CN116768727A - Method for continuously synthesizing triphosgene in micro-channel reactor - Google Patents
Method for continuously synthesizing triphosgene in micro-channel reactor Download PDFInfo
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- CN116768727A CN116768727A CN202210216552.0A CN202210216552A CN116768727A CN 116768727 A CN116768727 A CN 116768727A CN 202210216552 A CN202210216552 A CN 202210216552A CN 116768727 A CN116768727 A CN 116768727A
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- 238000000034 method Methods 0.000 title claims abstract description 31
- UCPYLLCMEDAXFR-UHFFFAOYSA-N triphosgene Chemical compound ClC(Cl)(Cl)OC(=O)OC(Cl)(Cl)Cl UCPYLLCMEDAXFR-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 230000002194 synthesizing effect Effects 0.000 title abstract description 6
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 239000000460 chlorine Substances 0.000 claims abstract description 27
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims description 45
- 238000002425 crystallisation Methods 0.000 claims description 16
- 230000008025 crystallization Effects 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 16
- 239000003999 initiator Substances 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 12
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 8
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 239000011541 reaction mixture Substances 0.000 claims description 6
- -1 alkyl peroxides Chemical class 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 239000012264 purified product Substances 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 25
- 230000035484 reaction time Effects 0.000 abstract description 4
- 238000010924 continuous production Methods 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 36
- 238000003756 stirring Methods 0.000 description 24
- 239000007789 gas Substances 0.000 description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 20
- 230000002572 peristaltic effect Effects 0.000 description 18
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- 239000002994 raw material Substances 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 8
- 230000000007 visual effect Effects 0.000 description 8
- 239000007788 liquid Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000005660 chlorination reaction Methods 0.000 description 4
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000007664 blowing Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- HCUYBXPSSCRKRF-UHFFFAOYSA-N diphosgene Chemical compound ClC(=O)OC(Cl)(Cl)Cl HCUYBXPSSCRKRF-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/06—Preparation of esters of carbonic or haloformic acids from organic carbonates
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/08—Purification; Separation; Stabilisation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The application discloses a method for synthesizing triphosgene in a continuous flow mode in a microchannel reactor. In a microchannel reactor, under the irradiation of ultraviolet light, dimethyl carbonate and chlorine continuously react at a certain temperature to generate triphosgene. The method can accurately control the reaction temperature, the chlorine consumption, the short reaction time, the high yield and the good product quality, and realizes the continuous production.
Description
Technical Field
The application belongs to the field of organic synthesis, and particularly relates to a method for continuously synthesizing triphosgene in a microchannel reactor.
Background
Triphosgene, also known as solid phosgene, is chemically known as dimethyl bis (trichloromethyl) Carbonate, and is known as Bis (trichloromethyl) Carbonate, BTC for short. As a substitute for phosgene (gas) and diphosgene (liquid), the aqueous emulsion is stable at room temperature, is easy to transport and use, has low toxicity and mild reaction conditions, and is widely applied to the fields of organic synthesis of medicines, pesticides, dyes, high polymer materials and the like.
At present, a dimethyl carbonate (DMC) chlorination method is a general method for preparing triphosgene, namely, metered dimethyl carbonate is added into a reaction kettle at one time, then chlorine is introduced, the reaction temperature is raised, and ultraviolet light with certain intensity is used for initiating the reaction.
Both the change of the reaction condition and the improvement of the production device belong to batch production technology. To date, there has been no report on the preparation of triphosgene by chlorination of dimethyl carbonate in a continuous flow mode in a microchannel reactor. Accordingly, there is a great need in the art to provide a process for the rapid and efficient production of triphosgene.
Disclosure of Invention
The object of the present application is to provide a method for continuous flow synthesis of triphosgene in a microchannel reactor.
In a first aspect of the present application, there is provided a method for continuous flow synthesis of triphosgene in a microchannel reactor comprising the steps of:
(a) Providing a material A and a material B, wherein the material A is a dimethyl carbonate (DMC) solution containing an initiator; the material B is chlorine;
(b) Pumping the material A and the material B into a reactor to form a reaction mixture;
(c) Under the condition of ultraviolet irradiation, the reaction mixture reacts in a reactor to obtain the triphosgene product.
