CN110407256A - The production technology of nanometer ferro oxide - Google Patents
The production technology of nanometer ferro oxide Download PDFInfo
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- CN110407256A CN110407256A CN201910725192.5A CN201910725192A CN110407256A CN 110407256 A CN110407256 A CN 110407256A CN 201910725192 A CN201910725192 A CN 201910725192A CN 110407256 A CN110407256 A CN 110407256A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- 238000005516 engineering process Methods 0.000 title claims abstract description 19
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 106
- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- 239000002245 particle Substances 0.000 claims abstract description 36
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 26
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 25
- 230000001376 precipitating effect Effects 0.000 claims abstract description 24
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 84
- 229910052742 iron Inorganic materials 0.000 claims description 52
- 239000000758 substrate Substances 0.000 claims description 31
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 24
- 239000002699 waste material Substances 0.000 claims description 24
- 239000000706 filtrate Substances 0.000 claims description 23
- -1 iron ion Chemical class 0.000 claims description 21
- 150000001875 compounds Chemical class 0.000 claims description 19
- 239000000047 product Substances 0.000 claims description 18
- 238000001238 wet grinding Methods 0.000 claims description 18
- 150000002500 ions Chemical class 0.000 claims description 17
- 238000007493 shaping process Methods 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 230000002452 interceptive effect Effects 0.000 claims description 10
- 230000002708 enhancing effect Effects 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 238000004090 dissolution Methods 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 230000003750 conditioning effect Effects 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 6
- 239000002893 slag Substances 0.000 claims description 5
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 3
- 238000009837 dry grinding Methods 0.000 claims description 3
- 229910001447 ferric ion Inorganic materials 0.000 claims description 3
- 229910001448 ferrous ion Inorganic materials 0.000 claims description 3
- 238000002955 isolation Methods 0.000 claims description 3
- 238000007726 management method Methods 0.000 claims description 3
- 238000004816 paper chromatography Methods 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 23
- 238000001556 precipitation Methods 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 12
- 239000010842 industrial wastewater Substances 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 8
- 238000005474 detonation Methods 0.000 abstract description 6
- 239000010865 sewage Substances 0.000 abstract description 5
- 230000009471 action Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 239000002440 industrial waste Substances 0.000 abstract description 3
- 238000002347 injection Methods 0.000 abstract description 3
- 239000007924 injection Substances 0.000 abstract description 3
- 239000011541 reaction mixture Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 13
- 238000005299 abrasion Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000004065 wastewater treatment Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 238000009966 trimming Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- 230000005526 G1 to G0 transition Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- IYRDVAUFQZOLSB-UHFFFAOYSA-N copper iron Chemical compound [Fe].[Cu] IYRDVAUFQZOLSB-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 231100000566 intoxication Toxicity 0.000 description 2
- 230000035987 intoxication Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 239000002341 toxic gas Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses the production technologies of nanometer ferro oxide, belong to nano iron oxide production field, the production technology of nanometer ferro oxide, it is that raw material prepares nanometer ferro oxide using industrial waste water, save the cost of sewage treatment, save the operating cost of factory, during preparing nanometer ferro oxide, using the alkaline scrap material of industrial wastes simultaneously as adjusting raw material, further save the cost of factory's operation, during carrying out nano iron oxide production using wet-precipitated, a large amount of bubbles will be generated under the action of the strainer of block-resistant protection cover and flow spoiler before ammonium hydroxide as precipitating reagent injection reaction mixture, these bubbles can discharge big energy in instant of detonation, promote the progress of precipitation reaction, while the energy for generation of exploding can also inhibit the excessive enrichment of ferric oxide particles plumule, it is not likely to produce precipitation process The ferric oxide particles of individual enormous sizes, are not easy to have an impact the preparation of nanometer ferro oxide.
Description
Technical field
The present invention relates to nano iron oxide production fields, more specifically to the production technology of nanometer ferro oxide.
