CN107244698B - 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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- CN107244698B CN107244698B CN201710460469.7A CN201710460469A CN107244698B CN 107244698 B CN107244698 B CN 107244698B CN 201710460469 A CN201710460469 A CN 201710460469A CN 107244698 B CN107244698 B CN 107244698B
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- iron oxide
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- oxide red
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 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 25
- 239000000463 material Substances 0.000 claims abstract description 22
- 239000000779 smoke Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000203 mixture Substances 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 9
- 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
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000001963 growth medium Substances 0.000 claims description 49
- 238000007873 sieving Methods 0.000 claims description 28
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 27
- 239000002245 particle Substances 0.000 claims description 20
- 230000004069 differentiation Effects 0.000 claims description 18
- 239000000835 fiber Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 11
- 238000003756 stirring 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
- 239000011780 sodium chloride Substances 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
- 230000010355 oscillation Effects 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 abstract description 6
- 239000000843 powder Substances 0.000 abstract description 5
- 239000000049 pigment Substances 0.000 abstract description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 abstract 1
- 229960005191 ferric oxide Drugs 0.000 description 44
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 43
- 239000002351 wastewater Substances 0.000 description 8
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 229910001448 ferrous ion Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 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
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 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
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 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
- 239000002585 base Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 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
- 238000000354 decomposition reaction Methods 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
- 150000002431 hydrogen Chemical class 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
- 230000002906 microbiologic effect Effects 0.000 description 1
- 244000005700 microbiome Species 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
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 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 methods of iron oxide red, belong to powder pigment technical field.The present invention crushes pyrite cinder, collects crushed material, crushed material, bacterium solution and deionized water are put into container and stirred, and stands, and filtrate is collected in filtering；Put the filtrate into bruisher and smash to pieces, collection smash mixture to pieces, to smash to pieces in mixture be added iron powder until iron powder be not redissolved, then stop be added iron powder, filtered, collect smoke filtrate；Triethanolamine, smoke filtrate and ammonium hydrogen carbonate are put into container and stirred up to no Precipitation, then is stood, is filtered, filter residue is collected, by filter residue and drying, collects dried object；Dried object is calcined, calcined material is collected, iron oxide red can be obtained.The iron oxide red that the present invention is prepared is not susceptible to reunite under high temperature environment, and dispersion performance is good, has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of iron oxide red, belong to powder pigment technical field.
Background technique
Iron oxide red has natural and artificial two kinds.Natural title is western red, is substantially pure iron oxide, for red
Powder.Due to the difference of production method and operating condition, their crystal structure and physical behavior has very big difference, color
It changes 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), when calcination, releases oxygen, can be by hydrogen and-carbonoxide also
Former Cheng Tie, it is not soluble in water, it 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, and oil-free infiltration property and water infiltration property, nontoxic, highest is allowed dense in air
Degree is 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 process two, raw using wet process
During producing iron oxide red, acid waste water largely containing ferrous ion can be generated, ferrous matter in waste water
Measuring score is 0.1~0.3%, and the source of waste water is mainly the water after isolating finished product iron oxide red in reaction container
The waste water that solution and washing iron oxide red generate, this wastewater pH is 3~4, and contains a large amount of ferrous ion, it is necessary at
Reason could qualified discharge.And roasting method is mainly green vitriol roasting method in dry method, and oxidation is made by high-temperature calcination in ferrous sulfate
Iron oxide red.Production technology calcination generates sulfur monoxide and sulfur dioxide, seriously pollutes environment, is only suitable for small-scale production.It removes
Other than this, there are also iron oxide yellows, iron black calcination method, which is simple and convenient to operate, but crystal group is easily caused by high temperature
Poly- and bad dispersibility.
It would therefore be highly desirable to generation will not be generated when preparing iron oxide red largely containing the acid waste water of ferrous ion by finding,
And the iron oxide red being prepared has preferable dispersion performance, preparation method not easy to reunite under the high temperature conditions.
