阅读说明：本技术 一种超高纯度四氯化碳的提纯方法及提纯设备 (Purification method and purification equipment of ultrahigh-purity carbon tetrachloride ) 是由 周巧荣 张亚峰 沈爱萍 于 2021-06-30 设计创作，主要内容包括：本发明公开了一种超高纯度四氯化碳的提纯方法,一,首先经过四氯化碳的精馏塔(1)进行初次精馏；二,然后连续出料依次进入四氯提纯相分离器(5)和四氯提纯共沸塔(6)进行碱洗共沸处理后,得到高纯度的四氯化碳产品进入高纯四氯贮槽(7)。本发明公开了一种超高纯度四氯化碳的提纯设备,它主要包括精馏塔(1)和提纯塔(4),提纯塔(4)底部的出料口Ⅲ依次经过四氯提纯塔釜冷却器Ⅰ(18)、四氯提纯塔釜泵(19)、四氯提纯碱洗中和泵(20)与四氯提纯相分离器(5)的进口相连通,四氯提纯相分离器(5)的出口依次经过四氯提纯共沸进料泵Ⅲ(21)、四氯提纯共沸塔(6)与高纯四氯贮槽(7)相连通。(The invention discloses a purification method of ultrahigh-purity carbon tetrachloride, which comprises the following steps of firstly, carrying out primary rectification through a rectification tower (1) of the carbon tetrachloride; and secondly, continuously discharging the carbon tetrachloride, and sequentially feeding the carbon tetrachloride into a tetrachloro purification phase separator (5) and a tetrachloro purification azeotropic tower (6) for alkali washing azeotropic treatment to obtain a high-purity carbon tetrachloride product, and feeding the high-purity carbon tetrachloride product into a high-purity tetrachloro storage tank (7). The invention discloses a purifying device of ultra-high purity carbon tetrachloride, which mainly comprises a rectifying tower (1) and a purifying tower (4), wherein a discharge hole III at the bottom of the purifying tower (4) is communicated with an inlet of a tetrachloro purifying phase separator (5) through a tetrachloro purifying tower kettle cooler I (18), a tetrachloro purifying tower kettle pump (19) and a tetrachloro purifying alkali washing neutralizing pump (20) in sequence, and an outlet of the tetrachloro purifying phase separator (5) is communicated with a high-purity tetrachloro storage tank (7) through a tetrachloro purifying azeotropic feed pump III (21) and a tetrachloro purifying azeotropic tower (6) in sequence.)

1. A method for purifying ultrahigh-purity carbon tetrachloride comprises the following steps:

firstly, carrying out primary rectification through a rectifying tower (1) of carbon tetrachloride: crude carbon tetrachloride is pumped into the rectifying tower (1) through a feeding pump I (23) and continuously fed into the rectifying tower (1), a control valve (2) is arranged at the inlet of the rectifying tower (1), and the control valve (2) regulates and controls the flow of the carbon tetrachloride entering the rectifying tower (1);

step two, then a steam valve of the reboiler I (3) is adjusted to heat the tower kettle of the rectifying tower (1), the tower top temperature of the rectifying tower (1) is controlled between 75 ℃ and 78 ℃, the tower top pressure of the rectifying tower (1) is 0.005MPa, the reflux ratio is controlled between 4.5 and 5.5, when the component analysis of the material at the top of the tower reaches 99.5 percent, the material is extracted and enters a purifying tower (4), the pressure at the top of the purifying tower (4) is 0.005MPa, the temperature is controlled at 76 ℃, the gap discharging is carried out in the product at the top of the tower, the content of 1, 2-dichloroethane is controlled to be less than or equal to 15 percent, so that the content of light components in the components is controlled to be less than or equal to 15 percent, the components in the tower bottom are qualified by analysis, the content of carbon tetrachloride is more than 99.9 percent, and then the materials are continuously discharged and sequentially enter a tetrachloro purification phase separator (5) and a tetrachloro purification azeotropic tower (6) for alkali washing azeotropic treatment, and a high-purity carbon tetrachloride product is obtained and enters a high-purity tetrachloro storage tank (7).

2. The purification method of ultra-high purity carbon tetrachloride according to claim 1, wherein the flow rate of carbon tetrachloride into the rectifying column (1) is controlled to be 1.0 to 1.5m by the control valve (2) in the first step³/h。

3. The purification method of ultra-high purity carbon tetrachloride according to claim 1, wherein the reflux ratio in the second step is controlled to 5.

4. The purification method of ultra-high purity carbon tetrachloride according to claim 1, wherein the temperature of the top of the rectifying column (1) in the second step is controlled to 76 ℃.

