TWI831090B - Method and device for manufacturing compounds from isobutyric acid and acetic anhydride - Google Patents

Abstract

A device and a method for manufacturing compounds from isobutyric acid and acetic anhydride are provided. The method for manufacturing compounds from isobutyric acid and acetic anhydride includes the following steps. Isobutyric acid is reacted with acetic anhydride to obtain a first mixture, wherein the first mixture includes isobutyric anhydride and acetic acid. The first mixture is subjected to a first purification process to obtain isobutyric anhydride and acetic acid. The isobutyric anhydride is subjected to a pyrolysis process to obtain a second mixture, wherein the second mixture includes dimethyl ketene, isobutyric acid and isobutyric anhydride. A gas-liquid separation process is performed on the second mixture to obtain dimethyl ketene gas and a liquid, wherein the liquid includes isobutyric acid and isobutyric anhydride. The liquid is collected, and then the isobutyric acid in the liquid is reacted with acetic anhydride.

Description

Methods for preparing compounds using isobutyric acid and acetic anhydride and devices for preparing compounds using isobutyric acid and acetic anhydride

The present disclosure relates to a method and device for preparing compounds using isobutyric acid and acetic anhydride.

2,2,4,4-tetramethyl-1,3-cyclobutanediol (CBDO) is a multifunctional intermediate with a symmetrical structure. It is widely used in the synthesis of copolyesters, such as high-performance polyesters that can replace polycarbonate (PC). The glass transition temperature of traditional polyester is low, and its application in medium and high temperature fields is subject to certain limitations. Adding 2,2,4,4-tetramethyl-1,3-cyclobutanediol can significantly improve the glass transition temperature, weather resistance and transparency of polyester. Polyester synthesized using 2,2,4,4-tetramethyl-1,3-cyclobutanediol has excellent physical properties similar to bisphenol A, such as high impact strength, excellent dimensional stability, glass transfer The temperature is high.

Continuous improvement and control of chemical reaction processes (such as environmentally friendly processes, reduction of energy consumption and waste emissions, improvement of yield and purity) are the goals of continuous efforts in the chemical industry. Based on the above, the industry needs a novel production process of 2,2,4,4-tetramethyl-1,3-cyclobutanediol to increase the yield of the product and reduce the production of by-products.

According to embodiments of the present disclosure, the present disclosure provides a method of preparing a compound using isobutyric acid and acetic anhydride. The method for preparing compounds using isobutyric acid and acetic anhydride includes the following steps. Isobutyric acid and acetic anhydride are reacted to obtain a first mixture, wherein the first mixture includes isobutyric anhydride and acetic acid. The first mixture is subjected to a first purification process to obtain isobutyric anhydride and acetic acid; the isobutyric anhydride is subjected to a cracking process to obtain a second mixture, wherein the second mixture includes dimethyl ketene, isobutyric acid and isobutyric acid. acid anhydride; perform a gas-liquid separation process on the second mixture to obtain dimethylketene gas and a liquid, wherein the liquid contains isobutyric acid and isobutyric anhydride; and collect the liquid, and make the isobutyric acid in the liquid Reacts with acetic anhydride. According to embodiments of the present disclosure, the method of preparing a compound using isobutyric acid and acetic anhydride may further include at least one of the following steps. After performing the first purification process, the acetic acid is collected. A jet suction process is used to collect the dimethylketene gas at 5°C to 25°C and normal pressure (eg, about 750 Torr to 770 Torr). Dimerization of dimethyl ketene yields 2,2,4,4-tetramethyl-1,3-cyclobutanedione. 2,2,4,4-Tetramethyl-1,3-cyclobutanedione is mixed with a solvent to obtain a solution, wherein the solid content of the solution is 5 wt% to 20 wt%. The solution is hydrogenated with hydrogen to obtain a third mixture, wherein the third mixture includes 2,2,4,4-tetramethyl-1,3-cyclobutanediol, hydrogen, and a solvent. The third mixture is subjected to a second purification process to obtain 2,2,4,4-tetramethyl-1,3-cyclobutanediol.

According to embodiments of the present disclosure, the present disclosure provides a device for preparing compounds from isobutyric acid and acetic anhydride. The device for preparing compounds from isobutyric acid and acetic anhydride includes a feeding unit; a first reaction unit, wherein the feeding unit is connected to the first reaction unit to introduce isobutyric acid and acetic anhydride from the feeding unit into the a first reaction unit, wherein the isobutyric acid reacts with acetic anhydride in the first reaction unit to obtain a first mixture, wherein the first mixture includes isobutyric anhydride and acetic acid; a first purification unit, wherein the first reaction unit Connected to the first purification unit to introduce the first mixture into the first purification unit, wherein the first mixture undergoes a first purification process in the first purification unit to obtain isobutyric anhydride and acetic acid; a cracking unit , wherein the first purification unit is connected to the cracking unit to introduce isobutyric anhydride into the cracking unit, wherein isobutyric anhydride undergoes a cracking process in the cracking unit to obtain a second mixture, wherein the second mixture contains dimethyl Enone, isobutyric acid and isobutyric anhydride; and, a gas-liquid separation unit, wherein the cracking unit is connected to the gas-liquid separation unit to introduce the second mixture into the gas-liquid separation unit, wherein the second mixture is in the gas-liquid separation unit. The separation unit separates dimethyl ketene gas and a liquid, wherein the liquid includes isobutyric acid and isobutyric anhydride, and the feeding unit is connected to the gas-liquid separation unit to introduce the liquid into the feeding unit. According to embodiments of the present disclosure, the method of preparing a compound using isobutyric acid and acetic anhydride may further include at least one of the following units. An acetic acid collection unit, wherein the acetic acid collection unit is connected to the first purification unit for collecting acetic acid obtained from the first purification unit. A second reaction unit, wherein the gas-liquid separation unit is connected to the second reaction unit to introduce the dimethyl ketene gas into the second reaction unit, wherein the dimethyl ketene gas is in the second reaction unit The reaction forms 2,2,4,4-tetramethyl-1,3-cyclobutanedione. A suction unit, wherein the second reaction unit is connected to the gas-liquid separation unit through the suction unit, wherein the suction unit performs a jet suction process on the dimethyl ketene gas to make the second reaction The unit receives the dimethylketene gas at 5°C to 25°C and normal pressure (eg, 750 Torr to 770 Torr). A solvent supply unit, wherein the solvent supply unit is connected to the suction unit to supply a solvent to the suction unit for the spray suction process. A solid-liquid separation unit, wherein the second reaction unit is connected to the solid-liquid separation unit to separate the solvent and 2,2,4,4-tetramethyl-1,3-cyclobutane di The ketone is introduced into the solid-liquid separation unit to separate 2,2,4,4-tetramethyl-1,3-cyclobutanedione from the solvent in solid form. A hydrogenation unit, wherein the solid-liquid separation unit is connected with the hydrogenation unit to introduce 2,2,4,4-tetramethyl-1,3-cyclobutanedione into the hydrogenation unit, wherein the solvent supply unit is connected with the hydrogenation unit The unit is connected to introduce the solvent into the hydrogenation unit, wherein the 2,2,4,4-tetramethyl-1,3-cyclobutanedione reacts with hydrogen in the presence of the solvent to obtain a third mixture, wherein the The third mixture contains 2,2,4,4-tetramethyl-1,3-cyclobutanediol, hydrogen, and solvent. A second purification unit, wherein the hydrogenation unit is connected to the second purification unit to introduce the third mixture into the second purification unit, wherein the third mixture undergoes a purification process in the second purification unit to obtain 2, 2, 4, 4-Tetramethyl-1,3-cyclobutanediol, hydrogen, and solvent. A collection unit, wherein the collection unit is connected to the second purification unit for collecting 2,2,4,4-tetramethyl-1,3-cyclobutanediol.

