CN112499593A - Automatic strengthening system and process for preparing hydrogen peroxide based on anthraquinone method - Google Patents
Automatic strengthening system and process for preparing hydrogen peroxide based on anthraquinone method Download PDFInfo
- Publication number
- CN112499593A CN112499593A CN201910867797.8A CN201910867797A CN112499593A CN 112499593 A CN112499593 A CN 112499593A CN 201910867797 A CN201910867797 A CN 201910867797A CN 112499593 A CN112499593 A CN 112499593A
- Authority
- CN
- China
- Prior art keywords
- hydrogenation
- hydrogen
- liquid
- anthraquinone
- tower
- 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
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 114
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 150000004056 anthraquinones Chemical class 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 56
- 238000005728 strengthening Methods 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 160
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 143
- 239000001257 hydrogen Substances 0.000 claims abstract description 106
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 106
- 238000006243 chemical reaction Methods 0.000 claims abstract description 90
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 85
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 73
- 239000012224 working solution Substances 0.000 claims abstract description 31
- -1 2-ethyl hydrogen anthraquinone Chemical class 0.000 claims abstract description 22
- 239000000839 emulsion Substances 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 13
- 238000012546 transfer Methods 0.000 claims abstract description 13
- 239000003570 air Substances 0.000 claims description 74
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 74
- 230000008569 process Effects 0.000 claims description 34
- 238000012545 processing Methods 0.000 claims description 34
- SJEBAWHUJDUKQK-UHFFFAOYSA-N 2-ethylanthraquinone Chemical compound C1=CC=C2C(=O)C3=CC(CC)=CC=C3C(=O)C2=C1 SJEBAWHUJDUKQK-UHFFFAOYSA-N 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 31
- 239000003054 catalyst Substances 0.000 claims description 28
- 230000005540 biological transmission Effects 0.000 claims description 26
- 239000007789 gas Substances 0.000 claims description 26
- 150000002431 hydrogen Chemical class 0.000 claims description 24
- 230000001276 controlling effect Effects 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 19
- 239000012530 fluid Substances 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 16
- 238000000605 extraction Methods 0.000 claims description 11
- 239000012071 phase Substances 0.000 claims description 11
- 238000007599 discharging Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 230000020477 pH reduction Effects 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- 238000005191 phase separation Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 2
- 230000005501 phase interface Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 10
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 10
- 238000002156 mixing Methods 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- YEVQZPWSVWZAOB-UHFFFAOYSA-N 2-(bromomethyl)-1-iodo-4-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=C(I)C(CBr)=C1 YEVQZPWSVWZAOB-UHFFFAOYSA-N 0.000 description 5
- 229910052763 palladium Inorganic materials 0.000 description 5
- 239000002253 acid Substances 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- HWOWEGAQDKKHDR-UHFFFAOYSA-N 4-hydroxy-6-(pyridin-3-yl)-2H-pyran-2-one Chemical compound O1C(=O)C=C(O)C=C1C1=CC=CN=C1 HWOWEGAQDKKHDR-UHFFFAOYSA-N 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000007130 inorganic reaction Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
- C01B15/022—Preparation from organic compounds
- C01B15/023—Preparation from organic compounds by the alkyl-anthraquinone process
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to an automatic strengthening system and a process for preparing hydrogen peroxide based on an anthraquinone method, which comprises the following steps: raw material supply unit, reaction unit, separation unit, micro-interface generator and automatic control unit. The reaction unit is internally provided with the micro-interface generator, hydrogen and air are smashed into micro-bubbles in the micro-interface generator, the micro-bubbles have additional pressure, and the micro-bubbles are not easy to mutually merge when colliding with each other, so that the phase interface area is larger than that of hydrogen before smashing, the hydrogen micro-bubbles are easier to mix with the working solution containing anthraquinone derivatives to form gas-liquid emulsion, the air bubbles are easier to mix with the hydrogenated solution containing 2-ethyl hydrogen anthraquinone to form gas-liquid emulsion, the effect of strengthening mass transfer in a lower preset operation condition range is achieved, and the yield of hydrogenation reaction and oxidation reaction is increased.
Description
Technical Field
The invention relates to the technical field of preparation of hydrogen peroxide by anthraquinone, in particular to an automatic strengthening system and process for preparing hydrogen peroxide by an anthraquinone method.
Background
The hydrogen peroxide is an important inorganic peroxide, an important petrochemical raw material and a fine chemical product, can be applied to the fields of fabric, paper pulp decoloration, chemical synthesis, wastewater treatment, medical treatment, metallurgy, military industry, food processing and the like, has the characteristics of oxidability, bleachability, green and environment-friendly use process and the like, and can be used as an oxidant, a bleaching agent, a disinfectant, a polymer initiator, a cross-linking agent, a propellant and the like. The production method of hydrogen peroxide includes anthraquinone method, electrolytic method, isopropanol oxidation method, inorganic reaction method, and direct hydrogen-oxygen synthesis method. Among them, the anthraquinone process is the mainstream method for producing hydrogen peroxide at home and abroad at present. With the stricter environmental regulations, the production capacity of products such as propylene oxide and green caprolactam produced by a hydrogen peroxide direct oxidation process (HPPO process) is increased, so that the market demand of hydrogen peroxide is vigorous.
Chinese patent publication No.: CN107473188A discloses a production process for preparing hydrogen peroxide by anthraquinone process, comprising the following steps: sequentially connecting a hydrogenation hypergravity reactor, an oxidation hypergravity reactor and an extraction hypergravity reactor in series; inputting hydrogen and anthraquinone-containing solution into a feeding cavity to perform gas-liquid two-phase efficient mixing to form a gas-liquid mixture for hydrogenation reaction to obtain anthraquinone-containing working solution; inputting oxygen and the working solution containing anthraquinone into a feeding cavity to carry out gas-liquid two-phase efficient mixing to form a gas-liquid mixture for oxidation reaction to obtain the working solution containing hydrogen peroxide and anthraquinone; feeding working solution containing hydrogen peroxide and anthraquinone and deionized water into an extraction supergravity reactor for extraction; and separating after extraction to obtain hydrogen peroxide. It can be seen that the method has the following problems:
firstly, in the method, only hydrogen and anthraquinone-containing solution are input into a feeding cavity for gas-liquid two-phase efficient mixing, the hydrogen enters a hydrogenation hypergravity reactor to form large bubbles, and the bubbles cannot be fully contacted with a catalyst and anthraquinone derivative working solution due to overlarge volume, so that the hydrogenation efficiency of the system is reduced.
Secondly, the method cannot automatically optimize and regulate the temperature and pressure of the system according to the real-time parameters of the reaction system, so that the reaction efficiency of the system is influenced.
Disclosure of Invention
Therefore, the invention provides an automatic strengthening system and process for preparing hydrogen peroxide based on an anthraquinone method, which are used for solving the problem of low system reaction efficiency caused by-products generated by uneven mixing of materials in the prior art.
