CN112978743A - Preparation method of high-acid-resistance modified lithium magnesium silicate - Google Patents
Preparation method of high-acid-resistance modified lithium magnesium silicate Download PDFInfo
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Abstract
The invention discloses a preparation method of high acid-resistant modified lithium magnesium silicate, which is characterized by comprising the following steps of: firstly, manganese salt, ferric salt, silica sol and the like are used as raw materials, and magnesium lithium silicate with a layered structure is prepared through a high-temperature hydrothermal reaction; the lattice structure has a large number of trioctahedral and tetrahedral holes and can accommodate more H+Therefore, the modified starch still shows excellent tackifying and thickening performances in acid solution with higher concentration, and can be widely applied to occasions involving acidity in the industries of paint, detergent, cosmetics, electronic chemicals, environmental protection treatment and the like.
Description
Technical Field
The invention relates to the field of synthesis of trioctahedral layered silicate mineral magnesium lithium silicate, in particular to a method for synthesizing magnesium lithium silicate with a large number of cavities in a lamella crystal, strong acid resistance and excellent thickening performance.
Background
Lithium magnesium silicate (commonly known as "hectorite") is a trioctahedral layered silicate mineral whose unit cell is composed of an upper and a lower layer of Si-O tetrahedra sandwiching a layer of Li/Mg-O trioctahedral. The magnesium lithium silicate is a typical two-dimensional nano mineral material, and the theoretical chemical components of the magnesium lithium silicate are as follows: SiO 22 55%-60%、MgO 24%-30%、Na2O 2.5%-3.0%、Li20.5 to 1.0 percent of O. The crystal structure unit (platelet) of magnesium lithium silicate is a nano-level fine thin sheet, and the surface of the sheet is covered with Na+And the like exchangeable cations; when the lithium magnesium silicate particles are mixed with water, the water is Na-coated+Adsorbing to the surface of the platelets, thereby gradually spreading the platelets apart and until the platelets are completely separated from each other. Since the layer surface (end surface) of the platelet is negatively charged and the side surface is positively charged, the separated platelets can rapidly form a colloid structure of a three-dimensional space (namely 'card house') in an end surface-side electrostatic attraction manner") to further increase the viscosity of the aqueous system, and the aqueous system has the characteristics of high suspension property, thickening property, thixotropy and the like, so that the lithium magnesium silicate is an ideal thickening rheological agent of the aqueous system.
Although conventional lithium magnesium silicate is excellent in thickening and thickening properties in water, its thickening ability rapidly deteriorates (the larger the acid concentration, the larger the deterioration degree) by contacting only a small amount of acid, mainly because of H in the acid solution+Rapid destruction of the lattice structure by dehydroxylation, leading to Zn2+、Mg2+、Fe3+Continuously separating out, so that the trioctahedral and the tetrahedron are damaged quickly in sequence; if the acid concentration is slightly higher, most or all of the lamellar structure and interlaminar domains of the lithium magnesium silicate are destroyed, at which point the thickening, properties of the magnesium silicate are almost completely lost. This is a technical bottleneck in the field of rheological additives and has not been properly solved. Therefore, how to prepare the magnesium lithium silicate with excellent acid resistance is a technical problem which is urgently needed to be solved by related industries at home and abroad at present.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the lithium magnesium silicate with a large number of holes in a platelet, strong acid resistance and excellent thickening performance and the preparation method thereof. The preparation method adopts manganese salt, ferric salt, silica sol and the like as raw materials, and magnesium lithium silicate is synthesized under the high-temperature hydrothermal condition; adding it into acid solution with higher concentration, and containing a certain amount of H due to more holes in lattice structure+Still exhibits excellent thickening and viscosity-increasing properties, and thus can be widely used in the fields of paints, detergents, cosmetics, electronic chemicals, medicines, and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high acid resistance modified lithium magnesium silicate is characterized by comprising the following steps: the preparation method comprises the following steps of:
(1) firstly, 0.01-0.05 part of manganese salt, 1-5 parts of ferric salt, 30-60 parts of silica sol and 500 parts of pure water are added into a hydrothermal reaction kettle and fully stirred for 10-30 min;
(2) then adding 0.1-0.5 part of copper salt, 1-5 parts of zinc salt, 5 parts of sodium carbonate and 20-40 parts of magnesium salt, fully stirring for 10-30 min, raising the temperature to 120-180 ℃ in a sealed manner, and carrying out heat preservation reaction for 30-60 min;
(3) and stopping reaction discharging, filtering and fully washing the reaction solution, and drying the collected filter cake at 300-400 ℃ for 10-30 min to obtain the modified lithium magnesium silicate.
