CN111793084A - Microchannel reactor and preparation method of high-content dichlorvos - Google Patents
Microchannel reactor and preparation method of high-content dichlorvos Download PDFInfo
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- CN111793084A CN111793084A CN202010701250.3A CN202010701250A CN111793084A CN 111793084 A CN111793084 A CN 111793084A CN 202010701250 A CN202010701250 A CN 202010701250A CN 111793084 A CN111793084 A CN 111793084A
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- OEBRKCOSUFCWJD-UHFFFAOYSA-N dichlorvos Chemical compound COP(=O)(OC)OC=C(Cl)Cl OEBRKCOSUFCWJD-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229950001327 dichlorvos Drugs 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 74
- HFFLGKNGCAIQMO-UHFFFAOYSA-N trichloroacetaldehyde Chemical compound ClC(Cl)(Cl)C=O HFFLGKNGCAIQMO-UHFFFAOYSA-N 0.000 claims abstract description 25
- CYTQBVOFDCPGCX-UHFFFAOYSA-N trimethyl phosphite Chemical compound COP(OC)OC CYTQBVOFDCPGCX-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000002808 molecular sieve Substances 0.000 claims abstract description 8
- 239000012528 membrane Substances 0.000 claims abstract description 7
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011148 porous material Substances 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 15
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 4
- 239000010779 crude oil Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000003495 polar organic solvent Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 230000000903 blocking effect Effects 0.000 claims 2
- 239000002904 solvent Substances 0.000 claims 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 229940050176 methyl chloride Drugs 0.000 abstract description 6
- 238000007086 side reaction Methods 0.000 abstract description 3
- 238000005086 pumping Methods 0.000 abstract description 2
- 230000036632 reaction speed Effects 0.000 abstract description 2
- 238000009835 boiling Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- RNFNDJAIBTYOQL-UHFFFAOYSA-N chloral hydrate Chemical compound OC(O)C(Cl)(Cl)Cl RNFNDJAIBTYOQL-UHFFFAOYSA-N 0.000 description 2
- 229960002327 chloral hydrate Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229940029273 trichloroacetaldehyde Drugs 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 240000000249 Morus alba Species 0.000 description 1
- 235000008708 Morus alba Nutrition 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- 241000255901 Tortricidae Species 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 230000000895 acaricidal effect Effects 0.000 description 1
- 239000000642 acaricide Substances 0.000 description 1
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- GAUZCKBSTZFWCT-UHFFFAOYSA-N azoxybenzene Chemical compound C=1C=CC=CC=1[N+]([O-])=NC1=CC=CC=C1 GAUZCKBSTZFWCT-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000003958 fumigation Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000013537 high throughput screening Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003986 organophosphate insecticide Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 235000013616 tea Nutrition 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- NFACJZMKEDPNKN-UHFFFAOYSA-N trichlorfon Chemical compound COP(=O)(OC)C(O)C(Cl)(Cl)Cl NFACJZMKEDPNKN-UHFFFAOYSA-N 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
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- 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 Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/113—Esters of phosphoric acids with unsaturated acyclic alcohols
-
- 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
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- 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
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a micro-channel reactor which is of a three-layer sandwich structure, wherein a flow heating medium is arranged in an upper layer and a lower layer, and a reaction space of a multistage series heart-shaped structure is arranged in a middle layer; the upper layer is provided with holes communicated with the reaction space in the middle layer for vacuum pumping in part, and the holes are covered with a molecular sieve or a semipermeable membrane with the pore diameter of 0.6-0.7 nm. The method is used for producing the dichlorvos, the temperature of a heating medium is 40-50 ℃, and the air pressure of a reaction space is negative pressure of-0.02 to-0.08 MPa. When methyl chloride and water vapor are volatilized, trimethyl phosphite and chloral are not entrained, side reaction is not generated, chloral cannot form hydrate, and the reaction speed and the conversion rate are improved.
Description
Technical Field
The invention relates to a structure of micro-channel reaction equipment and a preparation method of dichlorvos.
Background
Dichlorvos is a broad-spectrum organophosphorus insecticide and acaricide, is known for quick action, and has the advantages of low residue, no odor and the like. Because of its high vapor pressure, mainly gas phase action (also having contact action), so it has good effect on some hidden pests, such as leaf roller and moth larva. The medicine is not needed to be sprayed at high temperature, and the good effect can be exerted by fumigation. It can be used for vegetables, mulberry and tea because of its low residual toxicity.
