CN110075779A - A kind of injection reactor and calcium monohydrogen phosphate, nanometer or micro-powder synthetic method for powder body material synthesis - Google Patents
A kind of injection reactor and calcium monohydrogen phosphate, nanometer or micro-powder synthetic method for powder body material synthesis Download PDFInfo
- Publication number
- CN110075779A CN110075779A CN201910466144.9A CN201910466144A CN110075779A CN 110075779 A CN110075779 A CN 110075779A CN 201910466144 A CN201910466144 A CN 201910466144A CN 110075779 A CN110075779 A CN 110075779A
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- China
- Prior art keywords
- spray
- hole
- dashpot
- ontology
- injection
- 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.)
- Granted
Links
- 238000002347 injection Methods 0.000 title claims abstract description 55
- 239000007924 injection Substances 0.000 title claims abstract description 55
- 239000000463 material Substances 0.000 title claims abstract description 41
- 239000000843 powder Substances 0.000 title claims abstract description 38
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 title claims abstract description 16
- 235000019700 dicalcium phosphate Nutrition 0.000 title claims abstract description 16
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 15
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 15
- 238000010189 synthetic method Methods 0.000 title claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 40
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical class OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Substances [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 16
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 13
- 239000007921 spray Substances 0.000 claims abstract description 13
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 9
- 235000011116 calcium hydroxide Nutrition 0.000 claims abstract description 9
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 8
- 229910052751 metal Chemical class 0.000 claims abstract description 8
- 239000002184 metal Chemical class 0.000 claims abstract description 8
- 239000012266 salt solution Substances 0.000 claims abstract description 7
- 229910000000 metal hydroxide Inorganic materials 0.000 claims abstract description 3
- 150000004692 metal hydroxides Chemical class 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 14
- 239000008267 milk Substances 0.000 claims description 12
- 210000004080 milk Anatomy 0.000 claims description 12
- 235000013336 milk Nutrition 0.000 claims description 12
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 10
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 10
- 239000004571 lime Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 210000003238 esophagus Anatomy 0.000 claims description 7
- 239000000376 reactant Substances 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 16
- 239000011162 core material Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 239000007795 chemical reaction product Substances 0.000 description 8
- 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
- 238000010586 diagram Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 230000003139 buffering effect Effects 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 208000033962 Fontaine progeroid syndrome Diseases 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 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
- 206010054949 Metaplasia Diseases 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
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 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
- 239000002253 acid Substances 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000001413 cellular effect Effects 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
- 239000012611 container material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007423 decrease Effects 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
- 238000001035 drying Methods 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
- 239000012467 final product Substances 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
- 150000002431 hydrogen Chemical class 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
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- MVZXTUSAYBWAAM-UHFFFAOYSA-N iron;sulfuric acid Chemical compound [Fe].OS(O)(=O)=O MVZXTUSAYBWAAM-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 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
- 230000015689 metaplastic ossification Effects 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 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
- 239000002245 particle Substances 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
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035939 shock Effects 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
- 230000003068 static effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000004073 vulcanization 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
Abstract
The present invention discloses a kind of injection reactor and calcium monohydrogen phosphate, nanometer or micro-powder synthetic method for powder body material synthesis.The reactor spray-hole I is set to ontology and is connected to feed inlet I；I periphery of spray-hole or side set dashpot I and are connected to the feed inlet II on ontology, and dashpot I sets the spray-hole II for being directed toward spray-hole I；Or ontology sets dashpot II and dashpot I, dashpot I sets the spray-hole II for being directed toward spray-hole I, and ontology sets up feed inlet I separately, feed inlet II is connected to dashpot II, dashpot I, and spray-hole I is connected to dashpot II.Milk of lime or lye/reducing agent are collided by the phosphoric acid or metal salt solution jet stream of the lower spray of spray-hole I and spray-hole II in the synthetic method generates calcium monohydrogen phosphate, nanometer or micron metal hydroxide or metal-powder.Reactant of the present invention forms hanging collision through spray-hole II and I, solves the problems, such as in traditional reactive tank that product incomplete mixing, lot stability be poor and microreactor in synthetic powder when channel blockage.
