CN111558358A - Thin film reactor and process for continuous production of alkyl anthraquinone by using same - Google Patents
Thin film reactor and process for continuous production of alkyl anthraquinone by using same Download PDFInfo
- Publication number
- CN111558358A CN111558358A CN202010265461.7A CN202010265461A CN111558358A CN 111558358 A CN111558358 A CN 111558358A CN 202010265461 A CN202010265461 A CN 202010265461A CN 111558358 A CN111558358 A CN 111558358A
- Authority
- CN
- China
- Prior art keywords
- reaction
- material cavity
- thin film
- cavity
- heat
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
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
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2475—Membrane reactors
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C46/00—Preparation of quinones
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2603/00—Systems containing at least three condensed rings
- C07C2603/02—Ortho- or ortho- and peri-condensed systems
- C07C2603/04—Ortho- or ortho- and peri-condensed systems containing three rings
- C07C2603/22—Ortho- or ortho- and peri-condensed systems containing three rings containing only six-membered rings
- C07C2603/24—Anthracenes; Hydrogenated anthracenes
Abstract
The invention relates to a thin film reactor and a process for continuous production of alkyl anthraquinone by using the same, which comprises the following steps: BB acid and fuming sulfuric acid are fully mixed in proportion, a thin film reactor is adopted to enable the mixed solution to carry out a closed-loop reaction at a certain temperature, reaction liquid after the closed-loop reaction automatically flows into a elutriation process, and the alkyl anthraquinone is obtained through separation. The process can realize continuous production, achieves higher production efficiency and lower production energy consumption compared with the prior art, reduces the generation of waste acid, and is beneficial to environmental protection.
Description
Technical Field
The invention relates to a production process for preparing alkylanthraquinone, in particular to a continuous production process for preparing alkylanthraquinone by adopting a thin film reactor.
Background
At present, the alkyl anthraquinone is mainly produced at home and abroad by a phthalic anhydride method, ketoacid generated by phthalic anhydride and alkylbenzene under the action of a catalyst is firstly used, and BB acid is dehydrated by fuming sulfuric acid to produce the alkyl anthraquinone.
European patent EP0055951B1 describes BB acid with 20% SO3The fuming sulfuric acid is reacted for 2 hours in a kettle way at the temperature of 100 ℃ according to the mass ratio of 1: 5, and the 2-ethyl anthraquinone is obtained with the yield of about 80 percent. The method has high oleum concentration and is easy to overflow SO3The method has the advantages of gas, intermittent production, poor production environment, slow heat transfer of equipment, long reaction time, more byproducts and large amount of waste acid, and is not beneficial to industrialization and environmental protection.
Japanese patent JP2255637A changes the kettle type process into a tubular continuous production process, uses a special mixing device, and mixes BB acid and oleum (containing 20% SO)3) Uniformly mixing the raw materials according to the mass ratio of 1:3, controlling the mixing temperature to be lower than 50 ℃, quickly heating the mixture to 170 ℃ by a microwave heater, and allowing the mixture to enter a tubular reactor for reaction, wherein the yield is about 90%. The method reduces the consumption of fuming sulfuric acid, has better yield, but has the problems of complex process of a mixing device and a microwave device, easy corrosion and easy blockage of a static mixer unit arranged in a pipeline reactor and the like, and limits the wide application of the method.
The process disclosed in Chinese patent CN101633612 comprises the steps of respectively placing fuming sulfuric acid and 2- (4-ethyl benzoyl) benzoic acid in a storage tank, heating the 2- (4-ethyl benzoyl) benzoic acid to 125-190 ℃ to keep the 2- (4-ethyl benzoyl) benzoic acid in a liquid state, rapidly mixing the fuming sulfuric acid and the 2- (4-ethyl benzoyl) benzoic acid in a Y-shaped jet mixer, then feeding the mixture into a tubular reactor, controlling the reaction temperature in the tubular reactor to be 120-180 ℃, reacting for 2-10 min, feeding the obtained reaction liquid into a hydrolysis kettle for hydrolysis, and separating out a product 2-ethyl anthraquinone. Although the adopted jet flow mixer is improved in mixing, the tubular reactor has the problems of slow temperature rise, easy blockage and the like, and the normal production is influenced.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a film reactor and a process for continuous production of alkylanthraquinone, wherein the process can realize continuous production, achieve higher production efficiency and lower production energy consumption than the prior art, reduce the generation of waste acid, is beneficial to environmental protection, has simple and reliable equipment, and can realize stable and continuous operation.
