CN116217355A - Process for producing fluoroacetal compound - Google Patents
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- CN116217355A CN116217355A CN202310506030.9A CN202310506030A CN116217355A CN 116217355 A CN116217355 A CN 116217355A CN 202310506030 A CN202310506030 A CN 202310506030A CN 116217355 A CN116217355 A CN 116217355A
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- C07C41/56—Preparation of compounds having groups by reactions producing groups by condensation of aldehydes, paraformaldehyde, or ketones
Abstract
The application relates to a preparation method of a fluoro acetal compound, which comprises the following steps: reacting an aldehyde polymer compound with a fluoroalcohol compound in the presence of a depolymerizing agent to prepare the fluoroacetal compound. The preparation method of the fluoro-acetal compound can effectively improve the synthesis efficiency of the fluoro-acetal compound and is beneficial to industrial production.
Description
Technical Field
The application relates to the technical field of compound preparation, in particular to a preparation method of a fluoro-acetal compound.
Background
In recent years, as the application range of lithium batteries is becoming wider, the lithium batteries are widely applied to energy storage power supply systems such as hydraulic power stations, firepower stations, wind power stations, solar power stations and the like, and various fields such as electric tools, electric bicycles, electric motorcycles, electric automobiles, military equipment, aerospace and the like.
The fluoroacetal compound is a common electrolyte solvent in a lithium battery, but the existing preparation method of the fluoroacetal compound has the problems of long reaction time and low production efficiency.
Disclosure of Invention
The preparation method of the fluoro-acetal compound can effectively improve the synthesis efficiency of the fluoro-acetal compound and is beneficial to industrial production.
The technical proposal is as follows:
a preparation method of a fluoro acetal compound comprises the following steps:
reacting an aldehyde polymer compound with a fluoroalcohol compound in the presence of a depolymerizing agent to prepare the fluoroacetal compound.
In one embodiment, the aldehyde polymer compound includes one or both of paraformaldehyde and polyacetaldehyde.
In one embodiment, the fluoroalcohol compound includes one or more of 2-fluoroethanol, 2-fluoroethanol, and 2, 2-fluoroethanol.
In one embodiment, the molar ratio of the aldehyde polymer compound to the fluoroalcohol compound is 1: (1.5-5).
In one embodiment, the temperature of the reaction is 50-80 ℃; optionally, the reaction temperature is 50-70 ℃.
In one embodiment, the reaction time is 1 to 24 hours; optionally, the reaction time is 4-24 hours; further alternatively, the reaction time is 5-20 hours.
In one embodiment, the depolymerizing agent comprises concentrated sulfuric acid.
In one embodiment, the depolymerization agent is added in an amount of 1 mL-4 mL per 1mol of the aldehyde polymer compound; optionally, the depolymerization agent is added in an amount of 1 mL-3 mL per 1mol of the aldehyde polymer compound.
In one embodiment, after the reaction is completed, a post-treatment step is further included, including one or both of extraction and rectification.
In one embodiment, the extraction comprises the steps of:
adding an organic solvent into the reaction solution after the reaction is finished, separating phases, and collecting an organic solvent phase;
washing and drying the organic solvent with saturated saline water;
optionally, the organic solvent includes one or both of dichloromethane and acetonitrile.
In one embodiment, the rectifying comprises the steps of:
and (3) treating the product obtained by extraction by adopting a rectifying tower, wherein the bottom temperature of the rectifying tower is controlled to be 75-130 ℃, the temperature of the rectifying tower section is 80-85 ℃, the temperature of the tower top is 45-90 ℃, and the reflux ratio is (1-20) (1-10).
