CN106517352B - The preparation method of the lower iron oxide red seed crystal of joint auxiliary agent guiding - Google Patents
The preparation method of the lower iron oxide red seed crystal of joint auxiliary agent guiding Download PDFInfo
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- CN106517352B CN106517352B CN201610901249.9A CN201610901249A CN106517352B CN 106517352 B CN106517352 B CN 106517352B CN 201610901249 A CN201610901249 A CN 201610901249A CN 106517352 B CN106517352 B CN 106517352B
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- 239000013078 crystal Substances 0.000 title claims abstract description 57
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000012752 auxiliary agent Substances 0.000 title claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 30
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011259 mixed solution Substances 0.000 claims abstract description 25
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002002 slurry Substances 0.000 claims abstract description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 18
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 16
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 16
- 239000004571 lime Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000013019 agitation Methods 0.000 claims abstract description 13
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 9
- 239000011780 sodium chloride Substances 0.000 claims abstract description 9
- 229910001448 ferrous ion Inorganic materials 0.000 claims abstract description 7
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 159000000013 aluminium salts Chemical class 0.000 claims abstract description 6
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims abstract description 6
- 239000010440 gypsum Substances 0.000 claims abstract description 6
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 6
- 238000007873 sieving Methods 0.000 claims abstract description 6
- 239000004744 fabric Substances 0.000 claims abstract description 5
- 235000011116 calcium hydroxide Nutrition 0.000 claims abstract description 4
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 4
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 238000012216 screening Methods 0.000 claims abstract description 3
- 229960002163 hydrogen peroxide Drugs 0.000 claims abstract 4
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 11
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 9
- 230000001804 emulsifying effect Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 7
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 4
- 239000011790 ferrous sulphate Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 229910052603 melanterite Inorganic materials 0.000 claims description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 27
- 229960005191 ferric oxide Drugs 0.000 description 26
- 239000001062 red colorant Substances 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a kind of preparation method for combining the lower iron oxide red seed crystal of auxiliary agent guiding, comprise the following steps：The ferrous iron solution purified is taken, phosphoric acid is added and aluminium salt stirs and the first mixed solution is made, it is 100 300g/L to adjust ferrous iron concentration in the first mixed solution, standby；Water intaking, sodium chloride and lime, stir and the second mixed solution are made, and the mass concentration that milk of lime is caused after stirring is 2 3%；Second mixed solution is heated to 40 60 DEG C, the first mixed solution is added under agitation and the 3rd mixed solution is made, the pH value of the 3rd mixed solution of regulation is 10 11；First added under agitation into the 3rd mixed solution and hydrogenperoxide steam generator is reacted, untill without ferrous ion；It is iron oxide red seed crystal that manufactured iron red crystal seed formation slurry is carried out screening to remove gypsum and impurity, the slurry under sieving by the screen cloth of 300 400 mesh.The preparation method of the present invention is safe and green.
Description
Technical field
The invention belongs to the preparing technical field of iron oxide red, is aoxidized more particularly to one kind joint auxiliary agent guiding is lower
The preparation method of iron red crystal seed formation.
Background technology
Ferric oxide red colorant is a kind of very important inorganic pigment, and wide model is used for the industries such as coating, building materials, and it produces work
Skill route is more, and using crystal seed preparation+second oxidation ferric oxide red colorant is produced mostly in wet process technique, at present with
During ferrous iron is prepared for the crystal seed of raw material, nertralizer is made using ammoniacal liquor more, air oxidation is passed through and forms crystal seed.But due to producing work
There is following problem using industrial ammonia in skill：When ammoniacal liquor transport, using upper dangerous；Second, ammonia is produced in production process
The environmental issues such as nitrogen；Third, production cost height.Therefore, it is necessary to develop safer and green production technology to produce oxygen
Change iron oxide red.
The content of the invention
It is an object of the invention to solve the dangerous not environmentally problem of traditional iron oxide red production technology, and provide one
The production technology of the safe and green iron oxide red of kind.
