CN110951280B - Copper-chromium black toner prepared by solid-phase sintering method promoted by molybdenum oxide and manganese oxide and preparation method thereof - Google Patents

Copper-chromium black toner prepared by solid-phase sintering method promoted by molybdenum oxide and manganese oxide and preparation method thereof Download PDF

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CN110951280B
CN110951280B CN201911186543.6A CN201911186543A CN110951280B CN 110951280 B CN110951280 B CN 110951280B CN 201911186543 A CN201911186543 A CN 201911186543A CN 110951280 B CN110951280 B CN 110951280B
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copper
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chromium black
black toner
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CN110951280A (en
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郁加良
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Huangshan Jingtemei New Materials Co ltd
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    • 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
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • 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
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/041—Grinding
    • 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
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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  • Organic Chemistry (AREA)
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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, simple and easily obtained operation process and high purity; after the product is used for sizing agent, the product has the advantages of good blackness, low temperature and good covering power.

Description

Copper-chromium black toner prepared by solid-phase sintering method promoted by molybdenum oxide and manganese oxide and preparation method thereof
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 manganese oxide and a preparation method thereof.
Background
The traditional preparation method of the copper-chromium black mainly comprises a solid phase method and a liquid phase method. Generally, the copper-chromium black prepared by the traditional liquid phase method is superior to the copper-chromium black prepared by the traditional solid phase method in terms of purity and uniformity. However, the traditional liquid phase method for preparing the copper-chromium black also has the defects of high requirements on raw materials, complex process, high temperature and high pressure, high requirements on equipment, long reaction time, high production cost, secondary pollution and no contribution to industrial production. The traditional solid phase method for preparing the copper-chromium black has the advantages of higher reaction temperature which generally needs about 1200 ℃, high energy consumption, lower reaction activity, uneven and insufficient reaction, more steps and complex operation.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the preparation method of the copper-chromium black agent, which has simple process and can effectively reduce the reaction temperature of the solid phase method so as to reduce the production energy consumption, and the prepared product has good covering power and high blackness. The technical scheme is as follows:
a copper-chromium black dye agent prepared by a solid-phase sintering method promoted by molybdenum oxide and manganese oxide is spinel-shaped; the copper-chromium black toner is prepared by taking 50-70% of chromium oxide, 19-40% of copper oxide, 5-18% of manganese oxide and 0.1-3% of molybdenum oxide as raw materials in percentage by weight and calcining at high temperature.
Furthermore, the copper-chromium black toner takes 55.4 percent of chromic oxide, 34 percent of copper oxide, 10 percent of manganese oxide and 0.6 percent 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 manganese 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 manganese oxide promoted solid-phase sintering method takes chromium oxide and copper oxide as raw materials and manganese oxide and molybdenum oxide as mineralizers, wherein the manganese oxide and the molybdenum oxide can play a role in promoting the catalysis of particle sintering, the reaction activity among particles is improved, the reaction temperature is reduced, and the reaction is more uniform and thorough.
2. According to the method for preparing the copper-chromium black toner by using the solid-phase sintering method promoted by molybdenum oxide and manganese oxide, the agglomerated color groups can be broken up by adopting mechanical ball milling, so that the particles are distributed more uniformly, 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 manganese 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 manganese 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
Figure BDA0002292533680000031
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 870 ℃ 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 carrying out heat preservation for 60min at the temperature of 850 ℃ 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) putting the mixture obtained in the step (1) into a clay sagger, and sintering at 930 ℃ 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 900 ℃ 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 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 carrying out heat preservation for 120min at the temperature of 915 ℃ 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.
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
Figure BDA0002292533680000041
As can be seen from Table 2, the acid resistance of each example reaches the first grade, which indicates that the acid resistance of each example is better; the invention has bright color, high color rendering and pure color; the light transmittance of each example is less than 0.02MPa, which shows that the covering power of the invention is good, and the particle size value obtained by testing shows that the particles of the invention are uniformly distributed.
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.
The copper-chromium black toner prepared by the invention has strong tinting strength, high stability and low product cost, and can meet the requirements of various fields on the copper-chromium black toner. After the copper-chromium black toner prepared by the invention is applied to slurry, the product has the advantages of good blackness, low temperature and good covering power.
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 (4)

1. A copper-chromium black colorant prepared by a solid-phase sintering method promoted by molybdenum oxide and manganese oxide is characterized in that: the copper-chromium black toner is prepared by sintering 50-70 wt% of chromium oxide, 19-40 wt% of copper oxide, 5-18 wt% of manganese oxide and 0.1-3 wt% of molybdenum oxide at high temperature for 1-1.5 h.
2. The copper-chromium black toner prepared by the solid-phase sintering method promoted by molybdenum oxide and manganese oxide according to claim 1, wherein: the copper-chromium black toner takes 55.4 percent of chromic oxide, 34 percent of copper oxide, 10 percent of manganese oxide and 0.6 percent of molybdenum oxide as raw materials according to the weight percentage.
3. The method for preparing the copper-chromium black toner prepared by the solid-phase sintering method promoted by molybdenum oxide and manganese oxide according to claim 1, which is characterized by comprising 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 the high temperature of 850-870 ℃ for 1-1.5 h 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 the copper-chromium black toner by the solid-phase sintering method promoted by molybdenum oxide and manganese oxide according to claim 3, wherein the method comprises the following steps: and (4) performing ball milling in the step (3) until D99 is 5-5.5 mu m.
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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
CN113943017B (en) * 2020-07-16 2023-12-26 中国石油天然气股份有限公司 Copper-chromium black raw material treatment method and copper-chromium black
CN114075397A (en) * 2020-08-12 2022-02-22 江苏山由帝奥节能新材股份有限公司 High-temperature-resistant water-based paint and furnace door liner applying same
CN113603356B (en) * 2021-09-09 2023-03-21 黄山市晶特美新材料有限公司 Black pigment with strong absorption to visible light and preparation method thereof
CN116023805A (en) * 2022-12-29 2023-04-28 淄博颜光颜料有限公司 High-tinting strength copper-chromium black pigment and preparation process thereof

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