Preparation method and preparation device of diethyl sulfate

Abstract

The present invention belongs to the technical field of preparation of chemical products, and specifically relates to a preparation method and a preparation device of diethyl sulfate. The preparation method of diethyl sulfate described in the present invention comprises the following steps: adding ethanol, an acid binding agent, and a stabilizer into a reaction tank, the obtained mixed solution is sequentially passed through a desalting tank, a low-temperature tubular device, and a sub-low-temperature tubular device for cyclic precooling and insoluble matter distribution in the filter layer of the desalting tank, sulfuryl chloride is injected into the reaction tank, and a cyclic desalting reaction is carried out to obtain a reaction solution; the reaction solution is subjected to post-treatment to obtain diethyl sulfate. The preparation method of diethyl sulfate provided by the present invention improves product benefits, is simple to operate, reduces the generation of by-products, has high conversion rate and high selectivity, and the present invention also provides a preparation device for diethyl sulfate.

Description

Technical Field

[0001] The invention belongs to the technical field of preparation of chemical products, and in particular relates to a preparation method and a preparation device for diethyl sulfate. Background Art

[0002] As a multifunctional ethylating agent, diethyl sulfate (DES) occupies a pivotal position in the fine chemical industry. It is not only an indispensable synthetic raw material in key fields such as medicine, dyes, and pesticides, but also widely used in the manufacturing process of industrial products such as plastics, resins, coatings, and inks, injecting strong impetus into the development of these industries. Especially in the field of medicine, diethyl sulfate, as a drug intermediate and synthetic reagent, participates in the synthesis of antibiotics, hormones, and certain anticancer drugs, and plays an irreplaceable role in improving medical standards and protecting human health. At the same time, its unique floral fragrance also makes it popular in the flavor industry such as edible flavors, perfume flavors, and soap flavors.

[0003] The preparation process of diethyl sulfate faces many challenges. At present, the synthesis routes of diethyl sulfate mainly include sulfur trioxide ether method, ethylene sulfate method, and ethyl hydrogen sulfate / sodium sulfate method. Although these methods can meet production needs to a certain extent, each of them has defects to varying degrees.

[0004] The sulfur trioxide ether method is a method for preparing diethyl sulfate using sulfur trioxide and diethyl ether as raw materials and diethyl sulfate or reaction synthesis liquid as diluent. Although it has the advantages of no waste acid and high yield, side reactions such as polymerization and oxidation of ether are prone to occur during the reaction, resulting in a high impurity content in the product, which increases the difficulty of subsequent separation and purification.

[0005] The method of preparing diethyl sulfate by using ethyl hydrogen sulfate or a mixture containing ethyl hydrogen sulfate and sulfate or hydrochloride optimizes the original ethanol sulfate method and ethylene sulfate method. However, due to the small experimental volume, there may be deviations after data amplification, and the experimental data show that the yield is low, which is difficult to meet the needs of large-scale production.

[0006] In addition, the existing diethyl sulfate preparation process also has problems such as cumbersome production process operation, high difficulty in reaction control, high technical requirements for operators, many by-products in the reaction process, high difficulty in subsequent distillation, and low production efficiency. These problems not only limit the production scale and quality of diethyl sulfate, but also increase production costs, affecting its wide application in various fields. Summary of the invention

[0007] The technical problem to be solved by the present invention is to overcome the above-mentioned defects in the prior art, provide a method for preparing diethyl sulfate, improve product benefits, simplify operation, reduce the generation of by-products, and have high conversion rate and high selectivity. The present invention also provides a device for preparing diethyl sulfate.

[0008] The preparation method of diethyl sulfate of the present invention comprises the following steps: adding ethanol, an acid binding agent and a stabilizer into a reaction tank, the obtained mixed solution is sequentially passed through a desalting tank, a low-temperature tubular device and a sub-low-temperature tubular device for cyclic precooling and the insoluble matter is distributed in the filter layer of the desalting tank, sulfuryl chloride is injected into the reaction tank, and a cyclic desalting reaction is carried out to obtain a reaction solution; and the reaction solution is subjected to post-treatment to obtain diethyl sulfate.

[0009] The control temperature of the low-temperature tubular device is 3-8°C; the control temperature of the sub-low-temperature tubular device is 8-13°C; and the control temperature of the reaction tank is 1-5°C.