On one hand, the invention provides an automatic strengthening system for preparing hydrogen peroxide based on an anthraquinone method, which comprises the following steps:
a raw material supply unit for supplying the reaction raw material containing anthraquinone derivative working solution, hydrogen, catalyst and air;
the reaction unit is connected with the raw material supply unit and is used for providing reaction sites for hydrogenation reaction and oxidation reaction;
the separation unit is connected with the reaction unit and is used for extracting and separating the materials output by the reaction unit;
the micro-interface generator is arranged at a designated position in the reaction unit, is connected with the raw material supply unit, converts the pressure energy of gas and/or the kinetic energy of liquid into the surface energy of bubbles and transmits the surface energy of the bubbles to the gas, so that the gas is crushed to form micron-sized bubbles with the diameter of more than or equal to 1 mu m and less than 1mm, the thickness of a liquid film is reduced, the mass transfer resistance is reduced, and the mass transfer efficiency and the reaction efficiency of a gas phase and a liquid phase are enhanced within a preset operating condition range;
and the automatic control unit is connected with the raw material supply unit, the reaction unit and the separation unit and is used for intelligently controlling the system.
Further, the reaction unit includes:
the hydrogenation tower is used for providing a reaction site for the anthraquinone derivative-containing working solution and hydrogen, at least one micro-interface processor is arranged at the bottom end inside the hydrogenation tower, and the hydrogenation tower comprises: a hydrogen return pipeline arranged on the side wall for returning hydrogen, a first tail gas outlet arranged on the top for discharging tail gas;
the hydrogenated liquid processor is connected with the hydrogenation tower and is used for filtering and cooling the hydrogenated material output by the hydrogenation tower;
the oxidation reaction tower is connected with the hydrogenated liquid processor and used for providing a reaction site for the material and the oxygen output by the hydrogenated liquid processor, at least one micro-interface processor is arranged at the bottom end inside the oxidation reaction tower, and the oxidation reaction tower comprises: the material reflux pipeline is arranged on the side wall and used for feeding back materials output by the oxidation reaction tower, and the second tail gas outlet is arranged at the top and used for discharging tail gas.
Further, the hydrogenation liquid treater comprises:
the filter is arranged on the side wall of the hydrogenation tower and is used for filtering the hydrogenation liquid;
a cooler connected with the filter and used for cooling the hydrogenation liquid;
and the hydrogenated liquid transmission pipeline is connected with the cooler and is used for transmitting the hydrogenated liquid.
Further, the raw material supply unit includes:
a hydrogen supply coupled to the micro-interface processor in the hydrogenation column for supplying hydrogen to the hydrogenation column, the hydrogen supply comprising: the hydrogen supply tank is used for storing hydrogen, and the hydrogen transmission pipe is connected with the hydrogen supply tank and used for transmitting hydrogen;
a working liquid supplier connected to the hydrogenation tower and located above the hydrogenation supplier for supplying the working liquid containing anthraquinone derivatives to the hydrogenation tower;
a catalyst supply port connected to the hydrogenation column and located above the working liquid supplier for putting a catalyst into the hydrogenation supplier;
an air supplier connected to the micro-interface processor in the oxidation reaction tower for supplying air to the oxidation reaction tower, the air supplier comprising: the air supply tank is used for storing air, and the air delivery pipe is connected with the air supply tank and used for delivering the air.
Further, the working fluid supplier includes:
a working liquid supply tank for storing a working liquid containing anthraquinone derivatives;
the heater is connected with the working solution supply tank and is used for preheating the working solution containing anthraquinone derivatives;
and the working liquid conveying pipe is connected with the heater and is used for conveying the working liquid.
Further, the separation unit includes:
the extractor is used for carrying out countercurrent extraction on the material output by the oxidation reaction tower and pure water;
the oil-water separator is connected with the extractor and is used for carrying out water phase and oil phase separation on the material output by the extractor;
and the purifier is connected with the oil-water separator and is used for purifying the water phase.
Further, the extractor comprises
A pure water feed pipe disposed at the top of the extractor for delivering pure water to the interior of the extractor;
the pure water acidification metering pump is connected with the pure water feeding pipeline and is used for adding phosphoric acid to adjust the acidity of the pure water;
and the pure water pump is connected with the pure water feeding pipeline and is used for conveying the pure water.
Further, the automatic control unit comprises an intelligent sensing module, a cloud processing module, an intelligent control module, an emergency early warning module and a power supply module, the intelligent sensing module, the intelligent control module, the emergency early warning module and the power supply module are all connected with the cloud processing module, wherein the intelligent sensing module is used for collecting data and transmitting the collected electric signals to the cloud processing module, the cloud processing module is used for carrying out cloud database analysis, screening and comparison on data parameters returned by the intelligent sensing module, optimizing optimal control parameters and sending corresponding control instructions to the intelligent control module, meanwhile, when the data parameters reach the preset value of the operation limit, the cloud processing module sends a corresponding instruction to the emergency early warning module, the intelligent control module is used for controlling and adjusting the system, the emergency early warning module is used for early warning the operation limit, and the power supply module is used for supplying electric energy to the automatic control unit.
Further, the smart sensor module includes:
a temperature sensor for temperature detection, the temperature sensor comprising: a first temperature sensor arranged in the heater and used for detecting the temperature of the working fluid containing anthraquinone derivatives, a second temperature sensor arranged in the hydrogenation tower and used for detecting the hydrogenation reaction temperature, a third temperature sensor arranged in the cooler and used for detecting the cooling temperature of the hydrogenation liquid, and a fourth temperature sensor arranged in the oxidation reaction tower and used for detecting the oxidation reaction temperature;
a pressure sensor for pressure detection, the pressure sensor comprising: the first pressure sensor is arranged in the hydrogenation tower and used for detecting the hydrogenation reaction pressure, and the second pressure sensor is arranged in the oxidation reaction tower and used for detecting the oxidation reaction pressure;
a flow sensor for flow sensing, the flow sensor comprising: a first flow sensor arranged in the hydrogen conveying pipe and used for detecting the flow of hydrogen, a second flow sensor arranged in the working liquid conveying pipe and used for detecting the flow of the anthraquinone derivative-containing working liquid, a third flow sensor arranged in the air conveying pipe and used for detecting the flow of air, and a fourth flow sensor arranged in the hydrogenated liquid conveying pipe and used for detecting the flow of the hydrogenated liquid;
the intelligent control module comprises:
the first controller is arranged on the heater and used for controlling the heating temperature of the heater;
a second controller provided on the cooler to control a cooler cooling temperature;
the first control valve is arranged on the hydrogen transmission pipe and used for controlling the air input into the hydrogenation tower;
the second control valve is arranged on the working liquid transmission pipe and used for controlling the liquid inlet amount entering the hydrogenation tower;
the third control valve is arranged on the air conveying pipe and used for controlling the air inflow entering the oxidation reaction tower;
and the fourth control valve is arranged on the hydrogenated liquid transmission pipeline and used for controlling the liquid inlet amount entering the oxidation reaction tower.