In order to achieve the purpose, the invention adopts the following technical scheme:
a thin film reactor comprises a reaction material cavity, a heat conduction material cavity, a reaction material inlet, a reaction material outlet, a heat conduction material inlet, a heat conduction material outlet, a temperature measuring instrument jack, a gas phase material outlet and a discharge outlet;
the reaction material cavity and the heat-conducting material cavity are attached together; the reaction material inlet and the reaction material outlet are respectively positioned at two ends of the reaction material cavity; the heat-conducting material inlet and the heat-conducting material outlet are respectively positioned at two ends of the heat-conducting material cavity; the temperature measuring instrument jack is positioned on the heat conducting material cavity; the gas-phase material outlet is positioned at the top of the reaction material cavity; the discharge port is positioned at the bottom of the reaction material cavity.
The reaction material cavity and the heat conduction material cavity are flat plate cavities or arc cavities or cylindrical cavities; the reaction material cavity and the heat conduction material cavity are attached together through bolts; the horizontal height of the reaction material inlet is higher than that of the reaction material outlet; an access hole is formed in the reaction material cavity; and a support is arranged on the heat-conducting material cavity.
The thickness of the inner cavity of the reaction material cavity is 1-6 mm, and preferably 2-5 mm. Such a thickness of the internal cavity allows the reaction mass to form a thin film therein, so that the reaction mass can be heated by the heat conductive material quickly and uniformly, and the fluid resistance of the reaction mass forming the thin film is small.
The thin film reactor has the advantages of high heat transfer efficiency, small fluid flow resistance and the like, has simple structure, is not easy to block, is convenient to overhaul, has low manufacturing cost, and can realize large-scale popularization and application.
A process for continuous production of alkyl anthraquinone by using a thin film reactor comprises the following steps: BB acid and fuming sulfuric acid are fully mixed in proportion, a thin film reactor is adopted to enable the mixed solution to carry out a closed-loop reaction at a certain temperature, reaction liquid after the closed-loop reaction automatically flows into a elutriation process, and the alkyl anthraquinone is obtained through separation.
The continuous production process of the alkyl anthraquinone is characterized by comprising the following steps: BB acid, a solvent and fuming sulfuric acid are fully mixed according to a proportion, and the solvent is evaporated out in a film reactor for recycling.
The BB acid is 2- [ (4-ethylphenyl) benzoyl ] benzoic acid, 2- [ (4-tert-amylphenyl) benzoyl ] benzoic acid, 2- [ (4-tert-butylphenyl) benzoyl ] benzoic acid, 2- [ (4-butylphenyl) benzoyl ] benzoic acid or 2- [ (4-methylphenyl) benzoyl ] benzoic acid; the alkyl anthraquinone is 2-ethyl anthraquinone, 2-tertiary amyl anthraquinone, 2-tertiary butyl anthraquinone, 2-butyl anthraquinone or 2-methyl anthraquinone.
The solvent is one or a combination of more of dichloromethane, trichloromethane, carbon tetrachloride, dichloroethane or carbon disulfide.
The weight ratio of the BB acid to the fuming sulfuric acid is 1: 2-10, and preferably 1: 2-5.
The weight ratio of the BB acid to the solvent is 1: 0.5-5, preferably 1: 0.5-2.
The reaction temperature is 110-190 ℃, and preferably 130-150 ℃.
The invention uses the thin film reactor to replace an intermittent kettle type or continuous tubular reactor, reduces the heating time and the reaction time, and effectively reduces the production energy consumption. In the reaction process, the reaction liquid automatically flows into the elutriation kettle from the thin film reactor, so that transmission equipment is saved, the production efficiency is improved, and the production cost and the energy consumption are effectively reduced.
The BB acid dissolved by the solvent can be better dispersed in the fuming sulfuric acid, so that the condition that sulfonation or carbonization byproducts are generated due to local excess of materials in the material mixing process is avoided, the using amount of the fuming sulfuric acid is reduced, the generation of waste acid is reduced, and the environment friendliness is facilitated.
The invention realizes the continuous reaction of BB acid, solvent and fuming sulfuric acid after homogeneous mixing, and improves the continuous level of a production device. In the reaction process, the thin film reactor can evaporate the solvent for recycling, thereby realizing continuous production.
Drawings
FIG. 1 is a front view of a thin film reactor.
FIG. 2 is a bottom view of a thin film reactor.
FIG. 3 is a schematic diagram of the process equipment for continuous production of alkylanthraquinone by the thin film reactor.