[0010] The flow rate of sulfuryl chloride injected into the reaction tank (3) is 6.5-16.6 kg / h. After the injection is completed, the duration of the cyclic desalination reaction is 1-2 hours.

[0011] The acid binding agent is sodium formate or sodium acetate, and the stabilizer is ethyl formate or ethyl acetate.

[0012] The molar ratio of sulfuryl chloride to ethanol is 0.52-0.55:1; the molar ratio of the acid binding agent to ethanol is 0.94-0.97:1; and the molar ratio of the stabilizer to the acid binding agent is 0.3-0.5:1.

[0013] The post-treatment is first eluted with an organic elution solvent and then distilled.

[0014] The organic elution solvent is dichloromethane, n-pentane or isopentane.

[0015] The distillation is carried out at -0.098MPa to sequentially distill out the stabilizer, formic acid or acetic acid, and diethyl sulfate.

[0016] The diethyl sulfate preparation device comprises a reaction tank, a desalting tank, a low-temperature tubular device, and a sub-low-temperature tubular device. The liquid outlet of the reaction tank is connected to the desalting tank, the liquid outlet of the desalting tank is connected to a liquid separator, the gas outlet of the reaction tank is connected to a packing tower, the packing tower is connected to the sub-low-temperature tubular device, the sub-low-temperature tubular device is connected to the low-temperature tubular device, and the low-temperature tubular device is connected to the desalting tank and the liquid separator.

[0017] The reaction tank is connected to the sulfuryl chloride tank, the top of the desalting tank is connected to the organic washing liquid tank and the water washing liquid tank, and the top of the packing tower is connected to the residual gas absorption device.

[0018] Specifically, the preparation method of diethyl sulfate comprises the following steps:

[0019] (1) Ethanol, acid binding agent and stabilizer are mixed and added to the reaction tank. Then, the mixed solution is passed through a desalting tank, a low-temperature tubular device (3-8°C) and a sub-low-temperature tubular device (8-13°C) in sequence under stirring for cyclic precooling and distribution of insoluble matter in the filter layer of the desalting tank. The sulfuryl chloride in the sulfuryl chloride tank is slowly pumped into the reaction tank. The temperature in the reaction tank is controlled at 1-5°C to carry out a cyclic desalting reaction. The sulfuryl chloride is added for 3-5 hours. After the addition is completed, the cyclic reaction is continued for 1-2 hours.

[0020] (2) After the reaction is completed, the reaction liquid is pumped out for distillation, and then the reaction liquid is placed in a desalting tank for 1-2 hours to flow and absorb the adsorbed reaction liquid, and then the reaction liquid is pumped into the liquid to be distilled. The target product on the filtered salt is eluted twice with a low-boiling organic solvent (dichloromethane / n-pentane / isopentane) in the organic washing liquid tank, and the internal circulation is carried out for 45-90 minutes in turn, and then the liquid to be distilled is pumped into the distillation liquid for distillation; the water in the water washing liquid tank is pumped into the desalting tank to dissolve sodium chloride in water, and the dissolved liquid is pumped into the liquid separation tank for liquid separation treatment. The organic phase is separated and dehydrated and reused as the organic washing liquid, and the water phase is reused as the water washing liquid after the salt is separated;

[0021] (3) The solvent of the mixed liquid to be distilled is distilled off under normal pressure, and then the stabilizer, formic acid or acetic acid, and diethyl sulfate are distilled off in sequence under negative pressure of -0.098 MPa, and the stabilizer is recycled to obtain the target product diethyl sulfate.

[0022] The preparation process of diethyl sulfate of the present invention is:

[0023] ;

[0024] Sulfuryl chloride reacts with ethanol to produce diethyl sulfate and hydrogen chloride.

[0025] ;

[0026] The generated hydrogen chloride reacts with a carboxylate (RCOONa is sodium acetate or sodium formate) to generate sodium chloride and carboxylic acid, thereby removing the dissolved hydrogen chloride in the liquid phase reaction system.

[0027] Compared with the prior art, the present invention has the following beneficial effects:

[0028] (1) The method for preparing diethyl sulfate of the present invention uses by-product sulfuryl chloride as a raw material, which has low raw material cost and high recovery rate.

[0029] (2) The method for preparing diethyl sulfate of the present invention has a simple synthesis route, which ensures the operability of subsequent industrialization, and greatly reduces the occurrence of side reactions by lowering the temperature and removing hydrogen chloride from the system.

