CN110075779B - Jet reactor for powder material synthesis and powder synthesis method - Google Patents
Jet reactor for powder material synthesis and powder synthesis method Download PDFInfo
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- CN110075779B CN110075779B CN201910466144.9A CN201910466144A CN110075779B CN 110075779 B CN110075779 B CN 110075779B CN 201910466144 A CN201910466144 A CN 201910466144A CN 110075779 B CN110075779 B CN 110075779B
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- jet
- injection hole
- hole
- injection
- buffer groove
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- 239000000463 material Substances 0.000 title claims abstract description 42
- 239000000843 powder Substances 0.000 title claims abstract description 36
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 14
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 10
- 238000001308 synthesis method Methods 0.000 title claims abstract description 6
- 238000002347 injection Methods 0.000 claims abstract description 116
- 239000007924 injection Substances 0.000 claims abstract description 116
- 238000002156 mixing Methods 0.000 claims abstract description 65
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical class OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 21
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 21
- 239000004571 lime Substances 0.000 claims abstract description 21
- 239000008267 milk Substances 0.000 claims abstract description 21
- 210000004080 milk Anatomy 0.000 claims abstract description 21
- 235000013336 milk Nutrition 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 16
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 15
- 239000011575 calcium Substances 0.000 claims abstract description 15
- 229910052751 metal Chemical class 0.000 claims abstract description 13
- 239000002184 metal Chemical class 0.000 claims abstract description 13
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 13
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 8
- 239000012266 salt solution Substances 0.000 claims abstract description 8
- 229910000000 metal hydroxide Inorganic materials 0.000 claims abstract description 4
- 150000004692 metal hydroxides Chemical class 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 11
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 16
- 239000000725 suspension Substances 0.000 abstract description 6
- 239000000376 reactant Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 11
- 239000007921 spray Substances 0.000 description 11
- 239000007795 chemical reaction product Substances 0.000 description 9
- 239000011162 core material Substances 0.000 description 9
- 239000012530 fluid Substances 0.000 description 8
- 238000005265 energy consumption Methods 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000002829 reductive effect Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 2
- 235000019700 dicalcium phosphate Nutrition 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003116 impacting effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 230000036961 partial effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000006115 defluorination reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/20—Jet mixers, i.e. mixers using high-speed fluid streams
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/20—Jet mixers, i.e. mixers using high-speed fluid streams
- B01F25/28—Jet mixers, i.e. mixers using high-speed fluid streams characterised by the specific design of the jet injector
-
- 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
- B01J19/0053—Details of the reactor
-
- 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
- B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/322—Preparation by neutralisation of orthophosphoric acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Cosmetics (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a jet reactor for synthesizing powder materials and a method for synthesizing calcium hydrophosphate, nano or micron powder. The reactor jet hole I is arranged on the body and communicated with the feed inlet I; a buffer groove I is arranged at the periphery or one side of the injection hole I and is communicated with a feed inlet II on the body, and the buffer groove I is provided with an injection hole II pointing to the injection hole I; or the body is provided with a buffer groove II and a buffer groove I, the buffer groove I is provided with an injection hole II pointing to the injection hole I, the body is provided with a feed inlet I, a feed inlet II and the buffer groove II which are communicated, and the injection hole I is communicated with the buffer groove II. In the synthesis method, lime milk or alkali liquor/reducing agent is sprayed downwards from an injection hole I and is collided with phosphoric acid or metal salt solution jet flow of an injection hole II to generate calcium hydrophosphate, nano or micron metal hydroxide or metal powder. The reactant forms suspension collision through the injection hole II and the injection hole I, and solves the problems of uneven mixing of products in the traditional reaction tank, poor batch stability and channel blockage during powder synthesis in the microreactor.
Description
Technical Field
The invention belongs to the technical field of chemical equipment, and particularly relates to a spraying reactor for synthesizing powder materials, which has the advantages of simple structure, uniform mixing, low energy consumption and on-line mixing, and a method for synthesizing calcium hydrophosphate, nano or micron powder.
