CN117772062A - Sulfur dichloride synthesizing system and method - Google Patents
Sulfur dichloride synthesizing system and method Download PDFInfo
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- CN117772062A CN117772062A CN202311778797.3A CN202311778797A CN117772062A CN 117772062 A CN117772062 A CN 117772062A CN 202311778797 A CN202311778797 A CN 202311778797A CN 117772062 A CN117772062 A CN 117772062A
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- FWMUJAIKEJWSSY-UHFFFAOYSA-N sulfur dichloride Chemical compound ClSCl FWMUJAIKEJWSSY-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 17
- PXJJSXABGXMUSU-UHFFFAOYSA-N disulfur dichloride Chemical compound ClSSCl PXJJSXABGXMUSU-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 27
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000007791 liquid phase Substances 0.000 claims abstract description 10
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 24
- 239000000460 chlorine Substances 0.000 claims description 24
- 229910052801 chlorine Inorganic materials 0.000 claims description 22
- 230000003068 static effect Effects 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000012071 phase Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- NHYCGSASNAIGLD-UHFFFAOYSA-N chlorine monoxide Inorganic materials Cl[O] NHYCGSASNAIGLD-UHFFFAOYSA-N 0.000 claims description 2
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Abstract
The invention discloses a sulfur dichloride synthesizing system, which comprises a synthesizing device, a separating device and a circulating device; the synthesis device comprises a raw material mixing module and a reaction module, wherein the reaction module comprises an inner pipe and an outer pipe, and the raw material mixing module is connected to one end of the inner pipe; the other end of the inner tube is connected with the separation device through a connecting tube, the separation device is connected with the circulation device through a liquid phase tube, and the circulation device is connected with the synthesis device through a circulating sulfur monochloride conveying tube. The sulfur dichloride content prepared by the method is higher than 90%, and the highest content is 93.7%.
Description
Technical Field
The invention relates to the technical field of sulfur dichloride production, in particular to a sulfur dichloride synthesis system and method.
Background
The thionyl chloride is an important inorganic fine chemical product and has wide application in industries such as medicine, pesticide, dye, chemical industry and the like and organic synthesis reaction, and the sulfur dichloride is an important intermediate for synthesizing the thionyl chloride.
The production method of sulfur dichloride mainly comprises the steps of carrying out chlorination reaction on sulfur monochloride and chlorine at a certain temperature to generate sulfur dichloride, wherein the reaction equation is as follows:
S 2 CL 2 +CL 2 ＝2SCL 2
the method for synthesizing sulfur dichloride in industry adopts a bubbling reaction kettle, the temperature is controlled at 70-90 ℃, the pressure is controlled at 0.15-0.2MPag, and a large amount of chlorine is introduced into sulfur monochloride liquid to generate sulfur dichloride gas.
The inventors have found that this method has the following disadvantages: firstly, due to the characteristic of material distribution of a kettle-type reactor, during amplification, chlorine input by a distributor is unevenly distributed, backmixing is serious, and the conversion rate of sulfur monochloride is affected.
Secondly, the ratio of the inner volume of the kettle to the outer surface area of the kettle is smaller, and the heat exchange area is smaller during mass production, so that the evaporation of sulfur dichloride is not facilitated, the forward reaction is not facilitated from the aspect of reaction balance, and the productivity of sulfur dichloride is influenced.
And thirdly, the reaction temperature is higher when the sulfur dichloride is synthesized, high-grade heat sources such as steam are needed to be used for heating, a large amount of low-grade heat sources are not used in the production process of the thionyl chloride, and if the sulfur dichloride can be produced by utilizing the low-grade heat sources, the method plays an important role in energy conservation and consumption reduction in the production of the thionyl chloride.
Disclosure of Invention
In order to solve the above problems, the present invention provides a sulfur dichloride synthesis system, comprising: a synthesizing device, a separating device and a circulating device;
the synthesis device comprises a raw material mixing module and a reaction module, wherein the reaction module comprises an inner pipe and an outer pipe, and the raw material mixing module is connected to one end of the inner pipe;
the other end of the inner tube is connected with the separating device through a connecting tube, the separating device is connected with the circulating device through a liquid phase tube, and the circulating device is connected with the synthesizing device through a circulating sulfur chloride conveying tube.
Further, the raw material mixing module is a static mixer.
