Synthesis device of 2-thiophenecarboxaldehyde

Abstract

The utility model discloses a 2-thiophenecarboxaldehyde synthesis device which comprises a reaction section device, a hydrolysis section device and a distillation section device, and the reaction section device comprises a first raw material tank and a reaction kettle; the hydrolysis section device comprises a second raw material tank, a hydrolysis kettle, a first receiving tank and a second receiving tank, the outlet end of the reaction kettle and the outlet end of the second raw material tank are connected with the inlet end of the hydrolysis kettle, and the outlet end of the hydrolysis kettle is connected with the inlet end of the first receiving tank and the material inlet and outlet end of the second receiving tank; the distillation section device comprises a normal-pressure distillation device and a reduced-pressure distillation device; the atmospheric distillation device comprises a first distillation kettle and a condenser; the reduced pressure distillation device comprises a second distillation kettle, a product receiving kettle and a vacuum pump, the outlet end of the condenser is connected with the inlet end of the second distillation kettle, and a valve is arranged between the outlet end of the condenser and the inlet end of the second distillation kettle. The process is advanced and reasonable, low in production cost, high in product purity and stable in quality, and continuous automatic production can be carried out.

Description

TECHNICAL FIELD

[0001] The utility model relates to synthetic device technical field, concretely relates to a 2 -thiophene formaldehyde's synthetic device. BACKGROUND

[0002] 2-thiophene formaldehyde is an important pharmaceutical intermediate, is used to introduce thiophene group in organic compound, for example, is used for synthesizing broad-spectrum anthelmintic drug thiabendazole and drug cephalosporin, clopidogrel, prasugrel etc.

[0003] For synthesis method, CN201610525015.9 provides a production process of thiophene formaldehyde, with thiophene, N, N-dimethylformamide (DMF) and phosgene as raw materials, but raw material phosgene has acute toxicity, so it is difficult to industrialize, if using triphosgene (solid phosgene) to replace traditional raw material phosgene, the toxicity is reduced, but in industrial scale, the safety is poor, and the subsequent purification is difficult, and the purity of final product is low.

[0004] For purification method, CN201810238496.4 provides a purification method of 2-thiophene formaldehyde crude product, water vapor is introduced into the reaction kettle, and 2-bromothiophene and water are evaporated together, the distillate is separated in the phase separator, the oil phase is collected, and 2-thiophene formaldehyde preliminary treatment product is obtained, and pure 2-thiophene formaldehyde is obtained by rectification. First, if 2-bromothiophene does not exist in the crude product, the purification method is not suitable, second, more heat is consumed for evaporation with water and rectification, and the cost is increased by designing or selecting a suitable rectification tower, finally, although rectification can obtain high purity in theory, the higher the purity, the lower the purification efficiency, and the lower the yield.

[0005] Therefore, for the industrial synthesis of 2-thiophene formaldehyde, it is urgent to improve the synthesis and purification method, and equip with a new and efficient synthesis device to improve the product purity and yield. UTILITY MODEL CONTENT

[0006] To solve the above problems, the utility model provides a 2-thiophene formaldehyde's synthetic device, including reaction section device, hydrolysis section device and distillation section device, the distillation section device includes atmospheric distillation device and vacuum distillation device, and the process is advanced and reasonable, the production cost is low, the product purity is high, the quality is stable, and continuous automatic production can be carried out.

[0007] On the one hand, the utility model provides a 2-thiophene formaldehyde's synthetic device, including reaction section device, hydrolysis section device and distillation section device;

[0008] The reaction section device includes a first raw material tank and a reaction kettle, and the outlet end of the first raw material tank is connected with the inlet end of the reaction kettle;

[0009] The hydrolysis section device comprises a second raw material tank, a hydrolysis kettle, a first receiving tank and a second receiving tank, the outlet end of the reaction kettle and the outlet end of the second raw material tank are connected with the inlet end of the hydrolysis kettle, and the outlet end of the hydrolysis kettle is connected with the inlet end of the first receiving tank and the material inlet and outlet end of the second receiving tank;

[0010] The distillation section device comprises an atmospheric distillation device and a vacuum distillation device.

