CN102875493B - The method of epoxy aliphatic acid methyl ester is prepared in Continuous Flow micro passage reaction - Google Patents
The method of epoxy aliphatic acid methyl ester is prepared in Continuous Flow micro passage reaction Download PDFInfo
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Abstract
The present invention relates to a kind of method utilizing micro passage reaction to prepare epoxy aliphatic acid methyl ester, its concrete steps are as follows: first catalyzer formic acid and concentrated hydrochloric acid are prepared by a certain percentage, respectively by three volume pumps, fatty acid methyl ester, Catalyzed by Formic Acid agent and hydrogen peroxide are squeezed in micro passage reaction again, reaction product is washed, be separated and drying, obtain final product epoxy aliphatic acid methyl ester; The whole process of the present invention is thermopositive reaction, and peroxyformic acid and epoxy aliphatic acid methyl ester synthesize simultaneously.Use the present invention to produce epoxy aliphatic acid methyl ester, effectively can control the temperature of reaction process, security is high, module good mixing effect, and the product quality be obtained by reacting is high, and the present invention is Continuous Flow reaction, and process is continuous, and production efficiency is high.
Description
Technical field
The present invention relates to and utilize micro passage reaction to carry out fatty acid methyl ester epoxidation reaction, particular content comprises and utilizes the channel module that be made up of multiple miniature complete mixing flow structural unit to be combined into enhancing mixed type micro passage reaction (the high-throughput micro passage reaction of such as Corning Inc. Corning Incorporated), this reactor is utilized to synthesize the method for softening agent epoxy aliphatic acid methyl ester, that a kind of oxygenant peroxyformic acid that completes in micro passage reaction configures, raw material preheating, the continuous flow process process of epoxidization reaction process.Present method can under 30 ~ 70 DEG C of reaction conditionss the synthesizing epoxy fatty acid methyl ester of continuous safety.
Technical background
Epoxy aliphatic acid methyl ester is light yellow liquid at normal temperatures, the novel environment-friendlyplasticizer plasticizer of to be a kind of with crude vegetal be raw material.It can substitute dioctyl phthalate (DOP) (DOP) or dibutyl phthalate (DBP) effectively, for polyvinyl chloride plastic material products, epoxy aliphatic acid methyl ester is added in polyvinyl chloride plastic material products, the cost of manufacture of this type of material can not only be made to decrease, its many physicals, as resist processing, heat-resistant aging, folding resistance etc. also can be improved to some extent; In the course of processing of polyvinyl chloride film or leatheroid, used as additive by epoxy aliphatic acid methyl ester, effect is better.
The traditional synthetic method of epoxy aliphatic acid methyl ester be fatty acid methyl ester, formic acid, hydrogen peroxide under sulphuric acid catalysis effect at 45 ~ 65 DEG C in tank reactor stirring reaction tens hours, reaction terminates rear static layering, removing aqueous phase, then obtain product epoxy aliphatic acid methyl ester by underpressure distillation.There is long reaction time in this technique, hydrogen peroxide consumption is large, the shortcoming such as easily to blast.
CN 10239120 A disclose a kind of fatty acid methyl ester is mixed with formic acid, phosphoric acid heat up after add hydrogen peroxide, first react in atmospheric conditions, then react under vacuum, then vacuum breaker is to normal pressure, then again add hydrogen peroxide, successively react under normal pressure and vacuum condition.The method speed of reaction improves, and oxirane value is promoted to 3.5% ~ 5.0%
CN 101284821 A discloses a kind of based on ionic liquid-catalyzed epoxy aliphatic acid methyl ester preparation method, iodine number is greater than the fatty acid methyl ester 100 parts of 80, after 10 ~ 30 parts, formic acid, ionic-liquid catalyst 1-10 part mixes, stirring is warming up to 50-70 DEG C, drip concentration 28-55% hydrogen peroxide 30-70 part, control to drip off in two hours, continue reaction 3-6 hour, oxirane value reaches more than 3%.
