Equipment for producing trifluoroethyl acetate

Abstract

The utility model relates to the technical field of fluorine chemical industry, in particular to equipment for producing trifluoroethyl acetate, which comprises a reactor, the upper part of the reactor is connected with a dropping pipe, the bottom of the reactor is connected with a coarse distillation tower through a first discharge pipe, and the bottom end of the coarse distillation tower is connected with a rectifying tower through a second discharge pipe. The top end of the coarse distillation tower is connected with a neutralizing tower through a gas outlet pipe, and the reactor is a glass-lined stirring reaction kettle. According to the utility model, the problems of low purity of trifluoroethyl acetate, difficulty in meeting the use requirements of lithium batteries and the like in the prior art are solved, the yield is increased, and the market competitiveness of companies is improved; the process is simple, operation is convenient, and equipment requirements are low; the reaction control is safer.

Description

Technical Field

[0001] The utility model relates to the technical field of fluorine chemical industry, in particular to equipment for producing trifluoroethyl acetate. Background Art

[0002] 2,2,2-trifluoroethyl acetate (TFEA), also known as trifluoroethyl acetate, CAS No. 406-95-1, molecular formula C 4 H 5 F 3 O 2 , molecular weight 142, density 1.258 g / cm 3 , boiling point 78 ℃, flash point 11 ℃, refractive index 1.32. 2,2,2-Trifluoroethyl acetate is widely used in the field of fluorine chemical industry, mainly in batteries, biomedicine and fluoride.

[0003] However, trifluoroethyl acetate produced by the prior art cannot effectively control the acidity and moisture in the reactor and cannot meet the electronic grade requirements, and therefore cannot be used as a solvent for lithium battery electrolyte. Summary of the invention

[0004] The technical problem to be solved by the utility model is to provide a device for producing trifluoroethyl acetate to solve the above problem.

[0005] The utility model solves the above technical problem through a technical solution: a device for producing trifluoroethyl acetate, comprising a reactor, wherein the upper part of the reactor is connected with a dripping pipe, the bottom of the reactor is connected with a crude distillation tower through a first discharge pipe, the bottom end of the crude distillation tower is connected with a rectifying tower through a second discharge pipe, and the top end of the crude distillation tower is connected with a neutralization tower through an air outlet pipe.

[0006] As a preferred technical solution of the utility model, the reactor is a glass-lined stirred reactor.

[0007] As a preferred technical solution of the utility model, the reaction pressure in the glass-lined stirred reactor is maintained at 0.25-0.5 MPa, and the reaction temperature is 80-130°C.

[0008] As a preferred technical solution of the utility model, the neutralization tower is filled with an alkaline solution.

[0009] As a preferred technical solution of the utility model, the neutralization tower is filled with a saturated calcium hydroxide solution.

[0010] As a preferred technical solution of the utility model, the reaction temperature of the neutralization tower is 120-150°C.

[0011] Since the utility model adopts such a structure, the problems of low purity of trifluoroethyl acetate in the existing process and difficulty in meeting the requirements for use in lithium batteries are solved, the output is increased and the company's market competitiveness is improved; the process is simple, the operation is easy, the equipment requirements are low; and the reaction control is safer. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Figure 1 The utility model is a structural schematic diagram of a device for producing trifluoroethyl acetate.

[0013] In the figure: 1 is a reactor, 2 is a first discharge pipe, 3 is a crude distillation tower, 4 is a second discharge pipe, 5 is a rectifying tower, 6 is an outlet pipe, and 7 is a neutralization tower. DETAILED DESCRIPTION

[0014] The utility model is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0015] like Figure 1 As shown, the utility model is a device for producing trifluoroethyl acetate, characterized in that it comprises a reactor 1, the upper part of the reactor 1 is connected with a dripping pipe, the bottom of the reactor 1 is connected with a crude distillation tower 3 through a first discharge pipe 2, the bottom end of the crude distillation tower 3 is connected with a rectifying tower 5 through a second discharge pipe 4, and the top of the crude distillation tower 3 is connected with a neutralization tower 7 through an outlet pipe 6. During production, 2,2,2-trifluoroethanol is added to a glass-lined stirred reactor, acetyl chloride is added dropwise under stirring, and a small amount of reflux reaction is maintained. After the addition is completed, the temperature is raised and the reaction is stirred for 1 hour with full reflux, and the hydrogen chloride gas in the reaction material is removed by reflux through the crude distillation tower, and the crude trifluoroethyl acetate is obtained by rectification, and then the finished product trifluoroethyl acetate is obtained by rectification through the finished product rectification tower.

