A chloroform drying device

Abstract

The present application relates to chloroform drying technical field, specifically provide a kind of chloroform drying device, the chloroform drying device of the present application, comprising: chloroform dryer, for receiving chloroform raw materials, and the chloroform raw materials are dried;Chloroform collection tank, it is connected with the chloroform dryer by pipeline, for collecting residual in the liquid phase material in the chloroform dryer;Drying circulating pump, it is connected with the chloroform collection tank by pipeline, for the liquid phase material collected in the chloroform collection tank is dried;Activation gas supply device, it is connected with the chloroform dryer by pipeline, for providing activation gas to the chloroform dryer;Tail gas condenser, it is connected with the chloroform dryer by pipeline, for cooling the tail gas in the chloroform dryer, and condensate is transported to the chloroform collection tank.The chloroform drying device significantly improves the drying effect of chloroform, and reduces the loss of chloroform raw materials.

Description

Technical Field

[0001] This invention relates to the field of chloroform drying technology, and more specifically to a chloroform drying apparatus. Background Technology

[0002] As a raw material for fluorination reactions, the water content of chloroform is a crucial quality indicator. High water content severely impacts the lifespan of the catalyst (SbCl5) and the quality of the fluorination reaction. To reduce the influence of excess water in chloroform on the catalyst, it is necessary to dry and dehydrate the chloroform using a chloroform drying unit. Currently, the operation method for drying the water content in chloroform using molecular sieves is as follows: all chloroform storage tanks and tank trucks supplying material to the fluorination reaction station must pass through a dryer for dehydration (inlet and outlet water content difference ≥ 50 ppm). The dryer needs to be periodically switched and activated to ensure drying quality.

[0003] In existing chloroform feedstock supply processes, qualified chloroform or chloroform stored in chloroform storage tanks is directly pumped to the chloroform metering tank of the downstream fluorination reaction unit. This chloroform supply process has the following drawbacks:

[0004] 1. When the water content of chloroform stored in the chloroform storage tank increases, it cannot be dried and dehydrated, resulting in a high water content in the chloroform raw material supplied to the downstream fluorination reaction production unit, which affects the catalyst's service life.

[0005] 2. The chloroform in the chloroform storage area that is recovered to the chloroform tank via the chloroform condenser generally has a high water content and cannot be directly used as raw material for downstream fluorination reaction production units, resulting in waste of raw materials. Summary of the Invention

[0006] The purpose of this invention is to provide a chloroform drying device that dries and removes water from the chloroform material during its transfer and transportation process, thereby reducing the water content of the chloroform within a certain range (the difference between inlet and outlet water content Δ = inlet water content - outlet water content ≥ 50 ppm), indirectly improving the service life of the fluorination reaction catalyst (SbCl5) and the quality of the fluorination reaction.

[0007] To achieve the above objectives, the present invention provides a chloroform drying apparatus, comprising: a chloroform dryer for receiving chloroform raw material and drying the chloroform raw material; a chloroform collection tank connected to the chloroform dryer via a pipeline for collecting liquid material remaining in the chloroform dryer; a drying circulation pump connected to the chloroform collection tank via a pipeline for drying the liquid material collected in the chloroform collection tank; an activation gas supply device connected to the chloroform dryer via a pipeline for supplying activation gas to the chloroform dryer; and a tail gas condenser connected to the chloroform dryer via a pipeline for cooling the tail gas in the chloroform dryer and conveying the condensate to the chloroform collection tank.

[0008] Furthermore, the chloroform dryer is equipped with a molecular sieve.

[0009] Furthermore, sampling devices are provided at the outlet and inlet of the chloroform dryer.

[0010] Furthermore, the chloroform collection tank is equipped with a first sampling valve.

[0011] Furthermore, a second sampling valve is provided at the outlet of the drying circulation pump.

[0012] Furthermore, it also includes an activation gas heater for heating the activation gas before delivering it to the chloroform dryer.

[0013] Furthermore, it also includes a steam pipeline, and the chloroform dryer is equipped with a jacket. The steam pipeline is connected to the jacket of the chloroform dryer for heating the chloroform dryer.

[0014] Furthermore, a safety valve is installed at the top of the chloroform dryer, and the overpressure relief port of the safety valve is connected to the chloroform collection tank.

[0015] Furthermore, the activating gas is nitrogen.