In one embodiment, the rectifying comprises a first rectifying stage, a second rectifying stage, a third rectifying stage, a fourth rectifying stage, a fifth rectifying stage, and a sixth rectifying stage;
in the first rectifying stage, controlling the bottom temperature of the rectifying tower to be 75-80 ℃, the tower section temperature to be 80-85 ℃, the tower top temperature to be 45-50 ℃ and the reflux ratio to be 1 (8-10);
in the second rectifying stage, the bottom temperature of the rectifying tower is controlled to be 94-99 ℃, the tower section temperature is 80-85 ℃, the tower top temperature is 68-73 ℃, and the reflux ratio is 1 (4-6);
in the third rectifying stage, the bottom temperature of the rectifying tower is controlled to be 94-99 ℃, the tower section temperature is controlled to be 80-85 ℃, the tower top temperature is controlled to be 75-80 ℃, and the reflux ratio is 1 (1-3);
in the fourth rectifying stage, the bottom temperature of the rectifying tower is controlled to be 97-102 ℃, the tower section temperature is controlled to be 80-85 ℃, the tower top temperature is controlled to be 80-85 ℃, and the reflux ratio is (14-16): 1;
in the fifth rectifying stage, the bottom temperature of the rectifying tower is controlled to be 104-109 ℃, the tower section temperature is 80-85 ℃, the tower top temperature is 85-90 ℃, and the reflux ratio is (18-20): 1;
in the sixth rectifying stage, the bottom temperature of the rectifying tower is controlled to be 125-130 ℃, the tower section temperature is controlled to be 80-85 ℃, the tower top temperature is controlled to be 85-90 ℃, and the reflux ratio is (18-20): 1.
Effects of the invention
According to the preparation method of the fluoro-acetal compound, the aldehyde polymer compound and the fluoro-alcohol compound are used as raw materials, and the raw materials are reacted and prepared in the presence of the depolymerizing agent, so that the synthesis efficiency of the fluoro-acetal compound can be effectively improved, and the method is beneficial to industrial production.
Drawings
FIG. 1 is a hydrogen spectrum of bis-fluoroethoxymethane prepared according to an embodiment of the present application;
FIG. 2 is a graph of carbon spectrum of bis-fluoroethoxy methane prepared according to an embodiment of the present application;
FIG. 3 is a fluorine spectrum of difluoromethoxy-methane prepared according to an embodiment of the present application;
FIG. 4 is a mass spectrum of difluoromethoxy-methane prepared according to an embodiment of the present application;
FIG. 5 is a gas chromatogram of difluoromethoxy-methane prepared according to an embodiment of the present application.
Detailed Description
Hereinafter, embodiments of a method for producing a fluoroacetal compound of the present application are specifically disclosed with reference to the drawings. However, unnecessary detailed description may be omitted. For example, detailed descriptions of well-known matters and repeated descriptions of the actual same structure may be omitted. This is to avoid that the following description becomes unnecessarily lengthy, facilitating the understanding of those skilled in the art. Furthermore, the drawings and the following description are provided for a full understanding of the present application by those skilled in the art, and are not intended to limit the subject matter recited in the claims.
The "range" disclosed herein is defined in terms of lower and upper limits, with a given range being defined by the selection of a lower and an upper limit, the selected lower and upper limits defining the boundaries of the particular range. Ranges that are defined in this way can be inclusive or exclusive of the endpoints, and any combination can be made, i.e., any lower limit can be combined with any upper limit to form a range. For example, if ranges of 60-120 and 80-110 are listed for a particular parameter, it is understood that ranges of 60-110 and 80-120 are also contemplated. Furthermore, if the minimum range values 1 and 2 are listed, and if the maximum range values 3,4 and 5 are listed, the following ranges are all contemplated: 1-3, 1-4, 1-5, 2-3, 2-4 and 2-5. In this application, unless otherwise indicated, the numerical range "a-b" represents a shorthand representation of any combination of real numbers between a and b, where a and b are both real numbers. For example, the numerical range "0-5" means that all real numbers between "0-5" have been listed throughout, and "0-5" is simply a shorthand representation of a combination of these values. When a certain parameter is expressed as an integer of 2 or more, it is disclosed that the parameter is, for example, an integer of 2, 3,4, 5, 6, 7, 8, 9, 10, 11, 12 or the like.
All embodiments and alternative embodiments of the present application may be combined with each other to form new solutions, unless specifically stated otherwise.