In the invention, the manganese salt is one or any combination of manganese chloride, manganese sulfate, manganese nitrate and manganese acetate; the ferric salt is one or any combination of ferric chloride, ferric sulfate and ferric nitrate; the copper salt is one or any combination of copper chloride, copper sulfate and copper nitrate; the zinc salt is one or any combination of zinc chloride, zinc sulfate and zinc nitrate; the magnesium salt is one or any combination of magnesium chloride, magnesium sulfate and magnesium nitrate.
Firstly, manganese salt, ferric salt and silica sol are mixed in water, and then SiO is added under the salting-out action2The sol particles gradually separate out and adsorb Mn2+And Fe3+(ii) a Mn during the subsequent high temperature hydrothermal reaction2+-Fe3+/SiO2Will convert to Mn-Fe/Si-O tetrahedra. In the present invention, a trace amount of Mn2+The material is very important, and plays a role in promoting mineralization crystallization on the formation of a magnesium lithium silicate layered structure; if the amount of manganese salt is less than 0.01 part, Mn is added2+-Fe3+/SiO2Cannot be converted into Mn-Fe/Si-O tetrahedron; if the amount of the manganese salt is more than 0.05 part, only Mn (OH) can be generated in the high-temperature hydrothermal reaction stage2、Fe(OH)3And SiO2And (4) precipitating. Meanwhile, if the amount of the iron salt is less than 1 part, the number of holes in the Mn-Fe/Si-O tetrahedron is too small to trap and hold a large amount of H+(ii) a If the amount of the iron salt is more than 5 parts, the Mn-Fe/Si-O tetrahedron is unstable and is easily converted into Fe (OH) during the hydrothermal reaction at high temperature3、SiO2And precipitating.
Then copper salt, zinc salt, sodium carbonate and magnesium salt are added into the reaction system, and under the action of hydrolysisPremature Cu (OH) is slowly formed2-Zn(OH)2-Mg(OH)2And (4) coprecipitation. In the high-temperature hydrothermal reaction process (120-180 ℃ and heat preservation reaction for 30-60 min), Mn is used for the coprecipitation2+-Fe3+/SiO2Gradually stacking and arranging the templates and slowly forming a Cu-Zn-Mg-O trioctahedron; and after the high-temperature hydrothermal reaction is finished, drying the fully washed filter cake at 300-400 ℃ for 10-30 min, and completely curing the layered structure to obtain the modified lithium magnesium silicate. In the present invention, Mn must be formed first2+-Fe3+/SiO2Post production of Cu (OH)2-Zn(OH)2-Mg(OH)2Coprecipitation is carried out, and the coprecipitation is used as a template to be gradually accumulated, so that a layered structure can be formed in a high-temperature hydrothermal reaction stage. In addition, the copper salt and the zinc salt also play a role in promoting the formation of mineralized crystals, so if the amount of the copper salt is less than 0.1 part or the amount of the zinc salt is less than 1 part, not only is the stable lamellar structure difficult to form, but also the number of holes in the Cu-Zn-Mg-O trioctahedron is rapidly reduced, so that the Cu-Zn-Mg-O trioctahedron is very easy to be subjected to H+Attack to be destroyed; if the dosage of the copper salt is more than 0.5 part or the dosage of the zinc salt is more than 5 parts, the Cu-Zn-Mg-O trioctahedral is unstable and is easily converted into Cu (OH) in the high-temperature hydrothermal reaction process2、Zn(OH)2、Mg(OH)2And (4) precipitating. In addition, if the hydrothermal reaction temperature is less than 120 ℃ or the hydrothermal reaction time is less than 10min, the layered structure is immature and easily collapses; if the hydrothermal reaction temperature is higher than 180 ℃ or the reaction time is more than 30min, the number of cavities is obviously reduced, and the H resistance of the lithium magnesium silicate is obviously reduced+Ability to erode.
The modified magnesium lithium silicate prepared by the invention has a brand new lattice structure completely different from the conventional magnesium lithium silicate: the upper and lower layers are Cu-Zn-Mg-O trioctahedral (no isomorphous replacement exists, so that the charge is zero); ② the middle layer is Mn-Fe/Si-O tetrahedron (a small amount of Fe in tetrahedron)3+And trace amount of Mn2+Isomorphously displacing part of Si4+And therefore exhibit a negative charge); obviously, the overall modified magnesium lithium silicate lattice prepared by the invention is negative in charge. The upper and lower layers of conventional lithium magnesium silicate are zero-charge Si-O-IVThe middle layer of the surface body is Li/Mg-O trioctahedral with negative charges, and the whole crystal lattice structure of the surface body presents negative charges.