On the other hand, the invention provides an automatic strengthening process for preparing hydrogen peroxide based on an anthraquinone method, which comprises the following steps:
step 1: feeding the working liquid containing anthraquinone derivatives into the hydrogenation column through the hydrogen gas supplier, and feeding the catalyst into the hydrogenation column through the catalyst supply port;
step 2: hydrogen is conveyed into the hydrogenation tower through the hydrogen supplier, the hydrogen conveying pipe conveys the hydrogen to the micro-interface generator, and the micro-interface generator breaks the hydrogen to form micron-scale micro-scale bubbles;
and step 3: the micro-interface generator outputs micron-sized bubbles to the hydrogenation tower and mixes the micron-sized bubbles with the working solution containing anthraquinone derivatives to form gas-liquid emulsion, the gas-liquid emulsion is subjected to hydrogenation reaction under the action of a catalyst to generate hydrogenated liquid containing 2-ethyl hydrogen anthraquinone solution, and meanwhile, hydrogen which is not fully reacted is returned to the hydrogenation tower along a hydrogen return pipeline;
and 4, step 4: the hydrogenated liquid containing the 2-ethyl hydrogen anthraquinone solution enters a hydrogenated liquid processor, the hydrogenated liquid containing the 2-ethyl hydrogen anthraquinone passes through a filter, entrained solid impurities remain in the filter, filtrate is discharged from the bottom of the filter and enters the cooler, and the cooled hydrogenated liquid containing the 2-ethyl hydrogen anthraquinone enters the bottom of the oxidation reaction tower;
and 5: air is conveyed into the oxidation reaction tower through the air supplier, the air conveying pipe conveys the air to the micro-interface generator, and the micro-interface generator breaks the air to form micron-scale micro-scale bubbles;
step 6: the micro-interface generator outputs micron-sized bubbles to the oxidation reaction tower and mixes the micron-sized bubbles with the hydrogenated liquid containing 2-ethyl anthraquinone to form a gas-liquid emulsion, the gas-liquid emulsion is subjected to oxidation reaction to generate a mixture containing 2-ethyl anthraquinone and hydrogen peroxide, and meanwhile, the insufficiently oxidized mixture flows upwards and flows along the material backflow pipeline;
and 7: the mixture containing 2-ethyl anthraquinone and hydrogen peroxide enters the bottom of an extractor, pure water is regulated by a pure water acidification metering pump to regulate the acidity of the pure water, is transmitted into the extractor through a pure water feeding pipeline, is subjected to countercurrent extraction with the mixture containing 2-ethyl anthraquinone and hydrogen peroxide, and enters an oil-water separator, raffinate is discharged along the bottom of the oil-water separator, extract liquid flows out along the top of the oil-water separator and enters a purifier, and hydrogen peroxide as a product flows out along the purifier;
and 8: the first temperature sensor, the second temperature sensor, the third temperature sensor and the fourth temperature sensor respectively detect the temperature of a working fluid containing anthraquinone derivatives, the reaction temperature of a hydrogenation tower, the cooling temperature of a hydrogenation liquid and the reaction temperature of an oxidation reaction tower, when the temperature is not matched with a preset value, the corresponding first temperature sensor, the second temperature sensor, the third temperature sensor or the fourth temperature sensor sends an electric signal to the cloud processing module, the cloud processing module sends a control command to the corresponding first controller or second controller, the temperature control function is realized by adjusting the power of the heater or the cooler, and when the temperature reaches a preset limit value, the cloud processing module receives the electric signal, transmits the signal to the emergency early warning module and gives an alarm;
the first pressure sensor and the second pressure sensor respectively monitor the reaction pressure of the hydrogenation tower and the reaction pressure of the oxidation reaction tower, the first flow sensor, the second flow sensor, the third flow sensor and the fourth flow sensor respectively monitor the hydrogen flow of a hydrogen transmission pipe, the anthraquinone derivative-containing working liquid flow of a working liquid transmission pipe, the air flow of an air transmission pipe and the hydrogenation liquid flow of a hydrogenation liquid transmission pipeline, when the pressure is not matched with a preset value, the corresponding first pressure sensor or the second pressure sensor sends an electric signal to a cloud processing module, the cloud processing module sends a control command to the corresponding first control valve, the second control valve, the third control valve and the fourth control valve, and the reaction material amount entering the hydrogenation tower or the oxidation reaction tower is controlled by adjusting the corresponding flow, therefore, the control over the reaction rate and the reaction pressure is realized, and when the pressure reaches a preset limit value, the cloud processing module receives an electric signal, transmits the signal to the emergency early warning module and gives an alarm.
Compared with the prior art, the reaction unit is internally provided with the micro-interface generator, the hydrogen and the air are broken into micro-bubbles in the micro-interface generator, the micro-bubbles have additional pressure, and the micro-bubbles are not easy to mutually merge when colliding with each other, so that the phase interface area is larger than that of the hydrogen which is not broken, the micro-bubbles of the hydrogen are easier to mix with the working solution containing anthraquinone derivatives to form gas-liquid emulsion, the air bubbles are easier to mix with the hydrogenated solution containing 2-ethyl hydrogen anthraquinone to form gas-liquid emulsion, the effect of strengthening mass transfer in a lower preset operating condition range is achieved, and the yield of hydrogenation reaction and oxidation reaction is increased.
In particular, the micro-interface generator can break the input hydrogen and air into micro-bubbles, so that the phase interface area is greatly increased, the mass transfer and the reaction are promoted, the reaction pressure and the reaction temperature in the reaction unit can be reduced, the energy consumption is saved, and the whole reaction device is safer.
Furthermore, an automatic control unit is arranged in the whole reaction system, so that a worker can know the real-time situation of each data transmitted back by the intelligent sensing module at any time through the mobile equipment, and can realize accurate control of the temperature and the pressure in the whole reactor through changing a preset value, thereby further improving the reaction efficiency.
Drawings
FIG. 1 is a schematic structural diagram of an automatic strengthening system for preparing hydrogen peroxide based on an anthraquinone process;
FIG. 2 is a control flow chart of the automatic strengthening system for preparing hydrogen peroxide based on the anthraquinone process.
Detailed Description
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principle of the present invention, and do not limit the scope of the present invention.
It should be noted that in the description of the present invention, the terms of direction or positional relationship indicated by the terms "upper", "lower", "left", "right", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, which are only for convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
Furthermore, it should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Fig. 1 is a schematic structural diagram of an automatic strengthening system for preparing hydrogen peroxide based on an anthraquinone process, which includes a raw material supply unit 1 (not shown), a reaction unit 2 (not shown), a separation unit 3 and a micro-interface generator 4, where the raw material supply unit 1 is connected to the reaction unit 2 and is used to supply a working solution containing anthraquinone derivatives, hydrogen, a catalyst and air to reaction raw materials, the reaction unit 2 is connected to the separation unit 3 and is used to provide reaction sites for hydrogenation and oxidation reactions, and the separation unit 3 is used to extract and separate materials output by the reaction unit.
With continued reference to fig. 1, the reaction unit 2 includes a hydrogenation tower 21, a hydrogenation liquid processor 22 and an oxidation reaction tower 23, an output end of the hydrogenation tower 21 is connected to an input end of the hydrogenation liquid processor 22, an output end of the hydrogenation liquid processor 22 is connected to an input end of the oxidation reaction tower 23, the hydrogenation tower 21 is used for providing a reaction site for the anthraquinone derivative-containing working solution and the hydrogen gas, the hydrogenation liquid processor 22 is connected to the hydrogenation tower 21 and the oxidation reaction tower 23 and is used for filtering and cooling the hydrogenated material output by the hydrogenation tower, the oxidation reaction tower 23 is used for providing a reaction site for the material output by the hydrogenation liquid processor and the oxygen gas, at least one micro interface processor 4 is arranged at the bottom end of each of the hydrogenation tower 21 and the oxidation reaction tower 23 and is used for respectively crushing the hydrogen gas and the oxygen gas into micron-sized bubbles and mixing the micron-sized bubbles, and the working fluid containing anthraquinone derivatives and the hydrogenated fluid containing 2-ethyl hydrogen anthraquinone solution in the hydrogenation tower and the oxidation reaction tower are mixed to form gas-liquid emulsion, and it is understood that the hydrogenation tower 21 and the hydrogenation tower 21 can be tubular reactors, fixed bed reactors, etc., as long as the specified working state of the hydrogenation tower 21 and the oxidation reaction tower 23 can be met.