In another preferred embodiment, the molar ratio of dimethyl carbonate to initiator is from 0.1 to 2.0wt%, preferably from 0.2 to 0.5wt%.
In another preferred embodiment, the reactor is a visualized continuous flow microchannel reactor.
In another preferred embodiment, the material a is fed into the reactor by a peristaltic pump.
In another preferred embodiment, the chlorine gas is introduced into the reactor through a gas flow meter.
In another preferred embodiment, the reactor further comprises a temperature control device, and the temperature control device is a heat exchanger.
In a further preferred embodiment, in step (c), the reaction temperature is from 60 to 100 ℃, preferably from 80 to 90 ℃.
In another preferred embodiment, in the step (c), the reaction mixture is left and reacted in the reactor for a residence time of 5 to 100 seconds.
In another preferred embodiment, in said step (c), said residence time is from 10 to 30 seconds.
In another preferred embodiment, the method further comprises the following purification steps:
(d) Discharging the triphosgene product through a micro-channel, and feeding the triphosgene product into a crystallization reactor;
(e) Cooling crystallization is carried out in a crystallization reactor, thereby obtaining a purified product.
In another preferred embodiment, the step (d) further includes: a nitrogen sweep was used to completely crystallize the product.
In another preferred embodiment, in step (d), the method further comprises: the reaction off-gas is absorbed downstream of the crystallization reactor with sodium hydroxide solution.
In another preferred embodiment, the sodium hydroxide solution is 5-20wt% sodium hydroxide solution.
In another preferred embodiment, the liquid holdup of the microchannel is 2-3mL.
In another preferred embodiment, the molar ratio of DMC to material B in material A is 1:6-7.2, preferably 1:6.3-6.6.
In another preferred embodiment, the initiator is selected from the group consisting of: alkyl peroxides, azo alkanes, or combinations thereof; preferably, the initiator is selected from the group consisting of: di-t-butyl peroxide, azobisisobutyronitrile, or combinations thereof.
In another preferred embodiment, in step (c), the ultraviolet light is irradiated at an intensity of 125-375W, preferably 250W.
In another preferred embodiment, the ultraviolet light has a wavelength of 290-390nm, preferably 365nm.
In another preferred example, the sample injection speed of the material A is 1.62-32.4ml/min.
In another preferred example, the sample injection speed of the material B is 0.46-11.13ml/min.
It is understood that within the scope of the present application, the above-described technical features of the present application and technical features specifically described below (e.g., in the examples) may be combined with each other to constitute new or preferred technical solutions. And are limited to a space, and are not described in detail herein.
Detailed Description
The inventor of the present application has conducted extensive and intensive studies to develop a novel method for preparing triphosgene by continuous flow in a microchannel reactor for the first time through mass screening. The method has the advantages of simple process flow, high product yield, short reaction time, high chlorine utilization rate and good product quality, and is suitable for industrial production. On this basis, the present application has been completed.
Method for synthesizing BTC (BTC) by chlorination of DMC (DMC) in microchannel reactor
The application provides a mode for preparing triphosgene by continuous flow of a microchannel reactor, in particular to a process route for synthesizing triphosgene (BTC) from dimethyl carbonate (DMC). The process route has the advantages of precisely controlling the reaction temperature, the chlorine consumption and the reaction time, completing the reaction within tens of seconds to minutes, having high chlorine utilization rate and excellent product quality, and importantly realizing continuous production instead of commonly adopted batch method production.
The method mainly comprises the following steps:
(1) The preparation of raw materials:
preparing a feed liquid containing dimethyl carbonate and an initiator: dimethyl carbonate (DMC) is liquid at normal temperature, an initiator is solid or liquid, and the initiator is added into DMC, stirred uniformly and subjected to microchannel continuous reaction. DMC was added to the four-necked flask, initiator was added under stirring at room temperature, and stirring was continued to mix well for use.
(2) The reaction process comprises the following steps:
in a preferred embodiment of the present application, triphosgene production is carried out using a visualized continuous flow microchannel reactor. Specifically, DMC (containing initiator) is passed through peristaltic pump, chlorine gas is passed through gas flowmeter, check valve and safety valve, and two materials are fed into reactor according to a certain proportion. And (3) carrying out chlorination reaction under the conditions of ultraviolet lamp irradiation, T=40-100 ℃, molar ratio excess of chlorine to DMC-containing feed liquid of 0-10% and residence time of 5-100s, thus obtaining crude BTC.