In order to realize according to object of the present invention and further advantage, there is provided the lower iron oxide of one kind joint auxiliary agent guiding
The preparation method of red crystal seed, comprises the following steps：
Step 1: taking the ferrous iron solution purified, add phosphoric acid and aluminium salt stirs and the first mixed solution is made, add
Phosphoric acid and ferrous mol ratio be n (PO4 3-)：n(Fe2+)=1：50-60, the aluminium salt of addition are n (Al with ferrous mol ratio3 +)：n(Fe2+)=1：10-20, it is 100-300g/L to adjust ferrous iron concentration in the first mixed solution, standby；
Step 2: water intaking, sodium chloride and lime, stir, the mass concentration that milk of lime is caused after stirring is 2-3%,
The addition of sodium chloride is the 10% of lime quality, continues stirring and emulsifying 1-4h and the second mixed solution is made；
Step 3: the second mixed solution is heated into 40-60 DEG C, adding the first mixed solution under agitation, to be made the 3rd mixed
Solution is closed, the pH value of the 3rd mixed solution of regulation is 10-11；
Step 4: first adding sodium hexametaphosphate dispersant solution into the 3rd mixed solution under agitation, peroxide is added
Change hydrogen solution to be reacted, untill without ferrous ion, as iron oxide red seed crystal slurry；
Step 5: manufactured iron red crystal seed formation slurry is carried out into screening by the screen cloth of 300-400 mesh removes gypsum and impurity,
Slurry under sieve is iron red crystal seed formation.
Preferably, the mass ratio of ferrous sulfate and lime is FeSO in step 34·7H2O：Lime=100：29-31.
Preferably, CaO content is more than 90% in lime used in step 2, and granularity is 300-400 mesh.
Preferably, the stirring and emulsifying time is 3h in step 2.
Preferably, the mass concentration of the calgon added in step 4 is 1%, and its addition is FeSO4·7H2O
The 1% of quality.
Preferably, the mass concentration of hydrogen peroxide is 20-50%, its addition and ferrous sulfate mole in step 4
Than for n (FeSO4)：n(H2O2)=2:1.05.It is further preferred that the mass concentration of hydrogen peroxide is 20-30% in step 4.
Preferably, the mode of heating in step 3 heats for steam, and heating-up temperature is 45-55 DEG C.
Preferably, the screen cloth to be sieved in step 5 is 400 mesh.
Preferably, ferrous iron concentration is 150-250g/L in the first mixed solution in step 1.
The present invention comprises at least following beneficial effect：
(1) formation of the auxiliary agent phosphoric acid energy induced oxidation iron red crystal seed formation of addition of the invention, the side of addition one of auxiliary agent aluminium salt
Face can lure that iron oxide red produces small particle crystal seed into, on the other hand can promote the formation of big particle diameter gypsum particle, sodium chloride can increase
Add the solubility of lime, using milk of lime as nertralizer, hydrogen peroxide is oxidant, while in the common work of auxiliary agent calgon
Under, particle diameter difference very big iron oxide red seed crystal and gypsum particle are ultimately formed, facilitates point of iron oxide red seed crystal and gypsum
From, and then obtain uniform particle, bright-colored and high tinting strength, tinting power iron oxide red seed crystal；
(2) raw material used in invention is either transporting still safer in use, no hazards, and
Raw material used in the present invention is green, environment will not be caused to bear, used raw material is simple and easy to get and cost is low
Honest and clean, reaction temperature of the invention is 40-60 DEG C, good without high temperature, energy-conserving and environment-protective, obtained iron oxide red seed crystal quality.
Further advantage, target and the feature of the present invention embodies part by following explanation, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Brief description of the drawings
Fig. 1 is iron oxide red seed crystal preparation technology.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples, to make those skilled in the art's reference
Specification word can be implemented according to this.
It should be noted that experimental method described in following embodiments, is conventional method unless otherwise specified, institute
Reagent and material are stated, unless otherwise specified, is commercially obtained.
Embodiment one
Fig. 1 is seen, Step 1: to 10m3The concentration matched somebody with somebody after purification is added in tubbing of ferrous iron be 445g/L seven water sulfuric acid it is sub-
Ferrous solution 2.7m3, add 85% phosphoric acid 5L, add 100 kilograms of 16 water aluminum sulfate afterwards, finally plus clear water is to 8m3Place,
Stir molten equal；
Step 2: in 36m3Crystal seed reactor in be put into bottom water 15m3, start stirring, add 325 mesh content CaO=
90.3% 375 kilograms of calcium lime powder, add 50 kilograms of sodium chloride, stirring and emulsifying 3 hours；；
Step 3: open crystal seed reactor steam valve be passed through steam heating, be warming up to 55 DEG C and stop steam, under agitation to
Crystal seed reactor adds the 8m prepared3Copperas solution, system pH=10.3；
Step 4: adding molten equal calgon (12 kilograms) solution of 120L to crystal seed reactor, and stir；
30% hydrogen peroxide 210L is added from crystal seed reactor bottom under stirring, now slurry is without ferrous ion；
Step 7: the reciprocating sieve that seed slurry is pumped into 400 mesh sieves, oversize removes, and obtains sieving lower seed slurry i.e.
For iron oxide red seed crystal, then it is pumped into oxidation barrel and is aoxidized and obtain ferric oxide red colorant.