Specifically, the hydrogenation tower 21 includes a hydrogen return line 211 and a first tail gas outlet 212, wherein the hydrogen return line 211 is disposed on the side wall for returning hydrogen, and the first tail gas outlet 212 is disposed on the top for discharging tail gas.
Specifically, the hydrogenated liquid processor 22 includes a filter 221, a cooler 222 and a hydrogenated liquid transfer line 223, the filter 221 is disposed on the side wall of the hydrogenation tower and connected to the liquid phase material output end of the hydrogenation tower 21 for filtering the hydrogenated liquid, the cooler 222 is connected to the filter for cooling the hydrogenated liquid, and the hydrogenated liquid transfer line 223 is connected to the cooler for transferring the hydrogenated liquid.
It is understood that the type and power of the filter 221 and the cooler 222 are not particularly limited in this embodiment, as long as the filter 221 and the cooler 222 can achieve their designated operating states.
Specifically, the oxidation reaction tower 23 comprises a material return line 231 and a second tail gas outlet 232, wherein the material return line 231 is arranged on the side wall and used for returning the material output by the oxidation reaction tower, and the second tail gas outlet 232 is arranged at the top and used for discharging the tail gas.
With continued reference to fig. 1, the raw material supply unit 1 includes a hydrogen gas supplier 11 (not shown), a working liquid supplier 12, a catalyst supply port 13, and an air supplier 14, the hydrogen gas supplier 11 is connected to the micro-interface processor in the hydrogenation column to supply hydrogen gas to the hydrogenation column, the working liquid supplier 12 is connected to and above the hydrogenation supplier to supply the anthraquinone derivative-containing working liquid to the hydrogenation column, the catalyst supply port 13 is connected to and above the working liquid supplier to discharge the catalyst into the hydrogenation supplier, and the air supplier 14 is connected to the micro-interface processor in the oxidation column to supply air to the oxidation column.
Specifically, the hydrogen supply device 11 includes a hydrogen supply tank 111 for storing hydrogen, and a hydrogen transfer pipe 112 connected to the hydrogen supply tank for transferring hydrogen.
Specifically, the working fluid supplier 12 includes a working fluid supply tank 121 for storing the working fluid containing anthraquinone derivatives, a heater 122 connected to the working fluid supply tank for preheating the working fluid containing anthraquinone derivatives, and a working fluid transfer pipe 123 connected to the heater for transferring the working fluid.
Specifically, the air supplier 14 includes an air supply tank 141 for storing air, and an air transfer pipe 142 connected to the air supply tank 142 for transferring air.
It is understood that the materials and dimensions of the hydrogen gas delivery pipe 112, the working fluid delivery pipe 123 and the air delivery pipe 142 are not particularly limited in this embodiment, as long as the hydrogen gas, the working fluid and the air are delivered in specified volumes within specified time.
With reference to fig. 1, the separation unit 3 includes an extractor 31, an oil-water separator 32 and a purifier 33, the extractor 31 is used for performing counter-current extraction on the material output from the oxidation reaction tower and pure water, the oil-water separator 32 is connected to the extractor and is used for performing water-phase and oil-phase separation on the material output from the extractor, and the purifier 33 is connected to the oil-water separator and is used for purifying the water phase.
Specifically, the extractor 31 includes a pure water feeding pipe 311, a pure water acidification metering pump 312 and a pure water pump 313, wherein the pure water feeding pipe 311 is arranged at the top of the extractor and used for conveying pure water to the inside of the extractor, the pure water acidification metering pump 312 is connected with the pure water feeding pipe and used for adding phosphoric acid to adjust the acidity of the pure water, and the pure water pump 313 is connected with the pure water feeding pipe and used for conveying the pure water.
It is understood that the types and powers of the pure water acid adding metering pump 312 and the pure water pump 313 are not particularly limited in this embodiment, as long as the pure water acid adding metering pump 312 and the pure water pump 313 can reach their designated operating states.
When the system is operated, raw materials are conveyed into a reaction unit 2 through a raw material supply unit 1, wherein, working solution containing anthraquinone derivatives enters a heater 122 from a working solution supply tank 121, the working solution containing anthraquinone derivatives enters the heater 122 and is preheated through the heater 122, then the working solution is conveyed into a hydrogenation tower 21 through a working solution conveying pipe 123, a catalyst enters the hydrogenation tower 21 along a catalyst supply port 13, meanwhile, hydrogen enters a hydrogen conveying pipe 112 from a hydrogen supply tank 111 and is input into a micro-interface generator 4 in the hydrogenation tower 21, the micro-interface generator 4 breaks the hydrogen into micron-sized bubbles and enables the micron-sized bubbles and the working solution containing anthraquinone derivatives to be mixed to form gas-liquid emulsion, the gas-liquid emulsion is subjected to hydrogenation reaction under the action of the catalyst to generate hydrogenation solution containing 2-ethyl hydrogen anthraquinone solution, and tail gas in the reaction process is discharged out of the system through a first tail gas outlet 212, outputting the hydrogenated liquid containing the 2-ethyl hydrogen anthraquinone solution after reaction to a hydrogenated liquid processor 22, meanwhile, feeding the hydrogen which is not fully reacted back to the hydrogenation tower 21 along a hydrogen return pipeline 211, improving the utilization rate of the hydrogen, filtering solid impurities in the hydrogenated liquid by a filter 221 after the hydrogenated liquid containing the 2-ethyl hydrogen anthraquinone solution enters the hydrogenated liquid processor 22, cooling the filtrate to a proper temperature by a cooler 222, feeding the cooled hydrogenated liquid to the lower part of an oxidation reaction tower 23 along a hydrogenated liquid transmission pipeline 223, feeding air into an air transmission pipe 142 from an air supply tank 141 and inputting the air to a micro interface generator 4 in an oxidation reaction tower 23, crushing the air by the micro interface generator 4 to form micron-scale bubbles and mixing the micron-scale bubbles with the hydrogenated liquid containing the 2-ethyl hydrogen anthraquinone solution to form a gas-liquid emulsion, carrying out oxidation reaction on the gas-liquid emulsion to generate a mixture containing 2-ethylanthraquinone and hydrogen peroxide, discharging tail gas in the reaction process out of the system through a second tail gas outlet 232, feeding the mixture containing the 2-ethylanthraquinone and the hydrogen peroxide after the reaction which is not fully reacted back into an oxidation reaction tower 23 to improve the oxidation rate, then outputting the mixture containing the 2-ethylanthraquinone and the hydrogen peroxide to a separation unit 3, feeding the mixture containing the 2-ethylanthraquinone and the hydrogen peroxide to the bottom of an extractor 31, adjusting the acidity of pure water through a pure water acid and metering pump 312, transmitting the pure water into the extractor 31 through a pure water feeding pipeline 311, carrying out countercurrent extraction with the mixture containing the 2-ethylanthraquinone and the hydrogen peroxide, increasing the concentration of the hydrogen peroxide in the extractor 31 from top to bottom, and feeding the hydrogen peroxide into a water-oil separator 32 along the bottom of the extractor 31 for water-oil separation, the raffinate is discharged along the bottom of the oil-water separator 32, the extract flows out along the top of the oil-water separator 32 and enters the purifier 33, and the hydrogen peroxide product flows out along the purifier 33.
