CN116999872A - Triethyl phosphite tubular production device and synthesis process - Google Patents
Triethyl phosphite tubular production device and synthesis process Download PDFInfo
- Publication number
- CN116999872A CN116999872A CN202311064667.3A CN202311064667A CN116999872A CN 116999872 A CN116999872 A CN 116999872A CN 202311064667 A CN202311064667 A CN 202311064667A CN 116999872 A CN116999872 A CN 116999872A
- Authority
- CN
- China
- Prior art keywords
- pipe
- tubular reactor
- triethyl phosphite
- pipeline
- reactor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims description 13
- 230000015572 biosynthetic process Effects 0.000 title description 5
- 238000003786 synthesis reaction Methods 0.000 title description 5
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000003860 storage Methods 0.000 claims abstract description 17
- 238000003825 pressing Methods 0.000 claims abstract description 15
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 35
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 14
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 6
- 239000002893 slag Substances 0.000 claims description 6
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 claims description 5
- 229940117389 dichlorobenzene Drugs 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000012043 crude product Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000010924 continuous production Methods 0.000 claims description 2
- 238000007086 side reaction Methods 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 238000005192 partition Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000006081 fluorescent whitening agent Substances 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/141—Esters of phosphorous acids
- C07F9/142—Esters of phosphorous acids with hydroxyalkyl compounds without further substituents on alkyl
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
Abstract
The invention provides a tubular production device and a production process for continuously producing triethyl phosphite, wherein the production device comprises a raw material tank, a tubular reactor, a filter pressing system and a rectification system; the raw material tanks comprise a phosphorus trichloride storage tank, an absolute ethyl alcohol storage tank and a two-liquid mixing storage tank, and are respectively connected with the tubular reactor through pipelines; the ammonia is connected with the tubular reactor through a pipeline, the tubular reactor is connected with the filter pressing system through a pipeline, and the filter pressing system is connected with the rectification system through a pipeline. The production device of triethyl phosphite can fully mix raw materials, remove reaction heat, thereby increasing reaction yield which can reach more than 98 percent; the contact time of raw materials can be reduced, and side reactions can be reduced, so that the product content is up to 99.80%.
Description
Technical Field
The invention relates to the field of production and manufacturing of triethyl phosphite, in particular to a tubular device for producing triethyl phosphite and a green synthesis process.
Background
Triethyl phosphite is an organic phosphorus reagent widely applied to the fields of pesticides, plastics, medicines and the like, is mainly used for producing antioxidants, fluorescent whitening agents, flame retardants and various medical intermediates, and has good market prospect.
In the traditional process, such as CN116332986A, kettle reaction production is adopted, a large amount of acid binding agent is needed due to the particularity of the triethyl phosphite synthesis process, and a large amount of salt is produced in the production process, so that the stirring and heat conduction effects are poor, the side reaction in the reaction process is more, the product yield is lower, and generally only about 90 percent. In addition, the traditional method such as CN214106095U adopts a water washing desalting method, a large amount of wastewater is brought in the production process, the environmental pollution is large, and the production process is very environment-friendly.
Disclosure of Invention
The invention firstly provides a tubular production device of triethyl phosphite, which comprises a raw material tank, a tubular reactor, a filter pressing system and a rectification system; the raw material tanks comprise a phosphorus trichloride storage tank, an absolute ethyl alcohol storage tank and a two-liquid mixing storage tank, and are respectively connected with the tubular reactor through pipelines;
the ammonia is connected with the tubular reactor through a pipeline, the tubular reactor is connected with the filter pressing system through a pipeline, the filter pressing system is connected with the rectification system through a pipeline, and the tubular reactor system comprises a heat exchange system and a stirring system.
Preferably, the tubular reactor has a volume of 1.5 to 5L, preferably 3L.