[0016] In the utility model, the reactor is a glass-lined stirred reactor, the reaction pressure in the glass-lined stirred reactor is maintained at 0.25-0.5 MPa, and the reaction temperature is 80-130° C. The glass-lined stirred reactor has the characteristics of good resistance to solvent corrosion, wear resistance, and aging resistance.

[0017] In the utility model, the neutralization tower 7 is filled with an alkaline solution, and the chlorine in the crude distillation tower 3 is neutralized by the alkaline solution to avoid environmental pollution.

[0018] In the utility model, the neutralization tower 7 is filled with a saturated calcium hydroxide solution, and the reaction temperature of the neutralization tower 7 is 120-150° C. The saturated calcium hydroxide solution can be neutralized with chlorine to form a calcium chloride solution, thereby avoiding environmental pollution.

[0019] The production process of the utility model is:

[0020] CF 3 CH 2OH + CH 3 COCl → CF 3 CH 2 -O-OCCH 3 + HCl

[0021] Ca(OH) 2 + 2HCl → CaCl 2 + 2H 2 O

[0022] Add 2,2,2-trifluoroethanol to a glass-lined stirred reactor, add acetyl chloride dropwise while stirring, keep a small amount of reflux reaction, after the addition is completed, heat up and stir for 1 hour with full reflux, remove hydrogen chloride gas in the reaction material through reflux in a crude distillation tower, distill to obtain crude trifluoroethyl acetate, and then distill through a finished product distillation tower to obtain finished trifluoroethyl acetate. The finished trifluoroethyl acetate has a content greater than 99.99%, an acidity less than 10PPm, a moisture content less than 100PPm, and a yield greater than 98%, which is an electronic grade high-purity product; during the reaction, hydrogen chloride gas is neutralized with a saturated calcium hydroxide solution to form a calcium chloride aqueous solution; the utility model has the characteristics of simple process, easy operation, low equipment requirements, and safer reaction control.

[0023] The description and application of the utility model here are illustrative and are not intended to limit the scope of the utility model to the above-described embodiments. Variations and changes of the embodiments disclosed here are possible, and the actual replacement of the embodiments and the various components equivalent to those of ordinary skill in the art are well known. It should be clear to those skilled in the art that the utility model can be implemented in other forms, structures, arrangements, proportions, and with other elements, materials, and components without departing from the spirit or essential features of the utility model. Other variations and changes can be made to the embodiments disclosed here without departing from the spirit or essential features of the utility model.

Claims

1. A device for producing trifluoroethyl acetate, characterized in that: The invention comprises a reactor (1), wherein the upper part of the reactor (1) is connected to a dripping pipe, the bottom of the reactor (1) is connected to a crude distillation tower (3) via a first discharge pipe (2), the bottom end of the crude distillation tower (3) is connected to a rectification tower (5) via a second discharge pipe (4), and the top end of the crude distillation tower (3) is connected to a neutralization tower (7) via an outlet pipe (6).

2. A method for producing trifluoroethyl acetate according to claim 1, characterized in that: The reactor is a glass-lined stirred reactor.

3. A kind of equipment for producing trifluoroethyl acetate according to claim 2, characterized in that: The reaction pressure in the glass-lined stirred reactor is maintained at 0.25-0.5 MPa, and the reaction temperature is 80-130°C.

4. A method for producing trifluoroethyl acetate according to claim 1, characterized in that: The neutralization tower (7) is filled with an alkaline solution.

5. A device for producing trifluoroethyl acetate according to claim 4, characterized in that: The neutralization tower (7) is filled with a saturated calcium hydroxide solution.

6. A device for producing trifluoroethyl acetate according to claim 5, characterized in that: The reaction temperature of the neutralization tower (7) is 120-150°C.

Images