More than invent and all adopt traditional batch tank reactor, feed way is also the dropwise dropping adopted, although substantially increase the speed of reaction and the quality of product, but, because the generation of peroxy acid in this reaction is a strong exothermal reaction, react the sharply rising along with temperature, therefore for reaction safety or very difficult control.
Summary of the invention
It is long to the present invention be directed to the traditional mode of production epoxy aliphatic acid methyl ester procedure time, and oxirane value is low, and reaction process security is difficult to a kind of novel efficient Continuous Flow production technique that the problems such as control propose.Raw material volume pump is squeezed in reactor, the kinetic energy of liquid dependence own completes mixing mass transfer in the module, without the need to the device that applied mechanical stirs, its mixed effect will be far superior to stir the mass transfer effect produced, and in micro passage reaction, greatly can improve the control to temperature of reaction, avoid the phenomenon having local superheating in process, improve security.
For achieving the above object, the technical solution used in the present invention is:
Use micro passage reaction to prepare a method for epoxy aliphatic acid methyl ester, concrete steps are as follows:
1) catalyst preparation: under room temperature, by formic acid solution and concentrated hydrochloric acid mix and blend by a certain percentage, is mixed with homogeneous phase solution, stand-by as catalyzer.
2) catalyzer of upper step gained is with this reaction raw materials fatty acid methyl ester via two volume pumps, squeezes into first piece of module preheating of micro passage reaction by a certain percentage; Oxidant hydrogen peroxide squeezes into reactor second piece of module preheating by the 3rd volume pump, and preheating temperature is identical with temperature of reaction; Three strands of materials, entering after the 3rd piece of module start mass transfer reaction, continue through a series of quality transmission type module sustained reaction, pick out finally by after coil pipe cooling; Reaction process residence time in micro passage reaction is 80 ~ 150s, and temperature of reaction is 30 ~ 70 DEG C, and reaction pressure is 0 ~ 8bar.
3) product obtained through separatory, washing, centrifugal and dewater by anhydrous sodium sulphate, obtain the last product needed.
Wherein said mass transfer enhancement type micro passage reaction module, in this module Micro Channel Architecture be once-through type channel architecture as or strengthen mixing cardioid channel architecture.
The micro passage reaction that the present invention relates to is formed by polylith module assembled, is divided into once-through type channel module and strengthens mixed type channel module by structure.The material of this module is silicon single crystal, special glass, pottery, the stainless steel scribbling corrosion resistant coating or metal alloy, tetrafluoroethylene etc.Reactive system can be anticorrosion withstand voltage, and it is different and different that voltage endurance capability looks material, and reacting Maximum safe pressure in system is 15 ~ 30bar.
The present invention carries out Continuous Flow fatty acid methyl ester epoxidation, and system comprises raw material preheating module and reaction module, and concrete module number is determined by reaction time.Method of attachment is: catalyzer and raw material preheating module and oxidizer preheat wired in parallel, then connects with epoxidation reaction module group.
Fatty acid methyl ester epoxidation of the present invention catalyzer used is formic acid (88%) and concentrated hydrochloric acid (35%) mixture, and wherein the mol ratio of formic acid and concentrated hydrochloric acid is 45:1 ~ 15:1; Oxygenant is hydrogen peroxide (35%), and wherein the mol ratio of hydrogen peroxide and fatty acid methyl ester is 1:1 ~ 5:1.
Provided by the inventionly in Continuous Flow micro passage reaction, carry out epoxidation with Continuous Flow reactive mode prepare epoxy aliphatic acid methyl ester, raw material all squeezes into micro passage reaction by volume pump.Reactor carrys out the temperature needed for fine adjustment reaction by adjustment recirculation cooler, and the actual temperature of reaction is recorded by thermopair.In reaction process, by the mol ratio regulating the flow of volume pump to come feed change and oxygenant, raw material is after tensimeter, safety valve, check valve, and the pressure in reaction system is recorded by tensimeter monitoring.Raw material first carries out preheating respectively in micro passage reaction, then hybrid reaction, after tens seconds to the residence time of several minutes, obtains epoxidation product epoxy aliphatic acid methyl ester at discharge port.