According to embodiments of the present disclosure, the present disclosure provides a method of preparing a compound using isobutyric acid and acetic anhydride. The method for preparing compounds using isobutyric acid and acetic anhydride is carried out with the above-mentioned device and includes the following steps. Isobutyric acid and acetic anhydride are reacted in the first reaction unit to obtain a first mixture, wherein the first mixture includes isobutyric anhydride and acetic acid. The first mixture is introduced into the first purification unit to perform a first purification process on the first mixture to obtain isobutyric anhydride and acetic acid. Isobutyric anhydride is introduced into a cracking unit to perform a cracking process on isobutyric anhydride to obtain a second mixture, wherein the second mixture includes dimethyl ketene, isobutyric acid and isobutyric anhydride. The second mixture is introduced into a gas-liquid separation unit to perform a gas-liquid separation process on the second mixture to obtain dimethyl ketene gas and a liquid, wherein the liquid includes isobutyric acid and isobutyric anhydride. The liquid is introduced into the feed unit. According to embodiments of the present disclosure, the method of preparing a compound using isobutyric acid and acetic anhydride may further include at least one of the following steps. Isobutyric acid and acetic anhydride are introduced into the first reaction unit from the feeding unit. The acetic acid obtained is introduced into an acetic acid collection unit. A liquid containing isobutyric acid and isobutyric anhydride is introduced into the first reaction unit from the feeding unit to react the isobutyric acid and acetic anhydride in the liquid. The dimethylketene gas is introduced into a second reaction unit. Dimethylketene gas is dimerized in the second reaction unit to form 2,2,4,4-tetramethyl-1,3-cyclobutanedione. A suction unit is used to perform a jet suction process on dimethyl ketene to introduce dimethyl ketene gas from the gas-liquid separation unit into the second reaction unit. A solvent supply unit is used to supply a solvent to the suction unit to perform the spray suction process. 2,2,4,4-tetramethyl-1,3-cyclobutanedione and the solvent are mixed in a hydrogenation unit to obtain a solution, wherein the solid content of the solution is 5 wt% to 20 wt%. The solution and hydrogen are hydrogenated in the hydrogenation unit to obtain a third mixture, wherein the third mixture includes 2,2,4,4-tetramethyl-1,3-cyclobutanediol, hydrogen, and solvents. The third mixture is introduced into a second purification unit to perform a second purification process on the third mixture to obtain 2,2,4,4-tetramethyl-1,3-cyclobutanediol, hydrogen, and solvent . The solvent supply unit is used to recover the solvent separated by the second purification process. The hydrogen separated by the second purification process is introduced into the hydrogenation unit. The 2,2,4,4-tetramethyl-1,3-cyclobutanediol separated in the second purification process is introduced into a collection unit.

The method and device for preparing compounds using isobutyric acid and acetic anhydride described in the present disclosure are described in detail below. It should be understood that the following description provides many different embodiments or examples for implementing different aspects of the present invention. The specific components and arrangements described below are only used to briefly describe the present invention. Of course, these are only examples and not limitations of the present invention. Furthermore, repeated reference numbers or designations may be used in different embodiments. These repetitions are only for the purpose of simply and clearly describing the present invention and do not imply any correlation between the different embodiments and/or structures discussed.

It is to be understood that elements specifically described or illustrated may exist in a variety of forms known to those skilled in the art. The ordinal numbers used in the specification and claims, such as "first", "second", "third", etc., are used to modify the elements of the claim. They do not in themselves imply or represent that the claim element has any previous elements. Ordinal numbers do not represent the order between a certain request component and another request component, or the order in the manufacturing method. The use of these ordinal numbers is only used to enable one request component with a certain name to be compared with another request with the same name. Components can be clearly distinguished.

The present disclosure provides a method and device for preparing compounds using isobutyric acid and acetic anhydride. According to embodiments of the present disclosure, the compound prepared using isobutyric acid and acetic anhydride may be acetic acid, dimethylketene, 2,2,4,4-tetramethyl-1,3-cyclobutanedione, and or 2,2,4,4-Tetramethyl-1,3-cyclobutanediol. The method of preparing compounds using isobutyric acid and acetic anhydride described in the present disclosure can be a continuous process, and the device for preparing compounds using isobutyric acid and acetic anhydride can be applied to the method of preparing compounds using isobutyric acid and acetic anhydride. .

According to embodiments of the present disclosure, the methods and devices for preparing compounds using isobutyric acid and acetic anhydride may not only include the preparation and cleavage of isobutyric anhydride, but may further include dimerization of dimethyl ketene gas, and Hydrogenation reaction of 2,2,4,4-tetramethyl-1,3-cyclobutanedione. According to the embodiments of the present disclosure, the methods and devices of the present disclosure for preparing compounds using isobutyric acid and acetic anhydride can process by-products (such as isobutyric acid) obtained after the cleavage of isobutyric anhydride and unreacted starting materials (such as isobutyric acid). butyric anhydride) for recycling.

According to embodiments of the present disclosure, the methods and devices of the present disclosure for preparing compounds using isobutyric acid and acetic anhydride can use a jet suction process to collect the obtained dimethylketene gas. Since the pressure difference in the jet suction process comes from the flow rate of the solvent, dimethyl ketene gas can be collected at 5°C to 25°C and normal pressure (for example, 750 Torr to 770 Torr) to improve the concentration of dimethyl ketene gas. Collection efficiency. The conventional technology uses a low-temperature and low-pressure liquid phase absorption process to collect liquid dimethyl ketene. Therefore, it is necessary to use low pressure (for example, less than 80 Torr) to reduce the boiling point of dimethyl ketene and store it at low temperature (for example, less than -10°C). Collect dimethylketene under the environment. Therefore, compared with the conventional low-temperature and low-pressure liquid phase absorption process, the present disclosure uses a jet suction process to collect dimethyl ketene gas, which can not only significantly reduce energy consumption, but also reduce the loss of dimethyl ketene (i.e. Increase the yield of dimethylketene).

According to embodiments of the present disclosure, the methods and devices of the present disclosure for preparing compounds using isobutyric acid and acetic anhydride are to perform a dimerization reaction on dimethyl ketene at a relatively low temperature (for example, less than 75°C) to form 2,2 ,4,4-tetramethyl-1,3-cyclobutanedione. In this way, the formation of by-products (such as oligomers) can be reduced and the selectivity of 2,2,4,4-tetramethyl-1,3-cyclobutanedione can be improved. According to the embodiments of the present disclosure, the selectivity of 2,2,4,4-tetramethyl-1,3-cyclobutanedione formed through the dimerization reaction can be as high as over 96%.

According to the embodiments of the present disclosure, the methods and devices of the present disclosure for preparing compounds using isobutyric acid and acetic anhydride are used to prepare 2,2,4,4-tetramethyl-1 at relatively low temperatures (for example, less than 80°C). , 3-cyclobutanedione undergoes hydrogenation reaction. In this way, the generation of by-products (such as cyclic ketone by-products, ring-open ketone by-products, or 2,2,4-trimethyl-1,3-pentanediol) can be greatly reduced. According to the embodiments of the present disclosure, the selectivity of forming 2,2,4,4-tetramethyl-1,3-cyclobutanediol through hydrogenation reaction can be as high as more than 96%.