Background
In the industries of petroleum, chemical industry, rubber, pesticides, dyes, medicines, foods and the like, the technological processes of vulcanization, nitration, hydrogenation, hydrocarbylation, polymerization, condensation and the like are based on the premise of fully mixing reaction materials, so that the uniformity of mixing can greatly influence the distribution of final products, the yield and quality of target products, and simultaneously influence the design of the whole production process, energy consumption and other indexes.
Therefore, it is an important goal of mixing how to ensure efficient, low consumption of the mixing process and high homogeneity of the mixture. Currently, mixing between two or more phases generally has two ways:
1. batch mixing: the premix is placed in the same vessel and mixed by means of a paddle therein. The mode is simple in structure, but on-line mixing cannot be realized, so that production efficiency is low, and the materials generated after the mixing reaction are difficult to uniformly mix under the condition of generating high-viscosity materials, so that the generated materials after the reaction are partially uneven, and the stability of product batches is poor.
2. In-line mixing: the premixed materials are continuously mixed. Although the production efficiency is higher, the mixing process still needs to be completed through stirring or mutually impacting reaction in the container, so that the materials are difficult to uniformly mix under the condition that high-viscosity materials are generated after the mixing reaction, and the relatively high-viscosity materials can generate large and complex friction resistance when the generated materials and the container wall relatively move due to the mutually impacting reaction in the container, so that the high-viscosity materials are not easy to flow and separate in the cavity, the cavity of the container is easy to be blocked, and the cleaning is inconvenient.
The jet reactor uses high-speed mobile phase to unwind other phases, so that two phases or multiple phases are mutually impacted to fully mix materials, and compared with the stirring and mixing, the jet reactor has the advantages of low energy consumption, easy realization of on-line mixing, high heat transfer efficiency and mass transfer efficiency, high reaction rate, capability of obviously reducing the volume of the reactor and shortening the reaction time, and is a high-efficiency multiphase reactor. However, the conventional spray reactor is provided with a mixing chamber for uniform mixing, and can adapt to the mixing reaction of common products, but for the direct synthesis reaction such as nano-sized and micro-sized powder and the calcium hydrophosphate generating process, the viscosity of the reaction product after the reaction of phosphoric acid and lime milk is very high to form foam in the calcium hydrophosphate synthesis reaction, and the reaction product with high viscosity can cause difficulty in flowing and separating in the mixing chamber, so that not only is the two phases difficult to uniformly mix, but also certain partial acid of the product is high, and certain partial calcium is high, so that the batch stability of the product is poor, but also the cavity of the container is easy to be blocked and the cleaning is inconvenient. Therefore, the direct synthesis reaction of the calcium hydrophosphate is generally carried out by adopting trough stirring, but the equipment occupies large area, the maintenance and repair cost of the equipment is high, the strength requirement of the stirrer is high, the energy consumption is high, the online continuous production is difficult to realize, and the production efficiency is lower.
Disclosure of Invention
The invention aims at providing a spray reactor for synthesizing powder materials, which has the advantages of simple structure, uniform mixing, low energy consumption and on-line mixing, and the invention aims at providing a method for synthesizing calcium hydrophosphate based on the spray reactor for synthesizing the powder materials, and the invention aims at providing a method for synthesizing nano or micro powder based on the spray reactor for synthesizing the powder materials.
The first object of the present invention is achieved by: the device comprises a body, a feed inlet I, a feed inlet II, an injection hole I, a buffer groove I and an injection hole II, wherein the injection hole I is arranged in the middle or on one side of the body, and the feed inlet I is arranged on the upper or side wall of the body and is communicated with the injection hole I; the body is provided with a closed buffer groove I at the periphery of the injection hole I in the middle or at the other side of the injection hole I at one side, the bottom of the buffer groove I is provided with an injection hole II, the outlet of which is obliquely directed to the extending direction of the injection hole I, and the upper part or the side wall of the body is provided with a feed inlet II and is communicated with the buffer groove I; or this internal inclosed buffer tank II that sets up, the periphery or the one side of this internal buffer tank II set up inclosed buffer tank I, buffer tank I's tank bottom portion is equipped with the jet orifice II that the export slope was directional jet orifice I extending direction, upper portion or the lateral wall of body set up feed inlet I and communicate with buffer tank II, jet orifice I communicates with buffer tank II bottom or lateral wall, upper portion or the lateral wall of body set up feed inlet II and communicate with buffer tank I.