Preferably, the tubular reactor comprises a reaction unit, a pressure stabilizing heat exchange unit and a control unit. The reaction unit comprises a pipe body, a jacket, a stirring device, a first pipeline, a second pipeline and a mixing isolator with built-in annular distributors which are arranged oppositely, wherein the tail ends of the first pipeline and the second pipeline are respectively connected with the annular distributors, the two annular distributors are positioned in the mixing isolator, the periphery of the mixing isolator is fixedly arranged in the pipe body by using a connecting rod, a plurality of liquid outlets are uniformly formed in the side surfaces of the mixing isolator, and one-way valves are formed in the liquid outlets.
Preferably, a discharge hole is formed in the side face of the pipe body, and the height of the discharge hole does not exceed the height of the contact part of the first pipeline and the pipe body.
Preferably, the lowest part of the pipe body is provided with a slag discharging port, and the height of the slag discharging port is lower than that of the contact part of the second pipeline and the pipe body.
Preferably, the stirring device of the tubular reactor is arranged on a tube cover at the top of the tube body, and a group of stirring devices can be arranged. The stirring device comprises a motor, a transmission shaft and a stirring shaft which are sequentially connected, the stirring shaft is fixed on the pipe cover through a bearing, the lower end of the stirring shaft stretches into the pipe body, paddles are arranged at the part stretching into the pipe body, the paddles are arranged in a staggered manner from top to bottom, and the paddles of adjacent stirring devices are not contacted with each other.
Preferably, both the stirring shaft of the tubular reactor and the outer jacket of the reactor are designed to be heat exchanged by passing a circulating exchange medium, such as cold water, which greatly increases the heat exchange capacity of the system.
In another aspect, the invention also provides a process for continuously producing triethyl phosphite by using the pipe-type production device, which comprises the following steps:
pumping phosphorus trichloride into a tubular reactor through a metering pump and a flow meter;
pumping the anhydrous ethanol and the two-phase liquid into a tubular reactor according to a proportion by matching a metering pump with a flowmeter;
after the feed liquid is pumped in, ammonia gas is introduced into a pipe body through a middle inlet of the pipe-type reactor;
after the reaction, the obtained material of the tubular reactor flows into a filter pressing system to recycle ammonium chloride, and the triethyl phosphite crude product is pumped into a rectification system;
and (3) rectifying the crude triethyl phosphite by a two-stage rectifying system, and collecting to obtain qualified triethyl phosphite.
Preferably, the di-liquid comprises solvent dichlorobenzene and acid-binding agent N, N-dimethylaniline, wherein the weight ratio of the dichlorobenzene to the N, N-dimethylaniline is 3-10:1, and more preferably 4:1.
Preferably, the feeding mole ratio of the ethanol to the N, N-dimethylaniline in the two-way liquid is 1:1.1-1.5, more preferably 1:1.1.
Preferably, the feeding mole ratio of the ethanol to the phosphorus trichloride is 3.1-3.5:1, more preferably 3.1:1.
Preferably, the molar ratio of the ammonia gas to the N, N-dimethylaniline in the two-way liquid is 1-1.5:1, more preferably 1.1:1.
The reaction rate of phosphorus trichloride and ethanol is very fast, the feeding passing clearance (clearance between a stirring shaft and the reactor wall) of the tubular reactor is millimeter to centimeter level, the capacity is small, the stock of materials is small, the double heat exchange of an outer jacket and a stirring pump is designed, the reaction can be greatly accelerated, and the material residence time in the tubular reactor is 5-10 s, preferably 5s.
Preferably, the material reaction temperature in the tubular reactor is 50-70 ℃, more preferably 70 ℃.
Advantages of the tubular production device of triethyl phosphite of the invention include:
the gap of the tubular reactor is small, the stirring effect is obvious, the heat exchange area of the reaction is large, raw materials can be fully mixed, and the heat of the reaction is removed, so that the reaction yield is increased, and the yield can reach more than 98%;
the tubular reactor has small volume and short reaction time, can reduce the contact time of raw materials and side reaction, thereby having high product content of up to 99.80 percent.
And compared with the traditional washing and drying process, the post-treatment of the reaction synthesis greatly reduces waste water by adopting filter pressing treatment aiming at salt (ammonium chloride) generated by a system, and the process is environment-friendly.
