CN110075773A - The method of its synthesis benzocainum of micro-reactor apparatus and application - Google Patents
The method of its synthesis benzocainum of micro-reactor apparatus and application Download PDFInfo
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- CN110075773A CN110075773A CN201910467800.7A CN201910467800A CN110075773A CN 110075773 A CN110075773 A CN 110075773A CN 201910467800 A CN201910467800 A CN 201910467800A CN 110075773 A CN110075773 A CN 110075773A
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- 238000000034 method Methods 0.000 title claims abstract description 33
- BLFLLBZGZJTVJG-UHFFFAOYSA-N benzocaine Chemical compound CCOC(=O)C1=CC=C(N)C=C1 BLFLLBZGZJTVJG-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 19
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 19
- 230000003197 catalytic effect Effects 0.000 claims abstract description 92
- 230000008676 import Effects 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims description 50
- 239000003054 catalyst Substances 0.000 claims description 30
- 239000001257 hydrogen Substances 0.000 claims description 27
- 229910052739 hydrogen Inorganic materials 0.000 claims description 27
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Natural products CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 16
- OTLNPYWUJOZPPA-UHFFFAOYSA-N 4-nitrobenzoic acid Chemical compound OC(=O)C1=CC=C([N+]([O-])=O)C=C1 OTLNPYWUJOZPPA-UHFFFAOYSA-N 0.000 claims description 13
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 229960004756 ethanol Drugs 0.000 claims description 10
- 230000009471 action Effects 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 230000032050 esterification Effects 0.000 claims description 7
- 238000005886 esterification reaction Methods 0.000 claims description 7
- PHWSCBWNPZDYRI-UHFFFAOYSA-N ethyl 4-nitrobenzoate Chemical compound CCOC(=O)C1=CC=C([N+]([O-])=O)C=C1 PHWSCBWNPZDYRI-UHFFFAOYSA-N 0.000 claims description 7
- 238000005984 hydrogenation reaction Methods 0.000 claims description 7
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 claims description 7
- 150000002431 hydrogen Chemical class 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 230000002194 synthesizing effect Effects 0.000 claims description 4
- 238000000889 atomisation Methods 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- CPNMAYYYYSWTIV-UHFFFAOYSA-N ethyl 2-nitrobenzoate Chemical compound CCOC(=O)C1=CC=CC=C1[N+]([O-])=O CPNMAYYYYSWTIV-UHFFFAOYSA-N 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 11
- 230000008901 benefit Effects 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 238000001311 chemical methods and process Methods 0.000 abstract description 2
- 238000010924 continuous production Methods 0.000 abstract description 2
- 210000003128 head Anatomy 0.000 description 55
- 239000000047 product Substances 0.000 description 22
- 208000003251 Pruritus Diseases 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000000202 analgesic effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 238000007086 side reaction Methods 0.000 description 4
- 206010002091 Anaesthesia Diseases 0.000 description 3
- 206010052428 Wound Diseases 0.000 description 3
- 208000027418 Wounds and injury Diseases 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 230000037005 anaesthesia Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 208000014617 hemorrhoid Diseases 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 210000004400 mucous membrane Anatomy 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- TWLLPUMZVVGILS-UHFFFAOYSA-N Ethyl 2-aminobenzoate Chemical compound CCOC(=O)C1=CC=CC=C1N TWLLPUMZVVGILS-UHFFFAOYSA-N 0.000 description 2
- 208000002193 Pain Diseases 0.000 description 2
- 208000025865 Ulcer Diseases 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 229960005274 benzocaine Drugs 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- ZPUCINDJVBIVPJ-LJISPDSOSA-N cocaine Chemical compound O([C@H]1C[C@@H]2CC[C@@H](N2C)[C@H]1C(=O)OC)C(=O)C1=CC=CC=C1 ZPUCINDJVBIVPJ-LJISPDSOSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- MTZQAGJQAFMTAQ-UHFFFAOYSA-N ethyl benzoate Chemical compound CCOC(=O)C1=CC=CC=C1 MTZQAGJQAFMTAQ-UHFFFAOYSA-N 0.000 description 2
- 235000021050 feed intake Nutrition 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 230000036407 pain Effects 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 238000007039 two-step reaction Methods 0.000 description 2
- 231100000397 ulcer Toxicity 0.000 description 2
- ALYNCZNDIQEVRV-UHFFFAOYSA-N 4-aminobenzoic acid Chemical compound NC1=CC=C(C(O)=O)C=C1 ALYNCZNDIQEVRV-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 206010002153 Anal fissure Diseases 0.000 description 1
- 208000016583 Anus disease Diseases 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- 229940090898 Desensitizer Drugs 0.000 description 1
- 208000009531 Fissure in Ano Diseases 0.000 description 1
- 208000006877 Insect Bites and Stings Diseases 0.000 description 1
- NNJVILVZKWQKPM-UHFFFAOYSA-N Lidocaine Chemical compound CCN(CC)CC(=O)NC1=C(C)C=CC=C1C NNJVILVZKWQKPM-UHFFFAOYSA-N 0.000 description 1
- 206010068319 Oropharyngeal pain Diseases 0.000 description 1
- VNQABZCSYCTZMS-UHFFFAOYSA-N Orthoform Chemical compound COC(=O)C1=CC=C(O)C(N)=C1 VNQABZCSYCTZMS-UHFFFAOYSA-N 0.000 description 1
- 208000005141 Otitis Diseases 0.000 description 1
- 201000007100 Pharyngitis Diseases 0.000 description 1
- 206010042496 Sunburn Diseases 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 238000001949 anaesthesia Methods 0.000 description 1
- 230000003444 anaesthetic effect Effects 0.000 description 1
- 230000036592 analgesia Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000001139 anti-pruritic effect Effects 0.000 description 1
- 239000003908 antipruritic agent Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 208000020670 canker sore Diseases 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229960003920 cocaine Drugs 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 210000000883 ear external Anatomy 0.000 description 1
