CN110540487A - System for purifying methyl chloride and method for treating organic matters in methyl chloride gas by substituted sulfuric acid adsorption - Google Patents
System for purifying methyl chloride and method for treating organic matters in methyl chloride gas by substituted sulfuric acid adsorption Download PDFInfo
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- CN110540487A CN110540487A CN201810522442.0A CN201810522442A CN110540487A CN 110540487 A CN110540487 A CN 110540487A CN 201810522442 A CN201810522442 A CN 201810522442A CN 110540487 A CN110540487 A CN 110540487A
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- Prior art keywords
- tower
- methyl chloride
- organic matter
- rectifying tower
- separator
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- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 title claims abstract description 228
- 229940050176 methyl chloride Drugs 0.000 title claims abstract description 81
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical class OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000001179 sorption measurement Methods 0.000 title claims description 10
- 239000005416 organic matter Substances 0.000 claims abstract description 76
- 239000007789 gas Substances 0.000 claims description 73
- 238000000926 separation method Methods 0.000 claims description 35
- 238000010992 reflux Methods 0.000 claims description 9
- 230000006835 compression Effects 0.000 claims description 5
- 238000007906 compression Methods 0.000 claims description 5
- 239000002912 waste gas Substances 0.000 claims description 5
- 239000010865 sewage Substances 0.000 claims description 4
- 238000004065 wastewater treatment Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 239000012530 fluid Substances 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 239000011368 organic material Substances 0.000 claims 2
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 4
- NEHMKBQYUWJMIP-NJFSPNSNSA-N chloro(114C)methane Chemical compound [14CH3]Cl NEHMKBQYUWJMIP-NJFSPNSNSA-N 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- 239000005562 Glyphosate Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000012824 chemical production Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 description 2
- 229940097068 glyphosate Drugs 0.000 description 2
- 239000002920 hazardous waste Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
the invention discloses a system for purifying methyl chloride, which comprises a gas compressor, a non-condensable gas separator, a methyl chloride rectifying tower condenser, a methyl chloride rectifying tower separator, an organic matter separating tower condenser, an organic matter rectifying tower separator, an organic matter separating tower reboiler, a methyl chloride rectifying tower reboiler and a methyl chloride rectifying tower, wherein the gas compressor is connected with the non-condensable gas separator, the non-condensable gas separator is connected with the methyl chloride rectifying tower, the methyl chloride rectifying tower is connected with the methyl chloride rectifying tower reboiler, the non-condensable gas separator, the methyl chloride rectifying tower separator and the organic matter separating tower, and the methyl chloride rectifying tower condenser is connected with the methyl chloride rectifying tower separator. The invention has wide application range, no sulfuric acid is generated in the treatment process, the loss of sulfuric acid is removed, the environmental protection problem of treating dangerous waste sulfuric acid is solved, the recovered organic matters are reused, and the economic benefit is improved.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a system for purifying chloromethane and a method for adsorbing and treating organic matters in chloromethane gas by substituted sulfuric acid.
Background
the technology (organic silicon and the like) taking methyl chloride as a target product or raw material in chemical production and the technology (such as the synthesis of glyphosate and the like) with methyl chloride by-products have the problem of purification of the methyl chloride. In the original process, sulfuric acid is used for adsorbing organic matters and water in methyl chloride when organic impurities in the methyl chloride are removed, and the methyl chloride is purified. The sulfuric acid is used as a consumable supplement, and the waste sulfuric acid is used for dangerous waste treatment. The use of sulfuric acid in the process causes that the process is not clean and complicated, the environmental protection requirement of waste acid treatment is high, and organic matters cannot be utilized. Therefore, a clean production process is urgently needed to replace a sulfuric acid adsorption method for purifying methyl chloride.
disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a system and a method for purifying chloromethane, so that no sulfuric acid is generated in the treatment process, the loss of sulfuric acid is removed, and the environmental protection problem of treating hazardous waste sulfuric acid is further solved. The recovered organic matters are reused, and the economic benefit is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
The invention discloses a system for purifying methyl chloride, which comprises a gas compressor, a non-condensable gas separator, a methyl chloride rectifying tower condenser, a methyl chloride rectifying tower separator, an organic matter separating tower condenser, an organic matter rectifying tower separator, an organic matter separating tower reboiler, a methyl chloride rectifying tower reboiler and a methyl chloride rectifying tower, wherein the gas compressor is connected with the non-condensable gas separator which is connected with the methyl chloride rectifying tower, the methyl chloride rectifying tower is connected with the methyl chloride rectifying tower reboiler, the non-condensable gas separator, the methyl chloride rectifying tower separator and the organic matter separating tower, the methyl chloride rectifying tower condenser is connected with the methyl chloride rectifying tower separator, the organic matter separating tower is connected with the organic matter separating tower reboiler, the organic matter separating tower condenser and the organic matter rectifying tower separator, the organic matter separation tower condenser is connected with the organic matter rectifying tower separator. The non-condensable gas separator, the chloromethane rectifying tower separator and the organic matter rectifying tower separator are all connected with a waste gas treatment device through exhaust pipes. The organic matter separation tower is connected with a wastewater treatment device through a sewage discharge pipe. The gas compressor is connected with a chloromethane feeding pipe.