Figure 1 is a flow chart of a method 10 for preparing a compound using isobutyric acid and acetic anhydride according to an embodiment of the present disclosure.

The method 10 of the present disclosure for preparing compounds using isobutyric acid and acetic anhydride includes the following steps. First, isobutyric acid and acetic anhydride are reacted (for example, esterification reaction) to obtain a first mixture (step 12), wherein the first mixture includes isobutyric anhydride and acetic acid. According to embodiments of the present disclosure, isobutyric acid and acetic anhydride can be thoroughly mixed before performing the reaction. Next, the first mixture obtained in step 12 is subjected to a first purification process to obtain isobutyric anhydride and acetic acid (step 14). According to embodiments of the present disclosure, the first purification process may include a distillation process. According to embodiments of the present disclosure, the first purification process may include a stirring process and a distillation process. Before performing a distillation process on the first mixture, a stirring process is performed on the first mixture. According to an embodiment of the present disclosure, after performing the first purification process, the acetic acid is collected. Next, the isobutyric anhydride obtained in step 14 is subjected to a cracking process to obtain a second mixture, wherein the second mixture includes dimethyl ketene, isobutyric acid and isobutyric anhydride (step 16). In this cracking process, isobutyric anhydride can be preheated at 280°C to 350°C, and then isobutyric anhydride is heated to between 400°C and 500°C to thermally crack isobutyric anhydride. According to embodiments of the present disclosure, the pressure of the cracking process can be between 60 Torr and 120 Torr, the process time can be between 0.01 seconds and 1 second, and the conversion rate of isobutyric anhydride can be greater than or equal to 45%. For example, between 45% and 70%. According to embodiments of the present disclosure, the cracking process can be performed after mixing a carrier gas (such as argon or nitrogen) and isobutyric anhydride gas. Next, a gas-liquid separation process is performed on the second mixture obtained in step 16 to obtain dimethyl ketene gas and a liquid, wherein the liquid includes isobutyric acid and isobutyric anhydride (step 18).

According to the embodiment of the present disclosure, after performing the gas-liquid separation process, the method 10 of preparing a compound using isobutyric acid and acetic anhydride may further include: collecting the liquid, and removing the isobutyric acid and acetic anhydride in the liquid. reaction (step 20).

Figure 2 is a flow chart of a method 50 for preparing a compound using isobutyric acid and acetic anhydride according to certain embodiments of the present disclosure. According to the embodiment of the present disclosure, after performing the gas-liquid separation process, the method 50 of preparing the compound using isobutyric acid and acetic anhydride may further include: using a jet suction process at 5°C to 25°C and 750 Torr to Collect the dimethylketene gas at 770 Torr (step 22). This disclosure uses a jet suction process to collect dimethyl ketene gas. In addition to significantly reducing energy consumption (that is, dimethyl ketene can be collected under normal pressure without cooling the temperature below -10°C), it can also reduce the amount of dimethyl ketene gas. Escape of methyl ketene (i.e. increase the yield of dimethyl ketene). According to an embodiment of the present disclosure, the pressure difference of the jet suction process comes from the flow rate of the solvent, and the solvent used may be an ester solvent, such as isobutyl isobutyrate, ethyl propionate, or octyl acetate. According to embodiments of the present disclosure, during the jet suction process, the solvent can dissolve (absorb) dimethylketene to form an ester solution containing dimethylketene. According to embodiments of the present disclosure, the dimethylketene concentration of the dimethylketene-containing ester solution may be 10 wt% to 40wt%, based on the total weight of the dimethylketene and solvent. According to an embodiment of the present disclosure, after collecting the dimethyl ketene gas (or forming an ester solution containing dimethyl ketene), the method 50 of preparing a compound using isobutyric acid and acetic anhydride may further include : Dimerization reaction of dimethylketene to obtain 2,2,4,4-Tetramethyl-1,3-cyclobutanedione , TMCD) (step 24). According to embodiments of the present disclosure, the temperature of the dimerization reaction can be controlled between 20°C and 75°C. If the reaction temperature is too low, the reaction is too slow and the reaction time needs to be increased. If the reaction temperature is too high, by-products (such as polyester or polyketone oligomers) will be produced during the dimerization reaction, which will reduce the production of 2,2,4,4-tetramethyl-1,3-cyclobutanedi. Ketone yield and purity. For example, if dimethyl ketene is dimerized at 75°C, the amount of polyester or polyketone oligomer obtained will increase approximately 1.42 times (compared to dimethyl ketene dimerized at 70°C). (compared to the amount of polyester or polyketone oligomer obtained from the polymerization reaction). According to embodiments of the present disclosure, the dimerization reaction time may be between 2 hours and 24 hours.

In addition, according to embodiments of the present disclosure, the dimerization reaction can be performed in an inert gas (such as nitrogen or argon) environment. According to embodiments of the present disclosure, dimethyl ketene can undergo dimerization reaction in the presence of a catalyst. The disclosure does not limit the catalyst used, and it can be a conventional catalyst used for dimerization of dimethyl ketene. According to the embodiments of the present disclosure, if an ester solvent (such as isobutyl isobutyrate) is used, the solubility of ester solvent to 2,2,4,4-tetramethyl-1,3-cyclobutanedione is low. , the 2,2,4,4-tetramethyl-1,3-cyclobutanedione formed after the dimerization reaction tends to precipitate. Therefore, after the dimerization reaction is completed, a process (such as a recrystallization process and/or a filtration process) can be used to collect the 2,2,4,4-tetramethyl-1,3-cyclobutanedione solid, and use a solvent to Carry out cleaning to obtain high-purity 2,2,4,4-tetramethyl-1,3-cyclobutanedione (purity can be greater than 99wt%).

According to an embodiment of the present disclosure, after performing a dimerization reaction on dimethyl ketene, the method 50 of preparing a compound using isobutyric acid and acetic anhydride may further include: converting 2, 2, 4 obtained in step 24, 4-Tetramethyl-1,3-cyclobutanedione is mixed with a solvent to obtain a solution (step 26), and the solution obtained in step 26 is hydrogenated with hydrogen to obtain a third mixture, wherein the third mixture is The third mixture contains 2,2,4,4-tetramethyl-1,3-cyclobutanediol, hydrogen, and solvent (step 28). According to embodiments of the present disclosure, the solid content of the solution may be 5 wt% to 20 wt%. According to an embodiment of the present disclosure, the solution containing 2,2,4,4-tetramethyl-1,3-cyclobutanedione can be hydrogenated with hydrogen in the presence of a catalyst to form 2,2, 4,4-Tetramethyl-1,3-cyclobutanediol (2,2,4,4-Tetramethyl-1,3-cyclobutanediol, CBDO). The disclosure does not limit the catalyst used, and it can be a conventional catalyst used for hydrogenating 2,2,4,4-tetramethyl-1,3-cyclobutanedione. According to embodiments of the present disclosure, the hydrogen pressure of the hydrogenation reaction may be between 10 bar and 120 bar, for example, between 30 bar and 70 bar. According to embodiments of the present disclosure, the temperature of the hydrogenation reaction may be 50°C to 80°C, and the pressure of the hydrogenation reaction may be 1MPa to 10MPa. Table 1 shows the selectivity of each product obtained from the hydrogenation reaction of 2,2,4,4-tetramethyl-1,3-cyclobutanedione at 60°C and 135°C (other reaction conditions are the same).

