Purification method of high-purity organic solvent carbon tetrachloride

Abstract

The invention discloses a purification method of high-purity organic solvent carbon tetrachloride, which comprises the following steps: S100, configuring a multi-stage extractive distillation tower system which comprises a first extractive distillation tower, a second extractive distillation tower, a third extractive distillation tower and an extractant recovery tower which are connected in series, pumping crude carbon tetrachloride into the distillation towers through a feeding pump, continuously feeding, and recycling the extractant from the first extractive distillation tower to the second extractive distillation tower; the flow is regulated and controlled through the control valve; s200, setting the working temperature of a reboiler in a first extractive distillation tower to be 120 DEG C, setting the working temperature of a reboiler in a third extractive distillation tower to be 110 DEG C, setting the working temperature of a reboiler in an extraction agent recovery tower to be 100 DEG C, and respectively carrying out primary purification, deep refining and solvent recovery of carbon tetrachloride, and carrying out three times of cyclic operation; and S300, arranging a nano filter, treating effluent from the third extractive distillation tower, and successfully removing trace organic compounds by setting the size of a filter hole to be 1nm. According to the invention, the purification efficiency of carbon tetrachloride is obviously improved, the energy consumption required by unit yield is greatly reduced, and the production cost is saved.

Description

Technical Field

[0001] The invention relates to the technical field of carbon tetrachloride processing, in particular to a method for purifying high-purity organic solvent carbon tetrachloride. Background Art

[0002] Carbon tetrachloride is mainly used as an excellent solvent, dry cleaning agent, fire extinguishing agent, refrigerant, leaching agent for spices, and pesticides. Traditional methods for purifying carbon tetrachloride mainly use extraction or distillation processes. The distillation method is a method of separating carbon tetrachloride from a mixed system by utilizing the difference in boiling points between carbon tetrachloride and impurities; the extraction method is a method of using an extractant to effectively extract impurities from carbon tetrachloride. However, this method often faces problems such as incomplete removal of impurities, low purification efficiency, and high energy consumption. With the increasingly urgent demand for the chemical industry to transform towards green and environmental protection, how to improve purification efficiency while reducing energy consumption has become a key issue that needs to be solved. Summary of the invention

[0003] The invention aims to solve the main problems existing in the traditional purification method, that is, it is difficult to completely remove impurities during the purification process of carbon tetrachloride, the purification cycle is long and the energy consumption is high, and these problems limit the technical problems of production efficiency and economic benefits.

[0004] To achieve the purpose of the present invention, the present invention adopts the following technical solutions:

[0005] A method for purifying high-purity organic solvent carbon tetrachloride comprises the following steps:

[0006] S100: configuring a multi-stage extractive distillation tower system, including a first extractive distillation tower, a second extractive distillation tower, a third extractive distillation tower, and an extractant recovery tower arranged in series, wherein crude carbon tetrachloride is pumped into the distillation tower through a feed pump, and the feed is continuously fed, and the flow rate is regulated by a control valve;

[0007] S200: The first extractive distillation tower is set to have a reboiler operating temperature of 120° C., the third extractive distillation tower is set to have a reboiler operating temperature of 110° C., and the extractant recovery tower is set to have a reboiler operating temperature of 100° C., and preliminary purification, deep refining and solvent recovery of carbon tetrachloride are respectively performed, and the operation is repeated three times;

[0008] S300: A nano filter is set to process the effluent from the third extractive distillation tower, and trace organic compounds are successfully removed by setting the filter pore size to 1 nm.

[0009] In some embodiments, in step S100, the crude carbon tetrachloride flow rate is controlled at 1.3-1.5 m 3 / h, continuously feeding into the distillation tower and heating by steam.

[0010] In some embodiments, in step S200, when the component analysis of the top material reaches 99.5%, the material is withdrawn and enters the purification tower. The top pressure of the purification tower is 0.005 MPa and the temperature is controlled at 76°C.

[0011] In some embodiments, an ultrasonic transducer and a microwave generator are integrated inside the extractive distillation tower to optimize the mass transfer process and enhance the dissolution rate and separation efficiency of impurities.

[0012] In some embodiments, the ultrasonic transducer frequency is preferably 20kHz-50kHz, and the microwave power is preferably 600W-1200W.