Background technique
Nano iron oxide is a kind of multifunctional material.When ferric oxide particles size is small arrives nanoscale (1~100nm),
Surface atom number, specific surface area and surface can etc. sharply increased with the reduction of partial size, thus show small-size effect,
The features such as quantum size effect, skin effect and macro quanta tunnel effect, has good optical property, magnetism, catalytic
It can wait, the preparation method of nano iron oxide can be divided into wet process and dry method.Wet process mainly includes hydro-thermal method, forced hydrolysis method, coagulates
Glue-sol method, colloid chemistry methods, microemulsion method and chemical precipitation method etc..Dry method specifically includes that flame thermal decomposition, gas phase are heavy
Product, low-temperature plasma chemical vapour deposition technique (PCVD), solid phase method and laser thermal decomposition method etc..
The industrial wastewater for being largely rich in iron ion, these usual works are easily generated in factory related with ironwork producing
Industry waste water needs just be discharged into environment after reaching discharge standard into after crossing sewage treatment, and sewage treatment can make factory
Biggish production cost is afforded, therefore, some factories start with the auxiliary products such as these industrial wastewaters production reduced iron powder,
While rationally utilizing industrial wastewater resource, mitigate the production burden of factory.
Means are utilized in numerous industrial wastewaters, quality the technique for having a kind of hydrometallurgy nano iron oxide: is compared into chlorination
Ferrous aqueous solution, clean iron plate and iron oxide seed crystal are put into reaction kettle, are kept the temperature, then precipitating reagent is added into kettle, into
The stirring of row duration stops reaction when pH value of reaction system is between 4-5, passes through filters pressing, drying, crushing and roller later
Formula temperature programming calcining, can be obtained nano iron oxide.
Above method reaction condition is relatively simple, lower production costs, but during iron oxide precipitating, iron oxide
Particle will appear enrichment phenomenon, and the degree being enriched with is different, it is difficult to form the ferric oxide particles group of identical size and specification, therefore
In order to produce the nano iron oxide with practicability, need to carry out more complicated shaping work to the ferric oxide particles that precipitating generates
Sequence is added significantly to cost for wastewater treatment.
Summary of the invention
1. technical problems to be solved
Aiming at the problems existing in the prior art, the purpose of the present invention is to provide the production technologies of nanometer ferro oxide, it can
The phenomenon that realize during nano iron oxide is precipitated and produced, reduce the enrichment of individual nano iron oxide cruelties, give birth to precipitating
At nano iron oxide particle size and specification it is roughly the same, reduce the cost of subsequent trimming, substantially reduce wastewater treatment
Cost, increase the line balancing rate of factory.
2. technical solution
To solve the above problems, the present invention adopts the following technical scheme that.
The production technology of nanometer ferro oxide, the production technology of nanometer ferro oxide, key step are as follows:
S1, waste liquid PH are adjusted, and waste liquid is transported in waste liquid conditioning tank, and it is useless that suitable industrial alkaline is mixed into waste liquid conditioning tank
Slag, such as furnace carbon slag adjust the PH of waste liquid to neutrality, waste liquid are filtered, primary filtrate is obtained, facilitates subsequent interfering ion
Removal；
S2, interfering ion removal adjust acquisition primary filtrate to S1 waste liquid PH and utilize paper chromatography by the iron ion and copper in filtrate
Ion isolation obtains filtrate containing iron ion, since iron copper chemical property is close, and is equally the predominantly copper and iron in industrial wastewater
Ion needs to separate copper and iron ion, prevents copper ion from polluting subsequent nano iron oxide；
S3, object purify, and enough dilute hydrochloric acid is added in the filtrate containing iron ion obtained into the removal of S2 interfering ion, adjusts
PH to the 2-3 of the filtrate containing iron ion keeps iron ion fully oxidized, converts ferric ion for part divalent ferrous ion, then
Filters pressing is carried out to filtrate containing iron ion, obtains solid iron containing compounds；
S4 pretreatment of raw material carries out flush clean to the solid iron containing compounds obtained in the purification of S3 object using methanol,
The solid iron containing compounds cleaned are air-dried again later, is finally crushed using ball mill dry grinding, obtains iron containing compounds powder
End, cleaning can draw the interfering ion of solid-state iron containing compounds surface adhesion, and solid-state iron containing compounds are milled to powder can be with
Accelerate subsequent dissolution；
The dissolution of S5 object, the iron containing compounds powder diluted hydrochloric acid dissolution that will be obtained in S4 pretreatment of raw material, and make mixed liquor
PH be maintained at 4-5；
S6 wet-precipitated, into mixed liquor, duration is filled with ammonium hydroxide as precipitating reagent, is stirred during precipitating, obtains
Ferric oxide particles；
The ferric oxide particles that S6 wet-precipitated obtains are added in ball mill and carry out wet-milling, make nano oxidized by S7 wet-milling shaping
The size and specification of iron finished product are roughly the same；
S8 screening air-dries, and sieves after the nano iron oxide finished product that S7 wet-milling shaping obtains is air-dried, receives to what cannot be sieved
Rice iron oxide finished product re-starts S7 wet-milling shaping, until nano iron oxide finished product can be sieved, makes nano iron oxide end product rule
Very little and specification is substantially close.