The modified magnesium lithium silicate prepared by the invention contains enough holes in Mn-Fe/Si-O tetrahedron and Cu-Zn-Mg-O trioctahedron, and has excellent salt resistance. When the modified lithium magnesium silicate is placed in an acid solution, H+Rapidly migrate into Cu-Zn-Mg-O trioctahedral and Mn-Fe/Si-O tetrahedron; h is greater in the lattice structure than in the case of a lattice structure containing more holes+The modified magnesium lithium silicate mainly occupies the holes and attacks the lattice structure in a dehydroxylation mode, so that the modified magnesium lithium silicate has excellent acid resistance. The advantage is the most core innovation point of the invention, and the key technical bottleneck that the acid resistance of the existing smectite minerals such as lithium magnesium silicate, bentonite and montmorillonite is extremely poor is thoroughly solved.
Compared with the prior art, the invention has the beneficial effects that: the largest key technical problem that the viscosity performance of the magnesium lithium silicate is rapidly deteriorated in an acid solution is thoroughly solved by obviously increasing the number of holes in the trioctahedron and the tetrahedron of the magnesium lithium silicate, and the blank of related technologies at home and abroad is filled up, so that the magnesium lithium silicate can be widely applied to occasions involving acidity in the industries of coatings, detergents, cosmetics, electronic chemicals, environmental protection treatment, medicines, foods and the like.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
A high acid resistance modified magnesium lithium silicate and a preparation method thereof are characterized in that: the preparation method comprises the following steps of:
(1) firstly, 0.01 part of manganese chloride, 1 part of ferric sulfate, 30 parts of silica sol and 500 parts of pure water are added into a hydrothermal reaction kettle and fully stirred for 10 min;
(2) then adding 0.1 part of copper nitrate, 1 part of zinc chloride, 5 parts of sodium carbonate and 20 parts of magnesium sulfate, fully stirring for 10min, raising the temperature to 120 ℃ in a closed manner, and carrying out heat preservation reaction for 30 min;
(3) and then stopping reaction discharging, filtering and fully washing the reaction solution, and drying the collected filter cake at 300 ℃ for 10min to obtain the modified lithium magnesium silicate No. 1.
Example 2
A high acid resistance modified magnesium lithium silicate and a preparation method thereof are characterized in that: the preparation method comprises the following steps of:
(1) firstly, 0.03 part of manganese sulfate, 0.02 part of manganese nitrate, 2.5 parts of ferric chloride, 2.5 parts of ferric nitrate, 60 parts of silica sol and 500 parts of pure water are added into a hydrothermal reaction kettle and fully stirred for 30 min;
(2) then adding 0.2 part of copper chloride, 0.3 part of copper sulfate, 4 parts of zinc sulfate, 1 part of zinc nitrate, 5 parts of sodium carbonate, 20 parts of magnesium chloride and 20 parts of magnesium nitrate, fully stirring for 30min, raising the temperature to 180 ℃ in a sealed manner, and carrying out heat preservation reaction for 60 min;
(3) and then stopping reaction discharging, filtering and fully washing the reaction solution, and drying the collected filter cake at 400 ℃ for 30min to obtain the modified lithium magnesium silicate No. 2.
Example 3
A high acid resistance modified magnesium lithium silicate and a preparation method thereof are characterized in that: the preparation method comprises the following steps of:
(1) firstly, 0.01 part of manganese sulfate, 0.01 part of manganese nitrate, 0.01 part of manganese acetate, 0.5 part of ferric chloride, 1.5 parts of ferric sulfate, 1 part of ferric nitrate, 40 parts of silica sol and 500 parts of pure water are added into a hydrothermal reaction kettle and fully stirred for 20 min;
(2) then adding 0.1 part of copper chloride, 0.1 part of copper sulfate, 0.1 part of copper nitrate, 1.3 parts of zinc chloride, 1 part of zinc sulfate, 1.4 parts of zinc nitrate, 5 parts of sodium carbonate, 5 parts of magnesium chloride, 10 parts of magnesium sulfate and 16 parts of magnesium nitrate, fully stirring for 20min, raising the temperature to 140 ℃ in a sealed manner, and carrying out heat preservation reaction for 40 min;
(3) and then stopping reaction discharging, filtering and fully washing the reaction solution, and drying the collected filter cake at 330 ℃ for 15min to obtain the modified lithium magnesium silicate No. 3.
