CN217856075U - Reaction device for synthesizing OPP (oriented polypropylene) through micro-channel - Google Patents
Reaction device for synthesizing OPP (oriented polypropylene) through micro-channel Download PDFInfo
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- CN217856075U CN217856075U CN202221728879.8U CN202221728879U CN217856075U CN 217856075 U CN217856075 U CN 217856075U CN 202221728879 U CN202221728879 U CN 202221728879U CN 217856075 U CN217856075 U CN 217856075U
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Abstract
The utility model discloses a reaction device for synthesizing OPP by micro-channels, which comprises a micro-channel reactor, wherein the micro-channel reactor is connected with a sodium storage tank and a dibenzofuran storage tank, the micro-channel reactor is connected with a quenching device, and the quenching device is connected with a filter by a fourth material conveying pump; the discharge end at the bottom of the filter is connected with an acidification tank, the acidification tank is connected with an extraction tank, the discharge end at the lower layer of the extraction tank is connected with a liquid drying tank, and the liquid drying tank is connected with a distiller; the lower layer discharge end of the extraction tank is connected with an organic extraction liquid storage tank; the top discharge end of filter links to each other with the solid drying jar, and the solid drying jar links to each other with retrieving the dibenzofuran storage tank, and it links to each other with the dibenzofuran storage tank to retrieve the dibenzofuran storage tank. The utility model discloses using the microchannel as technical means, utilizing liquid dibenzofuran and fused sodium as the raw materials, the technical route mass transfer heat transfer of synthetic OPP is quick, and safety ring protects, and no three wastes produce, does not have extra solvent, and the cost is suitable, is favorable to the reaction process to become more meticulous and controls.
Description
Technical Field
The utility model belongs to the technical field of fine chemistry industry, a manufacturing of midbody o-phenylphenol is related to, concretely relates to reaction unit of synthetic OPP of microchannel.
Background
The o-phenylphenol (OPP) is an important novel fine chemical product and an organic intermediate, is researched and produced from the 70 th century abroad, has the global market demand of 50000 tons/year at present, and is widely applied to the fields of sterilization, corrosion prevention, printing and dyeing auxiliaries, surfactants, synthesis of stabilizers of novel plastics, resins and high polymer materials, synthesis of novel phosphorus-containing flame retardants and the like. It has been reported that o-phenylphenol can be used instead of phenol to synthesize a novel phenol-formaldehyde resin having thermal stability and low water absorption, which can be used for synthesizing a cholesterol ester hydrolysis inhibitor, an anticonvulsant drug, an anti-inflammatory drug and an analgesic drug and certain dermatological drugs, and a developer for synthesizing pressure-sensitive and heat-sensitive paper. The novel phosphorus-containing flame-retardant intermediate DOPO with wide application can be synthesized by using o-phenylphenol as a raw material. In conclusion, the o-phenylphenol has wide market demands and wide market prospects at home and abroad.
The traditional OPP synthesis method mainly comprises the following synthesis methods: 1. the separation process, which is obtained by separating distillation residues generated in the phenol production by the sulfonation process, is also limited as the phenol sulfonation process is gradually eliminated. 2. The diazotization hydrolysis method of the aminobiphenyl has the defects of difficult acquisition of raw materials and serious pollution. 3. The biphenyl is sulfonated and hydrolyzed by using sulfuric acid, alkali-melted by using sodium hydroxide and then acidified, and three wastes are prominent. 4. The condensation dehydrogenation method of cyclohexanone is the mainstream production method at present, and the process has high requirements on catalysts, harsh requirements on reaction conditions and incomplete recycling of the catalysts. At present, the research at home and abroad mainly focuses on the aspect of catalyst development of the cyclohexanone method. 5. Chlorobenzene and phenol are used as raw materials to synthesize o-phenylphenol by a phase transfer catalysis method. 6. The dibenzofuran method, heating dibenzofuran and sodium metal in solvent at about 200 deg.C, acid hydrolysis, is expensive, and in addition, US2862035 uses petroleum ether to react under high pressure, which requires high equipment. In another article, sodium is replaced by lithium metal, and the lithium metal is refluxed in dioxane, so that the raw material is expensive and the cost is high. Patent CN104230670A proposes replacing sodium with sodium hydrogen and using dibenzofuran as solvent. US400023 employs high temperature hydrogenation of dibenzofuran at 400 c, requiring expensive catalysts. Japanese patent JP56020533A is prepared by reacting dibenzofuran with sodium hydrogen in tetralin at 225 deg.C and then acidifying, and easily obtains benzene ring hydrogenation byproduct.
