Synthesis device of bis (trifluoromethyl) disulfide
By designing a synthesis device including a reactor, a distillation column and an insulation filter, the problem that the existing device cannot flexibly switch the reaction mode and the solubility of the material changes was solved, and the synthesis of bis(trifluoromethyl) disulfide with high yield and high purity was achieved.
Patent Information
- Application Number
- CN202422540333.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-21
- Publication Date
- 2025-09-19
- Estimated Expiration
- 2034-10-21
AI Technical Summary
Existing synthesis equipment cannot flexibly switch between continuous or intermittent reactions. The solubility of the material changes with temperature, resulting in low product yield. Additional separation equipment is required to improve purity, increasing production costs.
A synthesis device including a reactor, a distillation column, a condenser, and a heat-insulating filter was designed. The reaction was heated by a jacket and solids were removed by a heat-insulating filter to achieve continuous or intermittent reaction switching, and the product purity was improved by reactive distillation.
It enables flexible switching of reaction modes according to order conditions, solves the problem of material solubility changes, improves product yield and purity, and reduces the need for additional separation equipment.
Smart Images
Figure CN223351687U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of synthesis devices, in particular to a synthesis device for bis(trifluoromethyl)disulfide. Background Art
[0002] Bis(trifluoromethyl) disulfide is an important chemical intermediate with wide applications in medicine, pesticides, materials, etc.
[0003] A method for synthesizing bis(trifluoromethyl)disulfide salt is mentioned in the prior art. However, the method does not describe the preparation method of bis(trifluoromethyl)disulfide, but only uses bis(trifluoromethyl)disulfide as a raw material to synthesize its salt.
[0004] As the existing devices are used, the shortcomings of this technology are gradually exposed, mainly in the following aspects:
[0005] First, existing synthesis equipment can only perform continuous synthesis reactions or intermittent synthesis reactions, and cannot be flexibly switched according to order conditions.
[0006] Second, the solubility of existing materials in solvents changes with temperature, resulting in a low product yield; and in order to improve the purity of the product, other separation devices are required, which increases production costs.
[0007] As can be seen from the above, the existing technology obviously has inconveniences and defects in actual use, so it is necessary to improve it. Utility Model Content
[0008] In response to the defects in the existing technology, the utility model provides a synthesis device for bis(trifluoromethyl) disulfide, which is used to solve the problems that the devices in traditional technologies either have to perform continuous synthesis reactions or can only perform intermittent synthesis reactions, and cannot be flexibly switched according to order conditions; the solubility of existing materials in solvents changes with temperature, resulting in a low product yield; and in order to improve the purity of the product, other separation devices are required, which increases production costs.
[0009] In order to achieve the above-mentioned purpose, the present utility model provides the following technical solutions.
[0010] The synthesis device of bis(trifluoromethyl)disulfide comprises a reactor, the top of which is connected to a distillation column, the distillation column is connected to a condenser, and the outlet end of the condenser is connected in parallel to a product extraction pipeline and a reflux pipeline.
[0011] The reactor is provided with a discharge port connected to two heat-insulating filters through a discharge pipeline. The discharge ports of the two heat-insulating filters are commonly connected to a filtrate storage tank, and the filtrate storage tank is connected to a return liquid pipeline connected to the reactor.
[0012] As an optimized solution, the outer wall of the reactor and the outer wall of the thermal insulation filter are both provided with thermal insulation jackets.
[0013] As an optimized solution, the reflux line is connected to the top of the distillation column.
[0014] As an optimized solution, a nitrogen pressurized inlet is provided on the top of the thermal insulation filter.
[0015] As an optimized solution, a washing liquid inlet is further provided on the top of the heat-insulating filter.
[0016] As an optimized solution, a supporting mesh plate is fixedly connected to the thermal insulation filter, and a filter cloth is provided on the upper surface of the supporting mesh plate.
[0017] As an optimized solution, the top of the thermal insulation filter is provided with an inlet connected to the discharge pipeline, and the discharge port of the thermal insulation filter is provided at the bottom of the thermal insulation filter.
