CN112479932A - Preparation process of dimethylcarbamoyl chloride - Google Patents
Preparation process of dimethylcarbamoyl chloride Download PDFInfo
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- CN112479932A CN112479932A CN202011459571.3A CN202011459571A CN112479932A CN 112479932 A CN112479932 A CN 112479932A CN 202011459571 A CN202011459571 A CN 202011459571A CN 112479932 A CN112479932 A CN 112479932A
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- YIIMEMSDCNDGTB-UHFFFAOYSA-N Dimethylcarbamoyl chloride Chemical compound CN(C)C(Cl)=O YIIMEMSDCNDGTB-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims abstract description 122
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000000463 material Substances 0.000 claims abstract description 58
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 32
- 239000007789 gas Substances 0.000 claims abstract description 30
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 28
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 238000011049 filling Methods 0.000 claims abstract description 13
- 238000005070 sampling Methods 0.000 claims abstract description 10
- 230000008016 vaporization Effects 0.000 claims abstract description 10
- 239000006200 vaporizer Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000000758 substrate Substances 0.000 claims description 13
- 238000001514 detection method Methods 0.000 claims description 8
- 238000010009 beating Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- 238000009826 distribution Methods 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 230000001502 supplementing effect Effects 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 238000012797 qualification Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 abstract description 7
- 239000002351 wastewater Substances 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 32
- 238000010025 steaming Methods 0.000 description 12
- 230000001276 controlling effect Effects 0.000 description 7
- 238000004064 recycling Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000575 pesticide Substances 0.000 description 3
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 description 2
- RVOLLAQWKVFTGE-UHFFFAOYSA-N Pyridostigmine Chemical compound CN(C)C(=O)OC1=CC=C[N+](C)=C1 RVOLLAQWKVFTGE-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- LULNWZDBKTWDGK-UHFFFAOYSA-M neostigmine bromide Chemical compound [Br-].CN(C)C(=O)OC1=CC=CC([N+](C)(C)C)=C1 LULNWZDBKTWDGK-UHFFFAOYSA-M 0.000 description 2
- 229960001499 neostigmine bromide Drugs 0.000 description 2
- OSZNNLWOYWAHSS-UHFFFAOYSA-M neostigmine methyl sulfate Chemical compound COS([O-])(=O)=O.CN(C)C(=O)OC1=CC=CC([N+](C)(C)C)=C1 OSZNNLWOYWAHSS-UHFFFAOYSA-M 0.000 description 2
- 229960002253 neostigmine methylsulfate Drugs 0.000 description 2
- 229960002290 pyridostigmine Drugs 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 239000005923 Pirimicarb Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- YFGYUFNIOHWBOB-UHFFFAOYSA-N pirimicarb Chemical compound CN(C)C(=O)OC1=NC(N(C)C)=NC(C)=C1C YFGYUFNIOHWBOB-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- NKNFWVNSBIXGLL-UHFFFAOYSA-N triazamate Chemical compound CCOC(=O)CSC1=NC(C(C)(C)C)=NN1C(=O)N(C)C NKNFWVNSBIXGLL-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C269/00—Preparation of derivatives of carbamic acid, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C269/00—Preparation of derivatives of carbamic acid, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C269/08—Separation; Purification; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation process of dimethylcarbamoyl chloride, which comprises the steps of vaporizing liquid dimethylamine by a vaporizer, entering a dimethylamine buffer tank, opening a steam accompanying pipe preheating valve, introducing phosgene, preheating, introducing dimethylamine, reacting until the material liquid level in a synthesis kettle reaches 2/3, stopping the reaction, transferring the material into a deacidification kettle, opening a nitrogen valve, removing gas, transferring the material into a rectifying kettle after the gas removal is finished, carrying out vacuum heating, collecting a finished product by a finished product tank, sampling the material in the finished product tank once every 2 hours, detecting, ensuring that the content of the dimethylcarbamoyl chloride is more than or equal to 98 percent, opening the finished product tank to collect a bottom discharge valve after the gas removal is finished, and filling, wherein the process has the advantages of simple operation, low reaction temperature, high yield of the prepared dimethylcarbamoyl chloride and low waste water amount generated by the reaction, the reaction time is greatly shortened.
Description
Technical Field
The invention relates to the technical field of chemical synthesis, in particular to a preparation process of dimethylcarbamoyl chloride.