5. A purifying device of ultra-high purity carbon tetrachloride is characterized by mainly comprising a rectifying tower (1), wherein a feed inlet I (8) is arranged on the side surface of the rectifying tower (1), a feed pipe is connected to the feed inlet I (8), one end of the feed pipe is connected with a feed pump I (23), the other end of the feed pipe is communicated with the feed inlet I (8) of the rectifying tower, a discharge outlet I (9) at the top of the rectifying tower (1) is communicated with an inlet of a collecting groove I (10), a tower top condenser I (11) is arranged between the discharge outlet I (9) of the rectifying tower (1) and the inlet of the collecting groove I (10), an outlet of the collecting groove I (10) is communicated with an inlet of a tetrachloro finished product groove (12), a reflux pump I (13) is arranged between the outlet of the collecting groove I (10) and the inlet of the tetrachloro finished product groove (12), an outlet of the tetrachloro finished product groove (12) is communicated with a feed inlet II (14) of the purifying tower (4), a tetrachloro purification feed pump II (15) is arranged between the outlet of the tetrachloro finished product tank (12) and the feed inlet II (14) of the purification tower (4), a top discharge port II (16) of the purification tower (4) is communicated with the inlet of a tetrachloro purification tower top collecting tank II (17), a tower top condenser II (18) is arranged between the discharge port II of the top of the purification tower (4) and the inlet of the tetrachloro purification tower top collecting tank II (17), the outlet of the tetrachloro purification tower top collecting tank II (17) is communicated with the reflux port at the upper part of the purification tower (4) through a reflux pump II (24), a discharge port III at the bottom of the purification tower (4) is communicated with the inlet of a tetrachloro purification phase separator (5) through a tetrachloro purification tower kettle cooler I (18), a tetrachloro purification tower kettle pump (19) and a tetrachloro purification alkali washing neutralizing pump (20) in sequence, the outlet of the tetrachloro purification phase separator (5) is communicated with the inlet of the tetrachloro purification azeotropic purification tower (6) through a tetrachloro azeotropic purification feed pump III (21) in sequence, the outlet of the tetrachloro purification azeotropic tower (6) is communicated with a high-purity tetrachloro storage tank (7).

6. The apparatus for purifying ultra-high purity carbon tetrachloride according to claim 5, wherein the feed pipe is provided with a control valve (2) at a position close to the feed inlet I (8) at the side of the rectification column (1).

7. The purifying apparatus of ultra-high purity carbon tetrachloride according to claim 5, wherein a cooler II (22) is provided at the bottom of the rectifying tower (1), and a reboiler I (3) is provided between the cooler II (22) and the rectifying tower (1).

8. The apparatus for purifying ultra-high purity carbon tetrachloride according to claim 5, wherein a reboiler II (23) for the purification column is provided between the cooler I (18) of the tetrachloro purification column and the side of the purification column (4).

9. The apparatus for purifying ultra-high purity carbon tetrachloride according to claim 5, wherein a tetrachloro purification azeotropic column condenser III (24) is provided at the top of said tetrachloro purification azeotropic column (6).

10. The apparatus for purifying ultra-high purity carbon tetrachloride according to claim 5, wherein a condenser IV (25) is provided between the lower part of said tetrachloro purification azeotropic tower (6) and the high purity tetrachloro storage tank (7).

Technical Field

The invention relates to a purification method and purification equipment of ultrahigh-purity carbon tetrachloride.

Background

At present, after the byproduct carbon tetrachloride of the methane chloride device is rectified, the content of the obtained carbon tetrachloride after removing heavy components does not exceed 99.5 percent, and the requirement of high purity can not be met. The crude carbon tetrachloride is treated by a rectifying tower, so that the main content of the carbon tetrachloride is not more than 99.5 percent after high-boiling-point substances such as trichloroethylene, tetrachloroethylene and the like are removed, and the requirement of high purity cannot be met. After rectification, the finished carbon tetrachloride product mainly contains trace amounts of dichloromethane and trichloromethane, bromochloromethane, 1, 2-dichloroethane, dichloromethane and trichloromethane, and bromochloromethane, wherein the boiling point temperature of the bromochloromethane is lower than that of tetrachloro, the boiling point temperature of the 1, 2-dichloroethane is 83 ℃ and higher than that of the carbon tetrachloride, but the boiling point is reduced after the 1, 2-dichloroethane can form an azeotrope with the carbon tetrachloride, the carbon tetrachloride is still a light component, and the carbon tetrachloride is accumulated on the top of the tower and is difficult to remove, so that the main content is influenced.

Disclosure of Invention

The invention provides a purification method and purification equipment of ultrahigh-purity carbon tetrachloride, which remove trace impurity in the carbon tetrachloride to obtain a high-purity carbon tetrachloride product.