- 208000019258 ear infection Diseases 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000002008 hemorrhagic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000007803 itching Effects 0.000 description 1
- 229960004194 lidocaine Drugs 0.000 description 1
- 239000003589 local anesthetic agent Substances 0.000 description 1
- 229960005015 local anesthetics Drugs 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000004084 narcotic analgesic agent Substances 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 210000004126 nerve fiber Anatomy 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 239000004006 olive oil Substances 0.000 description 1
- 235000008390 olive oil Nutrition 0.000 description 1
- 229950006098 orthocaine Drugs 0.000 description 1
- 206010033072 otitis externa Diseases 0.000 description 1
- 125000000636 p-nitrophenyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1*)[N+]([O-])=O 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229960004919 procaine Drugs 0.000 description 1
- MFDFERRIHVXMIY-UHFFFAOYSA-N procaine Chemical compound CCN(CC)CCOC(=O)C1=CC=C(N)C=C1 MFDFERRIHVXMIY-UHFFFAOYSA-N 0.000 description 1
- 239000001944 prunus armeniaca kernel oil Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 210000001044 sensory neuron Anatomy 0.000 description 1
- 210000004999 sex organ Anatomy 0.000 description 1
- 230000009182 swimming Effects 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- GKCBAIGFKIBETG-UHFFFAOYSA-N tetracaine Chemical compound CCCCNC1=CC=C(C(=O)OCCN(C)C)C=C1 GKCBAIGFKIBETG-UHFFFAOYSA-N 0.000 description 1
- 208000004371 toothache Diseases 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/04—Formation of amino groups in compounds containing carboxyl groups
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00851—Additional features
- B01J2219/00867—Microreactors placed in series, on the same or on different supports
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00873—Heat exchange
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00891—Feeding or evacuation
Abstract
The invention discloses a kind of methods of its synthesis benzocainum of micro-reactor apparatus and application, micro-reactor apparatus is at least made of a unit, and the unit includes head tank I, head tank II, the micro- reactor tank I of fixed-bed catalytic, the micro- reactor tank II of fixed-bed catalytic, constant flow pump I, constant flow pump II, cooling tank, receiving tank and the gas heating tank；The import of the constant flow pump I is connected with the head tank I, and the outlet of the constant flow pump I is connected with the import of the micro- reactor tank I of the fixed-bed catalytic, so that the material of the head tank I is pumped into the micro- reactor tank I of the fixed-bed catalytic by the constant flow pump I；The product exit of the micro- reactor tank I of fixed-bed catalytic is connected with the import of the head tank II.Its present invention have many advantages, such as structure simply, without enlarge-effect, operating condition is easily controllable and intrinsic safety, had using micro- chemical process that micro-reactor apparatus carries out and batch process is replaced with continuous process, process intensification, the safety is improved, the advantages that product property changes, distributed production.
Description
Technical field
The present invention relates to a kind of methods of its synthesis benzocainum of micro-reactor apparatus and application, belong to chemical technology field.
Background technique
Currently, benzocainum, chemical name is ethylaminobenzoate, structural formula are as follows:
Ethylaminobenzoate alias benzocainum (ABEE).Colourless rhomboid crystallization, it is odorless tasteless.Molecular weight
165.19.Fusing point is 91~92 DEG C.It is soluble in alcohol, ether, chloroform.Apricot kernel oil, olive oil, diluted acid can be dissolved in.It is insoluble in water.It is clinical
It is upper for the surface of a wound, ulcer surface, burn, skin wiping is split and the analgesia of hemorrhoid, antipruritic.Anaesthesine is a kind of fat-soluble surface anesthesia
Agent, compared with other several local anaesthetics such as lidocaine, dicaine, action intensity is smaller, thus when acting on mucous membrane
It will not make one not feeling good because of anesthetic effect.It is a kind of fat-soluble stronger drug, so the rouge easily with mucous membrane or skin
Layer combines, but be not easy to penetrate and into generating toxicity in human body.Anaesthesine can be used as Suo Fang difficult to understand, Orthocaine, procaine etc.
Precursor raw material；Meanwhile it in medicine again be used as local anesthetic, have analgesic, itching-relieving action, be mainly used for the surface of a wound, ulcer surface,
Mucomembranous surface and hemorrhoid narcotic analgesic and disease of itching, ointment also act as the analgesic of the lubrications such as nasopharyngeal catheter, interior prominent sight glass.It is temporarily slow
Solve the discomfort of pain and itch skin, mild burn, sunburn, wound and insect bites.Aural preparations are used to mitigate acute fill
Hemorrhagic, dense property otitis externa, the pain for otitis of swimming and itch and ear external application.To toothache, sore-throat, canker sore, various hemorrhoid
Sore, anal fissure, pruritus vulvue are also effectively, to keep ejaculation slow as male sex organ desensitizer.Or it is used as conduit and interior mirror tube
Anesthesia lubricant.Benzocainum local use acts on the nerve fiber of skin, mucous membrane, and the conduction of block nerves impulsion makes
Various feeling transitory loss benumb sensory nerve ending and generate analgesic, itching-relieving action.Benzocainum local anaesthesia effect is more general
Shandong cacaine is weak, external application can slow-absorbing, persistent has analgesic, itching-relieving action.Benzocainum toxicity is only the 1/20 of cocaine
~1/160.