Background
Dimethylcarbamyl chloride is an intermediate of carbamate pesticides such as pirimicarb, triazamate and the like, and is also used as an intermediate of medicines, dyes, synthetic materials and other fine chemicals, such as neostigmine bromide, neostigmine methylsulfate, pyridostigmine and the like, and is also used for synthesizing medicines, pesticides, dyes, plastics, synthetic materials and other fine organic chemical products, such as neostigmine bromide, neostigmine methylsulfate, pyridostigmine, carbamate pesticides and the like.
The yield of the dimethylcarbamoyl chloride prepared by the existing preparation process of the dimethylcarbamoyl chloride is low, a large amount of wastewater is generated in the reaction process, the reaction temperature is high, the requirements on the reaction environment are strict, and the reaction time is long.
Disclosure of Invention
The invention aims to provide a preparation process of dimethylcarbamoyl chloride
The technical problems to be solved by the invention are as follows:
the yield of the dimethylcarbamoyl chloride prepared by the existing preparation process of the dimethylcarbamoyl chloride is low, a large amount of wastewater is generated in the reaction process, the reaction temperature is high, the requirements on the reaction environment are strict, and the reaction time is long.
The purpose of the invention can be realized by the following technical scheme:
a preparation process of dimethylcarbamoyl chloride comprises the following steps: vaporizing liquid dimethylamine by a vaporizer and entering a dimethylamine buffer tank, starting a steam tracing pipe preheating valve, introducing phosgene and preheating, introducing dimethylamine for reaction until the material liquid level in a synthesis kettle reaches 2/3, stopping the reaction, transferring the material into a deacidification kettle, opening a nitrogen valve, removing gas, transferring the material into a rectifying kettle after the gas removal is finished, carrying out vacuum heating, collecting a finished product by using a finished product groove, sampling the material in the finished product groove once every 2 hours, detecting, ensuring that the content of dimethylcarbamoyl chloride is not less than 98%, opening the finished product groove to collect a bottom discharge valve until the rectification is finished, and filling.
Further, the preparation process comprises the following specific steps:
step S1: introducing liquid dimethylamine into a vaporizer, vaporizing the liquid dimethylamine at the temperature of 80 ℃, and then delivering gaseous dimethylamine into a distribution cylinder;
step S2: opening a phosgene and dimethylamine steam tracing pipe preheating valve, preheating for 30min, introducing phosgene after preheating for 10min, opening a dimethylamine regulating valve after introducing phosgene for 10min, introducing dimethylamine for reaction until the liquid level of the material in the synthesis kettle reaches 2/3, and stopping synthesis for 30-40 h;
step S3: closing dimethylamine and phosgene inlet valves, opening a bottom valve of a synthesis kettle, putting the materials into a deacidification kettle, closing the bottom valve of the synthesis kettle, opening a nitrogen valve on the deacidification kettle, introducing nitrogen, performing gas driving for 8 hours, sampling, detecting until the content of the dimethylaminocarbonyl chloride in the substrate is detected to be qualified, stopping the gas driving after the detection is qualified, and continuing the gas driving until the detection is unqualified;
step S4: opening a discharge valve of a deacidification kettle and a feed valve on a rectifying kettle, starting a material transfer pump of the deacidification kettle, conveying materials of the deacidification kettle into the rectifying kettle, closing the feed valve of the rectifying kettle and the discharge valve of the deacidification kettle after the material transfer is finished, closing an emptying valve of the deacidification kettle, opening a vacuum valve on the rectifying kettle until the rectifying kettle is vacuum, opening a feed valve of a finished product tank under the condition that the temperature is 80 ℃, rectifying, and keeping qualified rectified materials until the rectification is finished;
step S5: and (3) when the temperature of the rectifying kettle rises and the temperature of the rectifying tower falls, closing a feed valve of the finished product tank, introducing nitrogen to break vacuum, opening a vent valve of the finished product tank, supplementing nitrogen to enable the rectifying kettle to have micro positive pressure, then beating a discharge valve of the finished product tank to start discharging and filling.
Further, the preheating temperature in the step S2 is 80 ℃, and the phosgene introducing flow rate is 30m3H, dimethylamine feed rate 15m3/h。
Further, the nitrogen gas introduction flow rate in the step S3 is 20m3And h, the qualification standard of the substrate is that the content of the dimethylcarbamoyl chloride in the substrate is more than or equal to 98 percent.