[0011] The atmospheric distillation device comprises a first distillation kettle and a condenser, the material inlet and outlet end of the second receiving tank is connected with the inlet end of the first distillation kettle, and the outlet end of the first distillation kettle is connected with the inlet end of the condenser.

[0012] The vacuum distillation device comprises a second distillation kettle, a product receiving kettle and a vacuum pump, the outlet end of the condenser is connected with the inlet end of the second distillation kettle, a valve is arranged between the outlet end of the condenser and the inlet end of the second distillation kettle, the outlet end of the second distillation kettle is connected with the inlet end of the product receiving kettle, and the outlet end of the product receiving kettle is connected with the vacuum pump.

[0013] The synthetic device is divided into a reaction section device, a hydrolysis section device and a distillation section device according to production sections; under such a design, the whole process from raw materials to products can be realized without transferring materials, after the reaction of the previous batch of materials is completed and enters the hydrolysis section, a new batch of raw materials can be timely put in, continuous production is realized, automatic production can be realized by using a central control program, the production cycle is shortened, and the quality of products is more stable.

[0014] The functions of the hydrolysis section device include hydrolysis of intermediates and extraction of products into an organic phase, two-step operations are combined and carried out in the same kettle, land occupation is saved, equipment cost is reduced, and the water phase and the organic phase are respectively received by the first receiving tank and the second receiving tank, so that the operation is simple; the distillation section uses atmospheric distillation equipment and vacuum distillation equipment in sequence to purify, and different impurities are respectively removed; after the crude product is purified in the extraction, atmospheric distillation and vacuum distillation devices in sequence, high-quality products with a purity of > 99.3% can be obtained.

[0015] A valve is arranged between the atmospheric distillation equipment and the vacuum distillation equipment (between the outlet end of the condenser and the inlet end of the second distillation kettle), when the vacuum distillation is carried out, only the valve needs to be closed, the operation is more simple, and the loss of products can be reduced.

[0016] In some modes, the outlet end of the first raw material tank is located at the bottom of the first raw material tank, and the height of the outlet end of the first raw material tank is higher than that of the inlet end of the reaction kettle.

[0017] In some modes, the outlet end of the first raw material tank is provided with a flow control valve.

[0018] In some modes, the outlet end of the second raw material tank is located at the bottom of the second raw material tank, and the height of the outlet end of the second raw material tank is higher than that of the inlet end of the hydrolysis kettle.

[0019] In some modes, the second raw material tank outlet end is provided with a flow control valve.

[0020] In some modes, the inlet end of the first raw material tank and the inlet end of the second raw material tank are each provided with a plurality of valves.

[0021] In some modes, the hydrolysis kettle outlet end is located at the bottom of the hydrolysis kettle, and the hydrolysis kettle outlet end is provided with a valve.

[0022] In some modes, the first receiving tank inlet end is provided with a valve, and a valve is arranged between the hydrolysis kettle outlet end and the second receiving tank material inlet and outlet end.

[0023] In some modes, the reaction kettle, the hydrolysis kettle, the first distillation kettle, the second distillation kettle and the product receiving kettle are each provided with a temperature control set.

[0024] In some modes, the reaction kettle, the hydrolysis kettle, the first distillation kettle, the second distillation kettle and the product receiving kettle are each provided with a stirring paddle.

[0025] Preferably, the stirring paddle inside the product receiving kettle is a device specially designed for 2-thiophene formaldehyde synthesis and purification, and the structure is that the stirring paddle inside the product receiving kettle comprises a stirring paddle blade and a refrigeration jacket, the refrigeration jacket is wrapped on the surface of the stirring paddle blade, the refrigeration jacket is filled with refrigerant inside, and the inlet end and the outlet end of the refrigeration jacket are connected with an external circulating cold trap.

[0026] Further, the lowermost stirring blade of the stirring paddle inside the product receiving kettle is located at the bottom of the product receiving kettle, the uppermost stirring blade of the stirring paddle inside the product receiving kettle is located at the top of the product receiving kettle, and a plurality of stirring blades are uniformly arranged between the lowermost stirring blade and the uppermost stirring blade.

[0027] If the above stirring paddle device is not used, the temperature inside the product receiving kettle is not uniform, part of the product vapor is not condensed in time and is sucked away by the vacuum pump, resulting in a decrease in yield.

