CN112569877B - Modified bentonite inorganic gel and preparation method and application thereof - Google Patents
Modified bentonite inorganic gel and preparation method and application thereof Download PDFInfo
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- CN112569877B CN112569877B CN202011454161.XA CN202011454161A CN112569877B CN 112569877 B CN112569877 B CN 112569877B CN 202011454161 A CN202011454161 A CN 202011454161A CN 112569877 B CN112569877 B CN 112569877B
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0056—Preparation of gels containing inorganic material and water
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
Abstract
The invention discloses a modified bentonite inorganic gel and a preparation method thereof, wherein the method comprises the following steps: s1: preparing bentonite inorganic gel ore pulp; s2: adding inorganic minerals into the prepared gel ore pulp, stirring and mixing, and then carrying out an aging reaction; s3: and drying the aged slurry to obtain the product. The invention not only can prepare the bentonite inorganic gel with good dispersibility, but also can keep the suspension performance of the inorganic gel in a water dispersion system, and the product of the invention has good application prospect in the fields of water-suspended pesticides, water-based paint and the like.
Description
Technical Field
The invention belongs to the field of inorganic gel, relates to a method for modifying functionality of bentonite inorganic gel, and particularly relates to modified bentonite inorganic gel and a preparation method and application thereof.
Background
The bentonite inorganic gel is a natural inorganic gel product with certain purity, which is obtained by taking clay minerals (such as smectite, bentonite and the like) containing bentonite inorganic gel components as raw materials and performing the procedures of crushing, pulping, separation and purification, gelling, drying and the like on the raw materials. The bentonite inorganic gel has unique layered magnesium aluminum silicate structure, and Na is mainly distributed between layers + . The nano-silver particles can form a special 'card house' structure when dispersed in an aqueous solution, show excellent suspension property, rheological property, colloid property and the like, and have wide application in the fields of toothpaste, cosmetics, paint, medicine and the like.
At present, the preparation methods of the bentonite inorganic gel mainly comprise the following steps:
qijun et al (preparation of high performance montmorillonite inorganic mineral gel. Qijun et al (chemical minerals and processing, 2007 (6): 16-18)) studied the optimal process conditions for preparing inorganic gel from purified calcium bentonite in Shandong. The montmorillonite inorganic mineral gel with excellent performance is prepared by using NaF as a sodium treatment agent, sodium pyrophosphate as a phosphating agent and calcium oxide as a gelling agent through sodium treatment, phosphating and gelling processes.
Qian ju et al (qian ju et al, coatings industry, 2010,40 (10)) investigated the effect of sodium pyrophosphate on the structure of modified bentonite by modifying an aqueous bentonite solution with sodium pyrophosphate as a dispersant, and investigated the effect of bentonite concentration (5-10%) on the structure of the dispersion system.
The Chinese invention patent CN1363515A discloses a preparation method of natural magnesium aluminum silicate inorganic gel, and the main steps of the invention comprise wet pulping, viscosity reducer dispersion, centrifugal separation and purification, pre-activation treatment, sodium ion modification, post-treatment and the like.
The Chinese invention patent CN1257103C discloses a preparation method of high-purity aluminum magnesium silicate inorganic gel, which mainly comprises the following processing procedures of raw material crushing, pulping, centrifugal separation and purification, magnetic separation and iron removal, secondary modification, ore pulp concentration, washing, drying and the like.
However, the bentonite inorganic gel prepared by the methods has extremely strong hydrophilic performance, and when the bentonite inorganic gel enters an application system such as water-suspended pesticide, water-based paint and the like, the powder is agglomerated due to too high hydration speed, so that the dispersion time of the bentonite in an aqueous medium is prolonged. Although the dispersion time is long, the indexes such as the suspension percentage and the viscosity of the bentonite do not have influence, along with the increasing requirements of manufacturers on raw materials, additives and auxiliary materials and the strict control on the production efficiency and the cost, the existing bentonite inorganic gel has low dispersion speed in an aqueous system, influences the production efficiency and is difficult to meet the requirements of the manufacturers; therefore, there is a need to develop an inorganic gel of bentonite which can be completely dispersed in an aqueous system in a short time.
In order to solve the technical problems, the conventional method for assisting the dispersion of the inorganic gel of the bentonite is to reduce the dispersion time by adding an inorganic dispersant such as sodium pyrophosphate and the like. However, the addition of inorganic dispersants such as sodium pyrophosphate and the like disturbs the charge balance on the surface of the layered magnesium aluminum silicate structure, thereby destroying the 'card room type' space structure originally built by mutual attraction of positive and negative charges, causing the final viscosity of the aqueous solution of the bentonite inorganic gel to be too low, even failing to form the inorganic gel structure, and losing the original suspension assisting performance.