Produce benzocainum economic value added with higher by raw material of ethyl p-nitrobenzoate, be benzocainum into
The preferable approach of row deep processing.Mainstream production method industrial at present is the reduction of palladium carbon hydrogenation catalyst.Due to intermittent reaction
The speed of the characteristic of kettle, reaction is slow, and yield is low, and risk is high, and hydrogen is not easily recycled, and increases many costs.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies of existing technologies, a kind of micro-reactor apparatus is provided, it has
Have the advantages that structure it is simple, without enlarge-effect, operating condition is easily controllable and intrinsic safety, use micro-reactor apparatus to carry out micro-
Chemical process, which has, replaces batch process with continuous process, and process intensification, the safety is improved, and product property changes, and distributing is raw
The advantages that production.
In order to solve the above-mentioned technical problem, the technical scheme is that a kind of micro-reactor apparatus, it is at least by an equipment
Unit composition, the unit include that head tank I, head tank II, the micro- reactor tank I of fixed-bed catalytic, fixed-bed catalytic are micro- anti-
Answer tank II, constant flow pump I, constant flow pump II, cooling tank, receiving tank and the gas heating tank；Wherein,
The import of the constant flow pump I is connected with the head tank I, the outlet of the constant flow pump I and the fixed-bed catalytic
The import of micro- reactor tank I is connected, so that the material of the head tank I is pumped into the fixed-bed catalytic is micro- anti-by the constant flow pump I
It answers in tank I；
The product exit of the micro- reactor tank I of fixed-bed catalytic is connected with the import of the head tank II, so that described solid
Fixed bed is catalyzed the product that micro- reactor tank I is generated and enters the head tank II；
The import of the constant flow pump II is connected with the outlet of the head tank II, the outlet of the constant flow pump II with it is described solid
The first import that fixed bed is catalyzed micro- reactor tank II is connected so that the constant flow pump II material of the head tank II is pumped into it is described
In the micro- reactor tank II of fixed-bed catalytic；
The import of the gas heating tank is for feeding hydrogen and nitrogen or hydrogen, the outlet of the gas heating tank and institute
The second import for stating the micro- reactor tank II of fixed-bed catalytic is connected, to be at least passed through hydrogen to the micro- reactor tank II of the fixed-bed catalytic
Gas；
It is equipped with and is connected with the first import for the material being pumped into be atomized simultaneously in the micro- reactor tank II of fixed-bed catalytic
With the atomizer for the hydrogen mixing being passed through；
The import of the cooling tank is connected with the product exit of the micro- reactor tank II of the fixed-bed catalytic, the cooling tank
Outlet is connected with the receiving tank.
Micro-reactor apparatus further includes constent temperature heater, the constent temperature heater respectively with the head tank I, head tank II,
The micro- reactor tank I of fixed-bed catalytic, the micro- reactor tank II of fixed-bed catalytic are connected with the collet of cooling tank.
Further, the aperture of the atomizer is 0.5mm.
Further, the receiving tank is the head tank I of next unit.
Further, the outlet of the constant flow pump I is also connected with the import of the head tank I, to be followed by the constant flow pump I
Material in head tank I described in ring.
Further, the outlet of the constant flow pump II is also connected with the import of the head tank II, to pass through the constant flow pump
II recycles the material in the head tank II.
Further, the import of the gas heating tank is connected or and hydrogen by air inlet valve group with hydrogen gas cylinder and nitrogen cylinder
Gas cylinder is connected.
The present invention also provides a kind of method for synthesizing benzocainum, method carries out in the above micro-reactor apparatus.
Further, include: in the step of method
The paranitrobenzoic acid solution that solvent is ethyl alcohol is placed in head tank I, by constant flow pump I by head tank I to nitre
Yl benzoic acid solution is pumped into the micro- reactor tank I of fixed-bed catalytic, under the action of catalyst in the micro- reactor tank I of fixed-bed catalytic
Esterification is carried out, ethyl p-nitrobenzoate solution is obtained；
Ethyl p-nitrobenzoate solution is placed in head tank II, by constant flow pump II by the p-nitrophenyl first of head tank II
Acetate solution is pumped into the micro- reactor tank II of fixed-bed catalytic by atomizer atomization and mixes with the hydrogen being passed through, in fixation
Carry out hydrogenation under the action of the catalyst that bed is catalyzed in micro- reactor tank II, after by processing obtain benzocainum.
Further, head tank I temperature is 70 DEG C, 80~85 DEG C of the micro- reactor tank I temperature of fixed-bed catalytic, and reaction pressure is
0.4MPa, feed rate 5ml/min；
Further, head tank II temperature is 70~80 DEG C, and the micro- reactor tank II temperature of fixed-bed catalytic is 140 DEG C, reaction pressure
Power is 17~35 kilograms, and feed rate is 80~120ml/min.
Further, the catalyst in the micro- reactor tank I of fixed-bed catalytic is azochlorosulfonate acid resin catalyst；
And/or the catalyst in the micro- reactor tank II of fixed-bed catalytic is palladium-carbon catalyst or platinum Al catalysts.
Further, before using micro-reactor apparatus synthesis benzocainum, dehydrated alcohol is used to constant flow pump I and constant flow pump II
It is calibrated.