[0016] Furthermore, the cooling medium used in the exhaust gas condenser is water at 5°C.

[0017] Compared with the existing direct supply of chloroform raw materials, the present invention has the following advantages:

[0018] The chloroform drying apparatus of this application embodiment is a continuously operating drying device in the entire system of chloroform storage and use, and does not affect the chloroform delivery rate in the entire system. It maintains the original chloroform feeding efficiency of the system while also improving the quality of the chloroform raw material supply to a certain extent. All related utilities—nitrogen, steam, and industrial water—are readily available, have low difficulty and cost of use, and are effectively recycled and subjected to related harmless treatment. The nitrogen heater used for activating the chloroform dryer has a built-in PLC temperature control cabinet, making operation relatively automated.

[0019] The chloroform drying apparatus of this application reduces the water content of chloroform by an average of 50 ppm after drying compared to before drying. The entire chloroform drying apparatus is a closed-loop system, effectively collecting and recycling all liquid materials and energy involved; the gaseous phase of the material is recovered and reused after condensation, and the exhaust gas is treated by an environmental protection device. Moreover, the chloroform drying process is continuous and does not affect the stability of the production process. As an additional intermediate step, it does not reduce production efficiency. The chloroform with high water content that was recovered to the chloroform collection tank from the original chloroform tank area via the exhaust gas condenser can be dried to a suitable standard using the drying circulation pump and then supplied to the downstream fluorination reaction unit, avoiding raw material waste. Attached Figure Description

[0020] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0021] Figure 1 This is a schematic diagram of the chloroform drying apparatus in an embodiment of the present invention.

[0022] Reference numerals: 1. Chloroform dryer; 2. Chloroform collection tank; 3. Drying circulation pump; 4. Tail gas condenser; 5. Activated gas heater. Detailed Implementation

[0023] Preferred embodiments of the present invention will now be described with reference to the accompanying drawings. Those skilled in the art should understand that these embodiments are merely illustrative of the technical principles of the present invention and are not intended to limit the scope of protection of the present invention. Those skilled in the art can make adjustments as needed to adapt to specific application scenarios.

[0024] First, it should be noted that in the description of this invention, the terms "upper," "lower," "left," "right," "vertical," "horizontal," "longitudinal," "inner," and "outer," which indicate directional or positional relationships, are based on the directional or positional relationships shown in the accompanying drawings. These are merely for ease of description and do not indicate or imply that the device or element must have a specific orientation, or be constructed and operated in a specific orientation; therefore, they should not be construed as limitations on this invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0025] Furthermore, it should be noted that, in the description of this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0026] like Figure 1 As shown in the figure, an embodiment of the present invention provides a chloroform drying device, which includes: a chloroform dryer 1, a chloroform collection tank 2, a drying circulation pump 3, a tail gas condenser 4, and an activation gas supply device (not shown in the figure).

[0027] Specifically, the chloroform dryer 1 is used to receive chloroform raw materials and dry them. A molecular sieve is installed in the chloroform dryer 1. The molecular sieve has many uniformly sized channels and neatly arranged pores in its structure. Molecular sieves with different pore sizes separate molecules of different sizes and shapes; furthermore, it has high adsorption capacity, strong selectivity, and high temperature resistance, making it suitable for drying and dehydrating chloroform raw materials passing through the chloroform dryer 1.

[0028] The inlet pipeline of chloroform dryer 1 is connected to the outlet pipeline of the chloroform transfer pump in the chloroform storage tank area, and is also connected to the pipeline connected to the outlet of the drying circulation pump 3; so that chloroform dryer 1 can be used to dry chloroform transported in the chloroform tank area and the chloroform unloading area; it can also be used to dry the non-conforming chloroform material temporarily stored in the chloroform collection tank 2 in the chloroform drying area.

[0029] The chloroform raw material enters the chloroform dryer 1 from the bottom through the main inlet valve of the chloroform dryer 1 via the main transfer pipe from the chloroform tank area. After being dried and dehydrated by the molecular sieve in the chloroform dryer 1, the raw material leaves the chloroform dryer 1 through the top outlet valve and returns to the chloroform unloading and transfer pump outlet main pipe in the chloroform tank area, or is directly transported to the downstream chloroform metering tank device for the fluorination reaction through a pipeline connected to the outlet of the drying circulation pump 3.