Further, the inner tube and the outer tube are disposed horizontally, and the cross section perpendicular to the plane of the tube is concentric circular.
Further, the separation device is a gas-liquid separation tank, the tank top is connected with a liquid phase pipe, and the tank bottom is connected with a gas phase pipe.
Further, the circulating device is a circulating pump and is connected with a circulating sulfur monochloride conveying pipe and a sulfur monochloride output pipe.
Further, a flow regulating mechanism is arranged in front of and behind the synthesizing device.
Further, a temperature and pressure monitoring mechanism is arranged in the synthesis device.
A method for synthesizing sulfur dichloride, comprising the following steps:
s1: inputting chlorine and sulfur monochloride into a synthesis device from one end of an inner pipe connected with a static mixer, inputting a heat source into the synthesis device from one end of an outer pipe far away from an inlet of the chlorine and the sulfur monochloride, and heating the chlorine and the sulfur monochloride for synthesis reaction;
s2: and the synthesis reaction product enters a gas-liquid separation tank from the other end of the inner pipe for separation to obtain a gas phase composed of chlorine and sulfur dichloride and a sulfur monochloride liquid phase.
S3: the sulfur monochloride is returned to the synthesis unit via a recycling unit.
In the step S1, chlorine and sulfur monoxide enter the synthesis device and are fully mixed through the raw material mixing module, and then the synthesis reaction is completed in the reaction module.
Further, in the step S1, the heat source in the outer tube is hot water at 70-90 ℃.
Further, in S1, the horizontal flow direction of sulfur monochloride and chlorine gas in the inner pipe is opposite to the horizontal flow direction of hot water in the outer pipe.
Further, in the step S1, the opposite flow direction means that the flow direction of the inner tube and the outer tube material in each heat exchange area is opposite, but the flow direction of the inner tube and the outer tube material in the whole heat exchanger is opposite, namely: sulfur chloride, chlorine and a heat source enter the heat exchanger from different ends of the same section of heat exchange area, enter from different ends of the next section of heat exchange area, and leave the heat exchanger from different ends of the same section of heat exchange area.
Further, in the step S1, the overlapping portion of the inner tube and the outer tube is a heat exchange area.
Further, in S1, the synthesis reaction conditions are: the temperature is 60-65 ℃ and the pressure is 0.1-0.45MPa.
Further, in the step S3, the circulating device may send sulfur monochloride out of the reaction system.
Compared with the prior art, the invention has the beneficial effects that:
1. the front section of the sulfur dichloride synthesis system uses a static mixer, so that chlorine and sulfur monochloride are fully mixed, the condition of uneven distribution is avoided, the interface updating speed of the static mixer is high, and the reaction speed of the chlorine and the sulfur monochloride is accelerated; because of the use of the static mixer, the phase interface is in a continuously updated state, so that the heat and mass transfer effects are better, the reduction of the temperature gradient in the whole reaction area is facilitated, and the reaction temperature control is more accurate;
2. the sulfur dichloride synthesis system adopts a sleeve-type reactor, the specific surface area of the material per unit mass is larger, the reaction mass transfer and heat transfer effects are better, and the low-grade heat source (hot water at 70-100 ℃) in the production of thionyl chloride is used, so that the sulfur dichloride synthesis system has better energy saving and consumption reduction effects.
3. The initial temperature difference between the sulfur monochloride and the chlorine and the heat source is larger, the temperature of the sulfur monochloride and the chlorine can be quickly increased to the reaction temperature, the reaction time is shortened, the subsequent temperature difference is smaller, and the reaction temperature is stable.
4. The sulfur monochloride which is not fully reacted enters the sulfur dichloride synthesizer again, so that the substrate concentration is increased, the forward progress of the reaction balance is promoted, and the reaction rate and the sulfur dichloride concentration are improved.
5. The sulfur dichloride synthesis system can freely adjust the load of the production system according to the capacity and the residence time, and has better freedom than a kettle type bubbling reactor.
6. The invention also achieves two unexpected technical effects: 1, as sulfur monochloride and chlorine are fully mixed, the reaction temperature rises rapidly and stably, and the reaction proceeds positively, a product with higher sulfur monochloride content can be obtained without adding a catalyst; secondly, because the sulfur monochloride content in the product is high, distillation operation is not needed, and the process flow is simplified.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of the sulfur dichloride synthesis reaction according to the present example;
fig. 2 is a schematic view of the sulfur dichloride synthesizer according to the present embodiment.