Further, the temperature of the rectifying still in the rectifying part in the step S4 is 80-100 ℃, the flow rate of the finished product is 300-400L/h, and the qualified standard of the rectified product is that the content of the dimethylcarbamoyl chloride in the rectified product is more than or equal to 98 percent.
The invention has the beneficial effects that: the invention relates to a preparation process of dimethylcarbamoyl chloride, which comprises the steps of vaporizing liquid dimethylamine by a vaporizer, entering a dimethylamine buffer tank, opening a steam accompanying pipe preheating valve, introducing phosgene, preheating, introducing dimethylamine, reacting until the material liquid level in a synthesis kettle reaches 2/3, stopping the reaction, transferring the material into a deacidification kettle, opening a nitrogen valve, removing gas, transferring the material into a rectifying kettle after the gas removal is finished, carrying out vacuum heating, collecting a finished product by using a finished product tank, sampling the material in the finished product tank once every 2 hours, detecting, ensuring that the content of the dimethylcarbamoyl chloride is more than or equal to 98 percent, and obtaining the dimethylcarbamoyl chloride after the rectification is finished.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow diagram of a process for preparing dimethylcarbamoyl chloride of the present invention.
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. 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.
Example 1
A preparation process of dimethylcarbamoyl chloride is shown in figure 1, and comprises the following specific steps:
step S1: introducing liquid dimethylamine into a vaporizer, vaporizing the liquid dimethylamine at the temperature of 80 ℃, and then delivering gaseous dimethylamine into a distribution cylinder;
step S2: starting a phosgene and dimethylamine steam tracing pipe preheating valve, preheating for 30min at the temperature of 80 ℃, and preheating for 10min at the phosgene flow rate of 30m3Introducing phosgene under the condition of/h, opening a dimethylamine regulating valve after introducing the phosgene for 10min, and controlling the flow of dimethylamine to be 15m3Introducing dimethylamine for reaction under the condition of/h until the liquid level of the materials in the synthesis kettle reaches 2/3, and stopping synthesis, wherein the reaction time is 30 h;
step S3: closing dimethylamine and phosgene inlet valves, opening a bottom valve of a synthesis kettle, putting the materials into a deacidification kettle, closing the bottom valve of the synthesis kettle, opening a nitrogen valve on the deacidification kettle, and controlling the nitrogen flow to be 20m3Introducing nitrogen under the condition of/h, carrying out gas removal for 8 hours, sampling, detecting until the content of the dimethylcarbamoyl chloride in the substrate is not less than 98%, stopping gas removal, and if the detection is not qualified, continuing to remove the gas until the substrate is qualified;
step S4: opening a discharge valve of a deacidification kettle and a feed valve on a rectifying still, starting a material transfer pump of the deacidification kettle, conveying materials of the deacidification kettle into the rectifying still, closing the feed valve of the rectifying still and the discharge valve of the deacidification kettle after the material transfer is finished, closing an exhaust valve of the deacidification kettle, opening a vacuum valve on the rectifying still until the rectifying still is vacuum, distilling at the temperature of 80 ℃, opening a feed valve of a finished product tank, rectifying at the temperature of 80 ℃ and the flow of 300L/h, and keeping the content of the dimethylcarbamoyl chloride in the rectified material to be more than or equal to 98 percent until the rectification is finished;
step S5: when the temperature of the rectifying kettle rises and the temperature of the rectifying tower falls, closing a feed valve of a finished product tank, introducing nitrogen to break vacuum, opening a vent valve of the finished product tank, supplementing nitrogen to enable the pressure in the rectifying kettle to be slightly positive, and then beating a discharge valve of the finished product tank to start discharging and filling;
step S6: transferring the bottom material of each batch of the rectifying still to a residue steaming still, and starting a residue steaming still vacuum system for distillation when 5 batches are obtained. Transferring the collected low-boiling-point components into a rectifying still for recycling, and filling the residue in the residue steaming still into a barrel to be treated according to dangerous waste.