And (3) blowing nitrogen into the crude product in a crystallization reactor, naturally cooling and crystallizing to obtain a product, and absorbing tail gas by 10% sodium hydroxide solution.
Compared with the prior art, the application has the main advantages that:
(1) The triphosgene is produced in a continuous production mode, so that the production efficiency is greatly improved;
(2) The reaction time is short, the existing ten and twenty hours are shortened to tens of seconds or even tens of seconds, and the method is suitable for industrial production;
(3) The temperature is easy to control, and the safety coefficient is high;
(4) The utilization rate of chlorine is high, and basically no chlorine remains in the product;
(5) The materials are fully contacted, and the yield is high and the quality is excellent.
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. The experimental methods, in which specific conditions are not noted in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. Percentages and parts are by weight unless otherwise indicated.
Example 1
1. Raw material preparation: DMC (200.0 g) was put into a four-necked flask (500 ml), followed by stirring at room temperature, followed by addition of di-t-butyl peroxide (0.4 g) with stirring, and stirring was continued for 15 min.
2. Pumping the prepared DMC solution into a visual continuous flow micro-channel reactor through a peristaltic pump, opening a chlorine valve, and entering the reactor through a gas flowmeter; controlling the temperature to react at 80 ℃ through a heat exchanger; the ultraviolet lamp (125W) was turned on. The molar ratio of DMC to chlorine is controlled to be 1 by adjusting a peristaltic pump and a flowmeter: 6.3; the two materials stay in the reactor for 10s to react; after the reaction, the chloride was continuously discharged through the microchannel reactor, and was introduced into a crystallization flask, purged with nitrogen (tail gas was absorbed with 10% sodium hydroxide solution), and cooled and crystallized to obtain 251.8g of a white solid (yield 96.6%, purity 98.8%).
Example 2
1. Raw material preparation: DMC (200.0 g) was put into a four-necked flask (500 ml), followed by stirring at room temperature, followed by addition of di-t-butyl peroxide (0.4 g) with stirring, and stirring was continued for 15 min.
2. The prepared DMC material enters a visual continuous flow micro-channel reactor through a peristaltic pump, a chlorine valve is opened, and the DMC material enters the reactor through a gas flowmeter; controlling the temperature to react at 80 ℃ through a heat exchanger; turning on an ultraviolet lamp (125W); the molar ratio of DMC to chlorine is controlled to be 1 by adjusting a peristaltic pump and a flowmeter: 6.3. the two materials stay for 20s in the reactor to react; after the reaction, the chloride was continuously discharged through a microchannel reactor, and was introduced into a crystallization flask, purged with nitrogen (tail gas was absorbed with 10% sodium hydroxide solution), and cooled and crystallized to obtain 253.6g of a white solid (yield 97.3%, purity 98.5%).
Example 3
1. Raw material preparation: DMC (200.0 g) was put into a four-necked flask (500 ml), followed by stirring at room temperature, followed by addition of di-t-butyl peroxide (0.4 g) with stirring, and stirring was continued for 15 min.
2. The prepared DMC material enters a visual continuous flow micro-channel reactor through a peristaltic pump, a chlorine valve is opened, and the DMC material enters the reactor through a gas flowmeter; controlling the temperature to be 85 ℃ through a heat exchanger for reaction; the ultraviolet lamp (250W) was turned on. The molar ratio of DMC to chlorine is controlled to be 1 by adjusting a peristaltic pump and a flowmeter: 6.3. the two materials stay for 30s in the reactor to react; after the reaction, the chloride is continuously discharged through a microchannel reactor, enters a crystallization reaction bottle, is purged by nitrogen (tail gas is absorbed by 10% sodium hydroxide solution), and is cooled and crystallized to obtain 256.7g of white solid (yield 98.5%, purity 98.9%).
Example 4
1. Raw material preparation: DMC (200.0 g) was put into a four-necked flask (500 ml), and azobisisobutyronitrile (0.6 g) was added while stirring at room temperature, followed by stirring for 15 minutes.
