CN107244698A - A kind of preparation method of iron oxide red - Google Patents
A kind of preparation method of iron oxide red Download PDFInfo
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- CN107244698A CN107244698A CN201710460469.7A CN201710460469A CN107244698A CN 107244698 A CN107244698 A CN 107244698A CN 201710460469 A CN201710460469 A CN 201710460469A CN 107244698 A CN107244698 A CN 107244698A
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- Prior art keywords
- iron oxide
- oxide red
- culture medium
- preparation
- filtrate
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000000706 filtrate Substances 0.000 claims abstract description 36
- 241000894006 Bacteria Species 0.000 claims abstract description 26
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 23
- 239000000779 smoke Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 9
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 9
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 9
- 239000003818 cinder Substances 0.000 claims abstract description 9
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052683 pyrite Inorganic materials 0.000 claims abstract description 9
- 239000011028 pyrite Substances 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims abstract description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000001963 growth medium Substances 0.000 claims description 49
- 238000007873 sieving Methods 0.000 claims description 27
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 24
- 230000004069 differentiation Effects 0.000 claims description 18
- 239000000835 fiber Substances 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 11
- LQLQRFGHAALLLE-UHFFFAOYSA-N 5-bromouracil Chemical compound BrC1=CNC(=O)NC1=O LQLQRFGHAALLLE-UHFFFAOYSA-N 0.000 claims description 7
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 claims description 7
- 239000001888 Peptone Substances 0.000 claims description 6
- 108010080698 Peptones Proteins 0.000 claims description 6
- 238000012258 culturing Methods 0.000 claims description 6
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 6
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 6
- 235000019319 peptone Nutrition 0.000 claims description 6
- 230000001954 sterilising effect Effects 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 239000003643 water by type Substances 0.000 claims description 6
- AIUDWMLXCFRVDR-UHFFFAOYSA-N dimethyl 2-(3-ethyl-3-methylpentyl)propanedioate Chemical class CCC(C)(CC)CCC(C(=O)OC)C(=O)OC AIUDWMLXCFRVDR-UHFFFAOYSA-N 0.000 claims description 5
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 5
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 5
- 229940066779 peptones Drugs 0.000 claims description 5
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 5
- 239000012138 yeast extract Substances 0.000 claims description 5
- 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 description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 239000002574 poison Substances 0.000 claims 1
- 231100000614 poison Toxicity 0.000 claims 1
- 238000004659 sterilization and disinfection Methods 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 4
- 239000000049 pigment Substances 0.000 abstract description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 44
- 229960005191 ferric oxide Drugs 0.000 description 44
- 239000000243 solution Substances 0.000 description 19
- 239000002351 wastewater Substances 0.000 description 8
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 229910001448 ferrous ion Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 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 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 244000061458 Solanum melongena Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 229960004424 carbon dioxide Drugs 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 description 1
- 150000002506 iron compounds Chemical class 0.000 description 1
- -1 iron ion Chemical class 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003471 mutagenic agent Substances 0.000 description 1
- 231100000707 mutagenic chemical Toxicity 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical class [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000001062 red colorant Substances 0.000 description 1
- 238000005406 washing Methods 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]
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Disinfection, Sterilisation Or Deodorisation Of Air (AREA)
- Fertilizers (AREA)
Abstract
The present invention relates to a kind of preparation method of iron oxide red, belong to powder pigment technical field.The present invention is crushed pyrite cinder, collects crushed material, and crushed material, bacterium solution and deionized water are put into container and stirred, and is stood, and filtrate is collected in filtering；Filtrate is put into bruisher and smashed to pieces, mixture is smashed in collection to pieces, iron powder is added in mixture until iron powder is not redissolved, then stops adding iron powder to smashing to pieces, progress suction filtration collects smoke filtrate；Triethanolamine, smoke filtrate and ammonium hydrogen carbonate are put into container stirring until without Precipitation, then stood, filters, collects filter residue, by filter residue and drying, collect dried object；Dried object is calcined, calcined material is collected, you can iron oxide red is obtained.The iron oxide red that the present invention is prepared is not susceptible to reunite in high temperature environments, and dispersive property is good, has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation method of iron oxide red, belong to powder pigment technical field.