Disclosure of Invention
The invention provides a method for modifying the dispersibility of inorganic bentonite gel, aiming at the problems that the conventional inorganic bentonite dispersant disturbs the charge balance on the surface of a lamellar structure of the inorganic bentonite gel, destroys the 'card-house' space structure of the lamellar structure of the bentonite, causes the viscosity of aqueous solution of the inorganic bentonite gel to be too low, even can not form the structure of the inorganic bentonite gel and loses the original auxiliary suspension property in the prior art, and the production efficiency is influenced because the inorganic bentonite gel is low in dispersion speed in an aqueous system. The invention realizes the aim of the dispersion speed of the modified bentonite inorganic gel in a water-based system by adding a proper amount of inorganic mineral to carry out composite modification on the bentonite inorganic gel.
In order to achieve the purpose, the invention provides a modified bentonite inorganic gel, which is prepared by compounding and modifying bentonite inorganic gel and inorganic minerals, wherein the inorganic minerals are fine purified attapulgite and/or sepiolite.
Preferably, the amount of the inorganic mineral is 10-200% of the mass of the bentonite inorganic gel.
Furthermore, the dosage of the inorganic mineral is 10-100% of the mass of the bentonite inorganic gel.
The invention also provides a preparation method of the modified bentonite inorganic gel, which comprises the following steps:
step S1: preparing bentonite inorganic gel pulp;
step S2: adding inorganic minerals into the bentonite inorganic gel ore pulp prepared in the step S1, stirring and mixing, and then carrying out an aging reaction;
and step S3: and (3) drying the slurry subjected to the aging reaction in the step (S2) to obtain the modified bentonite inorganic gel with good dispersibility.
As a preferred embodiment of the present invention, the specific operations of step S1 are: the powdery bentonite inorganic gel raw material is added with water to prepare bentonite inorganic gel ore pulp with the concentration of 5-15 wt%. Preferably, the concentration of the prepared bentonite inorganic gel ore pulp can be: for example, 5wt%, 6wt%, 7wt%, 8wt%, 9wt%, 10wt%, 11wt%, 12wt%, 13wt%, 14wt%, or 15wt%, etc.
As a preferable scheme of the invention, the inorganic mineral in the step S2 is any one or a combination of two of finely purified attapulgite and sepiolite; preferably, the amount of the inorganic mineral used in step S2 is 10% to 200%, more preferably 10% to 100%, of the mass of the bentonite inorganic gel.
In a preferred embodiment of the present invention, the stirring and mixing time in the step S2 is 1 to 2 hours, such as 1 hour, 1.5 hours, or 2 hours. The temperature for stirring and mixing in the step S2 is 20 to 40 ℃, for example, 20 ℃, 23 ℃, 25 ℃, 27 ℃, 30 ℃, 33 ℃, 35 ℃, 37 ℃ or 40 ℃.
In a preferred embodiment of the present invention, the temperature of the aging reaction in the step S2 is 20 to 40 ℃, for example, 20 ℃, 23 ℃, 25 ℃, 27 ℃, 30 ℃, 33 ℃, 35 ℃, 37 ℃ or 40 ℃.
Preferably, the aging reaction time in step S2 is 2 to 5 days, such as 2 days, 3 days, 4 days, 5 days, and the like, and more preferably 3 days.
In the invention, after inorganic mineral is added, stirred, mixed and modified, the slurry needs to be aged for a certain time, so that the modification is fully carried out, and the optimal modification effect is achieved.
In a preferred embodiment of the present invention, the drying in step S3 is spray drying, and the drying temperature is preferably 90 to 110 ℃, for example, 90 ℃, 93 ℃, 95 ℃, 97 ℃, 100 ℃, 103 ℃, 105 ℃, 107 ℃, or 110 ℃.
The drying time is adjusted according to actual needs, and is not particularly limited herein.
The invention also provides application of the modified bentonite inorganic gel, and the modified bentonite inorganic gel can be applied to water-suspended pesticides and water-based coatings.
The invention improves the structure of the bentonite inorganic gel by adding a proper amount of inorganic mineral to realize the aim of the dispersion speed of the modified bentonite inorganic gel in a water-based system, and the key factors are the selection and the dosage of the inorganic mineral and the aging time of the reaction slurry.