It may be implemented to reduce showing for individual nano iron oxide cruelty enrichments during nano iron oxide is precipitated and produced
As the nano iron oxide particle size and specification for generating precipitating are roughly the same, reduce the cost of subsequent trimming, substantially subtract
The cost of small wastewater treatment increases the line balancing rate of factory.
Further, it during S1 waste liquid PH is adjusted, S3 object purifies and S6 wet-precipitated, needs to keep logical
Wind avoids being enriched with the intoxication accident generated because of toxic gas.
Further, it during the wet-precipitated, needs persistently to instill dilute hydrochloric acid into mixed liquor, makes mixed liquor
PH remains at 4-5, and after the completion of precipitation reaction, filtrate and solid are separated by filtration acquisition ferric oxide particles.
Further, in the S7 wet-milling shaping, wet grinding media select methanol, as medium methanol wet-milling process
In can make ferric oxide particles crush it is more uniform, while methanol can also using ball milling process wash away nano iron oxide at
The foreign ion on product surface makes nano iron oxide finished product be easy to keep pure.
Further, the wet-precipitated container includes reaction bed, and delivery pipe, the conveying are equipped in the reaction bed
Pipe includes that the supervisor of horizontal paving is fixedly connected on the branched pipes on being responsible for multiple, and reaction bed passes through multiple delivery pipes and reaction bed
Inside it is connected, check valve is fixedly connected in multiple branched pipes, one end of the branched pipe management reaction bed is fixed is connected
It is connected to block-resistant protection cover, the Anti-stop cover includes first substrate and the second substrate, is consolidated between the first substrate and the second substrate
Surely it is connected with strainer, the second substrate is fixedly connected with branched pipe, and delivery pipe runs through the second substrate, and precipitating reagent ammonium hydroxide is passing through
It crosses reaction bed and after delivery pipe enters block-resistant protection cover, the flow-disturbing effect through filter screen can make ammonium hydroxide form a large amount of bubbles, these
The high energy energy of moment is exploded and is generated in bubble meeting after being discharged into reaction bed in the mixed liquor in reaction bed, acceleration precipitated
Journey, and play certain inhibiting effect to the barbarous enrichment of ferric oxide particles, is that the size of ferric oxide particles is more uniform, wherein
The one end of delivery pipe far from reaction bed is connected to ammonium hydroxide storing unit stationary phase, and delivery pipe is connected with high-pressure hydraulic pump, by height
Water pump conveys precipitating reagent ammonium hydroxide into delivery pipe.
Further, the first substrate is located at the upside of the second substrate, and the volume of first substrate is much larger than the second base
Plate, i.e. block-resistant protection cover are integrally in inversed taper platform shape, and the ferric oxide particles for generating precipitating are not easy be not enriched on strainer, are not easy
Filter net jam is caused, is not easy to influence the normal discharge of precipitating reagent ammonium hydroxide.
Further, it is fixedly connected with multiple flow spoilers on the strainer, the flow spoiler includes fixed column and flow disturbing cover,
The fixed column is fixedly connected on strainer, and the flow disturbing cover is socketed in the outside of fixed column, and digging in the fixed column has work
Slot is moved, push plate is fixedly connected between the flow disturbing cover inner wall, and push plate runs through loose slot, fixes between the loose slot inner wall
It is connected with limit slide bar, and limits slide bar and runs through push plate, is fixedly connected with compression between the limit slide bar and loose slot inner wall
Spring, and compressed spring is located at side of the push plate far from flow disturbing cover, and compressed spring is socketed in the outside of limit slide bar, is compressing
Under spring and the ammonium hydroxide collective effect of flowing, flow disturbing cover can move back and forth in the outside of fixed column, play flow-disturbing effect.
