CN112675667A - Recovery and absorption system and method for chloromethane in alkyl metal production process - Google Patents
Recovery and absorption system and method for chloromethane in alkyl metal production process Download PDFInfo
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Abstract
The invention discloses a system and a method for recovering and absorbing methyl chloride in the production process of alkyl metal, which comprises a buffer tank, a vacuum pump, an elution tower, a solvent pump, a condenser, a recovery tank and a connecting pipeline, wherein the buffer tank is connected with the vacuum pump through the connecting pipeline, the vacuum pump is connected with the elution tower through the connecting pipeline, the elution tower is connected with the condenser through the connecting pipeline, the condenser is connected with the recovery tank through the connecting pipeline, and the upper end and the lower end of the elution tower are also connected with the solvent pump through the connecting pipeline. The invention solves the problems that the existing chloromethane absorption device is incomplete in absorption, cannot carry out integrated recovery operation, causes resource waste, greatly reduces the efficiency, cannot ensure the operation safety, is complex to operate and is likely to generate unnecessary leakage.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a system and a method for recovering and absorbing methyl chloride in the production process of alkyl metal.
Background
Chloromethane is colorless and easy to liquefy gas, and is stored in a steel cylinder after being pressurized and liquefied. Belongs to organic halide. Slightly soluble in water, and easily soluble in chloroform, diethyl ether, ethanol, and acetone. Easy combustion, easy explosion and moderate harm. In the process of producing alkyl metal, chloromethane is used as a main raw material, and a rectifying tower is used for refining and separating in the production process. As the gas at the top of the rectifying tower is pressurized and recycled by two-stage condensation, more noncondensable gas still exists. In order to keep the normal operation of the rectifying tower, the non-condensable gas needs to be continuously discharged from the top of the rectifying tower. The high content of methyl chloride in the discharged gas causes the loss of raw materials and environmental pollution if the discharged gas is not recycled.
In the alkyl metal production process, the inevitable discharge of methyl chloride exists, the operation is complicated, and unnecessary leakage is likely to occur. In consideration of the pyrophoricity of the metal alkyls, the whole system needs to be isolated from air, and the harm can be avoided only in a better closed environment. The process for recovering the methyl chloride in the tail gas is roughly divided into a pressurized condensation type, a physical adsorption type and a direct combustion type. Basically, the recovery rate is low, so most of methyl chloride is not recycled and is directly discharged into the atmosphere, and environmental pollution and resource loss are caused.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a system and a method for recovering and absorbing methyl chloride in the production process of alkyl metal, which solve the problems that the existing methyl chloride absorption device cannot completely absorb the methyl chloride, cannot carry out integrated recovery operation, causes resource waste, greatly reduces the efficiency, cannot ensure the operation safety, is complex to operate and is likely to generate unnecessary leakage.
In order to achieve the purpose, the invention adopts the technical scheme that:
the utility model provides a recovery absorption system of methyl chloride in alkyl metal production process, includes buffer tank, vacuum pump, drip washing tower, solvent pump, condenser, recovery jar and connecting line, the buffer tank passes through connecting line and vacuum pump connection, the vacuum pump passes through connecting line and is connected with the drip washing tower, the drip washing tower passes through connecting line and is connected with the condenser, the condenser passes through connecting line and is connected with the recovery jar, the upper and lower both ends of drip washing tower still are connected with the solvent pump through connecting line.
The method for absorbing methyl chloride in the alkyl metal production process comprises the following steps,
(A) when the methyl chloride is absorbed, opening the first valve and closing the second valve; driven by a vacuum pump, the chloromethane enters the buffer tank from the gas inlet through the first check valve and the upper inlet valve;
(B) then the gas passes through a buffer tank gas outlet, passes through a third valve at the inlet of the vacuum pump, a fourth valve at the outlet of the vacuum pump and a second check valve, and then enters the leaching tower;
(C) the absorption liquid driven by the displacement pump flows out from the bottom of the leaching tower, passes through the absorption liquid outlet valve, enters the valve and returns to the top of the inner cavity of the leaching tower, and the chloromethane is subjected to hedging contact absorption.
