CN110255624B - Method for controlling viscosity of iron oxide yellow by buffer system - Google Patents
Method for controlling viscosity of iron oxide yellow by buffer system Download PDFInfo
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- CN110255624B CN110255624B CN201910589805.7A CN201910589805A CN110255624B CN 110255624 B CN110255624 B CN 110255624B CN 201910589805 A CN201910589805 A CN 201910589805A CN 110255624 B CN110255624 B CN 110255624B
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- sodium hydroxide
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000007853 buffer solution Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims description 12
- 239000013078 crystal Substances 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 29
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 29
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 29
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims description 134
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 87
- 239000000243 solution Substances 0.000 claims description 44
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 23
- 230000035484 reaction time Effects 0.000 claims description 19
- 238000007254 oxidation reaction Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 11
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 claims description 11
- 238000010790 dilution Methods 0.000 claims description 10
- 239000012895 dilution Substances 0.000 claims description 10
- 230000003647 oxidation Effects 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 10
- 239000010935 stainless steel Substances 0.000 claims description 10
- 230000001502 supplementing effect Effects 0.000 claims description 10
- QTYWBJZOZDYCGB-UHFFFAOYSA-L potassium;sodium;2-carboxybenzoate;hydroxide Chemical compound [OH-].[Na+].[K+].OC(=O)C1=CC=CC=C1C([O-])=O QTYWBJZOZDYCGB-UHFFFAOYSA-L 0.000 claims description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims 3
- 241000209094 Oryza Species 0.000 claims 2
- 235000007164 Oryza sativa Nutrition 0.000 claims 2
- 235000009566 rice Nutrition 0.000 claims 2
- 239000002245 particle Substances 0.000 abstract description 20
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 239000003513 alkali Substances 0.000 abstract description 5
- 235000011121 sodium hydroxide Nutrition 0.000 description 15
- 238000000227 grinding Methods 0.000 description 11
- 239000003153 chemical reaction reagent Substances 0.000 description 10
- 238000000576 coating method Methods 0.000 description 10
- 239000000049 pigment Substances 0.000 description 10
- 238000003860 storage Methods 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 7
- 239000001034 iron oxide pigment Substances 0.000 description 7
- 238000000967 suction filtration Methods 0.000 description 7
- 239000001052 yellow pigment Substances 0.000 description 7
- 238000007599 discharging Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000872 buffer Substances 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000002585 base Substances 0.000 description 2
- IBUIVNCCBFLEJL-UHFFFAOYSA-M sodium;phosphoric acid;chloride Chemical compound [Na+].[Cl-].OP(O)(O)=O IBUIVNCCBFLEJL-UHFFFAOYSA-M 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- XPFJYKARVSSRHE-UHFFFAOYSA-K trisodium;2-hydroxypropane-1,2,3-tricarboxylate;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound [Na+].[Na+].[Na+].OC(=O)CC(O)(C(O)=O)CC(O)=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O XPFJYKARVSSRHE-UHFFFAOYSA-K 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 229910014314 BYK190 Inorganic materials 0.000 description 1
- 229910002588 FeOOH Inorganic materials 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000010242 baoji Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- -1 coatings Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000012858 packaging process Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- 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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/22—Compounds of iron
- C09C1/24—Oxides of iron
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention relates to a novel method for producing low-viscosity iron oxide yellow in a buffer system, which adopts seed crystals to oxidize in the buffer system, stabilizes the pH condition without generating violent pH change due to the impact of ferrous sulfate and liquid alkali, and enables the seed crystals to grow under the condition of stable pH, so that the iron oxide yellow particles can grow more uniformly on one hand, and the iron oxide yellow particles growing in a relatively stable pH environment are not easy to generate bifurcation, the surfaces of the particles are smoother, the length-diameter ratio is reduced, and the viscosity is as low as 36Ku on the other hand.
Description
Technical Field
The invention relates to a low-viscosity iron oxide yellow pigment, in particular to a method for preparing low-viscosity iron oxide yellow in a buffer system by controlling reaction.