[0030] (3) The preparation device of the present invention is used to prepare diethyl sulfate, and the reaction site activity is high, the reaction conversion rate is high, and the selectivity is high. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 It is a schematic diagram of the device for preparing diethyl sulfate of the present invention.

[0032] In the figure: 1. Sulfuryl chloride tank; 2. 1# pump; 3. Reaction tank; 4. 2# pump; 5. Packing tower; 6. Residual gas absorption device; 7. 3# pump; 8. Desalting tank; 9. Low-temperature tubular device; 10. Sub-low-temperature tubular device; 11. 4# pump; 12. Organic washing liquid tank; 13. Water washing liquid tank; 14. Separation tank. DETAILED DESCRIPTION

[0033] The present invention will be further described below in conjunction with specific embodiments.

[0034] The devices used in the following embodiments are as follows: Figure 1 As shown, the preparation device of diethyl sulfate includes a reaction tank 3, a desalting tank 8, a low-temperature tubular device 9, and a sub-low-temperature tubular device 10. The liquid outlet of the reaction tank 3 is connected to the desalting tank 8, the liquid outlet of the desalting tank 8 is connected to a liquid separator 14, the gas outlet of the reaction tank 3 is connected to a packing tower 5, the packing tower 5 is connected to the sub-low-temperature tubular device 10, the sub-low-temperature tubular device 10 is connected to the low-temperature tubular device 9, and the low-temperature tubular device 9 is connected to the desalting tank 8.

[0035] The reaction tank 3 is connected to the sulfuryl chloride tank 1 , the top of the desalting tank 8 is connected to the organic washing liquid tank 12 and the water washing liquid tank 13 , and the top of the packing tower 5 is connected to the residual gas absorption device 6 .

[0036] A 1# pump 2 is arranged between the sulfuryl chloride tank 1 and the reaction tank 3, a 2# pump 4 is arranged between the liquid outlet of the reaction tank 3 and the desalting tank 8, a 4# pump 11 is arranged on the pipeline connecting the tank top of the desalting tank 8 with the organic washing liquid tank 12 and the water washing liquid tank 13, and a 3# pump 7 is arranged on the tank bottom pipeline of the desalting tank 8.

[0037] The sulfuryl chloride used in the present invention is by-product sulfuryl chloride, the content of which is ≥98.5%, and the content of ethanol is ≥99.9%.

[0038] Example 1

[0039] The preparation method of diethyl sulfate comprises the following steps:

[0040] (1) 20 kg of ethanol, 33.444 kg of sodium acetate and 15.284 kg of ethyl acetate were mixed and added to the reaction tank 3. Then, the mixed solution was passed through the desalting tank 8, the low-temperature tubular device 9 (the temperature was controlled at 5°C) and the sub-low-temperature tubular device 10 (the temperature was controlled at 11°C) in turn under stirring conditions for cyclic precooling and distribution of insoluble matter in the filter layer of the desalting tank 8. The sulfuryl chloride in the sulfuryl chloride tank 1 was slowly pumped into the reaction tank 3. The temperature in the reaction tank 3 was controlled at 3°C ​​for cyclic desalting reaction. The sulfuryl chloride was added for 4 hours and a total of 31.794 kg was added. After the addition was completed, the cyclic reaction was continued for 1.5 hours.

[0041] (2) After the reaction is completed, the reaction liquid in the reaction tank 3 is pumped out for distillation; then the reaction liquid adsorbed by the falling flow in the desalting tank 8 is pumped out for distillation; the low-boiling organic solvent dichloromethane in the organic washing liquid tank 12 is eluted with the target product diethyl sulfate on the filtered salt twice, and the internal circulation is carried out for 75 minutes, and the eluate is pumped out for distillation; the water in the water washing liquid tank 13 is pumped into the desalting tank 8, and the dissolved sodium chloride is pumped into the liquid separation tank 14 for liquid separation treatment. The organic phase is separated and dehydrated and then reused as the organic washing liquid, and the water phase is reused as the water washing liquid after the salt is separated;

[0042] (3) The mixed liquid to be distilled out in step (2) is distilled off dichloromethane under normal pressure, and then ethyl acetate, acetic acid and diethyl sulfate are distilled off in sequence under negative pressure of -0.098 MPa. The ethyl acetate is recycled to obtain 62.854 kg of the target product diethyl sulfate.