In the method for absorbing methyl chloride in the alkyl metal production process, the absorption liquid used in the leaching tower (3) is one or a mixture of more of 1, 3-dichloropropane, white oil, ethyl acetoacetate, ethyl 2-chloroacetoacetate, 1, 2-dichloropropane, 1-dichlorobutane, 1, 2-dichlorobutane, 1, 3-dichlorobutane, 1, 4-dichlorobutane, 2-dichlorobutane and 2, 3-dichlorobutane.
In the method for absorbing methyl chloride in the alkyl metal production process, when the methyl chloride is absorbed, the refrigerant outlet valve and the refrigerant inlet valve are opened, and the temperature in the leaching tower is maintained at-25 ℃ to 0 ℃.
The method for recovering methyl chloride in the alkyl metal production process comprises the following steps,
(A) when the methyl chloride is recovered, opening the second valve and closing the first valve; closing the vacuum pump and the solvent pump, and closing the refrigerant outlet valve and the refrigerant inlet valve;
(B) and opening a heating medium outlet valve and a heating medium inlet valve, switching to a heating medium heating elution tower, gasifying the chloromethane, then passing through a second valve and a condenser inlet valve, cooling in a condenser, and then passing through a liquid receiving port of the recovery tank to enter the recovery tank.
In the method for recovering methyl chloride in the alkyl metal production process, the heating temperature of the leaching tower is 25-0 ℃ and the temperature of the condenser is-40 ℃ to-20 ℃ during the recovery of the methyl chloride.
In the recovery method of methyl chloride in the alkyl metal production process, the liquid level of the absorption liquid in the leaching tower is 1/3-2/3.
The invention has the beneficial effects that: the invention has safe and reliable operation, convenient operation and very good absorption and recovery effect, can greatly improve the absorption rate by utilizing an integrated condensation, leaching and absorption mode, directly switches the recovery mode, saves energy and cost, simplifies the operation process, improves the utilization rate and can better meet the use requirement.
Drawings
FIG. 1 is a process flow diagram of the present invention.
In the figure: 1. the device comprises a buffer tank, 2, a vacuum pump, 3, a leaching tower, 4, a solvent pump, 5, a condenser, 6, a recovery tank, 7, a connecting pipeline, 8, a gas inlet, 9, a first check valve, 10, an upper inlet valve, 11, a first valve, 12, a second valve, 13, a third valve, 14, a fourth valve, 15, a second check valve, 16, an absorption liquid outlet valve, 17, an absorption liquid inlet valve, 18, a refrigerant outlet valve, 19, a refrigerant inlet valve, 20, a heat medium outlet valve, 21, a heat medium inlet valve, 22 and a condenser inlet valve.
Detailed Description
In order to make the objects, 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 below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1: the utility model provides a recovery absorption system of methyl chloride in alkyl metal production process, including buffer tank 1, vacuum pump 2, drip washing tower 3, solvent pump 4, condenser 5, recovery tank 6 and connecting line 7, buffer tank 1 is connected with vacuum pump 2 through connecting line 7, vacuum pump 2 is connected with drip washing tower 3 through connecting line 7, drip washing tower 3 is connected with condenser 5 through connecting line 7, condenser 5 is connected with recovery tank 6 through connecting line 7, the upper and lower both ends of drip washing tower 3 still are connected with solvent pump 4 through connecting line 7.
A method for absorbing chloromethane in the production process of alkyl metal comprises the following steps,
(A1) when methyl chloride is absorbed, the first valve 11 is opened, and the second valve 12 is closed; driven by the vacuum pump 2, methyl chloride enters the buffer tank 1 from the gas inlet 8 through the first check valve 9 and the upper inlet valve 10;
(B1) then the gas passes through a gas outlet of the buffer tank 1, passes through a third valve 13 at an inlet of the vacuum pump 2, a fourth valve 14 at an outlet of the vacuum pump 2 and a second check valve 15, and then enters the leaching tower 3;
(C1) the absorption liquid driven by the displacement pump 4 flows out from the bottom of the elution tower 3, passes through the absorption liquid outlet valve 16, and then enters the valve 17 to return to the top of the inner cavity of the elution tower 3, so that the chloromethane is absorbed by the opposite contact.