The production method of the epoxy aliphatic acid methyl ester that the present invention relates to has following characteristics compared with prior art:
1) native system is Continuous Flow reaction, and the reaction times is only several seconds to several minutes, substantially reduces the reaction times.
2) the mass transfer enhancement mixed type module that native system uses improves the mass transfer mixed effect of material, adds the transformation efficiency of reaction, improves the oxirane value of product.
3) the equipment micro passage reaction adopted accurately controls temperature of reaction by recirculation cooler, and good heat-transfer process keeps homo(io)thermism; The pressure of real-time detection reaction system, ensures the safety of process.
Accompanying drawing explanation
Fig. 1 is the process flow diagram that invention fatty acid methyl ester epoxidation prepares epoxy aliphatic acid methyl ester;
Fig. 2 is the reactor used module map of the present invention; 1-Corning craspedodrome channel module, 2-Corning cardioid module;
Fig. 3 is Continuous Flow micro passage reaction setting drawing used in the present invention; 1,2,3-head tank, 4,5,6-volume pump, 7,8,9-tensimeter, 11-Corning craspedodrome channel module, 10,12,13-Corning strengthens mixing module, 14-product collection tank, 15-recirculation cooler.
Embodiment
The foregoing describe the present invention, the illustrative explanation of following examples implementation result of the present invention, can not be interpreted as it is limiting the scope of the invention.
The following example system carries out in microreactor according to the requirement of the inventive method.With reference to Fig. 1 technical process of the present invention, the reactor used module map of composition graphs 2 the present invention; 1-Corning craspedodrome channel module, 2-Corning cardioid module;
Utilize the setting drawing of Fig. 3, according to following step: the Catalyzed by Formic Acid agent in fatty acid methyl ester in head tank 1 and head tank 2 is squeezed in cardioid module 10 via volume pump 4 volume pump 5 and carried out a mixed preheating by (1) respectively, by tensimeter 7,8 testing process pressure, temperature is set by recirculation cooler 15; (2) hydrogen peroxide in head tank 3 is squeezed in craspedodrome channel module 11 and is carried out preheating by volume pump 6, detects wherein pressure by tensimeter 9; (3) preheated raw material enters mixing module 12,13, at the temperature set, carry out hybrid reaction; (4) by the product access product tank 14 that microchannel is obtained by reacting, then through washing, after being separated drying, final product is obtained.
Embodiment 1
(1) device: Corning high-throughput micro passage reaction, determine craspedodrome channel module number according to material number of share of stock, hybrid reaction number of modules is determined according to flow velocity and reaction time, and model calling mode is determined with reference to Fig. 3, and heat transferring medium is thermal oil.
(2) catalyst preparation: accurately take 640g formic acid and 40g concentrated hydrochloric acid, pour in beaker and stir, sealing saves backup.
(3) volumetric flow rate of pump 1 pump 2 pump 3 is set than being Catalyzed by Formic Acid agent: fatty acid methyl ester: hydrogen peroxide=0.5:1:1, after three strands of materials are mixed by module 10, module 11 preheating respectively, used time enters module 12 and reacts, recirculation cooler setting temperature of reaction is 42 DEG C, and now the mol ratio of fatty acid methyl ester and hydrogen peroxide is 1:1.
Product is through washing, and separatory, after drying, measure (hydrochloric acid acetone) according to GBT_1677-1981 softening agent oxirane value and carry out titration detection to product, the product oxirane value of survey is 2.78%
Embodiment 2
(1) device: Corning high-throughput micro passage reaction, determine craspedodrome channel module number according to material number of share of stock, hybrid reaction number of modules is determined according to flow velocity and reaction time, and model calling mode is determined with reference to Fig. 3, and heat transferring medium is thermal oil.