Table 1 Hydrogenation reaction temperature Selection rate (%) CBDO cyclic ketone products Ring-open ketone products TMPD 135℃ 89.9 0.26 7.5 2.4 60℃ 99.2 0.14 0.06 0

It can be seen from Table 1 that although the hydrogenation rate increases as the temperature rises, if the temperature of the hydrogenation process is too high, by-products (cyclic ketone products, ring-opened ketone products, or 2,2,4- The ratio of 2,2,4-Trimethyl-1,3-pentanediol (TMPD).

According to an embodiment of the present disclosure, after hydrogenating 2,2,4,4-tetramethyl-1,3-cyclobutanedione, the method of preparing a compound using isobutyric acid and acetic anhydride 50 It may further include: performing a second purification process on the third mixture to obtain 2,2,4,4-tetramethyl-1,3-cyclobutanediol (step 30). According to embodiments of the present disclosure, the second purification process may include a phase separation process to recover hydrogen and obtain a solution including 2,2,4,4-tetramethyl-1,3-cyclobutanediol and a solvent. . According to embodiments of the present disclosure, the second purification process may further include a distillation process to recover the solvent and remove by-products (cyclic ketone by-products, ring-opened ketone by-products) to obtain 2,2,4,4-tetrakis Methyl-1,3-cyclobutanediol.

According to embodiments of the present disclosure, the present disclosure also provides a device for preparing compounds using isobutyric acid and acetic anhydride. Figure 3 is a schematic diagram of a device 100 for preparing compounds using isobutyric acid and acetic anhydride according to an embodiment of the present disclosure.

As shown in Figure 3, the device 100 for preparing compounds using isobutyric acid and acetic anhydride may include a feeding unit 110, a first reaction unit 115, a first purification unit 120, a cracking unit 125, and a gas-liquid Separation unit 130. The feeding unit 110 is connected to the first reaction unit 115 to introduce isobutyric acid and acetic anhydride from the feeding unit 110 into the first reaction unit 115 . In the first reaction unit 115, the isobutyric acid reacts with acetic anhydride in the first reaction unit to obtain a first mixture, wherein the first mixture includes isobutyric anhydride and acetic acid. According to the embodiment of the present disclosure, the first reaction unit 115 may be, for example, a continuous stirred reactor. The first reaction unit 115 is connected to the first purification unit 120 to introduce the first mixture into the first purification unit 120 . The first mixture can be subjected to a first purification process in the first purification unit to obtain isobutyric anhydride and acetic acid. According to embodiments of the present disclosure, the first purification unit 120 may include a distillation column. The first purification unit 120 is connected to the cleavage unit 125 to introduce isobutyric anhydride into the cleavage unit 125 . Isobutyric anhydride undergoes a cracking process in the cracking unit to obtain a second mixture, wherein the second mixture includes dimethyl ketene, isobutyric acid and isobutyric anhydride. According to embodiments of the present disclosure, the cracking unit 125 may include an evaporator and a cracking reactor (not shown). The isobutyric anhydride supplied from the purification unit 120 is preheated by the evaporator and then introduced into the cracking reactor for high-temperature cracking reaction. The cracking unit 125 is connected to the gas-liquid separation unit 130 to introduce the second mixture into the gas-liquid separation unit 130, wherein the second mixture is separated into a dimethyl ketene gas and a liquid in the gas-liquid separation unit 130, The liquid includes isobutyric acid and isobutyric anhydride, and the feeding unit 110 is connected to the gas-liquid separation unit 130 to introduce the liquid into the feeding unit 110 . According to the embodiment of the present disclosure, the feeding unit 110 may further introduce the liquid into the first reaction unit 115 to react with acetic anhydride. According to an embodiment of the present disclosure, the device 100 for preparing compounds using isobutyric acid and acetic anhydride may further include an acetic acid collection unit 135, wherein the acetic acid collection unit 135 is connected to the first purification unit 120 for collecting the first purification process. Acetic acid separated by unit 120.

Figure 4 is a schematic diagram of a device 200 for preparing compounds using isobutyric acid and acetic anhydride according to an embodiment of the present disclosure. According to the embodiment of the disclosure, the device for preparing compounds using isobutyric acid and acetic anhydride in the embodiment of the disclosure except the feeding unit 110, the first reaction unit 115, the first purification unit 120, the cracking unit 125, and In addition to the gas-liquid separation unit 130, it may further include a second reaction unit 140, a suction unit 145, a solvent supply unit 150, a solid-liquid separation unit 155, a hydrogenation unit 160, a second purification unit 165, and At least one of the collection units 170 .

According to an embodiment of the present disclosure, as shown in Figure 4, in order to dimerize dimethylketene to form 2,2,4,4-tetramethyl-1,3-cyclobutanedione, the gas-liquid The separation unit 130 may be connected with the second reaction unit 140 to introduce the dimethyl ketene gas into the second reaction unit 140 . The dimethyl ketene gas undergoes a dimerization reaction in the second reaction unit 140 to form 2,2,4,4-tetramethyl-1,3-cyclobutanedione.

According to the embodiment of the present disclosure, in order to enable the second reaction unit 140 to fully receive the dimethyl ketene gas obtained from the gas-liquid separation unit 130 at 5°C to 25°C and normal pressure (for example, 750 Torr to 770 Torr), The device 200 for preparing compounds using isobutyric acid and acetic anhydride according to the present disclosure may further include a suction unit 145 . The second reaction unit 140 is connected to the gas-liquid separation unit 130 through the suction unit, wherein the suction unit 145 can perform a spray suction process on the dimethyl ketene gas, so that the gas-liquid separation unit 130 The separated dimethylketene gas may be received by the second reaction unit 140 .

According to an embodiment of the present disclosure, the device 200 for preparing compounds using isobutyric acid and acetic anhydride may further include a solvent supply unit 150, wherein the solvent supply unit 150 is connected to the suction unit 145 to supply the suction. Unit 145 performs the spray pumping process with a solvent. During the jet suction process, the solvent can dissolve (absorb) dimethylketene to form an ester solution containing dimethylketene. According to the embodiment of the present disclosure, the dimethyl ketene gas collected by the second reaction unit 140 can also be further dissolved in the solvent to form an ester solution containing dimethyl ketene.

According to the embodiment of the present disclosure, the second reaction unit 140 can be used to dimerize dimethyl ketene to obtain 2,2,4,4-tetramethyl-1,3-cyclobutanedione (2 ,2,4,4-Tetramethyl-1,3-cyclobutanedione, TMCD). According to embodiments of the present disclosure, in the second reaction unit 140, the temperature of the dimerization reaction can be controlled between 20°C and 75°C to reduce the formation of by-products (such as oligomers) and improve 2,2,4 , selectivity of 4-tetramethyl-1,3-cyclobutanedione. According to embodiments of the present disclosure, an inert gas (such as nitrogen or argon) may be introduced into the second reaction unit 140 so that the dimerization reaction is performed in an inert gas environment. According to embodiments of the present disclosure, the second reaction unit 140 may include a reactor (such as a continuously stirred reactor) and a set of crystallizers (not shown). The dimethyl ketene supplied from the gas-liquid separation unit 130 undergoes a dimerization reaction through a stirred reactor, and the obtained 2,2,4,4-tetramethyl-1,3-cyclobutanedione (TMCD) is then passed through The crystallizer formed 2,2,4,4-tetramethyl-1,3-cyclobutanedione solid.

