CN113666381A - Preparation method of clay mineral for molecular sieve - Google Patents
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- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
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- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/44—Products obtained from layered base-exchange silicates by ion-exchange with organic compounds such as ammonium, phosphonium or sulfonium compounds or by intercalation of organic compounds, e.g. organoclay material
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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- C01P2006/80—Compositional purity
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Abstract
A preparation method of clay mineral for molecular sieve, in the purification step, the clay mineral is graded by adopting three times of centrifugal operation with different rotating speeds, the difficultly selected trace impurities (hard mineral, ultrafine particle mineral) and coarse particle mineral are removed in sequence, the particle size distribution is controlled, the ore pulp with fine particle size is obtained, and the raw material clay mineral is efficiently purified; in the modification step, the condition of ultrasonic assistance and heating is adopted, the condition of weak acid environment of the system is taken as a premise, the intercalation agent cetyl trimethyl ammonium chloride is added to modify the purified clay ore pulp, the layered structure of the mineral is stripped by ultrasonic, the heating condition accelerates the rate of inserting the cetyl trimethyl ammonium chloride into the layers of the mineral structure, so that the distance between the layers is increased, and finally the clay mineral for the molecular sieve with less metal impurities, large specific surface area and large pore volume is obtained.
Description
Technical Field
The invention belongs to the field of clay mineral processing, and particularly relates to a preparation method of a clay mineral for a molecular sieve.
Background
The clay mineral is the most main mineral component constituting clay rock, and mainly comprises minerals of kaolinite family, illite family, montmorillonite family, vermiculite family, sepiolite family and the like. The clay mineral generally has good ion exchange property, adsorbability, hydration expansibility, fire resistance, suspension property, plasticity and unique electrical, thermal and optical properties, can be widely applied to industries such as building materials, metallurgy, casting, petroleum, chemical engineering, daily use, plastics, rubber, papermaking, coating, chemical fertilizers, feeds, environmental protection, filter aids and the like after being processed, is an indispensable raw material for new technical leathers in China, and plays a significant role in the improvement and upgrading of the traditional industry in China, the formation and development of the new technical industries and the sustainable development of the national economy.
Under the background of "carbon neutralization", molecular sieves, a new material for adsorption and catalysis, are gradually gaining attention.
At present, the feasibility technologies of carbon neutralization have four major paths, namely energy transformation, carbon capture and utilization, low-carbon life and plant carbon sink. In the aspect of carbon capture and utilization, a molecular sieve adsorbent and a catalyst are used for collecting and storing carbon dioxide, so that emission reduction and utilization of industrial carbon are achieved; in the aspect of plant transformation, the zeolite water retention agent and the repairing agent are used for fixing water and the like to carry out soil moisture retention and repair, so as to achieve desert water fixation forestation, saline-alkali soil repair and the like. It is predicted that with the growing growth of new economic entities, the annual growth rate of the worldwide molecular sieve market in 2020-plus 2025 is 5.65%, which will reach $ 43.90 billion in 2025.
In a broad sense, molecular sieves refer to a class of porous materials having a pore size comparable to the size of a molecule and thus having molecular sieving capability; in a narrow sense, molecular sieves refer to crystalline silicates or aluminosilicates, which are porous solids having pore channels ordered in molecular size, i.e., zeolitic molecular sieves, formed from silica tetrahedra or alumina octahedra connected by oxygen bridges.
Clay minerals are one of the main materials for the synthesis of molecular sieves. The clay minerals are non-metal minerals containing silicon and aluminate, such as kaolin, halloysite, montmorillonite, attapulgite, sepiolite and the like, wherein the purity of useful minerals and the content of impurities are important factors influencing the quality of the molecular sieve.
Due to the years of unregulated mining of high quality minerals, non-metallic minerals have become increasingly depleted. In most of clay minerals existing in China, the content of impurities (such as quartz sand, mica, feldspar, magnetite, ilmenite, pyrite and alunite) is high, the difficulty in purifying and removing the impurities of the minerals is high, and metal impurities (such as magnetite, ilmenite, pyrrhotite, hematite, limonite and siderite) are difficult to sufficiently remove, so that the purity of products cannot reach the standard of the clay minerals for molecular sieves, and the requirements of the current high-end market on the specific surface and the pore volume of the clay minerals for molecular sieves are higher and higher.