Background technology
Iron oxide red has natural and artificial two kinds.Natural title is western red, is substantially pure iron oxide, is red
Powder.Due to production method and the difference of operating condition, their crystal structure and physical behavior has very big difference, color and luster
Change in orange light to blue light between purple light, covering power and tinting strength, tinting power are all very big, there is superior fast light, resistance to atmospheric effect, resistant
Foul smell body, all resistance to bases, apparent iron oxide red are the orange red trigonal system powder to aubergine, natural western red phase
To density 55.25,0.4~20 μm of fineness, 1565 DEG C of fusing point (decomposition) releases oxygen during calcination, can by hydrogen and-carbonoxide also
Original is water insoluble into iron, is dissolved in hydrochloric acid, sulfuric acid, is slightly soluble in nitric acid and ferment class, with excellent fast light, high temperature resistant, acidproof, resistance to
Alkali, rust-preventing characteristic, good dispersion, tinting strength, tinting power and covering power are very strong, oozing property of oil-free and oozing property of water, and nontoxic, highest is allowed dense in air
Spend for 5mg/m3。
The process route for producing ferric oxide red colorant is more, can be divided into dry method and the big technique of wet method two, be given birth to using wet method
Produce during iron oxide red, matter ferrous in the substantial amounts of acid waste water containing ferrous ion, waste water can be produced
It is 0.1~0.3% to measure fraction, and the aqueous solution after finished product iron oxide red is mainly isolated in the source of waste water from reaction container
And the waste water that washing iron oxide red is produced, this wastewater pH is 3~4, and contains substantial amounts of ferrous ion, it is necessary to by processing
Can qualified discharge.And roasting method is mainly green vitriol roasting method in dry method, iron oxide red is made by high-temperature calcination in ferrous sulfate.
Production technology calcination produces sulfur monoxide and sulfur dioxide, severe contamination environment, is only suitable for small-scale production.Except this with
Outside, also iron oxide yellow, iron black calcination method, the method technological process are simple and convenient to operate, but easily caused by high temperature crystal reunite and
Bad dispersibility.
It would therefore be highly desirable to the substantial amounts of acid waste water containing ferrous ion will not be produced when preparing iron oxide red by finding,
And the iron oxide red prepared has preferable dispersive property under the high temperature conditions, the preparation method reunited is difficult.
The content of the invention
The technical problems to be solved by the invention：It can be produced during for preparing iron oxide red currently with dry and wet big
The acid waste water containing ferrous ion of amount, and the iron oxide red prepared easily causes crystal to be reunited under the high temperature conditions, causes
The problem of bad dispersibility, there is provided a kind of preparation method of iron oxide red.
In order to solve the above technical problems, the present invention is using technical scheme as described below：
A kind of preparation method of iron oxide red, it is characterised in that the iron oxide red includes following preparation process：
（1）Pyrite cinder is crushed, crushed material is collected, crushed material, bacterium solution and deionized water are put into container and stirred,
Stand, filtrate is collected in filtering；
（2）Filtrate is put into bruisher and smashed to pieces, collection smash mixture to pieces, to smash to pieces in mixture add iron powder until iron powder not
It is redissolved, then stops adding iron powder, carries out suction filtration, collect smoke filtrate；
（3）Dimethylformamide, smoke filtrate and ammonium hydrogen carbonate are put into container stirring until without Precipitation, then stood, is filtered,
Filter residue is collected, by filter residue and drying, dried object is collected；
（4）Dried object is calcined, calcined material is collected, you can iron oxide red is obtained.
The mass ratio of the crushed material, bacterium solution and deionized water is 1:3:1~1:5:1.
The mass ratio 1 of the dimethylformamide, smoke filtrate and ammonium hydrogen carbonate:6:3.
The calcination process is to be warming up to 790~860 DEG C with 6 DEG C/min, calcines 1~2h, you can.