[0013] In some embodiments, after the components of the extractive distillation tower are analyzed to be qualified, the carbon tetrachloride content is greater than 99.9%, and the continuous discharge enters the tetrachloride purification phase separator and the tetrachloride purification azeotropic tower in turn for alkali washing and azeotropic treatment to obtain a high-purity carbon tetrachloride product.

[0014] In some embodiments, in step S200, the volume ratio of the extractant to carbon tetrachloride is controlled within a certain range, for example, between 1:3 and 1:5.

[0015] In some embodiments, in each extractive distillation tower, the temperature adjustment range is ±1°C, and the pressure accuracy is controlled within ±0.05MPa to ensure the stability of temperature and pressure during the distillation process.

[0016] In some embodiments, in step S200, the tower top temperature is controlled between 75-78° C., the tower top pressure is 0.005 MPa, and the reflux ratio is controlled between 4.5-5.5.

[0017] The present invention provides a method for purifying high-purity organic solvent carbon tetrachloride, which has the following advantages:

[0018] The method for purifying high-purity organic solvent carbon tetrachloride provided in this embodiment significantly improves the purification efficiency of carbon tetrachloride, greatly reduces the energy consumption required per unit output, and saves production costs. The high-purity purification of carbon tetrachloride is achieved, reaching a purity level of more than 99.99%, broadening its potential in high-precision industrial applications. DETAILED DESCRIPTION

[0019] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described in combination with the present invention below. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0020] The present embodiment provides a method for purifying carbon tetrachloride of a high-purity organic solvent, comprising the following steps: S100: configuring a multi-stage extractive distillation tower system, including a first extractive distillation tower, a second extractive distillation tower, a third extractive distillation tower, and an extractant recovery tower arranged in series, and the crude carbon tetrachloride is pumped into the distillation tower through a feed pump, continuously fed, and the flow is regulated by a control valve; S200: the first extractive distillation tower sets the reboiler working temperature to 120°C, the third extractive distillation tower sets the reboiler working temperature to 110°C, and the extractant recovery tower sets the reboiler working temperature to 100°C, respectively, and the carbon tetrachloride is preliminarily purified, deeply refined, and the solvent is recovered, and three cycles are performed; S300: a nanofilter is set to process the effluent from the third extractive distillation tower, and the trace organic compounds are successfully removed by setting the filter pore size to 1nm. Through the innovative design of multi-stage series connection, the purification efficiency and product quality of carbon tetrachloride are significantly enhanced. The design of the multi-stage series extraction distillation tower system realizes step-by-step separation and effectively improves the purity of carbon tetrachloride.

[0021] Further, in step S100, the crude carbon tetrachloride flow rate is controlled at 1.3-1.5 m 3 / h, continuously feeding into the distillation tower and heating it with steam to ensure continuous supply.

[0022] Furthermore, in step S200, when the component analysis of the tower top material reaches 99.5%, the material is extracted and enters the purification tower. The top pressure of the purification tower is 0.005 MPa and the temperature is controlled at 76°C.

[0023] Furthermore, an ultrasonic transducer and a microwave generator are integrated inside the extractive distillation tower to optimize the mass transfer process and enhance the dissolution rate and separation efficiency of impurities. The integrated ultrasonic and microwave technologies enhance the mass transfer process and accelerate the removal of impurities. The ultrasonic transducer frequency is preferably 20kHz-50kHz, and the microwave power is preferably 600W-1200W. Under the same conditions as the basic example, the purity of carbon tetrachloride is further improved and the purification cycle is shortened by about 20%.

[0024] Furthermore, after the components of the extractive distillation tower are analyzed to be qualified, the carbon tetrachloride content is greater than 99.9%, and the continuous discharge enters the tetrachloride purification phase separator and the tetrachloride purification azeotropic tower in turn for alkali washing and azeotropic treatment to obtain a high-purity carbon tetrachloride product.

[0025] Furthermore, in step S200, controlling the volume ratio of the extractant to carbon tetrachloride within a certain range, for example, between 1:3 and 1:5, can significantly improve the purification effect.