In the figure: the reaction material cavity comprises a reaction material cavity 1, a heat-conducting material cavity 2, a reaction material inlet 3, a reaction material outlet 4, a heat-conducting material inlet 5, a heat-conducting material outlet 6, a thermometer jack 7, a gas-phase material outlet 8, a discharge hole 9, an access hole 10, a support 11, a bolt 12, a first mixer 13, a second mixer 14, a thin film reactor 15, a water separation kettle 16, a condenser 17, a recovered solvent receiving tank 18, a liquid level meter 19, a reaction liquid thermometer 20, a heat-conducting oil thermometer 21, a first flow regulating valve group 22 and a second flow regulating valve group 23.
Detailed Description
The following describes embodiments of the present invention with reference to the drawings.
Example 1
As shown in fig. 1 and 2, a thin film reactor includes a reaction material cavity 1, a heat-conducting material cavity 2, a reaction material inlet 3, a reaction material outlet 4, a heat-conducting material inlet 5, a heat-conducting material outlet 6, a thermometer jack 7, a gas-phase material outlet 8 and a discharge opening 9;
the reaction material cavity 1 and the heat-conducting material cavity 2 are attached together; the reaction material inlet 3 and the reaction material outlet 4 are respectively positioned at two ends of the reaction material cavity 1; the heat-conducting material inlet 5 and the heat-conducting material outlet 6 are respectively positioned at two ends of the heat-conducting material cavity 2; the thermometer jack 7 is positioned on the heat conduction material cavity 2; the gas-phase material outlet 8 is positioned at the top of the reaction material cavity 1; the discharge opening 9 is positioned at the bottom of the reaction material cavity 1.
Preferably, the reaction material cavity 1 and the heat conduction material cavity 2 are flat plate cavities or arc cavities or cylindrical cavities; the reaction material cavity 1 and the heat conduction material cavity 2 are attached to each other through bolts 12; the level of the reaction material inlet 3 is higher than that of the reaction material outlet 4; the reaction material cavity 1 is provided with an access hole 10; and a support 11 is arranged on the heat conduction material cavity 2.
The thickness of the inner cavity of the reaction material cavity 1 is 1-6 mm, and preferably 2-5 mm.
Example 2
The adopted equipment is shown in figure 3, and the implementation process is as follows: 2- [ (4-ethylphenyl) benzoyl ] benzoic acid and trichloromethane enter a first mixer 13 at the same time at the speed of 9KG/h and 10L/h (weight ratio is 1: 1.63) for quick mixing, the mixed mixture enters a second mixer 14 through a first flow regulating valve group 22 for regulating the flow 15L/h, the mixed mixture is continuously mixed in the second mixer 14 with 16.6L/h 20% fuming sulfuric acid (the weight ratio of the 2- [ (4-ethylphenyl) benzoyl ] benzoic acid to the fuming sulfuric acid is 1: 3.5), the mixed mixture enters a thin film reactor 15 through a second regulating valve group 23 for regulating the flow 32L/h, and the temperature of a reaction liquid thermometer 20 is stabilized at 140-145 ℃ by controlling the temperature of a heat conducting oil thermometer 21 on the thin film reactor 15; the solvent trichloromethane steam enters a condenser 17 from a gas phase material outlet 9 at the upper part of the thin film reactor 15, and the condensed solvent trichloromethane enters a recovered solvent receiving tank 18 for reuse; the reaction liquid automatically flows into a elutriation kettle 16, and is separated into layers after elutriation, and the upper layer substance is the product 2-ethyl anthraquinone. When the plant has stopped running, the residual material is discharged from the membrane reactor via the discharge opening 10.
The product 2-ethyl anthraquinone is a dark yellow solid, the purity of the product is 96% by liquid chromatography analysis, and the reaction yield is 90%.
Example 3
The adopted equipment is shown in figure 3, and the implementation process is as follows: 2- [ (4-tert-amylphenyl) benzoyl ] benzoic acid and dichloroethane enter a first mixer 13 at the same time at the speed of 7KG/h and 6L/h (weight ratio is 1: 1.1) for quick mixing, the mixed mixture enters a second mixer 14 through a first flow regulating valve bank 22 for regulating the flow rate of 12L/h, the mixed mixture is continuously mixed with 10L/h fuming sulfuric acid (the weight ratio of the 2- [ (4-tert-amylphenyl) benzoyl ] benzoic acid to the fuming sulfuric acid is 1: 2.72) in the second mixer 14, the mixed mixture enters a thin film reactor 15 through a second regulating valve bank 23 for regulating the flow rate of 22L/h, and the temperature of a reaction solution 20 is stabilized at 140-145 ℃ by controlling the temperature of heat conducting oil 21 on the thin film reactor 15; the dichloroethane vapor of the solvent enters a condenser 17 from a gas-phase material outlet 9 at the upper part of the thin film reactor 15, and the condensed dichloromethane solvent enters a recycled solvent receiving tank 18 for reuse; the reaction liquid automatically flows into a water precipitation kettle 16, and is separated into layers after water precipitation, and the upper layer substance is the 2-tertiary amyl anthraquinone. When the plant has stopped running, the residual material is discharged from the membrane reactor via the discharge opening 10.