Description
Technical field
The invention belongs to chemical equipment technical fields, and in particular to a kind of structure is simple, uniformly mixed, low energy consumption, can be
The injection reactor and calcium monohydrogen phosphate, nanometer or micro-powder synthetic method for powder body material synthesis of line mixing.
Background technique
In the industry such as petroleum, chemical industry, rubber, pesticide, dyestuff, medicine, food, vulcanization, hydrogenation, hydrocarbonylation, gathers at nitrification
Close, the technical process such as condensation are premised on participating in being sufficiently mixed of reaction mass, not only mixing uniformity can greatly influence
Final product distribution, the yield of target product and quality, and the indexs such as design and energy consumption for influencing all round process simultaneously.
Therefore, how to guarantee the efficient of mixed process, low consumption and mixture there is high uniformity to be the important mesh of mixing
Mark.Currently, the mixing between two-phase or multiphase usually has following two mode:
1, interval mixes: pre-mixed material being placed in same container, is mixed by agitating paddle therein.This mode
Structure is simple, but can not achieve on-line mixing, causes production efficiency low, and the shape for generating high-viscosity material after hybrid reaction
It is difficult to be uniformly mixed under condition, the material that generates is locally uneven after will cause reaction, and product batches stability is poor.
2, it on-line mixing: is continuously mixed between pre-mixed material.Although production efficiency is higher, mixed process still needs
By stir it is lower or in container mutual knock-on reaction is completed, not only stir for generation high-viscosity material after hybrid reaction
Be difficult to be uniformly mixed under situation, and if mutual knock-on reaction generates in container material viscosity it is higher, also result in generation
Material and chamber wall between relative motion when can generate larger and complicated frictional resistance, be unfavorable for high-viscosity material in the cavity
Flowing and separation, are also easy to blocked receptacle cavity and cleaning is inconvenient.
Injection reactor is that volume is mutually gone to inhale other phases using flow at high speed, so that mutually hitting between two-phase or multiphase to fill
Point mixed material, not only low energy consumption, Yi Shixian on-line mixing compared to being stirred, but also heat transfer efficiency and mass-transfer efficiency are high, instead
Answer rate fast, moreover it is possible to be reduced significantly the volume of reactor and shorten the reaction time, be a kind of efficient heterophase reactor.But tradition
Injection reactor in order to be uniformly mixed be provided with mixing chamber, although can adapt to the hybrid reaction of common product, for
The direct synthetic reaction of such as nanometer, micro-powder and calcium monohydrogen phosphate generating process, due to phosphoric acid in calcium monohydrogen phosphate synthetic reaction
Reaction product viscosity after reacting with milk of lime is very big, forms foam, and highly viscous reaction product will cause in mixing chamber
It is difficult to flow and separate, not only two-phase is difficult to be uniformly mixed, and causes the certain part acid of product high, some local Cas are high, cause to produce
Product lot stability is poor, and is also easy to blocked receptacle cavity and cleaning inconvenience.Therefore, anti-for the directly synthesis of calcium monohydrogen phosphate
It should be typically all to be produced using agitated trough, but its occupation area of equipment is big, and the Maintenance and Repair of equipment are costly, stir
It is high to mix device intensity requirement, energy consumption is high, it is difficult to realize that on-line continuous metaplasia produces, production efficiency is lower.
Summary of the invention
The first object of the present invention be to provide a kind of structure is simple, uniformly mixed, low energy consumption, can on-line mixing be used for
Powder body material synthesis injection reactor, second be designed to provide it is a kind of based on the injection reactor synthesized for powder body material
Calcium monohydrogen phosphate synthetic method, third is designed to provide a kind of nanometer based on the injection reactor synthesized for powder body material
Or micro-powder synthetic method synthetic method.