The working mechanism of the invention is as follows: each mineral has a specific structure, determining its characteristic properties; such as attapulgite, is an aqueous magnesium-rich silicate clay mineral having a chain layered structure, which belongs to the group consisting of 2: type 1 clay minerals, in each of 2: in the 1 unit structure layer, the angle tops of the tetrahedral wafers are reversed at a certain distance to form a layer chain, and due to the unique crystal structure of the attapulgite, the attapulgite has a plurality of special physical and chemical and technological properties, which are as follows: cation interchangeability, hydroscopicity, adsorption decoloration, large specific surface area (9.6-36 m < 2 >/g), colloid value and expansion capacity, and due to the performances, the cation exchange, hydroscopicity, adsorption decoloration, large specific surface area (9.6-36 m < 2 >/g), colloid value and expansion capacity are fast to disperse in water after being applied in the coating, the coating has good leveling property, shrinkage cavity and fish eye prevention, difficult sagging and the like, but the whole suspension performance is poor; the bentonite inorganic gel has a unique three-dimensional 'card house' structure, shows excellent suspension assisting performance, and utilizes the composite modification of the bentonite and the attapulgite to prepare a new product which has good suspension performance, can be dispersed in a water system quickly, and can assist in leveling, preventing sagging and preventing splashing in an aqueous coating.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
1. experiments prove that: when the bentonite inorganic gel obtained by the invention is prepared into 2.5% aqueous dispersion, the dispersion time is reduced to 8min from 15min of the original bentonite inorganic gel, the dispersion time is obviously reduced, the problem of long dispersion time of the existing bentonite inorganic gel in an aqueous system is solved, and meanwhile, the suspension performance of the aqueous dispersion is ensured to be not obviously changed.
2. The invention adopts inorganic mineral to carry out composite modification on the bentonite inorganic gel, and compared with the existing organic modifier, the invention has better environmental protection property and does not pollute the environment, thereby finding a better alternative scheme.
3. The modification method is simple and easy to implement, has low cost and is suitable for popularization and application.
Drawings
FIG. 1 is a process flow diagram of example 1 of the present invention.
Detailed Description
The present invention will be further understood by reference to the following examples, which are intended to illustrate the invention and not to represent all the technical solutions proposed by the invention, therefore, it should not be understood as a limitation to the general technical solutions of the present invention, and some insubstantial modifications which do not depart from the technical idea of the invention, such as simple changes or substitutions of technical features having the same or similar technical effects, will still fall within the scope of the present invention.
When the modified bentonite inorganic gel prepared in each of the following examples was formulated into a 1% aqueous dispersion (after standing for 24 hours), its suspensibility was measured by the following method:
148.5g of water is added into a 250mL beaker, 1.5g of a dried sample is weighed and put into the beaker, placed on a magnetic stirrer to be stirred for 30 minutes, poured into a 100mL measuring cylinder, and kept stand for 24 hours, and then the number of milliliters of separated water of slurry in the measuring cylinder is read.
The dispersion time of a 2.5% aqueous dispersion of the modified bentonite inorganic gel prepared in each of the following examples was measured as follows:
146.25g of water was added to a 250ml beaker, 3.75g of the dried sample was weighed and put into the beaker, and the beaker was placed on a magnetic stirrer to start dispersion, and the time was counted with a stopwatch. And observing the dispersion condition of the materials in the inorganic gel water dispersion until the materials are completely dispersed in the water, and recording the used time by pressing a stopwatch, namely the dispersion time.
Example 1:
adding 25kg of attapulgite (namely the using amount of the inorganic mineral is 25 percent of the mass of the inorganic gel raw material of the bentonite) into inorganic gel slurry with the solid content of 10 percent, preparing the inorganic gel slurry with the mass of the inorganic gel raw material of the bentonite of 100kg, stirring and mixing the inorganic gel slurry at 30 ℃ for 1.5h for modification reaction, aging the slurry at 30 ℃ for 3 days after the reaction, and then carrying out spray drying at 100 ℃ to obtain a modified product. As shown in fig. 1.
Example 2:
adding 50kg of modifier attapulgite (namely the amount of the inorganic mineral is 50 percent of the mass of the inorganic gel raw material of the bentonite) into slurry with the solid content of 8 percent, which is prepared from the inorganic gel raw material of the bentonite with the mass of 100kg, stirring and mixing the slurry for 2 hours at the temperature of 20 ℃ for modification reaction, aging the slurry for 3 days at the temperature of 20 ℃ after the reaction, and then carrying out spray drying at the temperature of 100 ℃ to obtain a modified product.
Example 3:
100kg of modifier attapulgite (namely the amount of the inorganic mineral is 100 percent of the mass of the raw material of the bentonite inorganic gel) is added into slurry with the solid content of 6 percent, the slurry is stirred and mixed for 2 hours at the temperature of 20 ℃ for modification reaction, the slurry is aged for 3 days at the temperature of 20 ℃ after the reaction, and then the slurry is spray-dried at the temperature of 100 ℃ to obtain a modified product.