After above-mentioned technical proposal, raw material used in the method for the present invention is liquid or is that can be dissolved in raw material
Solid matter, the product of generation are also liquid, suitable for micro-reactor apparatus of the invention.
Micro-reactor apparatus of the invention has the advantage of process intensification, the ester carried out in the micro- reactor tank I of fixed-bed catalytic
It is that paranitrobenzoic acid is sufficiently mixed in a very short period of time with sulfonic resin catalyst, and is guaranteed during changing reaction
The timely transmitting of heat of reaction, it is therefore prevented that traditional handicraft is because the reaction time is too long, mixed effect is limited and rate of heat transfer is slow
The generation of caused polymerization side reactions, reduces product impurity content, improves the conversion ratio of product；It is micro- anti-in fixed-bed catalytic
It answers in the hydrogenation carried out in tank II, due to being phase reaction, atomizer can be mixed hydrogen and liquid Quick uniform,
Mixed effect is substantially increased, completes reaction within a very short time, avoids product in popular response system because stirring not
Uniformly extend the reaction time, product is caused to hydrolyze and occur the side reactions such as polymerization under alkaline condition.Due to avoiding routine
Be stirred present in reaction and system heat transfer in terms of advantage, greatly improve combined coefficient, and be suitble to continuous close
At.
Therefore, the present invention has the following advantages that；
Micro-reactor apparatus of the invention, material are pumped by constant flow pump, ensure that the accurate and operation side of material metering
Just safety；Conveying and transfer of the material in reaction system are in a closed state, and make operation safety and environmental protection；It can also be right
Relevant technological parameter carries out online adjusting in real time, and technological parameter can intuitively be shown, conducive to the control to synthesis technology.
Micro-reactor apparatus of the invention is applied in synthesis benzocainum, the feed stock conversion and product benzene of two-step reaction
The purity of cacaine is helped compared with traditional handicraft height；Synthesis process continuous operation, saves reaction time and energy consumption, reaction process
Amplification is easy；Without the conventional chemical reaction device such as reaction kettle and condenser, relative device investment is low with maintenance cost；Raw material
It is directly pumped by constant flow pump, facilitate plus feed intake link, enhances the safety of operation；Process regulation is easy, can be online
Process conditions are adjusted as needed at any time.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of micro-reactor apparatus of the invention.
Specific embodiment
The present invention provides a kind of methods of its synthesis benzocainum of micro-reactor apparatus and application, and those skilled in the art can
To use for reference present disclosure, it is suitably modified realization of process parameters.In particular, it should be pointed out that all similar substitutions and modifications are to this
It is for the technical staff of field it will be apparent that they shall fall within the protection scope of the present invention.Method and application of the invention is
Through being described by preferred embodiment, related personnel obviously can not depart from the content of present invention, in spirit and scope to this
The methods and applications of text are modified or appropriate changes and combinations, carry out implementation and application the technology of the present invention.
As shown in Figure 1, a kind of micro-reactor apparatus, it is at least made of a unit, and the unit includes charging
The micro- reactor tank I3 of tank I1, head tank II2, fixed-bed catalytic, the micro- reactor tank II4 of fixed-bed catalytic, constant flow pump I5, constant flow pump II6,
Cooling tank 7, receiving tank 8 and the gas heating tank 9；Wherein,
The import of the constant flow pump I5 is connected with the head tank I1, and outlet and the fixed bed of the constant flow pump I5 is urged
The import for changing micro- reactor tank I3 is connected, so that the material of the head tank I1 is pumped into the fixed-bed catalytic by the constant flow pump I5
In micro- reactor tank I3；
The product exit of the micro- reactor tank I3 of fixed-bed catalytic is connected with the import of the head tank II2, so that described
The product that the micro- reactor tank I3 of fixed-bed catalytic is generated enters the head tank II2；
The import of the constant flow pump II6 is connected with the outlet of the head tank II2, the outlet of the constant flow pump II6 and institute
The first import for stating the micro- reactor tank II4 of fixed-bed catalytic is connected, so that the constant flow pump II6 is by the material of the head tank II2
It is pumped into the micro- reactor tank II4 of the fixed-bed catalytic；
The import of the gas heating tank 9 for feeding hydrogen and nitrogen or hydrogen, the outlet of the gas heating tank 9 with
The second import of the micro- reactor tank II4 of fixed-bed catalytic is connected, to be at least passed through to the micro- reactor tank II4 of the fixed-bed catalytic
Hydrogen；
It is equipped with and is connected with the first import for the material being pumped into be atomized simultaneously in the micro- reactor tank II4 of fixed-bed catalytic
With the atomizer for the hydrogen mixing being passed through；
The import of the cooling tank 7 is connected with the product exit of the micro- reactor tank II4 of the fixed-bed catalytic, the cooling tank
7 outlet is connected with the receiving tank 8.
Specifically, the micro- reactor tank I3 of the fixed-bed catalytic and micro- reactor tank II4 of fixed-bed catalytic is fixed bed catalyst
Device.
Specifically, micro-reactor apparatus further includes constent temperature heater, the constent temperature heater respectively with the head tank I1, into
The micro- reactor tank I3 of batch can II2, fixed-bed catalytic, the micro- reactor tank II4 of fixed-bed catalytic are connected with the collet of cooling tank 7.
The channel diameter of the micro- reactor tank II4 of fixed-bed catalytic is 5cm, and length 30cm-50cm, but not limited to this.
The aperture of the atomizer can be 0.5mm, and but not limited to this.
The receiving tank 8 is the head tank I1 of next unit.