Referring to fig. 1 and 2, the automatic control unit includes an intelligent sensing module, a cloud processing module, an intelligent control module, an emergency pre-warning module and a power supply module, all of which are connected to the cloud processing module, wherein the intelligent sensing module is used for data acquisition and transmitting acquired electrical signals to the cloud processing module, the cloud processing module is used for performing cloud database analysis, screening and comparison on data parameters returned by the intelligent sensing module, optimizing optimal control parameters, and sending corresponding control instructions to the intelligent control module, and when the data parameters reach a preset value of an operation limit, the cloud processing module sends corresponding instructions to the emergency pre-warning module, the intelligent control module is used for controlling and adjusting the system, and the emergency pre-warning module is used for pre-warning the operation limit, the power supply module is used for supplying electric energy to the automatic control unit.
The intelligent sensing module comprises:
the temperature sensor includes: a first temperature sensor arranged in the heater and used for detecting the temperature of the working fluid containing anthraquinone derivatives, a second temperature sensor arranged in the hydrogenation tower and used for detecting the hydrogenation reaction temperature, a third temperature sensor arranged in the cooler and used for detecting the cooling temperature of the hydrogenation liquid, and a fourth temperature sensor arranged in the oxidation reaction tower and used for detecting the oxidation reaction temperature;
a pressure sensor for pressure detection, the pressure sensor comprising: the first pressure sensor is arranged in the hydrogenation tower and used for detecting the hydrogenation reaction pressure, and the second pressure sensor is arranged in the oxidation reaction tower and used for detecting the oxidation reaction pressure;
a flow sensor for flow sensing, the flow sensor comprising: a first flow sensor arranged in the hydrogen conveying pipe and used for detecting the flow of hydrogen, a second flow sensor arranged in the working liquid conveying pipe and used for detecting the flow of the anthraquinone derivative-containing working liquid, a third flow sensor arranged in the air conveying pipe and used for detecting the flow of air, and a fourth flow sensor arranged in the hydrogenated liquid conveying pipe and used for detecting the flow of the hydrogenated liquid;
further, the intelligent control module 5 (shown in the figure) includes:
the first controller is arranged on the heater and used for controlling the heating temperature of the heater;
a second controller provided on the cooler to control a cooler cooling temperature;
a first control valve 51 provided on the hydrogen transfer pipe to control the amount of intake air to the hydrogenation tower;
a second control valve 52, which is arranged on the working liquid transmission pipe and is used for controlling the liquid inlet amount entering the hydrogenation tower;
a third control valve 53, which is arranged on the air delivery pipe and is used for controlling the air input into the oxidation reaction tower;
and a fourth control valve 54 arranged on the hydrogenated liquid transmission pipeline and used for controlling the liquid inlet amount entering the oxidation reaction tower.
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described below with reference to examples; it should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
An automatic strengthening process for preparing hydrogen peroxide based on an anthraquinone method comprises the following steps:
step 1: feeding the working liquid containing anthraquinone derivatives into the hydrogenation column through the hydrogen gas supplier, and feeding the catalyst into the hydrogenation column through the catalyst supply port;
step 2: hydrogen is conveyed into the hydrogenation tower through the hydrogen supplier, the hydrogen conveying pipe conveys the hydrogen to the micro-interface generator, and the micro-interface generator breaks the hydrogen to form micron-scale micro-scale bubbles;
and step 3: the micro-interface generator outputs micron-sized bubbles to the hydrogenation tower and mixes the micron-sized bubbles with the working solution containing anthraquinone derivatives to form gas-liquid emulsion, the gas-liquid emulsion is subjected to hydrogenation reaction under the action of a catalyst to generate hydrogenated liquid containing 2-ethyl hydrogen anthraquinone solution, and meanwhile, hydrogen which is not fully reacted is returned to the hydrogenation tower along a hydrogen return pipeline;
and 4, step 4: the hydrogenated liquid containing the 2-ethyl hydrogen anthraquinone solution enters a hydrogenated liquid processor, the hydrogenated liquid containing the 2-ethyl hydrogen anthraquinone passes through a filter, entrained solid impurities remain in the filter, filtrate is discharged from the bottom of the filter and enters the cooler, and the cooled hydrogenated liquid containing the 2-ethyl hydrogen anthraquinone enters the bottom of the oxidation reaction tower;
and 5: air is conveyed into the oxidation reaction tower through the air supplier, the air conveying pipe conveys the air to the micro-interface generator, and the micro-interface generator breaks the air to form micron-scale micro-scale bubbles;
step 6: the micro-interface generator outputs micron-sized bubbles to the oxidation reaction tower and mixes the micron-sized bubbles with the hydrogenated liquid containing 2-ethyl anthraquinone to form a gas-liquid emulsion, the gas-liquid emulsion is subjected to oxidation reaction to generate a mixture containing 2-ethyl anthraquinone and hydrogen peroxide, and meanwhile, the insufficiently oxidized mixture flows upwards and flows along the material backflow pipeline;
and 7: the mixture containing 2-ethyl anthraquinone and hydrogen peroxide enters the bottom of an extractor, pure water is regulated by a pure water acidification metering pump to regulate the acidity of the pure water, is transmitted into the extractor through a pure water feeding pipeline, is subjected to countercurrent extraction with the mixture containing 2-ethyl anthraquinone and hydrogen peroxide, and enters an oil-water separator, raffinate is discharged along the bottom of the oil-water separator, extract liquid flows out along the top of the oil-water separator and enters a purifier, and hydrogen peroxide as a product flows out along the purifier;
and 8: the first temperature sensor, the second temperature sensor, the third temperature sensor and the fourth temperature sensor respectively detect the temperature of a working fluid containing anthraquinone derivatives, the reaction temperature of a hydrogenation tower, the cooling temperature of a hydrogenation liquid and the reaction temperature of an oxidation reaction tower, when the temperature is not matched with a preset value, the corresponding first temperature sensor, the second temperature sensor, the third temperature sensor or the fourth temperature sensor sends an electric signal to the cloud processing module, the cloud processing module sends a control command to the corresponding first controller or second controller, the temperature control function is realized by adjusting the power of the heater or the cooler, and when the temperature reaches a preset limit value, the cloud processing module receives the electric signal, transmits the signal to the emergency early warning module and gives an alarm;
the first pressure sensor and the second pressure sensor respectively monitor the reaction pressure of the hydrogenation tower and the reaction pressure of the oxidation reaction tower, the first flow sensor, the second flow sensor, the third flow sensor and the fourth flow sensor respectively monitor the hydrogen flow of a hydrogen transmission pipe, the anthraquinone derivative-containing working liquid flow of a working liquid transmission pipe, the air flow of an air transmission pipe and the hydrogenation liquid flow of a hydrogenation liquid transmission pipeline, when the pressure is not matched with a preset value, the corresponding first pressure sensor or the second pressure sensor sends an electric signal to a cloud processing module, the cloud processing module sends a control command to the corresponding first control valve, the second control valve, the third control valve and the fourth control valve, and the reaction material amount entering the hydrogenation tower or the oxidation reaction tower is controlled by adjusting the corresponding flow, therefore, the control over the reaction rate and the reaction pressure is realized, and when the pressure reaches a preset limit value, the cloud processing module receives an electric signal, transmits the signal to the emergency early warning module and gives an alarm.