Summary of the invention
The technical problems to be solved by the invention: big for that can be generated when preparing iron oxide red currently with dry and wet
The acid waste water containing ferrous ion of amount, and the iron oxide red being prepared easily causes crystal to be reunited under the high temperature conditions, causes
The problem of bad dispersibility, provides a kind of preparation method of iron oxide red.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of preparation method of iron oxide red, which is characterized in that the iron oxide red includes following preparation step:
(1) pyrite cinder is crushed, collects crushed material, crushed material, bacterium solution and deionized water is put into container
Stirring is stood, and filtrate is collected in filtering；
(2) it puts the filtrate into bruisher and smashs to pieces, mixture is smashed in collection to pieces, and iron powder is added in mixture until iron to smashing to pieces
Powder is not redissolved, then stops that iron powder is added, and is filtered, collects smoke filtrate；
(3) dimethylformamide, smoke filtrate and ammonium hydrogen carbonate are put into container and are stirred up to no Precipitation, then stood,
Filter residue is collected in filtering, by filter residue and drying, collects dried object；
(4) dried object is calcined, collects calcined material, iron oxide red can be obtained.
The mass ratio of the crushed material, bacterium solution and deionized water is 1:3:1~1:5:1.
The mass ratio 1:6:3 of the dimethylformamide, smoke filtrate and ammonium hydrogen carbonate.
The calcination process is that 790~860 DEG C are warming up to 6 DEG C/min, calcines 1~2h.
The preparation of the bacterium solution includes following preparation step:
A. bloodstone is placed in air humidity is 35~40%, stands 3~5 days in the culturing room that temperature is 25~32 DEG C,
It is crushed again, crosses 200 meshes, collect sieving particle；
B. sieving particle is put into culture medium, additional amount is the 13~16% of culture medium quality, then culture medium is put into
In shaken cultivation case, set temperature is 25~32 DEG C, 20~22h of shaken cultivation；
C. the iron oxide and sieving granular mass of sieving granular mass 2~5% is added into culture medium after culture terminates
0.2~0.5% 5-bromouracil, 12~13h of Fiber differentiation, during Fiber differentiation, every 4~6h adds into culture medium
Enter to be sieved the iron oxide of granular mass 0.6~1.0%；
D. after Fiber differentiation, culture medium is filtered using 100 mesh gauzes, filtrate is collected, bacterium solution can be obtained.
The preparation of culture medium in the step b are as follows: according to parts 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 evenly, sterilizing, can obtain culture medium.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention carries out microorganism using the high bloodstone of iron oxide content as bacterium source first in control environment
Culture, by culture medium culture propagation, during culture propagation, uses 5-bromouracil as mutagens, with iron compound
As inducement, dominant bacteria cultivation is carried out, is obtained containing the bacterium solution for biting iron dominant bacteria；
(2) present invention carries out microbiological treatment to pyrite cinder by bacterium solution, has decomposed ferro element in pyrite cinder,
The solution containing iron ion is formed, the generation of acid waste water is avoided, re-forms in precipitation process, utilize dimethylformamide and carbon
Sour hydrogen ammonium is modified it, avoids the generation of the intergranular agglomeration in calcining temperature-rise period, reducing the later period forges
When burning between crystal agglomeration generation, improve the dispersion performance of iron oxide red.
Specific embodiment
The preparation of culture medium: according to parts by weight, 70~85 parts of deionized waters, 23~26 parts of yeast extracts, 10~16 are taken
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 evenly, and is put into autoclave sterilizer, and the sterilizing at 115 DEG C can obtain culture medium.
The preparation of bacterium solution:
A. bloodstone is placed in air humidity is 35~40%, stands 3~5 days in the culturing room that temperature is 25~32 DEG C,
It places into pulverizer and is crushed with 800r/min, cross 200 meshes, collect sieving particle；
B. sieving particle is put into culture medium, additional amount is the 13~16% of culture medium quality, then culture medium is put into
In shaken cultivation case, set temperature is 25~32 DEG C, with 20~22h of 120rpm shaken cultivation；
C. the iron oxide and sieving granular mass of sieving granular mass 2~5% is added into culture medium after culture terminates
0.2~0.5% 5-bromouracil, 12~13h of Fiber differentiation, during Fiber differentiation, every 4~6h adds into culture medium
Enter to be sieved the iron oxide of granular mass 0.6~1.0%；
D. after Fiber differentiation, culture medium is filtered using 100 mesh gauzes, filtrate is collected, bacterium solution can be obtained.