Compared with the dipterex alkaline hydrolysis method, the content of the dichlorvos produced by the one-step method dichlorvos clean production process is obviously improved, the content of the dichlorvos is stabilized to be more than 95 percent, and the highest content can reach 96 percent. The product contains low-boiling-point compounds such as chloral, trimethyl phosphite and the like which have great harm to people and livestock, the requirement on the content of the dichlorvos is continuously improved along with the expansion of dichlorvos users, the demand of 98 percent of high-content dichlorvos is more and more large, the production process of the dichlorvos is improved, and the increase of the content of the dichlorvos is imperative.
In the traditional kettle type production process, batch reaction is adopted, and after trimethyl phosphite is added into a reaction kettle, trichloroacetaldehyde is dripped. Because the exothermic quantity of the reaction is large and the heat exchange area of the jacket is small, the dropwise adding of the chloral takes longer time, so that the reaction time is long and the capacity of the reaction kettle is limited.
In order to solve the problem that reation kettle heat transfer area is little, increase heat transfer area through increasing built-in coil pipe, shorten reaction time, although the time of reaction has shortened, but also brought another problem, built-in coil pipe need occupy the space in the reation kettle, lead to the coefficient of charge of reation kettle interior material to descend, built-in coil pipe is difficult for fixing in reation kettle in addition, because the effect of long-term stirring, it is easy to lead to built-in coil pipe to reveal in bolt fastening department is not hard up or the friction, there is great potential safety hazard.
In addition, trimethyl phosphite reacts with chloral, the generated chloromethane gas partially carries trimethyl phosphite and chloral with lower boiling points, and chloral easily absorbs moisture, so that solid chloral hydrate appears at a flange of a chloromethane exhaust pipeline to block the pipeline.
Microchannel reactors (microreactors), microreactors fabricated using precision machining techniques with feature sizes between 10 and 300 microns (or 1000 microns), "micro" of a microreactor means that the channels of the process fluid are on the order of microns and does not mean that the physical dimensions of the microreactor are small or that the product yield is small. The microreactors can contain millions of microchannels and thus achieve high throughput.
Because of the high heat transfer efficiency of the micro-reactor, the reaction bed layer is nearly constant in temperature, which is beneficial to the proceeding of various chemical reactions. Wan et al oxidized aniline to azoxybenzene in a microreactor, DelSman et al studied selective oxidation of carbon monoxide in a microsystem, and microreactors were also applied to a series of reactions such as hydrogenation, oxidation of ammonia, oxidation of methanol to formaldehyde, water gas shift, and photocatalysis. In addition, the microreactor can be used for on-site production of certain toxic substances, intrinsic kinetic study on strong exothermic reaction and high-throughput screening of combinatorial chemistry such as catalysts, materials, drugs and the like.
Patent application No. 2018218006491's utility model discloses a heart-shaped K type microreactor, including reaction plate, apron, first heat transfer board and second heat transfer board, the second is partly led to the groove and is used for the passageway that feeds through each other heart-shaped little reacting chamber including a plurality of heart-shaped little reacting chamber, the inside of heart-shaped little reacting chamber is provided with K type drainage piece, the second seal groove has been seted up to the side of apron, the first half logical groove that is intestines shape setting has all been seted up to the side of first heat transfer board and second heat transfer board, and the first seal groove has been seted up in the outside that the groove was partly led to, first heat transfer board, reaction plate, apron and second heat transfer board closely assemble together through the bolt. The micro-reactor is easy to generate more side reactions.
Disclosure of Invention
The first object of the present invention is: provides a new process for preparing dichlorvos by using a microchannel reactor.
The technical scheme is as follows:
the new process comprises a material preparation working section, a micro-channel reaction working section and a crystallization powder extraction stage, and specifically comprises the following steps:
(1) material preparation: trimethyl phosphite and chloral raw materials are respectively placed in a container, and dry nitrogen is used as protective gas.
(2) Micro-channel reaction section: and (3) feeding the prepared material in the step (1) into a preheating module of the microchannel reactor through a metering pump, feeding the preheated material into a reaction module, discharging the reaction liquid after passing through the reaction module, performing gas-liquid separation in a flask after discharging, and discharging after cooling by a gas condenser.
(3) And (4) continuing the reaction stage: (2) and after discharging, overflowing the mixture into the next flask, and continuously keeping the temperature for 30 minutes under the condition of negative pressure to ensure that trimethyl phosphite and chloral are completely reacted, thus obtaining the dichlorvos crude oil.