Embodiment two
Step 1: to 10m3Ferrous iron is with ferrous sulfate heptahydrate solution 2.7m after addition purification in tubbing3(concentration 445g/
L), 85% phosphoric acid 5L is added, adds 100 kilograms of 16 water aluminum sulfate, finally adds clear water to 4.8m3Place, stir molten equal；
Step 2: in 36m3Crystal seed reactor in be put into bottom water 15m3, start stirring, add 325 mesh content CaO=
90.5% 375 kilograms of calcium lime powder, adds 50 kilograms of sodium chloride, stirs 3 hours；
Step 3: open crystal seed reactor steam valve be passed through steam heating, be warming up to 55 DEG C and stop steam, under agitation to
Crystal seed reactor adds the 4.8m prepared3Copperas solution, system pH=10.2；
Step 4: adding molten equal calgon (12 kilograms) solution of 120L to crystal seed reactor, and stir；Again
25% hydrogen peroxide 250L is added from crystal seed reactor bottom under agitation, now slurry is without ferrous ion；
Step 5: the reciprocating sieve that seed slurry is pumped into 400 mesh sieves, oversize removes, and obtains sieving lower seed slurry, i.e.,
For iron oxide red seed crystal, then it is pumped into oxidation barrel and aoxidize producing ferric oxide red colorant.
Embodiment three
Step 1: to 10m3Ferrous iron matches somebody with somebody the ferrous sulfate heptahydrate solution 2.7m added in tubbing after purification3(concentration 445g/
L), 85% phosphoric acid 5L is added, adds 100 kilograms of 16 water aluminum sulfate, finally adds clear water to 6m3Place, stir molten equal；
Step 2: in 36m3Crystal seed reactor in be put into bottom water 15m3, start stirring, add 325 mesh content CaO=
90.3% 375 kilograms of calcium lime powder, adds 50 kilograms of sodium chloride, stirring and emulsifying 3h；
Step 3: open crystal seed reactor steam valve be passed through steam heating, be warming up to 45 DEG C and stop steam, under agitation to
The 6m prepared is added in crystal seed reactor3Copperas solution, system pH=10.5；
Step 4: adding molten equal calgon (12 kilograms) solution of 120L into crystal seed reactor, and stir,
20% hydrogen peroxide 315L is added from crystal seed reactor bottom under agitation again, now slurry is without ferrous ion；
Step 5: the reciprocating sieve that seed slurry is pumped into 400 mesh sieves, oversize removes, and obtains sieving lower seed slurry, i.e.,
For iron oxide red seed crystal, then it is pumped into oxidation barrel and aoxidize producing ferric oxide red colorant.
Example IV
Step 1: to 10m3Ferrous iron matches somebody with somebody the ferrous sulfate heptahydrate solution 2.7m added in tubbing after purification3(concentration 445g/
L), 85% phosphoric acid 5.7L is added, adds 53 kilograms of six water alchlor, finally adds clear water to 5.5m3Place, stir molten equal；
Step 2: in 36m3Crystal seed reactor in be put into bottom water 15m3, start stirring, add 325 mesh content CaO=
90.3% 349 kilograms of calcium lime powder, adds 50 kilograms of sodium chloride, stirring and emulsifying 3h；
Step 3: open crystal seed reactor steam valve be passed through steam heating, be warming up to 45 DEG C and stop steam, under agitation to
The 6m prepared is added in crystal seed reactor3Copperas solution, system pH=10.5；
Step 4: adding molten equal calgon (12 kilograms) solution of 120L into crystal seed reactor, and stir,
25% hydrogen peroxide 250L is added from crystal seed reactor bottom under agitation again, now slurry is without ferrous ion；
Step 5: the reciprocating sieve that seed slurry is pumped into 400 mesh sieves, oversize removes, and obtains sieving lower seed slurry, i.e.,
For iron oxide red seed crystal, then it is pumped into oxidation barrel and aoxidize producing ferric oxide red colorant.
In order to illustrate beneficial effects of the present invention, ferric oxide red colorant made from Example one to example IV carries out grain
Footpath, color, Fe2O3Content, residue on sieve, water soluble salt content and oil absorption are tested, and obtain the data in table 1：
Table 1
Ferric oxide red colorant impurity produced by the present invention is less as can be seen from the above table, uniform particle sizes, it is bright-colored and
Se Ligao, therefore the iron oxide red seed crystal prepared with the present invention is practical, and the preparation technology safety and environmental protection of the present invention, it is adapted to
Promote.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, it is of the invention and unlimited
In specific details and shown here as the legend with description.