According to an embodiment of the present disclosure, the device 200 for preparing compounds using isobutyric acid and acetic anhydride may further include a solid-liquid separation unit 155, wherein the second reaction unit 140 is connected to the solid-liquid separation unit 155 to separate the The product obtained by the second reaction unit 140 (including solvent and 2,2,4,4-tetramethyl-1,3-cyclobutanedione solid) is introduced into the solid-liquid separation unit 155 . Through the solid-liquid separation unit 155, 2,2,4,4-tetramethyl-1,3-cyclobutanedione can be separated from the solvent in solid form. According to embodiments of the present disclosure, the solid-liquid separation unit 155 can be connected to the solvent supply unit 150 to utilize the solvent supply unit 150 to recover the solvent. According to the embodiment of the present disclosure, the solvent supply unit 150 can recover, purify, and reuse the solvent.

According to an embodiment of the present disclosure, the device 200 for preparing compounds using isobutyric acid and acetic anhydride may further include a hydrogenation unit 160, wherein the solid-liquid separation unit 155 is connected to the hydrogenation unit 160 to combine 2,2, 4,4-Tetramethyl-1,3-cyclobutanedione is introduced into the hydrogenation unit 160 . According to an embodiment of the present disclosure, the solvent supply unit 150 can be connected to the hydrogenation unit to introduce the solvent into the hydrogenation unit 160. 2,2,4,4-Tetramethyl-1,3-cyclobutanedione can be used in the hydrogenation process. Unit 160 performs a hydrogenation reaction to obtain a third mixture, wherein the third mixture includes 2,2,4,4-tetramethyl-1,3-cyclobutanediol, hydrogen, and a solvent. According to embodiments of the present disclosure, the hydrogenation unit 160 may include a stirrer, a gas supplier, and a reactor. The stirrer can mix 2,2,4,4-tetramethyl-1,3-cyclobutanedione with the solvent to form a solution, and introduce the solution into the reactor. The gas supplier can provide gas (such as hydrogen, or hydrogen and carrier gas) into the reactor, so that 2,2,4,4-tetramethyl-1,3-cyclobutanedione can react in the presence of hydrogen. Hydrogenation reaction takes place in the reactor.

According to an embodiment of the disclosure, the device 200 for preparing compounds using isobutyric acid and acetic anhydride may further include a second purification unit 165, wherein the hydrogenation unit 160 is connected to the second purification unit 165 to connect the third The mixture is introduced into the second purification unit 165. The third mixture can be subjected to a purification process in the second purification unit to separate 2,2,4,4-tetramethyl-1,3-cyclobutanediol, hydrogen, and solvent. According to embodiments of the present disclosure, the second purification unit 165 may be connected to the solvent supply unit 150 to utilize the solvent supply unit 150 to recover the solvent. According to embodiments of the present disclosure, the second purification unit 165 may introduce unreacted hydrogen gas into the hydrogenation unit 160. According to embodiments of the present disclosure, the second purification unit 165 may include a separator and a distillation column (not shown). The separator can separate gases (for example, including hydrogen and carrier gas) and liquids (for example, including 2,2,4,4-tetramethyl-1,3-cyclobutanediol, solvents, and by-products), The gas is introduced into the hydrogenation unit 160 and the liquid is introduced into the distillation column. This distillation tower can separate 2,2,4,4-tetramethyl-1,3-cyclobutanediol and the solvent from the liquid, and introduce the solvent into the solvent supply unit 150 . According to embodiments of the present disclosure, the solvent supply unit may include a purification component and a storage component (not shown). The purification component can purify the liquid recovered by the solid-liquid separation unit 155 and the second purification unit, so as to introduce the solvent into the suction unit 145 and the hydrogenation unit 160 for reuse.

According to an embodiment of the present disclosure, the device 200 for preparing compounds using isobutyric acid and acetic anhydride may further include a collection unit 170, wherein the collection unit 170 is connected to the second purification unit 165 for collecting 2,2 ,4,4-tetramethyl-1,3-cyclobutanediol.

According to embodiments of the present disclosure, the present disclosure provides a method of preparing a compound using isobutyric acid and acetic anhydride. The method of preparing compounds using isobutyric acid and acetic anhydride can be carried out using the device shown in Figure 3 or Figure 4. Figure 5 is a flow chart of a method 300 for preparing a compound using isobutyric acid and acetic anhydride according to an embodiment of the present disclosure. The method 300 can be performed using the device shown in Figure 3 .

According to an embodiment of the disclosure, the method 300 of preparing a compound using isobutyric acid and acetic anhydride includes the following steps. Isobutyric acid and acetic anhydride are introduced into the first reaction unit 115 from the feeding unit 110 (step 310). Isobutyric acid and acetic anhydride are subjected to a reaction (such as esterification reaction) in the first reaction unit to obtain a first mixture, wherein the first mixture includes isobutyric anhydride and acetic acid (step 320). According to embodiments of the present disclosure, isobutyric acid and acetic anhydride can be thoroughly mixed before performing the reaction. Next, the first mixture is introduced into the first purification unit 120 to perform a first purification process on the first mixture to obtain isobutyric anhydride and acetic acid (step 330). According to embodiments of the present disclosure, the first purification process may include a stirring process and a distillation process. Before performing a distillation process on the first mixture, a stirring process is performed on the first mixture. According to the embodiment of the present disclosure, after performing the first purification process, an acetic acid collection unit 135 can collect the acetic acid. Next, isobutyric anhydride is introduced from the first purification unit 120 into a cracking unit 125 to perform a cracking process on isobutyric anhydride to obtain a second mixture, wherein the second mixture includes dimethyl ketene, isobutyric acid and isobutyric acid. Anhydride (step 340). In this cracking process, isobutyric anhydride can be preheated at 280°C to 350°C, and then isobutyric anhydride is heated to between 400°C and 500°C to thermally crack isobutyric anhydride. According to embodiments of the present disclosure, the pressure of the cracking process can range from 60 Torr to 120 Torr, the process time can range from 0.01 seconds to 1 second, and the conversion rate of isobutyric anhydride can range from 50% to 70 between %. According to embodiments of the present disclosure, the cracking process can be performed after mixing a carrier gas (such as argon or nitrogen) and isobutyric anhydride gas. Next, the second mixture is introduced into a gas-liquid separation unit 130 to perform a gas-liquid separation process on the second mixture to obtain dimethyl ketene gas and a liquid, wherein the liquid includes isobutyric acid and isobutyric anhydride (step 350) .

According to an embodiment of the disclosure, after performing the gas-liquid separation process, the method 300 of preparing a compound using isobutyric acid and acetic anhydride may further include: introducing the liquid into the feeding unit 110 (step 360). According to an embodiment of the present disclosure, the method 300 of preparing a compound using isobutyric acid and acetic anhydride may further include: introducing a liquid from the feed unit 110 to the first reaction unit 115 so that the isobutyl in the liquid Acid and acetic anhydride react in the first reaction unit 115 .

Figures 6A and 6B are step flow charts of a method 400 for preparing compounds using isobutyric acid and acetic anhydride according to certain embodiments of the present disclosure. The method 400 can be performed using the device shown in Figure 4 .