The second object of the present invention is achieved by: lime milk is sprayed out through the spray holes I of the spray reactor to form lime milk flow, phosphoric acid is obliquely sprayed to the lime milk flow through at least two symmetrical spray holes II arranged on the periphery of the lime milk flow, and the lime milk flow and phosphoric acid react to generate calcium hydrophosphate in the process of jet collision and co-flow.
The third object of the present invention is achieved by: the alkali solution or the reducing agent solution is sprayed out through a spray hole I of the spray reactor to form a jet flow, the metal salt solution is obliquely sprayed to the jet flow from a spray hole II, and nano or micron metal hydroxide powder or metal powder is generated in the collision and flowing down process of the metal salt solution and the alkali solution or the reducing agent solution.
The invention has the beneficial effects that: according to the invention, the jet hole I is arranged in the middle part or on one side of the body, then the outlet extending direction of the body is inclined with the outlet extending direction of the jet hole I compared with the jet hole II on the outer side of the body, and the jet hole II generates necking action through the buffer groove I to enhance the turbulence degree of the jet material, so that the mixing effect between the jet hole I and the jet material of the jet hole I is enhanced, a traditional solid mixing chamber is omitted, the jet hole II and the jet material jetted by the jet hole I form suspension jet collision, millisecond mixing between the materials is realized, the difficult mixing problem that part of the materials still need to be mixed after a large amount of foam and/or high-viscosity reaction products are generated in the prior art is avoided, and the batch stability of the reaction products is good; and the suspension jet collision can also solve the problems of channel blockage and inconvenient cleaning when powder materials are synthesized in the microreactor, thereby realizing online mixing reaction. Therefore, the invention has the characteristics of simple structure, uniform mixing, low energy consumption and on-line mixing.
Drawings
FIG. 1 is a schematic diagram of the jet reactor according to the present invention;
FIG. 2 is one of the bottom views of FIG. 1 (spray hole type);
FIG. 3 is a second (annular) bottom view of FIG. 1;
FIG. 4 is a schematic diagram of a jet reactor according to a second embodiment of the present invention;
FIG. 5 is a schematic diagram of a third embodiment of the jet reactor according to the present invention;
FIG. 6 is a schematic diagram of the structural principle of the jet reactor of the present invention;
FIG. 7 is a schematic diagram of the structural principle of the jet reactor of the present invention;
FIG. 8 shows Fe produced by the jet reactor of the present invention 3 O 4 A nanoparticle morphology;
FIG. 9 shows Fe produced by the jet reactor of the present invention 3 O 4 A nanoparticle hysteresis loop;
in the figure: 1-body, 101-shell, 102-core, 2-feed inlet I, 3-feed inlet II, 4-jet orifice I, 5-buffer tank I, 6-jet orifice II, 7-buffer tank II, 8-center shaft, 801-mixed flow plate, 802-mixed flow cover and 9-mixing tube.
Detailed Description
The invention is further illustrated in the following figures and examples, which are not intended to be limiting in any way, and any alterations or modifications based on the teachings of the invention are within the scope of the invention.
As shown in fig. 1 to 4, the jet reactor for synthesizing powder materials comprises a body 1, a feed inlet i 2, a feed inlet ii 3, a jet hole i 4, a buffer tank i 5 and a jet hole ii 6, wherein the jet hole i 4 is arranged in the middle or at one side of the body 1, and the upper or side wall of the body 1 is provided with the feed inlet i 2 and is communicated with the jet hole i 4; the body 1 is provided with a closed buffer groove I5 at the periphery of an injection hole I4 in the middle or at the other side of the injection hole I4 at one side, the bottom of the buffer groove I5 is provided with an injection hole II 6, the outlet of which is obliquely directed to the extending direction of the injection hole I4, and the upper part or the side wall of the body 1 is provided with a feed inlet II 3 and communicated with the buffer groove I5; or set up inclosed buffer tank II 7 in the body 1, peripheral or one side of buffer tank II 7 set up inclosed buffer tank I5 in the body 1, buffer tank I5's tank bottom portion is equipped with the jet orifice II 6 that the export slope was directional jet orifice I4 extending direction, body 1's upper portion or lateral wall set up feed inlet I2 and with buffer tank II 7 intercommunication, jet orifice I4 and buffer tank II 7 bottom or lateral wall intercommunication, body 1's upper portion or lateral wall set up feed inlet II 3 and with buffer tank I5 intercommunication.
