display terminal (10), a product tank (11), a raw material tank (12), a tower head (13) and a reflux ratio controller (14). The electric control box (7) is fixedly connected to the outer surface of the profile frame (6), and the tower body (8) is fixedly connected to the outer surface of the profile frame (6).

3. The high-purity methylal synthesis test device according to claim 2, characterized in that: The tower body (8) is fixedly connected to the bottom kettle (5). Both feed pumps (9) are fixedly connected to the surface of the profile frame (6). The controller display terminal (10) is fixedly connected to the outer surface of the profile frame (6), and the controller display terminal (10) is electrically connected to the electric control box; Among them, the product tank (11) is fixedly connected to the outer surface of the profile frame (6), and the raw material tank (12) is fixedly connected to the outer surface of the profile frame (6).

4. A high-purity methylal synthesis test device according to claim 3, characterized in that: The tower head (13) is fixedly connected to the outer surface of the profile frame (6), the reflux ratio controller (14) is fixedly connected to the outer surface of the profile frame (6). The tower head (13) is fixedly connected to the tower body (8), the reflux ratio controller is fixedly connected to the tower head (13) and the tower body (8). The tower body (8) has 8 measuring ports on its tower body for temperature measurement or adjusting the feed position. The measuring port numbers of the distillation column from top to bottom are No. 1 - No. 8 in sequence; Among them, the input end of one feed pump (9) is fixedly communicated with the raw material liquid tank (4), and the output end of one feed pump (9) is fixedly communicated with the tower body (8).

5. The high-purity methylal synthesis test device according to claim 4, characterized in that: The input end of the other feed pump (9) is fixedly communicated with the raw material tank (12), and the output end of the other feed pump (9) is fixedly communicated with the tower body (8). One feed pump (9) can pump the raw material in the raw material liquid tank (4) into the tower body (8), and the other feed pump (9) can pump the raw material in the raw material tank (12) into the tower body (8).

6. The high-purity methylal synthesis test device according to claim 5, characterized in that: The electric control box (7) is electrically connected to the two feed pumps (9). The product tank (11) is connected to the tower head (13) through a hose, and the reflux ratio controller (14) is connected to the tower head (13).

7. A high-purity methylal synthesis test device, characterized in that: First, the following conditions are met: Bottom kettle liquid preparation: Prepare 300 ml of 16.67% methanol solution (including 250 ml of water and 50 ml of methanol); Continuous feeding: The raw material liquid tank (4) is a mixed liquid of 19% formaldehyde solution and 2% concentrated sulfuric acid catalyst, and the raw material tank (12) is 99.5% methanol. The feeding flow rate is controlled at 3.2 ml / min for formaldehyde and 2.2 ml / min for methanol; the feeding position is that the formaldehyde solution enters the tower body (8) from the 4th position, and the methanol solution enters the tower body (8) from the 7th position.

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