Further, it is connected with wear ring in the limit slide bar and push pedal bracket, and wear ring is fixedly connected with push plate,
And the outer wall of wear ring inner wall and limit slide bar provide to be connected with polishing layer, wear ring can reduce limit slide bar and push plate it
Between abrasion, can make to limit slide bar and push plate and be not susceptible to excessive abrasion, be not easy the connection limited between slide bar and push plate
It shakes.
Further, digging on the flow disturbing cover has a pair of of enhancing slot, between two enhancing slot and the loose slots
It is interspersed, enhancing slot can effectively increase the flow-disturbing effect of flow spoiler, increase the foaming effect of flow spoiler.
Further, multiple ultrasonic horns are fixedly connected in the trough floor of the reaction bed, and ultrasonic wave is sent out
It is uniformly interspersed between acoustic device and block-resistant protection cover.
3. beneficial effect
Compared with the prior art, the present invention has the advantages that
This programme is that raw material prepares nanometer ferro oxide using industrial waste water, saves the cost of sewage treatment, saves work
The operating cost of factory, it is former as adjusting using the alkaline scrap material of industrial wastes simultaneously during preparing nanometer ferro oxide
Material further saves the cost of factory's operation, will be as heavy during carrying out nano iron oxide production using wet-precipitated
A large amount of bubbles are generated under the action of the strainer of block-resistant protection cover and flow spoiler before the ammonium hydroxide injection reaction mixture of shallow lake agent,
These bubbles can discharge big energy in instant of detonation, promote the progress of precipitation reaction, while the energy for generation of exploding can also press down
The excessive enrichment of oxygenerating iron particle plumule, makes precipitation process be not likely to produce the ferric oxide particles of individual enormous sizes, is not easy pair
The preparation of nanometer ferro oxide has an impact, and the high frequency sound wave that ultrasonic horn generates can accelerate the explosion of bubble, together
When high frequency sound wave can also further suppress instant of detonation and can discharge big energy, promote the progress of precipitation reaction, while production of exploding
Raw energy can also inhibit the excessive enrichment of ferric oxide particles plumule, and precipitation process is made to be not likely to produce the oxidation of individual enormous sizes
Iron particle is not easy to have an impact the preparation of nanometer ferro oxide.
Detailed description of the invention
Fig. 1 is main flow schematic diagram of the invention.
Fig. 2 is the fragmentary side cross-sectional view of reaction bed of the invention.
Fig. 3 is the structural schematic diagram in Fig. 2 at A.
Fig. 4 is the structural schematic diagram in Fig. 3 at B.
Fig. 5 is the structural schematic diagram of block-resistant protection cover of the invention.
Fig. 6 is the front section view of flow spoiler of the invention.
Fig. 7 is the side view of flow spoiler of the invention.
Fig. 8 is the main view of flow spoiler of the invention.
Figure label explanation:
1 reaction bed, 2 delivery pipes, 3 check valves, 4 first substrates, 5 the second substrates, 6 strainers, 7 flow spoilers, 701 fixed columns, 702 are disturbed
Flow cover, 703 loose slots, 704 limit slide bars, 705 push plates, 706 compressed springs, 707 enhancing slots, 8 ultrasonic generators.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention；Technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description；Obviously；Described embodiments are only a part of the embodiments of the present invention；Instead of all the embodiments, it is based on
Embodiment in the present invention；It is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment；It shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the instruction such as term " on ", "lower", "inner", "outside", " top/bottom end "
Orientation or positional relationship be based on the orientation or positional relationship shown in the drawings, be merely for convenience of description the present invention and simplification retouch
It states, rather than the device or element of indication or suggestion meaning must have a particular orientation, be constructed and operated in a specific orientation,
Therefore it is not considered as limiting the invention.In addition, term " first ", " second " are used for description purposes only, and cannot understand
For indication or suggestion relative importance.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation " " is set
Be equipped with ", " be arranged/connect ", " connection " etc., shall be understood in a broad sense, such as " connection ", may be a fixed connection, be also possible to removable
Connection is unloaded, or is integrally connected；It can be mechanical connection, be also possible to be electrically connected；It can be directly connected, it can also be in
Between medium be indirectly connected, can be the connection inside two elements.It for the ordinary skill in the art, can be specific
Situation understands the concrete meaning of above-mentioned term in the present invention.