Background
The iron oxide yellow is also called as iron oxyhydroxide, has a molecular formula of FeOOH or Fe2O3 & H2O, is yellow powder, has needle-shaped particle shape, has higher tinting strength and covering power, is non-toxic and harmless, is an environment-friendly inorganic pigment, and has the light resistance reaching 6-7 grade. The iron oxide yellow pigment is widely applied to industries such as building materials, coatings, paints, plastics, rubbers, electronics, industrial catalysts, tobacco, cosmetics and the like.
The common iron oxide yellow has higher viscosity due to different surface charge distribution and particle morphology, and has more limitations in the coating application field. Compared with other axial crystal systems, such as the spherical iron oxide black of the iron oxide red is cubic, the iron oxide yellow is of a needle-shaped structure and has a large length-diameter ratio. Yellow iron oxide is therefore very resistant to flow and therefore has the greatest viscosity in most media coating systems, and is also a great problem in the coatings and paints sector.
The rheological properties of the coating are strictly required from production to storage, from application to film formation, and in these stages, the viscosity or the flow resistance is a key technical indicator of the coating due to the different concentrations of the pigments and the different shear and pressure forces to which the coating is subjected, and in the high shear grinding stage, in order to maximize the pigment content in the grinding base and to maximize the production efficiency, a lower viscosity of the grinding base is desired, and a lower viscosity is also desired during the mixing, transferring and packaging processes of the coating.
All components of the coating have a certain effect on viscosity, and the need to select the appropriate pigment to achieve the desired viscosity characteristics is a critical factor. At present, organic matters with high solid content and low volatility are important development objects of the coating industry, the solid content is determined by the viscosity of the pigment, and the paint has overhigh flow resistance and is extremely unfavorable for production due to overhigh viscosity of the pigment.
At present, relevant literature reports at home and abroad show that the viscosity of iron oxide yellow can be improved by changing the surface charge of the iron oxide yellow particles or reducing the length-diameter ratio of the iron oxide yellow particles, and a patent of 'a low-viscosity iron oxide yellow pigment' published by Zhejiang union pigment at home, which is an application number 201410767118.7, is a low-viscosity iron oxide yellow pigment, and the principle of the method is that the shape of part of iron oxide yellow pigment particles is destroyed by steel ball grinding, but the length-diameter ratio of all iron oxide yellow particles cannot be reduced on the whole, the viscosity of the pigment is reduced to a certain extent, but the effect is not obvious enough, and the hue of the pigment is changed; the Nantong Baoji pigment company published with a patent number ZL201310277999.X 'a method for reducing the viscosity of iron oxide yellow pigment' patent is that the viscosity of iron oxide yellow is improved by changing the charges on the surfaces of iron oxide yellow particles, the effect is ideal, but the improvement space is still provided; the 'low-viscosity iron oxide yellow' patent of Zhejiang Huayuan pigment application No. ZL201610596145.1 has certain effect of reducing the viscosity of the iron oxide yellow through high-pressure reaction and system temperature control, but the high-pressure reaction has high dangerous system degree and large energy consumption.
Disclosure of Invention
The invention aims to provide a novel method for producing low-viscosity iron oxide yellow in a buffer system, which adopts seed crystals to oxidize in the buffer system, stabilizes the pH condition without generating violent pH change due to the impact of ferrous sulfate and liquid alkali, and enables the seed crystals to grow under the relatively stably changed pH condition, so that the iron oxide yellow particles can grow more uniformly on one hand, and the iron oxide yellow particles growing in the relatively stable pH environment are not easy to generate bifurcation, the particle surfaces are smoother, the length-diameter ratio is controlled better, and the viscosity is reduced.