(2) catalyst preparation: accurately take 640g formic acid and 40g concentrated hydrochloric acid, pour in beaker and stir, sealing saves backup.
(3) volumetric flow rate of pump 1 pump 2 pump 3 is set than being Catalyzed by Formic Acid agent: fatty acid methyl ester: hydrogen peroxide=0.5:1:1.5, after three strands of materials are mixed by module 10, module 11 preheating respectively, used time enters module 12 and reacts, recirculation cooler setting temperature of reaction is 42 DEG C, and now the mol ratio of fatty acid methyl ester and hydrogen peroxide is 1:1.5.
Product is through washing, and separatory, after drying, measure (hydrochloric acid acetone) according to GBT_1677-1981 softening agent oxirane value and carry out titration detection to product, the product oxirane value of survey is 3.57%
Embodiment 3
(1) device: Corning high-throughput micro passage reaction, determine craspedodrome channel module number according to material number of share of stock, hybrid reaction number of modules is determined according to flow velocity and reaction time, and model calling mode is determined with reference to Fig. 3, and heat transferring medium is thermal oil.
(2) catalyst preparation: accurately take 640g formic acid and 40g concentrated hydrochloric acid, pour in beaker and stir, sealing saves backup.
(3) volumetric flow rate of pump 1 pump 2 pump 3 is set than being Catalyzed by Formic Acid agent: fatty acid methyl ester: hydrogen peroxide=1.0:1:2.5, after three strands of materials are mixed by module 10, module 11 preheating respectively, used time enters module 12 and reacts, setting temperature of reaction is 42 DEG C, and now the mol ratio of fatty acid methyl ester and hydrogen peroxide is 1:2.5.
Product is through washing, and separatory, after drying, measure (hydrochloric acid acetone) according to GBT_1677-1981 softening agent oxirane value and carry out titration detection to product, the product oxirane value of survey is 4.03%
Embodiment 4
(1) device: Corning high-throughput micro passage reaction, determine craspedodrome channel module number according to material number of share of stock, hybrid reaction number of modules is determined according to flow velocity and reaction time, and model calling mode is determined with reference to Fig. 3, and heat transferring medium is thermal oil.
(2) catalyst preparation: accurately take 640g formic acid and 40g concentrated hydrochloric acid, pour in beaker and stir, sealing saves backup.
(3) volumetric flow rate of pump 1 pump 2 pump 3 is set than being Catalyzed by Formic Acid agent: fatty acid methyl ester: hydrogen peroxide=1.0:1:2.5, after three strands of materials are mixed by module 10, module 11 preheating respectively, used time enters module 12 and reacts, recirculation cooler setting temperature of reaction is 52 DEG C, and now the mol ratio of fatty acid methyl ester and hydrogen peroxide is 1:2.5.
Product is through washing, and separatory, after drying, measure (hydrochloric acid acetone) according to GBT_1677-1981 softening agent oxirane value and carry out titration detection to product, the product oxirane value of survey is 5.17%
Embodiment 5
(1) device: Corning high-throughput micro passage reaction, determine craspedodrome channel module number according to material number of share of stock, hybrid reaction number of modules is determined according to flow velocity and reaction time, and model calling mode is determined with reference to Fig. 3, and heat transferring medium is thermal oil.
(2) catalyst preparation: accurately take 640g formic acid and 40g concentrated hydrochloric acid, pour in beaker and stir, sealing saves backup.
(3) volumetric flow rate of pump 1 pump 2 pump 3 is set than being Catalyzed by Formic Acid agent: fatty acid methyl ester: hydrogen peroxide=1.5:1:2.5, after three strands of materials are mixed by module 10, module 11 preheating respectively, used time enters module 12 and reacts, recirculation cooler setting temperature of reaction is 62 DEG C, and now the mol ratio of fatty acid methyl ester and hydrogen peroxide is 1:2.5.