Embodiment 1:
Referring to Fig. 1, the production technology of nanometer ferro oxide, key step are as follows:
S1, waste liquid PH are adjusted, and waste liquid is transported in waste liquid conditioning tank, and it is useless that suitable industrial alkaline is mixed into waste liquid conditioning tank
Slag, such as furnace carbon slag adjust the PH of waste liquid to neutrality, waste liquid are filtered, primary filtrate is obtained, facilitates subsequent interfering ion
Removal；
S2, interfering ion removal adjust acquisition primary filtrate to S1 waste liquid PH and utilize paper chromatography by the iron ion and copper in filtrate
Ion isolation obtains filtrate containing iron ion, since iron copper chemical property is close, and is equally the predominantly copper and iron in industrial wastewater
Ion needs to separate copper and iron ion, prevents copper ion from polluting subsequent nano iron oxide；
S3, object purify, and enough dilute hydrochloric acid is added in the filtrate containing iron ion obtained into the removal of S2 interfering ion, adjusts
PH to the 2-3 of the filtrate containing iron ion keeps iron ion fully oxidized, converts ferric ion for part divalent ferrous ion, then
Filters pressing is carried out to filtrate containing iron ion, solid iron containing compounds is obtained, during carrying out object purification, needs to keep
Ventilation avoids being enriched with the intoxication accident generated because of toxic gas；
S4 pretreatment of raw material carries out flush clean to the solid iron containing compounds obtained in the purification of S3 object using methanol,
The solid iron containing compounds cleaned are air-dried again later, is finally crushed using ball mill dry grinding, obtains iron containing compounds powder
End, cleaning can draw the interfering ion of solid-state iron containing compounds surface adhesion, and solid-state iron containing compounds are milled to powder can be with
Accelerate subsequent dissolution；
The dissolution of S5 object, the iron containing compounds powder diluted hydrochloric acid dissolution that will be obtained in S4 pretreatment of raw material, and make mixed liquor
PH be maintained at 4-5；
S6 wet-precipitated, into mixed liquor, duration is filled with ammonium hydroxide as precipitating reagent, is stirred during precipitating, obtains
Ferric oxide particles, and dilute hydrochloric acid is persistently instilled into mixed liquor, so that the PH of mixed liquor is remained at 4-5, it is complete in precipitation reaction
Filtrate and solid are separated by filtration acquisition ferric oxide particles by Cheng Hou；
The ferric oxide particles that S6 wet-precipitated obtains are added in ball mill and are added into ball mill enough by S7 wet-milling shaping
Medium methanol carries out wet-milling, and it is more uniform that during wet-milling ferric oxide particles can crush the methanol as medium,
Keep size and the specification of nano iron oxide finished product roughly the same, at the same methanol can also using ball milling process wash away it is nano oxidized
The foreign ion of iron finished surface makes nano iron oxide finished product be easy to keep pure.
S8 screening air-dries, and sieves after the nano iron oxide finished product that S7 wet-milling shaping obtains is air-dried, to cannot be sieved
Nano iron oxide finished product re-start S7 wet-milling shaping, until nano iron oxide finished product can be sieved, make nano iron oxide at
Product size and specification are substantially close.
It may be implemented to reduce showing for individual nano iron oxide cruelty enrichments during nano iron oxide is precipitated and produced
As the nano iron oxide particle size and specification for generating precipitating are roughly the same, reduce the cost of subsequent trimming, substantially subtract
The cost of small wastewater treatment increases the line balancing rate of factory.