The invention also discloses a method for adsorbing and treating organic matters in methyl chloride gas by using substituted sulfuric acid, which comprises the following steps:
S1, compressing to remove non-condensable gas:
S11, performing one-stage or multi-stage compression on the chloromethane gas containing the non-condensable gas, wherein a condenser is arranged behind each compression stage;
S12, performing membrane separation on the compressed gas, and discharging non-organic gas in the non-condensable gas;
s2, separation of methyl chloride:
S21, preheating methyl chloride and then feeding the preheated methyl chloride into a methyl chloride rectifying tower; preheating to 5-300 ℃ for feeding;
S22, pressurizing and controlling the chloromethane rectifying tower, wherein the pressure is 0.1-5.0 MPa; the top of the distillation tower is provided with a reflux condenser, a reflux tank, a reflux pump and a chloromethane rectifying tower; the rectifying tower is provided with two tower sections, namely a rectifying section and a stripping section, and is used for controlling the rectifying effect at the top and the bottom of the tower;
S23, a reboiler is arranged at the bottom of the tower to provide energy for the tower, and the bottom temperature is controlled to ensure that light components are not carried in the organic composition; the tower bottom enters an organic matter separation tower to separate the available components;
S3, recovering organic matters:
s31, feeding the fluid from the bottom of the chloromethane rectifying tower into an organic matter separation tower, taking out the organic matter from the top of the tower, and separating water from the bottom of the tower;
S32, recycling organic matters at the top of the tower, and enabling tower bottoms to enter a sewage treatment system.
Preferably, in the step S2, the temperature at the top of the organic matter separation tower is 30 to 120 ℃, and the pressure is 0 to 1 Mpa.
Preferably, in step S2, the temperature of the bottom of the organic matter separation tower is 60 to 150 ℃, and the pressure is 0 to 1.5 Mpa.
Preferably, in step S3, the temperature at the top of the methyl chloride rectification column is 30 to 180 ℃, and the pressure is 0.1 to 2.0 Mpa.
preferably, in step S3, the temperature of the bottom of the methyl chloride rectification column is 60 to 220 ℃, and the pressure is 0.2 to 3.0 Mpa.
compared with the prior art, the invention has the beneficial effects that:
1. The invention replaces the original method of adsorbing methyl chloride gas by sulfuric acid and separating organic phase with the purification treatment process of methyl chloride-carried organic phase, so that no sulfuric acid is generated in the treatment process, the loss of sulfuric acid is removed, the environmental protection problem of treating hazardous waste sulfuric acid is solved, the recovered organic matter is recycled, and the economic benefit is improved;
2. The invention has the environmental protection characteristic and the economic characteristic, is used for gas phase treatment in the processes of glyphosate synthesis, esterification, acidolysis and the like of byproduct chloromethane, and is also suitable for other chemical industries for producing monomer chloromethane by organic silicon and the like.
drawings
FIG. 1 is a flow chart of a system for purifying methyl chloride according to the present invention.
in the figure: 1 gas compressor, 2 non-condensable gas separator, 3 chloromethane rectifying tower condenser, 4 chloromethane rectifying tower separator, 5 organic matter separating tower condenser, 6 organic matter rectifying tower separator, 7 organic matter separating tower, 8 organic matter separating tower reboiler, 9 chloromethane rectifying tower reboiler and 10 chloromethane rectifying tower.
Detailed Description
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 only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1, a system for purifying methyl chloride comprises a gas compressor 1, a non-condensable gas separator 2, a methyl chloride rectifying tower condenser 3, a methyl chloride rectifying tower separator 4, an organic matter separating tower condenser 5, an organic matter rectifying tower separator 6, an organic matter separating tower 7, an organic matter separating tower reboiler 8, a methyl chloride rectifying tower reboiler 9 and a methyl chloride rectifying tower 10, wherein the gas compressor 1 is connected with the non-condensable gas separator 2, the non-condensable gas separator 2 is connected with the methyl chloride rectifying tower 10, the methyl chloride rectifying tower 10 is connected with the methyl chloride rectifying tower reboiler 9, the non-condensable gas separator 2, the methyl chloride separating tower separator 4, the organic matter separating tower 7, the methyl chloride rectifying tower condenser 3 is connected with the methyl chloride rectifying tower separator 4, the organic matter separating tower 7 is connected with the organic matter separating tower reboiler 8, the organic matter separating tower condenser 5, the non-condensable gas separator 2, the methyl chloride rectifying tower separator 4, the organic matter separating tower 7, The organic matter rectifying tower separator 6, the organic matter separating tower condenser 5 and the organic matter rectifying tower separator 6 are connected.