Disclosure of Invention
The invention provides a preparation method of a clay mineral for a molecular sieve, and aims to solve the problem that a product obtained by the existing preparation method of the clay mineral for the molecular sieve cannot meet high-end market standards.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of clay mineral for molecular sieve is characterized in that: the method comprises the following steps:
firstly, adding a dispersing agent into raw material clay minerals, wherein the addition amount of the dispersing agent is 1-3 per mill of the dry ore amount of the raw material clay minerals, adding water, mixing and fully pulping until particles of the raw material clay minerals are dissociated and are in a monomer separation state, and obtaining raw material ore pulp;
secondly, adding water into the raw material ore pulp for dilution to obtain diluted ore pulp with the solid content of 18-30%, sending the diluted ore pulp into a spiral classifier for continuous stirring, and removing hard minerals at the bottom of the spiral classifier to obtain primarily purified ore pulp;
thirdly, the primarily purified ore pulp is firstly sent into a centrifuge to be sequentially subjected to three times of centrifugal operation:
the first centrifugation is low-speed centrifugation, the rotation speed of the low-speed centrifugation is 1000-;
carrying out second centrifugation operation on the ore pulp left after the low-speed centrifugation, wherein the second centrifugation is medium-speed centrifugation, the rotating speed of the medium-speed centrifugation is 2300 minus one hour (2700 r/min), the medium-speed centrifugation enables the ultrafine particle minerals in the ore pulp to float on the upper layer of the ore pulp, and the ultrafine particle minerals on the upper layer of the ore pulp are separated and taken out so as to separate the ultrafine particle minerals on the upper layer of the ore pulp;
carrying out third centrifugation operation on the ore pulp subjected to medium-speed centrifugation and removing the ultrafine particle minerals, wherein the third centrifugation is high-speed centrifugation, the rotating speed of the high-speed centrifugation is 2900-;
fourthly, concentrating the fine particle ore pulp, adding an intercalation agent of hexadecyl trimethyl ammonium chloride, wherein the addition amount of the intercalation agent of the hexadecyl trimethyl ammonium chloride is 1.5-2.0% of the dry ore amount of the raw material clay mineral, adjusting the pH value to be 5.0-6.2, feeding the mixture into an ultrasonic reaction kettle, continuously stirring the mixture for full reaction for 2-6 hours, increasing the distance of internal lamellar structures of the mineral in the ore pulp under the ultrasonic condition, enabling the intercalation agent of the hexadecyl trimethyl ammonium chloride to be smoothly inserted between the lamellar structures, and enabling the stirring speed of the ultrasonic reaction kettle to be 800-;
fifthly, carrying out filter pressing and dehydration on the ore pulp after the reaction in the fourth step to obtain a filter cake;
sixthly, drying the filter cake prepared in the fifth step at the temperature of 150-;
and seventhly, roasting the powder prepared in the sixth step, heating the powder from room temperature to 400 ℃ at the speed of 9.0-9.5 ℃/min, heating the powder to 700 ℃ at the speed of 7.0-8.0 ℃/min, preserving the temperature for 2 hours at 700 ℃, removing the intercalation agent of hexadecyl trimethyl ammonium chloride, and cooling to obtain the clay mineral for the molecular sieve.
Preferably, the dispersing agent is one or more of water glass, sodium hexametaphosphate and sodium polyacrylate.
Preferably, the weight percentage of the ultrafine particle ore pulp in the third step in the ore pulp subjected to medium-speed centrifugation is 2-3%.
Preferably, sulfuric acid is used to adjust the pH in the fourth step.
Preferably, the hard minerals comprise quartz sand, feldspar, magnetite, pyrite and chlorite.
Preferably, in the fourth step, the fine particle ore pulp is concentrated to a solid content of 40-50%.