The preparation of iron oxide red:
(1) pyrite cinder is put into pulverizer, is crushed with 500r/min, crushed material is collected, by crushed material, bacterium
Liquid and deionized water 1:3:1~1:5:1 in mass ratio, are put into container, at 25~32 DEG C, stir 3~5h with 150r/min
Afterwards, 4~6h is stood, filtrate is collected in filtering；
(2) it puts the filtrate into bruisher, 10~15min is smashed to pieces with 12000r/min, mixture is smashed in collection to pieces, to smashing to pieces
In mixture be added iron powder until iron powder be not redissolved, then stop be added iron powder, filtered, collect smoke filtrate；
(3) dimethylformamide, smoke filtrate and ammonium hydrogen carbonate are put into container by 1:6:3 in mass ratio, at 50~55 DEG C
Under, it is stirred with 120r/min up to no Precipitation, then stand 1~2h, is filtered, collected filter residue, filter residue is put into 100 DEG C of baking ovens
Middle 2~3h of drying collects dried object；
(4) dried object is put into calcining furnace, is warming up to 790~860 DEG C with 6 DEG C/min, calcines 1~2h, collects calcining
Object can obtain iron oxide red.
Example 1
The preparation of culture medium: according to parts by weight, 85 parts of deionized waters, 26 parts of yeast extracts, 16 parts of peptones, 8 parts are taken
Sodium chloride, 6 parts of iron chloride, 1.1 parts of potassium dihydrogen phosphates and 1.0 parts of dipotassium hydrogen phosphates, stir evenly, are put into autoclave sterilizer
In, the sterilizing at 115 DEG C can obtain culture medium.
The preparation of bacterium solution:
A. bloodstone is placed in air humidity is 40%, stands 5 days in the culturing room that temperature is 32 DEG C, places into pulverizer
In crushed with 800r/min, cross 200 meshes, collect sieving particle；
B. sieving particle is put into culture medium, additional amount is the 16% of culture medium quality, then culture medium is put into oscillation
In incubator, set temperature is 32 DEG C, with 120rpm shaken cultivation 22h；
C. the iron oxide and sieving granular mass of sieving granular mass 5% is added into culture medium after culture terminates
0.5% 5-bromouracil, Fiber differentiation 13h, during Fiber differentiation, sieving particle matter is added into culture medium by every 6h
The iron oxide of amount 1.0%；
D. after Fiber differentiation, culture medium is filtered using 100 mesh gauzes, filtrate is collected, bacterium solution can be obtained.
The preparation of iron oxide red:
(1) pyrite cinder is put into pulverizer, is crushed with 500r/min, crushed material is collected, by crushed material, bacterium
Liquid and deionized water 1:5:1 in mass ratio, are put into container, at 32 DEG C, after stirring 5h with 150r/min, stand 6h, filter,
Collect filtrate；
(2) it puts the filtrate into bruisher, 15min is smashed to pieces with 12000r/min, mixture is smashed in collection to pieces, is mixed to smashing to pieces
In object be added iron powder until iron powder be not redissolved, then stop be added iron powder, filtered, collect smoke filtrate；
(3) dimethylformamide, smoke filtrate and ammonium hydrogen carbonate are put into container by 1:6:3 in mass ratio, at 55 DEG C, with
120r/min is stirred up to no Precipitation, then stands 2h, is filtered, and filter residue is collected, and filter residue is put into 100 DEG C of baking ovens dry
3h collects dried object；
(4) dried object is put into calcining furnace, is warming up to 860 DEG C with 6 DEG C/min, calcines 2h, collects calcined material, can obtain
Iron oxide red.