The first object of the present invention is achieved in that including ontology, feed inlet I, feed inlet II, spray-hole I, dashpot
I, spray-hole II, the spray-hole I is set in the middle part of ontology or side, the body upper part or side wall setting feed inlet I and with
Spray-hole I is connected to；Closed buffering is arranged in I periphery of spray-hole of the ontology at middle part or I other side of spray-hole in side
Slot I, the trench bottom of the dashpot I are equipped with the spray-hole II that outlet-inclined impeller vane is directed toward I extending direction of spray-hole, the ontology it is upper
Portion or side wall are arranged feed inlet II and are connected to dashpot I；Or the closed dashpot II of setting, the ontology in the ontology
Closed dashpot I is arranged in the periphery or side of inherent dashpot II, and the trench bottom of the dashpot I is directed toward equipped with outlet-inclined impeller vane
The spray-hole II of I extending direction of spray-hole, the top of the ontology or side wall setting feed inlet I are simultaneously connected to, institute with dashpot II
Spray-hole I is stated to be connected to II bottom of dashpot or side wall, the top of the ontology or side wall setting feed inlet II and with dashpot I
Connection.
The second object of the present invention is achieved in that milk of lime forms stone by the ejection of spray-hole I of injection reactor
Grey milk flow, phosphoric acid tilt directive lime milk flow, stone by be set to lime milk flow periphery at least two symmetrical spray-holes II
Grey milk flow reacts under jet stream collision, common stream in the process with phosphoric acid generates calcium monohydrogen phosphate.
The third object of the present invention is achieved in that lye or reducing agent solution pass through the spray-hole I of injection reactor
Ejection forms jet stream, and metal salt solution tilts directive jet stream by spray-hole II, and metal salt solution exists with lye or reducing agent solution
Jet stream collision, the metal hydroxides powder or metal-powder that nanometer or micron are generated during flowing down.
Beneficial effects of the present invention: spray-hole I by being set to the middle part or side of ontology by the present invention, then in ontology
The outlet extending direction inclination of outlet extending direction and spray-hole I is set compared to the spray-hole II of outer body, passes through buffering
Slot I makes spray-hole II generate necking down effect to enhance the less turbulence of spraying of material, thus strengthen with I spraying of material of spray-hole it
Between mixed effect, and traditional entity mixing chamber is omitted, so that the material shape that spray-hole II and spray-hole I eject
It is collided at hanging jet stream, not only realizes the Millisecond mixing between material, to avoid partially a large amount of in generation in the prior art
Still need after foam and/or high viscosity reaction product and be difficult to mix problem present in mixing, the batch of reaction product is steady
It is qualitative good；And hanging jet stream collides the difficulty of channel blockage and cleaning inconvenience when also can solve synthetic powder material in microreactor
Topic, so as to realize that on-line mixing is reacted.Therefore, the present invention is with structure is simple, uniformly mixed, low energy consumption, can mix online
The characteristics of conjunction.
Detailed description of the invention
Fig. 1 is one of the principle schematic diagram of injection reactor of the present invention；
Fig. 2 is one of bottom view of Fig. 1 (injection cellular type)；
Fig. 3 is two (circular-gaps) of the bottom view of Fig. 1；
Fig. 4 is the two of the principle schematic diagram of the injection reactor of the present invention；
Fig. 5 is the three of the principle schematic diagram of the injection reactor of the present invention；
Fig. 6 is the four of the principle schematic diagram of the injection reactor of the present invention；
Fig. 7 is the five of the principle schematic diagram of the injection reactor of the present invention；
Fig. 8 is Fe prepared by the injection-type reactor of the present invention3O4Nanoparticle pattern；
Fig. 9 is Fe prepared by the injection-type reactor of the present invention3O4Nanoparticle hysteresis loop；
In figure: 1- ontology, 101- shell, 102- core, 2- feed inlet I, 3- feed inlet II, 4- spray-hole I, 5- dashpot I, 6-
Spray-hole II, 7- dashpot II, 8- central axis, 801- bridge insert, 802- mixed flow cover, 9- mixing tube.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawings and examples, but is not subject in any way to the present invention
Limitation, based on present invention teach that made any changes and modifications, all belong to the scope of protection of the present invention.