Preferably, the three centrifugation operations can be performed in the same centrifuge or in three different centrifuges.
The pulping process is specifically a process of mixing clay minerals and water according to a certain proportion and then fully dispersing the mixture by using a high-speed pulp beater to dissociate mineral monomers, wherein the concentration (solid content) of ore pulp is 18-25%.
The solid content mentioned in the technical scheme refers to the solid content by weight.
The invention has the technical effects that:
1. according to the technical scheme, the clay minerals are graded by three centrifugal operations at different rotating speeds, so that refractory trace impurities (hard minerals and ultrafine particle minerals) and coarse particle minerals are removed in sequence, the particle size distribution is controlled, and ore pulp with fine particle size is obtained. The particle size distribution of the particles in the raw material ore pulp is very wide, and the step effectively purifies the raw material clay minerals and lays a cushion for the modification of the subsequent steps.
2. According to the technical scheme, the modification step adopts the conditions of ultrasonic assistance and heating, on the premise of a weakly acidic system, the intercalation agent cetyl trimethyl ammonium chloride is added to modify the purified clay ore pulp, the layered structure of the mineral is stripped by ultrasonic, and the heating condition accelerates the rate of inserting the cetyl trimethyl ammonium chloride into the layers of the mineral structure, so that the distance between the layers is increased.
3. In the subsequent steps, the hexadecyl trimethyl ammonium chloride is removed by roasting at different sectional heating rates, so that the system can be stably heated without local overheating, and on the other hand, the intercalation agent hexadecyl trimethyl ammonium chloride can be fully decomposed, and the clay mineral for the molecular sieve, which has widened interlayer spacing modification, low metal impurity content and larger specific surface and pore volume, is left.
Detailed Description
The invention is further described below with reference to the following examples:
example (b): preparation method of clay mineral for molecular sieve
1. A preparation method of clay mineral for molecular sieve is characterized in that: the method comprises the following steps:
firstly, adding a dispersing agent into raw material clay minerals, wherein the addition amount of the dispersing agent is 1-3 per mill of the dry ore amount of the raw material clay minerals, adding water, mixing and fully pulping until particles of the raw material clay minerals are dissociated and are in a monomer separation state, and obtaining raw material ore pulp;
secondly, adding water into the raw material ore pulp for dilution to obtain diluted ore pulp with the solid content of 18-30%, sending the diluted ore pulp into a spiral classifier for continuous stirring, and removing hard minerals at the bottom of the spiral classifier to obtain primarily purified ore pulp;
thirdly, the primarily purified ore pulp is firstly sent into a centrifuge to be sequentially subjected to three times of centrifugal operation:
the first centrifugation is low-speed centrifugation, the rotation speed of the low-speed centrifugation is 1000-;
carrying out second centrifugation operation on the ore pulp left after the low-speed centrifugation, wherein the second centrifugation is medium-speed centrifugation, the rotating speed of the medium-speed centrifugation is 2300 minus one hour (2700 r/min), the medium-speed centrifugation enables the ultrafine particle minerals in the ore pulp to float on the upper layer of the ore pulp, and the ultrafine particle minerals on the upper layer of the ore pulp are separated and taken out so as to separate the ultrafine particle minerals on the upper layer of the ore pulp;
carrying out third centrifugation operation on the ore pulp subjected to medium-speed centrifugation and removing the ultrafine particle minerals, wherein the third centrifugation is high-speed centrifugation, the rotating speed of the high-speed centrifugation is 2900-;
fourthly, concentrating the fine particle ore pulp, adding an intercalation agent of hexadecyl trimethyl ammonium chloride, wherein the addition amount of the intercalation agent of the hexadecyl trimethyl ammonium chloride is 1.5-2.0% of the dry ore amount of the raw material clay mineral, adjusting the pH value to be 5.0-6.2, feeding the mixture into an ultrasonic reaction kettle, continuously stirring the mixture for full reaction for 2-6 hours, increasing the distance of internal lamellar structures of the mineral in the ore pulp under the ultrasonic condition, enabling the intercalation agent of the hexadecyl trimethyl ammonium chloride to be smoothly inserted between the lamellar structures, and enabling the stirring speed of the ultrasonic reaction kettle to be 800-;
fifthly, carrying out filter pressing and dehydration on the ore pulp after the reaction in the fourth step to obtain a filter cake;
sixthly, drying the filter cake prepared in the fifth step at the temperature of 150-;
and seventhly, roasting the powder prepared in the sixth step, heating the powder from room temperature to 400 ℃ at the speed of 9.0-9.5 ℃/min, heating the powder to 700 ℃ at the speed of 7.0-8.0 ℃/min, preserving the temperature for 2 hours at 700 ℃, removing the intercalation agent of hexadecyl trimethyl ammonium chloride, and cooling to obtain the clay mineral for the molecular sieve.