In the figure: the synthesis apparatus 1, fresh sulfur monochloride and chlorine gas input pipe 101, shutoff valve 102, inner pipe 103, outer pipe 104, static mixer 105, inner pipe U-shaped connecting pipe 106, outer pipe connecting pipe 107, heat source input pipe 108, shutoff valve 109, shutoff valve 110, heat source output pipe 111, shutoff valve 112, connecting pipe 113, flange 114, gas-liquid separation tank 2, liquid phase pipe 201, gas phase pipe 202, sulfur monochloride circulating pump 3, shutoff valve 301, sulfur monochloride output pipe 302, circulating sulfur monochloride delivery pipe 303, and shutoff valve 304.
Detailed Description
Example 1
Referring to fig. 1 and 2, a sulfur dichloride synthesizing system comprises a synthesizing device 1, a separating device 2 and a circulating device 3, wherein the synthesizing device 1 consists of a raw material mixing module and a reaction module, the reaction module consists of an inner pipe 103 and an outer pipe 104, the inner pipe 103 and the outer pipe 104 are horizontally arranged, the cross section of the same plane is a concentric ring, the other end of the inner pipe 103 is connected with the separating device 2 through a connecting pipe 113, the separating device 2 is connected with the circulating device through a liquid phase pipe 201, the circulating device is connected with a fresh sulfur monochloride and chlorine input pipe 101 through a circulating sulfur monochloride conveying pipe 303, and a static mixer 3 is connected at one end of the inner pipe 103; the inner tube 103 and the outer tube 104 are welded separately, the inner tubes are connected by an inner tube U-shaped connecting tube 106, the inner tube 103 and the inner tube U-shaped connecting tube 106 are connected by a flange 114, the outer tube 104 is welded on the inner tube in sections, and the number of the inner tube 103 and the outer tube 104 is at least 1. The static mixer 3 is SV-3.5/50 model, and the sulfur monochloride circulating pump 3 is ATY-12 model.
Example 2
Referring to fig. 1, a method for synthesizing sulfur dichloride includes the steps of:
s1, regulating the flow of fresh sulfur monochloride in the input pipe 101 to be 2.5m 3 Per hour, chlorine flow of 2.5Nm 3 /h, the flow in the circulating sulfur monochloride conveying pipe 303 is adjusted to be 4m 3 And/h, hot water with the temperature of 70-90 ℃ is input from one end of the inner pipe 103 connected with the static mixer 105 and enters from the heat source conveying pipe 108, and the hot water is steam liquefied water in the production of thionyl chloride for energy conservation and environmental protection;
s2, the overlapping part of the inner tube 103 and the outer tube 104 is a heat exchange area, chlorine and sulfur monochloride are heated to carry out synthesis reaction, sulfur monochloride and chlorine and hot water enter from different ends of the same section of heat exchange area and enter from different ends of the next section of heat exchange area, finally leave from different ends of the same section of heat exchange area, the flow rate of the hot water is regulated to control the reaction temperature to 60 ℃, the pressure is 0.1MPag, and the pressure of the inner tube 103 is kept to be greater than that of the outer tube 104;
s3, the synthesized product enters a gas-liquid separation tank 2 through a connecting pipe 113, the separated gas phase is a sulfur dichloride finished product, the gas phase is sent to the next process from a gas phase pipe 202, the separated sulfur monochloride enters a sulfur monochloride circulating pump 3 through a liquid phase pipe 201, and the circulating pump can send the sulfur monochloride to a synthesizing device through a circulating sulfur monochloride conveying pipe or send the sulfur monochloride to other working sections through a sulfur monochloride output pipe.
Example 3
This example differs from example 2 in that the flow rate of the circulating sulfur monochloride in S1 is 3m 3 And/h, the remainder being exactly the same as in example 2.
Example 4
This example differs from example 2 in that the fresh sulfur monochloride flow in S1 is 3.5m 3 And/h, the flow rate of the circulating sulfur monochloride is 2.7m 3 And/h, the remainder being exactly the same as in example 2.
Example 5
This practice isThe examples differ from example 2 in that the fresh sulfur monochloride flow in S1 is 3.5m 3 And/h, the flow rate of the circulating sulfur monochloride is 2.7m 3 The synthesis temperature in S2 was 65℃and the remainder was exactly the same as in example 2.