Example 4:
adding 200kg modifier attapulgite (namely the amount of the inorganic mineral is 200 percent of the mass of the inorganic gel raw material of the bentonite) into slurry with the solid content of 5 percent, which is prepared from 100kg of the inorganic gel raw material of the bentonite, stirring and mixing the slurry for 2 hours at 20 ℃ for modification reaction, aging the slurry for 3 days at 20 ℃ after the reaction, and then carrying out spray drying at 100 ℃ to obtain a modified product.
Example 5:
the method comprises the following steps of adding 10kg of modifier attapulgite (namely the amount of inorganic minerals is 10 percent of the mass of the raw material of the inorganic bentonite gel) into slurry with the solid content of 15 percent prepared from the raw material of the inorganic bentonite gel of 100kg, stirring and mixing the slurry at 40 ℃ for 2 hours for modification reaction, aging the slurry at 40 ℃ for 2 days after the reaction, and then carrying out spray drying at 90 ℃ to obtain a modified product.
Example 6:
adding 200kg modifier attapulgite (namely the amount of the inorganic mineral is 200 percent of the mass of the inorganic gel raw material of the bentonite) into slurry with the solid content of 5 percent, which is prepared from 100kg of the inorganic gel raw material of the bentonite, stirring and mixing the slurry for 1h at 40 ℃ for modification reaction, aging the slurry for 5 days at 40 ℃ after the reaction, and then carrying out spray drying at 110 ℃ to obtain a modified product.
Comparative example 1:
the bentonite inorganic gel product conventional in the prior art was used as comparative example 1.
Comparative example 2:
the conventional attapulgite gel product in the prior art was used as comparative example 2.
The products prepared in examples 1 to 4 and comparative examples 1 to 2 were formulated into aqueous dispersions for dispersion time evaluation and suspension property evaluation, and the evaluation results are shown in Table 1.
Table 1: property test Table for products obtained in examples 1 to 4 and comparative examples 1 to 2
From the results of examples 1-4 and comparative examples 1-2, it can be seen that when 2.5% aqueous dispersion is prepared from the inorganic gel product prepared by the method of the present invention, the dispersion time is reduced from 15min of the original bentonite inorganic gel to 8min, and the dispersion time is significantly reduced, which indicates that the modifier has a modifying effect on the bentonite inorganic gel and solves the problem of long dispersion time of the existing bentonite inorganic gel in an aqueous system; in addition, when the modified inorganic gel product prepared by the method is prepared into 2.5% aqueous dispersion, the dispersion time is obviously reduced, and when the dosage of the modifier is less than 100%, the suspension performance of 1% aqueous dispersion (after standing for 24 h) is not obviously changed, so the application range of the modified inorganic gel product can be further expanded; the modification method is simple and easy to implement, low in cost and suitable for popularization and application.
The applicant states that the present invention is illustrated by the above examples to show the detailed method of the present invention, but the present invention is not limited to the above detailed method, that is, it does not mean that the present invention must rely on the above detailed method to be carried out. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of the raw materials of the product of the present invention, and the addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (3)
1. The preparation method of the modified bentonite inorganic gel is characterized in that the modified bentonite inorganic gel is prepared by compounding and modifying bentonite inorganic gel and inorganic minerals, wherein the inorganic minerals are finely purified attapulgite and/or sepiolite; the preparation method of the modified bentonite inorganic gel comprises the following steps:
step S1: preparing bentonite inorganic gel ore pulp, namely adding water into powdery bentonite inorganic gel raw materials to prepare the bentonite inorganic gel ore pulp with the concentration of 5-15 wt%;
step S2: adding inorganic minerals into the bentonite inorganic gel pulp prepared in the step S1, stirring and mixing for 1-2 h at the stirring and mixing temperature of 20-40 ℃, and then carrying out an aging reaction at the aging reaction temperature of 20-40 ℃ for 2-5 days; the inorganic mineral in the step S2 is one or the combination of two of fine purified attapulgite and sepiolite; the using amount of the inorganic mineral in the step S2 is 10-100% of the mass of the bentonite inorganic gel;
and step S3: and (3) spray-drying the slurry subjected to the aging reaction in the step (S2) at the drying temperature of 90-110 ℃ to obtain the modified bentonite inorganic gel with good dispersibility.
2. The modified bentonite inorganic gel prepared by the method for preparing the modified bentonite inorganic gel according to claim 1.
3. The use of the modified bentonite inorganic gel according to claim 2, wherein the modified bentonite inorganic gel is used in water-suspended pesticides, water-based coatings.
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