In order to achieve the purpose, the scheme adopts the following experimental scheme:
a method for controlling the viscosity of iron oxide yellow by a buffer system comprises the following steps:
1) preparing seed crystals:
adding 2-3 mol/L sodium hydroxide solution into 1-2 mol/L ferrous sulfate solution, controlling the reaction temperature at 25-35 ℃ and the reaction time at 14-17h, introducing air to the bottom of the reaction solution, and controlling the air amount at 200m3/h～500m3/h；
2) Adding a buffer system for oxidation:
a: controlling the content of the ferrous in the reaction barrel to be between 1.34 and 1.52 mol/L;
b: continuously introducing air, and controlling the air quantity at 250m3/h～350m3Heating to 60-65 ℃, and stopping heating:
c: continuously adding the buffer solution into the reaction barrel; adding a sodium hydroxide solution with the concentration of 2-3 mol/L, stopping adding the sodium hydroxide solution when the pH value reaches 4.0 +/-0.3, and reacting at the temperature of 80-88 ℃;
d: when the ferrous content is lower than 1.0mol/L, supplementing ferrous sulfate, and controlling the reaction content to be about 1.0mol/L by adopting a mode of multiple small amount operation;
3) post-treatment: after the reaction reaches the specified time, a valve of the reaction kettle is opened, the feed liquid is discharged, and the finished product is obtained after the feed liquid is filtered, rinsed, dried and ultrafine crushed.
In some preferred embodiments of the present invention, the buffer solution is potassium hydrogen phthalate-sodium hydroxide, sodium dihydrogen phosphate-hydrochloric acid buffer, or citric acid-sodium citrate; in some more preferred embodiments of the present invention, the buffer solution is potassium hydrogen phthalate-sodium hydroxide; in some further preferred embodiments of the present invention, the molar ratio of the potassium hydrogen phthalate to the sodium hydroxide in the potassium hydrogen phthalate-sodium hydroxide buffer solution is 1:80 to 1: 30; preferably, the molar ratio of the potassium hydrogen phthalate to the sodium hydroxide is 1: 50-1: 30.
In some preferred embodiments of the present invention, in the step 2) a, a certain amount of water is added for dilution, and the ferrous content is controlled to be between 1.34mol/L and 1.52 mol/L.
In some preferred embodiments of the invention, 50m is used3Adding 1.5mol/L ferrous sulfate solution into a stainless steel reaction barrel, and adding 2.5mol/L sodium hydroxide solution 7m3Simultaneously controlling the reaction temperature to be 30 ℃; controlling the total reaction time to be 15h, introducing air to the bottom of the reaction solution in the first 5-7 h, and controlling the air amount to be 230m3The air is introduced into the bottom of the reaction solution for 7 to 10 hours later, and the air quantity is controlled to be 460m3/h。
The method provided by the invention adopts the seed crystal to oxidize in a buffer system, the pH condition is stabilized without violent pH change caused by the impact of ferrous sulfate and liquid alkali, and the seed crystal is grown under the condition of stable pH, so that on one hand, the growth of ferrite yellow particles is more uniform, on the other hand, the ferrite yellow particles grown in a relatively stable pH environment are not easy to generate bifurcation, the particle surface is smoother, the length-diameter ratio is reduced, and the viscosity is as low as 36 Ku.
Drawings
Fig. 1 is a schematic structural diagram of a reaction barrel provided by the present invention.
Detailed Description
The reaction barrel used in the following embodiment has a reaction structure as shown in fig. 1, and as shown in fig. 1, the reaction barrel includes an open barrel body 1, and a ferrous sulfate pipeline 2, a liquid alkali pipeline (buffer solution pipeline) 3, a steam pipe 4 and a water pipe 5 which are led into the barrel body, and a ferrous sulfate solution is added into the barrel body through the ferrous sulfate pipeline; adding a sodium hydroxide solution into the barrel body through a liquid caustic soda pipeline; the reaction liquid in the barrel body can be heated by steam through a steam pipe; the ferrous content can be diluted by adding water through the water pipe; an air pipe 6 is also introduced into the bottom of the barrel body 1, and the air pipe 6 is provided with an air flow meter 7 so as to effectively control the air amount entering the reaction night.
