CN111232996A - Low-temperature calcination whitening process for talc ore, product and application thereof - Google Patents

Low-temperature calcination whitening process for talc ore, product and application thereof Download PDF

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CN111232996A
CN111232996A CN202010066331.0A CN202010066331A CN111232996A CN 111232996 A CN111232996 A CN 111232996A CN 202010066331 A CN202010066331 A CN 202010066331A CN 111232996 A CN111232996 A CN 111232996A
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talc
ore
low
temperature
stirring
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李旭娟
王茜
蔡宗佐
王玉琪
赵春雪
冯启明
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Southwest University of Science and Technology
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    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates
    • C01B33/22Magnesium silicates
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    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values

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  • Inorganic Chemistry (AREA)
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Abstract

The invention relates to the technical field of talc whitening technology, in particular to a low-temperature calcination whitening technology of talc ore, a product and application thereof, wherein the whitening technology comprises the following steps: crushing talc raw ore, and mixing the crushed talc raw ore with water to prepare ore pulp I; adding organic acid into the ore pulp I, heating and stirring to obtain ore pulp II; adding sodium chloride into the ore pulp II, uniformly stirring, and then filtering to obtain a filter material; calcining the filter material, naturally cooling to normal temperature, and taking out to obtain talcum powder; the low-temperature calcining whitening process has the advantages of high efficiency, environmental friendliness, simplicity in operation, no residual ions in the product and the like, and can be used for preparing talcum powder applied to plastics, medicines, foods, cosmetics or coatings.