The dispersing agent is one or more of water glass, sodium hexametaphosphate and sodium polyacrylate.
The weight percentage of the ultrafine particle ore pulp in the third step is 2-3% of the ore pulp subjected to medium-speed centrifugation.
In the fourth step, sulfuric acid is used to adjust the pH.
The hard minerals comprise quartz sand, feldspar, magnetite, pyrite and chlorite.
In the fourth step, the fine particle pulp is concentrated to a solid content of 40-50%.
The three centrifugation operations can be performed in the same centrifuge or in three different centrifuges.
Table 1 below shows the rotation speeds used by the first centrifuge (low-speed centrifugation), the second centrifuge (medium-speed centrifugation), and the third centrifuge (high-speed centrifugation) in the third step, as well as D50 of the slurry after removing the residual hard minerals (slurry obtained after the first centrifuge is centrifuged), D50 of the slurry after separating the extremely fine particle minerals (slurry obtained after the second centrifuge is centrifuged), and D50 of the fine particle slurry (slurry obtained after the third centrifuge is centrifuged).
TABLE 1 centrifuge rotational speed and corresponding particle size results
| Item | The rotating speed is 1200r/min | Rotating speed of 2500 r/min | Rotating speed 3120 r/min |
| Particle size (-2 μm) | 75 | 85 | 95 |
| D50(μm) | 5.0 | 3.5 | 1.2 |
Fully separating harmful impurities and clay minerals through a first step, a second step and a third step, and separating out coarse-particle clay minerals to finally obtain superfine clay ore pulp with the purity of more than 98 percent and the content of-2 mu m (the content of mineral particles less than 2 microns) of 95 percent;
the clay mineral for the molecular sieve prepared by the technical scheme has low content of metal impurities (Fe)2O3＜0.2%，TiO2＜0.02%，K2O＜0.06%，Na2O is less than 0.02 percent) and has a larger specific surface (100-220 m)2Per g) and pore volume (0.5 cm)3/g）。
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (7)
1. A preparation method of clay mineral for molecular sieve is characterized in that: the method comprises the following steps:
firstly, adding a dispersing agent into raw material clay minerals, wherein the addition amount of the dispersing agent is 1-3 per mill of the dry ore amount of the raw material clay minerals, adding water, mixing and fully pulping until particles of the raw material clay minerals are dissociated and are in a monomer separation state, and obtaining raw material ore pulp;
secondly, adding water into the raw material ore pulp for dilution to obtain diluted ore pulp with the solid content of 18-30%, sending the diluted ore pulp into a spiral classifier for continuous stirring, and removing hard minerals at the bottom of the spiral classifier to obtain primarily purified ore pulp;
thirdly, the primarily purified ore pulp is firstly sent into a centrifuge to be sequentially subjected to three times of centrifugal operation:
the first centrifugation is low-speed centrifugation, the rotation speed of the low-speed centrifugation is 1000-;
carrying out second centrifugation operation on the ore pulp left after the low-speed centrifugation, wherein the second centrifugation is medium-speed centrifugation, the rotating speed of the medium-speed centrifugation is 2300 minus one hour (2700 r/min), the medium-speed centrifugation enables the ultrafine particle minerals in the ore pulp to float on the upper layer of the ore pulp, and the ultrafine particle minerals on the upper layer of the ore pulp are separated and taken out so as to separate the ultrafine particle minerals on the upper layer of the ore pulp;