The preparation of the bacterium solution includes following preparation process：
A. it is 35~40% bloodstone to be placed in into air humidity, and temperature is to stand 3~5 days in 25~32 DEG C of culturing room, then is entered
Row is crushed, and crosses 200 mesh sieves, collects sieving particle；
B. sieving particle is put into culture medium, addition is the 13~16% of culture medium quality, then culture medium is put into vibration
In incubator, design temperature is 25~32 DEG C, 20~22h of shaken cultivation；
C. culture terminate after into culture medium add sieving granular mass 2~5% iron oxide and sieving granular mass 0.2~
0.5% 5-bromouracil, 12~13h of Fiber differentiation, during Fiber differentiation, every 4~6h adds sieving into culture medium
The iron oxide of granular mass 0.6~1.0%；
D. after Fiber differentiation terminates, culture medium is filtered using 100 mesh gauzes, filtrate is collected, you can bacterium solution is obtained.
Culture medium is prepared as in the step b：Count by weight, take 70~85 parts of deionized waters, 23~26 parts of ferment
Female medicinal extract, 10~16 parts of peptones, 5~8 parts of sodium chloride, 4~6 parts of iron chloride, 0.8~1.1 part of potassium dihydrogen phosphate and 0.7~
1.0 parts of dipotassium hydrogen phosphates, stir, sterilizing, you can obtain culture medium.
The present invention is compared with other method, and advantageous effects are：
（1）The present invention carries out microculture by the use of the high bloodstone of iron oxide content as bacterium source first in control environment,
By culture medium culture propagation, during culture propagation, using 5-bromouracil as mutagens, using iron compound as luring
Inducement element, carries out dominant bacteria cultivation, obtains containing the bacterium solution for biting iron dominant bacteria；
（2）The present invention carries out microbiological treatment by bacterium solution to pyrite cinder, has decomposed ferro element in pyrite cinder, is formed
Solution containing iron ion, it is to avoid the generation of acid waste water, re-forms in precipitation process, utilizes dimethylformamide and bicarbonate
Ammonium is modified to it, it is to avoid the generation of intergranular agglomeration in calcining temperature-rise period, when reducing later stage calcining
The generation of agglomeration between crystal, improves the dispersive property of iron oxide red.
Embodiment
The preparation of culture medium：Count by weight, take 70~85 parts of deionized waters, 23~26 parts of yeast extracts, 10~16
Part peptone, 5~8 parts of sodium chloride, 4~6 parts of iron chloride, 0.8~1.1 part of potassium dihydrogen phosphate and 0.7~1.0 part of phosphoric acid hydrogen two
Potassium, stirs, and is put into autoclave sterilizer, the sterilizing at 115 DEG C, you can obtain culture medium.
The preparation of bacterium solution：
A. it is 35~40% bloodstone to be placed in into air humidity, and temperature is to stand 3~5 days in 25~32 DEG C of culturing room, then is put
Enter in pulverizer and to be crushed with 800r/min, cross 200 mesh sieves, collect sieving particle；
B. sieving particle is put into culture medium, addition is the 13~16% of culture medium quality, then culture medium is put into vibration
In incubator, design temperature is 25~32 DEG C, with 20~22h of 120rpm shaken cultivations；
C. culture terminate after into culture medium add sieving granular mass 2~5% iron oxide and sieving granular mass 0.2~
0.5% 5-bromouracil, 12~13h of Fiber differentiation, during Fiber differentiation, every 4~6h adds sieving into culture medium
The iron oxide of granular mass 0.6~1.0%；
D. after Fiber differentiation terminates, culture medium is filtered using 100 mesh gauzes, filtrate is collected, you can bacterium solution is obtained.
The preparation of iron oxide red：
（1）Pyrite cinder is put into pulverizer, crushed with 500r/min, collect crushed material, by crushed material, bacterium solution and
Deionized water in mass ratio 1:3:1~1:5:1, it is put into container, at 25~32 DEG C, is stirred with 150r/min after 3~5h, it is quiet
4~6h is put, is filtered, filtrate is collected；
（2）Filtrate is put into bruisher, 10~15min is smashed to pieces with 12000r/min, mixture is smashed in collection to pieces, to smashing mixing to pieces
Iron powder is added in thing until iron powder is not redissolved, then stops adding iron powder, and progress suction filtration collects smoke filtrate；
（3）In mass ratio 1:6:3, dimethylformamide, smoke filtrate and ammonium hydrogen carbonate are put into container, at 50~55 DEG C, with
120r/min stirrings are until without Precipitation, then stand 1~2h, filter, and collect filter residue, and filter residue is put into 100 DEG C of baking ovens and done
Dry 2~3h, collects dried object；
（4）Dried object is put into calcining furnace, 790~860 DEG C are warming up to 6 DEG C/min, 1~2h is calcined, calcined material is collected, i.e.,
Iron oxide red can be obtained.