[0028] The refrigeration jacket is filled with low-temperature refrigerant and connected with an external cold trap for circulation, so that the refrigerant is always below the set temperature, thereby ensuring that the outer surface of the stirring paddle is also always below the set temperature; the refrigeration jacket is wrapped on the stirring paddle blade, the low-temperature surface area is larger, the product vapor is captured and condensed in time, and the yield is significantly improved.

[0029] The beneficial technical effects possessed by the utility model are:

[0030] 1. The 2-thiophene formaldehyde synthesis device of the utility model comprises a reaction section device, a hydrolysis section device and a distillation section device, different batches of feeding can be treated at the same time by each section device, the whole process from raw materials to products can be realized without transferring materials, continuous production can be realized, automatic production can be realized by using a central control program, the production cycle is shortened, and the quality of products is more stable;

[0031] 2. The functions of the hydrolysis section device include hydrolysis of intermediates and extraction of products into organic phase, two-step operation is carried out in the same kettle, land occupation is saved, equipment cost is reduced, water phase and organic phase are respectively received by the first receiving tank and the second receiving tank, and operation is simple;

[0032] 3. The distillation section uses atmospheric distillation equipment and vacuum distillation equipment in sequence to remove impurities with different properties; after the crude product is purified in the extraction, atmospheric distillation and vacuum distillation devices in sequence, high-quality products with purity > 99.3% can be obtained;

[0033] 4. A valve is arranged between the atmospheric distillation equipment and the vacuum distillation equipment, the valve is closed only when vacuum distillation is carried out, operation is more simple, and product loss is reduced;

[0034] 5. The feeding is carried out by using height difference, and flow control is carried out by using a control valve, so that energy is saved;

[0035] 6. The inlet end of the raw material tank is provided with multiple valves, selective feeding can be realized, land occupation is saved, and equipment cost is reduced;

[0036] 7. The temperature control kit and the distillation section device are combined, the products can be recovered by temperature combination between multiple kettles and pressure adjustment of the vacuum pump;

[0037] 8. The stirring paddle in the product receiving kettle is provided with a refrigeration jacket connected with a cold trap, refrigerant circulates in the refrigeration jacket, the refrigeration jacket is wrapped on the surface of the stirring paddle, and the larger low-temperature surface area of the refrigeration jacket is favorable for timely capturing product vapor and condensing. BRIEF DESCRIPTION OF DRAWINGS

[0038] Figure 1 It is a whole schematic view of the 2-thiophene formaldehyde synthesis device of the utility model;

[0039] Figure 2 It is a sectional structure schematic view of the stirring paddle in the product receiving kettle of the utility model;

[0040] Figure numerals: 1-first raw material tank, 11-first raw material valve, 12-second raw material valve, 13-first control valve, 14-first pipeline, 2-reactor, 21-first stirring paddle, 22-second control valve, 23-second pipeline, 3-second raw material tank, 31-third raw material valve, 32-fourth raw material valve, 33-third control valve, 4-hydrolysis tank, 41-second stirring paddle, 42-fourth control valve, 43-first receiving valve, 44-first receiving tank, 45-first discharge valve, 46-second receiving valve, 47-second receiving tank, 48-second discharge valve, 49- The third pipeline, 410-the fifth control valve, 5-the first distillation kettle, 51-the third stirring paddle, 52-the third discharge valve, 53-the fourth pipeline, 54-the sixth control valve, 6-the condenser, 61-the seventh control valve, 7-the second distillation kettle, 71-the fourth stirring paddle, 72-the fourth discharge valve, 73-the eighth control valve, 74-the fifth pipeline, 8-the product receiving kettle, 81-the fifth stirring paddle, 811-the refrigeration jacket inlet, 812-the refrigeration jacket, 813-the refrigeration jacket outlet, 82-the fifth discharge valve, 83-the ninth control valve, 84-the sixth pipeline, 9-the vacuum pump. DETAILED DESCRIPTION

[0041] The present invention will be further described below in conjunction with the accompanying drawings and embodiments. Identical components are denoted by the same reference numerals. It should be noted that the terms "front," "rear," "left," "right," "upper," and "lower" used in the following description refer to directions in the accompanying drawings, and the terms "bottom," "top," "inner," and "outer" refer to directions toward or away from the geometric center of a particular component, respectively.