The product 2-tert-amylanthraquinone was a tan waxy solid with a purity of 93.5% and a reaction yield of 85% by liquid chromatography.
Example 4
The adopted equipment is shown in figure 3, and the implementation process is as follows: 2- [ (4-tert-butylphenyl) benzoyl ] benzoic acid and carbon tetrachloride enter a first mixer 13 at the same time at the speed of 10KG/h and 5L/h (weight ratio is 1: 0.8) for rapid mixing, the mixed mixture enters a second mixer 14 through a first flow regulating valve bank 22 for regulating the flow rate of 14L/h, the mixed mixture continues to be mixed in the second mixer 14 through a 20L/h fuming sulfuric acid (the weight ratio of the 2- [ (4-tert-butylphenyl) benzoyl ] benzoic acid to the fuming sulfuric acid is 1: 3.8), the mixed mixture enters a thin film reactor 15 through a second regulating valve bank 23 for regulating the flow rate of 34L/h, and the temperature of a heat conducting oil thermometer 20 on the thin film reactor 15 is controlled to be stabilized at 130-135 ℃; the solvent carbon tetrachloride steam enters a condenser 17 from a gas phase material outlet 9 at the upper part of the thin film reactor 15, and the condensed solvent tetrachloromethane enters a recovered solvent receiving tank 18 for reuse; the reaction liquid automatically flows into a water precipitation kettle 16, and is layered after water precipitation, and the upper layer substance is the product 2-tert-butyl anthraquinone. When the plant has stopped running, the residual material is discharged from the membrane reactor via the discharge opening 10.
The product 2-tert-butyl anthraquinone is yellow powdery solid, and the purity of the product is 96.5 percent and the reaction yield is 92 percent by liquid chromatography analysis.
Example 5
The adopted equipment is shown in figure 3, and the implementation process is as follows: melting 5KG of 2- [ (4-ethylphenyl) benzoyl ] benzoic acid in a first mixer 13, adding the 2- [ (4-ethylphenyl) benzoyl ] benzoic acid into the first mixer 13 at a speed of 9KG/h, adjusting the flow rate of 8L/h by using a first flow adjusting valve bank 22, entering a second mixer 14, mixing with 16.6L/h of 20% fuming sulfuric acid (the weight ratio of the 2- [ (4-ethylphenyl) benzoyl ] benzoic acid to the fuming sulfuric acid is 1: 3.5) in the second mixer 14, adjusting the flow rate of 24L/h by using a second adjusting valve bank 23 after mixing, entering a thin film reactor 15, and stabilizing the temperature of a reaction liquid thermometer 20 at 140-145 ℃ by controlling the temperature of heat conducting oil 21 on the thin film reactor 15; after the reaction is finished, the reaction liquid automatically flows into a elutriation kettle 16, and is separated into layers after elutriation, and the upper layer substance is the product 2-ethyl anthraquinone. When the plant has stopped running, the residual material is discharged from the membrane reactor via the discharge opening 10.
The product, 2-ethylanthraquinone, was a brown solid, which was analyzed by liquid chromatography for purity 87.6% and reaction yield 79%.
Comparative example
The membrane reactor in the apparatus shown in FIG. 3 was replaced by a tubular reactor. The comparative example was carried out using modified equipment. The implementation process comprises the following steps: firstly, melting 5KG of 2- [ (4-ethylphenyl) benzoyl ] benzoic acid in a first mixer 13, then adding 2- [ (4-ethylphenyl) benzoyl ] benzoic acid into the first mixer 13 at a speed of 9KG/h, adjusting the flow rate of 8L/h through a first flow adjusting valve bank 22, entering a second mixer 14, mixing 16.6L/h of 20% fuming sulfuric acid (the weight ratio of the 2- [ (4-ethylphenyl) benzoyl ] benzoic acid to the fuming sulfuric acid is 1: 3.5) in the second mixer 14, adjusting the flow rate of 24L/h through a second flow adjusting valve bank 23 after mixing, entering a pipeline reactor, and stabilizing the temperature of a reaction liquid thermometer 20 at 140-145 ℃ by controlling the temperature of the pipeline reactor; the reaction liquid automatically flows into a water separation kettle, and is separated into layers after water separation, and the upper layer substance is the product 2-ethyl anthraquinone.
