CN113149635A - Environment-friendly inorganic pigment and preparation process thereof - Google Patents
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Abstract
The invention belongs to the technical field of inorganic pigments, and particularly relates to an environment-friendly inorganic pigment and a preparation process thereof. The environment-friendly inorganic pigment provided by the invention comprises the raw materials of titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, wherein the cerium oxide is cerium dioxide, and the mineralizer is Li2CO3. The preparation process of the environment-friendly inorganic pigment comprises the following steps: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1250-. The environment-friendly inorganic pigment disclosed by the invention has the advantages that titanium dioxide, nickel carbonate, cobalt carbonate and rare earth cerium oxide are cooperatively matched, and a mineralizer is added to reduce the calcination temperature to about 1300 ℃, so that the energy consumption is reduced, and the prepared inorganic pigmentStable property, good covering power and good tinting strength.
Description
Technical Field
The invention belongs to the technical field of inorganic pigments, and particularly relates to an environment-friendly inorganic pigment and a preparation process thereof.
Background
Traditional pigments are classified into organic color pastes and inorganic pigments. The organic color paste is prepared by chemical reaction between organic materials or between organic materials and inorganic materials, usually produces many toxic byproducts (waste liquid, waste residue, waste gas and the like), brings certain adverse effects to human life, work and learning environment, is easy to damage the health of people and the growth of other organisms, causes ecological imbalance and seriously pollutes the environment. Inorganic pigments are oxides of nonferrous metals, or some metal-insoluble metal salts, and are further classified into natural inorganic pigments, which are mineral pigments, and artificial inorganic pigments.
Natural inorganic pigments are mainly produced by calcining or directly crushing (drying) and grinding inorganic mineral aggregates. The artificial inorganic pigment is prepared by calcining or directly crushing (drying) and grinding inorganic mineral aggregate into powder, and then adding a small amount of coloring material for mixing. The use of natural inorganic pigments is highly appreciated because of their green and environmental benefits.
China is a large country for producing traditional inorganic pigments, the research and development of the inorganic pigments and the products mostly belong to traditional low-grade pigments with low profits, and green and environment-friendly new products with high added value and no toxicity are lacked. Some toxic pigments are still used in China in large quantities, such as chromium-based pigments, lead-chromium yellow pigments, cadmium orange pigments and cadmium red pigments, and harmful bulk pigments cannot be exported. However, these conventional natural inorganic pigments tend to have poor dispersibility and uneven color.
At present, the yellow inorganic pigment mainly comprises lead chrome yellow (lead chromate), zinc chrome yellow (zinc chromate), cadmium yellow (cadmium sulfide), iron yellow (hydrated iron oxide) and the like. Among them, lead chrome yellow (lead chromate) is the most widely used and the yield is the greatest. However, lead chrome yellow is easily darkened under sunlight; the covering power and the tinting strength of the zinc chrome yellow are poorer than those of the lead chrome yellow; the tinting strength and hiding power of cadmium yellow are not as good as those of lead-chromium yellow, the cost is higher, and the application is limited. Meanwhile, lead chrome yellow and cadmium yellow both contain heavy metals, and therefore cannot be used for coloring in some specific fields, and the application range is limited. The development of a safe, environment-friendly and low-cost substance which can replace the yellow inorganic pigment is of great significance.
Disclosure of Invention
The purpose of the invention is: an environment-friendly inorganic pigment is provided. The prepared inorganic pigment is non-toxic and pollution-free, has excellent physical, chemical and thermal stability, and is an environment-friendly product; the invention also provides a preparation process thereof.
The environment-friendly inorganic pigment provided by the invention comprises the raw materials of titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, wherein the cerium oxide is cerium dioxide, and the mineralizer is Li2CO3。
Preferably, the environment-friendly inorganic pigment comprises, by weight, 50-55 parts of titanium dioxide, 5-7 parts of nickel carbonate, 5-10 parts of cobalt carbonate, 12-15 parts of cerium oxide and 2.2-2.7 parts of a mineralizer.
Most preferably, the environment-friendly inorganic pigment comprises, by weight, 55 parts of titanium dioxide, 5 parts of nickel carbonate, 10 parts of cobalt carbonate, 15 parts of cerium oxide and 2.6 parts of a mineralizer.
The preparation process of the environment-friendly inorganic pigment comprises the following steps: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1250-.