Fig. 2-4 please be participate in, S6 wet-precipitated need to carry out in corresponding container, and container includes reaction bed 1, in reaction bed 1
It is equipped with delivery pipe 2, delivery pipe 2 includes that the supervisor of horizontal paving is fixedly connected on the branched pipes on being responsible for multiple, and reaction bed 1 is logical
It crosses in multiple delivery pipes 2 and reaction bed 1 and is connected, check valve 3, branched pipe management reaction are fixedly connected in multiple branched pipes
One end of bed 1 is fixedly connected with block-resistant protection cover, and Anti-stop cover includes first substrate 4 and the second substrate 5, first substrate 4 and second
Strainer 6 is fixedly connected between substrate 5, the second substrate 5 is fixedly connected with branched pipe, and delivery pipe 2 runs through the second substrate 5, is sunk
Agent ammonium hydroxide in shallow lake is entering block-resistant protection cover by reaction bed 1 and delivery pipe 2, and the flow-disturbing effect through filter screen 6 can be such that ammonium hydroxide is formed
A large amount of bubbles, these bubbles can explode in the mixed liquor in reaction bed 1 and generate the high energy of moment after being discharged into reaction bed 1
Energy accelerates precipitation process, and plays certain inhibiting effect to the barbarous enrichment of ferric oxide particles, is the ruler of ferric oxide particles
Very little more uniform, wherein the one end of delivery pipe 2 far from reaction bed 1 is connected to ammonium hydroxide storing unit stationary phase, and delivery pipe 2 and height
Water pump is connected, and precipitating reagent ammonium hydroxide is conveyed into delivery pipe 2 from high-pressure hydraulic pump, first substrate 4 is located at the upper of the second substrate 5
Side, and the volume of first substrate 4 is much larger than the second substrate 5, i.e. block-resistant protection cover is integrally in inversed taper platform shape, the oxygen for generating precipitating
Change iron particle to be not easy not to be enriched on strainer 6, does not easily cause strainer 6 to block, be not easy to influence the normal discharge of precipitating reagent ammonium hydroxide.
It please refers to and is fixedly connected with multiple flow spoilers 7 on Fig. 6-8 strainer 6, flow spoiler 7 includes fixed column 701 and flow disturbing cover
702, fixed column 701 is fixedly connected on strainer 6, and flow disturbing cover 702 is socketed in the outside of fixed column 701, is dug in fixed column 701
There is loose slot 703, push plate 705 is fixedly connected between 702 inner wall of flow disturbing cover, and push plate 705 runs through loose slot 703, loose slot
It is fixedly connected with limit slide bar 704 between 703 inner walls, and limits slide bar 704 and runs through push plate 705, limits slide bar 704 and loose slot
Compressed spring 706 is fixedly connected between 703 inner walls, and compressed spring 706 is located at side of the push plate 705 far from flow disturbing cover 702,
And compressed spring 706 is socketed in the outside of limit slide bar 704, and under compressed spring 706 and the ammonium hydroxide collective effect of flowing, flow-disturbing
Cover 702 can move back and forth in the outside of fixed column 701, play flow-disturbing effect, limit and connect in slide bar 704 and 705 bracket of push plate
It is connected to wear ring, and wear ring is fixedly connected with push plate 705, and the outer wall company of regulation of wear ring inner wall and limit slide bar 704
It is connected to polishing layer, wear ring can reduce the abrasion between limit slide bar 704 and push plate 705, can make to limit slide bar 704 and push away
Plate 705 is not susceptible to excessive abrasion, and the connection limited between slide bar 704 and push plate 705 is made to be less prone to shaking, flow disturbing cover 702
Upper cutting has a pair of of enhancing slot 707, is interspersed between two enhancings slot 707 and loose slots 703, and enhancing slot 707 can
Effectively to increase the flow-disturbing effect of flow spoiler 7, increases the foaming effect of flow spoiler 7, be fixedly connected in the trough floor of reaction bed 1
There are multiple ultrasonic horns 8, and is uniformly interspersed between ultrasonic horn 8 and block-resistant protection cover, ultrasonic wave
The overclocking sound wave that sounding device 8 generates can accelerate ammonium hydroxide bubbles burst, while inhibit the excessive enrichment of ferric oxide particles plumule.