The bottom of the buffer tank I5 is at least provided with two injection holes II 6 which are uniformly distributed around the injection hole I4 in the middle of the body 1, or the injection holes II 6 are annular gaps around the outlet end of the injection hole I4 in the middle of the body 1; or the tank bottom of the buffer tank I5 is at least provided with two injection holes II 6 or at least one injection hole II 6 in a gap shape, the tank bottom of the buffer tank II 7 is at least provided with two injection holes I4 or at least one injection hole I4 in a gap shape, and the injection holes I4 and the injection holes II 6 are respectively provided with two sides and the extending direction of the outlet is obliquely intersected.
The injection hole II 6 and the injection direction extension line of the injection hole I4 form an included angle alpha, and the included angle alpha is more than 5 degrees and less than 80 degrees.
The body 1 includes casing 101, core 102 is provided with the jet orifice I4 that runs through, core 102 sets up in casing 101 and with casing 101 one end fixed airtight connection, jet orifice I4 is at casing 101's fixed airtight link intercommunication feed inlet I2, form buffer tank I5 between the outer wall of core 102 and casing 101's inner wall, casing 101's bottom or lateral wall set up feed inlet II 3 and with buffer tank I intercommunication, core 102's the other end and casing 101 fixed airtight connection and be provided with at least two jet orifices II 6 with buffer tank I5 intercommunication, perhaps the other end of core 102 forms around jet orifice I4's exit end a week and with buffer tank I5 intercommunication's annular space jet orifice II 6 with casing 101.
The cross section of the outlet end of the injection hole I4 and/or the injection hole II 6 is circular, elliptical, rectangular, triangular or polygonal, the injection direction extension lines between the injection holes II 6 on the body 1 intersect at one point, or the injection direction extension lines of the injection holes II 6 on the body 1 and the extension lines of the injection holes I4 form a rotational flow structure, or the injection direction extension lines between at least two injection holes II 6 on the body 1 intersect at one point and the injection direction extension lines of the other injection holes II 6 and the extension lines of the injection holes I4 form a rotational flow structure.
The middle part of the jet hole I4 in the middle part of the body 1 is provided with a central shaft 8, and an annular gap is formed between the outlet end of the jet hole I4 and the central shaft 8.
As shown in fig. 6 and 7, the central shaft 8 extends outwards from the outlet end of the injection hole i 4 and is provided with a flow mixing plate 801 or a flow mixing cover 802 perpendicular to the extension line of the injection direction of the injection hole ii 6, and the upper surface of the flow mixing plate 801 or the flow mixing cover 802 is disposed at or below the intersection point of the extension line of the injection direction of the injection hole ii 6 and the extension line of the injection hole i 4.
The cross-sectional shape of the mixing plate 801 or the mixing cover 802 is the same as or similar to the shape of the outlet end of the injection hole i 4, and the mixing cover 802 has a "C" shape structure with an opening facing the outlet end of the injection hole i 4.
As shown in fig. 5, the body 1 is provided with a mixing tube 9 in the extending direction of the outlet end of the injection hole i 4, the mixing tube 9 includes a necking section, a vertical section, and a neck expansion section, wherein the upper edge of the necking section is peripherally connected with the injection hole ii 6 of the body 1 and the lower edge of the necking section is connected with the upper edge of the vertical section, the upper edge of the neck expansion section is connected with the lower edge of the vertical section, the vertical section is tubular or is consistent with the outlet end structure of the injection hole i 4, the necking section is a reverse frustum-shaped hollow structure, and the neck expansion section is a frustum-shaped hollow structure.
The inner wall surface of the mixing tube 9 is coated with a polytetrafluoroethylene coating.