As shown in Figures 1 to 4, the injection reactor for powder body material synthesis of the present invention includes including ontology 1, charging
Mouth I 2, feed inlet II 3, spray-hole I 4, dashpot I 5, spray-hole II 6, the spray-hole I 4 are set to 1 middle part of ontology or side,
1 top of ontology or side wall are arranged feed inlet I 4 and are connected to spray-hole I 4；Spray-hole I 4 periphery of the ontology 1 at middle part
Or closed dashpot I 5 is set in I 4 other side of spray-hole of side, the trench bottom of the dashpot I 5 refers to equipped with outlet-inclined impeller vane
To the spray-hole II 6 of I 4 extending direction of spray-hole, the top of the ontology 1 or side wall setting feed inlet II 3 and with dashpot I 5
Connection；Or the closed dashpot II 7 of setting in the ontology 1, the ontology 1 is interior to be set on the periphery of dashpot II 7 or side
Closed dashpot I 5 is set, the trench bottom of the dashpot I 5 is equipped with the spray-hole that outlet-inclined impeller vane is directed toward I 4 extending direction of spray-hole
II 6, the top of the ontology 1 or side wall are arranged feed inlet I 2 and are connected to dashpot II 7, the spray-hole I 4 and dashpot II
7 bottoms or side wall connection, the top of the ontology 1 or side wall are arranged feed inlet II 3 and are connected to dashpot I 5.
The trench bottom of the dashpot I 5 is at least provided with two spray-holes II 6 and is uniformly distributed in the spray at the middle part of ontology 1
I 4 periphery of perforation or spray-hole II 6 are the I 4 one week annular space in outlet end of spray-hole around 1 middle part of ontology；Or the buffering
The trench bottom of slot I 5 is at least provided with two spray-holes II 6 or at least one one-tenth gap-shaped spray-hole II 6, the dashpot II
7 trench bottom is at least provided with two spray-holes I 4 or at least one one-tenth gap-shaped spray-hole I 4, the spray-hole I 4 and spray
Perforation II 6 sets up two sides and outlet extending direction inclination intersection separately.
The injection direction extended line of the spray-hole II 6 and spray-hole I 4 forms angle α, and the angle of the angle α is big
In 5 ° and less than 80 °.
The ontology 1 includes shell 101, core 102, and the core 102 is provided with perforative spray-hole I 4, the core
102 are set in shell 101 and fix airtight connection with 101 one end of shell, and the spray-hole I 4 is closed in the fixation of shell 101
Connecting pin is connected to feed inlet I 2, and dashpot I 5, the shell 101 are formed between the outer wall of the core 102 and the inner wall of shell 101
Bottom or side wall setting feed inlet II 3 and be connected to dashpot I, the other end and shell 101 of the core 102 are fixed closed
Connect and be provided with the other end and shell of spray-hole II 6 or the core 102 that at least two are connected to dashpot I 5
101 form the annular space spray-hole II 6 being connected to around one Zhou Bingyu dashpot I 5 of the outlet end of spray-hole I 4.
The section of the outlet end of the spray-hole I 4 and/or spray-hole II 6 is circle, ellipse, rectangle, triangle or more
It is angular, the injection direction extended line between spray-hole II 6 on the ontology 1 intersect at a point or the ontology 1 on spray
The injection direction extended line of perforation II 6 and the extended line of spray-hole I 4 form at least two sprays on cyclone structure or ontology 1
Injection direction extended line between perforation II 6 intersects at a point and the injection direction extended line of remaining spray-hole II 6 and spray-hole I
4 extended line forms cyclone structure.
The middle part of the spray-hole I 4 at 1 middle part of ontology is provided with central axis 8, the outlet end and center of the spray-hole I 4
Annular space is formed between axis 8.