Detection and results
The sulfur dichloride content in the gas phase separated by the gas-liquid separation tank was measured, and the results are shown in Table 1
TABLE 1
| Project | Sulfur dichloride content (%) |
| Example 2 | 91.6 |
| Example 3 | 92.1 |
| Example 4 | 92.5 |
| Example 5 | 93.7 |
As can be seen from the table, the sulfur dichloride content prepared by the method is higher than 90% and is 93.7% at most.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
In the present invention, unless explicitly specified and limited otherwise, the terms "disposed," "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; the connection may be mechanical connection, direct connection or indirect connection through an intermediate medium, and may be internal connection of two elements or interaction relationship of two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. The synthesis system of sulfur dichloride is characterized by comprising a synthesis device (1), a separation device (2) and a circulation device (3);
the synthesis device (1) comprises a raw material mixing module (105) and a reaction module, wherein the reaction module comprises an inner pipe (103) and an outer pipe (104), and the raw material mixing module (105) is connected to one end of the inner pipe (103);
the other end of the inner tube (103) is connected with the separation device (2) through a connecting tube (113), the separation device (2) is connected with the circulation device (3) through a liquid-phase tube (201), and the circulation device (3) is connected with the synthesis device (1) through a circulating sulfur chloride conveying tube (303).
2. A sulfur dichloride synthesis system according to claim 1, wherein the raw material mixing module (105) is a static mixer.
3. A sulfur dichloride synthesis system according to claim 1, wherein the inner tube (103) and the outer tube (104) are horizontally disposed and the cross section perpendicular to the plane of the tube is concentric rings.
4. The sulfur dichloride synthesis system according to claim 1, wherein the separation device (2) is a gas-liquid separation tank, a liquid phase pipe (201) is connected to the tank top, and a gas phase pipe (202) is connected to the tank bottom.
5. The sulfur dichloride synthesizing system according to claim 1, wherein the circulating device (3) is a circulating pump, and is connected with a circulating sulfur monochloride conveying pipe (303) and a sulfur monochloride output pipe (302).
6. A method of synthesizing a sulfur dichloride synthesis system according to any one of claims 1-5, comprising the steps of:
s1: inputting chlorine and sulfur monochloride into a synthesis device (1) from one end of an inner pipe (103) connected with a static mixer (105), inputting a heat source into the synthesis device (1) from one end of an outer pipe (104) far away from an inlet of the chlorine and the sulfur monochloride, and heating the chlorine and the sulfur monochloride to carry out synthesis reaction;
s2: the synthesis reaction product enters a gas-liquid separation tank (2) from the other end of the inner tube (103) for separation to obtain a gas phase composed of chlorine and sulfur dichloride and a liquid phase composed of sulfur monochloride;
s3: the sulfur monochloride is returned to the synthesis unit (1) via a circulation unit (3).
7. The method for synthesizing sulfur dichloride according to claim 6, wherein in S1, chlorine and sulfur monoxide enter the synthesizing device (1) and are fully mixed by the raw material mixing module, and then the synthesizing reaction is completed in the reaction module.
8. The method for synthesizing sulfur dichloride according to claim 6, wherein in the step S1, the heat source in the outer tube (104) is hot water at 70-90 ℃.
9. The method for synthesizing sulfur dichloride according to claim 6, wherein in S1, the horizontal flow direction of sulfur monochloride and chlorine in the inner tube (103) is opposite to the horizontal flow direction of hot water in the outer tube (104).
10. The method for synthesizing sulfur dichloride according to claim 6, wherein in S3, the circulating device is further capable of sending sulfur monochloride out of the reaction system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311778797.3A CN117772062A (en) | 2023-12-22 | 2023-12-22 | Sulfur dichloride synthesizing system and method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311778797.3A CN117772062A (en) | 2023-12-22 | 2023-12-22 | Sulfur dichloride synthesizing system and method |
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| Publication Number | Publication Date |
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| CN117772062A true CN117772062A (en) | 2024-03-29 |
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| CN202311778797.3A Pending CN117772062A (en) | 2023-12-22 | 2023-12-22 | Sulfur dichloride synthesizing system and method |
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- 2023-12-22 CN CN202311778797.3A patent/CN117772062A/en active Pending
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