The absorption liquid used in the leaching tower 3 is one or a mixture of more of 1, 3-dichloropropane, white oil, ethyl acetoacetate, ethyl 2-chloroacetoacetate, 1, 2-dichloropropane, 1-dichlorobutane, 1, 2-dichlorobutane, 1, 3-dichlorobutane, 1, 4-dichlorobutane, 2-dichlorobutane and 2, 3-dichlorobutane.
When the methyl chloride is absorbed, the refrigerant outlet valve 18 and the refrigerant inlet valve 19 are opened, and the temperature in the leaching tower 3 is maintained to be-25-0 ℃.
A method for recovering methyl chloride in the production process of alkyl metal comprises the following steps,
(A2) when methyl chloride is recovered, the second valve 12 is opened, and the first valve 11 is closed; closing the vacuum pump 2 and the solvent pump 4, and closing the refrigerant outlet valve 18 and the refrigerant inlet valve 19;
(B2) and opening a heat medium outlet valve 20 and a heat medium inlet valve 21, switching to a heat medium heating elution tower 3, gasifying methyl chloride, then passing through a second valve 12 and a condenser inlet valve 22, cooling in a condenser 5, and then passing through a liquid receiving port of the recovery tank to enter the recovery tank 6.
When the methyl chloride is recovered, the heating temperature of the leaching tower 3 is 25-0 ℃, and the temperature of the condenser 5 is-40 ℃ to-20 ℃.
The liquid level of the absorption liquid in the leaching tower 3 is 1/3-2/3.
The upper part of the leaching tower is of a spraying structure, the absorbent is sprayed downwards from a top h port through a solvent pump B, chloromethane enters from a middle d port, the lower part of the leaching tower is of an inner coil structure, and a cold and heat medium can be switched to be used for cooling or heating; the outside of the recovery tank is provided with a cold insulation measure polyurethane cotton and has a weighing function.
When methyl chloride is absorbed, 1, 3-dichloropropane is selected as absorption liquid, the adding amount is 500g, the position of an elution tower 2/3 is reached, a second valve 12 is opened, and a first valve 11 is closed; driven by the vacuum pump 2, methyl chloride enters the buffer tank 1 from the gas inlet 8 through the first check valve 9 and the upper inlet valve 10; then the gas passes through a gas outlet of the buffer tank 1, passes through a third valve 13 at an inlet of the vacuum pump 2, a fourth valve 14 at an outlet of the vacuum pump 2 and a second check valve 15, and then enters the leaching tower 3; the absorption liquid driven by the displacement pump 4 flows out from the bottom of the elution tower 3, passes through the absorption liquid outlet valve 16, the absorption liquid inlet valve 17 returns to the top of the inner cavity of the elution tower 3, the chloromethane is absorbed in a flushing contact manner, the refrigerant outlet valve 18 and the refrigerant inlet valve 19 are opened, the temperature in the elution tower is maintained at-20 ℃, the chloromethane enters 20g, and the weight of the absorption liquid is 519.8 g. Absorbs 19.8g of chloromethane, and the absorptivity of the chloromethane is 99 percent.
When methyl chloride is recovered, the second valve 12 is opened, and the first valve 11 is closed; and (3) closing the vacuum pump 2 and the solvent pump 4, closing the refrigerant outlet valve 18 and the refrigerant inlet valve 19, opening the heat medium outlet valve 20 and the heat medium inlet valve 21, switching to a heat medium heating elution tower 3, gasifying the methyl chloride, then passing through a second valve 12 and a condenser inlet valve 22, cooling the gasified methyl chloride in the condenser 5, and then passing through a liquid receiving port of the recovery tank to enter the recovery tank, wherein the heating temperature of the elution tower is 30 ℃, the temperature of the condenser is-30 ℃, weighing 18.9g of the methyl chloride in the recovery tank, and the recovery rate of the methyl chloride is 95.5%.