Wherein:
the particle size of the product is controlled to be less than or equal to 400 meshes after ball milling.
The roasting is started to raise the temperature from room temperature, firstly raises the temperature to 800 ℃ at the temperature raising rate of 8 ℃/min, keeps the temperature for 1-2h, then raises the temperature to 1250 ℃ at the temperature raising rate of 5 ℃/min, keeps the temperature for 2-2.5h, and finally cools to room temperature at the temperature lowering rate of 3 ℃/min for crushing.
The roasting atmosphere is inert atmosphere.
The particle size of the obtained environment-friendly inorganic pigment is controlled to be 800-1000 meshes after the crushing.
The environment-friendly inorganic pigment prepared by the process is a yellow pigment.
According to the environment-friendly inorganic pigment, cobalt and nickel transition metal ions interact with rare earth ions to absorb photon energy and generate 3d electronic configuration, nonradiative transition between 4f-4f and 4f-5d electronic energy levels and Charge Transfer Band (CTB) transition between metal and anions, the absorbed energy is radiationless relaxed into a conduction band, and the other function of the rare earth ions is that photons are absorbed between the energy levels and radiation transition is generated, so that the material is colored and emits light.
Compared with the prior art, the invention has the following beneficial effects:
(1) the environment-friendly inorganic pigment disclosed by the invention is non-toxic and safe, has excellent CIE chromaticity, stable physical and chemical properties, good color uniformity and good weather resistance, light resistance, water resistance and heat resistance.
(2) According to the environment-friendly inorganic pigment, titanium dioxide, nickel carbonate, cobalt carbonate and rare earth cerium oxide are cooperatively matched, and a mineralizer is added to reduce the calcination temperature to about 1300 ℃, so that the energy consumption is reduced, and the prepared inorganic pigment has stable property, good covering power and good tinting strength.
(3) The preparation method of the environment-friendly inorganic pigment has the advantages of simple and convenient process, high automation degree, high yield and low requirement on equipment, and the prepared inorganic pigment has stable performance.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
The environment-friendly inorganic pigment described in this embodiment 1 is prepared from 55 parts by weight of titanium dioxide, 5 parts by weight of nickel carbonate, 10 parts by weight of cobalt carbonate, 15 parts by weight of cerium oxide and 2.6 parts by weight of mineralizer; the cerium oxide is cerium dioxide, and the mineralizer is Li2CO3。
The preparation process of the environment-friendly inorganic pigment described in the embodiment 1 comprises the following steps: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1280 ℃, cooling to room temperature, and crushing to prepare the environment-friendly inorganic pigment.
Wherein:
the particle size of the product is controlled to be less than or equal to 400 meshes after ball milling.
The roasting is started from room temperature, the temperature is firstly increased to 750 ℃ at the temperature increase rate of 8 ℃/min, the heat preservation is carried out for 1.5h, then the temperature is increased to 1280 ℃ at the temperature increase rate of 5 ℃/min, the heat preservation is carried out for 2.5h, and finally the temperature is cooled to room temperature at the temperature decrease rate of 3 ℃/min for crushing.
The roasting atmosphere is inert atmosphere.
The particle size of the obtained environment-friendly inorganic pigment is controlled to be 1000 meshes after the crushing.
The environment-friendly inorganic pigment prepared by the process is a yellow pigment.
Example 2
The environment-friendly inorganic pigment described in this embodiment 2 is prepared from, by weight, 50 parts of titanium dioxide, 5 parts of nickel carbonate, 7 parts of cobalt carbonate, 14 parts of cerium oxide, and 2.3 parts of a mineralizer; the cerium oxide is cerium dioxide, and the mineralizer is Li2CO3。
The preparation process of the environment-friendly inorganic pigment described in the embodiment 2 comprises the following steps: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1250 ℃, cooling to room temperature, and crushing to prepare the environment-friendly inorganic pigment.
Wherein:
the particle size of the product is controlled to be less than or equal to 400 meshes after ball milling.
The roasting is started from room temperature, the temperature is firstly increased to 780 ℃ at the temperature increase rate of 8 ℃/min, the temperature is kept for 2h, then the temperature is increased to 1250 ℃ at the temperature increase rate of 5 ℃/min, the temperature is kept for 2h, and finally the mixture is cooled to room temperature at the temperature decrease rate of 3 ℃/min and crushed.
The roasting atmosphere is inert atmosphere.