According to the calcium hydrophosphate synthesis method based on the jet reactor for powder material synthesis, lime milk is jetted out through the jet hole I of the jet reactor to form lime milk flow, phosphoric acid is obliquely jetted to the lime milk flow through at least two symmetrical jet holes II arranged on the periphery of the lime milk flow, and the lime milk flow reacts with phosphoric acid in the jet collision and co-flow processes to generate calcium hydrophosphate.
The injection holes II are uniformly distributed on the periphery of the injection hole I at the center, or the injection holes II are annular gaps around the injection hole I in a circle; the injection direction extension line of the injection hole II and the extension line of the injection hole I form an included angle alpha, and the included angle alpha is more than 5 degrees and less than 80 degrees.
According to the nano or micron powder synthesis method based on the jet reactor for powder material synthesis, alkali liquor or reducing agent solution is jetted out through the jet hole I of the jet reactor to form jet flow, metal salt solution is obliquely jetted to the jet flow from the jet hole II, and nano or micron metal hydroxide powder or metal powder is generated in the collision and flow-down processes of the metal salt solution and the alkali liquor or the reducing agent solution.
The alkali liquor comprises one or any mixture of sodium hydroxide, sodium carbonate, urea and ammonia water; the metal salt solution comprises one or at least two of nitrate, sulfate, phosphate and chloride of copper, cobalt, nickel, manganese, iron and silver metals; the reducing agent comprises formaldehyde and sodium borohydride.
The working principle and the working process of the invention are as follows:
according to the invention, the jet hole I is arranged in the middle part or on one side of the body, then the outlet extending direction of the body is inclined with the outlet extending direction of the jet hole I compared with the jet hole II on the outer side of the body, and the jet hole II generates necking action through the buffer groove I to enhance the turbulence degree of the jet material, so that the mixing effect between the jet hole I and the jet material of the jet hole I is enhanced, a traditional solid mixing chamber is omitted, the jet hole II and the jet material jetted by the jet hole I form suspension jet collision, millisecond mixing between the materials is realized, the difficult mixing problem that part of the materials still need to be mixed after a large amount of foam and/or high-viscosity reaction products are generated in the prior art is avoided, and the batch stability of the reaction products is good; and the suspension jet collision can also solve the problems of channel blockage and inconvenient cleaning when powder materials are synthesized in the microreactor, thereby realizing online mixing reaction. Further, the body is at least provided with two injection holes II which are uniformly distributed around the periphery of the outlet end of the middle injection hole I, or the injection holes II are annular gaps around the periphery of the outlet end of the middle injection hole I; through arranging a plurality of jet flows or annular jet flows, fluid sprayed by the jet holes II can surround the main flow of the jet hole I in the middle to form cross-flow mixing, so that the rapid and uniform mixing between the two fluid flows is realized; optionally, at least two injection holes II or at least one injection hole II in a gap shape are arranged at the bottom of the buffer groove I, at least two injection holes I or at least one injection hole I in a gap shape are arranged at the bottom of the buffer groove II corresponding to the other side, and the injection holes I are intersected with the extending direction of the outlet of the injection hole II; the low-viscosity nano powder and micro powder can form micro-jet through the jet hole, so that the purposes of rapid mixing and rapid reaction can be achieved when the suspended jet collides, and the uniformity of reaction products can be improved. Furthermore, the injection direction extension line of the injection hole II and the extension line of the injection hole I form an included angle which is more than 5 degrees and less than 80 degrees, and the jet length of the jet flow entering the injection hole I of the injection hole II can be further increased through the arrangement of the small included angle of the injection hole II and the injection hole I, so that the uniformity after mixing is improved. Further, the body adopts a split combined structure of the shell and the core body, so that the complexity of the body can be simplified, and the cost is reduced and the later use and maintenance are facilitated. Furthermore, the extending lines of the injection directions between the injection holes II on the body are intersected at one point and/or form a rotational flow structure, so that different injection holes can be adopted to better adapt to requirements according to different characteristics of materials and reaction products of the mixed reaction, and the yield and the uniformity of the mixture are improved. Furthermore, an annular gap is formed between the outlet end of the injection hole I and the central shaft, so that the turbulence degree of the fluid at the outlet end of the injection hole I can be increased, and the annular gap at the outlet end of the injection hole I can effectively compress the thickness of the