Example 2
The preparation of culture medium: according to parts by weight, 70 parts of deionized waters, 23 parts of yeast extracts, 10 parts of peptones, 5 parts are taken
Sodium chloride, 4 parts of iron chloride, 0.8 part of potassium dihydrogen phosphate and 0.7 part of dipotassium hydrogen phosphate, stir evenly, are put into autoclave sterilizer
In, the sterilizing at 115 DEG C can obtain culture medium.
The preparation of bacterium solution:
A. bloodstone is placed in air humidity is 35%, stands 3 days in the culturing room that temperature is 25 DEG C, places into pulverizer
In crushed with 800r/min, cross 200 meshes, collect sieving particle；
B. sieving particle is put into culture medium, additional amount is the 13% of culture medium quality, then culture medium is put into oscillation
In incubator, set temperature is 25 DEG C, with 120rpm shaken cultivation 20h；
C. the iron oxide and sieving granular mass of sieving granular mass 2% is added into culture medium after culture terminates
0.2% 5-bromouracil, Fiber differentiation 12h, during Fiber differentiation, sieving particle matter is added into culture medium by every 4h
The iron oxide of amount 0.6%；
D. after Fiber differentiation, culture medium is filtered using 100 mesh gauzes, filtrate is collected, bacterium solution can be obtained.
The preparation of iron oxide red:
(1) pyrite cinder is put into pulverizer, is crushed with 500r/min, crushed material is collected, by crushed material, bacterium
Liquid and deionized water 1:3:1 in mass ratio, are put into container, at 25 DEG C, after stirring 3h with 150r/min, stand 4h, filter,
Collect filtrate；
(2) it puts the filtrate into bruisher, 10min is smashed to pieces with 12000r/min, mixture is smashed in collection to pieces, is mixed to smashing to pieces
In object be added iron powder until iron powder be not redissolved, then stop be added iron powder, filtered, collect smoke filtrate；
(3) dimethylformamide, smoke filtrate and ammonium hydrogen carbonate are put into container by 1:6:3 in mass ratio, at 50 DEG C, with
120r/min is stirred up to no Precipitation, then stands 1h, is filtered, and filter residue is collected, and filter residue is put into 100 DEG C of baking ovens dry
2h collects dried object；
(4) dried object is put into calcining furnace, is warming up to 790 DEG C with 6 DEG C/min, calcines 1h, collects calcined material, can obtain
Iron oxide red.
Example 3
The preparation of culture medium: according to parts by weight, 80 parts of deionized waters, 24 parts of yeast extracts, 15 parts of peptones, 7 parts are taken
Sodium chloride, 5 parts of iron chloride, 0.9 part of potassium dihydrogen phosphate and 0.8 part of dipotassium hydrogen phosphate, stir evenly, are put into autoclave sterilizer
In, the sterilizing at 115 DEG C can obtain culture medium.
The preparation of bacterium solution:
A. bloodstone is placed in air humidity is 37%, stands 4 days in the culturing room that temperature is 30 DEG C, places into pulverizer
In crushed with 800r/min, cross 200 meshes, collect sieving particle；
B. sieving particle is put into culture medium, additional amount is the 15% of culture medium quality, then culture medium is put into oscillation
In incubator, set temperature is 31 DEG C, with 120rpm shaken cultivation 21h；
C. the iron oxide and sieving granular mass of sieving granular mass 3% is added into culture medium after culture terminates
0.3% 5-bromouracil, Fiber differentiation 12h, during Fiber differentiation, sieving particle matter is added into culture medium by every 5h
The iron oxide of amount 0.7%；
D. after Fiber differentiation, culture medium is filtered using 100 mesh gauzes, filtrate is collected, bacterium solution can be obtained.