As shown in Figure 6 and Figure 7, the outlet end of the 8 self-spray perforation I 4 of central axis extends outwardly and is provided with and spray-hole
II 6 injection direction extended line vertical bridge insert 801 or mixed flow cover 802, the upper table of the bridge insert 801 or mixed flow cover 802
Face is set to below the injection direction extended line of spray-hole II 6 and the extending line intersection point of spray-hole I 4 or intersection point.
The transverse cross-sectional shape of the bridge insert 801 or mixed flow cover 802 and the outlet end shape of spray-hole I 4 are identical or approximate,
The mixed flow cover 802 is " C " shape structure of outlet end of the opening towards spray-hole I 4.
As shown in figure 5, the ontology 1 is provided with mixing tube 9, the mixing tube in the outlet end extending direction of spray-hole I 4
9 include necking segment, vertical section, expand cervical part of esophagus, II 6 periphery of spray-hole of the upper edge of the necking segment and ontology 1 connect and lower edge and
Vertical section it is upper along connection, it is described expand cervical part of esophagus upper edge connect with the lower edge of vertical section, the vertical section for tubulose or with injection
The outlet end structure in hole I 4 is consistent, and the necking segment is reverse taper hollow structure, and the expansion cervical part of esophagus is pyramidal hollow structure.
The inner wall surface coating polytetrafluorethylecoatings coatings of the mixing tube 9.
The calcium monohydrogen phosphate synthetic method based on the injection reactor synthesized for powder body material of the present invention, milk of lime pass through
The ejection of spray-hole I of injection reactor forms lime milk flow, and phosphoric acid is symmetrical by be set to lime milk flow periphery at least two
Spray-hole II tilt directive lime milk flow, lime milk flow and phosphoric acid under jet stream collision, common stream during react generation phosphorus
Sour hydrogen calcium.
The spray-hole II is uniformly distributed in I periphery of spray-hole in center or the spray-hole II is around injection
The I 1 weeks annular spaces in hole；The injection direction extended line of the spray-hole II and the extended line of spray-hole I form angle α, the angle
The angle of α is greater than 5 ° and less than 80 °.
The nanometer or micro-powder synthetic method based on the injection reactor synthesized for powder body material of the present invention, lye
Or reducing agent solution forms jet stream by the ejection of spray-hole I of injection reactor, metal salt solution tilts directive by spray-hole II
Jet stream, metal salt solution and lye or reducing agent solution generate the metallic hydrogen of nanometer or micron during jet stream is collided, flowed down
Oxide powder or metal-powder.
The lye includes one of sodium hydroxide, sodium carbonate, urea, ammonium hydroxide or any mixing；The metal salt is molten
Liquid include one of copper, cobalt, nickel, manganese, iron, the nitrate of silver metal, sulfate, phosphate, chloride prepare solution or
At least two solution prepared；The reducing agent includes formaldehyde, sodium borohydride.