Example 4
A high acid resistance modified magnesium lithium silicate and a preparation method thereof are characterized in that: the preparation method comprises the following steps of:
(1) firstly, 0.01 part of manganese chloride, 0.01 part of manganese sulfate, 0.01 part of manganese nitrate, 0.01 part of manganese acetate, 2 parts of ferric chloride, 1 part of ferric sulfate, 1 part of ferric nitrate, 50 parts of silica sol and 500 parts of pure water are added into a hydrothermal reaction kettle and fully stirred for 25 min;
(2) then adding 0.1 part of copper chloride, 0.1 part of copper sulfate, 0.2 part of copper nitrate, 2 parts of zinc chloride, 1 part of zinc sulfate, 1.5 parts of zinc nitrate, 5 parts of sodium carbonate, 15 parts of magnesium chloride, 10 parts of magnesium sulfate and 10 parts of magnesium nitrate, fully stirring for 25min, raising the temperature to 120-180 ℃ in a sealed manner, and carrying out heat preservation reaction for 30-60 min;
(3) and then stopping reaction discharging, filtering and fully washing the reaction solution, and drying the collected filter cake at 380 ℃ for 25min to obtain the modified lithium magnesium silicate No. 4.
Comparative example 1
The amount of manganese chloride was changed to 0.005 part, and the remaining reaction parameters and process conditions were completely the same as those in example 1, and the modified lithium magnesium silicate thus prepared was denoted by No. 5.
Comparative example 2
The amount of manganese chloride was changed to 0.06 part, and the remaining reaction parameters and process conditions were completely the same as those in example 1, and the modified lithium magnesium silicate thus prepared was denoted by No. 6.
Comparative example 3
The amount of ferric sulfate was changed to 0.5 part, the remaining reaction parameters and process conditions were completely the same as those in example 1, and the modified lithium magnesium silicate thus prepared was denoted as No. 7.
Comparative example 4
The amount of ferric sulfate was changed to 6 parts, the remaining reaction parameters and process conditions were completely the same as those in example 1, and the modified lithium magnesium silicate thus prepared was designated as No. 8.
Comparative example 5
The amounts of copper chloride and copper sulfate were changed to 0.04 parts, and the remaining reaction parameters and process conditions were completely the same as those in example 2, and the modified lithium magnesium silicate thus prepared was denoted by No. 9.
Comparative example 6
The amounts of copper chloride and copper sulfate were changed to 0.3 part and 0.4 part, respectively, and the remaining reaction parameters and process conditions were completely the same as those in example 2, and the modified lithium magnesium silicate thus prepared was designated as No. 10.
Comparative example 7
The amounts of zinc sulfate and zinc nitrate were changed to 0.5 part and 0.4 part, respectively, and the remaining reaction parameters and process conditions were completely the same as those in example 2, and the modified lithium magnesium silicate thus prepared was designated as No. 11.
Comparative example 8
The amounts of zinc sulfate and zinc nitrate were changed to 2 parts and 4 parts, respectively, and the remaining reaction parameters and process conditions were completely the same as those in example 2, and the modified lithium magnesium silicate thus prepared was designated as No. 12.
Comparative example 9
The high-temperature hydrothermal reaction temperature was changed to 110 ℃ and the remaining reaction parameters and process conditions were completely the same as those in example 3, and the modified lithium magnesium silicate thus prepared was designated as No. 13.
Comparative example 10
The high temperature hydrothermal reaction time was changed to 20min, the remaining reaction parameters and process conditions were completely the same as those in example 3, and the modified lithium magnesium silicate prepared was denoted as No. 14.
Comparative example 11
The high-temperature hydrothermal reaction temperature was changed to 190 ℃ and the remaining reaction parameters and process conditions were completely the same as those in example 4, and the modified lithium magnesium silicate thus prepared was designated as No. 15.
Comparative example 12
The high temperature hydrothermal reaction time was changed to 70min, the remaining reaction parameters and process conditions were completely the same as in example 4, and the modified lithium magnesium silicate prepared was denoted as No. 16.
Comparative example 13
Firstly generating Cu (OH) in a reaction kettle2-Zn(OH)2-Mg(OH)2Coprecipitation to regenerate Mn2+-Fe3+/SiO2The remaining reaction parameters and process conditions were completely the same as in example 4, and the modified lithium magnesium silicate thus prepared was designated as No. 17.