As shown in Figure 1, the outlet of the constant flow pump I5 is also connected with the import of the head tank I1, to pass through the constant current
Pump I5 recycles the material in the head tank I1.
As shown in Figure 1, the outlet of the constant flow pump II6 is also connected with the import of the head tank II2, to pass through the perseverance
Stream pump II6 recycles the material in the head tank II2.
As shown in Figure 1, the import of the gas heating tank 9 be connected with hydrogen gas cylinder and nitrogen cylinder by air inlet valve group or
It is connected with hydrogen gas cylinder.It wherein, is into hydrogen or nitrogen by operating air inlet valve group to can choose the import of gas heating tank 9
Gas or hydrogen and nitrogen.
The present invention also provides a kind of method for synthesizing benzocainum, method carries out in the above micro-reactor apparatus.
The reaction equation for synthesizing benzocainum is as follows:
；
Specifically, include: in the step of method
The paranitrobenzoic acid solution that solvent is ethyl alcohol is placed in head tank I1, it will be in head tank I1 by constant flow pump I5
Paranitrobenzoic acid solution is pumped into the micro- reactor tank I3 of fixed-bed catalytic, the catalyst in the micro- reactor tank I3 of fixed-bed catalytic
Effect is lower to carry out esterification, obtains ethyl p-nitrobenzoate solution；
By ethyl p-nitrobenzoate solution be placed in head tank II2, by constant flow pump II6 by head tank II2 to nitre
Yl benzoic acid ethyl ester solution is pumped into the micro- reactor tank II4 of fixed-bed catalytic by atomizer atomization and mixes with the hydrogen being passed through
Close, catalyst in the micro- reactor tank II4 of fixed-bed catalytic under the action of, carries out hydrogenation, after by processing obtain benzene assistant card
Cause.
In the present invention, by processing after specifically: cleaning, decoloration, crystallizing and drying.
Head tank I1 temperature is 70 DEG C, 80~85 DEG C, reaction pressure 0.4MPa of the micro- reactor tank I3 temperature of fixed-bed catalytic,
Feed rate is 5ml/min；The restriction of these parameters mainly makes it preferably complete esterification, improves its conversion ratio.
Head tank II2 temperature is 70~80 DEG C, and the micro- reactor tank II4 temperature of fixed-bed catalytic is 140 DEG C, reaction pressure 17
~35 kilograms, feed rate is 80~120ml/min；The restriction of these parameters mainly makes it preferably complete hydrogenation,
Improve its conversion ratio.
Specifically, the catalyst in the micro- reactor tank I3 of fixed-bed catalytic is azochlorosulfonate acid resin catalyst；
It is palladium-carbon catalyst or platinum Al catalysts with the catalyst in the micro- reactor tank II4 of fixed-bed catalytic.
Before using micro-reactor apparatus synthesis benzocainum, constant flow pump I5 and constant flow pump II6 are carried out using dehydrated alcohol
Calibration.
Micro-reactor apparatus of the invention has the advantage of process intensification, the ester carried out in the micro- reactor tank I3 of fixed-bed catalytic
It is that paranitrobenzoic acid is sufficiently mixed in a very short period of time with sulfonic resin catalyst, and is guaranteed during changing reaction
The timely transmitting of heat of reaction, it is therefore prevented that traditional handicraft is because the reaction time is too long, mixed effect is limited and rate of heat transfer is slow
The generation of caused polymerization side reactions, reduces product impurity content, improves the conversion ratio of product；It is micro- anti-in fixed-bed catalytic
It answers in the hydrogenation carried out in tank II4, due to being phase reaction, atomizer can be mixed hydrogen and liquid Quick uniform
It closes, substantially increases mixed effect, complete reaction within a very short time, avoid product in popular response system because of stirring
Unevenly extend the reaction time, product is caused to hydrolyze and occur the side reactions such as polymerization under alkaline condition.Due to avoiding often
Be stirred present in rule reaction and system heat transfer in terms of advantage, greatly improve combined coefficient, and be suitble to continuous
Synthesis.
Micro-reactor apparatus of the invention, material are pumped by constant flow pump, ensure that the accurate and operation side of material metering
Just safety；Conveying and transfer of the material in reaction system are in a closed state, and make operation safety and environmental protection；It can also be right
Relevant technological parameter carries out online adjusting in real time, and technological parameter can intuitively be shown, conducive to the control to synthesis technology.
Micro-reactor apparatus of the invention is applied in synthesis benzocainum, the feed stock conversion and product benzene of two-step reaction
The purity of cacaine is helped compared with traditional handicraft height；Synthesis process continuous operation, saves reaction time and energy consumption, reaction process
Amplification is easy；Without the conventional chemical reaction device such as reaction kettle and condenser, relative device investment is low with maintenance cost；Raw material
It is directly pumped by constant flow pump, facilitate plus feed intake link, enhances the safety of operation；Process regulation is easy, can be online
Process conditions are adjusted as needed at any time.
In order that the present invention can be more clearly and readily understood, right below according to specific embodiment and in conjunction with attached drawing
The present invention is described in further detail.