In the preferred embodiment of the present invention, the number of reaction modules is determined by the feeding rate, and in order to ensure the reaction time, when the feeding flow is small, the number of modules needs to be increased to ensure the reaction time to be sufficient, and conversely, the number of modules needs to be decreased to prevent over-reaction.
In the step (2), the number of the reaction modules is 1-4, the feeding amount of trimethyl phosphite in the reaction modules is 20-80 g/min, the feeding amount of trichloroacetaldehyde is 20-95 g/min, the reaction temperature is 40-70 ℃, and the optimized temperature is 40-50 ℃; the reaction pressure is 0-0.5 MPa.
In the step (3), the operating pressure in the flask is minus 0.02 to minus 0.08Mpa, and the heat preservation temperature is 50 to 70 ℃.
The raw materials of the invention are dissolved by non-polar organic solvents such as benzene, carbon tetrachloride and the like, so that polar water molecules are difficult to dissolve mutually, water in the reaction is easier to volatilize and remove, and chloral hydrate cannot be formed.
The second object of the present invention is: provides a micro-channel reactor which can pump the gas generated by the reaction and is beneficial to the reaction and simultaneously can not lose other useful substances.
The technical scheme is as follows: the reaction module of the microchannel reactor is of a two-layer structure (the lower layer is provided with a flow heating medium, the lower layer is a reaction space of a multistage serial heart-shaped structure, a gas outlet communicated with the reaction space is formed in the upper surface right above the heart-shaped structure and used for sucking vacuum, the gas outlet is covered with a molecular sieve and other semipermeable membranes which can permeate chloromethane and water vapor and cannot permeate liquid and other macromolecules) or a three-layer sandwich structure (the upper layer and the lower layer are provided with the flow heating medium, the middle layer is a reaction space of the multistage serial heart-shaped structure, holes communicated with the reaction space of the middle layer and used for sucking vacuum are reserved on part of the upper layer, and the holes are covered with the semipermeable membranes).
The diameter of chloromethane molecule is 0.5-0.6nm, the diameter of water molecule is 0.4nm, the diameter of pore of molecular sieve or semi-permeable membrane is 0.6-0.7nm, so that chloromethane gas and water vapor can be evaporated, and trimethyl phosphite and chloral molecule can not be evaporated and passed through.
The air pressure of the reaction space is negative pressure of-0.02 to-0.08 MPa when the reaction space is vacuumized; the temperature required by the reaction is between 40 and 80 ℃. Considering that the boiling point of the liquid substance is reduced in the negative pressure environment; in order to avoid the gasification of trimethyl phosphite and chloral as two raw materials, the optimized temperature of the heating medium (reaction temperature) is 40-50 ℃, higher than the boiling point of chloromethane (-23.7 ℃) and lower than the boiling point of trimethyl phosphite (112 ℃) and the boiling point of chloral (97.8 ℃).
The beneficial effect of this scheme:
traditional kettle-type reaction, because heat transfer efficiency is low, reaction material is many, need use steam heating to target temperature, because the reaction is exothermic in the reaction process, need plus condensing equipment to cool down. The process is long in time consumption and high in energy consumption, and the reaction period is prolonged. In the traditional kettle type reaction process, paddle type stirring is used, and the generated chloromethane can take away trimethyl phosphite and chloral with lower boiling points, so that the material proportion is unbalanced.
When the microchannel reactor is used, the micron-sized reaction channel ensures that the material passing through the reactor in unit time is small and the generated heat is less. The oil bath heat exchange layers are arranged above and below the reaction layer, the heat exchange efficiency is far higher than that of a traditional reaction kettle, and the temperature can be raised and lowered in time. The mixing mode of the microchannel reactor is 'full-mixing plug flow', and the unique 'heart-shaped' structure of the microchannel reactor enables materials to be mixed more fully in the reactor, greatly improves the mass transfer efficiency, and has the most obvious influence on the reaction.
When the microchannel reactor with the special structure is used, chloromethane gas and water vapor are volatilized, trimethyl phosphite and chloral which have low boiling points but cannot be gasified are not carried, and extra loss of raw materials is not caused.
After methyl chloride is evaporated, no side reaction is generated, reaction products are volatilized, the forward reaction is facilitated, and the reaction speed and the conversion rate are improved.
After the water vapor is evaporated, chloral can not form hydrate, and the reaction space and the conveying pipeline can not be blocked.
Drawings
FIG. 1 is a schematic diagram of one configuration of a microchannel reactor of the present invention;
FIG. 2 is a schematic structural view of a heart-shaped reaction space unit according to the present invention;
in the figure, 1-upper layer; 2-middle layer; 3-lower layer; 4-holes; 6-molecular sieve; 5-a reaction space unit; 11-entrance to the fossa; 12-a barrier groove; 13-apical exit; 14-a reaction chamber.