All technical features and optional technical features of the present application may be combined with each other to form new technical solutions, unless specified otherwise.
All steps of the present application may be performed sequentially or randomly, preferably sequentially, unless otherwise indicated. For example, the method comprises steps (a) and (b), meaning that the method may comprise steps (a) and (b) performed sequentially, or may comprise steps (b) and (a) performed sequentially. For example, the method may further include step (c), which means that step (c) may be added to the method in any order, for example, the method may include steps (a), (b) and (c), may include steps (a), (c) and (b), may include steps (c), (a) and (b), and the like.
Reference herein to "comprising" and "including" means open ended, as well as closed ended, unless otherwise noted. For example, the terms "comprising" and "comprises" may mean that other components not listed may be included or included, or that only listed components may be included or included.
The term "or" is inclusive in this application, unless otherwise specified. For example, the phrase "a or B" means "a, B, or both a and B. More specifically, either of the following conditions satisfies the condition "a or B": a is true (or present) and B is false (or absent); a is false (or absent) and B is true (or present); or both A and B are true (or present).
An example of the present application provides a method for preparing a fluoroacetal compound, comprising the steps of:
reacting an aldehyde polymer compound with a fluoroalcohol compound in the presence of a depolymerizing agent to prepare the fluoroacetal compound.
The preparation method of the fluoro-acetal compound takes the aldehyde polymer compound and the fluoro-alcohol compound as raw materials, and the raw materials are reacted and prepared in the presence of the depolymerizing agent, so that the reaction time can be effectively shortened, the synthesis efficiency is improved, and the method is favorable for industrial production.
In some examples, the aldehyde polymer compound includes one or both of paraformaldehyde and polyacetaldehyde.
In some examples, the fluoroalcohol compound includes one or more of 2-fluoroethanol, 2-fluoroethanol, and 2, 2-fluoroethanol.
In some examples, the molar ratio of the aldehyde polymer compound to the fluoroalcohol compound is 1: (1.5-5). Specifically, the molar ratio of the aldehyde polymer compound to the fluoroalcohol compound includes, but is not limited to: 1:1.5, 1:2. 1:2.2, 1:2.5, 1:3. 1:3.5, 1:4. 1:4.5, 1:5.
the fluoroacetals prepared can be exemplified, without limitation, by: bis-fluoroethoxymethane, bis-difluoroethoxymethane, bis-trifluoroethoxymethane, and the like.
Without limitation, a desiccant may also be added during the reaction to timely remove moisture during the reaction. The drying agent may be exemplified by a molecular sieve.
In some examples, the temperature of the reaction is 50 ℃ to 80 ℃. The reaction temperature is reasonably controlled, and the reaction yield can be further improved. Specifically, the temperature of the reaction includes, but is not limited to: 50 ℃, 55 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃ or any two values thereof. Further, the reaction temperature is 50-70 ℃.
In some examples, the reaction time is 1h to 24h. The reaction time is reasonably controlled, and the reaction yield can be further improved. Specifically, the temperature of the reaction includes, but is not limited to: 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h, 10h, 11h, 12h, 13h, 14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h, 22h, 23h, 24h or a range formed by any two of the foregoing values. Further, the reaction time is 4-24 hours. Further, the reaction time is 5-20 hours.
In some examples, the depolymerizing agent comprises concentrated sulfuric acid.
In some examples, the depolymerization agent is added in an amount of 1 mL-4 mL per 1mol of the aldehyde polymer compound. The feeding amount of the depolymerizing agent is reasonably controlled, so that the yield of the reaction can be further improved. Specifically, the amount of the depolymerizing agent added per 1mol of the aldehyde-based polymer compound includes, but is not limited to: 1mL, 1.5mL, 2mL, 2.5mL, 3mL, 3.5mL, 4mL, or a range formed from any two of the foregoing values. Further, the feeding amount of the depolymerization agent is 1 mL-3 mL for every 1mol of the aldehyde polymer compound.
In addition, in some examples, after the reaction is complete, a post-treatment step is also included, including one or both of extraction and rectification.