Product is through washing, and separatory, after drying, measure (hydrochloric acid acetone) according to GBT_1677-1981 softening agent oxirane value and carry out titration detection to product, the product oxirane value of survey is 4.98%.
Claims (1)
1. in Continuous Flow micro passage reaction, prepare the method for epoxy aliphatic acid methyl ester, it is characterized in that, with reference to Fig. 1 technical process of the present invention, the reactor used module map of composition graphs 2 the present invention; 1-Corning craspedodrome channel module, 2-Corning cardioid module;
Utilize the setting drawing of Fig. 3, according to following step: fatty acid methyl ester in head tank 1 is squeezed in cardioid module 10 via volume pump 4 volume pump 5 with the Catalyzed by Formic Acid agent in head tank 2 and carried out mixing preheating by (1) respectively, by tensimeter 7,8 testing process pressure, temperature is set by recirculation cooler 15; (2) hydrogen peroxide in head tank 3 is squeezed in craspedodrome channel module 11 and is carried out preheating by volume pump 6, detects wherein pressure by tensimeter 9; (3) preheated raw material enters mixing module 12,13, at the temperature set, carry out hybrid reaction; (4) by the product access product tank 14 that microchannel is obtained by reacting, then through washing, after being separated drying, final product is obtained;
Concrete steps are:
(1) device: Corning high-throughput micro passage reaction, determine craspedodrome channel module number according to material number of share of stock, hybrid reaction number of modules is determined according to flow velocity and reaction time, and model calling mode is determined with reference to Fig. 3, and heat transferring medium is thermal oil;
(2) catalyst preparation: accurately take 640g formic acid and 40g concentrated hydrochloric acid, pour in beaker and stir, sealing saves backup;
The volumetric flow rate of setting pump 1 pump 2 pump 3 is than being Catalyzed by Formic Acid agent: fatty acid methyl ester: hydrogen peroxide=0.5:1:1, after three strands of materials are mixed by module 10, module 11 preheating respectively, enter module 12 to react simultaneously, recirculation cooler setting temperature of reaction is 42 DEG C, and now the mol ratio of fatty acid methyl ester and hydrogen peroxide is 1:1.
2. in Continuous Flow micro passage reaction, prepare the method for epoxy aliphatic acid methyl ester, it is characterized in that, with reference to Fig. 1 technical process of the present invention, the reactor used module map of composition graphs 2 the present invention; 1-Corning craspedodrome channel module, 2-Corning cardioid module;
Utilize the setting drawing of Fig. 3, according to following step: fatty acid methyl ester in head tank 1 is squeezed in cardioid module 10 via volume pump 4 volume pump 5 with the Catalyzed by Formic Acid agent in head tank 2 and carried out mixing preheating by (1) respectively, by tensimeter 7,8 testing process pressure, temperature is set by recirculation cooler 15; (2) hydrogen peroxide in head tank 3 is squeezed in craspedodrome channel module 11 and is carried out preheating by volume pump 6, detects wherein pressure by tensimeter 9; (3) preheated raw material enters mixing module 12,13, at the temperature set, carry out hybrid reaction; (4) by the product access product tank 14 that microchannel is obtained by reacting, then through washing, after being separated drying, final product is obtained;
Concrete steps are:
(1) device: Corning high-throughput micro passage reaction, determine craspedodrome channel module number according to material number of share of stock, hybrid reaction number of modules is determined according to flow velocity and reaction time, and model calling mode is determined with reference to Fig. 3, and heat transferring medium is thermal oil;
(2) catalyst preparation: accurately take 640g formic acid and 40g concentrated hydrochloric acid, pour in beaker and stir, sealing saves backup;
(3) volumetric flow rate of pump 1 pump 2 pump 3 is set than being Catalyzed by Formic Acid agent: fatty acid methyl ester: hydrogen peroxide=0.5:1:1.5, after three strands of materials are mixed by module 10, module 11 preheating respectively, enter module 12 to react simultaneously, recirculation cooler setting temperature of reaction is 42 DEG C, and now the mol ratio of fatty acid methyl ester and hydrogen peroxide is 1:1.5.