The product, 2-ethylanthraquinone, was a brown solid with a purity of 89.6% by liquid chromatography and a reaction yield of 62%. The gas generated by the reaction can not be discharged in time by the pipeline reactor, and the gas and the liquid are entrained, so that the liquid flow of the tubular reactor is not stable, and the phenomenon does not occur when the thin film reactor is used.
The above-described embodiments are merely preferred embodiments of the present invention, and should not be construed as limiting the present invention, and features in the embodiments and examples in the present application may be arbitrarily combined with each other without conflict. The protection scope of the present invention is defined by the claims, and includes equivalents of technical features of the claims. I.e., equivalent alterations and modifications within the scope hereof, are also intended to be within the scope of the invention.
Claims (10)
1. A film reactor is characterized by comprising a reaction material cavity (1), a heat-conducting material cavity (2), a reaction material inlet (3), a reaction material outlet (4), a heat-conducting material inlet (5), a heat-conducting material outlet (6), a thermometer jack (7), a gas-phase material outlet (8) and a discharge outlet (9);
the reaction material cavity (1) and the heat-conducting material cavity (2) are attached together; the reaction material inlet (3) and the reaction material outlet (4) are respectively positioned at two ends of the reaction material cavity (1); the heat-conducting material inlet (5) and the heat-conducting material outlet (6) are respectively positioned at two ends of the heat-conducting material cavity (2); the thermometer jack (7) is positioned on the heat conduction material cavity (2); the gas-phase material outlet (8) is positioned at the top of the reaction material cavity (1); the discharge opening (9) is positioned at the bottom of the reaction material cavity (1).
2. A thin film reactor according to claim 1 wherein: the reaction material cavity (1) and the heat conduction material cavity (2) are flat plate cavities or arc cavities or cylindrical cavities; the reaction material cavity (1) and the heat conduction material cavity (2) are attached together through bolts (12); the level of the reaction material inlet (3) is higher than that of the reaction material outlet (4); an access hole (10) is formed in the reaction material cavity (1); and a support (11) is arranged on the heat conduction material cavity (2).
3. A thin film reactor according to claim 1 wherein: the thickness of the inner cavity of the reaction material cavity (1) is 1-6 mm.
4. A thin film reactor according to claim 3 wherein: the thickness of an inner cavity of the reaction material cavity (1) is 2-5 mm.
5. A thin film reactor according to any of claims 1-4 for use in a continuous process for the production of alkylanthraquinones, characterized in that: BB acid and fuming sulfuric acid are fully mixed in proportion, a thin film reactor is adopted to enable the mixed solution to carry out a closed-loop reaction at a certain temperature, reaction liquid after the closed-loop reaction automatically flows into a elutriation process, and the alkyl anthraquinone is obtained through separation.
6. The process for the continuous production of alkylanthraquinones according to claim 5, wherein: BB acid, a solvent and fuming sulfuric acid are fully mixed according to a proportion, and the solvent is distilled out of the thin film reactor for recycling.
7. The continuous production process of alkylanthraquinone according to claim 6, wherein: the solvent is one or a combination of more of dichloromethane, trichloromethane, carbon tetrachloride, dichloroethane or carbon disulfide; the weight ratio of the BB acid to the fuming sulfuric acid is 1: 2-10; the weight ratio of the BB acid to the solvent is 1: 0.5-5.
8. The process for the continuous production of alkylanthraquinones according to claim 7, wherein: the weight ratio of the BB acid to the fuming sulfuric acid is 1: 2-5; the weight ratio of the BB acid to the solvent is 1: 0.5-2.
9. The process for the continuous production of alkylanthraquinones according to claim 5, wherein: the reaction temperature is 110-190 ℃.