[0030] To test the drying effect of chloroform dryer 1 on chloroform raw materials, sampling devices are installed at both the outlet and inlet of chloroform dryer 1. These devices are used to sample the chloroform raw materials before entering chloroform dryer 1 and the chloroform after drying in chloroform dryer 1, and to analyze the moisture content of the two chloroform samples. By comparing the moisture content of the two samples, the drying effect of chloroform dryer 1 on chloroform raw materials is verified, and it is determined whether the drying result meets the requirements.

[0031] The chloroform collection tank 2 is connected to the chloroform dryer 1 via a pipeline and is used to collect the liquid material remaining in the chloroform dryer 1. The liquid material is the insufficiently dried chloroform remaining in the chloroform dryer 1 during the drying process of the chloroform raw material. The chloroform collection tank 2 is equipped with a first sampling valve (not shown in the figure). Through the first sampling valve, a sample of the liquid material collected in the chloroform collection tank 2 can be collected, and the moisture content of the collected sample can be analyzed to determine whether it is up to standard.

[0032] The drying circulation pump 3 is connected to the chloroform collection tank 2 via pipeline and is used to dry the liquid material collected in the chloroform collection tank 2. When the liquid material obtained through the sampling valve set on the chloroform collection tank 2 is found to have excessive moisture content after testing, the drying circulation pump 3 will further dry the liquid material in the chloroform collection tank 2. A second sampling valve (not shown in the figure) is installed at the outlet of the drying circulation pump 3. Through the second sampling valve, a sample of the liquid material after drying by the drying circulation pump 3 can be collected, and the moisture content of the collected sample can be analyzed to determine whether it is qualified. If it is qualified, it is transported through pipeline to the chloroform storage tank or the chloroform metering tank of the downstream fluorination reaction. If it is unqualified, it is transported through pipeline to the inlet pipeline of the chloroform dryer 1 for drying again in the chloroform dryer 1.

[0033] An activating gas supply device (not shown in the figure) is connected to the chloroform dryer 1 via a pipeline and is used to supply activating gas to the chloroform dryer. In this embodiment, the activating gas is nitrogen. When the chloroform raw material is dried in the chloroform dryer 1, the activating gas supply device is connected to the chloroform dryer 1 via a pipeline and supplies activating gas, such as nitrogen, into the chloroform dryer 1. In order to reach a set temperature before the activating gas enters the chloroform dryer 1, an activating gas heater 5 is also provided on the activating gas transmission pipeline to heat the activating gas before it is delivered to the chloroform dryer 1. In a specific embodiment, the activating gas heater 5 can be an electric heating device equipped with a temperature control cabinet, capable of heating the activating gas to 200-300°C.

[0034] Based on the requirements of the activation process, during the drying of chloroform raw materials in chloroform dryer 1, steam needs to be supplied to chloroform dryer 1 to increase the temperature within chloroform dryer 1, thereby enhancing the activity of the activated molecules and accelerating the activation rate. Therefore, a steam pipeline is also installed in the chloroform drying device to supply steam to chloroform dryer 1, raising its temperature. For this purpose, chloroform dryer 1 is equipped with a jacket, and the steam pipeline is connected to the jacket, allowing steam to enter through the jacket rather than directly into chloroform dryer 1 for heating.

[0035] The tail gas condenser 4 is connected to the chloroform dryer 1 via a pipeline. It cools the tail gas in the chloroform dryer 1 and transports the condensate to the chloroform collection tank 2. During the drying process of the chloroform raw material in the chloroform dryer 1, an activating gas, such as nitrogen, needs to be introduced into the chloroform dryer 1. The nitrogen, upon passing through the chloroform dryer 1, carries away water molecules adsorbed in the molecular sieve and residual chloroform vapor, forming a tail gas mainly composed of nitrogen, water, and chloroform. This tail gas is transported to the tail gas condenser 4 via a pipeline, where it becomes condensate, which is then transported to the chloroform collection tank 2 via another pipeline. Because chloroform is insoluble in water, if the condensate contains water, it can be separated in the chloroform collection tank 2. The separated water can then be removed, and only the chloroform is recovered. Before recovery, a sample is taken through the first sampling valve installed on the chloroform collection tank 2, and the water content of the sample is tested to determine whether the water content of the recovered chloroform is acceptable. By recovering chloroform from the exhaust gas, the loss of chloroform raw materials can be reduced, and the difficulty of treating the waste gas can be lowered. The cooling medium used in the exhaust gas condenser 4 can be water at 5°C. This embodiment of the invention does not specifically limit the cooling medium used in the exhaust gas condenser 4.