Drawings
Fig. 1 is a continuous production apparatus of tubular triethyl phosphite according to the present invention, wherein a1 is a phosphorus trichloride storage tank, a2 is an absolute ethanol storage tank, a3 is a two-liquid storage tank, a4 is an ammonia storage tank, b is a tubular reactor, c is a filter pressing system, and d is a rectification system.
FIG. 2 is a tubular reactor apparatus of the present invention. Wherein:
the device comprises a 1-pipe body, a 2-jacket, a 3-stirring device, a 4-motor, a 5-stirring shaft, 6-paddles, a 7-ammonia inlet, an 8-first pipeline, a 9-second pipeline, a 10-first flowmeter, an 11-first one-way valve, a 12-second flowmeter, a 13-second one-way valve, a 14-mixing isolator, a 15-liquid outlet, a 16-connecting rod, a 17-first annular distributor, a 18-first nozzle, a 19-second annular distributor, a 20-second nozzle, a 21-slag discharge port, a 22-pipe body liquid outlet, a 23-jacket circulating water inlet, a 24-jacket circulating water outlet, a 25-stirring shaft circulating water inlet and a 26-stirring shaft circulating water outlet.
Detailed Description
The tubular production apparatus and production process of triethyl phosphite according to the present invention will be described in detail with reference to specific examples.
As shown in fig. 1, the tubular production device of triethyl phosphite comprises a raw material tank a, a tubular reactor b, a filter pressing system c and a rectification system d; the raw material tanks a comprise a phosphorus trichloride storage tank a1, an absolute ethyl alcohol storage tank a2 and a two-liquid storage tank a3, and the raw material tanks are respectively connected with the tubular reactor b through pipelines.
As shown in fig. 2, the tubular reactor b comprises a reaction unit, a pressure-stabilizing heat exchange unit and a control unit. The pressure-stabilizing heat exchange unit and the control unit can be common components of a tubular reactor. Wherein the reaction unit comprises a tube body 1, a jacket 2, a stirring device 3, a first pipe 8 and a second pipe 9, and a mixing separator 14 with an annular distributor (a first annular distributor 17 and a second annular distributor 19) arranged oppositely inside. The first pipeline 8 enters the pipe body from the right side of the pipe body, the second pipeline 9 enters the pipe body from the left side of the pipe body, the tail ends of the first pipeline 8 and the second pipeline 9 are respectively connected with annular distributors, the two annular distributors are positioned in the mixed isolator 14, the periphery of the mixed isolator 14 is fixedly arranged in the pipe body 1 by using a connecting rod 16, a plurality of liquid outlets 15 are uniformly formed in the side face of the mixed isolator, and the liquid outlets 15 are all provided with one-way valves.
The mixing partition 14 is fixed to the lower part of the reactor and serves as a partition, which is not fixed or connected to the stirring shaft. The materials of the first channel 8 and the second channel 9 can be thoroughly mixed in the mixing partition 14 by means of an annular distributor. The mixing separator 14 can be arranged in a short cylinder shape, materials can flow out from the liquid outlet 15 after being uniformly mixed by the mixing separator 14, and 1-4 liquid outlets 15 can be arranged.
The first nozzle 18 and the second nozzle 20 are respectively arranged on the first annular distributor 17 and the second annular distributor 19, phosphorus trichloride enters the first annular distributor 17 of the mixing isolator 14 from the first pipeline 8 through the first flowmeter 10 during reaction, and the first pipeline 8 is provided with the first one-way valve 11. The anhydrous ethanol and the two-way liquid are mixed and then enter a second annular distributor 19 of the mixing isolator 14 from a second pipeline 9 through a second flowmeter 12, and a second one-way valve 13 is arranged on the first pipeline 9. The materials in the two annular distributors are respectively sprayed by the first nozzle 18 and the second nozzle 20, and the materials are fully mixed for reaction. The reacted material flows into the pipe body 1 through the liquid outlet 15 of the mixing separator 14.