Example 2
A preparation process of dimethylcarbamoyl chloride is shown in figure 1, and comprises the following specific steps:
step S1: introducing liquid dimethylamine into a vaporizer, vaporizing the liquid dimethylamine at the temperature of 80 ℃, and then delivering gaseous dimethylamine into a distribution cylinder;
step S2: starting a phosgene and dimethylamine steam tracing pipe preheating valve, preheating for 30min at the temperature of 80 ℃, and preheating for 10min at the phosgene flow rate of 30m3Introducing phosgene under the condition of/h, opening a dimethylamine regulating valve after introducing the phosgene for 10min, and controlling the flow of dimethylamine to be 15m3Introducing dimethylamine for reaction under the condition of/h until the liquid level of the materials in the synthesis kettle reaches 2/3, and stopping synthesis, wherein the reaction time is 32 h;
step S3: closing dimethylamine and phosgene inlet valves, opening a bottom valve of a synthesis kettle, putting the materials into a deacidification kettle, closing the bottom valve of the synthesis kettle, opening a nitrogen valve on the deacidification kettle, and controlling the nitrogen flow to be 20m3Introducing nitrogen under the condition of/h, carrying out gas removal for 8 hours, sampling, and detecting until the substrate is detectedIf the content of the medium dimethylcarbamoyl chloride is not less than 98 percent, stopping gas driving, and if the detection is not qualified, continuing to drive gas until the gas is qualified;
step S4: opening a discharge valve of a deacidification kettle and a feed valve on a rectifying still, starting a material transfer pump of the deacidification kettle, conveying materials of the deacidification kettle into the rectifying still, closing the feed valve of the rectifying still and the discharge valve of the deacidification kettle after the material transfer is finished, closing an exhaust valve of the deacidification kettle, opening a vacuum valve on the rectifying still until the rectifying still is vacuum, distilling at the temperature of 80 ℃, opening a feed valve of a finished product tank, rectifying at the temperature of 85 ℃ and the flow of 320L/h, and keeping the content of the dimethylcarbamoyl chloride in the rectified material to be more than or equal to 98 percent until the rectification is finished;
step S5: when the temperature of the rectifying kettle rises and the temperature of the rectifying tower falls, closing a feed valve of a finished product tank, introducing nitrogen to break vacuum, opening a vent valve of the finished product tank, supplementing nitrogen to enable the pressure in the rectifying kettle to be slightly positive, and then beating a discharge valve of the finished product tank to start discharging and filling;
step S6: transferring the bottom material of each batch of the rectifying still to a residue steaming still, and starting a residue steaming still vacuum system for distillation when 5 batches are obtained. Transferring the collected low-boiling-point components into a rectifying still for recycling, and filling the residue in the residue steaming still into a barrel to be treated according to dangerous waste.
Example 3
A preparation process of dimethylcarbamoyl chloride is shown in figure 1, and comprises the following specific steps:
step S1: introducing liquid dimethylamine into a vaporizer, vaporizing the liquid dimethylamine at the temperature of 80 ℃, and then delivering gaseous dimethylamine into a distribution cylinder;
step S2: starting a phosgene and dimethylamine steam tracing pipe preheating valve, preheating for 30min at the temperature of 80 ℃, and preheating for 10min at the phosgene flow rate of 30m3Introducing phosgene under the condition of/h, opening a dimethylamine regulating valve after introducing the phosgene for 10min, and controlling the flow of dimethylamine to be 15m3Introducing dimethylamine for reaction under the condition of/h until the liquid level of the materials in the synthesis kettle reaches 2/3, and stopping synthesis, wherein the reaction time is 35 h;
step S3: closing dimethylamine and phosgene inlet valves, opening the valves to synthesizeA bottom valve of the kettle, after the materials are put into the deacidification kettle, the bottom valve of the synthesis kettle is closed, a nitrogen valve on the deacidification kettle is opened, and the nitrogen flow is 20m3Introducing nitrogen under the condition of/h, carrying out gas removal for 8 hours, sampling, detecting until the content of the dimethylcarbamoyl chloride in the substrate is not less than 98%, stopping gas removal, and if the detection is not qualified, continuing to remove the gas until the substrate is qualified;
step S4: opening a discharge valve of a deacidification kettle and a feed valve on a rectifying still, starting a material transfer pump of the deacidification kettle, conveying materials of the deacidification kettle into the rectifying still, closing the feed valve of the rectifying still and the discharge valve of the deacidification kettle after the material transfer is finished, closing an exhaust valve of the deacidification kettle, opening a vacuum valve on the rectifying still until the rectifying still is vacuum, distilling at the temperature of 80 ℃, opening a feed valve of a finished product tank, rectifying at the temperature of 90 ℃ and the flow of 350L/h, and keeping the content of the dimethylcarbamoyl chloride in the rectified material to be more than or equal to 98 percent until the rectification is finished;
step S5: when the temperature of the rectifying kettle rises and the temperature of the rectifying tower falls, closing a feed valve of a finished product tank, introducing nitrogen to break vacuum, opening a vent valve of the finished product tank, supplementing nitrogen to enable the pressure in the rectifying kettle to be slightly positive, and then beating a discharge valve of the finished product tank to start discharging and filling;
step S6: transferring the bottom material of each batch of the rectifying still to a residue steaming still, and starting a residue steaming still vacuum system for distillation when 5 batches are obtained. Transferring the collected low-boiling-point components into a rectifying still for recycling, and filling the residue in the residue steaming still into a barrel to be treated according to dangerous waste.