The particle size of the obtained environment-friendly inorganic pigment is controlled to be 900 meshes after the crushing.
The environment-friendly inorganic pigment prepared by the process is a yellow pigment.
Example 3
The environmentally friendly inorganic pigment of example 3, toThe raw materials comprise, by weight, 52 parts of titanium dioxide, 6 parts of nickel carbonate, 5 parts of cobalt carbonate, 13 parts of cerium oxide and 2.4 parts of mineralizer; the cerium oxide is cerium dioxide, and the mineralizer is Li2CO3。
The preparation process of the environment-friendly inorganic pigment described in this embodiment 3 is as follows: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1270 ℃, cooling to room temperature, and crushing to prepare the environment-friendly inorganic pigment.
Wherein:
the particle size of the product is controlled to be less than or equal to 400 meshes after ball milling.
The roasting is started from room temperature, the temperature is firstly increased to 730 ℃ at the heating rate of 8 ℃/min, the temperature is kept for 2h, then the temperature is increased to 1270 ℃ at the heating rate of 5 ℃/min, the temperature is kept for 2.2h, and finally the mixture is cooled to room temperature at the cooling rate of 3 ℃/min and crushed.
The roasting atmosphere is inert atmosphere.
The particle size of the obtained environment-friendly inorganic pigment is controlled to be 800 meshes after the crushing.
The environment-friendly inorganic pigment prepared by the process is a yellow pigment.
Example 4
The environment-friendly inorganic pigment described in this embodiment 4 is prepared from, by weight, 54 parts of titanium dioxide, 7 parts of nickel carbonate, 5 parts of cobalt carbonate, 15 parts of cerium oxide, and 2.5 parts of a mineralizer; the cerium oxide is cerium dioxide, and the mineralizer is Li2CO3。
The preparation process of the environment-friendly inorganic pigment described in this embodiment 4 is as follows: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1300 ℃, cooling to room temperature, and crushing to obtain the environment-friendly inorganic pigment.
Wherein:
the particle size of the product is controlled to be less than or equal to 400 meshes after ball milling.
The roasting is started from room temperature, the temperature is firstly increased to 800 ℃ at the temperature increase rate of 8 ℃/min, the temperature is kept for 1.5h, then the temperature is increased to 1300 ℃ at the temperature increase rate of 5 ℃/min, the temperature is kept for 2h, and finally the mixture is cooled to room temperature at the temperature decrease rate of 3 ℃/min and crushed.
The roasting atmosphere is inert atmosphere.
The particle size of the obtained environment-friendly inorganic pigment is controlled to be 900 meshes after the crushing.
The environment-friendly inorganic pigment prepared by the process is a yellow pigment.
Example 5
The environment-friendly inorganic pigment described in this embodiment 5 is prepared from 55 parts by weight of titanium dioxide, 6 parts by weight of nickel carbonate, 10 parts by weight of cobalt carbonate, 15 parts by weight of cerium oxide, and 2.7 parts by weight of a mineralizer; the cerium oxide is cerium dioxide, and the mineralizer is Li2CO3。
The preparation process of the environment-friendly inorganic pigment described in this embodiment 5 is as follows: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1290 ℃, cooling to room temperature, and crushing to prepare the environment-friendly inorganic pigment.
Wherein:
the particle size of the product is controlled to be less than or equal to 400 meshes after ball milling.
The roasting is started from room temperature, the temperature is firstly increased to 780 ℃ at the heating rate of 8 ℃/min, the temperature is kept for 2h, then the temperature is increased to 1290 ℃ at the heating rate of 5 ℃/min, the temperature is kept for 2.5h, and finally the mixture is cooled to room temperature at the cooling rate of 3 ℃/min and crushed.
The roasting atmosphere is inert atmosphere.
The particle size of the obtained environment-friendly inorganic pigment is controlled to be 1000 meshes after the crushing.
The environment-friendly inorganic pigment prepared by the process is a yellow pigment.
Comparative example 1
The inorganic pigment in the comparative example 1 is the same as the preparation process of the environment-friendly inorganic pigment in the example 1, and the only difference is that the raw materials of the inorganic pigment are different in composition, and the raw materials of the inorganic pigment in the comparative example 1 comprise 55 parts by weight of titanium dioxide and 55 parts by weight of carbonic acid5 parts of nickel, 12 parts of cerium oxide and 2.3 parts of mineralizer; the cerium oxide is cerium dioxide, and the mineralizer is Li2CO3. The finally obtained environment-friendly inorganic pigment is a yellow pigment.