Detailed Description
The microchannel reactor shown in fig. 1 has a three-layer sandwich structure, wherein the upper layer and the lower layer are provided with flowing heating media, and the middle layer is a reaction space with a multistage series heart-shaped structure; the upper layer is provided with holes for vacuum pumping communicated with the reaction space in the middle layer in a local reserved mode, and the holes are covered with molecular sieves.
1. 252 g of trimethyl phosphite (99.6%) and 300 g of chloral (99.7%) are weighed by a balance, the feeding amount of trimethyl phosphite is adjusted to be 75.6g/min and the feeding amount of chloral is adjusted to be 90.0g/min, the temperature of a reaction module is set to be 50 ℃, gas-liquid separation is carried out in a four-mouth flask after 3 reaction modules, methyl chloride gas is cooled and then is removed from a vacuum system, a methyl chloride recovery device is removed, the temperature in the four-mouth flask is maintained at 70 ℃, the vacuum degree is-0.08 MPa, the retention time of materials in the four-mouth flask is 1 hour, 444.96g of colorless transparent oily liquid is obtained, the content is 99.32%, and the yield is 98.76%.
2. The total weight of 504 g trimethyl phosphite (99.6%) and 600 g chloral (99.7%) is measured by a balance, the feeding amount of trimethyl phosphite is adjusted to be 50.4g/min, the feeding amount of chloral is adjusted to be 60.0g/min, the temperature of a reaction module is set to be 50 ℃, gas-liquid separation is carried out in a four-mouth flask after 2 reaction modules are carried out, methyl chloride gas is cooled and then is removed from a vacuum system, a methyl chloride recovery device is removed, the temperature in the four-mouth flask is maintained at 70 ℃, the vacuum degree is-0.06 MPa, the retention time of materials in the four-mouth flask is 1 hour, 893.68g colorless transparent oily liquid is obtained, the content is 99.47%, and the yield is 99.36%.
Claims (6)
1. A preparation method of high-content dichlorvos is characterized by comprising the following steps: the method specifically comprises the following steps:
(1) material preparation: respectively placing trimethyl phosphite and chloral raw materials in a container, and taking dry nitrogen as protective gas;
(2) adopting the microchannel reactor as claimed in claim 1 or 2, feeding the prepared material in (1) into a preheating module of the microchannel reactor through a metering pump, feeding the preheated material into a reaction module, and discharging the reaction solution after passing through the reaction module;
(3) and (4) continuing the reaction stage: (2) and after discharging, overflowing into a flask, and continuously keeping the temperature for 30 minutes under the condition of negative pressure to ensure that trimethyl phosphite and chloral are completely reacted, thus obtaining the dichlorvos crude oil.
2. The method of claim 1 for producing high levels of dichlorvos, wherein: the air pressure of the reaction space is negative pressure of-0.02 to-0.08 MPa when the reaction space is vacuumized; the reaction temperature is between 40 and 80 ℃.
3. The method for preparing high-level dichlorvos according to claim 1 or 2, characterized in that: the raw materials adopt non-polar organic solvent benzene or carbon tetrachloride as solvent.
4. A micro-channel reactor is characterized in that a reaction module of the reactor is of a two-layer structure or a three-layer sandwich structure, a lower layer of the reactor is provided with a flow heating medium, an upper layer of the reactor is a reaction space in multistage series connection, and the upper surface of the upper layer is provided with a gas outlet communicated with the reaction space; the gas outlet is covered with a molecular sieve or a semipermeable membrane; when the three layers are adopted, the upper layer and the lower layer are provided with flowing heating media, and the middle layer is a reaction space with a multistage series heart-shaped structure; the upper layer is provided with holes communicated with the reaction space of the middle layer in a local reserved manner, and the holes are covered with a molecular sieve or a semipermeable membrane.
5. The microchannel reactor of claim 4, wherein: the pore diameter of the molecular sieve or the semi-permeable membrane is 0.6-0.7 nm.
6. The microchannel reactor of claim 4 or 5, wherein: the reaction space is a heart-shaped structure, materials flow in from a concave heart pit and flow out from a convex heart tip, and a blocking groove for blocking direct flow of the materials is arranged in the heart shape.
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| CN116926692A (en) * | 2023-09-18 | 2023-10-24 | 江苏青昀新材料有限公司 | Flash spinning heart-shaped microreactor |
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