[0043] Example 2

[0044] The preparation method of diethyl sulfate comprises the following steps:

[0045] (1) 20.5 kg of ethanol, 35.374 kg of sodium acetate and 19.583 kg of ethyl acetate were mixed and added to the reaction tank 3. Then, the mixed solution was passed through the desalting tank 8, the low-temperature tubular device 9 (the temperature was controlled at 8°C) and the sub-low-temperature tubular device 10 (the temperature was controlled at 13°C) in turn under stirring conditions for cyclic precooling and distribution of insoluble matter in the filter layer of the desalting tank 8. The sulfuryl chloride in the sulfuryl chloride tank 1 was slowly pumped into the reaction tank 3. The temperature in the reaction tank 3 was controlled at 5°C for cyclic desalting reaction. The sulfuryl chloride was added for 3 hours and a total of 31.675 kg was added. After the addition was completed, the cyclic reaction was continued for 1 hour.

[0046] (2) After the reaction is completed, the reaction liquid in the reaction tank 3 is pumped out for distillation; then the reaction liquid adsorbed by the falling flow in the desalting tank 8 is pumped out for distillation; the low-boiling organic solvent dichloromethane in the organic washing liquid tank 12 is eluted with the target product diethyl sulfate on the filtered salt twice, and the internal circulation is carried out for 90 minutes, and the eluate is pumped out for distillation; the water in the water washing liquid tank 13 is pumped into the desalting tank 8, and the dissolved sodium chloride is pumped into the liquid separation tank 14 for liquid separation treatment. The organic phase is separated and dehydrated and then reused as the organic washing liquid, and the water phase is reused as the water washing liquid after the salt is separated;

[0047] (3) The mixed liquid to be distilled out in step (2) is distilled off dichloromethane under normal pressure, and then ethyl acetate, acetic acid and diethyl sulfate are distilled off in sequence under negative pressure of -0.098 MPa. The ethyl acetate is recycled to obtain 64.171 kg of the target product diethyl sulfate.

[0048] Example 3

[0049] The preparation method of diethyl sulfate comprises the following steps:

[0050] (1) 20.3 kg of ethanol, 35.029 kg of sodium acetate and 11.635 kg of ethyl acetate were mixed and added to the reaction tank 3. Then, the mixed solution was passed through the desalting tank 8, the low-temperature tubular device 9 (the temperature was controlled at 3°C) and the sub-low-temperature tubular device 10 (the temperature was controlled at 8°C) in turn under stirring conditions for cyclic precooling and distribution of insoluble matter in the filter layer of the desalting tank 8. The sulfuryl chloride in the sulfuryl chloride tank 1 was slowly pumped into the reaction tank 3. The temperature in the reaction tank 3 was controlled at 1°C for cyclic desalting reaction. The sulfuryl chloride was added for 5 hours and a total of 33.176 kg was added. After the addition was completed, the cyclic reaction was continued for 2 hours.

[0051] (2) After the reaction is completed, the reaction liquid in the reaction tank 3 is pumped out for distillation; then the reaction liquid adsorbed by the falling flow in the desalting tank 8 is pumped out for distillation; the low-boiling organic solvent dichloromethane in the organic washing liquid tank 12 is eluted with the target product diethyl sulfate on the filtered salt twice, and the internal circulation is carried out for 45 minutes, and the eluate is pumped out for distillation; the water in the water washing liquid tank 13 is pumped into the desalting tank 8, and the dissolved sodium chloride is pumped into the liquid separation tank 14 for liquid separation treatment. The organic phase is separated and dehydrated and then reused as the organic washing liquid, and the water phase is reused as the water washing liquid after the salt is separated;

[0052] (3) The mixed liquid to be distilled out in step (2) is distilled off dichloromethane under normal pressure, and then ethyl acetate, acetic acid and diethyl sulfate are distilled off in sequence under negative pressure of -0.098 MPa. The ethyl acetate is recycled to obtain 63.655 kg of the target product diethyl sulfate.

[0053] Example 4

[0054] The preparation method of diethyl sulfate comprises the following steps:

[0055] (1) 20.1 kg of ethanol, 34.684 kg of sodium acetate and 19.201 kg of ethyl acetate were mixed and added to the reaction tank 3. Then, the mixed solution was passed through the desalting tank 8, the low-temperature tubular device 9 (the temperature was controlled at 8°C) and the sub-low-temperature tubular device 10 (the temperature was controlled at 13°C) in turn under stirring conditions for cyclic precooling and distribution of insoluble matter in the filter layer of the desalting tank 8. The sulfuryl chloride in the sulfuryl chloride tank 1 was slowly pumped into the reaction tank 3. The temperature in the reaction tank 3 was controlled at 5°C for cyclic desalting reaction. The sulfuryl chloride was added for 5 hours and a total of 32.849 kg was added. After the addition was completed, the cyclic reaction was continued for 2 hours.