Working principle and the course of work of the present invention:
Then by the way that spray-hole I to be set to the middle part or side of ontology outlet extending direction and spray is arranged in ontology in the present invention
The outlet extending direction inclination of perforation I makes spray-hole II generate necking down compared to the spray-hole II of outer body by dashpot I
It acts on to enhance the less turbulence of spraying of material, to strengthen the mixed effect between I spraying of material of spray-hole, and saves
Traditional entity mixing chamber has been omited, so that the material that spray-hole II and spray-hole I eject forms hanging jet stream and collides, it is not only real
Millisecond mixing between existing material, to avoid partially generating a large amount of foams and/or high viscosity reaction life in the prior art
It is difficult to mix problem present in mixing at still needing after object, the lot stability of reaction product is good；And hanging jet stream touches
The problem of channel blockage and cleaning inconvenience when also can solve synthetic powder material in microreactor is hit, it is online mixed so as to realize
Close reaction.Further, ontology at least provided with two spray-holes II and be uniformly distributed in middle part spray-hole I outlet end periphery,
Or spray-hole II is around the one week annular space in the outlet end of middle part spray-hole I；By setting multiple jets or annular jet, so that
The main fluid that the fluid that spray-hole II sprays can surround the spray-hole I at middle part forms cross-flow mixing, to realize two fluids
Between Quick uniform mixing；Optionally, I trench bottom of dashpot is at least provided with two spray-holes II or at least one one-tenth gap
The spray-hole II of shape, II trench bottom of dashpot of the corresponding other side is at least provided with two spray-holes I or at least one one-tenth gap
The spray-hole I of shape, spray-hole I intersect with the outlet extending direction of spray-hole II；It can make nano-powder, the micro-powder of low viscosity
Microjet is formed through spray-hole, so as to make hanging jet stream achieve the purpose that quickly mixing and fast reaction when colliding, is conducive to
Improve the uniformity of reaction product.Further, the injection direction extended line of spray-hole II and the extended line of spray-hole I are formed
Angle is to be arranged by the small angle of spray-hole II and spray-hole I greater than 5 ° and less than 80 °, can further increase spray-hole
II jet stream enters the jet length of I fluid of spray-hole, to improve mixed uniformity.Further, ontology using shell with
The Split assembled structure of core, can simplify the complexity of ontology, to be conducive to reduce cost and the working service convenient for the later period.
Further, the injection direction extended line between the spray-hole II on ontology intersects at a point and/or is formed cyclone structure, is all
For the ease of that different spray-holes can be taken better according to the material of hybrid reaction and the different characteristics of reaction product
It meets the needs of, consequently facilitating improving yield and mixed uniformity.Further, the outlet end of spray-hole I and center between centers shape
At annular space, the outlet end Hydrodynamic turbulence degree of spray-hole I can be increased, and the outlet end annular space of spray-hole I can be pressed effectively
The thickness of contracting wherein fluid, consequently facilitating the height by reduceds space scale and strong hanging shock, between realization material
Effect mixing, reaction.Further, the vertical bridge insert of main fluid is set to below the jet mixing point or mixing point of central axis
Or mixed flow cover, can by mixing when or mixing after fluid collision, further increase the uniformity of mixing.Further, originally
Body includes necking segment, vertical section, the mixing tube for expanding cervical part of esophagus in the outlet end extending direction setting of spray-hole I, and jet stream can be made mixed
Fluid after conjunction is evenly dispersed in vertical section, suspends, forms whole turbulent flow, to keep reaction more abundant；The production of generation
Object gradually decreases its flow velocity by expansion cervical part of esophagus, is seen off product using increased static pressure.Further, the inner wall of mixing tube
External coating polytetrafluorethylecoatings coatings, using its low frictional properties, wearability and moisture resistance, under conditions of pressure at right angle is constant,
It can be effectively reduced the resistance of high viscosity reactant in the flowing direction, thus under conditions of driving force is constant, it can be with
Effectively increase the less turbulence of fluid-mixing, to increase the uniformity of reaction product, and solves high viscous in the prior art
Spend the problem at the mixing uniformity bottom of reactant.In conclusion the present invention has, structure is simple, uniformly mixed, low energy consumption, can be
The characteristics of line mixes.
As depicted in figs. 1 and 2, by taking calcium monohydrogen phosphate synthesizes as an example: phosphoric acid is after defluorinate purified treatment, by phosphoric acid from feed inlet
II 3 pressure input in dashpot I 5, while milk of lime is pressed into spray-hole I 4 from feed inlet I 2 with pressure, milk of lime in pressure and
The outlet end of self-spray perforation I 4 sprays under gravity, and inclination is injected into milk of lime to phosphoric acid in self-spray perforation II 6 under stress
In, the concurrent GCMS computer of collisional mixing reacts the phosphoric acid of injection in the sky with milk of lime, and the product for forming foam-like falls into bottom
Calcium monohydrogen phosphate mixed solution is obtained in container, is separated by solid-liquid separation through precipitating and slurry, obtains feed phosphoric acid hydrogen after then drying
Calcium product, such as table 1.