According to an embodiment of the present disclosure, after using the gas-liquid separation unit 130 to perform a gas-liquid separation process on the second mixture, the method 400 of preparing a compound using isobutyric acid and acetic anhydride may include: using a suction unit 145. Perform a jet suction process on the dimethyl ketene gas to introduce the dimethyl ketene gas from the gas-liquid separation unit 130 into the second reaction unit 140 (step 410). Through the jet suction process, the second reaction unit described in the present disclosure can collect the dimethyl ketene gas in an environment of 5°C to 25°C and 750 Torr to 770 Torr (ie, normal pressure). According to an embodiment of the present disclosure, the pressure difference of the jet suction process comes from the flow rate of the solvent, and the solvent used may be an ester solvent, such as isobutyl isobutyrate, ethyl propionate, or octyl acetate. According to embodiments of the present disclosure, during the jet suction process, the solvent can dissolve (absorb) dimethylketene to form an ester solution containing dimethylketene. According to embodiments of the present disclosure, the dimethylketene concentration of the dimethylketene-containing ester solution may be 10 wt% to 70wt%, based on the total weight of the dimethylketene and solvent. According to the embodiment of the present disclosure, a solvent supply unit 150 can be connected to the suction unit 145 to supply a solvent to the suction unit 145 for the spray suction process. During the jet suction process, the solvent can dissolve (absorb) dimethylketene to form an ester solution containing dimethylketene. According to the embodiment of the present disclosure, the dimethyl ketene gas collected by the second reaction unit 140 can also be further dissolved in the solvent to form an ester solution containing dimethyl ketene.

According to an embodiment of the present disclosure, after introducing dimethyl ketene into the second reaction unit 140, the method 400 of preparing a compound using isobutyric acid and acetic anhydride may include: adding dimethyl ketene gas in the second reaction unit 140. A dimerization reaction is performed in the second reaction unit 140 to form 2,2,4,4-tetramethyl-1,3-cyclobutanedione (step 420). According to the embodiment of the present disclosure, the temperature of the second reaction unit 140 can be controlled between 20°C and 75°C. In other words, the dimerization reaction is carried out at 20°C to 75°C. If the reaction temperature is too low, the reaction is too slow and the reaction time needs to be increased. If the reaction temperature is too high, polyester or polyketone oligomers will be produced during the dimerization reaction, reducing the yield and purity of 2,2,4,4-tetramethyl-1,3-cyclobutanedione. . According to embodiments of the present disclosure, the dimerization reaction time may be between 2 hours and 24 hours. In addition, according to embodiments of the present disclosure, an inert gas (such as nitrogen or argon) can be introduced into the second reaction unit 140 so that the dimerization reaction is performed in an inert gas environment. According to the embodiments of the present disclosure, if an ester solvent (such as isobutyl isobutyrate) is used, the solubility of ester solvent to 2,2,4,4-tetramethyl-1,3-cyclobutanedione is low. , the 2,2,4,4-tetramethyl-1,3-cyclobutanedione formed after the dimerization reaction tends to precipitate. Therefore, after the dimerization reaction is completed, a process (such as a recrystallization process and/or a filtration process) can be used to collect the 2,2,4,4-tetramethyl-1,3-cyclobutanedione solid, and use a solvent to Carry out cleaning to obtain high-purity 2,2,4,4-tetramethyl-1,3-cyclobutanedione (purity can be greater than 96wt%).

According to an embodiment of the present disclosure, after performing a dimerization reaction on dimethyl ketene, the method 400 of preparing a compound using isobutyric acid and acetic anhydride may include: converting the dimerization product (including 2, 2, 4,4-tetramethyl-1,3-cyclobutanedione and solvent) are introduced into a solid-liquid separation unit 155 from the second reaction unit 140 to perform a solid-liquid separation process (step 430). Specifically, in the solid-liquid separation unit 155, the product of the dimerization reaction (including 2,2,4,4-tetramethyl-1,3-cyclobutanedione and solvent) can pass through the solid-liquid separation unit 155. The separation process separates 2,2,4,4-tetramethyl-1,3-cyclobutanedione from the solvent in solid form. According to the embodiment of the present disclosure, the solid-liquid separation unit 155 can be connected to the solvent supply unit 150 , so the liquid separated by the solid-liquid separation unit 155 can be introduced into the solvent supply unit 150 for recovery, so that the solvent can be recycled through the solvent supply unit 150 Purify and reuse.

According to the embodiment of the present disclosure, after performing the solid-liquid separation process, the method 400 of preparing a compound using isobutyric acid and acetic anhydride may further include: converting 2,2,4,4-tetramethyl-1,3 - cyclobutanedione and solvent are introduced into a hydrogenation unit 160 and mixed to obtain a solution (step 440). Then, the hydrogenation unit 160 is used to perform a hydrogenation reaction on the obtained solution to obtain a third mixture, wherein the third mixture includes 2,2,4,4-tetramethyl-1,3-cyclobutanediol, hydrogen , and solvent (step 450). According to the embodiment of the present disclosure, the 2,2,4,4-tetramethyl-1,3-cyclobutanedione can be introduced into the hydrogenation unit 160 from the solid-liquid separation unit 155, and the solvent can be introduced from the solvent supply unit 150 introduced into the hydrogenation unit 160. According to the embodiment of the present disclosure, a gas (such as hydrogen, or hydrogen and carrier gas) can be introduced into the hydrogenation unit 160 so that 2,2,4,4-tetramethyl-1,3-cyclobutanedione and hydrogen Carry out hydrogenation reaction. The solution may have a solids content of 5 to 20 wt%. In addition, according to embodiments of the present disclosure, the solution containing 2,2,4,4-tetramethyl-1,3-cyclobutanedione can be hydrogenated with hydrogen in the presence of a catalyst to form 2, 2,4,4-Tetramethyl-1,3-cyclobutanediol. According to embodiments of the present disclosure, the hydrogen pressure of the hydrogenation reaction may be between 10 bar and 120 bar, for example, between 30 bar and 70 bar. According to embodiments of the present disclosure, the temperature of the hydrogenation reaction may be 50°C to 80°C, and the pressure of the hydrogenation reaction may be 1MPa to 10MPa. Since the hydrogenation reaction is carried out at relatively low temperatures, by-products (such as cyclic ketone by-products, ring-opened ketone by-products, or 2,2,4-trimethyl-1,3-pentanediol) can be significantly reduced. ) generation.

According to an embodiment of the present disclosure, after performing the hydrogenation reaction, the method 400 of preparing a compound using isobutyric acid and acetic anhydride may further include: introducing the third mixture into a second purification unit 165 to purify the third mixture. A second purification process is performed to obtain 2,2,4,4-tetramethyl-1,3-cyclobutanediol, hydrogen, and solvent (step 460). According to embodiments of the present disclosure, the second purification process may include a phase separation process to recover hydrogen and obtain a solution including 2,2,4,4-tetramethyl-1,3-cyclobutanediol and a solvent. . According to embodiments of the present disclosure, the second purification process may further include a distillation process to recover the solvent and remove by-products (cyclic ketone by-products, ring-opened ketone by-products) to obtain 2,2,4,4-tetrakis Methyl-1,3-cyclobutanediol. According to the embodiment of the present disclosure, after performing the second purification process, the solvent supply unit 150 can be used to recover the solvent separated by the second purification process, and the hydrogen separated by the second purification process can be used by the second purification process. Purification unit 165 is introduced into this second reaction unit 160 .

According to an embodiment of the disclosure, after performing the second purification process, the method 400 of preparing a compound using isobutyric acid and acetic anhydride may further include: 2, 2, 4, 4 separated by the second purification process. Tetramethyl-1,3-cyclobutanediol is introduced into a collection unit 170 (step 470).