In some examples, the extracting comprises the steps of:
adding dichloromethane into the reaction solution after the reaction is finished, separating phases, and collecting dichloromethane phases;
the dichloromethane phase was washed with saturated brine and dried.
The purity of the product can be effectively improved by washing with saturated saline.
In some examples, the rectifying includes the steps of:
and (3) treating the product obtained by extraction by adopting a rectifying tower, wherein the bottom temperature of the rectifying tower is controlled to be 75-130 ℃, the tower section temperature is 80-85 ℃, the tower top temperature is 45-90 ℃, and the reflux ratio is (1-20) (1-10). It is understood that the "reflux ratio" refers to the ratio of the time for extracting the rectification product and the time for continuously refluxing the material to the rectification tower for rectification in the rectification process, for example, the reflux ratio of 1:10 indicates that 1min is extracted for each rectification product, and the rest material is refluxed to the rectification tower for continuously rectifying for 10min, so that the cycle is adopted.
The rectification treatment is carried out under specific conditions, so that the purity of the product can be effectively improved under the condition of higher yield.
Further, the rectification includes a first rectification stage, a second rectification stage, a third rectification stage, a fourth rectification stage, a fifth rectification stage, and a sixth rectification stage.
In the first rectifying stage, the bottom temperature of the rectifying tower is controlled to be 75-80 ℃, the tower section temperature is 80-85 ℃, the tower top temperature is 45-50 ℃, and the reflux ratio is 1 (8-10).
Specifically, in the first rectification stage, the bottom temperature includes, but is not limited to: 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃, 80 ℃ or any two values thereof.
Specifically, in the first rectification stage, the column section temperatures include, but are not limited to: 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃ or any two values thereof.
Specifically, in the first rectification stage, the overhead temperature includes, but is not limited to: 45 ℃, 46 ℃, 47 ℃, 48 ℃, 49 ℃, 50 ℃ or any two values thereof.
Specifically, in the first rectification stage, reflux ratios include, but are not limited to: 1:8, 1:8.5, 1:9, 1:9.5, 1:10, or a range formed by any two of the foregoing values.
In the second rectifying stage, the bottom temperature of the rectifying tower is controlled to be 94-99 ℃, the tower section temperature is 80-85 ℃, the tower top temperature is 68-73 ℃, and the reflux ratio is 1 (4-6).
Specifically, in the second rectification stage, the bottom temperature includes, but is not limited to: 94 ℃, 95 ℃, 96 ℃, 97 ℃, 98 ℃, 99 ℃ or any two values of the above ranges.
Specifically, in the second rectification stage, the column section temperatures include, but are not limited to: 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃ or any two values thereof.
Specifically, in the second rectification stage, the overhead temperature includes, but is not limited to: 68 ℃, 69 ℃, 70 ℃, 71 ℃, 72 ℃, 73 ℃ or any two values thereof.
Specifically, in the second rectification stage, reflux ratios include, but are not limited to: 1:4, 1:4.5, 1:5, 1:5.5, 1:6, or a range formed by any two of the foregoing values.
In the third rectifying stage, the bottom temperature of the rectifying tower is controlled to be 94-99 ℃, the tower section temperature is 80-85 ℃, the tower top temperature is 75-80 ℃, and the reflux ratio is 1 (1-3).
Specifically, in the third rectification stage, the bottom temperature includes, but is not limited to: 94 ℃, 95 ℃, 96 ℃, 97 ℃, 98 ℃, 99 ℃ or any two values of the above ranges.
Specifically, in the third rectification stage, the column section temperatures include, but are not limited to: 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃ or any two values thereof.
Specifically, in the third rectification stage, the overhead temperature includes, but is not limited to: 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃, 80 ℃ or any two values thereof.
Specifically, in the third rectification stage, reflux ratios include, but are not limited to: 1:1, 1:1.5, 1:2, 1:2.5, 1:3, or a range formed by any two of the foregoing values.