The invention adopts the following technical scheme: a method for purifying ultrahigh-purity carbon tetrachloride comprises the following steps: firstly, carrying out primary rectification through a rectifying tower of carbon tetrachloride: crude carbon tetrachloride is pumped into the rectifying tower through a feeding pump I and is continuously fed into the rectifying tower, a control valve is arranged at the inlet of the rectifying tower and regulates the flow of the carbon tetrachloride entering the rectifying tower; and step two, a steam valve of the reboiler I is adjusted to heat a tower kettle of the rectifying tower, the tower top temperature of the rectifying tower is controlled to be 75-78 ℃, the tower top pressure of the rectifying tower is 0.005MPa, the reflux ratio is controlled to be 4.5-5.5, when the component analysis of a material at the tower top reaches 99.5%, the material is extracted and enters a purifying tower, the tower top pressure of the purifying tower is 0.005MPa, the temperature is controlled to be 76 ℃, the intermittent discharging of which the content of 1 and 2-dichloroethane is controlled to be less than or equal to 15% in a product at the tower top is performed, so that the content of light components in the component is controlled to be less than or equal to 15%, the component analysis of the tower kettle is qualified, the content of carbon tetrachloride is greater than 99.9%, and then the continuous discharging is sequentially performed with alkali washing azeotropic treatment in a tetrachloro purifying phase separator and a tetrachloro purifying tower, and the high-purity tetrachloro carbon tetrachloride product is obtained and enters a high-purity tetrachloro storage tank.

In the first step of the invention, the flow of carbon tetrachloride entering the rectifying tower is controlled to be 1.0-1.5m by the control valve³H is used as the reference value. In the second step of the invention, the reflux ratio is controlled to be 5. In the second step of the invention, the temperature at the top of the rectifying tower is controlled at 76 ℃.

The invention discloses a purifying device of ultra-high purity carbon tetrachloride, which mainly comprises a rectifying tower, wherein a feed inlet I is arranged on the side surface of the rectifying tower, a feed pipe is connected with the feed inlet I, one end of the feed pipe is connected with a feed pump I, the other end of the feed pipe is communicated with the feed inlet I of the rectifying tower, a discharge outlet I at the top of the rectifying tower is communicated with an inlet of a receiving tank I, a tower top condenser I is arranged between the discharge outlet I of the rectifying tower and the inlet of the receiving tank I, an outlet of the receiving tank I is communicated with an inlet of a tetrachloro finished product tank, a reflux pump I is arranged between an outlet of the receiving tank I and the inlet of the tetrachloro finished product tank, an outlet of the tetrachloro finished product tank is communicated with a feed inlet II of the purifying tower, a tetrachloro purifying feed pump II is arranged between the outlet of the tetrachloro finished product tank and the feed inlet of the purifying tower, a discharge outlet II at the top of the purifying tower is communicated with the inlet of the tetrachloro purifying tower top receiving tank II, and a tower top condenser II is arranged between a discharge hole II at the top of the purification tower and an inlet of a tetrachloro purification tower top collecting groove II, an outlet of the tetrachloro purification tower top collecting groove II is communicated with a reflux port at the upper part of the purification tower through a reflux pump II, a discharge hole III at the bottom of the purification tower is communicated with an inlet of a tetrachloro purification phase separator through a tetrachloro purification tower kettle cooler I, a tetrachloro purification tower kettle pump and a tetrachloro purification alkali washing neutralization pump in sequence, an outlet of the tetrachloro purification phase separator is communicated with an inlet of a tetrachloro purification azeotropic tower through a tetrachloro purification azeotropic feed pump III in sequence, and an outlet of the tetrachloro purification azeotropic tower is communicated with a high-purity tetrachloro storage tank.

And a control valve is arranged at a position, close to the feed inlet I on the side surface of the rectifying tower, on the feed pipe. The bottom of the rectifying tower is provided with a cooler II, and a reboiler I is arranged between the cooler II and the rectifying tower. And a purification tower reboiler II is arranged between the tetrachloro purification tower kettle cooler I and the side surface of the purification tower. And a tetrachloro purification azeotropic tower condenser III is arranged at the top of the tetrachloro purification azeotropic tower. And a condenser IV is arranged between the lower part of the tetrachloro purification azeotropic tower and the high-purity tetrachloro storage tank.

The invention has the following beneficial effects: after the technical scheme is adopted, the method and the equipment can obtain the carbon tetrachloride with the content of 99.5% by the rectifying tower aiming at that the 1, 2-dichloroethane in the crude carbon tetrachloride can form an azeotrope with the carbon tetrachloride, and then obtain the carbon tetrachloride with the content of 99.9% by the purifying tower, thereby realizing the continuous and removal of impurities with different properties, removing trace impurities in the carbon tetrachloride and obtaining the high-purity carbon tetrachloride. The equipment adopted by the invention can effectively purify twice, not only can further improve the purification effect, but also has simple and convenient operation and further improves the purification efficiency.

Drawings

FIG. 1 is a schematic structural diagram of the present invention.