The stirring device 3 of the tubular reactor is arranged on a tube cover at the top of the tube body 1 and comprises a motor 4, a transmission shaft (shielding not shown) and a stirring shaft 5 which are sequentially connected, the stirring shaft 5 is fixed on the tube cover through a bearing, the lower end of the stirring shaft extends into the tube body 1, paddles 6 are arranged at the part extending into the tube body 1, and the paddles 6 are arranged in a staggered manner from top to bottom and are not contacted with each other. Both the stirring shaft 5 and the jacket 2 of the reactor are designed with heat exchange lines through which the circulating cooling water can be introduced to increase the heat exchange capacity. The jacket 2 is provided with a circulating water inlet 23 and a circulating water outlet 24, and the stirring shaft 5 is provided with a circulating water inlet 25 and a circulating water outlet 26.
The side of the pipe body 1 can be provided with a discharge hole, and the height of the discharge hole does not exceed the height of the contact part of the first pipeline 8 and the pipe body. The lowest part of the pipe body 1 is provided with a slag discharge port 21.
In the reaction, ammonia gas is required to be continuously introduced for neutralizing hydrogen chloride generated by the reaction, and the ammonia gas enters the pipe body 1 from the ammonia gas storage tank a4 through the ammonia gas inlet 7.
During production, an operator firstly opens a circulating water valve of a jacket of the tubular reactor system b and opens a cooling water valve of the rectification system d;
pumping phosphorus trichloride into a mixing isolator 14 of a tubular reactor b through a first pipeline 8 by a metering pump and a matching flowmeter; and regulating and controlling the feeding flow of the phosphorus trichloride to be 30kg/h.
The weight ratio of the solvent dichlorobenzene to the acid-binding agent N, N-dimethylaniline in the two-mixture solution is 4:1. Pumping the anhydrous ethanol and the two-way liquid into a tubular reactor b according to the ratio of 30:165 (mass ratio) by a metering pump and a flowmeter; the feeding mole ratio of the ethanol and the phosphorus trichloride is controlled at 3.1:1.
After the feed liquid is pumped in, ammonia gas is pressurized and then is introduced into the middle inlet of the tubular reactor b through a flowmeter; the feed rate was controlled at 23Kg/h. The molar ratio of the ammonia to the N, N-dimethylaniline is 1.1:1.
The temperature of the tubular reactor was controlled at 68.+ -. 2 ℃.
After the reaction, the obtained material of the tubular reactor flows into a filter pressing system c to obtain ammonium chloride for recovery, and the triethyl phosphite crude product is pumped into a rectification system d;
and (3) rectifying the crude triethyl phosphite by a two-stage rectifying system d, and collecting to obtain qualified triethyl phosphite.
Through detection and material conversion, the yield of the triethyl phosphite is about 98.50 percent and reaches more than 98 percent through the tubular production device of the triethyl phosphite; the content of triethyl phosphite was about 99.80%.
The present inventors compared the existing production process (such as CN116332986 a) for producing triethyl phosphite by kettle reaction with the pipe type production device of the present invention, and the related parameters are as follows:
as is clear from the comparison of the tables, the tubular production device of triethyl phosphite has the advantages that the yield and the content of the triethyl phosphite are obviously due to the existing kettle-type reaction, and no wastewater which is not friendly to the environment is generated.
Finally, it should be noted that: the above embodiments are only for illustrating the technical aspects of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the above embodiments, it should be understood by those of ordinary skill in the art that: modifications and equivalents may be made to the specific embodiments of the invention without departing from the spirit and scope of the invention, which is intended to be covered by the claims.
Claims (10)
1. A tubular production device of triethyl phosphite comprises a raw material tank, a tubular reactor, a filter pressing system and a rectification system; the raw material tanks comprise a phosphorus trichloride storage tank, an absolute ethyl alcohol storage tank and a two-liquid mixing storage tank, and are respectively connected with the tubular reactor through pipelines;
the ammonia is connected with the tubular reactor through a pipeline, the tubular reactor is connected with the filter pressing system through a pipeline, and the filter pressing system is connected with the rectification system through a pipeline.
2. The pipe production apparatus according to claim 1, wherein the volume of the pipe reactor is 1.5 to 5L, and the residence time of the material in the pipe reactor is 5 to 10s.