Claims (9)
1. a kind of preparation method for combining the lower iron oxide red seed crystal of auxiliary agent guiding, its feature is as comprising the following steps：
Step 1: taking the ferrous iron solution purified, add phosphoric acid and aluminium salt stirs and the first mixed solution is made, the phosphorus of addition
Acid is n (PO with ferrous mol ratio4 3-)：n(Fe2+)=1：50-60, the aluminium salt of addition are n (Al with ferrous mol ratio3+)：n
(Fe2+)=1：10-20, it is 100-300g/L to adjust ferrous iron concentration in the first mixed solution, standby；
Step 2: water intaking, sodium chloride and lime, stir, and so that the mass concentration of milk of lime is 2-3% after stirring, chlorination
The addition of sodium is the 13% of lime quality, continues stirring and emulsifying 1-4h and the second mixed solution is made；
Step 3: the second mixed solution is heated into 40-60 DEG C, adding the first mixed solution under agitation, that the 3rd mixing is made is molten
Liquid, the pH value of the 3rd mixed solution of regulation is 10-11；
Step 4: first adding sodium hexametaphosphate solution into the 3rd mixed solution under agitation, add hydrogenperoxide steam generator and enter
Row reaction, untill without ferrous ion, as iron red crystal seed formation slurry, wherein, the mass concentration of the calgon of addition is
1%, its addition is FeSO4·7H2The 1% of O mass；
Step 5: manufactured iron red crystal seed formation slurry is carried out into screening by the screen cloth of 300-400 mesh removes gypsum and impurity, under sieve
Slurry be iron oxide red seed crystal.
2. the preparation method of the lower iron oxide red seed crystal of joint auxiliary agent guiding as claimed in claim 1, it is characterised in that step 3
The mass ratio of middle ferrous sulfate and lime is FeSO4·7H2O：Lime=100：29-31.
3. the preparation method of the lower iron oxide red seed crystal of joint auxiliary agent guiding as claimed in claim 2, it is characterised in that step 2
CaO content is more than 90% in lime used, and granularity is 300-400 mesh.
4. the preparation method of the lower iron oxide red seed crystal of joint auxiliary agent guiding as claimed in claim 1, it is characterised in that step 2
The middle stirring and emulsifying time is 3h.
5. the preparation method of the lower iron oxide red seed crystal of joint auxiliary agent guiding as claimed in claim 1, it is characterised in that step 4
The mass concentration of middle hydrogen peroxide is 20-50%, and the mol ratio of its addition and ferrous sulfate is n (FeSO4)：n(H2O2)=2:
1.05。
6. the preparation method of the lower iron oxide red seed crystal of joint auxiliary agent guiding as claimed in claim 5, it is characterised in that step 4
The mass concentration of middle hydrogen peroxide is 20-30%.
7. the preparation method of the lower iron oxide red seed crystal of joint auxiliary agent guiding as claimed in claim 1, it is characterised in that step 3
In mode of heating be steam heating, heating-up temperature be 45-55 DEG C.
8. the preparation method of the lower iron oxide red seed crystal of joint auxiliary agent guiding as claimed in claim 1, it is characterised in that step 5
The screen cloth of middle sieving is 400 mesh.
9. the preparation method of the lower iron oxide red seed crystal of joint auxiliary agent guiding as claimed in claim 1, it is characterised in that step 1
In in the first mixed solution ferrous iron concentration be 150-250g/L.
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| DE59605913D1 (en) * | 1995-10-26 | 2000-10-26 | Bayer Ag | Color-pure, yellowish iron oxide red pigments, process for their preparation and their use |
| CN101239742A (en) * | 2008-03-20 | 2008-08-13 | 徐惠峰 | Method for extracting ultra-fine ferric oxide by using waste slag |
| CN101423257B (en) * | 2008-11-07 | 2011-01-05 | 浙江正奇化工有限公司 | Method for preparing nano grade iron oxide red |
| CN101417821B (en) * | 2008-11-20 | 2010-10-13 | 四川大学 | Method for preparing iron oxide red and cogenerating trisodium phosphate by ferro-phosphorus |
| CN102976413B (en) * | 2012-10-29 | 2014-06-25 | 中国有色集团（广西）平桂飞碟股份有限公司 | Two-step oxidation production method for iron oxide red pigment |
| CN103539206B (en) * | 2013-10-23 | 2015-07-01 | 中国有色集团（广西）平桂飞碟股份有限公司 | Wet method for preparing iron oxide red through introducing crystal form accelerant |
| CN103834814B (en) * | 2014-03-11 | 2015-09-09 | 斯莱登（北京）化工科技有限公司 | A kind of method preparing red iron oxide with copper nickel slag |
| CN105349778B (en) * | 2015-10-21 | 2017-04-19 | 黄钰雪 | Clean production method for recycling yellow phosphorus, iron oxide red or precious metal from ferrophosphorus |
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2016
- 2016-10-17 CN CN201610901249.9A patent/CN106517352B/en active Active
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