Example 1
The system and the process are used for preparing hydrogen peroxide by an anthraquinone method, wherein:
hydrogenation reaction: in the process, a palladium catalyst is added into a hydrogenation tower, anthraquinone derivative-containing working solution consisting of 2-Ethyl Anthraquinone (EAQ), heavy aromatic hydrocarbon (AR) and trioctyl phosphate is introduced, wherein the concentration of the EAQ is 110g/L, the reaction temperature is 35 ℃, the reaction pressure is 0.10MPa, and the gas-liquid ratio in a micro-interface generator is 400: 1.
and (3) oxidation reaction: in the process, the reaction temperature in the hydrogenation tower is 38 ℃, the reaction pressure is 0.15MPa, and the gas-liquid ratio in the micro-interface generator is 600: 1.
example 2
The system and the process are used for preparing hydrogen peroxide by an anthraquinone method, wherein:
hydrogenation reaction: in the process, a palladium catalyst is added into a hydrogenation tower, anthraquinone derivative-containing working solution consisting of 2-Ethyl Anthraquinone (EAQ), heavy aromatic hydrocarbon (AR) and trioctyl phosphate is introduced, wherein the concentration of the EAQ is 120g/L, the reaction temperature is 37 ℃, the reaction pressure is 0.13MPa, and the gas-liquid ratio in a micro-interface generator is 500: 1.
and (3) oxidation reaction: in the process, the reaction temperature in the hydrogenation tower is 40 ℃, the reaction pressure is 0.17MPa, and the gas-liquid ratio in the micro-interface generator is 700: 1.
example 3
The system and the process are used for preparing hydrogen peroxide by an anthraquinone method, wherein:
hydrogenation reaction: in the process, a palladium catalyst is added into a hydrogenation tower, anthraquinone derivative-containing working solution consisting of 2-Ethyl Anthraquinone (EAQ), heavy aromatic hydrocarbon (AR) and trioctyl phosphate is introduced, wherein the concentration of the EAQ is 125g/L, the reaction temperature is 39 ℃, the reaction pressure is 0.14MPa, and the gas-liquid ratio in a micro-interface generator is 600: 1.
and (3) oxidation reaction: in the process, the reaction temperature in the hydrogenation tower is 42 ℃, the reaction pressure is 0.19MPa, and the gas-liquid ratio in the micro-interface generator is 750: 1.
example 4
The system and the process are used for preparing hydrogen peroxide by an anthraquinone method, wherein:
hydrogenation reaction: in the process, a palladium catalyst is added into a hydrogenation tower, anthraquinone derivative-containing working solution consisting of 2-Ethyl Anthraquinone (EAQ), heavy aromatic hydrocarbon (AR) and trioctyl phosphate is introduced, wherein the concentration of the EAQ is 130g/L, the reaction temperature is 41 ℃, the reaction pressure is 0.17MPa, and the gas-liquid ratio in a micro-interface generator is 700: 1.
and (3) oxidation reaction: in the process, the reaction temperature in the hydrogenation tower is 45 ℃, the reaction pressure is 0.21MPa, and the gas-liquid ratio in the micro-interface generator is 800: 1.
example 5
The system and the process are used for preparing hydrogen peroxide by an anthraquinone method, wherein:
hydrogenation reaction: in the process, a palladium catalyst is added into a hydrogenation tower, anthraquinone derivative-containing working solution consisting of 2-Ethyl Anthraquinone (EAQ), heavy aromatic hydrocarbon (AR) and trioctyl phosphate is introduced, wherein the concentration of the EAQ is 135g/L, the reaction temperature is 38 ℃, the reaction pressure is 0.19MPa, and the gas-liquid ratio in a micro-interface generator is 800: 1.
and (3) oxidation reaction: in the process, the reaction temperature in the hydrogenation tower is 45 ℃, the reaction pressure is 0.23MPa, and the gas-liquid ratio in the micro-interface generator is 850: 1.
comparative example
The hydrogen peroxide is prepared by an anthraquinone process by using the prior art, wherein the process parameters selected in the embodiment are the same as those in the embodiment 5.
After detection, the hydrogenation efficiency and the oxidation reaction conversion rate are shown in the following table after the system and the process and the prior art are used:
so far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention; various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An automatic strengthening system for preparing hydrogen peroxide based on an anthraquinone method is characterized by comprising the following steps:
a raw material supply unit for supplying the reaction raw material containing anthraquinone derivative working solution, hydrogen, catalyst and air;
the reaction unit is connected with the raw material supply unit and is used for providing reaction sites for hydrogenation reaction and oxidation reaction;
the separation unit is connected with the reaction unit and is used for extracting and separating the materials output by the reaction unit;
the micro-interface generator is arranged at a designated position in the reaction unit, is connected with the raw material supply unit, converts the pressure energy of gas and/or the kinetic energy of liquid into the surface energy of bubbles and transmits the surface energy of the bubbles to the gas, so that the gas is crushed to form micron-sized bubbles with the diameter of more than or equal to 1 mu m and less than 1mm, the thickness of a liquid film is reduced, the mass transfer resistance is reduced, and the mass transfer efficiency and the reaction efficiency of a gas phase and a liquid phase are enhanced within a preset operating condition range;
and the automatic control unit is connected with the raw material supply unit, the reaction unit and the separation unit and is used for intelligently controlling the system.
2. The automatic strengthening system for preparing hydrogen peroxide based on the anthraquinone process according to claim 1, wherein the reaction unit comprises:
the hydrogenation tower is used for providing a reaction site for the anthraquinone derivative-containing working solution and hydrogen, at least one micro-interface processor is arranged at the bottom end inside the hydrogenation tower, and the hydrogenation tower comprises: a hydrogen return pipeline arranged on the side wall for returning hydrogen, a first tail gas outlet arranged on the top for discharging tail gas;
the hydrogenated liquid processor is connected with the hydrogenation tower and is used for filtering and cooling the hydrogenated material output by the hydrogenation tower;
the oxidation reaction tower is connected with the hydrogenated liquid processor and used for providing a reaction site for the material and the oxygen output by the hydrogenated liquid processor, at least one micro-interface processor is arranged at the bottom end inside the oxidation reaction tower, and the oxidation reaction tower comprises: the material reflux pipeline is arranged on the side wall and used for feeding back materials output by the oxidation reaction tower, and the second tail gas outlet is arranged at the top and used for discharging tail gas.
3. The automatic strengthening system for preparing hydrogen peroxide based on the anthraquinone process according to claim 2, wherein the hydrogenation liquid processor comprises:
the filter is arranged on the side wall of the hydrogenation tower and is used for filtering the hydrogenation liquid;
a cooler connected with the filter and used for cooling the hydrogenation liquid;
and the hydrogenated liquid transmission pipeline is connected with the cooler and is used for transmitting the hydrogenated liquid.
4. The automatic strengthening system for preparing hydrogen peroxide based on the anthraquinone process according to claim 1, wherein the raw material supply unit comprises:
a hydrogen supply coupled to the micro-interface processor in the hydrogenation column for supplying hydrogen to the hydrogenation column, the hydrogen supply comprising: the hydrogen supply tank is used for storing hydrogen, and the hydrogen transmission pipe is connected with the hydrogen supply tank and used for transmitting hydrogen;
a working liquid supplier connected to the hydrogenation tower and located above the hydrogenation supplier for supplying the working liquid containing anthraquinone derivatives to the hydrogenation tower;
a catalyst supply port connected to the hydrogenation column and located above the working liquid supplier for putting a catalyst into the hydrogenation supplier;
an air supplier connected to the micro-interface processor in the oxidation reaction tower for supplying air to the oxidation reaction tower, the air supplier comprising: the air supply tank is used for storing air, and the air delivery pipe is connected with the air supply tank and used for delivering the air.