3. in Continuous Flow micro passage reaction, prepare the method for epoxy aliphatic acid methyl ester, it is characterized in that, with reference to Fig. 1 technical process of the present invention, the reactor used module map of composition graphs 2 the present invention; 1-Corning craspedodrome channel module, 2-Corning cardioid module;
Utilize the setting drawing of Fig. 3, according to following step: fatty acid methyl ester in head tank 1 is squeezed in cardioid module 10 via volume pump 4 volume pump 5 with the Catalyzed by Formic Acid agent in head tank 2 and carried out mixing preheating by (1) respectively, by tensimeter 7,8 testing process pressure, temperature is set by recirculation cooler 15; (2) hydrogen peroxide in head tank 3 is squeezed in craspedodrome channel module 11 and is carried out preheating by volume pump 6, detects wherein pressure by tensimeter 9; (3) preheated raw material enters mixing module 12,13, at the temperature set, carry out hybrid reaction; (4) by the product access product tank 14 that microchannel is obtained by reacting, then through washing, after being separated drying, final product is obtained;
Concrete steps are:
(1) device: Corning high-throughput micro passage reaction, determine craspedodrome channel module number according to material number of share of stock, hybrid reaction number of modules is determined according to flow velocity and reaction time, and model calling mode is determined with reference to Fig. 3, and heat transferring medium is thermal oil;
(2) catalyst preparation: accurately take 640g formic acid and 40g concentrated hydrochloric acid, pour in beaker and stir, sealing saves backup;
The volumetric flow rate of setting pump 1 pump 2 pump 3 is than being Catalyzed by Formic Acid agent: fatty acid methyl ester: hydrogen peroxide=1.0:1:2.5, after three strands of materials are mixed by module 10, module 11 preheating respectively, enter module 12 to react simultaneously, setting temperature of reaction is 42 DEG C, and now the mol ratio of fatty acid methyl ester and hydrogen peroxide is 1:2.5.
4. in Continuous Flow micro passage reaction, prepare the method for epoxy aliphatic acid methyl ester, it is characterized in that, with reference to Fig. 1 technical process of the present invention, the reactor used module map of composition graphs 2 the present invention; 1-Corning craspedodrome channel module, 2-Corning cardioid module;
Utilize the setting drawing of Fig. 3, according to following step: fatty acid methyl ester in head tank 1 is squeezed in cardioid module 10 via volume pump 4 volume pump 5 with the Catalyzed by Formic Acid agent in head tank 2 and carried out mixing preheating by (1) respectively, by tensimeter 7,8 testing process pressure, temperature is set by recirculation cooler 15; (2) hydrogen peroxide in head tank 3 is squeezed in craspedodrome channel module 11 and is carried out preheating by volume pump 6, detects wherein pressure by tensimeter 9; (3) preheated raw material enters mixing module 12,13, at the temperature set, carry out hybrid reaction; (4) by the product access product tank 14 that microchannel is obtained by reacting, then through washing, after being separated drying, final product is obtained;
Concrete steps are:
(1) device: Corning high-throughput micro passage reaction, determine craspedodrome channel module number according to material number of share of stock, hybrid reaction number of modules is determined according to flow velocity and reaction time, and model calling mode is determined with reference to Fig. 3, and heat transferring medium is thermal oil;
(2) catalyst preparation: accurately take 640g formic acid and 40g concentrated hydrochloric acid, pour in beaker and stir, sealing saves backup;
The volumetric flow rate of setting pump 1 pump 2 pump 3 is than being Catalyzed by Formic Acid agent: fatty acid methyl ester: hydrogen peroxide=1.0:1:2.5, after three strands of materials are mixed by module 10, module 11 preheating respectively, enter module 12 to react simultaneously, recirculation cooler setting temperature of reaction is 52 DEG C, and now the mol ratio of fatty acid methyl ester and hydrogen peroxide is 1:2.5.