3. The tubular production apparatus according to claim 1 or 2, wherein the tubular reactor comprises a reaction unit, a pressure-stabilizing heat exchange unit, and a control unit, the reaction unit comprising a tubular body, a jacket, a stirring device, a first pipe and a second pipe, and a mixing separator having an annular distributor arranged oppositely therein; the tail ends of the first pipeline and the second pipeline are respectively connected with annular distributors, the two annular distributors are positioned in the mixed isolator, the periphery of the mixed isolator is fixedly arranged in the pipe body by using a connecting rod, a plurality of liquid outlets are uniformly formed in the side surfaces of the mixed isolator, and the liquid outlets are all provided with one-way valves.
4. The pipe production device according to claim 1, wherein a discharge port is arranged on the side surface of the pipe body, and the height of the discharge port is not more than the height of a contact part between the first pipeline and the pipe body; the lowest part of the pipe body is provided with a slag discharging port, and the height of the slag discharging port is lower than that of the contact part of the second pipeline and the pipe body.
5. The pipe production apparatus according to claim 1, wherein the stirring device of the pipe reactor is mounted on a pipe cover at the top of the pipe body, provided with a set of stirring devices; the stirring device comprises a motor, a transmission shaft and a stirring shaft which are sequentially connected, the stirring shaft is fixed on the pipe cover through a bearing, the lower end of the stirring shaft stretches into the pipe body, paddles are arranged at the part stretching into the pipe body, the paddles are arranged in a staggered manner from top to bottom, and the paddles of adjacent stirring devices are not contacted with each other.
6. The pipe production apparatus according to claim 1, wherein both the stirring shaft of the pipe reactor and the outer jacket of the reactor are designed to be permeable to a circulating exchange medium.
7. A process for continuously producing triethyl phosphite by using the pipe production apparatus according to any one of the preceding claims 1 to 6, comprising the steps of:
pumping phosphorus trichloride into a tubular reactor through a metering pump and a flow meter;
pumping the anhydrous ethanol and the two-phase liquid into a tubular reactor according to a proportion by matching a metering pump with a flowmeter;
after the feed liquid is pumped in, ammonia gas is introduced into a pipe body through a middle inlet of the pipe-type reactor;
after the reaction, the obtained material of the tubular reactor flows into a filter pressing system to recycle ammonium chloride, and the triethyl phosphite crude product is pumped into a rectification system;
and (3) rectifying the crude triethyl phosphite by a two-stage rectifying system, and collecting to obtain qualified triethyl phosphite.
8. The process for continuously producing triethyl phosphite according to claim 7, wherein the said two-component liquid comprises solvent dichlorobenzene and acid-binding agent N, N-dimethylaniline, the weight ratio of dichlorobenzene and N, N-dimethylaniline is 3-10:1, preferably 4:1.
9. The process for continuously producing triethyl phosphite according to claim 7, wherein the molar ratio of the feed of N, N-dimethylaniline in ethanol and in the two-component liquid is 1:1.1-1.5, the molar ratio of the feed of ethanol and phosphorus trichloride is 3.1-3.5:1, and the molar ratio of the feed of N, N-dimethylaniline in ammonia and in the two-component liquid is 1-1.5:1.
10. The process for the continuous production of triethyl phosphite according to claim 7, wherein the material reaction temperature in the tubular reactor is 50-70 ℃, preferably 70 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311064667.3A CN116999872A (en) | 2023-08-23 | 2023-08-23 | Triethyl phosphite tubular production device and synthesis process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311064667.3A CN116999872A (en) | 2023-08-23 | 2023-08-23 | Triethyl phosphite tubular production device and synthesis process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116999872A true CN116999872A (en) | 2023-11-07 |
Family
ID=88567273
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311064667.3A Pending CN116999872A (en) | 2023-08-23 | 2023-08-23 | Triethyl phosphite tubular production device and synthesis process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116999872A (en) |
-
2023
- 2023-08-23 CN CN202311064667.3A patent/CN116999872A/en active Pending
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