Benzene-free carbon disulfide production system
By employing a fractional distillation and washing process, using a reaction vessel, a crude distillation column, and a rectification column, the problem of high benzene content in existing benzene-free carbon disulfide production has been solved, achieving the production of high-purity benzene-free carbon disulfide and meeting the requirements of environmental protection and chemical purity.
Patent Information
- Application Number
- CN202423229954.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-26
- Publication Date
- 2026-01-02
- Estimated Expiration
- 2034-12-26
AI Technical Summary
Existing benzene-free carbon disulfide production processes are unable to efficiently produce high-purity benzene-free carbon disulfide, and the purity is not high. Furthermore, existing production processes suffer from high benzene content, making them difficult to process.
A staged distillation system is adopted, including a reaction vessel, a crude distillation column, a staged distillation unit, and a distillation column. Through staged distillation and washing processes, the benzene content in the raw material is reduced, and high-purity benzene-free carbon disulfide is obtained through molecular sieve adsorption and oxidant treatment.
The production of high-purity benzene-free carbon disulfide has been achieved. Through fractional distillation and washing processes, the benzene content in the raw materials has been reduced, thereby increasing the purity of the benzene-free carbon disulfide and meeting the requirements for environmental protection and chemical purity.
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Figure CN223746996U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model belongs to benzene-free carbon bisulfide purification technical field, especially relates to a benzene-free carbon bisulfide production system. BACKGROUND
[0002] Benzene-free carbon bisulfide is a colorless or light yellow transparent liquid, has irritating smell, is volatile and flammable. When storing, usually requires the container with water to cover the surface, and is far from the fire, heat source, keeps the container sealed. The traditional carbon bisulfide may mix a certain amount of benzene in production and preparation, which limits its use range. And benzene-free carbon bisulfide avoids this problem, meets the current social requirements of environmental protection and chemical purity. And benzene-free carbon bisulfide has high purity and good stability, which makes it can maintain excellent performance in the application in multiple fields. For example, in the field of chromatographic analysis, benzene-free carbon bisulfide can be used as a solvent or stationary phase in chromatographic analysis, improves the separation effect of chromatographic column. In detection and analysis, it is mainly used for detecting benzene series in environment such as water, soil and air, and determining toxic substances in workplace air, such as saturated alkane compounds, halogenated alkane compounds, aromatic hydrocarbon compounds, polycyclic aromatic hydrocarbon compounds, aliphatic ester compounds, aliphatic ether compounds and aliphatic ketone compounds. In detection, carbon bisulfide is mainly used for extracting or analyzing samples, and then combined with gas chromatography (GC) or gas chromatography-mass spectrometry (GC-MS) method to carry out qualitative and quantitative analysis.
[0003] However, the existing benzene-free carbon bisulfide is generally produced by directly distilling after molecular sieve adsorption, and the obtained benzene-free carbon bisulfide is actually a low benzene grade product, and the benzene content is generally between 10-50 ppm, so it is not easy to obtain benzene-free grade product, and it is greatly affected by raw materials. The larger the benzene content in the raw material, the more difficult it is to process to benzene-free. Only carbon bisulfide with benzene content below 1000 ppm can be processed. UTILITY MODEL CONTENT
[0004] The application aims at the above problems, and provides a benzene-free carbon bisulfide production system, which can improve the problem that the existing production process still contains benzene and has low purity.
[0005] The technical scheme adopted by the utility model is as follows: a benzene-free carbon bisulfide production system, the system comprises: a reaction kettle for water bath heating of a three-necked bottle, the three-necked bottle is placed with industrial benzene-free carbon bisulfide; and the three-necked bottle is connected with a first-stage rectification device; the first-stage rectification device comprises a first-stage rectification tower and a first-stage condenser, the first-stage rectification tower is connected with the three-necked bottle and is used for primary distillation of raw materials; the first-stage condenser is connected with the output end of the first-stage rectification tower; a second-stage rectification device is used for secondary distillation operation of raw materials, and the second-stage rectification device is the same in structure as the first-stage rectification device and comprises a second-stage rectification tower and a second-stage condenser.
[0006] Due to the arrangement of the above structure, the industrial benzene-free carbon disulfide is subjected to fractional distillation, and benzene-free carbon disulfide with different purities at different stages can be obtained, and finally completely benzene-free carbon disulfide can be output, thereby improving the purity of benzene-free carbon disulfide.