2. The prepared DMC material enters a visual continuous flow micro-channel reactor through a peristaltic pump, a chlorine valve is opened, and the DMC material enters the reactor through a gas flowmeter; controlling the temperature to react at 80 ℃ through a heat exchanger; the ultraviolet lamp (250W) was turned on. The molar ratio of DMC to chlorine is controlled to be 1 by adjusting a peristaltic pump and a flowmeter: 6.3. the two materials stay in the reactor for 25s to react; after the reaction, the chloride is continuously discharged through a microchannel reactor, enters a crystallization reaction bottle, is purged by nitrogen (tail gas is absorbed by 10% sodium hydroxide solution), and is cooled and crystallized to obtain 256.6g of white solid (yield 98.5%, purity 99.1%).
Example 5
1. Raw material preparation: DMC (200.0 g) was put into a four-necked flask (500 ml), followed by stirring at room temperature, followed by addition of di-t-butyl peroxide (0.6 g) with stirring, and stirring was continued for 15 min.
2. The prepared DMC material enters a visual continuous flow micro-channel reactor through a peristaltic pump, a chlorine valve is opened, and the DMC material enters the reactor through a gas flowmeter; controlling the temperature to react at 80 ℃ through a heat exchanger; turning on an ultraviolet lamp (250W); the molar ratio of DMC to chlorine is controlled to be 1 by adjusting a peristaltic pump and a flowmeter: 6.3. the two materials stay in the reactor for 40s to react; after the reaction, the chloride is continuously discharged through a microchannel reactor, enters a crystallization reaction bottle, is purged by nitrogen (tail gas is absorbed by 10% sodium hydroxide solution), and is cooled and crystallized to obtain 256.6g of white solid (yield 98.5%, purity 99.3%).
Example 6
1. Raw material preparation: DMC (200.0 g) was put into a four-necked flask (500 ml), followed by stirring at room temperature, followed by addition of di-t-butyl peroxide (0.6 g) with stirring, and stirring was continued for 15 min.
2. The prepared DMC material enters a visual continuous flow micro-channel reactor through a peristaltic pump, a chlorine valve is opened, and the DMC material enters the reactor through a gas flowmeter; controlling the temperature to be 85 ℃ through a heat exchanger for reaction; turning on an ultraviolet lamp (250W); the molar ratio of DMC to chlorine is controlled to be 1 by adjusting a peristaltic pump and a flowmeter: 6.6. the two materials stay in the reactor for 40s to react; after the reaction, the chloride is continuously discharged through a microchannel reactor, enters a crystallization reaction bottle, is purged by nitrogen (tail gas is absorbed by 10% sodium hydroxide solution), and is cooled and crystallized to obtain 258.1g of white solid (yield 99.0% and purity 99.5%).
Example 7
1. Raw material preparation: DMC (200.0 g) was put into a four-necked flask (500 ml), and azobisisobutyronitrile (1.2 g) was added while stirring at room temperature, followed by stirring for 15 minutes.
2. The prepared DMC material enters a visual continuous flow micro-channel reactor through a peristaltic pump, a chlorine valve is opened, and the DMC material enters the reactor through a gas flowmeter; controlling the temperature to react at 80 ℃ through a heat exchanger; the ultraviolet lamp (250W) was turned on. The molar ratio of DMC to chlorine is controlled to be 1 by adjusting a peristaltic pump and a flowmeter: 6.3. the two materials stay for 30s in the reactor to react; after the reaction, the chloride is continuously discharged through a microchannel reactor, enters a crystallization reaction bottle, is purged by nitrogen (tail gas is absorbed by 10% sodium hydroxide solution), and is cooled and crystallized to obtain 258.1g of white solid (yield 99.0%, purity 99.3%).
Example 8
1. Raw material preparation: DMC (200.0 g) was put into a four-necked flask (500 ml), followed by stirring at room temperature, followed by addition of di-t-butyl peroxide (0.6 g) with stirring, and stirring was continued for 15 min.
2. The prepared DMC material enters a visual continuous flow micro-channel reactor through a peristaltic pump, a chlorine valve is opened, and the DMC material enters the reactor through a gas flowmeter; controlling the temperature to react at 95 ℃ through a heat exchanger; turning on an ultraviolet lamp (250W); the molar ratio of DMC to chlorine is controlled to be 1 by adjusting a peristaltic pump and a flowmeter: 6.6. the two materials stay for 30s in the reactor to react; after the reaction, chloride is continuously discharged through the microchannel reactor, enters a crystallization reaction bottle, is purged by nitrogen (tail gas is absorbed by 10% sodium hydroxide solution), and is cooled and crystallized to obtain 254.2g of white solid (yield 97.0%, purity 99.0%).