Detailed Description

In figure 1, the invention provides a purifying device of ultra-high purity carbon tetrachloride, which mainly comprises a rectifying tower 1, wherein a feed inlet I8 is arranged on the side surface of the rectifying tower 1, a feed pipe is connected with the feed inlet I8, a control valve 2 is arranged on the feed pipe at a position close to the feed inlet I8 on the side surface of the rectifying tower 1, one end of the feed pipe is connected with a feed pump I23, the other end of the feed pipe is communicated with the feed inlet I8 of the rectifying tower, a cooler II 22 is arranged at the bottom of the rectifying tower 1, a reboiler I3 is arranged between the cooler II 22 and the rectifying tower 1, a discharge outlet I9 at the top of the rectifying tower 1 is communicated with an inlet of a collecting tank I10, a tower top condenser I11 is arranged between the discharge outlet I9 of the rectifying tower 1 and the inlet of the collecting tank I10, an outlet of the collecting tank I10 is communicated with an inlet of a tetrachloro finished product tank 12, a reflux pump I13 is arranged between an outlet of the collecting tank I10 and an inlet of the tetrachloro finished product tank 12, an outlet of the tetrachloro finished product tank 12 is communicated with a feed inlet II 14 of the purifying tower 4, a tetrachloro purification feed pump II 15 is arranged between the outlet of the tetrachloro finished product tank 12 and the feed inlet II 14 of the purifying tower 4, a top discharge outlet II 16 of the purifying tower 4 is communicated with an inlet of a top collecting tank II 17 of the tetrachloro purifying tower, a tower top condenser II 18 is arranged between the discharge outlet II of the top of the purifying tower 4 and the inlet of the top collecting tank II 17 of the tetrachloro purifying tower, an outlet of the top collecting tank II 17 of the tetrachloro purifying tower is communicated with a reflux port at the upper part of the purifying tower 4 through a reflux pump II 24, a discharge outlet III at the bottom of the purifying tower 4 is sequentially communicated with an inlet of a tetrachloro purifying tower kettle cooler I18, a tetrachloro purifying tower kettle pump 19, a tetrachloro purifying alkali washing neutralization pump 20 and a tetrachloro purifying phase separator 5, a reboiler II 23 is arranged between the tetrachloro purifying tower kettle cooler I18 and the side surface of the purifying tower 4, an outlet of the tetrachloro purification phase separator 5 is communicated with an inlet of a tetrachloro purification azeotropic tower 6 through a tetrachloro purification azeotropic feed pump III 21 in sequence, a tetrachloro purification azeotropic tower condenser III 24 is arranged at the top of the tetrachloro purification azeotropic tower 6, an outlet of the tetrachloro purification azeotropic tower 6 is communicated with a high-purity tetrachloro storage tank 7, and a condenser IV 25 is arranged between the lower part of the tetrachloro purification azeotropic tower 6 and the high-purity tetrachloro storage tank 7.

The invention also discloses a purification method of the ultrahigh-purity carbon tetrachloride, which comprises the following steps: firstly, carrying out primary rectification through a rectifying tower 1 of carbon tetrachloride: crude carbon tetrachloride is pumped into a rectifying tower 1 through a feeding pump I23 and continuously fed into the rectifying tower 1, a control valve 2 is arranged at an inlet of the rectifying tower 1, the control valve 2 regulates and controls the flow of the carbon tetrachloride entering the rectifying tower 1, and in the first step, the control valve 2 controls the flow of the carbon tetrachloride entering the rectifying tower 1 to be 1.0-1.5m³H is used as the reference value. (ii) a Step two, then adjusting a steam valve of a reboiler I3 to heat a tower kettle of a rectifying tower 1, controlling the temperature of the tower top of the rectifying tower 1 to be between 75 and 78 ℃, controlling the temperature of the tower top of the rectifying tower 1 to be 76 ℃ in the embodiment, controlling the pressure of the tower top of the rectifying tower 1 to be 0.005MPa, controlling the reflux ratio to be 4.5 to 5.5, controlling the reflux ratio to be 5 in the step two in the embodiment, when the component analysis of the material at the tower top reaches 99.5%, extracting the material to enter a purifying tower 4, controlling the pressure of the tower top of the purifying tower 4 to be 0.005MPa, controlling the temperature to be 76 ℃, controlling the content of 1 and 2-dichloroethane in the product at the tower top to be less than or equal to 15% to discharge in a clearance way that the content of light components in the components is controlled to be less than or equal to 15%, the component analysis of the tower kettle is qualified, controlling the content of carbon tetrachloride to be more than 99.9%, then continuously discharging the material to enter a tetrachloro purifying phase separator 5 and a tetrachloro purifying tower 6 to be subjected to undergo alkali azeotropic treatment, the obtained high-purity carbon tetrachloride enters a high-purity tetrachloro storage tank 7.