[0026] Furthermore, in each extractive distillation tower, the temperature adjustment range is ±1°C and the pressure accuracy is controlled at ±0.05MPa to ensure the stability of temperature and pressure during the distillation process.

[0027] Furthermore, in step S200, the tower top temperature is controlled between 75-78°C, the tower top pressure is 0.005MPa, and the reflux ratio is controlled between 4.5-5.5.

[0028] The method for purifying high-purity organic solvent carbon tetrachloride provided in this embodiment significantly improves the purification efficiency of carbon tetrachloride, greatly reduces the energy consumption required per unit output, and saves production costs. The high-purity purification of carbon tetrachloride is achieved, reaching a purity level of more than 99.99%, broadening its potential in high-precision industrial applications.

[0029] The technical principle of the present invention is described above in combination with specific embodiments, but it should be noted that the above descriptions are only for explaining the principle of the present invention and cannot be interpreted as a specific limitation on the protection scope of the present invention in any way. Based on the explanation here, technicians in this field can think of other specific embodiments or equivalent replacements of the present invention without paying creative work, which will fall within the protection scope of the present invention.

Claims

1. A method for purifying high-purity organic solvent carbon tetrachloride, characterized in that: The following steps are involved: S100: configuring a multi-stage extractive distillation tower system, including a first extractive distillation tower, a second extractive distillation tower, a third extractive distillation tower, and an extractant recovery tower arranged in series, wherein crude carbon tetrachloride is pumped into the distillation tower through a feed pump, and the feed is continuously fed, and the flow rate is regulated by a control valve; S200: The first extractive distillation tower is set to have a reboiler operating temperature of 120° C., the third extractive distillation tower is set to have a reboiler operating temperature of 110° C., and the extractant recovery tower is set to have a reboiler operating temperature of 100° C., and preliminary purification, deep refining and solvent recovery of carbon tetrachloride are respectively performed, and the operation is repeated three times; S300: A nano filter is set to process the effluent from the third extractive distillation tower, and trace organic compounds are successfully removed by setting the filter pore size to 1 nm.

2. The method for purifying high-purity organic solvent carbon tetrachloride according to claim 1, characterized in that: In step S100, the crude carbon tetrachloride flow rate is controlled at 1.3-1.5 m 3 / h, continuously feeding into the distillation tower and heating by steam.

3. The method for purifying high-purity organic solvent carbon tetrachloride according to claim 2, characterized in that: In step S200, when the component analysis of the material at the top of the tower reaches 99.5%, the material is taken out and enters the purification tower. The pressure at the top of the purification tower is 0.005 MPa and the temperature is controlled at 76°C.

4. The method for purifying high-purity organic solvent carbon tetrachloride according to claim 3, characterized in that: The extractive distillation tower is integrated with ultrasonic transducers and microwave generators to optimize the mass transfer process and enhance the dissolution rate and separation efficiency of impurities.

5. The method for purifying high-purity organic solvent carbon tetrachloride according to claim 4, characterized in that: The ultrasonic transducer frequency is preferably 20kHz-50kHz, and the microwave power is preferably 600W-1200W.

6. The method for purifying high-purity organic solvent carbon tetrachloride according to claim 5, characterized in that: After the components of the extractive distillation tower are analyzed to be qualified, the carbon tetrachloride content is greater than 99.9%, and the continuous discharge enters the tetrachloride purification phase separator and the tetrachloride purification azeotropic tower in turn for alkali washing and azeotropic treatment to obtain a high-purity carbon tetrachloride product.

7. The method for purifying high-purity organic solvent carbon tetrachloride according to claim 6, characterized in that: In step S200, the volume ratio of the extractant to carbon tetrachloride is controlled within a certain range, for example, between 1:3 and 1:

5.

8. The method for purifying high-purity organic solvent carbon tetrachloride according to claim 7, characterized in that: In each extractive distillation tower, the temperature adjustment range is ±1°C and the pressure accuracy is controlled at ±0.05MPa to ensure the stability of temperature and pressure during the distillation process.

9. The method for purifying high-purity organic solvent carbon tetrachloride according to claim 8, characterized in that: In step S200, the tower top temperature is controlled between 75-78°C, the tower top pressure is 0.005MPa, and the reflux ratio is controlled between 4.5-5.5.