Preparing a buffer solution:
group A is sodium hydroxide solution without adding potassium hydrogen phthalate;
group B is potassium hydrogen phthalate and sodium hydroxide 1:30 of a buffer solution;
group C is potassium hydrogen phthalate and sodium hydroxide 1: 40 of a buffer solution;
group D is potassium hydrogen phthalate and sodium hydroxide 1:50 of a buffer solution;
group E is potassium hydrogen phthalate and sodium hydroxide 1: 60 of a buffer solution;
group F is potassium hydrogen phthalate and sodium hydroxide 1:80 of a buffer solution;
group G is 1:50 sodium dihydrogen phosphate-hydrochloric acid buffer solution;
group H was 1:50 citric acid-sodium citrate buffer.
Example 1
1) Seed crystal preparation:
a: preparing raw materials: 50m3Adding 1.5mol/L ferrous sulfate solution into a stainless steel reaction barrel, and adding into the reaction barrel with the volume of 7m3Sodium hydroxide solution with the concentration of 2.5mol/L, and simultaneously controlling the reaction temperature to be 25-35 ℃;
b: and (3) air volume control: controlling the total reaction time to be 14-17h, introducing air to the bottom of the reaction solution in the first 5-7 h, and controlling the air amount to be 230m3The air quantity is controlled to be 460m after 7-10h3H is used as the reference value. The final reaction material is used as a seed crystal for independent storage;
2) adding a buffer system for oxidation:
a: putting the prepared seed crystal into a reaction barrel, adding a certain amount of water for dilution, and controlling the ferrous content to be between 1.34mol/L and 1.52 mol/L;
b: introducing air into the feed liquid of the six groups of reaction barrels from the bottom, and controlling the air flow to be 300m3And h, simultaneously opening a steam valve to heat, and stopping heating when the temperature reaches 62 +/-2 ℃.
C: and after the temperature is stable, adding the buffer solution B group into a reaction barrel for reaction, stopping adding the reagent when the pH value reaches 4.0 +/-0.3, and then controlling the reaction temperature to be between 80 and 88 ℃ for oxidation reaction.
D: when the ferrous content is lower than 1.0mol/L, supplementing ferrous sulfate, and controlling the reaction content to be about 1.0mol/L by adopting a mode of multiple small amount operation;
3) post-treatment:
a: after the reaction reaches the specified time (the reaction time of the iron oxide pigment production is controlled according to the color requirement of the standard sample), opening a valve of the reaction barrel, discharging the feed liquid, and carrying out suction filtration, rinsing, drying and ultrafine grinding on the feed liquid to obtain the finished product.
Example 2
1) Seed crystal preparation:
a: preparing raw materials: 50m3Adding 1.5mol/L ferrous sulfate solution into a stainless steel reaction barrel, and adding into the reaction barrel with the volume of 7m3Sodium hydroxide solution with the concentration of 2.5mol/L, and simultaneously controlling the reaction temperature to be 25-35 ℃;
b: and (3) air volume control: controlling the total reaction time to be 14-17h, introducing air to the bottom of the reaction solution in the first 5-7 h, and controlling the air amount to be 230m3The air quantity is controlled to be 460m after 7-10h3H is used as the reference value. The final reaction material is used as a seed crystal for independent storage;
2) adding a buffer system for oxidation:
a: putting the prepared seed crystal into a reaction barrel, adding a certain amount of water for dilution, and controlling the ferrous content to be between 1.34mol/L and 1.52 mol/L;
b: introducing air into the feed liquid of the six groups of reaction barrels from the bottom, and controlling the air flow to be 300m3And h, simultaneously opening a steam valve to heat, and stopping heating when the temperature reaches 62 +/-2 ℃.
C: and after the temperature is stable, adding the buffer solution C group into a reaction barrel for reaction, stopping adding the reagent when the pH value reaches 4.0 +/-0.3, and then controlling the reaction temperature between 80 and 88 ℃ for oxidation reaction.
D: when the ferrous content is lower than 1.0mol/L, supplementing ferrous sulfate, and controlling the reaction content to be about 1.0mol/L by adopting a mode of multiple small amount operation;
3) post-treatment:
a: after the reaction reaches the specified time (the reaction time of the iron oxide pigment production is controlled according to the color requirement of the standard sample), opening a valve of the reaction barrel, discharging the feed liquid, and carrying out suction filtration, rinsing, drying and ultrafine grinding on the feed liquid to obtain the finished product.