Example 4
A preparation process of dimethylcarbamoyl chloride is shown in figure 1, and comprises the following specific steps:
step S1: introducing liquid dimethylamine into a vaporizer, vaporizing the liquid dimethylamine at the temperature of 80 ℃, and then delivering gaseous dimethylamine into a distribution cylinder;
step S2: starting a phosgene and dimethylamine steam tracing pipe preheating valve, preheating for 30min at the temperature of 80 ℃, and preheating for 10min at the phosgene flow rate of 30m3Introducing phosgene under the condition of/h, opening a dimethylamine regulating valve after introducing the phosgene for 10min, and controlling the flow of dimethylamine to be 15m3H ofUnder the condition, dimethylamine is introduced for reaction until the liquid level of the materials in the synthesis kettle reaches 2/3, the synthesis is stopped, and the reaction time is 40 hours;
step S3: closing dimethylamine and phosgene inlet valves, opening a bottom valve of a synthesis kettle, putting the materials into a deacidification kettle, closing the bottom valve of the synthesis kettle, opening a nitrogen valve on the deacidification kettle, and controlling the nitrogen flow to be 20m3Introducing nitrogen under the condition of/h, carrying out gas removal for 8 hours, sampling, detecting until the content of the dimethylcarbamoyl chloride in the substrate is not less than 98%, stopping gas removal, and if the detection is not qualified, continuing to remove the gas until the substrate is qualified;
step S4: opening a discharge valve of a deacidification kettle and a feed valve on a rectifying still, starting a material transfer pump of the deacidification kettle, conveying materials of the deacidification kettle into the rectifying still, closing the feed valve of the rectifying still and the discharge valve of the deacidification kettle after the material transfer is finished, closing an exhaust valve of the deacidification kettle, opening a vacuum valve on the rectifying still until the rectifying still is vacuum, distilling at the temperature of 80 ℃, opening a feed valve of a finished product tank, rectifying at the temperature of 100 ℃ and the flow of 400L/h, and keeping the content of the dimethylcarbamoyl chloride in the rectified material to be more than or equal to 98 percent until the rectification is finished;
step S5: when the temperature of the rectifying kettle rises and the temperature of the rectifying tower falls, closing a feed valve of a finished product tank, introducing nitrogen to break vacuum, opening a vent valve of the finished product tank, supplementing nitrogen to enable the pressure in the rectifying kettle to be slightly positive, and then beating a discharge valve of the finished product tank to start discharging and filling;
step S6: transferring the bottom material of each batch of the rectifying still to a residue steaming still, and starting a residue steaming still vacuum system for distillation when 5 batches are obtained. Transferring the collected low-boiling-point components into a rectifying still for recycling, and filling the residue in the residue steaming still into a barrel to be treated according to dangerous waste.
Comparative example
The comparative example is a common preparation process of the dimethylcarbamoyl chloride in the market, and comprises the following specific steps:
adopting a microreactor with 8 reaction templates as a reaction device, wherein the temperature of each reaction module in the microreactor is controlled at 190 ℃, introducing 136.4g of dimethylamine (99.0 percent and 3.0mol) into the microreactor at the speed of 68.2g/min through a gas mass flow meter, simultaneously introducing 371.3g of phosgene (80 percent and 3.0mol) into the microreactor at the speed of 185.7g/min, mixing and reacting, after the reaction is finished, cooling the obtained gas material to room temperature through a cooling device, condensing, collecting the cooled liquid material, and obtaining a crude product of the dimethylcarbamoyl chloride; after rectification, the dimethylcarbamyl chloride product is obtained.