5. The automatic strengthening system for preparing hydrogen peroxide based on the anthraquinone process according to claim 4, wherein the working liquid supplier comprises:
a working liquid supply tank for storing a working liquid containing anthraquinone derivatives;
the heater is connected with the working solution supply tank and is used for preheating the working solution containing anthraquinone derivatives;
and the working liquid conveying pipe is connected with the heater and is used for conveying the working liquid.
6. The automatic strengthening system for preparing hydrogen peroxide based on the anthraquinone process according to claim 1, wherein the separation unit comprises:
the extractor is used for carrying out countercurrent extraction on the material output by the oxidation reaction tower and pure water;
the oil-water separator is connected with the extractor and is used for carrying out water phase and oil phase separation on the material output by the extractor;
and the purifier is connected with the oil-water separator and is used for purifying the water phase.
7. The automatic strengthening system for preparing hydrogen peroxide based on the anthraquinone process according to claim 6, wherein the extractor comprises:
a pure water feed pipe disposed at the top of the extractor for delivering pure water to the interior of the extractor;
the pure water acidification metering pump is connected with the pure water feeding pipeline and is used for adding phosphoric acid to adjust the acidity of the pure water;
and the pure water pump is connected with the pure water feeding pipeline and is used for conveying the pure water.
8. The automatic strengthening system for preparing hydrogen peroxide based on the anthraquinone process as claimed in claim 1, wherein the automatic control unit comprises an intelligent sensing module, a cloud processing module, an intelligent control module, an emergency early warning module and a power supply module, the intelligent sensing module, the intelligent control module, the emergency early warning module and the power supply module are all connected with the cloud processing module, wherein the intelligent sensing module is used for collecting data and transmitting collected electric signals to the cloud processing module, the cloud processing module is used for performing cloud database analysis, screening and comparison on data parameters returned by the intelligent sensing module, optimizing optimal control parameters and sending corresponding control instructions to the intelligent control module, and when the data parameters reach a preset value of an operation limit, the cloud processing module sends corresponding instructions to the emergency early warning module, and the intelligent control module is used for controlling and adjusting the system, the emergency early warning module is used for early warning the operation limit, and the power supply module is used for supplying electric energy to the automatic control unit.
9. The automatic strengthening system for preparing hydrogen peroxide based on the anthraquinone process according to claim 8, wherein the intelligent sensing module comprises:
a temperature sensor for temperature detection, the temperature sensor comprising: a first temperature sensor arranged in the heater and used for detecting the temperature of the working fluid containing anthraquinone derivatives, a second temperature sensor arranged in the hydrogenation tower and used for detecting the hydrogenation reaction temperature, a third temperature sensor arranged in the cooler and used for detecting the cooling temperature of the hydrogenation liquid, and a fourth temperature sensor arranged in the oxidation reaction tower and used for detecting the oxidation reaction temperature;
a pressure sensor for pressure detection, the pressure sensor comprising: the first pressure sensor is arranged in the hydrogenation tower and used for detecting the hydrogenation reaction pressure, and the second pressure sensor is arranged in the oxidation reaction tower and used for detecting the oxidation reaction pressure;
a flow sensor for flow sensing, the flow sensor comprising: a first flow sensor arranged in the hydrogen conveying pipe and used for detecting the flow of hydrogen, a second flow sensor arranged in the working liquid conveying pipe and used for detecting the flow of the anthraquinone derivative-containing working liquid, a third flow sensor arranged in the air conveying pipe and used for detecting the flow of air, and a fourth flow sensor arranged in the hydrogenated liquid conveying pipe and used for detecting the flow of the hydrogenated liquid;
the intelligent control module comprises:
the first controller is arranged on the heater and used for controlling the heating temperature of the heater;
a second controller provided on the cooler to control a cooler cooling temperature;
the first control valve is arranged on the hydrogen transmission pipe and used for controlling the air input into the hydrogenation tower;
the second control valve is arranged on the working liquid transmission pipe and used for controlling the liquid inlet amount entering the hydrogenation tower;
the third control valve is arranged on the air conveying pipe and used for controlling the air inflow entering the oxidation reaction tower;
and the fourth control valve is arranged on the hydrogenated liquid transmission pipeline and used for controlling the liquid inlet amount entering the oxidation reaction tower.
10. An automatic strengthening process for preparing hydrogen peroxide based on an anthraquinone method is characterized by comprising the following steps:
step 1: feeding the working liquid containing anthraquinone derivatives into the hydrogenation column through the hydrogen gas supplier, and feeding the catalyst into the hydrogenation column through the catalyst supply port;
step 2: hydrogen is conveyed into the hydrogenation tower through the hydrogen supplier, the hydrogen conveying pipe conveys the hydrogen to the micro-interface generator, and the micro-interface generator breaks the hydrogen to form micron-scale micro-scale bubbles;
and step 3: the micro-interface generator outputs micron-sized bubbles to the hydrogenation tower and mixes the micron-sized bubbles with the working solution containing anthraquinone derivatives to form gas-liquid emulsion, the gas-liquid emulsion is subjected to hydrogenation reaction under the action of a catalyst to generate hydrogenated liquid containing 2-ethyl hydrogen anthraquinone solution, and meanwhile, hydrogen which is not fully reacted is returned to the hydrogenation tower along a hydrogen return pipeline;
and 4, step 4: the hydrogenated liquid containing the 2-ethyl hydrogen anthraquinone solution enters a hydrogenated liquid processor, the hydrogenated liquid containing the 2-ethyl hydrogen anthraquinone passes through a filter, entrained solid impurities remain in the filter, filtrate is discharged from the bottom of the filter and enters the cooler, and the cooled hydrogenated liquid containing the 2-ethyl hydrogen anthraquinone enters the bottom of the oxidation reaction tower;
and 5: air is conveyed into the oxidation reaction tower through the air supplier, the air conveying pipe conveys the air to the micro-interface generator, and the micro-interface generator breaks the air to form micron-scale micro-scale bubbles;
step 6: the micro-interface generator outputs micron-sized bubbles to the oxidation reaction tower and mixes the micron-sized bubbles with the hydrogenated liquid containing 2-ethyl anthraquinone to form a gas-liquid emulsion, the gas-liquid emulsion is subjected to oxidation reaction to generate a mixture containing 2-ethyl anthraquinone and hydrogen peroxide, and meanwhile, the insufficiently oxidized mixture flows upwards and flows along the material backflow pipeline;
and 7: the mixture containing 2-ethyl anthraquinone and hydrogen peroxide enters the bottom of an extractor, pure water is regulated by a pure water acidification metering pump to regulate the acidity of the pure water, is transmitted into the extractor through a pure water feeding pipeline, is subjected to countercurrent extraction with the mixture containing 2-ethyl anthraquinone and hydrogen peroxide, and enters an oil-water separator, raffinate is discharged along the bottom of the oil-water separator, extract liquid flows out along the top of the oil-water separator and enters a purifier, and hydrogen peroxide as a product flows out along the purifier;