The non-condensable gas separator 2, the chloromethane rectifying tower separator 4 and the organic matter rectifying tower separator 6 are all connected with a waste gas treatment device through exhaust pipes, the organic matter separating tower 7 is connected with a waste water treatment device through a blow-off pipe, and the gas compressor 1 is connected with a chloromethane feeding pipe.
The working principle is as follows: methyl chloride gas enters from a gas compressor 1, the gas enters a non-condensable gas separator 2 after being compressed by the gas compressor 1, non-organic gas is separated, the rest gas enters a methyl chloride rectifying tower 10 in a gas phase or a liquid phase, the gas at the top of the methyl chloride rectifying tower 10 sequentially passes through a methyl chloride rectifying tower condenser 3 and a methyl chloride rectifying tower separator 4 to be used as a reflux part, and methyl chloride is extracted as a product, the tower bottom of the methyl chloride rectifying tower 10 enters an organic matter separating tower 7, the gas at the top of the organic matter separating tower 7 sequentially passes through an organic matter separating tower condenser 5 and an organic matter rectifying tower separator 6, the non-condensable gas in the organic matter rectifying tower separator 6 is discharged into a waste gas treatment device through an exhaust pipe, the liquid organic matter in the organic matter rectifying tower separator 6 is extracted as a product, and the wastewater at the bottom of the organic matter separating tower 7 is discharged into a wastewater treatment device through a drain pipe, the non-condensable gas separator 2, the chloromethane rectifying tower separator 4 and the organic matter rectifying tower separator 6 discharge non-condensable gas into a waste gas treatment device through exhaust pipes.
a method for treating organic matters in chloromethane gas by substituted sulfuric acid adsorption comprises the following steps:
1) Compressing the chloromethane-containing gas with the mass concentration of 65-100% in a gas compressor; separating out non-organic gas in a non-condensing gas separator; organic gas is used as a raw material of a chloromethane rectifying tower; the non-organic gases enter the gas discharge manifold.
2) and the organic gas enters a methyl chloride rectifying tower for separation, the methyl chloride condensed by a condenser of the methyl chloride rectifying tower at the top is taken as reflux, and the methyl chloride is taken as a product to be extracted. A reboiler of the bottom chloromethane rectifying tower provides heat at the bottom of the tower to control organic matters to enter the organic matter separation tower, wherein the concentration of the chloromethane is low enough;
3) And the organic matter without chloromethane enters an organic matter separation tower, the organic matter condensed at the top of the organic matter separation tower through a condenser is taken as reflux, and the organic matter is taken as a product to be extracted. The reboiler of the bottom organic matter separating tower provides heat at the bottom of the tower and controls the impurity content of the bottom waste water to be low enough.
The experiment of the invention adopts an orthogonal experiment mode to sequentially simulate various factors influencing the reaction.
firstly, the method for removing the non-condensable gas by compressing the methyl chloride without sulfuric acid adsorption is used for orthogonal test. The temperature range is selected from 1-120 ℃, the pressure is 0.01-8 bar, and the gas concentration is as follows: 65 to 100 percent. The results are as follows.
from the experimental results it can be seen that there is a relationship with both temperature and pressure for the separation process. The kind of the recovered film was not evaluated in this experiment. The method for calculating the recovery rate of the organic gas comprises the following steps: Σ% recovery of organic gas = total amount of recovered organic gas/total amount of organic gas in raw material
the preferred separation conditions are 20 ℃ and 5 bar. The method is suitable for various concentration changes, and when the gas concentration is higher, the yield is better, and the concentration factor does not make a preferable condition.
a separation control method for treating chloromethane without sulfuric acid adsorption comprises the following experimental steps:
first, the compression separation method of the treated chloromethane without sulfuric acid adsorption is used for carrying out an orthogonal test. The temperature range of the tower top is 30-180 ℃, and the pressure is 1-20 bar. The results are as follows.
the preferred separation conditions are 150 ℃ and 10 bar. The heat energy utilization and separation effect of the tower are comprehensively analyzed. And the re-separation of the bottom is completed by the organic matter separating tower.
An experimental procedure of a separation control method of an organic matter separation tower without sulfuric acid adsorption comprises the following steps:
Firstly, an orthogonal test is carried out by the control method of the organic matter separation tower without sulfuric acid adsorption. The temperature of the top of the organic matter separation tower is 30-120 ℃, and the pressure is 0-1 Mpa. The results are as follows.