Based on the above, the method and device of the present disclosure for preparing compounds using isobutyric acid and acetic anhydride can be used to cleave isobutyric anhydride to obtain by-products (such as isobutyric acid) and unreacted starting materials (such as isobutyric anhydride) Reuse. In addition, the method and device for preparing compounds using isobutyric acid and acetic anhydride described in the present disclosure can use a jet suction process to collect the obtained dimethyl ketene gas, thereby significantly reducing energy consumption and improving the efficiency of dimethyl ketene. Yield. Furthermore, according to the embodiments of the present disclosure, the methods and devices of the present disclosure for preparing compounds using isobutyric acid and acetic anhydride are formed by performing a dimerization reaction on dimethyl ketene at a relatively low temperature (for example, less than 75°C). 2,2,4,4-Tetramethyl-1,3-cyclobutanedione. In this way, the generation of by-products (such as oligomers) can be reduced and the selectivity of 2,2,4,4-tetramethyl-1,3-cyclobutanedione can be improved (according to the embodiments of the present disclosure, the selectivity can be as high as 99% or more). On the other hand, the methods and devices of the present disclosure for preparing compounds using isobutyric acid and acetic anhydride are used to prepare 2,2,4,4-tetramethyl-1,3 at relatively low temperatures (for example, less than 80°C). -Cyclobutanedione undergoes hydrogenation reaction. In this way, the generation of by-products (such as cyclic ketone by-products, ring-open ketone by-products, or 2,2,4-trimethyl-1,3-pentanediol) can be greatly reduced.

Although the disclosure has been disclosed in several embodiments, this is not intended to limit the disclosure. Anyone with ordinary knowledge in the art can make any changes and modifications without departing from the spirit and scope of the disclosure. , therefore, the scope of protection of this disclosure shall be subject to the scope of the appended patent application.

10, 50, 300, 400: Methods for preparing compounds using isobutyric acid and acetic anhydride 12, 14, 16, 18, 20, 22, 24, 26, 28, 30, 310, 320, 330, 340, 350, 360, 410, 420, 430, 440, 450, 460, 470: Steps 100, 200: Device for preparing compounds using isobutyric acid and acetic anhydride 110: Feeding unit 115: First response unit 120: First purification unit 125:Cracking unit 130:Gas-liquid separation unit 135: Acetic acid collection unit 140: Second reaction unit 145:Suction unit 150: Solvent supply unit 155:Solid-liquid separation unit 160:Hydrogenation unit 165: Second purification unit 170: Collection unit

Figure 1 is a flow chart of a method 10 for preparing a compound using isobutyric acid and acetic anhydride according to an embodiment of the present disclosure. Figure 2 is a flow chart of a method 50 for preparing a compound using isobutyric acid and acetic anhydride according to certain embodiments of the present disclosure. Figure 3 is a schematic diagram of a device 100 for preparing compounds using isobutyric acid and acetic anhydride according to an embodiment of the present disclosure. Figure 4 is a schematic diagram of a device 200 for preparing compounds using isobutyric acid and acetic anhydride according to certain embodiments of the present disclosure. Figure 5 is a flow chart of a method 300 for preparing compounds using isobutyric acid and acetic anhydride according to certain embodiments of the present disclosure. Figures 6A and 6B are step flow diagrams of a method 400 for preparing compounds using isobutyric acid and acetic anhydride according to certain embodiments of the present disclosure.

10: Method for preparing compounds using isobutyric acid and acetic anhydride

12, 14, 16, 18, 20: Steps

Claims (34)