Embodiment 1:
It takes 22.4g paranitrobenzoic acid to be dissolved in ethanol solution (mass percentage of ethyl alcohol is 99.9%), is configured to
The paranitrobenzoic acid solution that percentage composition is 4%, is put into the head tank I1 of micro-reactor apparatus and recycles.It is micro- in fixed-bed catalytic
Azochlorosulfonate acid resin catalyst is loaded in reactor tank I3, and palladium-carbon catalyst or the catalysis of platinum aluminium are loaded in the micro- reactor tank II4 of fixed-bed catalytic
Agent, sets the head tank I1 temperature of micro-reactor apparatus as 70 DEG C, 80 DEG C of the micro- reactor tank I3 temperature of fixed-bed catalytic, and reaction pressure is
0.4MPa, flow 5ml/min.Constant flow pump I5 is opened, carries out esterification after solution is squeezed into the micro- reactor tank I3 of fixed-bed catalytic,
Reaction product receives in head tank II.Again after the micro- reactor tank II4 nitrogen of fixed-bed catalytic, hydrogen displacement three times, setting
Head tank II temperature is 70 DEG C, and the micro- reactor tank II of fixed-bed catalytic is 140 DEG C, and reaction pressure is 35 kilograms, flow 80ml/
min；Cooling tank is -5 DEG C, and liquid received in head tank II is squeezed into the micro- reactor tank II of fixed-bed catalytic by constant flow pump II6,
Logical hydrogen reaction, receives.In successive reaction, product sample three times and mixed once sample are taken, high performance liquid chromatography detection is used
After obtain, the conversion ratio of reaction is 97.46%.
Embodiment 2:
It takes 22.4g paranitrobenzoic acid to be dissolved in ethanol solution (mass percentage of ethyl alcohol is 99.9%), is configured to
The paranitrobenzoic acid solution that percentage composition is 4%, is put into the head tank I1 of micro-reactor apparatus and recycles.It is micro- in fixed-bed catalytic
Azochlorosulfonate acid resin catalyst is loaded in reactor tank I3, and palladium-carbon catalyst or the catalysis of platinum aluminium are loaded in the micro- reactor tank II of fixed-bed catalytic
Agent, sets the head tank I1 temperature of micro-reactor apparatus as 70 DEG C, 80 DEG C of the micro- reactor tank I3 temperature of fixed-bed catalytic, and reaction pressure is
0.4MPa, flow 5ml/min.Constant flow pump I5 is opened, carries out esterification after solution is squeezed into the micro- reactor tank I3 of fixed-bed catalytic,
Reaction product receives in head tank II.Again after the micro- reactor tank II4 nitrogen of fixed-bed catalytic, hydrogen displacement three times, setting
Head tank II temperature is 70 DEG C, and the micro- reactor tank II of fixed-bed catalytic is 140 DEG C, and reaction pressure is 17 kilograms, flow 80ml/
min；Cooling tank is -5 DEG C, and liquid received in head tank II is squeezed into the micro- reactor tank of fixed-bed catalytic by constant flow pump II6
II4 leads to hydrogen reaction, receives.In successive reaction, product sample three times and mixed once sample are taken, high performance liquid chromatography is used
It is obtained after detection, the conversion ratio of reaction is 96.53%.
Embodiment 3:
It takes 22.4g paranitrobenzoic acid to be dissolved in ethanol solution (mass percentage of ethyl alcohol is 99.9%), is configured to
The paranitrobenzoic acid solution that percentage composition is 4%, is put into the head tank I1 of micro-reactor apparatus and recycles.It is micro- in fixed-bed catalytic
Azochlorosulfonate acid resin catalyst is loaded in reactor tank I3, and palladium-carbon catalyst or the catalysis of platinum aluminium are loaded in the micro- reactor tank II4 of fixed-bed catalytic
Agent, sets the head tank I temperature of micro-reactor apparatus as 70 DEG C, 80 DEG C of the micro- reactor tank I temperature of fixed-bed catalytic, and reaction pressure is
0.4MPa, flow 5ml/min.Constant flow pump I5 is opened, carries out esterification after solution is squeezed into the micro- reactor tank I3 of fixed-bed catalytic,
Reaction product receives in head tank II.Again after the micro- reactor tank II4 nitrogen of fixed-bed catalytic, hydrogen displacement three times, setting
Head tank II temperature is 70 DEG C, and the micro- reactor tank II of fixed-bed catalytic is 140 DEG C, and reaction pressure is 35 kilograms, flow 120ml/
min；Cooling tank is -5 DEG C, and liquid received in head tank II is squeezed into the micro- reactor tank II4 of fixed-bed catalytic, leads to hydrogen reaction,
It receives.In successive reaction, product sample three times and mixed once sample are taken, with being obtained after high performance liquid chromatography detection, is reacted
Conversion ratio be 91.86%.
Micro-reactor apparatus used in above embodiments is purchased from Changzhou Rui Xi Biotechnology Co., Ltd, and ethyl alcohol is point
It analyses pure, is purchased from Jiangsu Yongfeng chemical reagent Co., Ltd.
Particular embodiments described above, pair present invention solves the technical problem that, technical scheme and beneficial effects carry out
It is further described, it should be understood that the above is only a specific embodiment of the present invention, is not limited to this
Invention, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in this hair
Within bright protection scope.
In the description of the present invention, it is to be understood that, indicating position or the term of positional relationship are based on shown in attached drawing
Orientation or positional relationship, be merely for convenience of description of the present invention and simplification of the description, rather than the equipment of indication or suggestion meaning
Or element must have a particular orientation, be constructed and operated in a specific orientation, therefore be not considered as limiting the invention.
In the present invention unless specifically defined or limited otherwise, term " installation ", " connected ", " connection ", " fixation " etc.
