CN110951281A - Copper-chromium black toner prepared by solid-phase sintering method promoted by molybdenum oxide and zinc oxide and preparation method thereof - Google Patents
Copper-chromium black toner prepared by solid-phase sintering method promoted by molybdenum oxide and zinc oxide and preparation method thereof Download PDFInfo
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- CN110951281A CN110951281A CN201911186551.0A CN201911186551A CN110951281A CN 110951281 A CN110951281 A CN 110951281A CN 201911186551 A CN201911186551 A CN 201911186551A CN 110951281 A CN110951281 A CN 110951281A
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- copper
- oxide
- black toner
- chromium black
- solid
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- 238000000034 method Methods 0.000 title claims abstract description 36
- GXDVEXJTVGRLNW-UHFFFAOYSA-N [Cr].[Cu] Chemical compound [Cr].[Cu] GXDVEXJTVGRLNW-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000005245 sintering Methods 0.000 title claims abstract description 25
- 239000007790 solid phase Substances 0.000 title claims abstract description 13
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims description 34
- 229910000476 molybdenum oxide Inorganic materials 0.000 title claims description 17
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 title claims description 17
- 239000011787 zinc oxide Substances 0.000 title claims description 17
- 238000002360 preparation method Methods 0.000 title description 5
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims description 9
- 238000004806 packaging method and process Methods 0.000 claims description 7
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 6
- 239000005751 Copper oxide Substances 0.000 claims description 6
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 6
- 229910000431 copper oxide Inorganic materials 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 3
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000003086 colorant Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 6
- 238000003911 water pollution Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 13
- 239000002245 particle Substances 0.000 description 12
- 239000004927 clay Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- JHWIEAWILPSRMU-UHFFFAOYSA-N 2-methyl-3-pyrimidin-4-ylpropanoic acid Chemical compound OC(=O)C(C)CC1=CC=NC=N1 JHWIEAWILPSRMU-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 229940116318 copper carbonate Drugs 0.000 description 1
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- C09C1/34—Compounds of chromium
- C09C1/346—Chromium oxides
-
- 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to the technical field of color agents, in particular to a copper-chromium black color agent prepared by a solid-phase sintering method and a method thereof. The invention has the advantages of easily obtained raw materials, low cost, low reaction temperature and simple operation process, and avoids water pollution caused by wet ball milling by dry ball milling.
Description
Technical Field
The invention belongs to the technical field of toner materials, and particularly relates to a copper-chromium black toner prepared by a solid-phase sintering method promoted by molybdenum oxide and zinc oxide and a method thereof.
Background
The traditional preparation method of the copper-chromium black mainly comprises a solid phase method and a liquid phase method. The solid phase method is usually to mix solid copper carbonate with high purity and sodium dichromate, or copper oxide and chromic oxide according to a certain proportion, grind into fine powder, then put into a calcining furnace to calcine for a period of time, and then rinse, filter, dry, grind to obtain the finished product. The traditional solid phase method for preparing the copper-chromium black has higher reaction temperature which generally needs about 1200 ℃, and has high energy consumption. Because the raw materials are solid, even if the raw materials are ground and mixed for a long time, the raw materials are not uniform, so that the contact area of reactant particles is small, the reaction activity is low, and the reaction is not uniform and sufficient. In order to meet the particle size requirement of application, the particles are often ground again, so that crystal lattices are easily damaged, impurities are brought, and the chemical resistance of the particles is reduced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the preparation method of the copper-chromium black toner, which has the advantages of simple process, less reaction conditions and lower energy consumption. The technical scheme is as follows:
a copper-chromium black dye agent prepared by a solid-phase sintering method promoted by molybdenum oxide and zinc oxide is spinel-shaped; the copper-chromium black toner is prepared by using 52-75% of chromium oxide, 22-44% of copper oxide, 1-6% of zinc oxide and 0.1-4% of molybdenum oxide as raw materials in percentage by weight and calcining at high temperature.
Furthermore, the copper-chromium black toner takes 62% of chromic oxide, 32% of copper oxide, 5% of zinc oxide and 1% of molybdenum oxide as raw materials according to the weight percentage.
The method for preparing the copper-chromium black toner by using the molybdenum oxide and zinc oxide promoted solid-phase sintering method comprises the following steps:
(1) putting the raw materials in the formula amount into an inclined mixer, and uniformly mixing to obtain a mixture;
(2) placing the mixture obtained in the step (1) in a sagger, and sintering at high temperature to obtain a color agent;
(3) and (3) mechanically ball-milling and crushing the color agent obtained in the step (2), and then packaging to obtain a finished product.
Further, the sintering temperature in the step (2) is 850-930 ℃.
Further, the sintering time in the step (2) is 1-3 h.
Further, the ball milling in the step (3) is carried out until the D99 is 5-5.5 μm.