Comparative example 2
The inorganic pigment in the comparative example 2 is the same as the preparation process of the environment-friendly inorganic pigment in the example 1, and has the only difference that the raw material composition of the inorganic pigment is different, and the raw material of the inorganic pigment in the comparative example 2 comprises 55 parts by weight of titanium dioxide, 5 parts by weight of nickel carbonate, 10 parts by weight of cobalt carbonate and 2.6 parts by weight of mineralizer; the mineralizer is Li2CO3(ii) a The finally obtained environment-friendly inorganic pigment is a yellow pigment.
Comparative example 3
The inorganic pigment in the comparative example 3 is the same as the preparation process of the environment-friendly inorganic pigment in the example 1, and has the only difference that the raw materials of the inorganic pigment are different in composition, and the raw materials of the inorganic pigment in the comparative example 3 comprise 55 parts by weight of titanium dioxide, 10 parts by weight of cobalt carbonate, 15 parts by weight of cerium oxide and 2.6 parts by weight of mineralizer; the cerium oxide is cerium dioxide, and the mineralizer is Li2CO3. The finally obtained environment-friendly inorganic pigment is a yellow pigment.
Comparative example 4
The inorganic pigment of comparative example 4 has the same composition as the raw material of the environment-friendly inorganic pigment of example 1, and the only difference is that the temperature is raised from room temperature, the temperature is raised to 1200 ℃ at the temperature raising rate of 8 ℃/min, the temperature is kept for 4h, and then the inorganic pigment is cooled to room temperature at the temperature lowering rate of 3 ℃/min for crushing. The finally obtained environment-friendly inorganic pigment is a yellow pigment.
The inorganic pigments prepared in examples 1 to 5 and comparative examples 1 to 4 were subjected to the performance test, and the results are shown in Table 1 below.
TABLE 1 inorganic pigment Performance test results
Claims (9)
1. An environment-friendly inorganic pigment, which is characterized in that: the raw material consists of titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and mineralizer, wherein the cerium oxide is cerium dioxide, and the mineralizer is Li2CO3。
2. The environmentally friendly inorganic pigment of claim 1, wherein: the raw materials comprise, by weight, 50-55 parts of titanium dioxide, 5-7 parts of nickel carbonate, 5-10 parts of cobalt carbonate, 12-15 parts of cerium oxide and 2.2-2.7 parts of a mineralizer.
3. The environmentally friendly inorganic pigment of any one of claims 1 or 2, wherein: the raw materials comprise, by weight, 55 parts of titanium dioxide, 5 parts of nickel carbonate, 10 parts of cobalt carbonate, 15 parts of cerium oxide and 2.6 parts of mineralizer.
4. A process for preparing an environmentally friendly inorganic pigment according to claim 1, wherein: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1250-.
5. The process for preparing an environmentally friendly inorganic pigment according to claim 4, wherein: the particle size of the product is controlled to be less than or equal to 400 meshes after ball milling.
6. The process for preparing an environmentally friendly inorganic pigment according to claim 4, wherein: the roasting is started to raise the temperature from room temperature, firstly raises the temperature to 800 ℃ at the temperature raising rate of 8 ℃/min, keeps the temperature for 1-2h, then raises the temperature to 1250 ℃ at the temperature raising rate of 5 ℃/min, keeps the temperature for 2-2.5h, and finally cools to room temperature at the temperature lowering rate of 3 ℃/min for crushing.
7. The process for preparing an environmentally friendly inorganic pigment according to claim 4, wherein: the roasting atmosphere is inert atmosphere.
8. The process for preparing an environmentally friendly inorganic pigment according to claim 4, wherein: the particle size of the obtained environment-friendly inorganic pigment is controlled to be 800-1000 meshes after the crushing.
9. The process for preparing an environmentally friendly inorganic pigment according to claim 4, wherein: the environment-friendly inorganic pigment prepared by the process is a yellow pigment.
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| CN115926529A (en) * | 2022-11-23 | 2023-04-07 | 广东金冠科技股份有限公司 | Preparation method of 3D anti-counterfeiting ink |
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| CN115926529A (en) * | 2022-11-23 | 2023-04-07 | 广东金冠科技股份有限公司 | Preparation method of 3D anti-counterfeiting ink |
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