Microreactors, i.e., microchannel reactors, utilize precision machining techniques to produce microreactors having feature sizes between 10 and 300 microns (or 1000 microns). Due to the internal microstructure, the micro-reactor equipment has extremely large specific surface area which can reach hundreds of times or even thousands of times of the specific surface area of the stirring kettle. The micro-reactor has excellent heat transfer and mass transfer capacity, can realize instantaneous uniform mixing of materials and high-efficiency heat transfer, so that a plurality of reactions which cannot be realized in the conventional reactor can be realized in the micro-reactor.
At present, microreactors are widely applied to research and development of chemical process, and the application of microreactors in commercial production is increasing day by day. The main application fields of the method comprise an organic synthesis process, preparation of micron and nanometer materials and production of daily chemicals. However, there is no report on the synthesis of OPP.
Disclosure of Invention
Not enough to prior art exists, the utility model aims to provide a synthetic OPP's of microchannel reaction unit solves the technical problem that the fine control of synthetic OPP's reaction remains further promotion among the prior art.
In order to solve the technical problem, the utility model discloses a following technical scheme realizes:
a reaction device for synthesizing OPP by a microchannel comprises a microchannel reactor, wherein the feed end of the microchannel reactor is connected with a sodium storage tank through a first feed delivery pump, the feed end of the microchannel reactor is also connected with a dibenzofuran storage tank through a second feed delivery pump, the discharge end of the microchannel reactor is connected with the feed end of a quencher through a third feed delivery pump, and the discharge end of the quencher is connected with the feed end of a filter through a fourth feed delivery pump;
the bottom discharge end of the filter is connected with the feed end of the acidification tank through a fifth material conveying pump, the discharge end of the acidification tank is connected with the feed end of the extraction tank through a sixth material conveying pump, the lower-layer discharge end of the extraction tank is connected with the feed end of the liquid drying tank through a seventh material conveying pump, and the discharge end of the liquid drying tank is connected with the distiller through an eighth material conveying pump; the lower layer discharge end of the extraction tank is connected with an organic extraction liquid storage tank;
the top discharge end of filter link to each other with the feed end of solid drying cylinder, the discharge end of solid drying cylinder links to each other with the feed end of retrieving the dibenzofuran storage tank through ninth feeding pump, the discharge end of retrieving the dibenzofuran storage tank links to each other with the dibenzofuran storage tank through tenth feeding pump.
The utility model discloses still have following technical characteristic:
the microchannel reactor comprises a reactor main body, wherein a feeding material inflow plate is arranged at the upper part in the reactor main body, a discharging material outflow plate is arranged at the lower part in the reactor main body, and a heat exchanger is arranged in the reactor main body between the feeding material inflow plate and the discharging material outflow plate; the top of the reactor main body is provided with a nitrogen inlet, and the bottom of the reactor main body is provided with a nitrogen outlet.
The first material conveying pump, the second material conveying pump, the third material conveying pump, the fourth material conveying pump, the fifth material conveying pump, the sixth material conveying pump, the seventh material conveying pump, the eighth material conveying pump, the ninth material conveying pump and the tenth material conveying pump all adopt advection pumps.
The sodium storage tank, the dibenzofuran storage tank and the dibenzofuran recovery storage tank comprise tank bodies, a high-frequency heating layer is arranged outside the tank bodies, and a metering scale is arranged at the bottom of the tank bodies.
Compared with the prior art, the utility model, following technological effect has:
(I) the utility model discloses a reaction unit is for traditional synthetic OPP reaction unit, uses the microchannel as technical means, utilizes liquid dibenzofuran and fused sodium as the raw materials, and synthetic OPP's technical route mass transfer heat transfer is quick, and safety ring protects, and no three wastes produce, does not have extra solvent, and the cost is suitable, is favorable to the reaction process control that becomes more meticulous. Is a synthesis method worthy of popularization.
(II) the reaction device of the utility model heats rapidly and evenly, and can greatly shorten the reaction time.
(III) the reaction quenching of the reaction device of the utility model is safe and reliable.
(IV) the reaction device of the utility model adopts organic solvent to extract products, which can improve the purity of the products.
(V) the utility model discloses a reaction unit reaction raw materials dibenzofuran is as the solvent when as the raw materials, has practiced thrift the cost, and the not complete dibenzofuran of reacting can be retrieved and is used mechanically.
Drawings
FIG. 1 is a schematic diagram showing the overall structure of a reaction apparatus for synthesizing OPP in a microchannel.
FIG. 2 is a schematic diagram of a microchannel reactor.