During carrying out wet-precipitated, delivery pipe 2 is used to convey precipitating reagent ammonium hydroxide, and ammonium hydroxide is arranged by block-resistant protection cover
Enter in the mixed liquor in reaction bed 1, and ammonium hydroxide can be stirred in filter screen 6 and flow spoiler 7 whens by strainer 6 and flow spoiler 7,
Especially flow spoiler 7, under the collective effect of swiftly flowing ammonium hydroxide and the compressed spring 706 in compressive state, flow disturbing cover
702 can move reciprocatingly along 701 surface of fixed column, greatly increase the blistering rate of ammonium hydroxide, and precipitating reagent ammonium hydroxide is entering in reaction bed 1
Mixed liquor in after, under the action of the high frequency sound wave that ultrasonic horn 8 generates, what precipitating reagent ammonium hydroxide was formed rise steep oneself-meeting it is fast
Speed explosion, instant of detonation can discharge big energy, promote the progress of precipitation reaction, while the energy for generation of exploding can also inhibit oxygen
The excessive enrichment for changing iron particle plumule, makes precipitation process be not likely to produce the ferric oxide particles of individual enormous sizes, is not easy to nanometer
The preparation of grade iron oxide has an impact.
It is that raw material prepares nanometer ferro oxide using industrial waste water, saves the cost of sewage treatment, save factory
Operating cost, during preparing nanometer ferro oxide, using simultaneously industrial wastes alkaline scrap material as adjusting raw material,
The cost for further saving factory's operation will be as precipitating during carrying out nano iron oxide production using wet-precipitated
A large amount of bubbles are generated under the action of the strainer 6 of block-resistant protection cover and flow spoiler 7 before the ammonium hydroxide injection reaction mixture of agent,
These bubbles can discharge big energy in instant of detonation, promote the progress of precipitation reaction, while the energy for generation of exploding can also press down
The excessive enrichment of oxygenerating iron particle plumule, makes precipitation process be not likely to produce the ferric oxide particles of individual enormous sizes, is not easy pair
The preparation of nanometer ferro oxide has an impact, and the high frequency sound wave that ultrasonic horn 8 generates can accelerate the explosion of bubble, together
When high frequency sound wave can also further suppress instant of detonation and can discharge big energy, promote the progress of precipitation reaction, while production of exploding
Raw energy can also inhibit the excessive enrichment of ferric oxide particles plumule, and precipitation process is made to be not likely to produce the oxidation of individual enormous sizes
Iron particle is not easy to have an impact the preparation of nanometer ferro oxide.
It is described above；It is merely preferred embodiments of the present invention；But scope of protection of the present invention is not limited thereto；
Anyone skilled in the art is in the technical scope disclosed by the present invention；According to the technique and scheme of the present invention and its
It improves design and is subject to equivalent substitution or change；It should be covered by the scope of protection of the present invention.
Claims (10)
1. the production technology of nanometer ferro oxide, it is characterised in that: its key step are as follows:
S1, waste liquid PH are adjusted, and waste liquid is transported in waste liquid conditioning tank, and it is useless that suitable industrial alkaline is mixed into waste liquid conditioning tank
Slag adjusts the PH of waste liquid to neutrality, waste liquid is filtered, primary filtrate is obtained；
S2, interfering ion removal adjust acquisition primary filtrate to S1 waste liquid PH and utilize paper chromatography by the iron ion and copper in filtrate
Ion isolation obtains filtrate containing iron ion；
S3, object purify, and enough dilute hydrochloric acid is added in the filtrate containing iron ion obtained into the removal of S2 interfering ion, adjusts
PH to the 2-3 of the filtrate containing iron ion keeps iron ion fully oxidized, converts ferric ion for part divalent ferrous ion, then
Filters pressing is carried out to filtrate containing iron ion, obtains solid iron containing compounds；
S4 pretreatment of raw material carries out flush clean to the solid iron containing compounds obtained in the purification of S3 object using methanol,
The solid iron containing compounds cleaned are air-dried again later, is finally crushed using ball mill dry grinding, obtains iron containing compounds powder
End；
The dissolution of S5 object, the iron containing compounds powder diluted hydrochloric acid dissolution that will be obtained in S4 pretreatment of raw material, and make mixed liquor
PH be maintained at 4-5；
S6 wet-precipitated, into mixed liquor, duration is filled with ammonium hydroxide as precipitating reagent, is stirred during precipitating, obtains
Ferric oxide particles；
The ferric oxide particles that S6 wet-precipitated obtains are added in ball mill and carry out wet-milling, make nano oxidized by S7 wet-milling shaping
The size and specification of iron finished product are roughly the same；
S8 screening air-dries, and sieves after the nano iron oxide finished product that S7 wet-milling shaping obtains is air-dried, receives to what cannot be sieved
Rice iron oxide finished product re-starts S7 wet-milling shaping, until nano iron oxide finished product can be sieved.