Example 1
The preparation of culture medium：Count by weight, take 85 parts of deionized waters, 26 parts of yeast extracts, 16 parts of peptones, 8 parts of chlorinations
Sodium, 6 parts of iron chloride, 1.1 parts of potassium dihydrogen phosphates and 1.0 parts of dipotassium hydrogen phosphates, stir, are put into autoclave sterilizer,
The sterilizing at 115 DEG C, you can obtain culture medium.
The preparation of bacterium solution：
A. bloodstone is placed in air humidity for 40%, temperature is standing in 32 DEG C of culturing room 5 days, place into pulverizer with
800r/min is crushed, and crosses 200 mesh sieves, collects sieving particle；
B. sieving particle is put into culture medium, addition is the 16% of culture medium quality, then culture medium is put into shaken cultivation
In case, design temperature is 32 DEG C, with 120rpm shaken cultivations 22h；
C. the iron oxide of sieving granular mass 5% and the granular mass 0.5% that sieves are added into culture medium after culture terminates
During Fiber differentiation, per 6h, sieving granular mass 1.0% is added into culture medium by 5-bromouracil, Fiber differentiation 13h
Iron oxide；
D. after Fiber differentiation terminates, culture medium is filtered using 100 mesh gauzes, filtrate is collected, you can bacterium solution is obtained.
The preparation of iron oxide red：
（1）Pyrite cinder is put into pulverizer, crushed with 500r/min, collect crushed material, by crushed material, bacterium solution and
Deionized water in mass ratio 1:5:1, it is put into container, at 32 DEG C, after 150r/min stirrings 5h, stands 6h, filter, collect
Filtrate；
（2）Filtrate is put into bruisher, 15min is smashed to pieces with 12000r/min, mixture is smashed in collection to pieces, to smashing to pieces in mixture
Iron powder is added until iron powder is not redissolved, then stops adding iron powder, progress suction filtration collects smoke filtrate；
（3）In mass ratio 1:6:3, dimethylformamide, smoke filtrate and ammonium hydrogen carbonate are put into container, at 55 DEG C, with 120r/
Min stirrings are until without Precipitation, then stand 2h, filter, and collect filter residue, and filter residue is put into 100 DEG C of baking ovens and dries 3h, collect
Dried object；
（4）Dried object is put into calcining furnace, 860 DEG C are warming up to 6 DEG C/min, 2h is calcined, calcined material is collected, you can must aoxidize
Iron oxide red.
Example 2
The preparation of culture medium：Count by weight, take 70 parts of deionized waters, 23 parts of yeast extracts, 10 parts of peptones, 5 parts of chlorinations
Sodium, 4 parts of iron chloride, 0.8 part of potassium dihydrogen phosphate and 0.7 part of dipotassium hydrogen phosphate, stir, are put into autoclave sterilizer,
The sterilizing at 115 DEG C, you can obtain culture medium.
The preparation of bacterium solution：
A. bloodstone is placed in air humidity for 35%, temperature is standing in 25 DEG C of culturing room 3 days, place into pulverizer with
800r/min is crushed, and crosses 200 mesh sieves, collects sieving particle；
B. sieving particle is put into culture medium, addition is the 13% of culture medium quality, then culture medium is put into shaken cultivation
In case, design temperature is 25 DEG C, with 120rpm shaken cultivations 20h；
C. the iron oxide of sieving granular mass 2% and the granular mass 0.2% that sieves are added into culture medium after culture terminates
During Fiber differentiation, per 4h, sieving granular mass 0.6% is added into culture medium by 5-bromouracil, Fiber differentiation 12h
Iron oxide；
D. after Fiber differentiation terminates, culture medium is filtered using 100 mesh gauzes, filtrate is collected, you can bacterium solution is obtained.