carrying out third centrifugation operation on the ore pulp subjected to medium-speed centrifugation and removing the ultrafine particle minerals, wherein the third centrifugation is high-speed centrifugation, the rotating speed of the high-speed centrifugation is 2900-;
fourthly, concentrating the fine particle ore pulp, adding an intercalation agent of hexadecyl trimethyl ammonium chloride, wherein the addition amount of the intercalation agent of the hexadecyl trimethyl ammonium chloride is 1.5-2.0% of the dry ore amount of the raw material clay mineral, adjusting the pH value to be 5.0-6.2, feeding the mixture into an ultrasonic reaction kettle, continuously stirring the mixture for full reaction for 2-6 hours, increasing the distance of internal lamellar structures of the mineral in the ore pulp under the ultrasonic condition, enabling the intercalation agent of the hexadecyl trimethyl ammonium chloride to be smoothly inserted between the lamellar structures, and enabling the stirring speed of the ultrasonic reaction kettle to be 800-;
fifthly, carrying out filter pressing and dehydration on the ore pulp after the reaction in the fourth step to obtain a filter cake;
sixthly, drying the filter cake prepared in the fifth step at the temperature of 150-;
and seventhly, roasting the powder prepared in the sixth step, heating the powder from room temperature to 400 ℃ at the speed of 9.0-9.5 ℃/min, heating the powder to 700 ℃ at the speed of 7.0-8.0 ℃/min, preserving the temperature for 2 hours at 700 ℃, removing the intercalation agent of hexadecyl trimethyl ammonium chloride, and cooling to obtain the clay mineral for the molecular sieve.
2. The method of claim 1, wherein: the dispersing agent is one or more of water glass, sodium hexametaphosphate and sodium polyacrylate.
3. The method of claim 1, wherein: the weight percentage of the ultrafine particle ore pulp in the third step is 2-3% of the ore pulp subjected to medium-speed centrifugation.
4. The method of claim 1, wherein: in the fourth step, sulfuric acid is used to adjust the pH.
5. The method of claim 1, wherein: the hard minerals comprise quartz sand, feldspar, magnetite, pyrite and chlorite.
6. The method of claim 1, wherein: in the fourth step, the fine particle pulp is concentrated to a solid content of 40-50%.
7. The method of claim 1, wherein: the three centrifugation operations can be performed in the same centrifuge or in three different centrifuges.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103289447A (en) * | 2012-02-24 | 2013-09-11 | 中国矿业大学(北京) | Dissociation method of coal-series hard kaolinite rock lamella |
| CN103482639A (en) * | 2013-09-27 | 2014-01-01 | 中国矿业大学(北京) | Preparation method of kaolinite/quaternary ammonium salt intercalation compound |
| CN109627425A (en) * | 2018-12-29 | 2019-04-16 | 苏州国建慧投矿物新材料有限公司 | A kind of modified alta-mud/epoxy resin composite material and preparation method thereof |
| CN110801813A (en) * | 2019-09-29 | 2020-02-18 | 浙江工业大学 | Preparation method of hexadecyl trimethyl ammonium bromide modified montmorillonite |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103289447A (en) * | 2012-02-24 | 2013-09-11 | 中国矿业大学(北京) | Dissociation method of coal-series hard kaolinite rock lamella |
| CN103482639A (en) * | 2013-09-27 | 2014-01-01 | 中国矿业大学(北京) | Preparation method of kaolinite/quaternary ammonium salt intercalation compound |
| CN109627425A (en) * | 2018-12-29 | 2019-04-16 | 苏州国建慧投矿物新材料有限公司 | A kind of modified alta-mud/epoxy resin composite material and preparation method thereof |
| CN110801813A (en) * | 2019-09-29 | 2020-02-18 | 浙江工业大学 | Preparation method of hexadecyl trimethyl ammonium bromide modified montmorillonite |
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