[0056] (2) After the reaction is completed, the reaction liquid in the reaction tank 3 is pumped out for distillation; then the reaction liquid adsorbed by the falling flow in the desalting tank 8 is pumped out for distillation; the low-boiling organic solvent n-pentane in the organic washing liquid tank 12 is eluted with the target product diethyl sulfate on the filtered salt twice, and the internal circulation is carried out for 90 minutes, and the eluate is pumped out for distillation; the water in the water washing liquid tank 13 is pumped into the desalting tank 8, and the dissolved sodium chloride is pumped into the liquid separation tank 14 for liquid separation treatment. The organic phase is separated and dehydrated and then reused as the organic washing liquid, and the water phase is reused as the water washing liquid after the salt is separated;

[0057] (3) The mixed liquid to be distilled out in step (2) is distilled off with n-pentane at normal pressure, and then ethyl acetate, acetic acid and diethyl sulfate are distilled off in sequence at a negative pressure of -0.098 MPa. The ethyl acetate is recycled to obtain 61.995 kg of the target product diethyl sulfate.

[0058] Example 5

[0059] The preparation method of diethyl sulfate comprises the following steps:

[0060] (1) 20 kg of ethanol, 28.61 kg of sodium formate and 9.638 kg of ethyl formate were mixed and added to the reaction tank 3. Then, the mixed solution was passed through the desalting tank 8, the low-temperature tubular device 9 (the temperature was controlled at 3°C) and the sub-low-temperature tubular device 10 (the temperature was controlled at 8°C) in turn under stirring conditions for cyclic precooling and distribution of insoluble matter in the filter layer of the desalting tank 8. The sulfuryl chloride in the sulfuryl chloride tank 1 was slowly pumped into the reaction tank 3. The temperature in the reaction tank 3 was controlled at 1°C for cyclic desalting reaction. The sulfuryl chloride was added for 3 hours and a total of 32.685 kg was added. After the addition was completed, the cyclic reaction was continued for 1.5 hours.

[0061] (2) After the reaction is completed, the reaction liquid in the reaction tank 3 is pumped out for distillation; then the reaction liquid adsorbed by the falling flow in the desalting tank 8 is pumped out for distillation; the low-boiling organic solvent isopentane in the organic washing liquid tank 12 is eluted with the target product diethyl sulfate on the filtered salt twice, and the internal circulation is carried out for 75 minutes in turn, and the eluate is pumped out for distillation; the water in the water washing liquid tank 13 is pumped into the desalting tank 8, and the dissolved sodium chloride is pumped into the liquid separation tank 14 for liquid separation treatment. The organic phase is separated and dehydrated and then reused as the organic washing liquid, and the water phase is reused as the water washing liquid after the salt is separated;

[0062] (3) The mixed liquid to be distilled out in step (2) is distilled off isopentane under normal pressure, and then ethyl formate, formic acid and diethyl sulfate are distilled off in sequence under negative pressure of -0.098 MPa. Ethyl formate is recycled to obtain 62.058 kg of the target product diethyl sulfate.

[0063] Comparative Example 1

[0064] This comparative example is the same as Example 1, except that the low-temperature tubular device 9 and the sub-low-temperature tubular device 10 in step (1) are omitted, the temperature in the reaction tank 3 is controlled to 11° C., and the other preparation conditions are the same.

[0065] Comparative Example 2

[0066] This comparative example is the same as Example 1, except that the low-temperature tubular device 9 (temperature controlled at 25° C.) and the sub-low-temperature tubular device 10 (temperature controlled at 35° C.) in step (1) are changed, and other preparation conditions are the same.

[0067] Comparative Example 3

[0068] This comparative example is the same as Example 1, except that the acid binding agent and stabilizer in step (1) are omitted, and other preparation conditions are the same.

[0069] Comparative Example 4

[0070] This comparative example is the same as Example 1, except that the molar ratio of the stabilizer ethyl acetate to the acid-binding agent sodium acetate in step (1) is reduced to 0.1:1, and the other preparation conditions are the same.