The product quality of 1 feed calcium monohydrogen phosphate of table
。
To prepare Fe using injection-type reactor shown in Fig. 33O4For nanoparticle: pressing the proportional arrangement of 2:1 first
Dilute sulfuric acid iron and ferrous sulfate solution are simultaneously uniformly mixed as solution A；Then using dilute ammonia solution as solution B；By two
Kind solution is connected respectively to the feed inlet II 3 and feed inlet I 2 of injection reactor by two hoses, then respectively through spray-hole I
4 and spray-hole II 6 be ejected into intermediate river conjunction and carry out neutralization reaction, collisional mixing is concurrent in the sky for solution A and the solution B of injection
GCMS computer reaction, falls into the container of bottom, through being separated by solid-liquid separation, wash with distilled water 2 ~ 3 times later；Obtained solid product is dried
Dry, grinding, can be obtained with Fe magnetic very well3O4Nanoparticle (Fig. 8).Detection discovery its with excellent magnetic performance,
Magnetic conductivity is big, coercivity is small, and hysteresis loop is very narrow, can be used for the core material of high frequency coil.The Fe being prepared3O4Nanometer
Particle hysteresis loop is as shown in Figure 9.
Claims (10)
1. a kind of injection reactor for powder body material synthesis, it is characterised in that including ontology (1), feed inlet I (2), charging
Mouth II (3), spray-hole I (4), dashpot I (5), spray-hole II (6), the spray-hole I (4) are set to ontology (1) middle part or one
Side, ontology (1) top or side wall are arranged feed inlet I (4) and are connected to spray-hole I (4)；The ontology (1) is at middle part
Closed dashpot I (5) is arranged in spray-hole I (4) other side of side in spray-hole I (4) periphery, the dashpot I (5)
Trench bottom is equipped with the spray-hole II (6) that outlet-inclined impeller vane is directed toward spray-hole I (4) extending direction, the top of the ontology (1) or side wall
Feed inlet II (3) are set and are connected to dashpot I (5)；Or the closed dashpot II (7) of setting in the ontology (1), it is described
Closed dashpot I (5), the trench bottom of the dashpot I (5) are set on the periphery of dashpot II (7) or side in ontology (1)
Be directed toward the spray-hole II (6) of spray-hole I (4) extending direction equipped with outlet-inclined impeller vane, the top of the ontology (1) or side wall be arranged into
Material mouth I (2) is simultaneously connected to dashpot II (7), and the spray-hole I (4) is connected to dashpot II (7) bottom or side wall, and described
The top of body (1) or side wall are arranged feed inlet II (3) and are connected to dashpot I (5).
2. the injection reactor for powder body material synthesis according to claim 1, it is characterised in that the dashpot I (5)
Trench bottom at least provided with two spray-holes II (6) and spray-hole I (4) periphery for being uniformly distributed in the middle part of ontology (1), or
Spray-hole II (6) is the one week annular space in spray-hole I (4) outlet end in the middle part of ontology (1)；Or the slot of the dashpot I (5)
Bottom is at least provided with two spray-holes II (6) or at least one one-tenth gap-shaped spray-hole II (6), the dashpot II (7)
Trench bottom at least provided with two spray-holes I (4) or at least one one-tenth gap-shaped spray-hole I (4), the spray-hole I (4)
Set up two sides separately with spray-hole II (6) and outlet extending direction inclination is intersected.
3. the injection reactor for powder body material synthesis according to claim 2, it is characterised in that the spray-hole II (6)
Angle α is formed with the injection direction extended line of spray-hole I (4), the angle of the angle α is greater than 5 ° and less than 80 °.