Example 3
1) Seed crystal preparation:
a: preparing raw materials: 50m3Adding 1.5mol/L ferrous sulfate solution into a stainless steel reaction barrel, and adding into the reaction barrel with the volume of 7m3Sodium hydroxide solution with the concentration of 2.5mol/L, and simultaneously controlling the reaction temperature to be 25-35 ℃;
b: and (3) air volume control: controlling the total reaction time to be 14-17h, introducing air to the bottom of the reaction solution in the first 5-7 h, and controlling the air amount to be 230m3The air quantity is controlled to be 460m after 7-10h3H is used as the reference value. The final reaction material is used as a seed crystal for independent storage;
2) adding a buffer system for oxidation:
a: putting the prepared seed crystal into a reaction barrel, adding a certain amount of water for dilution, and controlling the ferrous content to be between 1.34mol/L and 1.52 mol/L;
b: introducing air into the feed liquid of the six groups of reaction barrels from the bottom, and controlling the air flow to be 300m3And h, simultaneously opening a steam valve to heat, and stopping heating when the temperature reaches 62 +/-2 ℃.
C: and after the temperature is stable, adding the buffer solution group D into a reaction barrel for reaction, stopping adding the reagent when the pH value reaches 4.0 +/-0.3, and then controlling the reaction temperature to be between 80 and 88 ℃ for oxidation reaction.
D: when the ferrous content is lower than 1.0mol/L, supplementing ferrous sulfate, and controlling the reaction content to be about 1.0mol/L by adopting a mode of multiple small amount operation;
3) post-treatment:
a: after the reaction reaches the specified time (the reaction time of the iron oxide pigment production is controlled according to the color requirement of the standard sample), opening a valve of the reaction barrel, discharging the feed liquid, and carrying out suction filtration, rinsing, drying and ultrafine grinding on the feed liquid to obtain the finished product.
Example 4
1) Seed crystal preparation:
a: preparing raw materials: 50m3Adding 1.5mol/L ferrous sulfate solution into a stainless steel reaction barrel, and adding into the reaction barrel with the volume of 7m3Sodium hydroxide solution with the concentration of 2.5mol/L, and simultaneously controlling the reaction temperature to be 25-35 ℃;
b: and (3) air volume control: controlling the total reaction time to be 14-17h, introducing air to the bottom of the reaction solution in the first 5-7 h, and controlling the air amount to be 230m3The air quantity is controlled to be 460m after 7-10h3H is used as the reference value. The final reaction material is used as a seed crystal for independent storage;
2) adding a buffer system for oxidation:
a: putting the prepared seed crystal into a reaction barrel, adding a certain amount of water for dilution, and controlling the ferrous content to be between 1.34mol/L and 1.52 mol/L;
b: introducing air into the feed liquid of the six groups of reaction barrels from the bottom, and controlling the air flow to be 300m3And h, simultaneously opening a steam valve to heat, and stopping heating when the temperature reaches 62 +/-2 ℃.
C: and after the temperature is stable, adding the buffer solution E group into a reaction barrel for reaction, stopping adding the reagent when the pH value reaches 4.0 +/-0.3, and then controlling the reaction temperature between 80 and 88 ℃ for oxidation reaction.
D: when the ferrous content is lower than 1.0mol/L, supplementing ferrous sulfate, and controlling the reaction content to be about 1.0mol/L by adopting a mode of multiple small amount operation;
3) post-treatment:
a: after the reaction reaches the specified time (the reaction time of the iron oxide pigment production is controlled according to the color requirement of the standard sample), opening a valve of the reaction barrel, discharging the feed liquid, and carrying out suction filtration, rinsing, drying and ultrafine grinding on the feed liquid to obtain the finished product.