fluid in the annular gap, thereby being convenient for realizing efficient mixing and reaction between materials through reduced space scale and strong suspension impact. Still further, the mixing plate or the mixing cover which is arranged at the vertical position of the main fluid at or below the jet mixing point of the central shaft can further improve the uniformity of mixing by colliding the fluid during or after mixing. Furthermore, the body is provided with a mixing pipe comprising a necking section, a vertical section and a neck expansion section in the extending direction of the outlet end of the jet hole I, so that fluid mixed by jet flows can be uniformly dispersed, suspended and integrated turbulent flow is formed in the vertical section, and the reaction is more sufficient; the flow rate of the generated product is gradually reduced by the neck expansion section, and the product is sent out by using the increased static pressure. Still further, the inner wall surface of the mixing tube is coated with a polytetrafluoroethylene coating, and the resistance to low friction, abrasion and humidity is utilized, so that the resistance of the high-viscosity reactant in the flowing direction can be effectively reduced under the condition of unchanged vertical pressure, and the turbulence degree of the mixed fluid can be effectively increased under the condition of unchanged driving force, thereby increasing the uniformity of the reaction product, and solving the problem of low uniformity of mixing of the high-viscosity reactant in the prior art. In conclusion, the invention has the characteristics of simple structure, uniform mixing, low energy consumption and on-line mixing.
As shown in fig. 1 and 2, the calcium hydrogen phosphate is taken as an example: after defluorination and purification treatment, phosphoric acid is input into a buffer tank I5 from a feed inlet II 3 under pressure, lime milk is pressed into an injection hole I4 from a feed inlet I2 under pressure, lime milk is sprayed out from the outlet end of the injection hole I4 under the action of pressure and gravity, phosphoric acid is sprayed into the lime milk from an injection hole II 6 under pressure, the sprayed phosphoric acid and the lime milk collide in air and are mixed and react in a synthetic way, a foam-shaped product is formed and falls into a container at the bottom to obtain a calcium hydrophosphate mixed solution, and the calcium hydrophosphate product for feed is obtained after precipitation, slurry solid-liquid separation and drying, as shown in table 1.
TABLE 1 product quality of calcium hydrogen phosphate for feed
。
To prepare Fe using the jet reactor shown in FIG. 3 3 O 4 Nanoparticles are examples: firstly, preparing dilute ferric sulfate and ferrous sulfate solution according to the proportion of 2:1, and uniformly stirring and mixing to obtain solution A; then taking dilute ammonia water solution as solution B; the two solutions are respectively connected to a feed inlet II 3 and a feed inlet I2 of the injection reactor through two hoses, and then are respectively injected to a middle junction through an injection hole I4 and an injection hole II 6Carrying out neutralization reaction, carrying out air collision mixing on the sprayed solution A and the solution B, carrying out synthesis reaction, dropping into a container at the bottom, carrying out solid-liquid separation, and then washing with distilled water for 2-3 times; drying and grinding the obtained solid product to obtain Fe with good magnetism 3 O 4 Nanoparticles (fig. 8). The detection shows that the magnetic core material has excellent magnetic performance, large magnetic permeability, small coercive force and very narrow hysteresis loop, and can be used for magnetic core materials of high-frequency coils. Fe prepared 3 O 4 The hysteresis loop of the nanoparticle is shown in fig. 9.
Claims (7)
1. The jet reactor for synthesizing the powder material is characterized by comprising a body (1), a feed inlet I (2), a feed inlet II (3), a jet hole I (4), a buffer groove I (5) and a jet hole II (6); the injection hole I (4) is arranged in the middle of the body (1), the upper part or the side wall of the body (1) is provided with a feed inlet I (2) and is communicated with the injection hole I (4), the middle of the injection hole I (4) is provided with a central shaft (8), and an annular gap is formed between the outlet end of the injection hole I (4) and the central shaft (8); the periphery of the injection hole I (4) is provided with a closed buffer groove I (5), the bottom of the buffer groove I (5) is provided with an injection hole II (6) with an outlet obliquely pointing to the extending direction of the injection hole I (4), and the upper part or the side wall of the body (1) is provided with a feed inlet II (3) and communicated with the buffer groove I (5); the central shaft (8) is provided with a mixed flow plate (801) or a mixed flow cover (802) which is perpendicular to the main flow below the intersection point or the intersection point of the extension line of the injection direction of the injection hole II (6) and the extension line of the injection hole I (4), and the cross section shape of the mixed flow plate (801) or the mixed flow cover (802) is the same as or similar to the shape of the outlet end of the injection hole I (4); the injection hole II (6) and the injection direction extension line of the injection hole I (4) form an included angle alpha, and the included angle alpha is more than 5 degrees and less than 80 degrees.