4. the injection reactor for powder body material synthesis according to claim 3, it is characterised in that the ontology (1) includes
Shell (101), core (102), the core (102) are provided with perforative spray-hole I (4), and the core (102) is set to shell
Airtight connection, fixation closed company of the spray-hole I (4) in shell (101) are fixed in body (101) and with shell (101) one end
End connection feed inlet I (2) is connect, forms dashpot I (5) between the outer wall of the core (102) and the inner wall of shell (101), it is described
The bottom of shell (101) or side wall are arranged feed inlet II (3) and are connected to dashpot I, the other end and shell of the core (102)
Body (101) fixes airtight connection and is provided with spray-hole II (6) or the core that at least two are connected to dashpot I (5)
(102) the other end forms the annular space being connected to around one Zhou Bingyu dashpot I (5) of the outlet end of spray-hole I (4) with shell (101)
Spray-hole II (6).
5. according to claim 1 to the injection reactor for being used for powder body material synthesis described in 4 any one, it is characterised in that described
The section of the outlet end of spray-hole I (4) and/or spray-hole II (6) is circle, ellipse, rectangle, triangle or polygonal, institute
State the injection direction extended line between the spray-hole II (6) on ontology (1) intersect at a point or the ontology (1) on spray
The injection direction extended line of perforation II (6) and the extended line of spray-hole I (4) are formed on cyclone structure or ontology (1) at least
Injection direction extended line between two spray-holes II (6) intersects at a point and the injection direction of remaining spray-hole II (6) extends
The extended line of line and spray-hole I (4) forms cyclone structure.
6. the injection reactor for powder body material synthesis according to claim 5, it is characterised in that in the middle part of the ontology (1)
Spray-hole I (4) in the middle part of be provided with central axis (8), form ring between the outlet end and central axis (8) of the spray-hole I (4)
Gap.
7. the injection reactor for powder body material synthesis according to claim 6, it is characterised in that the central axis (8) is certainly
The outlet end of spray-hole I (4) extends outwardly and is provided with the bridge insert vertical with the injection direction extended line of spray-hole II (6)
(801) or mixed flow cover (802), the upper surface of the bridge insert (801) or mixed flow cover (802) is set to the spray of spray-hole II (6)
It penetrates below the extending line intersection point or intersection point of direction extended line and spray-hole I (4).
8. the injection reactor for powder body material synthesis according to claim 6, it is characterised in that the ontology (1) is being sprayed
The outlet end extending direction of perforation I (4) is provided with mixing tube (9), and the mixing tube (9) includes necking segment, vertical section, expands neck
Section, the upper edge of the necking segment is connect with (6) II periphery of spray-hole of ontology (1) and the upper edge of lower edge and vertical section connects, institute
The upper edge for stating expansion cervical part of esophagus is connect with the lower edge of vertical section, and the vertical section is tubulose or the outlet end structure one with spray-hole I (4)
It causes, the necking segment is reverse taper hollow structure, and the expansion cervical part of esophagus is pyramidal hollow structure.
9. a kind of calcium monohydrogen phosphate synthetic method based on the injection reactor synthesized for powder body material, it is characterised in that milk of lime
Lime milk flow is formed by the ejection of spray-hole I of injection reactor, phosphoric acid is by being set at least two of lime milk flow periphery
Symmetrical spray-hole II tilts directive lime milk flow, and lime milk flow reacts life under jet stream collision, common stream with phosphoric acid in the process
At calcium monohydrogen phosphate.
10. a kind of nanometer or micro-powder synthetic method, feature based on the injection reactor synthesized for powder body material exists
Jet stream is formed by the ejection of spray-hole I of injection reactor in lye or reducing agent solution, metal salt solution is inclined by spray-hole II
It slants to jet stream, metal salt solution and lye or reducing agent solution generate nanometer or micron during jet stream is collided, flowed down
Metal hydroxides powder or metal-powder.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111774220A (en) * | 2020-08-07 | 2020-10-16 | 昆明云仁轮胎制造有限公司 | Anti-adhesion treatment device and treatment method for tire tube |
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| CN110075779B (en) | 2024-02-09 |
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