5. in Continuous Flow micro passage reaction, prepare the method for epoxy aliphatic acid methyl ester, it is characterized in that, with reference to Fig. 1 technical process of the present invention, the reactor used module map of composition graphs 2 the present invention; 1-Corning craspedodrome channel module, 2-Corning cardioid module;
Utilize the setting drawing of Fig. 3, according to following step: fatty acid methyl ester in head tank 1 is squeezed in cardioid module 10 via volume pump 4 volume pump 5 with the Catalyzed by Formic Acid agent in head tank 2 and carried out mixing preheating by (1) respectively, by tensimeter 7,8 testing process pressure, temperature is set by recirculation cooler 15; (2) hydrogen peroxide in head tank 3 is squeezed in craspedodrome channel module 11 and is carried out preheating by volume pump 6, detects wherein pressure by tensimeter 9; (3) preheated raw material enters mixing module 12,13, at the temperature set, carry out hybrid reaction; (4) by the product access product tank 14 that microchannel is obtained by reacting, then through washing, after being separated drying, final product is obtained;
Concrete steps are:
(1) device: Corning high-throughput micro passage reaction, determine craspedodrome channel module number according to material number of share of stock, hybrid reaction number of modules is determined according to flow velocity and reaction time, and model calling mode is determined with reference to Fig. 3, and heat transferring medium is thermal oil;
(2) catalyst preparation: accurately take 640g formic acid and 40g concentrated hydrochloric acid, pour in beaker and stir, sealing saves backup;
(3) volumetric flow rate of pump 1 pump 2 pump 3 is set than being Catalyzed by Formic Acid agent: fatty acid methyl ester: hydrogen peroxide=1.5:1:2.5, after three strands of materials are mixed by module 10, module 11 preheating respectively, enter module 12 to react simultaneously, recirculation cooler setting temperature of reaction is 62 DEG C, and now the mol ratio of fatty acid methyl ester and hydrogen peroxide is 1:2.5.
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| CN104230775A (en) * | 2013-06-18 | 2014-12-24 | 中国石油化工股份有限公司 | Method for preparing dialkyl aminodithioformic acid by using one-step method |
| CN104557644B (en) * | 2013-10-09 | 2017-09-22 | 中国石油化工股份有限公司 | The method that dialkyl dithio amino formate is prepared using continuous flow tubular reactor |
| CN104592080A (en) * | 2014-11-26 | 2015-05-06 | 淄博正华助剂股份有限公司 | Method for preparing tert-butyl peroxyneodecanoate (BNP) through continuous flow |
| CN104587930B (en) * | 2014-12-24 | 2017-10-27 | 东南大学 | The synthesis of metal/carbon nanotube composite nano-line and special micro-/ nano reactor |
| CN104707547B (en) * | 2015-02-13 | 2016-11-02 | 清华大学 | A kind of method utilizing micro-reaction system synthesizing polyethylene butyral |
| CN105384709B (en) * | 2015-10-16 | 2018-04-27 | 华南理工大学 | A kind of method with micro passage reaction synthesizing epoxy fatty acid methyl ester |
| CN108164540B (en) * | 2017-12-14 | 2019-08-13 | 宜昌人福药业有限责任公司 | A method of synthesis Hydromorphone |
| CN110156982B (en) * | 2019-06-21 | 2022-02-08 | 常州中英新材料有限公司 | Liquid-liquid homogeneous phase method for synthesizing polyarylether by using continuous flow microchannel reactor |
| CN114682183B (en) * | 2020-12-31 | 2023-12-29 | 江苏同禾药业有限公司 | Continuous flow production method of lipoic acid bulk drug |
| CN113354758A (en) * | 2021-06-29 | 2021-09-07 | 南京先进生物材料与过程装备研究院有限公司 | Method for preparing epoxidized trans-1, 4-polyisoprene by using micro-reaction device |
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