In conclusion, when the device is used, the operation is safe and reliable, the operation is convenient and fast, the absorption and recovery effects are very good, the absorption rate can be greatly improved by utilizing an integrated condensing, leaching and absorbing mode, the recovery mode is directly switched, the energy and the cost are saved, the operation flow is simplified, the utilization rate is improved, and the use requirement can be better met.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (7)
1. A recovery absorption system of methyl chloride in alkyl metal production process which characterized in that: including buffer tank (1), vacuum pump (2), drip washing tower (3), solvent pump (4), condenser (5), recovery jar (6) and connecting line (7), buffer tank (1) is connected with vacuum pump (2) through connecting line (7), vacuum pump (2) are connected with drip washing tower (3) through connecting line (7), drip washing tower (3) are connected with condenser (5) through connecting line (7), condenser (5) are connected with recovery jar (6) through connecting line (7), the upper and lower both ends of drip washing tower (3) still are connected with solvent pump (4) through connecting line (7).
2. The method of claim 1 for absorbing methyl chloride during metal alkyl production, wherein the method comprises the following steps: comprises the following steps of (a) carrying out,
(A1) when the methyl chloride is absorbed, the first valve (11) is opened, and the second valve (12) is closed; driven by a vacuum pump (2), methyl chloride enters a buffer tank (1) from a gas inlet (8) through a first check valve (9) and an upper inlet valve (10);
(B1) then the gas passes through a gas outlet of the buffer tank (1), passes through a third valve (13) at an inlet of the vacuum pump (2), a fourth valve (14) at an outlet of the vacuum pump (2) and a second check valve (15), and then enters the leaching tower (3);
(C1) the absorption liquid driven by the displacement pump (4) flows out from the bottom of the elution tower (3), passes through the absorption liquid outlet valve (16), enters the valve (17) to return to the top of the inner cavity of the elution tower (3), and is used for carrying out hedging contact absorption on the chloromethane.
3. The method of claim 2 for absorbing methyl chloride during the production of metal alkyls, wherein: the absorption liquid used in the leaching tower (3) is one or a mixture of more of 1, 3-dichloropropane, white oil, ethyl acetoacetate, ethyl 2-chloroacetoacetate, 1, 2-dichloropropane, 1-dichlorobutane, 1, 2-dichlorobutane, 1, 3-dichlorobutane, 1, 4-dichlorobutane, 2-dichlorobutane and 2, 3-dichlorobutane.
4. The method of claim 2 for absorbing methyl chloride during the production of metal alkyls, wherein: and when the chloromethane is absorbed, opening a refrigerant outlet valve (18) and a refrigerant inlet valve (19) and maintaining the temperature in the leaching tower (3) to be-25-0 ℃.
5. The process according to claim 1, wherein the recovery of methyl chloride during the production of metal alkyls comprises: comprises the following steps of (a) carrying out,
(A2) when methyl chloride is recovered, the second valve (12) is opened, and the first valve (11) is closed; closing the vacuum pump (2) and the solvent pump (4), and closing a refrigerant outlet valve (18) and a refrigerant inlet valve (19);
(B2) and (3) opening a heat medium outlet valve (20) and a heat medium inlet valve (21), switching to a heat medium heating elution tower (3), gasifying methyl chloride, then passing through a second valve (12) and a condenser inlet valve (22), entering a condenser (5) for cooling, and then entering a recovery tank (6) through a liquid receiving port of the recovery tank.
6. The system for recovering and absorbing methyl chloride in the process of producing alkyl metal according to claim 6, which is characterized in that: when the methyl chloride is recovered, the heating temperature of the leaching tower (3) is 25-0 ℃, and the temperature of the condenser (5) is-40 ℃ to-20 ℃.
7. The system for recovering and absorbing methyl chloride in the process of producing alkyl metal according to claim 6, which is characterized in that: the liquid level of the absorption liquid in the leaching tower (3) is 1/3-2/3.
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Application publication date: 20210420 |