In the fourth rectifying stage, the bottom temperature of the rectifying tower is controlled to be 97-102 ℃, the tower section temperature is 80-85 ℃, the tower top temperature is 80-85 ℃, and the reflux ratio is (14-16): 1.
Specifically, in the fourth rectification stage, the bottom temperature includes, but is not limited to: 97 ℃, 98 ℃, 99 ℃, 100 ℃, 101 ℃, 102 ℃ or any two values of the above ranges.
Specifically, in the fourth rectification stage, the column section temperatures include, but are not limited to: 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃ or any two values thereof.
Specifically, in the fourth rectification stage, the overhead temperature includes, but is not limited to: 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃ or any two values thereof.
Specifically, in the fourth rectification stage, reflux ratios include, but are not limited to: 14:1, 14.5:1, 15:1, 15.5:1, 16:1, or a range formed by any two of the foregoing values.
In the fifth rectifying stage, the bottom temperature of the rectifying tower is controlled to be 104-109 ℃, the tower section temperature is 80-85 ℃, the tower top temperature is 85-90 ℃, and the reflux ratio is (18-20): 1.
Specifically, in the fifth rectification stage, the bottom temperature includes, but is not limited to: 104 ℃, 105 ℃, 106 ℃, 107 ℃, 108 ℃, 109 ℃ or any two values thereof.
Specifically, in the fifth rectification stage, the column section temperatures include, but are not limited to: 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃ or any two values thereof.
Specifically, in the fifth rectification stage, the overhead temperature includes, but is not limited to: 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃, 90 ℃ or any two values thereof.
Specifically, in the fifth rectification stage, reflux ratios include, but are not limited to: 18:1, 18.5:1, 19:1, 19.5:1, 20:1, or a range formed by any two of the foregoing values.
In the sixth rectifying stage, the bottom temperature of the rectifying tower is controlled to be 125-130 ℃, the tower section temperature is 80-85 ℃, the tower top temperature is 85-90 ℃, and the reflux ratio is (18-20): 1.
Specifically, in the sixth rectification stage, the bottom temperature includes, but is not limited to: 125 ℃, 126 ℃, 127 ℃, 128 ℃, 129 ℃, 130 ℃ or any two values thereof.
Specifically, in the sixth rectification stage, the column section temperatures include, but are not limited to: 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃ or any two values thereof.
Specifically, in the sixth rectification stage, the overhead temperature includes, but is not limited to: 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃, 90 ℃ or any two values thereof.
Specifically, in the sixth rectification stage, reflux ratios include, but are not limited to: 18:1, 18.5:1, 19:1, 19.5:1, 20:1, or a range formed by any two of the foregoing values.
Hereinafter, embodiments of the present application are described. The embodiments described below are exemplary only for the purpose of illustrating the present application and are not to be construed as limiting the present application. The examples are not to be construed as limiting the specific techniques or conditions described in the literature in this field or as per the specifications of the product. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The embodiment is a preparation method of a fluoro acetal compound (bis-fluoroethoxymethane), which comprises the following steps:
(1) 30g (1 mol) of paraformaldehyde, 141g (2.2 mol) of 2-fluoroethanol and 4A molecular sieve are put into a three-necked flask, 2mL of concentrated sulfuric acid is added dropwise at normal temperature by mechanical stirring, and the temperature is raised to 60 ℃ for reaction for 6 hours after the addition is completed.
(2) Extracting the reaction solution after the reaction in the step (1) with dichloromethane, and collecting a dichloromethane layer; the dichloromethane layer was washed with saturated brine, separated by a pear-shaped separating funnel, and the lower layer solution was dried over anhydrous sodium sulfate.