[0042] In the device of the present invention, except for adding raw materials, extraction phase separation and atmospheric distillation, the transportation of other materials in the pipeline is powered by pumps arranged in the corresponding pipelines, the kettles are equipped with temperature control kits, the valves can control the flow of materials, and the stirring paddle is equipped with a power system to drive its own rotation.

[0043] like Figure 1 The 2-thiophenecarboxaldehyde synthesis device shown includes a reaction section device, a hydrolysis section device and a distillation section device; the reaction section device includes a first raw material tank 1 and a reactor 2, and the outlet end of the first raw material tank 1 is connected to the inlet end 2 of the reactor through a first pipe 14;

[0044] The hydrolysis section device includes a second raw material tank 3, a hydrolysis kettle 4, a first receiving tank 44 and a second receiving tank 47. The outlet end of the reactor 2 is connected to the inlet end of the hydrolysis kettle 4 through a second pipe 23. The outlet ends of the second raw material tank 3 are both connected to the inlet end of the hydrolysis kettle 4. The outlet end of the hydrolysis kettle 4 is connected to the inlet end of the first receiving tank 44 and the material inlet and outlet end of the second receiving tank 47.

[0045] The distillation section device comprises a normal pressure distillation device and a reduced pressure distillation device; the normal pressure distillation device comprises a first distillation kettle 5 and a condenser 6, the material inlet and outlet end of a second receiving tank 47 is connected with the inlet end of the first distillation kettle 5 through a third pipeline 49, and the outlet end of the first distillation kettle 5 is connected with the inlet end of the condenser 6 through a fifth pipeline 53;

[0046] The reduced pressure distillation device comprises a second distillation kettle 7, a product receiving kettle 8 and a vacuum pump 9, the outlet end of the condenser 6 is connected with the inlet end of the second distillation kettle 7, a seventh control valve 61 is arranged between the outlet end of the condenser 6 and the inlet end of the second distillation kettle 7, the outlet end of the second distillation kettle 7 is connected with the inlet end of the product receiving kettle 8 through a sixth pipeline 74, and the outlet end of the product receiving kettle 8 is connected with the vacuum pump 9 through a seventh pipeline 84.

[0047] The first raw material tank 1 is made of PP, the reaction kettle 2 is made of enamel, the second raw material tank 3 is made of PP, the hydrolysis kettle 4 is made of enamel, the first receiving tank 44 and the second receiving tank 47 are both made of PP, the first distillation kettle 5 is made of enamel, the condenser 6 is made of 304 stainless steel, the second distillation kettle 7 is made of PP, the product receiving kettle 8 is made of enamel, the fourth pipeline 54 is made of 304 stainless steel, and the first pipeline 14, the second pipeline 23, the third pipeline 49, the fifth pipeline 74 and the sixth pipeline 84 are all made of PP.

[0048] The operation steps of the 2-thiophene formaldehyde synthesis device are as follows:

[0049] The first raw material valve 11 and the first control valve 13 are opened, the mixed raw material liquid containing thiophene and N,N-dimethylformamide (DMF) enters the inside of the reaction kettle 2 along the first raw material tank 1 and the first pipeline 14, and the first stirring paddle 21 is opened to uniformly mix the mixed raw material liquid; the first raw material valve 11 and the first control valve 13 are closed, the second raw material valve 12 is opened, and phosphorus oxychloride is added into the first raw material tank 1; the first control valve 13 is opened and the appropriate flow rate is controlled, so that the phosphorus oxychloride enters the reaction kettle 2 through the first pipeline 14 at a low flow rate, after the addition of the phosphorus oxychloride is completed, the temperature control sleeve of the reaction kettle 2 is set to heat to react, after a period of time, the material in the reaction kettle presents black brown, and is cooled to room temperature.