[0036] For safety, a safety valve can be installed at the top of the chloroform dryer 1, and the overpressure relief port of the safety valve can be connected to the chloroform collection tank 2, so that the chloroform discharged from the safety valve of the chloroform dryer 1 due to overpressure can be collected in the chloroform collection tank 2, thereby further reducing the loss of raw materials.

[0037] The chloroform drying apparatus of this application embodiment is a continuously operating drying device in the entire system of chloroform storage and use, and does not affect the chloroform delivery rate in the entire system. It maintains the original chloroform feeding efficiency of the system while also improving the quality of the chloroform raw material supply to a certain extent. All related utilities—nitrogen, steam, and industrial water—are readily available, have low difficulty and cost of use, and are effectively recycled and subjected to related harmless treatment. The nitrogen heater used for activating the chloroform dryer has a built-in PLC temperature control cabinet, making operation relatively automated.

[0038] The chloroform drying apparatus of this application reduces the water content of chloroform by an average of 50 ppm after drying compared to before drying. The entire chloroform drying apparatus is a closed-loop system, effectively collecting and recycling all liquid materials and energy involved; the gaseous phase of the material is recovered and reused after condensation, and the exhaust gas is treated by an environmental protection device. Moreover, the chloroform drying process is continuous and does not affect the stability of the production process. As an additional intermediate step, it does not reduce production efficiency. The chloroform with high water content that was recovered to the chloroform collection tank from the original chloroform tank area via the exhaust gas condenser can be dried to a suitable standard using the drying circulation pump and then supplied to the downstream fluorination reaction unit, avoiding raw material waste.

[0039] The technical solution of the present invention has been described above with reference to the preferred embodiments shown in the accompanying drawings. However, it will be readily understood by those skilled in the art that the scope of protection of the present invention is obviously not limited to these specific embodiments. Without departing from the principles of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after such changes or substitutions will all fall within the scope of protection of the present invention.

Claims

1. A chloroform drying apparatus, characterized in that, include: A chloroform dryer for receiving chloroform raw materials and drying the chloroform raw materials; A chloroform collection tank, which is connected to the chloroform dryer via a pipeline, is used to collect the liquid material remaining in the chloroform dryer; A drying circulation pump, which is connected to the chloroform collection tank via a pipeline, is used to dry the liquid material collected in the chloroform collection tank; An activating gas supply device, which is connected to the chloroform dryer via a pipeline, is used to supply activating gas to the chloroform dryer; An exhaust gas condenser, connected to the chloroform dryer via a pipeline, is used to cool the exhaust gas in the chloroform dryer and to transport the condensate to the chloroform collection tank. The inlet pipeline of the chloroform dryer is connected to the outlet pipeline of the drying circulation pump.

2. The chloroform drying apparatus according to claim 1, characterized in that, The chloroform dryer is equipped with a molecular sieve.

3. The chloroform drying apparatus according to claim 1, characterized in that, Sampling devices are installed at the outlet and inlet of the chloroform dryer.

4. The chloroform drying apparatus according to claim 1, characterized in that, The chloroform collection tank is equipped with a first sampling valve.

5. The chloroform drying apparatus according to claim 1, characterized in that, A second sampling valve is installed at the outlet of the drying circulation pump.

6. The chloroform drying apparatus according to claim 1, characterized in that, It also includes an activation gas heater for heating the activation gas before delivering it to the chloroform dryer.

7. The chloroform drying apparatus according to claim 1, characterized in that, It also includes a steam pipeline, and the chloroform dryer is equipped with a jacket. The steam pipeline is connected to the jacket of the chloroform dryer for heating the chloroform dryer.

8. The chloroform drying apparatus according to claim 1, characterized in that, A safety valve is installed at the top of the chloroform dryer, and the overpressure relief port of the safety valve is connected to the chloroform collection tank.

9. The chloroform drying apparatus according to claim 1, characterized in that, The activating gas is nitrogen.

10. The chloroform drying apparatus according to claim 1, characterized in that, The cooling medium used in the exhaust gas condenser is water at 5°C.

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