[0018] As an optimized solution, a first mud pump is provided on the discharge pipeline.
[0019] As an optimized solution, a second mud pump is provided on the liquid return pipeline.
[0020] As an optimized solution, a feed port is provided on the top of the reactor.
[0021] Compared with the prior art, the beneficial effects of the present invention are:
[0022] First, a solvent is added to the reactor through the feed port, and then the reaction raw materials are added again. The reactor is heated by a jacket to allow the reaction to proceed. The resulting product, bis(trifluoromethyl) disulfide, has a low boiling point and is passed through a distillation column into a condenser. The condenser condenses the product into a liquid, a portion of which is refluxed to the distillation column, and the remaining portion is extracted as the product. The material in the reactor is transferred to an insulated filter, where solids are removed by insulated filtration, and the liquid is returned to the reactor to continue the reaction.
[0023] By switching the discharge pipeline on and off, it can be continuous or intermittent, and can be switched flexibly according to the order situation;
[0024] This patent adopts a heat-insulating filtration device to solve the problem that the solubility of the material in the solvent changes with temperature, and the product yield is high. In addition, through reactive distillation, the collected product has high purity and does not require other separation devices. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the following briefly describes the drawings required for the specific embodiments or the description of the prior art. Similar elements or parts are generally identified by similar reference numerals throughout the drawings. Elements or parts in the drawings are not necessarily drawn to scale.
[0026] Figure 1 It is a structural diagram of the utility model;
[0027] Figure 2 This is a schematic structural diagram of the thermal insulation filter of the utility model.
[0028] In the figure: 1-reactor; 2-insulation jacket; 3-distillation column; 4-condenser; 5-reflux pipeline; 6-product production pipeline; 7-feed port; 8-discharge pipeline; 9-insulation filter; 10-filtrate storage tank; 11-return liquid pipeline; 12-first mud pump; 13-second mud pump; 14-filter cloth; 15-support mesh plate; 16-nitrogen pressurization inlet; 17-washing liquid inlet; 18-inlet; 19-drain port. DETAILED DESCRIPTION
[0029] The following embodiments of the technical solution of the present invention are described in detail with reference to the accompanying drawings. The following embodiments are only used to more clearly illustrate the technical solution of the present invention and are therefore only examples and are not intended to limit the scope of protection of the present invention.
[0030] like Figure 1 and Figure 2 As shown, the synthesis device of bis(trifluoromethyl)disulfide includes a reactor 1, a distillation column 3 is connected to the top of the reactor 1, a condenser 4 is connected to the distillation column 3, and a product extraction pipeline 6 and a reflux pipeline 5 are connected in parallel at the outlet end of the condenser 4.
[0031] The reactor 1 is provided with a discharge port connected to two heat-insulating filters 9 through a discharge pipeline 8. The discharge ports 19 of the two heat-insulating filters 9 are commonly connected to a filtrate storage tank 10. The filtrate storage tank is connected to a return liquid pipeline 11 connected to the reactor 1.
[0032] The outer wall of the reactor 1 and the outer wall of the heat-insulating filter 9 are both provided with a heat-insulating jacket 2 .
[0033] The reflux line 5 is connected to the top of the distillation column 3 .
[0034] A nitrogen pressurization inlet 16 is provided at the top of the heat-insulating filter 9 .
[0035] A washing liquid inlet 17 is also provided on the top of the heat-insulating filter 9 .
[0036] A supporting mesh plate 15 is fixedly connected to the heat-insulating filter 9 , and a filter cloth 14 is provided on the upper surface of the supporting mesh plate 15 .
[0037] The top of the heat-insulating filter 9 is provided with an inlet 18 connected to the discharge pipeline 8 , and the discharge port 19 of the heat-insulating filter 9 is provided at the bottom of the heat-insulating filter 9 .
[0038] The discharge pipeline 8 is provided with a first mud pump 12 .
[0039] A second mud pump 13 is provided on the liquid return pipeline 11 .
[0040] A feed port 7 is provided on the top of the reactor 1 .