[0050] Open the third raw material valve 31 and the third control valve 33, water enters the hydrolysis kettle 4 through the second raw material tank 3, the temperature control kit of the hydrolysis kettle 4 is set to heating, after completion, open the second control valve 22, the material in the reaction kettle 2 enters the hydrolysis kettle 4 along the second pipeline 23, at the same time, start the second stirring paddle 41; react for a period of time, at this time, open the third raw material valve 31 again, add sodium hydroxide solution to the second raw material tank 3, adjust the third control valve 33 to control the sodium hydroxide solution to enter the hydrolysis kettle 4 at a low flow rate, the instrument monitors the pH value of the material in the hydrolysis kettle 4, when the pH value reaches 6.5, close the third control valve 33; open the fourth raw material valve 32, toluene enters the hydrolysis kettle 4 along the second raw material tank 3 for extraction, after a period of time, close the second stirring paddle 41 and stand the liquid in the hydrolysis kettle 4, after a period of time, open the fourth control valve 42 and the first receiving valve 43, the lower aqueous phase enters the first receiving tank 44; after the aqueous phase is completely transferred, close the first receiving valve 43, open the second receiving valve 46, the remaining organic phase enters the second receiving tank 47; after the organic phase is completely transferred, close the second receiving valve 46, open the fifth control valve 410, the organic phase in the second receiving tank 47 enters the first distillation kettle 5 along the third pipeline 49.

[0051] The temperature control kit of the first distillation kettle 5 is set to heating, after heating to the appearance of reflux, it is set to heat preservation, after the reflux is stable, open the sixth control valve 54, steam enters the condenser 6 along the fourth pipeline 53, the seventh control valve 61 is opened by default, the steam is condensed into liquid and enters the second distillation kettle 7.

[0052] After the condenser 6 no longer condenses liquid, most of the product has been transferred into the second distillation kettle 7; at this time, close the seventh control valve 61, open the fourth stirring paddle 72, the eighth control valve 73, the ninth control valve 83 and the vacuum pump 9, carry out vacuum distillation, the product is distilled out and enters the product receiving kettle 8 through the fifth pipeline 74; the temperature control kit of the product receiving kettle 8 is set to low temperature, and the fifth stirring paddle 81 is opened, to ensure that the liquid material is uniformly cooled and no longer evaporates.

[0053] The cross-sectional view of the fifth stirring paddle 81 is shown in Figure 2 The fifth stirring paddle 81 contains 6 groups of symmetrical stirring paddle leaves, which cover the bottom to the top of the product receiving kettle 8, the outside of the stirring paddle leaves is wrapped with a refrigeration jacket 812, the inside of the refrigeration jacket 812 is filled with low-temperature refrigerant, the top is provided with a refrigeration jacket inlet 811 and a refrigeration jacket outlet 813, the refrigeration jacket inlet 811 and the refrigeration jacket outlet 813 are connected with an external cold trap; if the temperature control kit of the product receiving kettle 8 shows that the internal temperature is higher than the set temperature, the external cold trap quickly injects low-temperature refrigerant into the inside of the refrigeration jacket 812 from the refrigeration jacket inlet 811, the refrigerant originally heated and warmed in the inside of the refrigeration jacket 812 is discharged from the refrigeration jacket outlet 813 under the action of pressure, and returns to the external cold trap for recooling.

[0054] A part of impurities cannot be evaporated and are retained in the second distillation kettle 7, and another part of impurities are in the steam, which is pumped away by the vacuum pump 9; when the steam enters the product receiving kettle 8, the product steam therein contacts the rotating fifth stirring paddle 81, is condensed by cooling, and is retained in the product receiving kettle 8 at low temperature.

[0055] After a period of time, no product steam is condensed into the product receiving kettle 8, the vacuum pump 9 is closed, the fourth discharge valve 82 is opened, and the final product in the product receiving kettle 8 is discharged and collected; the temperature control sleeve of each kettle is closed, and the first discharge valve 45, the second discharge valve 48, the third discharge valve 52, and the fourth discharge valve 72 are opened in sequence, and the waste liquid is discharged and treated.

[0056] According to the above operation steps, under the design of the device of the utility model, the material will stay in each kettle of the device for a period of time, so that multiple batches of production operations can be performed at the same time, for example, three batches of products are synthesized at the same time, when the first batch of material is in the atmospheric distillation or vacuum distillation section, the second batch of material can be in the hydrolysis or extraction separation section, and the third batch of material can be in the heating reaction or cooling section; the central control program can be set to automatically perform continuous production of multiple batches to improve the yield.