2. The jet reactor for powder material synthesis according to claim 1, wherein at least two jet holes ii (6) are arranged at the bottom of the buffer tank i (5) and uniformly distributed around the jet hole i (4), or the jet hole ii (6) is an annular space surrounding the outlet end of the jet hole i (4).
3. The jet reactor for powder material synthesis according to claim 1, wherein the body (1) comprises a shell (101) and a core (102), the core (102) is provided with a penetrating jet hole I (4), and the core (102) is arranged in the shell (101) and fixedly and hermetically connected with one end of the shell (101); the injection hole I (4) is communicated with the feed inlet I (2) at a fixed airtight connection end of the shell (101), a buffer groove I (5) is formed between the outer wall of the core body (102) and the inner wall of the shell (101), and the bottom or the side wall of the shell (101) is provided with the feed inlet II (3) and is communicated with the buffer groove I (5); the other end of the core body (102) is fixedly and hermetically connected with the shell (101) and is provided with at least two injection holes II (6) communicated with the buffer groove I (5), or the other end of the core body (102) and the shell (101) form an annular gap injection hole II (6) which surrounds the outlet end of the injection hole I (4) and is communicated with the buffer groove I (5).
4. A jet reactor for powder material synthesis according to claim 1, 2 or 3, characterized in that the cross section of the outlet end of the jet orifice i (4) and/or the jet orifice ii (6) is circular, oval, rectangular, triangular or polygonal, the jet direction extension between the jet orifices ii (6) on the body (1) intersects at a point, or the jet direction extension of the jet orifice ii (6) on the body (1) and the extension of the jet orifice i (4) form a swirl structure, or the jet direction extension between at least two jet orifices ii (6) on the body (1) intersects at a point and the jet direction extensions of the remaining jet orifices ii (6) and the extension of the jet orifice i (4) form a swirl structure.
5. The jet reactor for powder material synthesis according to claim 1, wherein the body (1) is provided with a mixing pipe (9) in the extending direction of the outlet end of the jet hole i (4), the mixing pipe (9) comprises a necking section, a vertical section and a neck expansion section, the upper edge of the necking section is peripherally connected with the jet hole ii (6) of the body (1) and the lower edge of the necking section is connected with the upper edge of the vertical section, the upper edge of the neck expansion section is connected with the lower edge of the vertical section, the vertical section is tubular or is consistent with the outlet end structure of the jet hole i (4), the necking section is of an inverted cone-shaped hollow structure, and the neck expansion section is of a cone-shaped hollow structure; the inner wall surface of the mixing tube (9) is coated with a polytetrafluoroethylene coating.
6. A method for synthesizing calcium hydrophosphate based on the injection reactor for synthesizing powder materials according to claim 1, which is characterized in that lime milk is sprayed out through an injection hole I (4) of the injection reactor to form lime milk flow, phosphoric acid is obliquely sprayed to the lime milk flow through at least two symmetrical injection holes II (6) arranged on the periphery of the lime milk flow, and the lime milk flow and phosphoric acid react to generate calcium hydrophosphate in the process of jet collision and co-flow.
7. A nano or micron powder synthesis method based on the jet reactor for powder material synthesis according to claim 1, and is characterized in that alkali liquor or reducing agent solution is jetted out through a jet hole I (4) of the jet reactor to form jet flow, metal salt solution is obliquely jetted to the jet flow from a jet hole II (6), and nano or micron metal hydroxide powder or metal powder is generated in the collision and flowing down process of the metal salt solution and the alkali liquor or the reducing agent solution.
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