The preparation of iron oxide red：
（1）Pyrite cinder is put into pulverizer, crushed with 500r/min, collect crushed material, by crushed material, bacterium solution and
Deionized water in mass ratio 1:3:1, it is put into container, at 25 DEG C, after 150r/min stirrings 3h, stands 4h, filter, collect
Filtrate；
（2）Filtrate is put into bruisher, 10min is smashed to pieces with 12000r/min, mixture is smashed in collection to pieces, to smashing to pieces in mixture
Iron powder is added until iron powder is not redissolved, then stops adding iron powder, progress suction filtration collects smoke filtrate；
（3）In mass ratio 1:6:3, dimethylformamide, smoke filtrate and ammonium hydrogen carbonate are put into container, at 50 DEG C, with 120r/
Min stirrings are until without Precipitation, then stand 1h, filter, and collect filter residue, and filter residue is put into 100 DEG C of baking ovens and dries 2h, collect
Dried object；
（4）Dried object is put into calcining furnace, 790 DEG C are warming up to 6 DEG C/min, 1h is calcined, calcined material is collected, you can must aoxidize
Iron oxide red.
Example 3
The preparation of culture medium：Count by weight, take 80 parts of deionized waters, 24 parts of yeast extracts, 15 parts of peptones, 7 parts of chlorinations
Sodium, 5 parts of iron chloride, 0.9 part of potassium dihydrogen phosphate and 0.8 part of dipotassium hydrogen phosphate, stir, are put into autoclave sterilizer,
The sterilizing at 115 DEG C, you can obtain culture medium.
The preparation of bacterium solution：
A. bloodstone is placed in air humidity for 37%, temperature is standing in 30 DEG C of culturing room 4 days, place into pulverizer with
800r/min is crushed, and crosses 200 mesh sieves, collects sieving particle；
B. sieving particle is put into culture medium, addition is the 15% of culture medium quality, then culture medium is put into shaken cultivation
In case, design temperature is 31 DEG C, with 120rpm shaken cultivations 21h；
C. the iron oxide of sieving granular mass 3% and the granular mass 0.3% that sieves are added into culture medium after culture terminates
During Fiber differentiation, per 5h, sieving granular mass 0.7% is added into culture medium by 5-bromouracil, Fiber differentiation 12h
Iron oxide；
D. after Fiber differentiation terminates, culture medium is filtered using 100 mesh gauzes, filtrate is collected, you can bacterium solution is obtained.
The preparation of iron oxide red：
（1）Pyrite cinder is put into pulverizer, crushed with 500r/min, collect crushed material, by crushed material, bacterium solution and
Deionized water in mass ratio 1:4:1, it is put into container, at 30 DEG C, after 150r/min stirrings 4h, stands 5h, filter, collect
Filtrate；
（2）Filtrate is put into bruisher, 12min is smashed to pieces with 12000r/min, mixture is smashed in collection to pieces, to smashing to pieces in mixture
Iron powder is added until iron powder is not redissolved, then stops adding iron powder, progress suction filtration collects smoke filtrate；
（3）In mass ratio 1:6:3, dimethylformamide, smoke filtrate and ammonium hydrogen carbonate are put into container, at 52 DEG C, with 120r/
Min stirrings are until without Precipitation, then stand 2h, filter, and collect filter residue, and filter residue is put into 100 DEG C of baking ovens and dries 2h, collect
Dried object；
（4）Dried object is put into calcining furnace, 820 DEG C are warming up to 6 DEG C/min, 2h is forged, calcined material is collected, you can iron oxide is obtained
It is red.
Reference examples：The iron oxide red of Langfang City company production.
Iron oxide red to example 1 to example 3 and reference examples is detected.
Apparent density is detected using apparent density instrument.
Particle mean size is detected using laser particle analyzer.
Oil absorption and coloured light are detected according to GB 1863-2008 standards.
Testing result such as table 1.