The preferred separation conditions are 50 ℃ at the top and 0 bar. The effluent at the bottom of the tower can reach the disposal discharge level
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. A system for purifying methyl chloride is characterized by comprising a gas compressor (1), a non-condensable gas separator (2), a methyl chloride rectifying tower condenser (3), a methyl chloride rectifying tower separator (4), an organic matter separating tower condenser (5), an organic matter rectifying tower separator (6), an organic matter separating tower (7), an organic matter separating tower reboiler (8), a methyl chloride rectifying tower reboiler (9) and a methyl chloride rectifying tower (10), wherein the gas compressor (1) is connected with the non-condensable gas separator (2), the non-condensable gas separator (2) is connected with the methyl chloride rectifying tower (10), the methyl chloride rectifying tower (10) is connected with the methyl chloride rectifying tower reboiler (9), the non-condensable gas separator (2), the methyl chloride rectifying tower (4) and the organic matter separating tower (7), the methyl chloride rectifying tower condenser (3) is connected with the methyl chloride rectifying tower separator (4), the organic matter separation tower (7) is connected with an organic matter separation tower reboiler (8), an organic matter separation tower condenser (5) and an organic matter rectification tower separator (6), and the organic matter separation tower condenser (5) is connected with the organic matter rectification tower separator (6); the non-condensable gas separator (2), the chloromethane rectifying tower separator (4) and the organic matter rectifying tower separator (6) are connected with a waste gas treatment device through exhaust pipes; the organic matter separation tower (7) is connected with a wastewater treatment device through a sewage discharge pipe; the gas compressor (1) is connected with a chloromethane feeding pipe.
2. A method for treating organic matters in chloromethane gas by substituted sulfuric acid adsorption is characterized by comprising the following steps:
S1, compressing to remove non-condensable gas:
s11, performing one-stage or multi-stage compression on the chloromethane gas containing the non-condensable gas, wherein a condenser is arranged behind each compression stage;
s12, performing membrane separation on the compressed gas, and discharging non-organic gas in the non-condensable gas;
S2, separation of methyl chloride:
s21, preheating methyl chloride and then feeding the preheated methyl chloride into a methyl chloride rectifying tower; preheating to 5-300 ℃ for feeding;
S22, pressurizing and controlling the chloromethane rectifying tower, wherein the pressure is 0.1-5.0 MPa; the top of the distillation tower is provided with a reflux condenser, a reflux tank, a reflux pump and a chloromethane rectifying tower; the rectifying tower is provided with two tower sections, namely a rectifying section and a stripping section, and is used for controlling the rectifying effect at the top and the bottom of the tower;
S23, a reboiler is arranged at the bottom of the tower to provide energy for the tower, and the bottom temperature is controlled to ensure that light components are not carried in the organic composition; the tower bottom enters an organic matter separation tower to separate the available components;
S3, recovering organic matters:
s31, feeding the fluid from the bottom of the chloromethane rectifying tower into an organic matter separation tower, taking out the organic matter from the top of the tower, and separating water from the bottom of the tower;
S32, recycling organic matters at the top of the tower, and enabling tower bottoms to enter a sewage treatment system.
3. the method according to claim 2, wherein in step S2, the temperature at the top of the organic material separation column is 30-120 ℃ and the pressure is 0-1 MPa.
4. The method according to claim 2, wherein in step S2, the temperature of the bottom of the organic material separation column is 60-150 ℃ and the pressure is 0-1.5 MPa.
5. the method according to claim 2, wherein in step S3, the temperature at the top of the methyl chloride rectification column is 30-180 ℃ and the pressure is 0.1-2.0 MPa.
6. the method according to claim 2, wherein in step S3, the temperature at the bottom of the methyl chloride rectification column is 60-220 ℃, and the pressure is 0.2-3.0 MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810522442.0A CN110540487A (en) | 2018-05-28 | 2018-05-28 | System for purifying methyl chloride and method for treating organic matters in methyl chloride gas by substituted sulfuric acid adsorption |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810522442.0A CN110540487A (en) | 2018-05-28 | 2018-05-28 | System for purifying methyl chloride and method for treating organic matters in methyl chloride gas by substituted sulfuric acid adsorption |
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| CN110540487A true CN110540487A (en) | 2019-12-06 |
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| CN201810522442.0A Pending CN110540487A (en) | 2018-05-28 | 2018-05-28 | System for purifying methyl chloride and method for treating organic matters in methyl chloride gas by substituted sulfuric acid adsorption |
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Cited By (1)
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Application publication date: 20191206 |