(3) Transferring the solution dried in the step (2) into a rectifying bottle, and performing nitrogen protection by using high-purity nitrogen; after the whole rectifying tower is built, the reflux temperature of a condensing pipe is set at-20 ℃ by using an ice maker, the pressure of a system is controlled between-0.095 MPa and-0.1 MPa by using a water pump, and then the process of stage rectification is carried out, wherein the process is as follows:
in the first rectifying stage, the bottom temperature of the rectifying tower is controlled to be 78.3 ℃, the tower section temperature is 80 ℃, the tower top temperature is 46.7 ℃, and the reflux ratio is 1:10; the purity of the collected matter at the stage is 65.3 percent;
in the second rectifying stage, the bottom temperature of the rectifying tower is controlled to be 96.0 ℃, the tower section temperature is 83.2 ℃, the tower top temperature is 71.0 ℃, and the reflux ratio is 1:5, rectifying for 1h; the purity of the collected matter at the stage is 99.93 percent;
in the third rectifying stage, the bottom temperature of the rectifying tower is controlled to be 96.0 ℃, the tower section temperature is 82.6 ℃, the tower top temperature is 78.6 ℃, and the reflux ratio is 1:1, rectifying for 1h; the purity of the collected matter at the stage is 99.63%;
in the fourth rectifying stage, the bottom temperature of the rectifying tower is controlled to be 99.0 ℃, the tower section temperature is 82.6 ℃, the tower top temperature is 83 ℃, and the reflux ratio is 15:1, rectifying for 1h; the purity of the collected matter at the stage is 99.38%;
in the fifth rectifying stage, the bottom temperature of the rectifying tower is controlled to be 106 ℃, the tower section temperature is 83.0 ℃, the tower top temperature is 86 ℃, and the reflux ratio is 20:1, rectifying for 1h; the purity of the collected matter at the stage is 99.69%;
in the sixth rectifying stage, the bottom temperature of the rectifying tower is controlled to be 128 ℃, the tower section temperature is 83 ℃, the tower top temperature is 86.6 ℃, and the reflux ratio is 20:1, rectifying for 1h; the purity of the collection at this stage was 99.97%.
After the rectification is finished, the yield of the obtained product difluoromethoxy-methane is 78%, and fractions from the second rectification stage to the sixth rectification stage are collected uniformly, so that the purity is 99.96%.
The structure of the product bis fluoroethoxymethane is shown as follows:
the hydrogen spectrum is shown in FIG. 1, the carbon spectrum is shown in FIG. 2, the fluorine spectrum is shown in FIG. 3, the mass spectrum is shown in FIG. 4, and the gas chromatography is shown in FIG. 5.
Examples 2 to 18 are identical to example 1, with the main difference that part of the reaction parameters are changed, as shown in Table 1 below.
The procedure of examples 19 to 20 was the same as that of example 1, except that the raw materials used were different, and the fluoroacetal compound products having different structures were prepared, as shown in Table 1 below.
TABLE 1
Therefore, the preparation of the fluoroacetal compound product can be completed within 1-24 hours in the embodiment of the application, and the preparation of the fluoroacetal compound can be completed in 4-7 days in the traditional method, such as the preparation of mannitol and heptafluorobutyraldehyde obtained by sulfuric acid treatment.
Further, by reasonably controlling one or more of the parameters of reaction time, reaction temperature, dosage of concentrated sulfuric acid and the like, the yield and/or purity of the product can be optimized.
The present application is not limited to the above embodiment. The above embodiments are merely examples, and embodiments having substantially the same configuration and the same effects as those of the technical idea within the scope of the present application are included in the technical scope of the present application. Further, various modifications that can be made to the embodiments and other modes of combining some of the constituent elements in the embodiments, which are conceivable to those skilled in the art, are also included in the scope of the present application within the scope not departing from the gist of the present application.
Claims (17)
1. The preparation method of the fluoro-acetal compound is characterized by comprising the following steps:
reacting an aldehyde polymer compound with a fluoroalcohol compound in the presence of a depolymerizing agent to prepare the fluoroacetal compound.
2. The method for producing a fluoroacetal compound according to claim 1, wherein said aldehyde polymer compound comprises one or both of paraformaldehyde and polyacetaldehyde.
3. The method for producing a fluoroacetal compound according to claim 1, wherein the fluoroalcohol compound comprises one or more of 2-fluoroethanol, 2-fluoroethanol and 2, 2-fluoroethanol.