Comparative example 1 (batch production process)
Adding DMC (100.0 g) into a special chlorination reactor which is provided with an ultraviolet lamp (250W), a chlorine pipe and a built-in cooling coil, stirring at room temperature, adding di-tert-butyl peroxide (0.3 g), slowly adding chlorine, controlling the ventilation speed at the initial stage to ensure that the temperature of a reaction system is not more than 40 ℃, gradually thickening a reaction mixture along with the reaction, raising the temperature to T=80-85 ℃, continuously and slowly adding chlorine, keeping the temperature for reaction until the reactor is filled with yellow-green gas, continuously reacting for 2h, and absorbing tail gas by 10% alkali liquor. After the reaction, the whole reaction consumes 10 hours, the chlorine gas is stopped to be blown, and 292.3g (yield 89.7% and purity 99.0%) of white solid is obtained by cooling and crystallizing.
Comparative example 2 (batch production process)
Adding DMC (100.0 g) into a special chlorination reactor provided with an ultraviolet lamp (250W), a chlorine pipe and a built-in cooling coil, stirring at room temperature, adding azodiisobutyronitrile (0.2 g), slowly introducing chlorine, controlling the aeration speed at the initial stage to ensure that the temperature of a reaction system is not more than 40 ℃, gradually thickening a reaction mixture along with the reaction, raising the temperature to T=80-85 ℃, continuously introducing chlorine slowly, keeping the temperature for reaction until the reactor is filled with yellow-green gas, continuously reacting for 2h, and absorbing tail gas by 10% alkali liquor. After the reaction, the whole reaction consumes 10 hours, the chlorine gas is stopped to be blown in, nitrogen is blown in, and 293.6g (yield 90.1% and purity 89.8%) of white solid is obtained by cooling and crystallization.
By comparison, the method for preparing triphosgene by chlorination of dimethyl carbonate by using the continuous flow of the microchannel reactor can greatly reduce the reaction time, improve the product yield, and has the advantages of easily controlled reaction temperature and large-scale industrial application prospect.
All documents mentioned in this disclosure are incorporated by reference in this disclosure as if each were individually incorporated by reference. Further, it will be appreciated that various changes and modifications may be made by those skilled in the art after reading the above teachings, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
Claims (10)
1. A method for continuous flow synthesis of triphosgene in a microchannel reactor comprising the steps of:
(a) Providing a material A and a material B, wherein the material A is a dimethyl carbonate (DMC) solution containing an initiator; the material B is chlorine;
(b) Pumping the material A and the material B into a reactor to form a reaction mixture;
(c) Under the condition of ultraviolet irradiation, the reaction mixture reacts in a reactor to obtain the triphosgene product.
2. A process according to claim 1, wherein in step (c) the reaction temperature is 60-100 ℃, preferably 80-90 ℃.
3. The process of claim 1, wherein in step (c), the reaction mixture is allowed to remain and react in the reactor for a residence time of from 5 to 100 seconds.
4. A process according to claim 3, wherein in step (c), the residence time is from 10 to 30 seconds.
5. The method of claim 1, further comprising the step of purifying:
(d) Discharging the triphosgene product through a micro-channel, and feeding the triphosgene product into a crystallization reactor;
(e) Cooling crystallization is carried out in a crystallization reactor, thereby obtaining a purified product.
6. The method of claim 1 wherein the DMC in the material a and the material B are present in a molar ratio of 1:6-7.2, preferably 1:6.3-6.6.
7. The method of claim 1, wherein the initiator is selected from the group consisting of: alkyl peroxides, azo alkanes, or combinations thereof; preferably, the initiator is selected from the group consisting of: di-t-butyl peroxide, azobisisobutyronitrile, or combinations thereof.
8. The method of claim 1, wherein in step (c), the ultraviolet light is irradiated at an intensity of 125-375W, preferably 250W.
9. The method according to claim 1, wherein the sample injection speed of the material A is 1.62-32.4ml/min.
10. The method according to claim 1, wherein the sample introduction rate of the material B is 0.46-11.13ml/min.
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