By adopting the scheme, the method has the following advantages:
1. the method for preparing the copper-chromium black toner by utilizing the molybdenum oxide and zinc oxide promoted solid-phase sintering method takes chromium oxide and copper oxide as raw materials and zinc oxide and molybdenum oxide as mineralizers to promote particle sintering, improve the reactivity among particles, reduce the reaction temperature and enable the reaction to be more uniform and thorough.
2. The method for preparing the copper-chromium black toner by using the solid-phase sintering method promoted by the molybdenum oxide and the zinc oxide adopts mechanical ball milling to break up agglomerated color groups, so that the particles are more uniformly distributed, and secondary pollution caused by wet ball milling is avoided.
3. The copper-chromium black toner prepared by the method for preparing the copper-chromium black toner by the solid-phase sintering method promoted by molybdenum oxide and zinc oxide has high purity, uniform particles and complete crystal form, is applied to the technical field of slurry, and has the advantages of good blackness, low temperature and strong covering power.
4. The method for preparing the copper-chromium black toner by using the molybdenum oxide and zinc oxide promoted solid-phase sintering method has the advantages of lower reaction temperature, simple preparation method, fewer steps, low cost, benefit for environmental protection and contribution to batch production of factories and promotion of technical progress and development of the copper-chromium black toner.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The experimental procedures in the following examples are conventional procedures unless otherwise specified, and the experimental reagents and materials involved are conventional chemical reagents and materials unless otherwise specified.
The raw materials of the following examples are mixed according to the weight percentages shown in Table 1:
TABLE 1
Example 1
(1) The materials are mixed according to the weight percentage of the components in the table 1, and the mixed materials are mixed evenly by an inclined mixer.
(2) And (2) placing the mixture obtained in the step (1) into a clay sagger, and sintering at 860 ℃ for 90 min.
(3) And (3) mechanically ball-milling and crushing the color agent obtained in the step (2), and then packaging to obtain a finished product.
Example 2
(1) The materials are mixed according to the weight percentage of the components in the table 1, and the mixed materials are mixed evenly by an inclined mixer.
(2) And (2) placing the mixture obtained in the step (1) into a clay sagger, and preserving heat for 60min at 820 ℃ for sintering.
(3) And (3) mechanically ball-milling and crushing the color agent obtained in the step (2), and then packaging to obtain a finished product.
Example 3
(1) The materials are mixed according to the weight percentage of the components in the table 1, and the mixed materials are mixed evenly by an inclined mixer.
(2) And (2) placing the mixture obtained in the step (1) into a clay sagger, and sintering at the temperature of 960 ℃ for 180 min.
(3) And (3) mechanically ball-milling and crushing the color agent obtained in the step (2), and then packaging to obtain a finished product.
Example 4
(1) The materials are mixed according to the weight percentage of the components in the table 1, and the mixed materials are mixed evenly by an inclined mixer.
(2) And (2) placing the mixture obtained in the step (1) into a clay sagger, and sintering at the temperature of 900 ℃ for 150 min.
(3) And (3) mechanically ball-milling and crushing the color agent obtained in the step (2), and then packaging to obtain a finished product.
Example 5
(1) The materials are mixed according to the weight percentage of the components in the table 1, and the mixed materials are mixed evenly by an inclined mixer.
(2) And (2) placing the mixture obtained in the step (1) into a clay sagger, and sintering at 920 ℃ for 120 min.
(3) And (3) mechanically ball-milling and crushing the color agent obtained in the step (2), and then packaging to obtain a finished product.
The product performance test results obtained in the examples are shown in table 2, wherein the particle size distribution was measured by a particle size tester; acid resistance is tested according to ASTM C724-91 decision Standard; the color performance is measured by a color difference meter; the OD value and the transmittance were measured by a densitometer.
TABLE 2
As can be seen from Table 2, the particle sizes of the examples measured by the particle size tester are relatively uniform; the acid resistance of each example reaches the first grade, which shows that the acid resistance of each example is better; the light transmittance of each example is less than 0.02MPa, and the optical density OD value is about 4.2, which shows that the covering power of the invention is good.
The numerical values in the table are not very different, which shows that the copper chromium black toner of the invention prepared by the method of the invention can keep relatively stable characteristics, and the method of the invention has high recurrence rate.
Various other modifications and changes may occur to those skilled in the art from the foregoing description and drawings, and all such modifications and changes are intended to fall within the scope of the appended claims.
Claims (6)
1. A copper-chromium black colorant prepared by a solid-phase sintering method promoted by molybdenum oxide and zinc oxide is characterized in that: the copper-chromium black toner is prepared by using 52-75% of chromium oxide, 22-44% of copper oxide, 1-6% of zinc oxide and 0.1-4% of molybdenum oxide as raw materials in percentage by weight and calcining at high temperature.