A method for preparing compounds using isobutyric acid and acetic anhydride, including: reacting isobutyric acid and acetic anhydride to obtain a first mixture, wherein the first mixture includes isobutyric anhydride and acetic acid; performing a step on the first mixture A first purification process obtains isobutyric anhydride and acetic acid; a cracking process is performed on isobutyric anhydride to obtain a second mixture, wherein the second mixture includes dimethyl ketene, isobutyric acid and isobutyric anhydride; for the third The two mixtures are subjected to a gas-liquid separation process to obtain dimethyl ketene gas and a liquid, wherein the liquid contains isobutyric acid and isobutyric anhydride; a jet suction process is used to collect at 5°C to 25°C and 750Torr to 770Torr. The dimethyl ketene gas; and collecting the liquid, and reacting isobutyric acid and acetic anhydride in the liquid. The method of preparing a compound using isobutyric acid and acetic anhydride as described in claim 1 further includes: collecting the acetic acid after performing the first purification process. The method for preparing a compound using isobutyric acid and acetic anhydride as described in claim 1 further includes: performing a dimerization reaction on the dimethyl ketene to obtain 2,2,4,4-tetramethyl-1, 3-cyclobutanedione. The method of preparing a compound using isobutyric acid and acetic anhydride as described in claim 3, wherein the dimerization reaction temperature is 20°C to 75°C. The method for preparing a compound using isobutyric acid and acetic anhydride as described in claim 3, further comprising: mixing the 2,2,4,4-tetramethyl-1,3-cyclobutanedione with a solvent to obtain A solution, wherein the solid content of the solution is 5wt% to 20wt%; and the solution is subjected to a hydrogenation reaction with hydrogen to obtain a third mixture, wherein the third mixture contains 2,2,4,4-tetramethyl -1,3-cyclobutanediol, hydrogen, and solvent. The method of preparing a compound using isobutyric acid and acetic anhydride as described in claim 5, wherein the temperature of the hydrogenation reaction is 50°C to 80°C, and the pressure of the hydrogenation reaction is 1MPa to 10MPa. The method for preparing a compound using isobutyric acid and acetic anhydride as described in claim 5, further comprising: performing a second purification process on the third mixture to obtain 2,2,4,4-tetramethyl-1,3 -Cyclobutanediol. A device for preparing compounds using isobutyric acid and acetic anhydride, including: a feeding unit; a first reaction unit, wherein the feeding unit is connected to the first reaction unit to feed isobutyric acid and acetic anhydride from the feeding unit The material unit is introduced into the first reaction unit, wherein the isobutyl The acid reacts with acetic anhydride in the first reaction unit to obtain a first mixture, wherein the first mixture includes isobutyric anhydride and acetic acid; a first purification unit, wherein the first reaction unit is connected to the first purification unit to The first mixture is introduced into the first purification unit, wherein the first mixture is subjected to a first purification process in the first purification unit to obtain isobutyric anhydride and acetic acid; a cracking unit, wherein the first purification unit and the The cleavage unit is connected to introduce isobutyric anhydride into the cleavage unit, wherein isobutyric anhydride undergoes a cleavage process in the cleavage unit to obtain a second mixture, wherein the second mixture includes dimethyl ketene, isobutyric acid and isobutyric acid. Butyric anhydride; a gas-liquid separation unit, wherein the cracking unit is connected to the gas-liquid separation unit to introduce the second mixture into the gas-liquid separation unit, wherein the second mixture is separated into dimethyl in the gas-liquid separation unit Enone gas and a liquid, wherein the liquid contains isobutyric acid and isobutyric anhydride, wherein the feeding unit is connected to the gas-liquid separation unit to introduce the liquid into the feeding unit; a second reaction unit, wherein the The gas-liquid separation unit is connected to the second reaction unit to introduce the dimethyl ketene gas into the second reaction unit, wherein the dimethyl ketene gas reacts in the second reaction unit to form 2,2,4 , 4-tetramethyl-1,3-cyclobutanedione; and a suction unit, wherein the second reaction unit is connected to the gas-liquid separation unit through the suction unit, wherein the suction unit is The dimethyl ketene gas undergoes a jet suction process to make the second reaction unit operate at 5°C to 25°C and 750Torr to 770Torr. The dimethylketene gas is received below. The device for preparing compounds using isobutyric acid and acetic anhydride as described in claim 8, wherein the feeding unit introduces the liquid into the first reaction unit to react with acetic anhydride. The device for preparing compounds using isobutyric acid and acetic anhydride as described in claim 8, further comprising: an acetic acid collection unit, wherein the acetic acid collection unit is connected to the first purification unit for collecting the product obtained from the first purification unit. of acetic acid. The device for preparing compounds using isobutyric acid and acetic anhydride as described in claim 8, further comprising: a solvent supply unit, wherein the solvent supply unit is connected to the suction unit to supply a solvent to the suction unit for the spraying Aspiration process. The device for preparing compounds using isobutyric acid and acetic anhydride as described in claim 11, further comprising: a solid-liquid separation unit, wherein the second reaction unit is connected to the solid-liquid separation unit to combine the solvent and 2,2 ,4,4-tetramethyl-1,3-cyclobutanedione is introduced into the solid-liquid separation unit, so that 2,2,4,4-tetramethyl-1,3-cyclobutanedione is in solid form Separate from the solvent. The device for preparing compounds using isobutyric acid and acetic anhydride as described in claim 12, wherein the solid-liquid separation unit is connected to the solvent supply unit to utilize the solvent supply unit to recover the solvent. Preparation of chemical compounds using isobutyric acid and acetic anhydride as described in claim 12 The compound device further includes: a hydrogenation unit, wherein the solid-liquid separation unit is connected to the hydrogenation unit to introduce 2,2,4,4-tetramethyl-1,3-cyclobutanedione into the hydrogenation unit , wherein the solvent supply unit is connected to the hydrogenation unit to introduce the solvent into the hydrogenation unit, wherein the 2,2,4,4-tetramethyl-1,3-cyclobutanedione reacts with hydrogen in the presence of a solvent , a third mixture is obtained, wherein the third mixture contains 2,2,4,4-tetramethyl-1,3-cyclobutanediol, hydrogen, and a solvent. The device for preparing compounds using isobutyric acid and acetic anhydride as claimed in claim 14, further comprising: a second purification unit, wherein the hydrogenation unit is connected to the second purification unit to introduce the third mixture into the second purification unit , wherein the third mixture is subjected to a purification process in the second purification unit to obtain 2,2,4,4-tetramethyl-1,3-cyclobutanediol, hydrogen, and solvent. The device for preparing compounds using isobutyric acid and acetic anhydride as described in claim 15, wherein the second purification unit is connected to the solvent supply unit to utilize the solvent supply unit to recover the solvent. The device for preparing compounds using isobutyric acid and acetic anhydride as described in claim 15, wherein the second purification unit introduces the hydrogen into the hydrogenation unit. The device for preparing compounds using isobutyric acid and acetic anhydride as described in claim 15, further comprising: a collection unit, wherein the collection unit is connected to the second purification unit for Collect 2,2,4,4-tetramethyl-1,3-cyclobutanediol. A method for preparing compounds using isobutyric acid and acetic anhydride, which method is carried out using the device described in claim 8, including: reacting isobutyric acid and acetic anhydride in the first reaction unit to obtain the first mixture, wherein The first mixture includes isobutyric anhydride and acetic acid; the first mixture is introduced into the first purification unit to perform the first purification process on the first mixture to obtain isobutyric anhydride and acetic acid; isobutyric anhydride is introduced into the cracking unit A cracking process is performed on isobutyric anhydride to obtain the second mixture, wherein the second mixture includes dimethyl ketene, isobutyric acid and isobutyric anhydride; the second mixture is introduced into the gas-liquid separation unit to The second mixture is subjected to the gas-liquid separation process to obtain dimethyl ketene gas and a liquid, wherein the liquid contains isobutyric acid and isobutyric anhydride; the suction unit is used to perform a jet suction process on dimethyl ketene , to introduce dimethyl ketene gas from the gas-liquid separation unit into the second reaction unit; and introduce the liquid into the feeding unit. The method of preparing a compound using isobutyric acid and acetic anhydride as described in claim 19 further includes: introducing isobutyric acid and acetic anhydride into the first reaction unit from the feeding unit. The method of preparing a compound using isobutyric acid and acetic anhydride as described in claim 19, after performing the first purification process, further includes: The acetic acid obtained is introduced into an acetic acid collection unit. The method for preparing compounds using isobutyric acid and acetic anhydride as described in claim 19, after performing the gas-liquid separation process, further includes: introducing the liquid from the feeding unit to the first reaction unit to allow the liquid to Reaction of isobutyric acid with acetic anhydride. The method for preparing compounds using isobutyric acid and acetic anhydride as described in claim 19, after performing the gas-liquid separation process, further includes: introducing the dimethyl ketene gas into a second reaction unit; and introducing the two Methyl ketene gas undergoes dimerization reaction in the second reaction unit to form 2,2,4,4-tetramethyl-1,3-cyclobutanedione. The method of preparing a compound using isobutyric acid and acetic anhydride as described in claim 23, wherein the temperature of the dimerization reaction is 20°C to 75°C. The method of preparing a compound using isobutyric acid and acetic anhydride as described in claim 19, wherein the second reaction unit receives the dimethyl ketene gas at 5°C to 25°C and 750Torr to 770Torr. The method of preparing a compound using isobutyric acid and acetic anhydride as described in claim 19 further includes: using a solvent supply unit to supply a solvent to the suction unit to perform the jet suction process. The method for preparing compounds using isobutyric acid and acetic anhydride as described in claim 26, further comprising: The solvent and the 2,2,4,4-tetramethyl-1,3-cyclobutanedione are introduced into a solid-liquid separation unit to make the 2,2,4,4-tetramethyl-1,3- The cyclobutanedione is separated from the solvent in solid form. The method for preparing a compound using isobutyric acid and acetic anhydride as described in claim 23 further includes: combining the 2,2,4,4-tetramethyl-1,3-cyclobutanedione and a solvent in a Mix in the hydrogenation unit to obtain a solution, wherein the solid content of the solution is 5wt% to 20wt%. The method of preparing a compound using isobutyric acid and acetic anhydride as described in claim 28 further includes: hydrogenating the solution and hydrogen in the hydrogenation unit to obtain a third mixture, wherein the third mixture contains 2, 2,4,4-Tetramethyl-1,3-cyclobutanediol, hydrogen, and solvent. The method of preparing a compound using isobutyric acid and acetic anhydride as described in claim 29, wherein the temperature of the hydrogenation reaction is 50°C to 80°C, and the pressure of the hydrogenation reaction is 1MPa to 10MPa. The method of preparing a compound using isobutyric acid and acetic anhydride as described in claim 29, further comprising: introducing the third mixture into a second purification unit to perform a second purification process on the third mixture to obtain 2,2 ,4,4-tetramethyl-1,3-cyclobutanediol, hydrogen, and solvent. Preparation of chemical compounds using isobutyric acid and acetic anhydride as described in claim 31 The method of compound further includes: utilizing the solvent supply unit to recover the solvent separated by the second purification process. The method of preparing a compound using isobutyric acid and acetic anhydride as described in claim 30 further includes: introducing the hydrogen separated by the second purification process into the hydrogenation unit. The method for preparing a compound using isobutyric acid and acetic anhydride as described in claim 30, further comprising: converting 2,2,4,4-tetramethyl-1,3-cyclobutanediose separated in the second purification process. The alcohol is introduced into a collection unit.

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