[0007] Further, in order to distill the raw material multiple times, the first-stage distillation device is provided with two output ports, the first output port is connected with the second-stage distillation device for distillation again, and the second output port is connected with the first-stage condenser.
[0008] Further, in order to obtain the final product with high purity, the second-stage distillation device is provided with an output port, which is connected with the second-stage condenser for condensing the distilled gas.
[0009] Further, in order to improve the applicability of the system, the number of distillation devices is adjusted in real time, and valves are arranged between the first-stage distillation tower, the first-stage condenser, the second-stage distillation tower and the second-stage condenser.
[0010] Further, in order to obtain benzene-free carbon disulfide with different purities at different stages, the first-stage distillation device and the second-stage distillation device each include a receiver, and the receiver includes a first-stage receiver and a second-stage receiver, which are respectively connected with the first-stage condenser and the second-stage condenser for receiving benzene-free carbon disulfide products in stages.
[0011] Further, in order to control the temperature of the water bath heating, the temperature of the liquid water in the reaction kettle is measured in real time, and a water bath thermometer is arranged in the reaction kettle for measuring the temperature in the reaction kettle.
[0012] Further, in order to measure the reaction temperature of the raw material in the three-necked flask in real time, a reaction thermometer is arranged in the three-necked flask for real-time monitoring of the temperature in the three-necked flask.
[0013] Further, in order to measure the temperature of the reaction in the distillation tower in real time, and further control the reaction conditions, a distillation thermometer is connected with the first-stage distillation tower and the second-stage distillation tower, and the distillation thermometer is used to measure the temperature of the output gas from the distillation tower.
[0014] Further, in order to improve the purity of the product obtained by the production system, the production system further includes a rough distillation tower for reducing the benzene content in the industrial benzene-free carbon disulfide, the rough distillation tower is connected with a washing device for washing and filtering through the washing device, and the washing device is connected with the reaction kettle for feeding the washed benzene-free carbon disulfide into the reaction kettle for heating.
[0015] Further, in order to provide a raw material with less benzene content for subsequent fractional distillation, and improve the purity of carbon disulfide without benzene, the packing in the crude distillation column is molecular sieve.
[0016] To sum up, due to the adoption of the above technical scheme, the beneficial effects of the present application are:
[0017] By setting the primary and secondary rectification devices to fractionally rectify the industrial carbon disulfide without benzene, carbon disulfide without benzene with different purities at different stages can be obtained, and completely carbon disulfide without benzene can be finally output, thereby improving the purity of carbon disulfide without benzene.
[0018] The industrial carbon disulfide without benzene is rectified once in the crude distillation column to reduce the benzene content in the raw material, and then a small amount of oxidizing agent such as concentrated sulfuric acid is added for washing, and then the molecular sieve is added to the washed carbon disulfide for stirring, filtration, and finally the treated carbon disulfide is put into the fractional distillation system to obtain carbon disulfide without benzene. Thus the purity of carbon disulfide without benzene can be improved. BRIEF DESCRIPTION OF DRAWINGS
[0019] In order to more clearly illustrate the technical scheme of the embodiments of the present application, the following will briefly introduce the drawings needed in the embodiments. It should be understood that the following drawings only show some embodiments of the present application, and therefore should not be regarded as limiting the scope. For those skilled in the art, other related drawings can also be obtained without creative labor.
[0020] Figure 1 The present application is a schematic diagram of the overall structure.
[0021] Reference signs: 1, reaction kettle; 2, three-necked flask; 3, primary rectification column; 4, secondary rectification column; 5, primary condenser; 6, secondary condenser; 7, primary receiver; 8, secondary receiver; 9, water bath thermometer; 10, reaction thermometer; 11, distillation thermometer. DETAILED DESCRIPTION
[0022] The present application will be described in detail below with reference to the drawings.
[0023] In order to make the purpose, technical scheme and advantages of the present application more clear and explicit, the present application will be further described in detail below with reference to the drawings and examples. It should be understood that the specific examples described herein are only used to explain the present application, and are not intended to limit the present application.
[0024] A benzene-free carbon disulfide production system includes: a crude distillation column for reducing the benzene content in industrial benzene-free carbon disulfide; the crude distillation column is connected to a washing device for washing and filtering; the washing device is connected to a reaction vessel 1 for feeding the washed benzene-free carbon disulfide into the reaction vessel 1 for heating.
[0025] The reactor 1 is used to heat the three-necked flask 2 in a water bath. The three-necked flask 2 contains industrial benzene-free carbon disulfide. The three-necked flask 2 is connected to a primary distillation unit.