[0041] A stirring structure is provided in the reactor 1 .
[0042] The working principle of this device is:
[0043] First, a solvent is added to the reactor 1 through the feed port 7, and then the reaction raw materials are added again. The reactor 1 is heated by the jacket to allow the reaction to proceed. The product bis(trifluoromethyl) disulfide, due to its low boiling point, passes through the distillation column 3 and enters the condenser 4. The condenser 4 condenses the product into a liquid, a portion of which is refluxed to the distillation column 3, and the other portion is extracted as the product. The material in the reactor is transferred to the heat-insulating filter 9, where the solids are removed by heat-insulating filtration, and the liquid is returned to the reactor 1 to continue the reaction.
[0044] The discharge line 8 can be switched on and off continuously or intermittently, and can be switched flexibly according to the order situation;
[0045] This patent adopts a heat-insulating filtration device to solve the problem that the solubility of the material in the solvent changes with temperature, and the product yield is high. In addition, through reactive distillation, the collected product has high purity and does not require other separation devices.
[0046] The reaction process is:
[0047] Under the action of the solvent, the two reaction raw materials react to produce bis(trifluoromethyl) disulfide and triethylamine hydrochloride; the product bis(trifluoromethyl) disulfide is distilled, which has the advantage of being produced and withdrawn at the same time, reducing the occurrence of cascade side reactions and improving the product yield.
[0048] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the above embodiments, or make equivalent replacements for some or all of the technical features therein. These modifications or replacements do not deviate the essence of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present invention, and they should all be included in the scope of the claims and description of the present invention.
Claims
1. A synthesis device for bis(trifluoromethyl)disulfide, characterized in that: The invention comprises a reactor (1), wherein the top of the reactor (1) is connected to a distillation column (3), the distillation column (3) is connected to a condenser (4), and the outlet end of the condenser (4) is connected in parallel to a product extraction pipeline (6) and a reflux pipeline (5). The reactor (1) is provided with a discharge port connected to two heat-insulating filters (9) through a discharge pipeline (8); the discharge ports (19) of the two heat-insulating filters (9) are connected to a filtrate storage tank (10); and the filtrate storage tank is connected to a return liquid pipeline (11) connected to the reactor (1).
2. The synthesis device of bis(trifluoromethyl)disulfide according to claim 1, characterized in that: The outer wall of the reaction kettle (1) and the outer wall of the heat-insulating filter (9) are both provided with a heat-insulating jacket (2).
3. The synthesis device of bis(trifluoromethyl)disulfide according to claim 1, characterized in that: The reflux line (5) is connected to the top of the distillation column (3).
4. The synthesis device of bis(trifluoromethyl)disulfide according to claim 1, characterized in that: A nitrogen pressurizing inlet (16) is provided on the top of the heat-insulating filter (9).
5. The synthesis device of bis(trifluoromethyl)disulfide according to claim 1, characterized in that: The top of the heat-insulating filter (9) is also provided with a washing liquid inlet (17).
6. The synthesis device of bis(trifluoromethyl)disulfide according to claim 1, characterized in that: A supporting mesh plate (15) is fixedly connected to the heat-insulating filter (9), and a filter cloth (14) is provided on the upper surface of the supporting mesh plate (15).
7. The synthesis device of bis(trifluoromethyl)disulfide according to claim 1, characterized in that: The top of the heat-insulating filter (9) is provided with an inlet (18) connected to the discharge pipeline (8), and the discharge port (19) of the heat-insulating filter (9) is provided at the bottom of the heat-insulating filter (9).
8. The synthesis device of bis(trifluoromethyl)disulfide according to claim 1, characterized in that: The discharge pipeline (8) is provided with a first mud pump (12).
9. The synthesis device of bis(trifluoromethyl)disulfide according to claim 1, characterized in that: A second mud pump (13) is provided on the liquid return pipeline (11).
10. The synthesis device of bis(trifluoromethyl)disulfide according to claim 1, characterized in that: The top of the reactor (1) is provided with a feed port (7).