Table 1
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Apparent density（g·cm-3） | 0.29 | 0.30 | 0.28 | 0.35 |
| Particle mean size（μm） | 0.8 | 0.9 | 0.7 | 1.5 |
| Coloured light（Compared with standard） | It is similar | It is similar | It is similar | It is similar |
| Oil absorption（g/100g） | 18.4 | 19.2 | 17.9 | 15 |
As shown in Table 1, dispersive property is good at normal temperatures for the iron oxide red that prepared by the present invention, does not occur agglomeration.
The iron oxide red of example 1 to example 3 and reference examples is placed after 45min at temperature is 370 DEG C, examined again
Survey, testing result such as table 2.
Table 2
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Apparent density（g·cm-3） | 0.27 | 0.29 | 0.25 | 0.29 |
| Particle mean size（μm） | 0.9 | 0.10 | 0.8 | 1.8 |
| Coloured light（Compared with standard sample） | It is similar | It is similar | It is similar | It is similar |
| Oil absorption（g/100g） | 18.7 | 19.8 | 18.1 | 19 |
Tables 1 and 2 data are contrasted, it is known that iron oxide red apparent density and particle mean size change prepared by the present invention is not
Greatly, still with preferable dispersive property.
Claims (6)
1. a kind of preparation method of iron oxide red, it is characterised in that the iron oxide red includes following preparation process：
（1）Pyrite cinder is crushed, crushed material is collected, crushed material, bacterium solution and deionized water are put into container and stirred,
Stand, filtrate is collected in filtering；
（2）Filtrate is put into bruisher and smashed to pieces, collection smash mixture to pieces, to smash to pieces in mixture add iron powder until iron powder not
It is redissolved, then stops adding iron powder, carries out suction filtration, collect smoke filtrate；
（3）Dimethylformamide, smoke filtrate and ammonium hydrogen carbonate are put into container stirring until without Precipitation, then stood, is filtered,
Filter residue is collected, by filter residue and drying, dried object is collected；
（4）Dried object is calcined, calcined material is collected, you can iron oxide red is obtained.
2. the preparation method of iron oxide red according to claim 1, it is characterised in that the crushed material, bacterium solution and go from
The mass ratio of sub- water is 1:3:1~1:5:1.
3. the preparation method of iron oxide red according to claim 1, it is characterised in that the triethanolamine, smoke filtrate and
The mass ratio 1 of ammonium hydrogen carbonate:6:3.
4. the preparation method of iron oxide red according to claim 1, it is characterised in that the calcination process be with 6 DEG C/
Min is warming up to 790~860 DEG C, calcines 1~2h, you can.
5. the preparation method of iron oxide red according to claim 1, it is characterised in that the preparation of the bacterium solution includes as follows
Preparation process：
A. it is 35~40% bloodstone to be placed in into air humidity, and temperature is to stand 3~5 days in 25~32 DEG C of culturing room, then is entered
Row is crushed, and crosses 200 mesh sieves, collects sieving particle；
B. sieving particle is put into culture medium, addition is the 13~16% of culture medium quality, then culture medium is put into vibration
In incubator, design temperature is 25~32 DEG C, 20~22h of shaken cultivation；
C. culture terminate after into culture medium add sieving granular mass 2~5% iron oxide and sieving granular mass 0.2~
0.5% 5-bromouracil, 12~13h of Fiber differentiation, during Fiber differentiation, every 4~6h adds sieving into culture medium
The iron oxide of granular mass 0.6~1.0%；
D. after Fiber differentiation terminates, culture medium is filtered using 100 mesh gauzes, filtrate is collected, you can bacterium solution is obtained.
6. the preparation method of iron oxide red according to claim 5, it is characterised in that the system of culture medium in the step b
It is standby to be：Count by weight, take 70~85 parts of deionized waters, 23~26 parts of yeast extracts, 10~16 parts of peptones, 5~8 parts of chlorine
Change sodium, 4~6 parts of iron chloride, 0.8~1.1 part of potassium dihydrogen phosphate and 0.7~1.0 part of dipotassium hydrogen phosphate, stir, sterilization disappears
Poison, you can obtain culture medium.
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