The preparation of iron oxide red:
(1) pyrite cinder is put into pulverizer, is crushed with 500r/min, crushed material is collected, by crushed material, bacterium
Liquid and deionized water 1:4:1 in mass ratio, are put into container, at 30 DEG C, after stirring 4h with 150r/min, stand 5h, filter,
Collect filtrate；
(2) it puts the filtrate into bruisher, 12min is smashed to pieces with 12000r/min, mixture is smashed in collection to pieces, is mixed to smashing to pieces
In object be added iron powder until iron powder be not redissolved, then stop be added iron powder, filtered, collect smoke filtrate；
(3) dimethylformamide, smoke filtrate and ammonium hydrogen carbonate are put into container by 1:6:3 in mass ratio, at 52 DEG C, with
120r/min is stirred up to no Precipitation, then stands 2h, is filtered, and filter residue is collected, and filter residue is put into 100 DEG C of baking ovens dry
2h collects dried object；
(4) dried object is put into calcining furnace, is warming up to 820 DEG C with 6 DEG C/min, forge 2h, collected calcined material, oxygen can be obtained
Change iron oxide red.
Reference examples: the iron oxide red of Langfang City company production.
The iron oxide red of example 1 to example 3 and reference examples is detected.
Apparent density is detected using apparent density instrument.
Average particle size is detected using laser particle analyzer.
Oil absorption and coloured light are detected according to GB 1863-2008 standard.
Testing result such as table 1.
Table 1
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Apparent density (gcm-3) | 0.29 | 0.30 | 0.28 | 0.35 |
| Average particle 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, dispersion performance is good at normal temperature for iron oxide red prepared by the present invention, does not occur agglomeration.
By example 1 to the iron oxide red of example 3 and reference examples after temperature is to place 45min at 370 DEG C, examined again
It surveys, testing result such as table 2.
Table 2
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Apparent density (gcm-3) | 0.27 | 0.29 | 0.25 | 0.29 |
| Average particle 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 compared, it is known that iron oxide red apparent density and average particle size variation prepared by the present invention
Less, still there is preferable dispersion performance.
Claims (4)
1. a kind of preparation method of iron oxide red, which is characterized in that the iron oxide red includes following preparation step:
(1) pyrite cinder is crushed, collects crushed material, crushed material, bacterium solution and deionized water is put into container and stirred,
It stands, filtrate is collected in filtering；The preparation of the bacterium solution includes following preparation step:
A. bloodstone is placed in air humidity is 35~40%, stands 3~5 days in the culturing room that temperature is 25~32 DEG C, then into
Row crushes, and crosses 200 meshes, collects sieving particle；
B. sieving particle is put into culture medium, additional amount is the 13~16% of culture medium quality, then culture medium is put into oscillation
In incubator, set temperature is 25~32 DEG C, 20~22h of shaken cultivation；The preparation of the culture medium are as follows: according to parts by weight,
Take 70~85 parts of deionized waters, 23~26 parts of yeast extracts, 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 part of dipotassium hydrogen phosphate, stir evenly, sterilizing, can obtain culture medium；
C. culture terminate after into culture medium be added 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, sieving is added into culture medium by every 4~6h
The iron oxide of granular mass 0.6~1.0%；
D. after Fiber differentiation, culture medium is filtered using 100 mesh gauzes, filtrate is collected, bacterium solution can be obtained；
(2) put the filtrate into bruisher and smash to pieces, collection smash mixture to pieces, to smash to pieces in mixture be added iron powder until iron powder not
It is redissolved, then stops that iron powder is added, filtered, collect smoke filtrate；
(3) dimethylformamide, smoke filtrate and ammonium hydrogen carbonate are put into container and are stirred up to no Precipitation, then stood, filtered,
Filter residue is collected, by filter residue and drying, collects dried object；
(4) dried object is calcined, collects calcined material, iron oxide red can be obtained.
2. the preparation method of iron oxide red according to claim 1, which is characterized 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, which is characterized in that the dimethylformamide, smoke filtrate
With the mass ratio 1:6:3 of ammonium hydrogen carbonate.
4. the preparation method of iron oxide red according to claim 1, which is characterized in that the calcination process be with 6 DEG C/
Min is warming up to 790~860 DEG C, calcines 1~2h.
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