Fig. 3 is a schematic diagram of the sodium storage tank.
The meaning of the individual reference symbols in the figures is: 1-a microchannel reactor, 2-a material delivery pump, 3-a sodium storage tank, 4-a dibenzofuran storage tank, 5-a quencher, 6-a filter, 7-an acidification tank, 8-an extraction tank, 9-a liquid drying tank, 10-a distiller, 11-an organic extraction liquid storage tank, 12-a solid drying tank, 13-a recovered dibenzofuran storage tank and 14-a valve;
101-reactor body, 102-feed inflow plates, 103-effluent outflow plates, 104-heat exchanger, 105-nitrogen inlet, 106-nitrogen outlet;
201-a first delivery pump, 202-a second delivery pump, 203-a third delivery pump, 204-a fourth delivery pump, 205-a fifth delivery pump, 206-a sixth delivery pump, 207-a seventh delivery pump, 208-an eighth delivery pump, 209-a ninth delivery pump, 210-a tenth delivery pump;
301-tank body, 302-high frequency heating layer, 303-metering scale.
The following examples are provided to explain the present invention in further detail.
Detailed Description
It is to be understood that all components and devices of the present invention, unless otherwise specified, are intended to be exemplary of those known in the art. For example, the microchannel reactor is a microchannel reactor known in the art.
Valves are arranged on all pipelines of the device according to the embodiment, and are opened or closed according to process requirements. The utility model discloses well all valves all adopt the valve commonly used among the prior art.
Obey above-mentioned technical scheme, following the present utility model discloses a specific embodiment, it needs to explain that the utility model discloses do not confine following specific embodiment to, all fall into the protection scope of the utility model to the equivalent transform of doing on the basis of this application technical scheme.
Example 1:
this embodiment provides a reaction device for synthesizing OPP through a microchannel, as shown in fig. 1, including a microchannel reactor 1, a feed end of the microchannel reactor 1 is connected to a sodium storage tank 3 through a first feed pump 201, a feed end of the microchannel reactor 1 is further connected to a dibenzofuran storage tank 4 through a second feed pump 202, a discharge end of the microchannel reactor 1 is connected to a feed end of a quencher 5 through a third feed pump 203, and a discharge end of the quencher 5 is connected to a feed end of a filter 6 through a fourth feed pump 204.
The discharge end at the bottom of the filter 6 is connected with the feed end of the acidification tank 7 through a fifth feed pump 205, the discharge end of the acidification tank 7 is connected with the feed end of the extraction tank 8 through a sixth feed pump 206, the lower discharge end of the extraction tank 8 is connected with the feed end of the liquid drying tank 9 through a seventh feed pump 207, and the discharge end of the liquid drying tank 9 is connected with the distiller 10 through an eighth feed pump 208; the lower layer discharge end of the extraction tank 8 is connected with an organic extraction liquid storage tank 11.
The top discharge end of the filter 6 is connected with the feed end of the solid drying tank 12, the discharge end of the solid drying tank 12 is connected with the feed end of the dibenzofuran recovery storage tank 13 through the ninth material delivery pump 209, and the discharge end of the dibenzofuran recovery storage tank 13 is connected with the dibenzofuran storage tank 4 through the tenth material delivery pump 210.
As a preferable scheme of this embodiment, as shown in fig. 2, the microchannel reactor 1 includes a reactor main body 101, a feed inflow plate 102 is provided at an upper portion in the reactor main body 101, an effluent outflow plate 103 is provided at a lower portion in the reactor main body 101, and a heat exchanger 104 is provided in the reactor main body 101 between the feed inflow plate 102 and the effluent outflow plate 103; the top of the reactor body 101 is provided with a nitrogen inlet 105 and the bottom of the reactor body 101 is provided with a nitrogen outlet 106.
In the present embodiment, it is preferable that the main part of the reactor main body 101 is composed of a glass tube or a polytetrafluoroethylene tube having a tube diameter of 0.1 to 5 mm.
In this embodiment, a mixed solution of sodium and dibenzofuran enters the reactor main body 101 through the feed inflow plate 102, is heated and reacted in the reactor main body 101, and is then discharged through the discharge outflow plate 103. The heating temperature of the heat exchanger 104 is between 10 and 250 ℃.
As a preferable scheme of this embodiment, the first material delivery pump 201, the second material delivery pump 202, the third material delivery pump 203, the fourth material delivery pump 204, the fifth material delivery pump 205, the sixth material delivery pump 206, the seventh material delivery pump 207, the eighth material delivery pump 208, the ninth material delivery pump 209, and the tenth material delivery pump 210 all adopt advection pumps.