A comparison of examples 1-4 and the multiple ratio process for preparing dimethylcarbamoyl chloride is made, with the results shown in Table 1 below;
TABLE 1
As can be seen from Table 1 above, the yield of dimethylcarbamoyl chloride prepared by the processes for preparing dimethylcarbamoyl chloride of examples 1 to 4 was 89.93 to 99.32%, while the yield of dimethylcarbamoyl chloride prepared by the processes for preparing dimethylcarbamoyl chloride of comparative examples was 95.16%, indicating that the present invention has excellent yield, and the preparation process time is greatly shortened, the amount of waste water generated from the reaction is reduced, and the reaction temperature is low.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (5)
1. A preparation process of dimethylcarbamoyl chloride is characterized in that: the method comprises the following steps: vaporizing liquid dimethylamine by a vaporizer and entering a dimethylamine buffer tank, starting a steam tracing pipe preheating valve, introducing phosgene and preheating, introducing dimethylamine for reaction until the material liquid level in a synthesis kettle reaches 2/3, stopping the reaction, transferring the material into a deacidification kettle, opening a nitrogen valve, removing gas, transferring the material into a rectifying kettle after the gas removal is finished, carrying out vacuum heating, collecting a finished product by using a finished product groove, sampling the material in the finished product groove once every 2 hours, detecting, ensuring that the content of dimethylcarbamoyl chloride is not less than 98%, opening the finished product groove to collect a bottom discharge valve until the rectification is finished, and filling.
2. The process according to claim 1, wherein the preparation of dimethylcarbamoyl chloride comprises the steps of: the preparation process comprises the following specific steps:
step S1: introducing liquid dimethylamine into a vaporizer, vaporizing the liquid dimethylamine at the temperature of 80 ℃, and then delivering gaseous dimethylamine into a distribution cylinder;
step S2: opening a phosgene and dimethylamine steam tracing pipe preheating valve, preheating for 30min, introducing phosgene after preheating for 10min, opening a dimethylamine regulating valve after introducing phosgene for 10min, introducing dimethylamine for reaction until the liquid level of the material in the synthesis kettle reaches 2/3, and stopping synthesis for 30-40 h;
step S3: closing dimethylamine and phosgene inlet valves, opening a bottom valve of a synthesis kettle, putting the materials into a deacidification kettle, closing the bottom valve of the synthesis kettle, opening a nitrogen valve on the deacidification kettle, introducing nitrogen, performing gas driving for 8 hours, sampling, detecting until the content of the dimethylaminocarbonyl chloride in the substrate is detected to be qualified, stopping the gas driving after the detection is qualified, and continuing the gas driving until the detection is unqualified;
step S4: opening a discharge valve of a deacidification kettle and a feed valve on a rectifying kettle, starting a material transfer pump of the deacidification kettle, conveying materials of the deacidification kettle into the rectifying kettle, closing the feed valve of the rectifying kettle and the discharge valve of the deacidification kettle after the material transfer is finished, closing an emptying valve of the deacidification kettle, opening a vacuum valve on the rectifying kettle until the rectifying kettle is vacuum, opening a feed valve of a finished product tank under the condition that the temperature is 80 ℃, rectifying, and keeping qualified rectified materials until the rectification is finished;
step S5: and (3) when the temperature of the rectifying kettle rises and the temperature of the rectifying tower falls, closing a feed valve of the finished product tank, introducing nitrogen to break vacuum, opening a vent valve of the finished product tank, supplementing nitrogen to enable the rectifying kettle to have micro positive pressure, then beating a discharge valve of the finished product tank to start discharging and filling.
3. The process for preparing dimethylcarbamoyl chloride according to claim 2,the method is characterized in that: the preheating temperature in the step S2 is 80 ℃, and the phosgene introducing flow rate is 30m3H, dimethylamine feed rate 15m3/h。
4. The process according to claim 2 for the preparation of dimethylcarbamoyl chloride characterized in that: the nitrogen gas introduction flow rate in the step S3 is 20m3And h, the qualification standard of the substrate is that the content of the dimethylcarbamoyl chloride in the substrate is more than or equal to 98 percent.
5. The process according to claim 2 for the preparation of dimethylcarbamoyl chloride characterized in that: the distillation material part stated in the step S4 is that the temperature of the distillation kettle is 80-100 ℃, the flow rate of the finished product is 300-.
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| CN202011459571.3A Pending CN112479932A (en) | 2020-12-11 | 2020-12-11 | Preparation process of dimethylcarbamoyl chloride |
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Application publication date: 20210312 |