[0026] A primary distillation unit includes a primary distillation column 3 and a primary condenser 5. The primary distillation column 3 is connected to a three-necked flask 2 and is used for the initial distillation of the raw material. The primary condenser 5 is connected to the output end of the primary distillation column 3.
[0027] The secondary distillation unit is used to redistill the raw materials, and its structure is the same as that of the primary distillation unit.
[0028] The process is as follows: Industrial benzene-free carbon disulfide is first distilled in a crude distillation column to reduce the benzene content in the raw material. Then, a small amount of oxidant, such as concentrated sulfuric acid, is added for treatment and washing. Next, molecular sieves are added to the washed carbon disulfide, stirred, and filtered. Finally, the treated carbon disulfide is fed into a segmented distillation system (including a primary distillation unit and a secondary distillation unit) to obtain benzene-free carbon disulfide. This process improves the purity of benzene-free carbon disulfide.
[0029] Example 1
[0030] like Figure 1 As shown, one embodiment of this utility model is that the primary distillation apparatus includes:
[0031] The reactor 1 is used to heat the three-necked flask 2 in a water bath. The three-necked flask 2 contains industrial benzene-free carbon disulfide. The three-necked flask 2 is connected to a primary distillation unit.
[0032] A primary distillation unit includes a primary distillation column 3 and a primary condenser 5. The primary distillation column 3 is connected to a three-necked flask 2 and is used for the initial distillation of the raw material. The primary condenser 5 is connected to the output end of the primary distillation column 3. The output end of the primary condenser 5 is connected to a primary receiver 7. The finished product output from the primary distillation column 3 and the primary condenser 5 enters the primary receiver 7 through a pipeline for temporary storage.
[0033] This completes the initial distillation. In actual use, the number of distillations is determined based on the benzene content of the carbon disulfide-free disulfide.
[0034] Example 2
[0035] The utility model discloses a secondary rectification device for the secondary distillation operation of raw materials, and the secondary rectification device has the same structure as the primary rectification device. The secondary rectification device comprises a secondary condenser 6 and a secondary rectification tower 4, the input end of the secondary rectification tower 4 is connected with the output end of the primary rectification tower 3, and a valve (not shown in the figure) is arranged between the primary rectification tower 3 and the secondary rectification tower 4. When the raw materials need to be distilled only once, the valve is closed; when the raw materials need to be distilled multiple times, the valve is opened, the raw materials are distilled in the primary rectification tower 3, and then enter the secondary rectification tower 4 for secondary distillation. The distilled gas enters the secondary condenser 6 for condensation.
[0036] The benzene-free carbon disulfide obtained through two-stage rectification has improved purity.
[0037] Embodiment 3
[0038] In another embodiment of the utility model, the primary rectification device and the secondary rectification device both comprise a receiver, the receiver comprises a primary receiver 7 and a secondary receiver 8, the primary receiver 7 and the secondary receiver 8 are connected with the primary condenser 5 and the secondary condenser 6 respectively, and are used for receiving benzene-free carbon disulfide products in sections. If the secondary rectification device is the last rectification device, the secondary rectification device contains completely benzene-free carbon disulfide products.
[0039] Each production system is provided with a receiver, which is convenient for storing the generated products in sections. The more the sectional levels are, the higher the purity of the products received by the high-level receiver is, and the lower the purity of the products received by the low-level receiver is. Therefore, the system can obtain high-purity products, completely benzene-free carbon disulfide and low-purity products, low benzene carbon disulfide.
[0040] Embodiment 4
[0041] In another embodiment of the utility model, a reaction thermometer 10 is arranged in the three-necked flask 2, and the reaction thermometer 10 is used for monitoring the temperature in the three-necked flask 2 in real time.
[0042] In order to control the temperature of the industrial benzene-free carbon disulfide in the three-necked flask 2 in real time, so as to adjust the temperature of the liquid in the reaction kettle 1, the temperature in the reaction kettle 1 is measured by the water bath thermometer 9, so that the temperature is controlled at a temperature convenient for the evaporation of the industrial benzene-free carbon disulfide, and the production efficiency is improved.
[0043] Embodiment 5
[0044] In another embodiment of the utility model, the production system further comprises a crude distillation tower, the crude distillation tower is used for reducing the benzene content in the industrial benzene-free carbon disulfide, the crude distillation tower is connected with a washing device, and the washing device is used for washing and filtering; the washing device is connected with the reaction kettle 1, and is used for sending the washed benzene-free carbon disulfide into the reaction kettle 1 for heating.