2. the production technology of nanometer ferro oxide according to claim 1, it is characterised in that: in S1 waste liquid PH adjusting, S3
During object purification and S6 wet-precipitated, need to keep divulging information.
3. the production technology of nanometer ferro oxide according to claim 1, it is characterised in that: in S1 waste liquid PH adjusting, S3
During object purification and S6 wet-precipitated, need to keep divulging information.
4. the production technology of nanometer ferro oxide according to claim 1, it is characterised in that: in the S7 wet-milling shaping,
Wet grinding media selects methanol.
5. the production technology of nanometer ferro oxide according to claim 1, it is characterised in that: stating wet-precipitated container includes
Reaction bed (1) is equipped with delivery pipe (2) in the reaction bed (1), and the delivery pipe (2) includes the supervisor of horizontal paving and multiple solid
Surely the branched pipe being connected on supervisor, and reaction bed (1) is connected by the way that multiple delivery pipes (2) and reaction bed (1) are interior, Duo Gesuo
It states and is fixedly connected in branched pipe check valve (3), one end of branched pipe management reaction bed (1) is fixedly connected with anti-blocking guarantor
Shield, the Anti-stop cover includes first substrate (4) and the second substrate (5), between the first substrate (4) and the second substrate (5)
It is fixedly connected with strainer (6), the second substrate (5) is fixedly connected with branched pipe, and delivery pipe (2) runs through the second substrate (5).
6. the production technology of nanometer ferro oxide according to claim 5, it is characterised in that: first substrate (4) position
In the upside of the second substrate (5), and the volume of first substrate (4) is much larger than the second substrate (5), i.e. block-resistant protection cover is integrally in down
Taper type.
7. the production technology of nanometer ferro oxide according to claim 5, it is characterised in that: fixed on the strainer (6)
It is connected with multiple flow spoilers (7), the flow spoiler (7) includes fixed column (701) and flow disturbing cover (702), the fixed column (701)
It is fixedly connected on strainer (6), the flow disturbing cover (702) is socketed in the outside of fixed column (701), on the fixed column (701)
Cutting has loose slot (703), is fixedly connected with push plate (705) between flow disturbing cover (702) inner wall, and push plate (705) runs through
Loose slot (703) is fixedly connected with limit slide bar (704) between loose slot (703) inner wall, and limits slide bar (704) and pass through
It wears push plate (705), is fixedly connected with compressed spring (706) between the limit slide bar (704) and loose slot (703) inner wall, and
Compressed spring (706) is located at the side of push plate (705) far from flow disturbing cover (702), and compressed spring (706) is socketed in limit slide bar
(704) outside.
8. the production technology of nanometer ferro oxide according to claim 7, it is characterised in that: the limit slide bar (704)
With wear ring is connected in push plate (705) bracket, and wear ring is fixedly connected with push plate (705), and wear ring inner wall and limit
The outer wall of slide bar (704) provides to be connected with polishing layer.
9. the production technology of nanometer ferro oxide according to claim 7, it is characterised in that: state and opened on flow disturbing cover (702)
It is carved with a pair of of enhancing slot (707), is interspersed between two enhancing slots (707) and loose slot (703).
10. the production technology of nanometer ferro oxide according to claim 1, it is characterised in that: the slot of the reaction bed (1)
It is fixedly connected on bottom plate multiple ultrasonic horns (8), and between ultrasonic horn (8) and block-resistant protection cover uniformly
Be interspersed.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110841154A (en) * | 2019-11-22 | 2020-02-28 | 徐州达娇物资贸易有限公司 | Air humidifying device based on atomization treatment technology and using method thereof |
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