Description

Low-temperature calcination whitening process for talc ore, product and application thereof
Technical Field
The invention relates to the technical field of talc whitening processes, in particular to a low-temperature calcination whitening process of talc ore, and a product and application thereof.
Background
Non-metallic mineral materials have a wide range of uses in modern industry and national economy. The reserves of limestone, kaolin, graphite, talc and other mineral species in China are in the forefront of the world, and talc is an important nonmetallic mineral raw material. Talc is a hydrous layered silicate mineral, and is widely used in industries such as paper making, cosmetics, daily chemical industry, ceramics, plastics, building materials, rubber, and medicine because of its excellent electrical insulation, heat resistance, chemical stability, lubricity, oil absorption, covering power, and machinability. The whiteness of the talc is taken as an important index in most industries, and high whiteness and high purity are required. However, the high-quality talc resources with high whiteness and purity in China are few, 70% of the current talc resources are medium-low grade talc, and the whiteness of the talc resources cannot meet the use requirements and cannot be effectively utilized, so that a large amount of resources are wasted. Therefore, how to obtain high-quality talc with high whiteness by using the middle-grade and low-grade talc ore as a raw material has important significance for relieving the situation of short supply and short demand of the current market of high-grade talc resources and promoting the technical progress of talc industry in China.
At present, the talc whitening method includes calcination, bleaching agent, ore mixing, acid leaching, iron removal, calcium oxide removal and the like, and the calcination process is mainly used to obtain the talc with high whiteness at present. For example, the patent "process for preparing high-whiteness superfine talc powder from black talc" (application No. 200610101218.1), "a whitening method for black talc" (application No. 200910061358.4), "a method for preparing high-whiteness superfine talc powder from black talc" (application No. 201410504296.0) all adopt a calcination process to improve the whiteness of talc. However, the calcination temperature in the above processes is higher than the phase transition temperature (850 ℃) of talc, and the talc phase is transformed into enstatite with higher hardness (Mohs hardness 5.5) in the calcination process, so that the talc loses the characteristics of low hardness, lubricity, greasy feeling and the like, and cannot be applied to the fields requiring the use of the talc property, such as plastics, medicines, foods, cosmetics, coatings and the like, and the due value of the talc is lost. In this regard, the patent "a method for whitening low whiteness talc with the removal of calcium oxide" (application No. 201310476498.4) has been explored for obtaining high whiteness talc having talc characteristics. But the process is not environment-friendly and has health risks, such as volatile hydrochloric acid and is not friendly to equipment and operators; the sodium hydrosulfite is a strong oxidant, is inflammable, has irritation to eyes, respiratory tract and skin, and can cause the harm of headache, nausea, vomiting and the like. Recently, the patent "a calcining and apparatus for producing high-whiteness low-hardness talc using black talc" (accession number CN 206940443U) modified the calcining process to achieve low-temperature calcination of black talc by establishing oxidizing atmosphere conditions using an oxygen supply apparatus. However, this process is only applicable to the black talc ore containing only organic carbon. When the talc ore contains elements such as Fe, the talc powder is reddened by the oxidizing atmosphere, and the whiteness of the talc powder is affected. Therefore, a low-temperature whitening technology which is efficient in process, environment-friendly and universal is still to be explored.
Disclosure of Invention
The invention aims to provide a low-temperature calcining and whitening process of talc ore, a product and application thereof, and the process has the advantages of high efficiency, environmental friendliness, simplicity in operation and the like.
The technical purpose of the invention is realized by the following technical scheme:
a low-temperature calcining and whitening process of talc ore; the method comprises the following steps:
(1) crushing talc raw ore, and mixing the crushed talc raw ore with water to prepare ore pulp I;
(2) adding organic acid into the ore pulp I, heating and stirring to obtain ore pulp II;
(3) adding sodium chloride into the ore pulp II, uniformly stirring, and then filtering to obtain a filter material;
(4) and calcining the filter material, naturally cooling to normal temperature, and taking out to obtain the talcum powder.
Further, the whiteness of the talc raw ore in the step (1) is 25-60, and the granularity of the pulverized talc raw ore is 80-5000 meshes. The smaller the particle size, the higher the whiteness after calcination, the wider the application field of the talc powder prepared by the invention, can further limit the particle size of the talc raw ore according to the requirements of the specific application field, when used in the fields of cosmetics and medicine, the smaller the particle size of the talc raw ore is in the range value, and when used in the fields of plastics, coatings and the like, the larger the particle size of the talc raw ore is in the range value.
Further, in the step (1), the mass ratio of the talc raw ore to the water is 1: 4-8. The addition of water enables the talc raw ore to be uniformly mixed, and the subsequent steps of acidification, iron removal and the like are facilitated to be smoothly carried out.
Further, in the step (2), the mass ratio of the organic acid to the talc raw ore is 1-4:100, and the organic acid comprises at least one of formic acid, acetic acid and tartaric acid. The organic acid is added to remove iron in the talc raw ore, the organic acid has a bleaching effect, and compared with hydrochloric acid in the prior art, the organic acid is not easy to volatilize and is environment-friendly, and meanwhile, the residual organic acid is combusted in the subsequent calcining process and cannot be remained in the talc powder.
Further, in the step (2), the heating and stirring temperature is 40-100 ℃, and the heating and stirring time is 1-5 hours. Under the heating condition, the organic acid is ensured not to be volatilized, the reaction speed of the organic acid and the iron in the talc raw ore is promoted, and the iron in the talc raw ore is removed quickly and efficiently.
Further, in the step (3), the mass ratio of the sodium chloride to the talc raw ore is 1-4:100, and the stirring time is 2-15 minutes. The sodium chloride is used for removing iron in the talc raw ore, and the addition amount of the sodium chloride can be adaptively adjusted according to the whiteness and the like of the talc raw ore.
Further, in the step (4), the calcining temperature is 500-800 ℃, and the calcining time is 1-8 hours. The whiteness of the talcum powder is improved under the condition of keeping the mineral phase of the talcum unchanged due to the limitation of the calcining temperature, and in the calcining process in the prior art, dolomite is completely decomposed at the temperature of 850 ℃, and the talcum starts to generate phase change. With the rise of temperature, the phase of the talc is completely changed to generate enstatite; decomposition products of dolomite, respectively with SiO2The reaction produces enstatite and calcium silicate. After firing at 1150 ℃, the main phases in the sample are: enstatite, calcium silicate and silica. Further, the prior artThe calcination temperature is increased, although the whiteness of the talcum powder is further improved, the phase of the talcum powder is changed, the prepared talcum powder is not talc, and the characteristics of low hardness, lubricity, good greasy feeling and the like of the talc are lost.
Furthermore, the talcum powder is prepared by the low-temperature calcining and whitening process of the talc ore, and the whiteness of the talcum powder is 85-95.
Furthermore, the talcum powder prepared by the low-temperature calcining and whitening process is applied to the fields of plastics, medicines, foods, cosmetics or coatings.
Further, the filter material calcined in the step (4) is cooled to normal temperature, wherein the normal temperature is also called general temperature or room temperature, and is generally defined as 25 ℃, in the scheme, the filter material with high temperature after calcination is only required to be cooled to relatively lower temperature, and the temperature range specifically referred to at the normal temperature is not limited.