Example 5
1) Seed crystal preparation:
a: preparing raw materials: 50m3Adding 1.5mol/L ferrous sulfate solution into a stainless steel reaction barrel, and adding into the reaction barrel with the volume of 7m3Sodium hydroxide solution with the concentration of 2.5mol/L, and simultaneously controlling the reaction temperature to be 25-35 ℃;
b: and (3) air volume control: the total reaction time is controlled to be 14-17h, and the first 5-7 h isIntroducing air into the bottom of the reaction solution, and controlling the air volume at 230m3The air quantity is controlled to be 460m after 7-10h3H is used as the reference value. The final reaction material is used as a seed crystal for independent storage;
2) adding a buffer system for oxidation:
a: putting the prepared seed crystal into a reaction barrel, adding a certain amount of water for dilution, and controlling the ferrous content to be between 1.34mol/L and 1.52 mol/L;
b: introducing air into the feed liquid of the six groups of reaction barrels from the bottom, and controlling the air flow to be 300m3And h, simultaneously opening a steam valve to heat, and stopping heating when the temperature reaches 62 +/-2 ℃.
C: and after the temperature is stable, adding the buffer solution F group into a reaction barrel for reaction, stopping adding the reagent when the pH value reaches 4.0 +/-0.3, and then controlling the reaction temperature between 80 and 88 ℃ for oxidation reaction.
D: when the ferrous content is lower than 1.0mol/L, supplementing ferrous sulfate, and controlling the reaction content to be about 1.0mol/L by adopting a mode of multiple small amount operation;
3) post-treatment:
a: after the reaction reaches the specified time, a valve of the reaction barrel is opened, the feed liquid is discharged, and the finished product is obtained after the feed liquid is filtered, rinsed, dried and ultrafine crushed.
Example 6
1) Seed crystal preparation:
a: preparing raw materials: 50m3Adding 1.5mol/L ferrous sulfate solution into a stainless steel reaction barrel, and adding into the reaction barrel with the volume of 7m3Sodium hydroxide solution with the concentration of 2.5mol/L, and simultaneously controlling the reaction temperature to be 25-35 ℃;
b: and (3) air volume control: controlling the total reaction time to be 14-17h, introducing air to the bottom of the reaction solution in the first 5-7 h, and controlling the air amount to be 230m3The air quantity is controlled to be 460m after 7-10h3H is used as the reference value. The final reaction material is used as a seed crystal for independent storage;
2) adding a buffer system for oxidation:
a: putting the prepared seed crystal into a reaction barrel, adding a certain amount of water for dilution, and controlling the ferrous content to be between 1.34mol/L and 1.52 mol/L;
b, introducing air into the feed liquid of the two groups of reaction barrels from the bottom, and controlling the air flow to be 300m3Opening a steam valve to heat up at the same time, and stopping heating up when the temperature reaches 62 +/-2 ℃;
c: after the temperature is stable, adding the group G reagent into a reaction barrel for reaction, stopping adding the reagent when the pH value reaches 4.0 +/-0.3, and then controlling the reaction temperature between 80 ℃ and 88 ℃ for oxidation reaction;
d: when the ferrous content is lower than 1.0mol/L, supplementing ferrous sulfate, and controlling the reaction content to be about 1.0mol/L by adopting a mode of multiple small amount operation;
3) post-treatment:
a: after the reaction reaches the specified time (the reaction time of the iron oxide pigment production is controlled according to the color requirement of the standard sample), opening a valve of the reaction barrel, discharging the feed liquid, and carrying out suction filtration, rinsing, drying and ultrafine grinding on the feed liquid to obtain the finished product.