2. The copper-chromium black toner prepared by the solid-phase sintering method promoted with molybdenum oxide and zinc oxide according to claim 1, wherein: the copper-chromium black toner takes 62% of chromic oxide, 32% of copper oxide, 5% of zinc oxide and 1% of molybdenum oxide as raw materials according to weight percentage.
3. The method for preparing the copper-chromium black toner according to claim 1, which is prepared by a solid-phase sintering method promoted by molybdenum oxide and zinc oxide, wherein the method comprises the following steps: the method comprises the following steps:
(1) putting the raw materials in the formula amount into an inclined mixer, and uniformly mixing to obtain a mixture;
(2) placing the mixture obtained in the step (1) in a sagger, and sintering at high temperature to obtain a color agent;
(3) and (3) mechanically ball-milling and crushing the color agent obtained in the step (2), and then packaging to obtain a finished product.
4. The method for preparing a copper-chromium black toner according to claim 3, wherein the method comprises the steps of: the sintering temperature in the step (2) is 820-960 ℃.
5. The method for preparing a copper-chromium black toner according to claim 3, wherein the method comprises the steps of: the sintering time in the step (2) is 1-3 h.
6. The method for preparing a copper-chromium black toner according to claim 3, wherein the method comprises the steps of: and (4) performing ball milling in the step (3) until D99 is 5-5.5 mu m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911186551.0A CN110951281B (en) | 2019-11-28 | 2019-11-28 | Copper-chromium black toner prepared by solid-phase sintering method promoted by molybdenum oxide and zinc oxide and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911186551.0A CN110951281B (en) | 2019-11-28 | 2019-11-28 | Copper-chromium black toner prepared by solid-phase sintering method promoted by molybdenum oxide and zinc oxide and preparation method thereof |
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| Publication Number | Publication Date |
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| CN110951281A true CN110951281A (en) | 2020-04-03 |
| CN110951281B CN110951281B (en) | 2021-10-15 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111748222A (en) * | 2020-07-07 | 2020-10-09 | 衡水友谊新材料科技有限公司 | High-tinting strength copper-chromium black pigment and preparation method thereof |
| WO2023234160A1 (en) | 2022-06-02 | 2023-12-07 | Dic株式会社 | Copper chromium oxide spinel, resin composition of same, resin molded article, and method for producing copper chromium oxide spinel |
| JP7468801B1 (en) | 2022-06-02 | 2024-04-16 | Dic株式会社 | Copper oxide chromium spinel, its resin composition, and resin molded product |
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| US2309173A (en) * | 1939-01-21 | 1943-01-26 | Diehl Heinrich | Black ceramic pigments and method of preparation |
| JPH0450119A (en) * | 1990-06-16 | 1992-02-19 | Dainichiseika Color & Chem Mfg Co Ltd | Manufacturing method of fine particle composite oxide black pigment |
| CN109071962A (en) * | 2016-05-02 | 2018-12-21 | 谢珀德颜色公司 | Show thermal stability, acid condition resistance and good light fastness, pink and pansy pigment comprising one or more antimony and/or niobium oxide |
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2019
- 2019-11-28 CN CN201911186551.0A patent/CN110951281B/en active Active
Patent Citations (3)
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| US2309173A (en) * | 1939-01-21 | 1943-01-26 | Diehl Heinrich | Black ceramic pigments and method of preparation |
| JPH0450119A (en) * | 1990-06-16 | 1992-02-19 | Dainichiseika Color & Chem Mfg Co Ltd | Manufacturing method of fine particle composite oxide black pigment |
| CN109071962A (en) * | 2016-05-02 | 2018-12-21 | 谢珀德颜色公司 | Show thermal stability, acid condition resistance and good light fastness, pink and pansy pigment comprising one or more antimony and/or niobium oxide |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111748222A (en) * | 2020-07-07 | 2020-10-09 | 衡水友谊新材料科技有限公司 | High-tinting strength copper-chromium black pigment and preparation method thereof |
| CN111748222B (en) * | 2020-07-07 | 2021-10-01 | 衡水友谊新材料科技有限公司 | High-tinting strength copper-chromium black pigment and preparation method thereof |
| WO2023234160A1 (en) | 2022-06-02 | 2023-12-07 | Dic株式会社 | Copper chromium oxide spinel, resin composition of same, resin molded article, and method for producing copper chromium oxide spinel |
| JP7468801B1 (en) | 2022-06-02 | 2024-04-16 | Dic株式会社 | Copper oxide chromium spinel, its resin composition, and resin molded product |
| JP7509324B2 (en) | 2022-06-02 | 2024-07-02 | Dic株式会社 | Copper oxide chromium spinel, resin composition thereof, resin molded product, and method for producing copper oxide chromium spinel |
| JP7697566B2 (en) | 2022-06-02 | 2025-06-24 | Dic株式会社 | Copper oxide chromium spinel, resin composition thereof, resin molded product, and method for producing copper oxide chromium spinel |
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