4. The method for producing a fluoroacetal compound according to claim 1, wherein the molar ratio of the aldehyde polymer compound to the fluoroalcohol compound is 1: (1.5-5).
5. The method for producing a fluoroacetal compound according to claim 1, wherein the reaction temperature is 50 to 80 ℃.
6. The method for producing a fluoroacetal compound according to claim 5, wherein the reaction temperature is 50℃to 70 ℃.
7. The method for producing a fluoroacetal compound according to claim 1, wherein the reaction time is 1 to 24 hours.
8. The method for producing a fluoroacetal compound according to claim 7, characterized in that the reaction time is 4 to 24 hours.
9. The method for producing a fluoroacetal compound according to claim 8, wherein the reaction time is 5 to 20 hours.
10. The method for producing a fluoroacetal compound according to claim 1, wherein the depolymerizing agent comprises concentrated sulfuric acid.
11. The method for producing a fluoroacetal compound according to claim 1, wherein the depolymerizing agent is added in an amount of 1ml to 4ml per 1mol of the aldehyde polymer compound.
12. The method for producing a fluoroacetal compound according to claim 1, wherein the depolymerizing agent is added in an amount of 1ml to 3ml per 1mol of the aldehyde polymer compound.
13. The method for producing a fluoroacetal compound according to any one of claims 1 to 12, characterized by further comprising a post-treatment step after the completion of the reaction, the post-treatment step comprising one or both of extraction and rectification.
14. The method for producing a fluoroacetal compound according to claim 13, characterized in that the extraction comprises the steps of:
adding an organic solvent into the reaction solution after the reaction is finished, separating phases, and collecting an organic solvent phase;
the organic solvent was washed with saturated brine and dried.
15. The method for producing a fluoroacetal compound according to claim 14, characterized in that the organic solvent comprises one or both of dichloromethane and acetonitrile.
16. The method for producing a fluoroacetal compound according to claim 13, characterized in that said rectification comprises the steps of:
and (3) treating the product obtained by extraction by adopting a rectifying tower, wherein the bottom temperature of the rectifying tower is controlled to be 75-130 ℃, the temperature of the rectifying tower section is 80-85 ℃, the temperature of the tower top is 45-90 ℃, and the reflux ratio is (1-20) (1-10).
17. The method for producing a fluoroacetal compound according to claim 16, wherein said rectification comprises a first rectification stage, a second rectification stage, a third rectification stage, a fourth rectification stage, a fifth rectification stage, and a sixth rectification stage;
in the first rectifying stage, controlling the bottom temperature of the rectifying tower to be 75-80 ℃, the tower section temperature to be 80-85 ℃, the tower top temperature to be 45-50 ℃ and the reflux ratio to be 1 (8-10);
in the second rectifying stage, the bottom temperature of the rectifying tower is controlled to be 94-99 ℃, the tower section temperature is 80-85 ℃, the tower top temperature is 68-73 ℃, and the reflux ratio is 1 (4-6);
in the third rectifying stage, the bottom temperature of the rectifying tower is controlled to be 94-99 ℃, the tower section temperature is controlled to be 80-85 ℃, the tower top temperature is controlled to be 75-80 ℃, and the reflux ratio is 1 (1-3);
in the fourth rectifying stage, the bottom temperature of the rectifying tower is controlled to be 97-102 ℃, the tower section temperature is controlled to be 80-85 ℃, the tower top temperature is controlled to be 80-85 ℃, and the reflux ratio is (14-16): 1;
in the fifth rectifying stage, the bottom temperature of the rectifying tower is controlled to be 104-109 ℃, the tower section temperature is 80-85 ℃, the tower top temperature is 85-90 ℃, and the reflux ratio is (18-20): 1;
in the sixth rectifying stage, the bottom temperature of the rectifying tower is controlled to be 125-130 ℃, the tower section temperature is controlled to be 80-85 ℃, the tower top temperature is controlled to be 85-90 ℃, and the reflux ratio is (18-20): 1.
Priority Applications (1)
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