Example 7
1) Seed crystal preparation:
a: preparing raw materials: 50m3Adding 1.5mol/L ferrous sulfate solution into a stainless steel reaction barrel, and adding into the reaction barrel with the volume of 7m3Sodium hydroxide solution with the concentration of 2.5mol/L, and simultaneously controlling the reaction temperature to be 25-35 ℃;
b: and (3) air volume control: controlling the total reaction time to be 14-17h, introducing air to the bottom of the reaction solution in the first 5-7 h, and controlling the air amount to be 230m3The air quantity is controlled to be 460m after 7-10h3H is used as the reference value. The final reaction material is used as a seed crystal for independent storage;
2) adding a buffer system for oxidation:
a: putting the prepared seed crystal into a reaction barrel, adding a certain amount of water for dilution, and controlling the ferrous content to be between 1.34mol/L and 1.52 mol/L;
b, introducing air into the feed liquid of the two groups of reaction barrels from the bottom, and controlling the air flow to be 300m3Opening a steam valve to heat up at the same time, and stopping heating up when the temperature reaches 62 +/-2 ℃;
c: after the temperature is stable, adding the group H reagent into a reaction barrel for reaction, stopping adding the reagent when the pH value reaches 4.0 +/-0.3, and then controlling the reaction temperature between 80 ℃ and 88 ℃ for oxidation reaction;
d: when the ferrous content is lower than 1.0mol/L, supplementing ferrous sulfate, and controlling the reaction content to be about 1.0mol/L by adopting a mode of multiple small amount operation;
3) post-treatment:
a: after the reaction reaches the specified time (the reaction time of the iron oxide pigment production is controlled according to the color requirement of the standard sample), a valve of the reaction barrel is opened, the feed liquid is discharged, and the finished product is obtained by carrying out suction filtration, rinsing, drying and ultrafine grinding on the feed liquid.
Control group
1) Seed crystal preparation:
a: preparing raw materials: 50m3Adding 1.5mol/L ferrous sulfate solution into a stainless steel reaction barrel, and adding into the reaction barrel with the volume of 7m3Sodium hydroxide solution with the concentration of 2.5mol/L, and simultaneously controlling the reaction temperature to be 25-35 ℃;
b: and (3) air volume control: controlling the total reaction time to be 14-17h, introducing air to the bottom of the reaction solution in the first 5-7 h, and controlling the air amount to be 230m3The air quantity is controlled to be 460m after 7-10h3H is used as the reference value. The final reaction material is used as a seed crystal for independent storage;
2) adding a buffer system for oxidation:
a: putting the prepared seed crystal into a reaction barrel, adding a certain amount of water for dilution, and controlling the ferrous content to be between 1.34mol/L and 1.52 mol/L;
b: introducing air into the feed liquid of the six groups of reaction barrels from the bottom, and controlling the air flow to be 300m3And h, simultaneously opening a steam valve to heat, and stopping heating when the temperature reaches 62 +/-2 ℃.
C: and after the temperature is stable, adding the group A of buffer solution into a reaction barrel for reaction, stopping adding the reagent when the pH value reaches 4.0 +/-0.3, and then controlling the reaction temperature between 80 ℃ and 88 ℃ for oxidation reaction.
D: when the ferrous content is lower than 1.0mol/L, supplementing ferrous sulfate, and controlling the reaction content to be about 1.0mol/L by adopting a mode of multiple small amount operation;
3) post-treatment:
a: after the reaction reaches the specified time (the reaction time of the iron oxide pigment production is controlled according to the color requirement of the standard sample), opening a valve of the reaction barrel, discharging the feed liquid, and carrying out suction filtration, rinsing, drying and ultrafine grinding on the feed liquid to obtain the finished product.
Test example 1
The test method comprises the following steps:
stormer viscometer test method: firstly, adding BYK190 and BYK024 respectively 700g and 30g into a container matched with equipment, then adding 270g of distilled water, slowly adding 120g of iron oxide yellow pigment, using SFJ-400 to sand and disperse, using a multipurpose stirring machine 4500 rpm, stirring for 45 minutes, measuring the temperature, and measuring the data at 25 ℃ by using a KU-2VISCOMETER VISCOMETER.
Particle size test method: scanning electron microscope SEM.
And (3) testing results:
the length-diameter ratio and viscosity of the iron oxide yellow prepared in examples 1-7 and the control group were measured by the above methods, and are detailed in table 1
TABLE 1
Table 2 shows the pH change law of the reaction solution in example 3 after adding the potassium hydrogen phthalate-sodium hydroxide buffer solution with the molar ratio of 1: 50; in addition, Table 2 also shows the pH change of the reaction solution without adding a buffer solution:
TABLE 2 Potassium hydrogen phthalate with sodium hydroxide buffer and unbuffered pH
From the above, after the buffer solution is added, the seed crystal can grow under the condition of stable pH, the adverse effects of severe pH change generated by the impact of ferrous sulfate and liquid alkali on viscosity and length-diameter ratio are weakened, the iron oxide yellow particles grow more uniformly, the iron oxide yellow particles are not easy to generate bifurcation, the particle surface is smoother, the length-diameter ratio is reduced, and the viscosity is as low as 36 Ku.
