CN117446815A - Method for preparing montmorillonite with low ferric oxide content and application thereof - Google Patents

Method for preparing montmorillonite with low ferric oxide content and application thereof Download PDF

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Publication number
CN117446815A
CN117446815A CN202311470709.3A CN202311470709A CN117446815A CN 117446815 A CN117446815 A CN 117446815A CN 202311470709 A CN202311470709 A CN 202311470709A CN 117446815 A CN117446815 A CN 117446815A
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montmorillonite
oxide content
ion exchange
bentonite
iron oxide
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钟富
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Foshan Shunde District Topcod Industrial Co ltd
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Foshan Shunde District Topcod Industrial Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates
    • C01B33/36Silicates having base-exchange properties but not having molecular sieve properties
    • C01B33/38Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
    • C01B33/40Clays
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12Naturally occurring clays or bleaching earth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03CMAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00Magnetic separation
    • B03C1/02Magnetic separation acting directly on the substance being separated
    • B03C1/30Combinations with other devices, not otherwise provided for
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Abstract

The application relates to the field of drying agents, and particularly discloses a method for manufacturing montmorillonite with low ferric oxide content and application thereof. The preparation process of montmorillonite with low ferric oxide content includes milling, pulping, eliminating Dan Chutie, natural settling, oxidizing, press filtering, stoving, sieving and magnetic separation. The method for manufacturing montmorillonite with low ferric oxide content can be used for clothes drying agents, and has the advantage of low ferric oxide content.

Description

Method for preparing montmorillonite with low ferric oxide content and application thereof
Technical Field
The application relates to the field of drying agents, in particular to a method for manufacturing montmorillonite with low ferric oxide content and application thereof.
Background
Montmorillonite desiccant is a common absorbent product in life that helps us keep clothes, shoes and storage spaces dry. Montmorillonite is a natural mineral, and is widely used because of its excellent moisture absorption properties. In wet seasons or in wet environments, laundry is easily wet and mold grows, which may cause bad smell and damage to the laundry. To avoid these problems, we can use montmorillonite desiccant to absorb moisture in the air, keeping the clothes dry.
Montmorillonite desiccants have many advantages. Firstly, it is a natural non-toxic product, is harmless to human body, and does not have any harmful effect on clothes. Secondly, the montmorillonite drying agent has good moisture absorption effect, can continuously keep the drying of clothes, and effectively prevents mold from breeding and peculiar smell from generating. In addition, the montmorillonite drying agent is convenient to use, and can play a role only by being placed in a place for storing clothes.
After the clothing is manufactured, a clothing manufacturer usually adds a bagged drying agent into the package so as to prevent the clothing from getting moldy, deforming or generating peculiar smell and the like caused by wetting. However, in performing laundry detection, it is necessary to use a needle detector to detect whether there is a residual needle in the laundry. The working principle of the needle detector is that the electromagnetic induction principle is utilized to detect metal objects, and if the iron oxide content in the drying agent is higher, the needle detector can misjudge that a needle exists, so that the product is unqualified. There is a need for a montmorillonite desiccant having a low iron oxide content.
Disclosure of Invention
In order to reduce the ferric oxide content of montmorillonite, the application provides a method for manufacturing montmorillonite with low ferric oxide content and application thereof.
The method for manufacturing the montmorillonite with low ferric oxide content adopts the following technical scheme:
a method for producing montmorillonite with a low iron oxide content, comprising the steps of:
s1, grinding: grinding bentonite ore;
s2, pulping: mixing the ground bentonite with water according to the formula 1 (1-5) to form bentonite slurry;
s3, removing Dan Chutie: removing stones and ferromagnetic impurities in the bentonite slurry through a 100-150 mesh sieve;
s4, natural sedimentation: standing bentonite slurry after removing the stones and the iron for 8-12h to enable solid particles to be precipitated to the bottom;
s5, oxidation treatment: adding hydrogen peroxide into bentonite slurry, wherein the addition amount of the hydrogen peroxide is 5-10% of the mass of the bentonite slurry, keeping the temperature at 20-30 ℃, stirring for 2-4 hours at the stirring speed of 50-100r/min, standing for 1-2 hours, removing solid precipitate particles at the bottom after standing, separating supernatant from wet precipitate by a centrifuge, and cleaning the wet precipitate for 2-3 times by using deionized water to obtain montmorillonite slurry;
s6, filter pressing: packing montmorillonite slurry in filter cloth, and performing filter pressing by a filter press for 10-14 hours;
s7, drying: drying the montmorillonite subjected to filter pressing;
s8, screening: sieving with 150-200 mesh sieve;
s9, magnetic separation: and (3) placing the sieved montmorillonite into a magnetic separator to adsorb magnetic impurities, so as to obtain the montmorillonite with low ferric oxide content.
By adopting the technical scheme, the existence of impurities can be effectively reduced and the purity of montmorillonite can be improved as stones and ferromagnetic impurities are removed through sieving; oxygen atoms (OH) generated by the decomposition of hydrogen peroxide react with ferric oxide ions (Fe & lt3+ & gt) on the surface of ferric oxide to generate high-valence oxides of ferric oxide, the high-valence oxides precipitate in a solution, impurities such as ferric oxide in montmorillonite slurry are separated from supernatant liquid through the operation of removing solid precipitate particles at the bottom after standing, and therefore, the content of ferric oxide in montmorillonite is reduced; the sieved montmorillonite is put into a magnetic separator to adsorb magnetic impurities, so that the montmorillonite can be further purified, and the purity and quality of the montmorillonite are improved. By the method, the content of ferric oxide in the montmorillonite can be effectively reduced, and Fe is added 2 O 3 The content is reduced to below 1.0%, the requirement of the needle checking machine is met, and the montmorillonite after moisture absorption can be reused after baking, so that the montmorillonite has better comprehensive performance compared with salt desiccant and silica gel.
Optionally, the granularity of the bentonite after grinding in the step S1 is 30-80 μm.
By adopting the technical scheme, the content of ferric oxide in bentonite can be effectively controlled by controlling the grinding granularity of bentonite particles to be within 30-80 mu m. The smaller particle size helps to reduce the iron oxide content and provides a low iron oxide content montmorillonite product.
Optionally, a suspending agent is further added in the step S4, and the suspending agent comprises one or more of polyacrylamide, carboxymethyl cellulose and activated carbon.
By adopting the technical scheme, the dispersion and suspension stability of montmorillonite particles in the solution can be enhanced by adding the suspending agent. The suspending agents such as polyacrylamide, carboxymethyl cellulose, active carbon and the like have the adsorption and water absorption capacity, and can form a stable suspension system with bentonite particles. This helps to prevent particle deposition and agglomeration and improves product uniformity and stability. The suspending agents such as polyacrylamide, carboxymethyl cellulose and the like have higher viscosity and adhesion property. The viscosity of the solution can be regulated, the flow property is changed, and the sedimentation speed and the mixing uniformity of montmorillonite particles are favorably controlled. The activated carbon has stronger adsorption capacity. It can adsorb impurities and organic matters in the solution, purify the surface of montmorillonite particles, and improve the purity and quality of the product.
Optionally, in the step S5, after separating the supernatant from the wet precipitate by using a centrifuge, the separated wet precipitate is further subjected to an ion exchange treatment, and the ion exchange treatment adsorbs the iron oxide particles by using a resin.
By adopting the technical scheme, the ion exchange treatment can effectively remove the residual ferric oxide particles in the wet precipitate by using the ion exchange resin. The ion exchange resin has certain selectivity, and can selectively adsorb ferric oxide ions and carry out ion exchange reaction with the ferric oxide ions. Thus, the iron oxide content in the montmorillonite product can be obviously reduced, and the requirement of low iron oxide content is met. Iron oxide particles are adsorbed onto the resin by ion exchange treatment, thereby purifying the montmorillonite product. This helps to improve the purity of the product and remove impurities and impurities.
Optionally, the specific steps of the ion exchange treatment are as follows:
a1, adding ion exchange resin into the wet precipitate, stirring to enable the ion exchange resin to fully contact with the wet precipitate, and keeping the temperature at 30-50 ℃ and standing for 4-8h;
a2, after standing, separating bentonite slurry from the ion exchange resin through filtration and centrifugal treatment;
a3, washing the ion exchange resin by using a salt solution to remove impurities attached to the surface of the ion exchange resin;
and A4, eluting the ion exchange resin by using ethylenediamine tetraacetic acid, and collecting the ferric oxide eluted from the resin.
By adopting the technical scheme, the ferric oxide particles in the wet precipitate can be effectively adsorbed and removed through the steps of contact, standing, separation, washing, elution and the like. Therefore, the purity and stability of the montmorillonite can be improved, and the requirement of low ferric oxide content can be met. And the ferric oxide eluted from the resin can be recycled after being collected, so that the method has an environmental protection value.
Optionally, after the ion exchange treatment in the step S5 is completed, an alkaline washing treatment is further performed, and the specific operation process of the alkaline washing treatment is as follows: soaking montmorillonite slurry in 0.1-1% sodium hydroxide solution, maintaining at 24-50deg.C for 2-4 hr, and washing and separating.
By adopting the technical scheme, the alkaline washing treatment can effectively remove impurities in the wet precipitate. The sodium hydroxide can perform neutralization reaction with acidic impurities in the wet precipitate to change the acidic impurities into salts or water-soluble substances, thereby removing the impurities. The alkaline washing treatment helps to improve the purity of the montmorillonite product by removing impurities.
Optionally, the step S7 is performed with high-temperature steam treatment after drying, and the step S7 is performed with secondary drying after the high-temperature steam treatment.
By adopting the technical scheme, the high-temperature steam treatment can play roles in cleaning and sterilizing. The high-temperature steam can thoroughly remove pollutants, bacteria, microorganisms and other harmful substances remained on the surface of the product, prevent the montmorillonite from being poisoned by a person eating the montmorillonite by mistake and improve the safety of the montmorillonite product.
Optionally, the magnetic separation strength in the step S9 is 0.7-1.5T.
By adopting the technical scheme, the magnetic separation strength is 0.7-1.5T, so that the effective magnetic separation effect can be realized, and the ferric oxide is separated from the montmorillonite; magnetic separation can also help to increase the purity of the montmorillonite product.
The application of the montmorillonite with low ferric oxide content provided by the application adopts the following technical scheme:
a montmorillonite with low ferric oxide content is used in clothes drier.
In summary, the present application has the following beneficial effects:
1. because the stone and ferromagnetic impurities are removed by sieving, the method can effectively reduce the impuritiesThe quality exists, so that the purity of montmorillonite is improved; oxygen atoms (OH) generated by the decomposition of hydrogen peroxide react with ferric oxide ions (Fe & lt3+ & gt) on the surface of ferric oxide to generate high-valence oxides of ferric oxide, the high-valence oxides precipitate in a solution, impurities such as ferric oxide in montmorillonite slurry are separated from supernatant liquid through the operation of removing solid precipitate particles at the bottom after standing, and therefore, the content of ferric oxide in montmorillonite is reduced; the sieved montmorillonite is put into a magnetic separator to adsorb magnetic impurities, so that the montmorillonite can be further purified, and the purity and quality of the montmorillonite are improved. By the method, the content of ferric oxide in the montmorillonite can be effectively reduced, and Fe is added 2 O 3 The content is reduced to below 1.0%, the requirement of the needle checking machine is met, and the montmorillonite after moisture absorption can be reused after baking, so that the montmorillonite has better comprehensive performance compared with salt desiccant and silica gel.
2. The addition of a suspending agent is preferred in this application to enhance the dispersion and suspension stability of the montmorillonite particles in solution. The suspending agents such as polyacrylamide, carboxymethyl cellulose, active carbon and the like have the adsorption and water absorption capacity, and can form a stable suspension system with bentonite particles. This helps to prevent particle deposition and agglomeration and improves product uniformity and stability. The suspending agents such as polyacrylamide, carboxymethyl cellulose and the like have higher viscosity and adhesion property. The viscosity of the solution can be regulated, the flow property is changed, and the sedimentation speed and the mixing uniformity of montmorillonite particles are favorably controlled. The activated carbon has stronger adsorption capacity. It can adsorb impurities and organic matters in the solution, purify the surface of montmorillonite particles, and improve the purity and quality of the product.
3. The method can effectively adsorb and remove the ferric oxide particles in the bentonite slurry through the steps of contact, standing, separation, washing, elution and the like. Therefore, the purity and stability of the montmorillonite can be improved, and the requirement of low ferric oxide content can be met. And the ferric oxide eluted from the resin can be recycled after being collected, so that the method has an environmental protection value.
Detailed Description
The present application is described in further detail below with reference to examples.
This application is through multistage processing, sieves and gets rid of stone and ferromagnetic impurity, can reduce the existence of impurity effectively, uses oxidation treatment operation to get rid of ferric oxide in the montmorillonite, still ferroferric oxide, other heavy metal impurity, and the residual magnetic impurity is sieved the removal in the montmorillonite through the magnet separator at last, further improves the purity of montmorillonite.
The montmorillonite drying agent with low ferric oxide content has higher moisture absorption performance, and the montmorillonite after moisture absorption can be reused after baking, so that compared with salt drying agents and silica gel, the montmorillonite drying agent can be repeatedly utilized, the humidity control cost of products in the manufacturing, transporting and storing processes is reduced, the waste is reduced, the service life of the drying agent is prolonged, the sustainable utilization of resources is facilitated, meanwhile, the montmorillonite of the application does not contain toxic substances, is harmless to human bodies and environment, is more environment-friendly compared with some chemical moisture absorbents, does not need to worry about negative effects on human health and environment, and has high environmental protection value and economic value.
In addition to its use as a desiccant, montmorillonite has a wide range of applications, including toothpaste and antidiarrheal applications. Montmorillonite is often used as an abrasive in toothpaste, has good abrasive effect, can remove dirt and pigment on teeth, and provides cleaning and whitening effects. Among antidiarrheal agents, montmorillonite can adsorb and reduce water in the intestinal tract, and improve diarrhea symptoms.
Examples
Example 1
A method for producing montmorillonite with a low iron oxide content, comprising the steps of:
s1, grinding: 5000g of bentonite ore was ground to a particle size of 50. Mu.m.
S2, pulping: and mixing the ground bentonite with water according to a ratio of 1:2 to form bentonite slurry.
S3, removing Dan Chutie: stone and ferromagnetic impurities in the bentonite slurry were removed by using 120 mesh screen.
S4, natural sedimentation: and standing the bentonite slurry subjected to the stone removal and iron removal treatment for 10 hours to precipitate solid particles at the bottom.
S5, oxidation treatment: adding hydrogen peroxide into bentonite slurry, wherein the addition amount of the hydrogen peroxide is 8% of the mass of the bentonite slurry, keeping the temperature at 25 ℃, stirring for 3 hours at a stirring speed of 80r/min, standing for 2 hours, slowly pouring out the bentonite slurry through an inclined container and the like after standing is finished, leaving precipitate particles at the bottom, removing solid precipitate particles at the bottom, putting the bentonite slurry into a centrifuge, separating the bentonite slurry into supernatant and wet precipitate through centrifugation, removing the supernatant, and cleaning the wet precipitate for 3 times by using deionized water to obtain montmorillonite slurry.
S6, filter pressing: and packing montmorillonite slurry in filter cloth, and performing filter pressing through a filter press for 12 hours to remove redundant water.
S7, drying: and (3) drying the montmorillonite subjected to filter pressing to further remove water, performing high-temperature steam treatment after drying, and performing secondary drying after the high-temperature steam treatment.
S8, screening: the montmorillonite was sieved using a 180 mesh screen to ensure uniformity and consistency of the product particles.
S9, magnetic separation: and (3) putting the sieved montmorillonite into a magnetic separator for magnetic separation treatment, wherein the magnetic separation strength is set to be 1.2T, and adsorbing and removing magnetic impurities in the montmorillonite to obtain a montmorillonite product with low ferric oxide content.
Example 2
A method for producing montmorillonite with a low iron oxide content, comprising the steps of:
s1, grinding: 5000g of bentonite ore was ground to a particle size of 50. Mu.m.
S2, pulping: and mixing the ground bentonite with water according to a ratio of 1:2 to form bentonite slurry.
S3, removing Dan Chutie: stone and ferromagnetic impurities in the bentonite slurry were removed by using 120 mesh screen.
S4, natural sedimentation: adding 100g of polyacrylamide suspending agent into bentonite slurry subjected to stone removal and iron removal treatment, stirring for 5min, and standing for 10 hours after stirring is finished to precipitate solid particles to the bottom.
S5, oxidation treatment: adding hydrogen peroxide into bentonite slurry, wherein the addition amount of the hydrogen peroxide is 8% of the mass of the bentonite slurry, keeping the temperature at 25 ℃, stirring for 3 hours at a stirring speed of 80r/min, standing for 2 hours, slowly pouring out the bentonite slurry through an inclined container and the like after standing is finished, leaving precipitate particles at the bottom, removing solid precipitate particles at the bottom, putting the bentonite slurry into a centrifuge, separating the bentonite slurry into supernatant and wet precipitate through centrifugation, removing the supernatant, and cleaning the wet precipitate for 3 times by using deionized water to obtain montmorillonite slurry.
S6, filter pressing: and packing montmorillonite slurry in filter cloth, and performing filter pressing through a filter press for 12 hours to remove redundant water.
S7, drying: and (3) drying the montmorillonite subjected to filter pressing to further remove water, performing high-temperature steam treatment after drying, and performing secondary drying after the high-temperature steam treatment.
S8, screening: the montmorillonite was sieved using a 180 mesh screen to ensure uniformity and consistency of the product particles.
S9, magnetic separation: and (3) putting the sieved montmorillonite into a magnetic separator for magnetic separation treatment, wherein the magnetic separation strength is set to be 1.2T, and adsorbing and removing magnetic impurities in the montmorillonite to obtain a montmorillonite product with low ferric oxide content.
Example 3
A method for producing montmorillonite with a low iron oxide content, comprising the steps of:
s1, grinding: 5000g of bentonite ore was ground to a particle size of 50. Mu.m.
S2, pulping: and mixing the ground bentonite with water according to a ratio of 1:2 to form bentonite slurry.
S3, removing Dan Chutie: stone and ferromagnetic impurities in the bentonite slurry were removed by using 120 mesh screen.
S4, natural sedimentation: adding 100g of polyacrylamide suspending agent into bentonite slurry subjected to stone removal and iron removal treatment, stirring for 5min, and standing for 10 hours after stirring is finished to precipitate solid particles to the bottom.
S5, oxidation treatment: adding hydrogen peroxide into bentonite slurry, keeping the temperature at 25 ℃, stirring at 80r/min for 3h, standing for 2h, slowly pouring out the bentonite slurry through an inclined container and the like after standing is finished, leaving precipitate particles at the bottom, removing solid precipitate particles at the bottom, putting the bentonite slurry into a centrifuge, separating the bentonite slurry into supernatant and wet precipitate by centrifugation, removing supernatant, adding 3000g of ion exchange resin into the bentonite slurry, stirring for 5min, fully contacting the ion exchange resin with the bentonite slurry, keeping the temperature at 40 ℃ for 6h, washing the ion exchange resin with a salt solution of 0.5mol/L, removing impurities attached to the surface of the ion exchange resin, washing the wet precipitate for 3 times with deionized water, obtaining montmorillonite slurry, eluting the ion exchange resin with ethylenediamine tetraacetic acid, eluting ferric oxide from the resin, and collecting the ferric oxide.
S6, filter pressing: and packing montmorillonite slurry in filter cloth, and performing filter pressing through a filter press for 12 hours to remove redundant water.
S7, drying: and (3) drying the montmorillonite subjected to filter pressing to further remove water, performing high-temperature steam treatment after drying, and performing secondary drying after the high-temperature steam treatment.
S8, screening: the montmorillonite was sieved using a 180 mesh screen to ensure uniformity and consistency of the product particles.
S9, magnetic separation: and (3) putting the sieved montmorillonite into a magnetic separator for magnetic separation treatment, wherein the magnetic separation strength is set to be 1.2T, and adsorbing and removing magnetic impurities in the montmorillonite to obtain a montmorillonite product with low ferric oxide content.
Example 4
A method for producing montmorillonite with a low iron oxide content, comprising the steps of:
s1, grinding: 5000g of bentonite ore was ground to a particle size of 50. Mu.m.
S2, pulping: and mixing the ground bentonite with water according to a ratio of 1:2 to form bentonite slurry.
S3, removing Dan Chutie: stone and ferromagnetic impurities in the bentonite slurry were removed by using 120 mesh screen.
S4, natural sedimentation: adding 100g of polyacrylamide suspending agent into bentonite slurry subjected to stone removal and iron removal treatment, stirring for 5min, and standing for 10 hours after stirring is finished to precipitate solid particles to the bottom.
S5, oxidation treatment: adding hydrogen peroxide into bentonite slurry, keeping the temperature at 25 ℃, stirring at 80r/min for 3h, standing for 2h, slowly pouring out the bentonite slurry through an inclined container and the like after standing is finished, leaving precipitate particles at the bottom, removing solid precipitate particles at the bottom, putting the bentonite slurry into a centrifuge, separating the bentonite slurry into supernatant and wet precipitate through centrifugation, removing supernatant, adding 3000g of ion exchange resin into the bentonite slurry, stirring for 5min, fully contacting the ion exchange resin with the bentonite slurry, keeping the temperature at 40 ℃ for 6h, washing the ion exchange resin with a 0.5mol/L salt solution, removing impurities attached to the surface of the ion exchange resin, soaking the wet precipitate in a 1% sodium hydroxide solution, washing and separating the wet precipitate after keeping the temperature at 40 ℃ for 3h, washing the wet precipitate with deionized water for 3 times to obtain montmorillonite slurry, eluting the ion exchange resin with ethylene diamine tetraacetic acid, eluting ferric oxide from the resin, and collecting ferric oxide from the resin.
S6, filter pressing: and packing montmorillonite slurry in filter cloth, and performing filter pressing through a filter press for 12 hours to remove redundant water.
S7, drying: and (3) drying the montmorillonite subjected to filter pressing to further remove water, performing high-temperature steam treatment after drying, and performing secondary drying after the high-temperature steam treatment.
S8, screening: the montmorillonite was sieved using a 180 mesh screen to ensure uniformity and consistency of the product particles.
S9, magnetic separation: and (3) putting the sieved montmorillonite into a magnetic separator for magnetic separation treatment, wherein the magnetic separation strength is set to be 1.2T, and adsorbing and removing magnetic impurities in the montmorillonite to obtain a montmorillonite product with low ferric oxide content.
Example 5
A method for producing montmorillonite having a low iron oxide content, which differs from example 4 in that: and S4, selecting a carboxymethyl cellulose suspending agent.
Example 6
A method for producing montmorillonite having a low iron oxide content, which differs from example 4 in that: s4, selecting an activated carbon suspending agent.
Example 7
A method for producing montmorillonite having a low iron oxide content, which differs from example 4 in that: the magnetic separation strength in the step S9 is 0.7T.
Example 8
A method for producing montmorillonite having a low iron oxide content, which differs from example 4 in that: the magnetic separation strength in the step S9 is 1.5T.
Comparative example
Comparative example 1
A method for producing montmorillonite with a low iron oxide content, comprising the steps of:
s1, grinding: 5000g of bentonite ore was ground to a particle size of 50. Mu.m.
S2, pulping: and mixing the ground bentonite with water according to a ratio of 1:2 to form bentonite slurry.
S3, removing Dan Chutie: stone and ferromagnetic impurities in the bentonite slurry were removed by using 120 mesh screen.
S4, natural sedimentation: adding 100g of polyacrylamide suspending agent into bentonite slurry subjected to stone removal and iron removal treatment, stirring for 5min, and standing for 10 hours after stirring is finished to precipitate solid particles to the bottom.
S5, filter pressing: and packing montmorillonite slurry in filter cloth, and performing filter pressing through a filter press for 12 hours to remove redundant water.
S6, drying: and (3) drying the montmorillonite subjected to filter pressing to further remove water, performing high-temperature steam treatment after drying, and performing secondary drying after the high-temperature steam treatment.
S7, screening: the montmorillonite was sieved using a 180 mesh screen to ensure uniformity and consistency of the product particles.
S8, magnetic separation: and (3) putting the sieved montmorillonite into a magnetic separator for magnetic separation treatment, wherein the magnetic separation strength is set to be 1.2T, and adsorbing and removing magnetic impurities in the montmorillonite to obtain a montmorillonite product with low ferric oxide content.
Comparative example 2
A method for producing montmorillonite with a low iron oxide content, comprising the steps of:
s1, grinding: 5000g of bentonite ore was ground to a particle size of 50. Mu.m.
S2, pulping: and mixing the ground bentonite with water according to a ratio of 1:2 to form bentonite slurry.
S3, removing Dan Chutie: stone and ferromagnetic impurities in the bentonite slurry were removed by using 120 mesh screen.
S4, natural sedimentation: adding 100g of polyacrylamide suspending agent into bentonite slurry subjected to stone removal and iron removal treatment, stirring for 5min, and standing for 10 hours after stirring is finished to precipitate solid particles to the bottom.
S5, alkali washing: the montmorillonite slurry is soaked in 1% sodium hydroxide solution, and is washed and separated after heat preservation for 3 hours at 40 ℃.
S6, filter pressing: and packing montmorillonite slurry in filter cloth, and performing filter pressing through a filter press for 12 hours to remove redundant water.
S7, drying: and (3) drying the montmorillonite subjected to filter pressing to further remove water, performing high-temperature steam treatment after drying, and performing secondary drying after the high-temperature steam treatment.
S8, screening: the montmorillonite was sieved using a 180 mesh screen to ensure uniformity and consistency of the product particles.
S9, magnetic separation: and (3) putting the sieved montmorillonite into a magnetic separator for magnetic separation treatment, wherein the magnetic separation strength is set to be 1.2T, and adsorbing and removing magnetic impurities in the montmorillonite to obtain a montmorillonite product with low ferric oxide content.
Comparative example 3
A method for producing montmorillonite with a low iron oxide content, comprising the steps of:
s1, grinding: 5000g of bentonite ore was ground to a particle size of 50. Mu.m.
S3, removing Dan Chutie: the stone and ferromagnetic impurities in the bentonite are removed by using 120 mesh screen.
S4, oxidation treatment: adding hydrogen peroxide into bentonite slurry, keeping the temperature at 25 ℃, stirring at 80r/min for 3h, standing for 2h, slowly pouring out the bentonite slurry through an inclined container and the like after standing is finished, leaving precipitate particles at the bottom, removing solid precipitate particles at the bottom, putting the bentonite slurry into a centrifuge, separating the bentonite slurry into supernatant and wet precipitate by centrifugation, removing supernatant, adding 3000g of ion exchange resin into the bentonite slurry, stirring for 5min, fully contacting the ion exchange resin with the bentonite slurry, keeping the temperature at 40 ℃ for 6h, washing the ion exchange resin with a salt solution of 0.5mol/L, removing impurities attached to the surface of the ion exchange resin, washing the wet precipitate for 3 times with deionized water, obtaining montmorillonite slurry, eluting the ion exchange resin with ethylenediamine tetraacetic acid, eluting ferric oxide from the resin, and collecting the ferric oxide.
S5, filter pressing: and packing montmorillonite slurry in filter cloth, and performing filter pressing through a filter press for 12 hours to remove redundant water.
S6, drying: and (3) drying the montmorillonite subjected to filter pressing to further remove water, performing high-temperature steam treatment after drying, and performing secondary drying after the high-temperature steam treatment.
S7, screening: the montmorillonite was sieved using a 180 mesh screen to ensure uniformity and consistency of the product particles.
S8, magnetic separation: and (3) putting the sieved montmorillonite into a magnetic separator for magnetic separation treatment, wherein the magnetic separation strength is set to be 1.2T, and adsorbing and removing magnetic impurities in the montmorillonite to obtain a montmorillonite product with low ferric oxide content.
Performance test
Detection method
In examples 1 to 8 and comparative examples 1 to 3, 20g of montmorillonite was extracted as a sample, respectively, and the montmorillonite samples were dissolved in an equal amount of diluted hydrochloric acid to obtain 11 experimental groups, and the 11 experimental groups were subjected to iron oxide, ferroferric oxide and heavy metal detection using an atomic absorption spectrometer, and after the detection was completed, data were recorded and the content was calculated.
20g of montmorillonite was extracted as a sample in each of examples 1 to 8 and comparative examples 1 to 3, and the relative purity of montmorillonite was evaluated by subjecting the montmorillonite sample to X-ray diffraction analysis.
Table 1 statistics of the monitored data
As can be seen from the combination of example 4 and comparative example 1 and the combination of table 1, example 4 is different from comparative example 1 in that the oxidation treatment, the ion exchange treatment and the alkali washing steps are not performed in comparative example 1, and as can be seen from the examination, the iron oxide content in comparative example 1 is higher than 1%, the requirement of passing through a needle inspection machine is not met, the iron oxide content in montmorillonite prepared in example 4 is 0.67%, and is far lower than 1%, and the purity of montmorillonite is lower than that in example 4, thereby demonstrating that metal ions, impurity cations and the like in montmorillonite can be effectively removed through the oxidation treatment, the ion exchange treatment and the alkali washing steps, the iron oxide content is greatly reduced, and the purity and purity of montmorillonite are improved.
As can be seen from the combination of example 4 and comparative example 2 and the combination of table 1, example 4 is different from comparative example 2 in that comparative example 2 is not subjected to oxidation treatment but is subjected to only alkaline washing, which is mainly neutralization and removal of acidic substances by using an alkaline solution. However, alkali washing is not effective in removing impurities and oxides attached to the surface of montmorillonite. If the oxidation treatment is not carried out, inorganic salts, ferric oxide and other impurities in the bentonite still exist, so that the purity of the prepared montmorillonite sample is lower.
As can be seen from the combination of example 4 and comparative example 3 and the combination of table 1, example 4 is different from comparative example 3 in that the operations of beating and natural settling are not performed in comparative example 3, and beating and natural settling are not performed, and these impurities may remain in the bentonite slurry and cannot be effectively removed. This will result in a final prepared montmorillonite sample still containing higher levels of impurities, affecting purity. Beating and natural settling can provide better dispersion of bentonite solid particles and help remove some soluble impurities. If these two steps are skipped, solid particles in bentonite may be more difficult to disperse in the oxidation treatment solution, resulting in a reduced oxidation treatment effect. This will affect the purity and quality of the final montmorillonite sample.
It can be seen from the combination of examples 1 to 4 and table 1 that the iron oxide content of bentonite can be effectively controlled by controlling the grinding particle size of bentonite particles within the range of 30 to 80 μm. The smaller particle size helps to reduce the iron oxide content and provides a low iron oxide content montmorillonite product; the addition of the suspending agent can enhance the dispersion and suspension stability of the montmorillonite particles in the solution. The ion exchange treatment can effectively remove iron oxide particles in the solution using ion exchange resin. The ion exchange resin has certain selectivity, and can selectively adsorb ferric oxide ions and carry out ion exchange reaction with the ferric oxide ions. Thus, the iron oxide content in the montmorillonite product can be obviously reduced, and the requirement of low iron oxide content is met. Iron oxide particles are adsorbed onto the resin by ion exchange treatment, thereby purifying the montmorillonite product. The method is favorable for improving the purity of the product, removing impurities and impurities, and recycling the ferric oxide eluted from the resin after collection, thereby having environmental protection value. The alkaline washing treatment can effectively remove impurities in the montmorillonite slurry. The sodium hydroxide can perform neutralization reaction with acidic impurities in the montmorillonite slurry to change the acidic impurities into salts or water-soluble substances, so that the impurities are removed. By combining with the oxidation treatment step, the alkaline washing treatment helps to improve the purity of the montmorillonite product and further reduce the iron oxide content.
As can be seen in the combination of examples 4-6 and Table 1, the use of polyacrylamide as suspending agent works best in the preparation method of the present application.
As can be seen from the combination of examples 4 and examples 7 to 8 and table 1, the magnetic separation strength is 0.7 to 1.5T, so that an effective magnetic separation effect can be achieved, and iron oxide can be separated from montmorillonite; the magnetic separation can also help to improve the purity of the montmorillonite product, and the effect is optimal when the magnetic separation strength is set at 1.2 t.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.

Claims (9)

1. A method for producing montmorillonite having a low iron oxide content, comprising the steps of:
s1, grinding: grinding bentonite ore;
s2, pulping: mixing the ground bentonite with water according to the formula 1 (1-5) to form bentonite slurry;
s3, removing Dan Chutie: removing stones and ferromagnetic impurities in the bentonite slurry through a 100-150 mesh sieve;
s4, natural sedimentation: standing bentonite slurry after removing the stones and the iron for 8-12h to enable solid particles to be precipitated to the bottom;
s5, oxidation treatment: adding hydrogen peroxide into bentonite slurry, wherein the addition amount of the hydrogen peroxide is 5-10% of the mass of the bentonite slurry, keeping the temperature at 20-30 ℃, stirring for 2-4 hours at the stirring speed of 50-100r/min, standing for 1-2 hours, removing solid precipitate particles at the bottom after standing, separating supernatant from wet precipitate by a centrifuge, and cleaning the wet precipitate for 2-3 times by using deionized water to obtain montmorillonite slurry;
s6, filter pressing: packing montmorillonite slurry in filter cloth, and performing filter pressing by a filter press for 10-14 hours;
s7, drying: drying the montmorillonite subjected to filter pressing;
s8, screening: sieving with 150-200 mesh sieve;
s9, magnetic separation: and (3) placing the sieved montmorillonite into a magnetic separator to adsorb magnetic impurities, so as to obtain the montmorillonite with low ferric oxide content.
2. The method for producing a low iron oxide content montmorillonite according to claim 1, wherein: the granularity of the bentonite after grinding in the step S1 is 30-80 mu m.
3. The method for producing a low iron oxide content montmorillonite according to claim 1, wherein: and step S4, adding a suspending agent, wherein the suspending agent comprises one or more of polyacrylamide, carboxymethyl cellulose and activated carbon.
4. The method for producing a low iron oxide content montmorillonite according to claim 1, wherein: in the step S5, after the bentonite slurry is separated from the wet precipitate by a centrifugal machine, ion exchange treatment is needed to be carried out on the separated wet precipitate, and the ion exchange treatment is carried out to adsorb ferric oxide particles by resin.
5. The method for producing a low iron oxide content montmorillonite according to claim 4, wherein: the specific steps of the ion exchange treatment are as follows:
a1, adding ion exchange resin into the wet precipitate, stirring to enable the ion exchange resin to fully contact with the wet precipitate, and keeping the temperature at 30-50 ℃ and standing for 4-8h;
a2, after standing, separating bentonite slurry from the ion exchange resin through filtration and centrifugal treatment;
a3, washing the ion exchange resin by using a salt solution to remove impurities attached to the surface of the ion exchange resin;
and A4, eluting the ion exchange resin by using ethylenediamine tetraacetic acid, and collecting the ferric oxide eluted from the resin.
6. The method for producing a low iron oxide content montmorillonite according to claim 5, wherein: and (5) after the ion exchange treatment in the step (S5) is finished, alkali washing treatment is further carried out, wherein the specific operation process of the alkali washing treatment is as follows: soaking montmorillonite slurry in 0.1-1% sodium hydroxide solution, maintaining at 24-50deg.C for 2-4 hr, and washing and separating.
7. The method for producing a low iron oxide content montmorillonite according to claim 1, wherein: and S7, carrying out high-temperature steam treatment after drying in the step, and carrying out secondary drying after the high-temperature steam treatment.
8. The method for producing a low iron oxide content montmorillonite according to claim 1, wherein: the magnetic separation strength in the step S9 is 0.7-1.5T.
9. Use of a low iron oxide content montmorillonite manufacturing process according to any one of claims 1-8, characterized in that the low iron oxide content montmorillonite of the present application is used in laundry drying agents.
CN202311470709.3A 2023-11-07 2023-11-07 Method for preparing montmorillonite with low ferric oxide content and application thereof Pending CN117446815A (en)

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