As a preferable scheme of this embodiment, as shown in fig. 3, the sodium storage tank 3, the dibenzofuran storage tank 4 and the dibenzofuran recovery storage tank 13 each include a tank 301, a high-frequency heating layer 302 is disposed outside the tank 301, and a weighing scale 303 is disposed at the bottom of the tank 301.
In this embodiment, the high-frequency heating layer 302 can control temperature quickly and accurately. The tank 301 is made of FRP (fiber reinforced polymer composite material, high temperature resistant and acid and alkali resistant, and the weigher 303 is a multi-application reaction kettle weighing module with a known and commonly used PLC control module, and can accurately weigh the weight of the substance.
The utility model discloses a concrete process of microchannel synthesis OPP's reaction unit when synthesizing the OPP product is as follows:
the temperature for heating the raw material sodium in the sodium storage tank 3 is not lower than the melting point of sodium and not higher than the boiling point of dibenzofuran. The heating temperature of the raw material dibenzofuran in the dibenzofuran storage tank 4 and the recovered dibenzofuran in the recovered dibenzofuran storage tank 13 is not lower than the melting point of dibenzofuran and not higher than the boiling point of dibenzofuran. Generally, the temperature is preferably 100 to 200 ℃.
The raw materials are heated in a sodium storage tank 3 and a dibenzofuran storage tank 4 respectively to become small liquid beads and liquid, and then the small liquid beads and the liquid are mixed and enter a microchannel reactor 1.
The main reaction is in a microchannel reactor 1. Under the protection of nitrogen. Further preferably, the microchannel reactor 1 is connected with a known and commonly used GC detection device and a known and commonly used PLC central control device for control.
The reaction product and the unreacted dibenzofuran pass through the microchannel reactor 1 and then pass through a quencher 5. The quencher 5 is connected with a water pipeline and a temperature control device, when the temperature of the device is reduced to about 90 ℃, the liquid state of the mixture is kept, water is slowly dripped, and a small amount of unreacted residual sodium is quenched.
The reaction mixture passes through a quencher 5 and then enters a filter 6, the temperature is reduced to room temperature and then filtered, and filter residue is washed with water for 2 times and then enters a solid drying tank 12. The filtrate is combined with water washing liquid and enters an acidification tank 7. The acidification tank 7 is connected with a hydrochloric acid inlet, and the pH is slowly adjusted to 2-3 by dripping hydrochloric acid.
The solid drying tank 12 adopts a decompression drying mode to dry and recover the dibenzofuran at 70-80 ℃. And after drying, entering a dibenzofuran recovery storage tank 13. The dibenzofuran recovered in the dibenzofuran storage tank 13 is heated and then returned to the dibenzofuran storage tank 2 through a pipeline.
The aqueous phase produced from the acidification tank 7 is placed in an extraction tank 8. The extraction tank 8 is connected to an organic extract storage tank 11 in which an extraction solvent such as dichloromethane, ethyl acetate, toluene or other alkanes, halogenated hydrocarbons and other inert solvents are stored. After the aqueous phase is extracted for three times, the three wastes of the aqueous phase are treated, and the organic phase enters a liquid drying tank 9 in which an activated 4A molecular sieve is stored.
And (3) distilling the dried organic phase in the liquid drying tank 9 in a distiller 10, recovering the distilled solvent, drying and recycling, and cooling and crystallizing the residual yellowish liquid to obtain the product.
Example 2:
this example shows a method for OPP synthesis based on the microchannel OPP synthesis reaction apparatus and specific procedures given in example 1, wherein the specific reaction conditions include:
the sodium reservoir 3 was heated to 100 ℃ and 11.5kg (5 mol) of liquid beads of discharged sodium were added.
The dibenzofuran storage tank 4 was heated to 100 ℃ and 171.2kg (10 mol,98% content) in total was discharged.
The microchannel reactor 1 is protected by nitrogen, and is started to be heated to 120 ℃ for reaction for about 6 hours.
The methylene chloride entering the liquid dryer tank 9 was dried over 4A molecular sieves for 12 hours until the moisture was less than 0.3%. And (3) carrying out reduced pressure distillation on dichloromethane at 30 ℃, recycling the obtained solvent, cooling and crystallizing the residual liquid to obtain a target product OPP with the content of 34.7kg, the content of 95 percent and the yield of 77.5 percent.
The recovered dibenzofuran that entered the solid drying tank 12 was vacuum dried at 75 ℃ for 6 hours.