The acid can react with metals such as Fe and the like which cause color or metal oxides which cause color, so that the whiteness of the talc is improved; when the organic acid is used for replacing the inorganic acid, the organic acid interacts with the blackened organic carbon to play an activating role, so that the organic carbon is further promoted to be decomposed at low temperature, and the aim of improving the whiteness of the talc at lower calcining temperature is fulfilled.
The invention has the beneficial effects that:
1. the use of the organic acid is environment-friendly, the damage degree (corrosion) to equipment and machines is small, and the waste liquid is well treated;
2. the process can keep the phase of the talc unchanged and keep the original characteristics of the talc;
3. the invention has the advantages of simple process flow, low production cost, less impurity residue in the product and the like;
4. the whiteness of the talc ore prepared by the invention meets the application requirements of most fields, and is beneficial to expanding the application of low-grade talc resources in industries such as cosmetics, plastics, medicines and the like in China.
Drawings
FIG. 1 is an XRD pattern of talc ore calcined at 750 deg.C;
figure 2 is an XRD pattern of talc ore calcined at 850 deg.c.
Detailed Description
The technical effects of the present invention will be specifically described below by way of examples. It should be noted that the following examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as many insubstantial modifications and variations of the invention may be made by those skilled in the art without departing from the spirit and scope of the invention.
Example 1
A low-temperature calcining and whitening process of talc ore; the method comprises the following steps:
(1) pulverizing talc raw ore with whiteness of 34 into 80 meshes, weighing 100 g of raw ore, adding 400 g of water, and stirring for 10 minutes to prepare ore pulp I;
(2) adding 4 g of acetic acid into the ore pulp I, heating to 40 ℃, and stirring for 1 hour to obtain ore pulp II;
(3) adding 4 g of sodium chloride into the ore pulp II, stirring for 15 minutes, and then filtering to obtain a filter material;
(4) calcining the filter material at 800 ℃ for 8 hours, naturally cooling to normal temperature, and taking out to obtain the talcum powder.
The whiteness of the talcum powder is measured to be 92 degrees, the yield is 98 percent, the Fe content in the talcum powder is 0.011 percent, and the chlorine residual quantity is 0.21 percent.
Example 2
A low-temperature calcining and whitening process of talc ore; the method comprises the following steps:
(1) crushing talc raw ore with the whiteness of 47 to 100 meshes, weighing 100 g of raw ore, adding 400 g of water, and stirring for 10 minutes to prepare ore pulp I;
(2) adding 3.5 g of acetic acid into the ore pulp I, heating to 60 ℃, and stirring for 2 hours to obtain ore pulp II;
(3) adding 3 g of sodium chloride into the ore pulp II, stirring for 4 minutes, and then filtering to obtain a filter material;
(4) and calcining the filter material at 750 ℃ for 6 hours, naturally cooling to normal temperature, and taking out to obtain the talcum powder.
The whiteness of the talcum powder is 91 degrees, the yield is 97 percent, the Fe content in the talcum powder is 0.010 percent, and the residual chlorine content is 0.09 percent.
Example 3
A low-temperature calcining and whitening process of talc ore; the method comprises the following steps:
(1) crushing talc raw ore with the whiteness of 25 into 120 meshes, weighing 100 g of raw ore, adding 400 g of water, and stirring for 10 minutes to prepare ore pulp I;
(2) adding 2.5 g of formic acid into the ore pulp I, heating to 80 ℃, and stirring for 3 hours to obtain ore pulp II;
(3) adding 2.5 g of sodium chloride into the ore pulp II, stirring for 8 minutes, and then filtering to obtain a filter material;
(4) and calcining the filter material at 700 ℃ for 4 hours, naturally cooling to normal temperature, and taking out to obtain the talcum powder.
The whiteness of the talc powder was found to be 88 degrees, the yield was found to be 97%, and the residual chlorine content in the talc powder was found to be 0.15%.
Example 4
A low-temperature calcining and whitening process of talc ore; the method comprises the following steps:
(1) pulverizing talc raw ore with whiteness of 32 to 150 meshes, weighing 100 g of raw ore, adding 400 g of water, and stirring for 10 minutes to prepare ore pulp I;
(2) adding 2 g of formic acid into the ore pulp I, heating to 100 ℃, and stirring for 4 hours to obtain ore pulp II;
(3) adding 2 g of sodium chloride into the ore pulp II, stirring for 5 minutes, and then filtering to obtain a filter material;
(4) and calcining the filter material at 500 ℃ for 3 hours, naturally cooling to normal temperature, and taking out to obtain the talcum powder.
The whiteness of the talc powder was found to be 89 degrees, the yield was found to be 98%, and the residual chlorine content in the talc powder was found to be 0.16%.
Example 5
A low-temperature calcining and whitening process of talc ore; the method comprises the following steps:
(1) pulverizing talc raw ore with whiteness of 32 to 180 meshes, weighing 100 g of raw ore, adding 400 g of water, and stirring for 10 minutes to prepare ore pulp I;
(2) adding 1 g of organic acid into the ore pulp I, heating to 60 ℃, and stirring for 5 hours to obtain ore pulp II;
(3) adding 1 g of sodium chloride into the ore pulp II, stirring for 10 minutes, and then filtering to obtain a filter material;
(4) calcining the filter material at 800 ℃ for 1 hour, naturally cooling to normal temperature, and taking out to obtain the talcum powder.
The whiteness of the talcum powder is measured to be 90 degrees, the yield is 96 percent, and the residual chlorine content in the talcum powder is 0.08 percent.
Example 6
A low-temperature calcining and whitening process of talc ore; the method comprises the following steps:
(1) pulverizing talc raw ore with whiteness of 43 to 4500 meshes, weighing 100 g of raw ore, adding 400 g of water, and stirring for 10 minutes to prepare ore pulp I;
(2) adding 2 g of organic acid into the ore pulp I, heating to 55 ℃, and stirring for 1 hour to obtain ore pulp II;
(3) adding 1 g of sodium chloride into the ore pulp II, stirring for 10 minutes, and then filtering to obtain a filter material;
(4) and calcining the filter material at 750 ℃ for 3.5 hours, naturally cooling to normal temperature, and taking out to obtain the talcum powder.
The whiteness of the talcum powder is measured to be 92 degrees, the yield is 96 percent, and the residual chlorine content in the talcum powder is 0.06 percent.
Example 7
A low-temperature calcining and whitening process of talc ore; the method comprises the following steps:
(1) pulverizing talc raw ore with whiteness of 58 to 2500 meshes, weighing 100 g of raw ore, adding 400 g of water, and stirring for 10 minutes to prepare ore pulp I;
(2) adding 1.5 g of organic acid into the ore pulp I, heating to 60 ℃, and stirring for 2 hours to obtain ore pulp II;
(3) adding 2 g of sodium chloride into the ore pulp II, stirring for 15 minutes, and then filtering to obtain a filter material;
(4) calcining the filter material at 800 ℃ for 3 hours, naturally cooling to normal temperature, and taking out to obtain the talcum powder.
The whiteness of the talc was measured to be 93 degrees, the yield was 98%, and the chlorine residue in the talc was 0.17%.
Comparative example 1
The acetic acid in step (2) in example 1 was replaced with hydrochloric acid, and the remaining steps and experimental parameters were identical to those of example 1; the whiteness of the finally prepared talcum powder is 91 degrees, the yield is 97 percent, and the residual chlorine content in the talcum powder is 2.3 percent.
Comparative example 2
The calcination temperature in step (4) in example 1 was replaced with 850 ℃, and the remaining steps and experimental parameters were consistent with those of example 1; the whiteness of the finally prepared talcum powder is 93 degrees, the yield is 98 percent, and the residual chlorine content in the talcum powder is 0.9 percent.
The above embodiments are merely preferred embodiments of the present invention, which are provided for illustrating the technical solutions of the present invention and not for limiting the same, and it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the present invention, and all of them should be covered by the protection scope of the present invention.