[0057] In the case of simultaneous synthesis of three batches of products, the three batches of final products are sampled in sequence for high performance liquid chromatography detection, and the purity of the three batches of products is greater than 99.3%, which is high in purity and stable in quality.

[0058] The above is only the preferred embodiment of the utility model, and the protection scope of the utility model is not limited to the above-mentioned embodiments, and any technical solution belonging to the idea of the utility model belongs to the protection scope of the utility model. It should be noted that for ordinary technical personnel in the technical field, some improvements and decorations without departing from the principle of the utility model should be considered as the protection scope of the utility model.

Claims

1. An apparatus for the synthesis of 2-thiophenecarboxaldehyde, characterized by: The reaction section device, the hydrolysis section device and the distillation section device; the reaction section device comprises a first raw material tank and a reaction kettle, and the outlet end of the first raw material tank is connected with the inlet end of the reaction kettle; the hydrolysis section device comprises a second raw material tank, a hydrolysis kettle, a first receiving tank and a second receiving tank, and the outlet end of the reaction kettle and the outlet end of the second raw material tank are connected with the inlet end of the hydrolysis kettle, and the outlet end of the hydrolysis kettle is connected with the inlet end of the first receiving tank and the material inlet and outlet end of the second receiving tank; the distillation section device comprises an atmospheric distillation device and a vacuum distillation device; the atmospheric distillation device comprises a first distillation kettle and a condenser, and the material inlet and outlet end of the second receiving tank is connected with the inlet end of the first distillation kettle, and the outlet end of the first distillation kettle is connected with the inlet end of the condenser; the vacuum distillation device comprises a second distillation kettle, a product receiving kettle and a vacuum pump, and the outlet end of the condenser is connected with the inlet end of the second distillation kettle, and a valve is arranged between the outlet end of the condenser and the inlet end of the second distillation kettle, the outlet end of the second distillation kettle is connected with the inlet end of the product receiving kettle, and the outlet end of the product receiving kettle is connected with the vacuum pump.

2. The device for synthesis of 2-thiophenecarboxaldehyde according to claim 1, characterized by the fact that: The outlet end of the first raw material tank is located at the bottom of the first raw material tank, and the height of the outlet end of the first raw material tank is higher than the inlet end of the reaction kettle.

3. The apparatus for synthesis of 2-thiophenecarboxaldehyde according to claim 2, characterized in that: The outlet end of the first raw material tank is provided with a flow control valve.

4. The apparatus for synthesis of 2-thiophenecarboxaldehyde according to claim 1, wherein: The outlet end of the second raw material tank is located at the bottom of the second raw material tank, and the height of the outlet end of the second raw material tank is higher than the inlet end of the hydrolysis kettle.

5. The apparatus for synthesis of 2-thiophenecarboxaldehyde according to claim 4, characterized in that: The outlet end of the second raw material tank is provided with a flow control valve.

6. The device for synthesis of 2-thiophenecarboxaldehyde according to claim 1, characterized by the fact that: The inlet end of the first raw material tank and the inlet end of the second raw material tank are each provided with a plurality of valves.

7. The device for synthesis of 2-thiophenecarboxaldehyde according to claim 1, characterized by the fact that: The outlet end of the hydrolysis kettle is located at the bottom of the hydrolysis kettle, and the outlet end of the hydrolysis kettle is provided with a valve; the inlet end of the first receiving tank is provided with a first receiving valve, and a second receiving valve is arranged between the outlet end of the hydrolysis kettle and the material inlet and outlet end of the second receiving tank.

8. The device for synthesis of 2-thiophenecarboxaldehyde according to claim 1, characterized by the fact that: The reaction kettle, the hydrolysis kettle, the first distillation kettle, the second distillation kettle and the product receiving kettle are each provided with a temperature control set.

9. The device for synthesis of 2-thiophenecarboxaldehyde according to claim 1, characterized by the fact that: The stirring paddle in the product receiving kettle comprises a stirring paddle blade and a refrigeration jacket, the refrigeration jacket is wrapped on the surface of the stirring paddle blade, the inside of the refrigeration jacket is filled with refrigerant, and the inlet end and the outlet end of the refrigeration jacket are connected with an external circulating cold trap.

10. The apparatus for synthesis of 2-thiophenecarboxaldehyde according to claim 9, characterized in that: ​

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