Term shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or integral；It can be mechanical connect
It connects, is also possible to be electrically connected；It can be directly connected, can also can be in two elements indirectly connected through an intermediary
The interaction relationship of the connection in portion or two elements.It for the ordinary skill in the art, can be according to specific feelings
Condition understands the concrete meaning of above-mentioned term in the present invention.
In the description of the present invention, it should be noted that term " center ", "upper", "lower", "left", "right", "vertical",
The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, or be somebody's turn to do
Invention product using when the orientation or positional relationship usually put, be merely for convenience of description of the present invention and simplification of the description, without
It is that the device of indication or suggestion meaning or element must have a particular orientation, be constructed and operated in a specific orientation, therefore not
It can be interpreted as limitation of the present invention.In addition, term " first ", " second ", " third " etc. are only used for distinguishing description, and cannot manage
Solution is indication or suggestion relative importance.
In addition, the terms such as term "horizontal", "vertical", " pendency " are not offered as requiring component abswolute level or pendency, and
It is that can be slightly tilted.It is not to indicate the structure if "horizontal" only refers to that its direction is more horizontal with respect to for "vertical"
It has to fully horizontally, but can be slightly tilted.
In the present invention unless specifically defined or limited otherwise, fisrt feature can be on or below second feature
Directly contacted including the first and second features, also may include the first and second features be not direct contact but by them it
Between other characterisation contact.Moreover, fisrt feature is on second feature, top and above include fisrt feature second spy
Right above sign and oblique upper, or first feature horizontal height is merely representative of higher than second feature.Fisrt feature second feature it
Under, lower section and fisrt feature included below be directly below and diagonally below the second feature, or be merely representative of first feature horizontal height
Less than second feature.
Claims (12)
1. a kind of micro-reactor apparatus, it is at least made of a unit, which is characterized in that the unit includes head tank
I(1), head tank II(2), the micro- reactor tank I(3 of fixed-bed catalytic), the micro- reactor tank II(4 of fixed-bed catalytic), constant flow pump I(5), it is permanent
Stream pump II(6), cooling tank (7), receiving tank (8) and the gas heating tank (9)；Wherein,
The constant flow pump I(5) import be connected with the head tank I(1), the constant flow pump I(5) outlet and the fixed bed
Be catalyzed micro- reactor tank I(3) import be connected so that the constant flow pump I(5) material of the head tank I(1) is pumped into it is described solid
Fixed bed is catalyzed micro- reactor tank I(3) in；
The micro- reactor tank I(3 of fixed-bed catalytic) product exit be connected with the import of the head tank II(2) so that described
The micro- reactor tank I(3 of fixed-bed catalytic) generate product enter the head tank II(2)；
The constant flow pump II(6) import be connected with the outlet of the head tank II(2), the constant flow pump II(6) outlet with
The micro- reactor tank II(4 of fixed-bed catalytic) the first import be connected so that the constant flow pump II(6) by the head tank II
(2) material is pumped into the micro- reactor tank II(4 of the fixed-bed catalytic) in；
The import of the gas heating tank (9) for feeding hydrogen and nitrogen or hydrogen, the outlet of the gas heating tank (9) with
The micro- reactor tank II(4 of fixed-bed catalytic) the second import be connected, with to the micro- reactor tank II(4 of the fixed-bed catalytic) at least
It is passed through hydrogen；
The micro- reactor tank II(4 of fixed-bed catalytic) in be equipped be connected with the first import with for by the material being pumped into atomization simultaneously and
The atomizer for the hydrogen mixing being passed through；
The import of the cooling tank (7) is connected with the product exit of the micro- reactor tank II(4 of the fixed-bed catalytic), the cooling tank
(7) outlet is connected with the receiving tank (8).
2. micro-reactor apparatus according to claim 1, which is characterized in that
It further include constent temperature heater, the constent temperature heater is urged with the head tank I(1), head tank II(2), fixed bed respectively
Change micro- reactor tank I(3), the micro- reactor tank II(4 of fixed-bed catalytic) be connected with the collet of cooling tank (7).
3. micro-reactor apparatus according to claim 1, which is characterized in that
The aperture of the atomizer is 0.5mm.
4. micro-reactor apparatus according to claim 1, which is characterized in that
The receiving tank (8) is the head tank I(1 of next unit).
5. micro-reactor apparatus according to claim 1, which is characterized in that
The constant flow pump I(5) outlet be also connected with the import of the head tank I(1), with pass through the constant flow pump I(5) circulation
The head tank I(1) in material.
6. micro-reactor apparatus according to claim 1, which is characterized in that
The constant flow pump II(6) outlet be also connected with the import of the head tank II(2), with pass through the constant flow pump II(6)
Recycle the head tank II(2) in material.
7. micro-reactor apparatus according to claim 1, which is characterized in that
The import of the gas heating tank (9) by air inlet valve group be connected with hydrogen gas cylinder and nitrogen cylinder or with hydrogen gas cylinder phase
Even.
8. a kind of method for synthesizing benzocainum, it is characterised in that method is micro- anti-as described in any one of claims 1 to 7
It answers in equipment and carries out.
9. the method for synthesis benzocainum according to claim 8, it is characterised in that include: in the step of method
The paranitrobenzoic acid solution that solvent is ethyl alcohol is placed in head tank I(1), it will be in head tank I(1) by constant flow pump I(5)
Paranitrobenzoic acid solution be pumped into the micro- reactor tank I(3 of fixed-bed catalytic) in, in the micro- reactor tank I(3 of fixed-bed catalytic) in urge
Esterification is carried out under the action of agent, obtains ethyl p-nitrobenzoate solution；
Ethyl p-nitrobenzoate solution is placed in head tank II(2), by constant flow pump II(6) by pair in head tank II(2)
Ethyl nitrobenzoate solution is pumped into the micro- reactor tank II(4 of fixed-bed catalytic) in be atomized by atomizer and with the hydrogen that is passed through
Mixing, in the micro- reactor tank II(4 of fixed-bed catalytic) in catalyst under the action of carry out hydrogenation, after by processing obtain benzene
Help cacaine.