The results of viscosity comparison tests of modified magnesium lithium silicate Nos. 1 to 17 and imported magnesium lithium silicate (model: RD, BYK, Germany) prepared in the above examples are shown in Table 1. The testing process comprises the following steps: adding 2 parts of lithium magnesium silicate into 100 parts of various solutions, fully stirring for pulping, keeping the temperature in a water bath at 25 ℃ and standing for 24 hours, and then measuring the plastic viscosity.
Table 1 comparative test data
Note: x-it has no practical meaning of platelets due to the almost absence of lamellar structure; or the solution is quickly and completely invalid in a dilute sulfuric acid solution, and quickly delaminates after standing, so that the plastic viscosity and the thixotropy value cannot be measured.
As can be seen from table 1 comparing the test data: (1) the reaction parameters and the process conditions must be strictly limited within the technical requirements of the invention, otherwise, on one hand, most products (such as No.5, No.6 and the like) do not have a laminated structure, and on the other hand, part of products (such as No.7, No.15 and the like) have a laminated structure, but have extremely poor viscous performance in pure water and dilute acid solution and have no practicability at all. (2) The modified magnesium lithium silicate prepared by the invention contains a large number of cavities in the lattice structure, and when H & lt + & gt is submerged in the lattice structure, the cavities are occupied preferentially, so that the lattice structure is not damaged, the acid resistance of the modified magnesium lithium silicate is excellent (when the mass fraction of dilute sulfuric acid reaches 10%, the plastic viscosity of the dilute sulfuric acid is reduced by 20-30%), and the modified magnesium lithium silicate is far better than like products imported from abroad, and therefore, the modified magnesium lithium silicate has a bright application prospect in acidic occasions in the industries such as coatings, detergents, cosmetics, electronic chemicals, environmental protection treatment and the like.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (6)
1. A preparation method of high acid resistance modified lithium magnesium silicate is characterized by comprising the following steps: the preparation method comprises the following steps of:
(1) firstly, 0.01-0.05 part of manganese salt, 1-5 parts of ferric salt, 30-60 parts of silica sol and 500 parts of pure water are added into a hydrothermal reaction kettle and fully stirred for 10-30 min;
(2) then adding 0.1-0.5 part of copper salt, 1-5 parts of zinc salt, 5 parts of sodium carbonate and 20-40 parts of magnesium salt, fully stirring for 10-30 min, raising the temperature to 120-180 ℃ in a sealed manner, and carrying out heat preservation reaction for 30-60 min;
(3) and stopping reaction discharging, filtering and fully washing the reaction solution, and drying the collected filter cake at 300-400 ℃ for 10-30 min to obtain the modified lithium magnesium silicate.
2. The method for preparing the high acid resistance modified lithium magnesium silicate as claimed in claim 1, wherein the method comprises the following steps: the manganese salt is one or any combination of manganese chloride, manganese sulfate, manganese nitrate and manganese acetate.
3. The method for preparing the high acid resistance modified lithium magnesium silicate as claimed in claim 1, wherein the method comprises the following steps: the ferric salt is one or any combination of ferric chloride, ferric sulfate and ferric nitrate.
4. The method for preparing the high acid resistance modified lithium magnesium silicate as claimed in claim 1, wherein the method comprises the following steps: the copper salt is one or any combination of copper chloride, copper sulfate and copper nitrate.
5. The method for preparing the high acid resistance modified lithium magnesium silicate as claimed in claim 1, wherein the method comprises the following steps: the zinc salt is one or any combination of zinc chloride, zinc sulfate and zinc nitrate.
6. The method for preparing the high acid resistance modified lithium magnesium silicate as claimed in claim 1, wherein the method comprises the following steps: the magnesium salt is one or any combination of magnesium chloride, magnesium sulfate and magnesium nitrate.
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US3928663A (en) * | 1974-04-01 | 1975-12-23 | Amp Inc | Modified hectorite for electroless plating |
EP0088372A1 (en) * | 1982-03-05 | 1983-09-14 | Hoechst Aktiengesellschaft | Process for the production of synthetic hectorite |
CN88101836A (en) * | 1987-02-17 | 1988-12-07 | 阿姆斯特朗世界工业公司 | 2: 1 phyllosilicates of flocculation reach by its water-resistant product of making |
JPH06292831A (en) * | 1993-04-12 | 1994-10-21 | Mitsubishi Heavy Ind Ltd | Denitriding catalyst |
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