Test example 2
The color data of the plurality of samples prepared in example 3 and the color data of the standard sample are compared by adopting a national standard GB/T1864-.
TABLE 3
| L | a | b | |
| Standard sample 1 | 59.11 | 14.09 | 42.75 |
| Sample No. 1 | 58.94 | 14.12 | 42.78 |
| △E＝0.18 | -0.17 | 0.03 | 0.03 |
TABLE 4
| L | a | | |
| Standard sample | |||
| 2 | 59.08 | 14.15 | 42.77 |
| Sample No. 2 | 59.01 | 14.21 | 42.84 |
| △E＝0.12 | -0.07 | 0.06 | 0.07 |
TABLE 5
| L | a | b | |
| Standard sample 3 | 59.20 | 14.02 | 42.71 |
| Sample No. 3 | 59.11 | 14.11 | 42.76 |
| △E＝0.14 | -0.09 | 0.09 | 0.05 |
The difference between the GB/T1864-.
Claims (4)
1. A method for controlling the viscosity of iron oxide yellow by a buffer system is characterized by comprising the following steps:
1) preparing seed crystals:
adding 2-3 mol/L sodium hydroxide solution into 1-2 mol/L ferrous sulfate solution, controlling the reaction temperature to be 25-35 ℃, the reaction time to be 14-17h, introducing air to the bottom of a reaction night, and controlling the air amount to be 200m for carrying out thin film rice plantation/h-500 m for carrying out thin film rice plantation/h;
2) adding a buffer system for oxidation:
a: controlling the content of the ferrous iron in the reaction barrel to be 1.34-1.52 mol/L;
b: continuing introducing air, controlling the air amount to be in a range of 250-350 m for carrying out dry top planting, and stopping heating when the temperature is 60-65 ℃:
c: continuously adding the buffer solution into the reaction barrel; adding a sodium hydroxide solution with the concentration of 2-3 mol/L, stopping adding the sodium hydroxide solution when the pH value reaches 4.0 +/-0.3, and reacting at the temperature of 80-88 ℃; the buffer solution is a potassium hydrogen phthalate-sodium hydroxide buffer solution, and the molar ratio of the potassium hydrogen phthalate to the sodium hydroxide is 1: 80-1: 30;
d: when the ferrous content is lower than 1.0mol/L, supplementing ferrous sulfate, and controlling the reaction content to be about 1.0mol/L by adopting a mode of multiple small amount operation;
3) post-treatment:
after the reaction reaches the specified time, a valve of the reaction kettle is opened, the feed liquid is discharged, and the finished product is obtained after the feed liquid is filtered, rinsed, dried and ultrafine crushed.
2. The method for controlling the viscosity of iron oxide yellow by using the buffer system according to claim 1, wherein the molar ratio of the potassium hydrogen phthalate to the sodium hydroxide is 1: 50-1: 30.
3. The method for controlling the viscosity of the iron oxide yellow by using the buffer system according to claim 1, wherein in the step 2) A, a certain amount of water is added for dilution, and the content of ferrous iron is controlled to be 1.34-1.52 mol/L.
4. The method for controlling viscosity of iron oxide yellow according to claim 3, wherein the ferrous sulfate solution with the concentration of 1.5mol/L at 50m is added into a stainless steel reaction barrel, and then 2.5mol/L sodium hydroxide solution is added for carrying out thin film plantation at 7m while controlling the reaction temperature at 30 ℃; controlling the total reaction time to be 15h, introducing air to the bottom of the reaction liquid in the first 5-7 h, controlling the air quantity to be 230m for each h, and introducing air to the bottom of the reaction liquid in the last 7-10h, and controlling the air quantity to be 460m for each h.
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