10. the method for synthesis benzocainum according to claim 9, which is characterized in that
Head tank I(1) temperature be 70 DEG C, the micro- reactor tank I(3 of fixed-bed catalytic) 80 ~ 85 DEG C of temperature, reaction pressure 0.4MPa,
Feed rate is 5ml/min；
Head tank II(2) temperature be 70 ~ 80 DEG C, the micro- reactor tank II(4 of fixed-bed catalytic) temperature be 140 DEG C, reaction pressure be 17 ~
35 kilograms, feed rate is 80 ~ 120ml/min.
11. the method for synthesis benzocainum according to claim 9, which is characterized in that
The micro- reactor tank I(3 of fixed-bed catalytic) in catalyst be azochlorosulfonate acid resin catalyst；
And/or the micro- reactor tank II(4 of fixed-bed catalytic) in catalyst be palladium-carbon catalyst or platinum Al catalysts.
12. the method for synthesis benzocainum according to claim 7, which is characterized in that
Before using micro-reactor apparatus synthesis benzocainum, to constant flow pump I(5) and constant flow pump II(6) it is carried out using dehydrated alcohol
Calibration.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112934137A (en) * | 2021-01-28 | 2021-06-11 | 常州飞达新材料科技有限公司 | Multi-layer packed bed micro-reactor for benzocaine and reaction method |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3037046A (en) * | 1958-10-24 | 1962-05-29 | Abbott Lab | Benzocaine process |
| RU2302405C1 (en) * | 2006-01-27 | 2007-07-10 | Дагестанский государственный университет | P-aminobenzoic acid ethyl ester (anestesine) production process |
| CN102580643A (en) * | 2011-12-30 | 2012-07-18 | 微楷化学（大连）有限公司 | Micro-reaction device and application thereof in synthesis of glycidyl methacrylate |
| CN105315168A (en) * | 2015-11-27 | 2016-02-10 | 常州永和精细化学有限公司 | Environment-friendly preparation process of N-(4-ethoxy carbonyl phenyl)-N'-methyl-N'-phenyl formamidine intermediate |
| CN105348108A (en) * | 2015-12-08 | 2016-02-24 | 浙江优创材料科技股份有限公司 | Preparation method of dimethyl ethyl aminobenzoate midbody nitrobenzoic acid ethyl ester |
| CN105481707A (en) * | 2015-12-08 | 2016-04-13 | 浙江优创材料科技股份有限公司 | Preparation method of ethyl-4-dimethylaminobenzoate intermediate benzocaine |
| CN210279110U (en) * | 2019-05-31 | 2020-04-10 | 常州瑞曦生物科技有限公司 | Micro-reaction equipment |
| CN216005722U (en) * | 2021-07-31 | 2022-03-11 | 大连新阳光材料科技有限公司 | Production system for preparing ethyl p-aminobenzoate through continuous reaction |
-
2019
- 2019-05-31 CN CN201910467800.7A patent/CN110075773A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3037046A (en) * | 1958-10-24 | 1962-05-29 | Abbott Lab | Benzocaine process |
| RU2302405C1 (en) * | 2006-01-27 | 2007-07-10 | Дагестанский государственный университет | P-aminobenzoic acid ethyl ester (anestesine) production process |
| CN102580643A (en) * | 2011-12-30 | 2012-07-18 | 微楷化学（大连）有限公司 | Micro-reaction device and application thereof in synthesis of glycidyl methacrylate |
| CN105315168A (en) * | 2015-11-27 | 2016-02-10 | 常州永和精细化学有限公司 | Environment-friendly preparation process of N-(4-ethoxy carbonyl phenyl)-N'-methyl-N'-phenyl formamidine intermediate |
| CN105348108A (en) * | 2015-12-08 | 2016-02-24 | 浙江优创材料科技股份有限公司 | Preparation method of dimethyl ethyl aminobenzoate midbody nitrobenzoic acid ethyl ester |
| CN105481707A (en) * | 2015-12-08 | 2016-04-13 | 浙江优创材料科技股份有限公司 | Preparation method of ethyl-4-dimethylaminobenzoate intermediate benzocaine |
| CN210279110U (en) * | 2019-05-31 | 2020-04-10 | 常州瑞曦生物科技有限公司 | Micro-reaction equipment |
| CN216005722U (en) * | 2021-07-31 | 2022-03-11 | 大连新阳光材料科技有限公司 | Production system for preparing ethyl p-aminobenzoate through continuous reaction |
Non-Patent Citations (3)
| Title |
|---|
| 李丽娟等: "《过程控制》", 31 May 2019, 南京：东南大学出版社, pages: 87 * |
| 李文丽;赵杰;崔玉洁;: "苯佐卡因的合成工艺研究", 当代化工研究, no. 11 * |
| 穆金霞;殷学锋;: "微通道反应器在合成反应中的应用", 化学进展, no. 01, pages 293 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112934137A (en) * | 2021-01-28 | 2021-06-11 | 常州飞达新材料科技有限公司 | Multi-layer packed bed micro-reactor for benzocaine and reaction method |
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