Claims (9)

1. The low-temperature calcination whitening process of the talc ore is characterized by comprising the following steps of:
(1) crushing talc raw ore, and mixing the crushed talc raw ore with water to prepare ore pulp I;
(2) adding organic acid into the ore pulp I, heating and stirring to obtain ore pulp II;
(3) adding sodium chloride into the ore pulp II, uniformly stirring, and then filtering to obtain a filter material;
(4) and calcining the filter material, naturally cooling to normal temperature, and taking out to obtain the talcum powder.
2. The low-temperature calcination whitening process for talc ore according to claim 1, wherein the whiteness of talc raw ore in step (1) is 25-60, and the particle size of pulverized talc raw ore is 80-5000 mesh.
3. The low-temperature calcination whitening process for talc ore according to claim 1, wherein the mass ratio of talc raw ore to water in step (1) is 1: 4-8.
4. The low-temperature calcination whitening process for talc ore according to claim 1, wherein in step (2), the mass ratio of organic acid to talc raw ore is 1-4:100, and the organic acid comprises at least one of formic acid, acetic acid and tartaric acid.
5. The low-temperature calcination whitening process for talc ore according to claim 1, wherein the temperature of heating and stirring in step (2) is 40-100 ℃ and the time of heating and stirring is 1-5 hours.
6. The low-temperature calcination whitening process for talc ore according to claim 1, wherein in step (3), the mass ratio of sodium chloride to talc raw ore is 1-4:100, and the stirring time is 2-15 minutes.
7. The low-temperature calcination whitening process for talc ore according to claim 1, wherein in step (4), the calcination temperature is 500 ℃ to 800 ℃ and the calcination time is 1 to 8 hours.
8. Talc powder prepared by the low-temperature calcination and whitening process of talc ore according to any one of claims 1 to 7, wherein the whiteness of the talc powder is 85 to 95.
9. Use of talc according to claim 8 in the field of plastics, medicine, food, cosmetics or coatings.
CN202010066331.0A 2020-01-20 2020-01-20 Low-temperature calcination whitening process for talc ore, product and application thereof Pending CN111232996A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN116375045A (en) * 2023-03-21 2023-07-04 东北大学 Low-whiteness talcum low-temperature calcination whitening method

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CN116375045A (en) * 2023-03-21 2023-07-04 东北大学 Low-whiteness talcum low-temperature calcination whitening method

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