[0071] Comparative Example 5

[0072] This comparative example is the same as Example 1, except that the addition time of sulfuryl chloride in step (1) is increased to 1.5 h, and the other preparation conditions are the same.

[0073] The diethyl sulfate prepared in the above examples and comparative examples was tested for purity and its yield was calculated. The yields were all based on the mole of ethanol. The test results are shown in Table 1.

[0074] Table 1 Test results

[0075]

[0076] As can be seen from the results of Table 1, Comparative Example 1 cancels low temperature, sub-low temperature tubular device, and then raises the temperature of the reaction tank as a condition for increasing the reactivity of the reaction, and the yield and purity of the reaction are significantly lower than those of Example 1 under the same reaction time. Comparative Example 2 raises the temperature of the low temperature tubular device and the sub-low temperature tubular device from low temperature to normal temperature, which has a significant impact on the yield and purity of the reaction. It can be seen from Comparative Examples 3 and 4 that the acid binding agent and stabilizer are completely cancelled or the stabilizer addition ratio is reduced that in this reaction, the stabilizer and acid binding agent have a significant impact on the yield and purity of the product. Comparative Example 5 only changes the existence of the reaction under the condition that the addition amount does not change the reaction time, indicating that the acceleration of the amount of introduction needs to change other supporting parameters. And in the embodiments of the present invention, the yield and purity of the diethyl sulfate product are not greatly affected after the variables such as the temperature and pressure of each reaction process section are changed in a limited interval.

Claims

1. A method for preparing diethyl sulfate, characterized in that: The following steps are involved: Ethanol, an acid-binding agent, and a stabilizer are added to a reaction tank (3), and the obtained mixed solution is sequentially passed through a desalting tank (8), a low-temperature tubular device (9), and a sub-low-temperature tubular device (10) for cyclic precooling and distribution of insoluble matter in the filter layer of the desalting tank (8), and sulfuryl chloride is injected into the reaction tank (3) for cyclic desalting reaction to obtain a reaction solution; the reaction solution is post-treated to obtain diethyl sulfate; The controlled temperature of the low-temperature tubular device (9) is 3-8°C; the controlled temperature of the sub-low-temperature tubular device (10) is 8-13°C; and the controlled temperature of the reaction tank (3) is 1-5°C. The acid binding agent is sodium formate or sodium acetate; The stabilizer is ethyl formate or ethyl acetate; The molar ratio of the stabilizer to the acid binding agent is 0.3-0.5:

1.

2. The preparation method of diethyl sulfate according to claim 1, wherein: The flow rate of sulfuryl chloride injected into the reaction tank (3) is 6.5-16.6 kg / h. After the injection is completed, the duration of the cyclic desalination reaction is 1-2 hours.

3. The preparation method of diethyl sulfate according to claim 1, wherein: The molar ratio of sulfuryl chloride to ethanol is 0.52-0.55:1; the molar ratio of the acid binding agent to ethanol is 0.94-0.97:

1.

4. The preparation method of diethyl sulfate according to claim 1, wherein: The post-treatment is first eluted with an organic elution solvent and then distilled.

5. The preparation method of diethyl sulfate according to claim 4, characterized in that: The organic elution solvent is dichloromethane, n-pentane or isopentane.

6. The preparation method of diethyl sulfate according to claim 4, characterized in that: The distillation is carried out at -0.098MPa to sequentially distill out the stabilizer, formic acid or acetic acid, and diethyl sulfate.

7. A preparation device adopted by the method for preparing diethyl sulfate according to any one of claims 1 to 6, characterized in that: The invention comprises a reaction tank (3), a desalination tank (8), a low-temperature tubular device (9), and a sub-low-temperature tubular device (10); the liquid outlet of the reaction tank (3) is connected to the desalination tank (8); the liquid outlet of the desalination tank (8) is connected to a liquid separation tank (14); the gas outlet of the reaction tank (3) is connected to a packing tower (5); the packing tower (5) is connected to the sub-low-temperature tubular device (10); the sub-low-temperature tubular device (10) is connected to the low-temperature tubular device (9); and the low-temperature tubular device (9) is connected to the desalination tank (8).

8. The preparation device of diethyl sulfate according to claim 7, characterized in that: The reaction tank (3) is connected to the sulfuryl chloride tank (1), the top of the desalting tank (8) is connected to the organic washing liquid tank (12) and the water washing liquid tank (13), and the top of the packing tower (5) is connected to the residual gas absorption device (6).

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