The solid dibenzofuran entering the recovered dibenzofuran storage tank 13 was about 124.7kg, with a content of 99.1% and a recovery rate of 96.2%.
Example 3:
this example shows a method for OPP synthesis based on the microchannel OPP synthesis reaction apparatus and specific procedures given in example 1, wherein the specific reaction conditions include:
the sodium reservoir 3 was heated to 110 ℃ and 11.5kg (5 mol) of liquid beads of discharged sodium were added.
The dibenzofuran storage tank 4 was heated to 110 ℃ and a total of 342.4kg (20mol, 98% content) was discharged.
The microchannel reactor 1 is protected by nitrogen, and is started to be heated to 150 ℃ for reaction for about 5 hours.
The methylene chloride entering the liquid dryer tank 9 was dried over 4A molecular sieves for 12 hours until the moisture was less than 0.3%. And (3) carrying out reduced pressure distillation on dichloromethane at 30 ℃, recycling the obtained solvent, cooling and crystallizing the residual liquid to obtain a target product OPP with the content of 35.1kg, the content of 96 percent and the yield of 79.2 percent.
The recovered dibenzofuran that entered the solid drying tank 12 was vacuum dried at 75 ℃ for 6 hours.
The solid dibenzofuran entering the dibenzofuran recovery tank 13 is about 291.3kg, the content is 99.2%, and the recovery rate is 96.5%.
Claims (4)
1. A reaction device for synthesizing OPP by a microchannel comprises a microchannel reactor (1) and is characterized in that the feed end of the microchannel reactor (1) is connected with a sodium storage tank (3) through a first feed delivery pump (201), the feed end of the microchannel reactor (1) is also connected with a dibenzofuran storage tank (4) through a second feed delivery pump (202), the discharge end of the microchannel reactor (1) is connected with the feed end of a quencher (5) through a third feed delivery pump (203), and the discharge end of the quencher (5) is connected with the feed end of a filter (6) through a fourth feed delivery pump (204);
the bottom discharge end of the filter (6) is connected with the feed end of the acidification tank (7) through a fifth material conveying pump (205), the discharge end of the acidification tank (7) is connected with the feed end of the extraction tank (8) through a sixth material conveying pump (206), the lower-layer discharge end of the extraction tank (8) is connected with the feed end of the liquid drying tank (9) through a seventh material conveying pump (207), and the discharge end of the liquid drying tank (9) is connected with the distiller (10) through an eighth material conveying pump (208); the lower layer discharge end of the extraction tank (8) is connected with an organic extraction liquid storage tank (11);
the top discharge end of the filter (6) is connected with the feed end of the solid drying tank (12), the discharge end of the solid drying tank (12) is connected with the feed end of the dibenzofuran recovery storage tank (13) through a ninth material conveying pump (209), and the discharge end of the dibenzofuran recovery storage tank (13) is connected with the dibenzofuran storage tank (4) through a tenth material conveying pump (210).
2. The reactor for microchannel synthesis of OPP according to claim 1, wherein the microchannel reactor (1) comprises a reactor body (101), the upper part in the reactor body (101) is provided with a feed inlet plate (102), the lower part in the reactor body (101) is provided with an outlet plate (103), and a heat exchanger (104) is arranged in the reactor body (101) between the feed inlet plate (102) and the outlet plate (103); the top of the reactor main body (101) is provided with a nitrogen inlet (105), and the bottom of the reactor main body (101) is provided with a nitrogen outlet (106).
3. The apparatus for reaction of microchannel synthesis OPP according to claim 1, wherein the first feed delivery pump (201), the second feed delivery pump (202), the third feed delivery pump (203), the fourth feed delivery pump (204), the fifth feed delivery pump (205), the sixth feed delivery pump (206), the seventh feed delivery pump (207), the eighth feed delivery pump (208), the ninth feed delivery pump (209) and the tenth feed delivery pump (210) all adopt advection pumps.
4. The reaction device for synthesizing OPP by the micro-channel according to claim 1, wherein the sodium storage tank (3), the dibenzofuran storage tank (4) and the dibenzofuran recovery storage tank (13) all comprise a tank body (301), a high-frequency heating layer (302) is arranged outside the tank body (301), and a metering scale (303) is arranged at the bottom of the tank body (301).
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| CN202221728879.8U CN217856075U (en) | 2022-07-05 | 2022-07-05 | Reaction device for synthesizing OPP (oriented polypropylene) through micro-channel |
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| CN202221728879.8U CN217856075U (en) | 2022-07-05 | 2022-07-05 | Reaction device for synthesizing OPP (oriented polypropylene) through micro-channel |
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