and 8: the first temperature sensor, the second temperature sensor, the third temperature sensor and the fourth temperature sensor respectively detect the temperature of a working fluid containing anthraquinone derivatives, the reaction temperature of a hydrogenation tower, the cooling temperature of a hydrogenation liquid and the reaction temperature of an oxidation reaction tower, when the temperature is not matched with a preset value, the corresponding first temperature sensor, the second temperature sensor, the third temperature sensor or the fourth temperature sensor sends an electric signal to the cloud processing module, the cloud processing module sends a control command to the corresponding first controller or second controller, the temperature control function is realized by adjusting the power of the heater or the cooler, and when the temperature reaches a preset limit value, the cloud processing module receives the electric signal, transmits the signal to the emergency early warning module and gives an alarm;
the first pressure sensor and the second pressure sensor respectively monitor the reaction pressure of the hydrogenation tower and the reaction pressure of the oxidation reaction tower, the first flow sensor, the second flow sensor, the third flow sensor and the fourth flow sensor respectively monitor the hydrogen flow of a hydrogen transmission pipe, the anthraquinone derivative-containing working liquid flow of a working liquid transmission pipe, the air flow of an air transmission pipe and the hydrogenation liquid flow of a hydrogenation liquid transmission pipeline, when the pressure is not matched with a preset value, the corresponding first pressure sensor or the second pressure sensor sends an electric signal to a cloud processing module, the cloud processing module sends a control command to the corresponding first control valve, the second control valve, the third control valve and the fourth control valve, and the reaction material amount entering the hydrogenation tower or the oxidation reaction tower is controlled by adjusting the corresponding flow, therefore, the control over the reaction rate and the reaction pressure is realized, and when the pressure reaches a preset limit value, the cloud processing module receives an electric signal, transmits the signal to the emergency early warning module and gives an alarm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910867797.8A CN112499593A (en) | 2019-09-14 | 2019-09-14 | Automatic strengthening system and process for preparing hydrogen peroxide based on anthraquinone method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910867797.8A CN112499593A (en) | 2019-09-14 | 2019-09-14 | Automatic strengthening system and process for preparing hydrogen peroxide based on anthraquinone method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112499593A true CN112499593A (en) | 2021-03-16 |
Family
ID=74923643
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910867797.8A Pending CN112499593A (en) | 2019-09-14 | 2019-09-14 | Automatic strengthening system and process for preparing hydrogen peroxide based on anthraquinone method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112499593A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113477189A (en) * | 2021-07-14 | 2021-10-08 | 南京延长反应技术研究院有限公司 | Automatic mixing system and method based on micro-interface mixing tank |
| WO2023284028A1 (en) * | 2021-07-16 | 2023-01-19 | 南京延长反应技术研究院有限公司 | Micro-interface enhanced oxidation system and oxidation method for preparing hydrogen peroxide |
| WO2023284027A1 (en) * | 2021-07-16 | 2023-01-19 | 南京延长反应技术研究院有限公司 | Tower-type enhanced oxidation system and method for preparing hydrogen peroxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588176A (en) * | 2013-11-04 | 2014-02-19 | 扬州荣祥化工技术开发设计有限公司 | Production method of hydrogen peroxide |
| CN203612954U (en) * | 2013-09-27 | 2014-05-28 | 福州一化化学品股份有限公司 | Hydrogenation section system for hydrogen peroxide production with anthraquinone process |
| CN207581356U (en) * | 2017-11-30 | 2018-07-06 | 湖南中天元环境工程有限公司 | The reaction system of process for prepairng hydrogen peroxide by anthraquinone |
-
2019
- 2019-09-14 CN CN201910867797.8A patent/CN112499593A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203612954U (en) * | 2013-09-27 | 2014-05-28 | 福州一化化学品股份有限公司 | Hydrogenation section system for hydrogen peroxide production with anthraquinone process |
| CN103588176A (en) * | 2013-11-04 | 2014-02-19 | 扬州荣祥化工技术开发设计有限公司 | Production method of hydrogen peroxide |
| CN207581356U (en) * | 2017-11-30 | 2018-07-06 | 湖南中天元环境工程有限公司 | The reaction system of process for prepairng hydrogen peroxide by anthraquinone |
Non-Patent Citations (2)
| Title |
|---|
| 张志炳 等: ""多相反应体系的微界面强化简述"", 《化工学报》 * |
| 张焱焱: ""蒽醌法过氧化氢装置的生产控制及技术改造"", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113477189A (en) * | 2021-07-14 | 2021-10-08 | 南京延长反应技术研究院有限公司 | Automatic mixing system and method based on micro-interface mixing tank |
| WO2023284028A1 (en) * | 2021-07-16 | 2023-01-19 | 南京延长反应技术研究院有限公司 | Micro-interface enhanced oxidation system and oxidation method for preparing hydrogen peroxide |
| WO2023284027A1 (en) * | 2021-07-16 | 2023-01-19 | 南京延长反应技术研究院有限公司 | Tower-type enhanced oxidation system and method for preparing hydrogen peroxide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN213493579U (en) | Automatic strengthening system for preparing hydrogen peroxide based on anthraquinone method | |
| CN112499593A (en) | Automatic strengthening system and process for preparing hydrogen peroxide based on anthraquinone method | |
| CN213505981U (en) | System for preparing hydrogen peroxide based on anthraquinone method | |
| CN106629622A (en) | Hydrogenation method and hydrogenation device for oxanthranol-containing working solution | |
| CN102627714A (en) | System and process for production of polyvinyl chloride | |
| CN112499592A (en) | System and process for preparing hydrogen peroxide based on anthraquinone method | |
| CN107879337A (en) | Prepare the method and its equipment of graphene oxide | |
| CN102002395A (en) | Method and device for dissolving gas in liquid-phase circulating hydrodesulfurization system | |
| CN103449381B (en) | A kind of technique for anthraquinone compounds hydride suspension | |
| CN112375035A (en) | Continuous reaction system and method for preparing 2-chloronicotinic acid | |
| CN101353336A (en) | Method and system for preparing furfuryl alcohol by furfural liquid phase hydrogenation | |
| CN112499597A (en) | System and process for preparing hydrogen peroxide based on isopropanol method | |
| JP2024515084A (en) | Micro-interface-enhanced oxidation system and oxidation method for producing hydrogen peroxide solution | |
| CN113479850A (en) | Tower type enhanced oxidation system and method for preparing hydrogen peroxide | |
| CN202047018U (en) | Device for preparing cyclohexene from benzene through selective hydrogenation | |
| CN215540716U (en) | Tower type enhanced oxidation system for preparing hydrogen peroxide | |
| CN216987426U (en) | Multifunctional experimental device for gas-liquid reaction | |
| CN104562082A (en) | Method for preparing copper-containing solution by dissolving waste copper | |
| CN103611331A (en) | Supercritical extraction/reaction integrated device | |
| CN107473188A (en) | It is a kind of to use the anthraquinone production technology for preparing hydrogen peroxide | |
| CN103551086A (en) | Hydrogenation reaction device for refining caprolactam | |
| CN104861131B (en) | A kind of continuous technique for removing SEBS glues or SBS glue neutral and alkali impurity of industrialization | |
| CN210186491U (en) | Plant/traditional chinese medicine extract and continuous automatic flocculation equipment of water treatment | |
| CN213388443U (en) | Reinforcing system for preparing 1, 4-butanediol from butadiene and acetic acid | |
| CN213505982U (en) | Intelligent strengthening system for preparing hydrogen peroxide based on isopropanol method |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210316 |