10. The process for the continuous production of alkylanthraquinones according to claim 9, wherein: the reaction temperature is 130-150 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010265461.7A CN111558358A (en) | 2020-04-07 | 2020-04-07 | Thin film reactor and process for continuous production of alkyl anthraquinone by using same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010265461.7A CN111558358A (en) | 2020-04-07 | 2020-04-07 | Thin film reactor and process for continuous production of alkyl anthraquinone by using same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111558358A true CN111558358A (en) | 2020-08-21 |
Family
ID=72074159
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010265461.7A Pending CN111558358A (en) | 2020-04-07 | 2020-04-07 | Thin film reactor and process for continuous production of alkyl anthraquinone by using same |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111558358A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0548944A1 (en) * | 1991-12-26 | 1993-06-30 | Canon Kabushiki Kaisha | Chemical vapor deposition method and apparatus making use of liquid starting material |
| CN101633612A (en) * | 2009-08-20 | 2010-01-27 | 浙江工业大学 | Device and process for continuously producing 2-ethyl anthracene quinone in channelization way |
| WO2012034164A2 (en) * | 2010-09-13 | 2012-03-22 | The University Of Western Australia | Thin film tube reactor |
| CN103787352A (en) * | 2012-10-26 | 2014-05-14 | 中国石油化工股份有限公司 | Method for preparing molecular sieve |
| CN105056842A (en) * | 2015-07-23 | 2015-11-18 | 厦门大学 | Reaction apparatus and application thereof in synthesizing borate |
-
2020
- 2020-04-07 CN CN202010265461.7A patent/CN111558358A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0548944A1 (en) * | 1991-12-26 | 1993-06-30 | Canon Kabushiki Kaisha | Chemical vapor deposition method and apparatus making use of liquid starting material |
| CN101633612A (en) * | 2009-08-20 | 2010-01-27 | 浙江工业大学 | Device and process for continuously producing 2-ethyl anthracene quinone in channelization way |
| WO2012034164A2 (en) * | 2010-09-13 | 2012-03-22 | The University Of Western Australia | Thin film tube reactor |
| CN103787352A (en) * | 2012-10-26 | 2014-05-14 | 中国石油化工股份有限公司 | Method for preparing molecular sieve |
| CN105056842A (en) * | 2015-07-23 | 2015-11-18 | 厦门大学 | Reaction apparatus and application thereof in synthesizing borate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101633612B (en) | Device and process for continuously producing 2-ethyl anthracene quinone in channelization way | |
| CN107353208A (en) | 5 nitro-salicylic acid techniques are prepared using microchannel continuous flow reactor | |
| CN106674016A (en) | Method for synthesizing 2-chloro-5-nitrobenzoic acid through microchannel reactor | |
| CN101058734B (en) | Device for industrially synthesizing biological diesel oil by microwave and method thereof | |
| CN101423482A (en) | Integrated method of sulphonation and neutralization reaction | |
| CN103007862A (en) | Gas-liquid stirring reactor for synthesizing acrylic acid and ester through acetylene carbonylation method | |
| CN205774230U (en) | The device of continuous prodution methyl tetrahydro phthalic anhydride | |
| CN111558358A (en) | Thin film reactor and process for continuous production of alkyl anthraquinone by using same | |
| CN206858475U (en) | A kind of continuous process system of p-methyl benzenesulfonic acid | |
| CN113773179A (en) | Method for continuously and synchronously hydrolyzing acylation reaction liquid | |
| CN109422642A (en) | Refining methd, the production method and equipment of pharmaceutical grade sodium benzoate of benzoic acid | |
| CN207143010U (en) | The dehydration device of esterification products under a kind of acid condition | |
| CN103922898B (en) | A kind of Resorcinol continuous crystallisation technique | |
| CN216499225U (en) | Production device of 2-methylpyridine | |
| CN205856358U (en) | The continuous production device of 1 LOMAR PWA EINECS 246-676-2 | |
| KR100539285B1 (en) | Recovery system of waste polyester oligomer using hybrid process of methanolysis reactor and distillation | |
| CN206940777U (en) | A kind of production equipment of ton polyphenylene oxide | |
| CN113045370A (en) | Sulfonation method | |
| CN105777532B (en) | A kind of method of VC waste liquid recyclings production oxalic acid | |
| CN107033061A (en) | A kind of method of continuous stream reaction 3 methyl indols of synthesis | |
| US20230095165A1 (en) | Method for continuous synthesis of acylnaphthalene with acylation liquid | |
| CN217989308U (en) | Safety interlock system for vinylene carbonate production system | |
| CN218485811U (en) | Continuous production system of alkyl anthraquinone intermediate keto acid | |
| CN115197111B (en) | Continuous production method of dimethyl disulfide | |
| CN107963984B (en) | Continuous production system and method for p-toluenesulfonic acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |