CN109535776A - A kind of lithium bentonite and preparation method thereof - Google Patents

A kind of lithium bentonite and preparation method thereof Download PDF

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Publication number
CN109535776A
CN109535776A CN201811632313.3A CN201811632313A CN109535776A CN 109535776 A CN109535776 A CN 109535776A CN 201811632313 A CN201811632313 A CN 201811632313A CN 109535776 A CN109535776 A CN 109535776A
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China
Prior art keywords
bentonite
lithium
slurry
calcium
lithium bentonite
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CN201811632313.3A
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Chinese (zh)
Inventor
汪思孝
吴志能
任伟华
邵宣泽
周琳
王齐
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Suzhou Jian Hui Investment Mineral New Material Co Ltd
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Suzhou Jian Hui Investment Mineral New Material Co Ltd
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Application filed by Suzhou Jian Hui Investment Mineral New Material Co Ltd filed Critical Suzhou Jian Hui Investment Mineral New Material Co Ltd
Priority to CN201811632313.3A priority Critical patent/CN109535776A/en
Publication of CN109535776A publication Critical patent/CN109535776A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/40Compounds of aluminium
    • C09C1/42Clays
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22CFOUNDRY MOULDING
    • B22C3/00Selection of compositions for coating the surfaces of moulds, cores, or patterns
    • 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
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The invention discloses a kind of lithium bentonites and preparation method thereof, the described method comprises the following steps: the slurry that mass percent is 8-12% is made in calcium-base bentonite;Modifying agent is added into slurry and slurry is stirred, makes calcium-base bentonite that modified-reaction occur, the quality of the modifying agent is between the 1-10% of the quality of the calcium-base bentonite;It is purified to by the slurry of modified-reaction, obtains lithium bentonite slurry;Lithium bentonite slurry is aged;Lithium bentonite slurry after ageing is dried.The lithium bentonite prepared using method of the present invention, the performances such as suspension, purity are very excellent.

Description

A kind of lithium bentonite and preparation method thereof
Technical field
The present invention relates to cast paint technical field, a kind of particularly lithium bentonite and preparation method thereof.
Background technique
Lithium bentonite has high viscosity, high dispersive, higher suspension, high thixotroping and the spies such as nontoxic, tasteless, environmental-friendly Property, unique dioctahedron and trioctahedron mixed structure and resulting multifrequency nature make its viscosity, suspension, touching Denaturation etc. can have excellent suspension, anti-settling, thixotroping and thickening power in water base and polar solvent base medium, be cast paint Excellent suspension, thixotroping and thickening aids, greatly improve the suspension stability of cast paint.
So far, China not yet finds the lithium bentonite naturally produced, is added mainly by natural calcium-base bentonite Lithium salts is obtained through ion-exchange treatment with calcium ion, the magnesium ion in lithium ion displacement original soil crystal.Currently, it is swollen to prepare lithium base The method for moistening soil is usually in the majority with dry production, but due to dry method by mechanical force to the dry powder of calcium-base bentonite and modifying agent into Row is mediated, and the technique is more coarse, the ion exchange being unfavorable in bentonite, and alta-mud modification reaction is caused to be not enough, And dry method not can be removed extra impurity usually without purification step, thus, using the lithium bentonite of dry process, lithiumation Performance is not strong, and suspendability is poor, and application performance is bad.
Therefore, how to make bentonite abundant lithiumation in modified-reaction, improve the suspendability of lithium bentonite, reduce it Impurity content is the project that those skilled in the art have been devoted to research.
Summary of the invention
In order to overcome the defects of the prior art, the embodiment of the invention provides a kind of lithium bentonite and its preparation sides At least one of method, be used to solve the above problems.
The embodiment of the present application discloses: a kind of preparation method of lithium bentonite, comprising the following steps:
It is 8-12% slurry that mass percent, which is made, in calcium-base bentonite;
Modifying agent is added into slurry and slurry is stirred, makes calcium-base bentonite that modified-reaction, the modification occur The quality of agent is between the 1-10% of the quality of the calcium-base bentonite;
It is purified to by the slurry of modified-reaction, obtains lithium bentonite slurry;
Lithium bentonite slurry is aged;
Lithium bentonite slurry after ageing is dried.
Specifically, the modifying agent includes one or more of lithia, lithium hydroxide, lithium carbonate, lithium fluoride.
Specifically, in step " it is 8-12% slurry that calcium-base bentonite is made to mass percent ", the calcium base swelling The mass percent of soil is 10%.
Specifically, the quality of the modifying agent is between the 3-4% of the quality of the calcium-base bentonite.
Specifically, in step " being aged to lithium bentonite slurry ", when the ageing of the lithium bentonite slurry Between be 2-5 days.
Specifically, in step " being aged to lithium bentonite slurry ", when the ageing of the lithium bentonite slurry Between be 3 days.
Specifically, the drying means of use includes in step " the lithium bentonite slurry after ageing is dried " Spray drying.
The present embodiment also discloses a kind of lithium bentonite using the method preparation in the present embodiment, the lithium base swelling The swelling value of soil is between 70-95mL, and the suspensibility of the lithium bentonite is between 85-99%.
Beneficial effects of the present invention are as follows:
1. the method for preparing lithium bentonite using wet process, sends out calcium-base bentonite and modifying agent sufficiently under the conditions of liquid Raw ion exchange, i.e., sufficiently occur modified-reaction, hence it is evident that the suspension and swelling value for improving lithium bentonite solve existing The problem of dry process lithium bentonite suspension difference in system;
2. the lithium bentonite prepared by the way of in the present embodiment, when being configured to 1% aqueous dispersion, upper layer Without layering bleed, bottom only has a small amount of contamination precipitation or even free from admixture precipitating, purity significantly improve;
3. the modified-reaction in this method is simple and easy, cost is relatively low, is suitable for popularization and application.
For above and other objects, features and advantages of the invention can be clearer and more comprehensible, preferred embodiment is cited below particularly, And cooperate institute's accompanying drawings, it is described in detail below.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with It obtains other drawings based on these drawings.
Fig. 1 is the flow chart of the preparation method of lithium bentonite described in the embodiment of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
The preparation method of lithium bentonite described in the present embodiment, comprising the following steps:
The slurry that mass percent is 8-12% is made in calcium-base bentonite.Specifically, water is added in calcium-base bentonite In, it is stirred with mixing plant, forms slurry.Preferably, in the slurry, the quality percentage of the calcium-base bentonite It than being 10%, both can avoid that calcium-base bentonite concentration is excessive causes slurry viscosity big, and be unfavorable for the separating-purifying in later period, can also keep away Exempt from that calcium-base bentonite concentration is too small to cause slurry solid content low, so that the drying cost of later period slurry is very big.
Modifying agent is added into slurry, and slurry is stirred, makes calcium-base bentonite that modified-reaction sufficiently occur.Its In, the quality (that is, measuring by weight, the dosage of modifying agent) of the modifying agent is the 1- of the quality of the calcium-base bentonite Between 10%.The modifying agent includes one or more of lithia, lithium hydroxide, lithium carbonate, lithium fluoride.It is sent out according to test Existing, when the dosage of modifying agent is excessive, its viscosity of modified bentonite is larger, is not easy to purify, contain in lithium bentonite When more impurity, service performance will receive influence, and when amount of modifier is too small, alta-mud modification reaction is not enough filled Point, cause the suspendability of lithium bentonite poor.It is therefore advantageous to, the quality of the modifying agent is the calcium-base bentonite Quality 3-4% between.
It is purified to by the slurry of modified-reaction, obtains lithium bentonite slurry.Specifically, using seperator to slurry Material carries out separating-purifying, keeps impurity and pulp separation convenient, efficient.
Ageing 2-5 days is carried out to lithium bentonite slurry, guarantees that modified-reaction carries out sufficiently, so that modified effect reaches It optimizes.Preferably, the lithium bentonite slurry digestion time is 3 days, it is ensured that bentonite is sufficiently modified, is also beneficial to save It saves time, improves production efficiency.
Finally, the lithium bentonite slurry after ageing is dried.It is preferential swollen to lithium base by the way of spray drying Profit soil carries out, specifically, lithium bentonite is sprayed into powder of the mesh number between 200-300 mesh, so that lithium bentonite can be with It is dry rapidly.
In conclusion the preparation method of lithium bentonite described in the present embodiment, it is swollen to belong to a kind of wet production lithium base Moisten the method for soil.
The method in the present embodiment is further described using five specific implementation cases below
Case 1
The calcium-base bentonite raw material of 1t is added to the water, the slurry that calcium-base bentonite mass percent is 10% is made;
40Kg lithium carbonate is added into slurry, and slurry is stirred, makes calcium-base bentonite that modified-reaction occur;
It passes through separating-purifying to by the slurry of modified-reaction, obtains lithium bentonite slurry;
Ageing 3 days is carried out to lithium bentonite slurry;
Lithium bentonite slurry after ageing is spray-dried, modified lithium bentonite is obtained.
Case 2
The calcium-base bentonite raw material of 1t is added to the water, the slurry that calcium-base bentonite mass percent is 10% is made;
40Kg lithium fluoride is added into slurry, and slurry is stirred, makes calcium-base bentonite that modified-reaction occur;
It passes through separating-purifying to by the slurry of modified-reaction, obtains lithium bentonite slurry;
Ageing 3 days is carried out to lithium bentonite slurry;
Lithium bentonite slurry after ageing is spray-dried, modified lithium bentonite is obtained.
Case 3
The calcium-base bentonite raw material of 1t is added to the water, the slurry that calcium-base bentonite mass percent is 10% is made;
20Kg lithium carbonate and 20Kg lithium fluoride are added into slurry, and slurry is stirred, makes calcium-base bentonite Modified-reaction;
It passes through separating-purifying to by the slurry of modified-reaction, obtains lithium bentonite slurry;
Ageing 3 days is carried out to lithium bentonite slurry;
Lithium bentonite slurry after ageing is spray-dried, modified lithium bentonite is obtained.
Case 4
The calcium-base bentonite raw material of 1t is added to the water, the slurry that calcium-base bentonite mass percent is 10% is made;
80Kg lithium carbonate is added into slurry, and slurry is stirred, makes calcium-base bentonite that modified-reaction occur;
It passes through separating-purifying to by the slurry of modified-reaction, obtains lithium bentonite slurry;
Ageing 3 days is carried out to lithium bentonite slurry;
Lithium bentonite slurry after ageing is spray-dried, modified lithium bentonite is obtained.
Case 5
The calcium-base bentonite raw material of 1t is added to the water, the slurry that calcium-base bentonite mass percent is 10% is made;
40Kg lithium carbonate is added into slurry, and slurry is stirred, makes calcium-base bentonite that modified-reaction occur;
It passes through separating-purifying to by the slurry of modified-reaction, obtains lithium bentonite slurry;
Ageing 2 days is carried out to lithium bentonite slurry;
Lithium bentonite slurry after ageing is spray-dried, modified lithium bentonite is obtained.
By lithium bentonite (hereinafter referred to as comparative example) made of above-mentioned five specific implementation cases and existing dry method point It is not configured to corresponding dispersion to carry out swelling value, suspensibility and suspendability evaluation, wherein the test side of properties Method difference is as follows:
(1) swelling value
The dry soil samples for weighing 1.5g is put into the measuring cylinder with stopper of 100mL;
Then, the ammonium chloride solution that 5mL concentration is 1mol/L is added into graduated cylinder;
Then, water is added into graduated cylinder, when the solution in graduated cylinder reaches 100mL, stops adding water;
Then, beyond the Great Wall by graduated cylinder, the solution in graduated cylinder is shaken up and is stood, stood for 24 hours afterwards to the solution in graduated cylinder It is read.
(2) suspensibility
Dry soil samples with water is that 1:1 is uniformly mediated by the dry soil samples for weighing 30g ± 0.01g in mass ratio;
The kneading sample for weighing 30g, is placed in the beaker of 500mL;
120g anhydrous methanol is added into beaker, and uses dispersion machine with the revolving speed of 1200r/min to the solution in beaker It carries out high speed dispersion 15 minutes;
The solution that dispersion is completed is poured into the measuring cylinder with stopper of 100mL, when the solution in graduated cylinder reaches 100mL, is covered Plug, and graduated cylinder is placed in 20 DEG C of thermostatic chamber and is stood for 24 hours, then observed reading.
(3) 1% aqueous dispersions stand observation precipitating for 24 hours
198g ± 0.01g water is weighed to be put into 250mL beaker;
Drying sample 2g ± 0.01g is weighed to be put into the water in above-mentioned beaker;
Dispersion 15min is carried out to the sample in beaker using magnetic stirrer, until will burn after sample is evenly dispersed in water Cup sealing, which is placed in 20 DEG C of thermostatic chamber, to be stood for 24 hours;
Observe dispersion upper layer bleed and bottom precipitation situation.
Test result is as follows shown in table 1 for the properties of above-mentioned five cases and comparative example:
The performance comparison of table 1 case 1 to 5 and comparative example
Lithium bentonite described in the present embodiment, swelling value between 70-95mL, suspensibility between 85-99%, And after its 1% aqueous dispersion is stood for 24 hours, without layering bleed, bottom only has a small amount of contamination precipitation or even free from admixture precipitating on upper layer, Performance is very excellent.
Compared with prior art, the lithium bentonite being prepared using the method in the present embodiment, is had the advantage that
1. the method for preparing lithium bentonite using wet process, sends out calcium-base bentonite and modifying agent sufficiently under the conditions of liquid Raw ion exchange, i.e., sufficiently occur modified-reaction, hence it is evident that the suspension and swelling value for improving lithium bentonite solve existing Dry process lithium bentonite suspends the problem of small difference in system;
2. the lithium bentonite prepared by the way of in the present embodiment, when being configured to 1% aqueous dispersion, upper layer Without layering bleed, bottom only has a small amount of contamination precipitation or even free from admixture precipitating, purity significantly improve;
3. the modified-reaction in this method is simple and easy, cost is relatively low, is suitable for popularization and application.
Specific embodiment is applied in the present invention, and principle and implementation of the present invention are described, above embodiments Explanation be merely used to help understand method and its core concept of the invention;At the same time, for those skilled in the art, According to the thought of the present invention, there will be changes in the specific implementation manner and application range, in conclusion in this specification Appearance should not be construed as limiting the invention.

Claims (8)

1. a kind of preparation method of lithium bentonite, which comprises the following steps:
It is 8-12% slurry that mass percent, which is made, in calcium-base bentonite;
Modifying agent is added into slurry and slurry is stirred, makes calcium-base bentonite that modified-reaction occur, the modifying agent Quality is between the 1-10% of the quality of the calcium-base bentonite;
It is purified to by the slurry of modified-reaction, obtains lithium bentonite slurry;
Lithium bentonite slurry is aged;
Lithium bentonite slurry after ageing is dried.
2. the preparation method of lithium bentonite according to claim 1, which is characterized in that the modifying agent includes oxidation One or more of lithium, lithium hydroxide, lithium carbonate, lithium fluoride.
3. the preparation method of lithium bentonite according to claim 1, which is characterized in that in step " by calcium-base bentonite It is 8-12% slurry that mass percent, which is made, " in, the mass percent of the calcium-base bentonite is 10%.
4. the preparation method of lithium bentonite according to claim 1, which is characterized in that the quality of the modifying agent is institute Between the 3-4% for stating the quality of calcium-base bentonite.
5. the preparation method of lithium bentonite according to claim 1, which is characterized in that in step " to lithium bentonite Slurry is aged " in, the digestion time of the lithium bentonite slurry is 2-5 days.
6. the preparation method of lithium bentonite according to claim 5, which is characterized in that in step " to lithium bentonite Slurry is aged " in, the digestion time of the lithium bentonite slurry is 3 days.
7. the preparation method of lithium bentonite according to claim 1, which is characterized in that in step " to the lithium after ageing Bentonite grout is dried " in, the drying means of use includes spray drying.
8. lithium bentonite made of a kind of preparation method described in any one of claim 1 to 7, which is characterized in that The swelling value of the lithium bentonite is between 70-95mL, and the suspensibility of the lithium bentonite is between 85-99%.
CN201811632313.3A 2018-12-29 2018-12-29 A kind of lithium bentonite and preparation method thereof Pending CN109535776A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114261968A (en) * 2021-12-15 2022-04-01 苏州国建慧投矿物新材料有限公司 Lithium-based modified composite clay and preparation method thereof
CN115475906A (en) * 2022-10-28 2022-12-16 西南科技大学 Molding sand adhesive, molding sand and preparation method

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CN102923985A (en) * 2012-11-30 2013-02-13 吉林大学 Method using lithium bentonite as cement product additive
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114261968A (en) * 2021-12-15 2022-04-01 苏州国建慧投矿物新材料有限公司 Lithium-based modified composite clay and preparation method thereof
CN114261968B (en) * 2021-12-15 2023-01-06 苏州国建慧投矿物新材料有限公司 Lithium-based modified composite clay and preparation method thereof
CN115475906A (en) * 2022-10-28 2022-12-16 西南科技大学 Molding sand adhesive, molding sand and preparation method

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