[0045] The step of rough distillation is not necessary when the benzene content in the raw material is very small, less than 100 ppm, and the step of rough distillation can be omitted; when the benzene content in the raw material is relatively high, through the step of rough distillation, the subsequent rectification can be more convenient, and completely benzene-free carbon disulfide can be obtained through fewer rectification devices, thereby improving the purity of benzene-free carbon disulfide.
[0046] Embodiment 6
[0047] Another embodiment of the utility model is that the rough distillation column filler is a molecular sieve. The benzene content in the raw material is reduced by rough distillation first, then an oxidizing agent is added to the rough distillation column for treatment and adsorption with a molecular sieve, and then fractional rectification is carried out through a benzene-free carbon disulfide production system to obtain completely benzene-free carbon disulfide products.
[0048] When the benzene content is relatively high, rough distillation operation is required first, and the molecular sieve in the rough distillation column can reduce the benzene content, thereby providing less benzene-containing raw material for subsequent fractional rectification and improving the purity of benzene-free carbon disulfide.
[0049] Embodiment 7
[0050] According to the above embodiments, the fractional rectification device of the embodiment can increase or decrease the rectification device according to the actual use, and at the same time, in order to avoid too many rectification devices, a rough distillation device is arranged before the rectification device to rough distill industrial benzene-free carbon disulfide, remove most of the benzene therein, and make the subsequent rectification more convenient.
[0051] The above only describes the preferred embodiments of the utility model, and does not limit the utility model, and any modification, equivalent replacement and improvement within the spirit and principle of the utility model should be included in the protection scope of the utility model.
Claims
1. A system for the production of benzene- free carbon disulfide, characterized by, The system comprises: a reaction kettle for water bath heating of a three-necked flask in which industrial benzene-free carbon disulfide is placed, and the three-necked flask is connected with a first-stage rectification device; the first-stage rectification device comprises a first-stage rectification tower and a first-stage condenser, the first-stage rectification tower is connected with the three-necked flask and used for primary distillation of raw materials, and the first-stage condenser is connected with an output end of the first-stage rectification tower; a second-stage rectification device for secondary distillation of raw materials, and the second-stage rectification device has the same structure as the first-stage rectification device and comprises a second-stage rectification tower and a second-stage condenser.
2. The system for producing carbon disulfide without benzene according to claim 1, wherein In the first-stage rectification device, the first-stage rectification tower is provided with two output ports, a first output port is connected with the second-stage rectification device and used for secondary distillation, and a second output port is connected with the first-stage condenser.
3. The system for producing a benzene dithiocarbonic acid-free product according to claim 2, characterized by, In the second-stage rectification device, the second-stage rectification tower is provided with an output port connected with the second-stage condenser and used for condensation of distilled gas.
4. The system for producing carbon disulfide free of phenyldisulfide according to claim 3, characterized by Valves are arranged between the first-stage rectification tower, the first-stage condenser, the second-stage rectification tower and the second-stage condenser.
5. The system for producing a benzene dithio carbon-free product according to claim 3, wherein The first-stage rectification device and the second-stage rectification device both comprise receivers, the receivers comprise a first-stage receiver and a second-stage receiver, the first-stage receiver and the second-stage receiver are connected with the first-stage condenser and the second-stage condenser respectively, and are used for segmented reception of benzene-free carbon disulfide products.
6. The system for producing a benzene carbon disulfide-free product according to claim 1, wherein The reaction kettle is provided with a water bath thermometer for measurement of the temperature in the reaction kettle.
7. The system for producing a benzene carbon disulfide-free product according to claim 1, wherein The three-necked flask is provided with a reaction thermometer for real-time monitoring of the temperature in the three-necked flask.
8. The system for producing a benzene carbon disulfide-free product according to claim 1, wherein The first-stage rectification tower and the second-stage rectification tower are both connected with distillation thermometers for measurement of the temperature of output gas from the rectification tower.
9. The system for producing carbon disulfide-free benzene according to claim 1, wherein The production system further comprises a crude distillation tower for reduction of the benzene content in industrial benzene-free carbon disulfide, the crude distillation tower is connected with a washing device for washing and filtering, the washing device is connected with the reaction kettle, and the washing device is used for feeding the washed benzene-free carbon disulfide into the reaction kettle for heating.
10. The benzene-free carbon disulfide production system according to claim 9, characterized in that: The packing in the crude distillation tower is molecular sieve.