CN113003582A - Preparation method of high-salt-resistance high-performance modified lithium magnesium silicate - Google Patents
Preparation method of high-salt-resistance high-performance modified lithium magnesium silicate Download PDFInfo
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Abstract
The invention discloses a preparation method of high-salt-resistance high-performance modified lithium magnesium silicate, which is characterized by comprising the following steps of: firstly, taking strontium salt, magnesium salt, lithium salt, silica sol and the like as raw materials, and preparing magnesium lithium silicate with a layered structure through a high-temperature hydrothermal reaction; the lamellar crystal has small charge quantity and poor affinity with various cations, and can quickly form a gel structure of a card house, so that the lamellar crystal still keeps excellent thickening capacity in a high-concentration salt solution, and can be widely used as a thickening agent, a thixotropic agent, a stabilizer and a suspending agent in the industries of toothpaste, cosmetics, emulsion paint, medicine and the like.
Description
Technical Field
The invention relates to the field of synthesis of a trioctahedral layered silicate mineral magnesium lithium silicate, in particular to a synthesis method of magnesium lithium silicate with small charge, strong salt resistance and excellent thickening performance.
Background
Lithium magnesium silicate (hectorite), also known as laponite, is composed of two layers of coterminous silicon-oxygen tetrahedra (Si-O tetrahedra) sandwiched between two layers of coterminous magnesium-oxygen trioctahedral (Mg-O trioctahedral) 2: the type 1T-O-T silicate mineral containing crystal water and having a periodic layered arrangement structure. Due to isovalent isomorphous substitution, Mg in Mg-O trioctahedral of the lattice structure2+Is covered with Li+And the like, which causes the unbalance of lattice charges, namely, a certain amount of permanent negative charges are generated on the end face; in order to maintain electrical balance, a large number of exchangeable cations such as K must be present between the layers+、Na+、Ca2+Etc., these cations can adsorb several layers of water molecules, thereby forcing the platelets to separate from each other (i.e., swell) and until they are completely separated (i.e., delaminated). The numerous platelets thus formed utilize the negative charges on the cross section and the positive charges on the side surface,the structure of 'card house' is formed through electrostatic attraction, so that water molecules are bound to a certain degree and cannot flow freely, namely, the phenomenon of thickening and thickening is macroscopically shown.
As an ideal rheological additive for thickening, the lithium magnesium silicate is widely applied to the industries of water-based paint, detergent, cosmetics and the like. However, if the formulation contains a large amount of salt (such as inorganic salt, ionic surfactant, etc.), Ca is particularly preferred2+、Mg2+、Al3+The thickening and thickening properties of magnesium lithium silicate, which is an equivalent divalent or trivalent salt, are rapidly and significantly reduced. This is mainly due to Na+、Ca2+、Al3+The cations can generate electrostatic attraction with the lithium magnesium silicate platelets with negative charges, so that a 'card house' structure cannot be formed smoothly, and the thickening capacity of the thickening agent is reduced sharply. The higher the salt concentration is, the larger the cation number is, the poorer the thickening effect of thickening by magnesium lithium silicate. This is the most critical technical bottleneck in the current rheological additive field, and has always plagued the magnesium lithium silicate field. Therefore, how to prepare the magnesium lithium silicate which still has excellent tackifying and thickening capabilities in a salt solution 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 a preparation method of lithium magnesium silicate with less charge, strong salt resistance and excellent thickening performance. The preparation method adopts strontium salt, magnesium salt, lithium salt, silica sol and the like as raw materials, and magnesium lithium silicate is synthesized under the high-temperature hydrothermal condition; the gel structure can almost completely avoid the negative effects of various cations, can still smoothly form a 'card house' gel structure in a high-concentration salt solution, and keeps excellent viscosity performance, so that the gel structure can be widely applied to industries such as toothpaste, cosmetics, emulsion paint, medicine and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high-salt-resistance high-performance modified lithium magnesium silicate is characterized by comprising the following steps: the preparation method comprises the following steps of:
(1) firstly, adding 1-5 parts of strontium salt, 30-60 parts of magnesium salt, 0.1-0.5 part of lithium salt, 5 parts of sodium carbonate and 500 parts of pure water into a hydrothermal reaction kettle and fully stirring for 10-30 min;
(2) then adding 0.2-0.8 part of zinc salt, 0.2-0.8 part of aluminum salt and 20-50 parts of silica sol, fully and uniformly stirring, then raising the temperature to 120-150 ℃ in a closed manner, and carrying out heat preservation reaction for 30-60 min;
(3) and stopping reaction discharging, filtering and fully washing the reaction solution, and roasting the collected filter cake at the high temperature of 200-300 ℃ for 30-60 min to obtain the modified magnesium lithium silicate.
In the invention, the strontium salt is one or two of strontium chloride and strontium nitrate which are combined randomly; the magnesium salt is one or any combination of magnesium chloride, magnesium sulfate and magnesium nitrate; the lithium salt is one or any combination of more of lithium chloride, lithium sulfate, lithium nitrate and lithium hydroxide; the zinc salt is one or any combination of zinc chloride, zinc sulfate and zinc nitrate; the aluminum salt is one or any combination of aluminum chloride, aluminum sulfate and aluminum nitrate.
Firstly, mixing strontium salt, magnesium salt, sodium carbonate and lithium salt in water, and simultaneously carrying out hydrolysis reaction on the strontium salt and the magnesium salt to gradually generate very unstable Sr (OH)2And Mg (OH)2(the coprecipitation host is Mg (OH))2With only a small amount of Sr (OH)2And doped with a trace amount of Li+) The development degree of a precipitation structure system is poor and immature, so that the Li/Sr-Mg-O trioctahedral crystal is easily converted into the Li/Sr-Mg-O trioctahedral crystal in a subsequent high-temperature hydrothermal reaction stage. In the present invention, the amount of strontium salt is important: if the strontium salt is less than 1 part, only part of Li is present+/Sr(OH)2-Mg(OH)2Coprecipitation can be converted to trioctahedral form mainly due to Sr2+The catalyst plays a role in promoting the formation of a magnesium lithium silicate layered structure; if the dosage of the strontium salt is more than 5 parts, only Sr (OH) can be generated in the subsequent high-temperature hydrothermal reaction stage2And Mg (OH)2Two kinds of precipitates. At the same time, only water-soluble strontium salts (if strontium sulfate or other sparingly water-soluble strontium salts are used instead, it is not possible at all to useFormation of Li+/Sr(OH)2-Mg(OH)2Coprecipitation). Furthermore, because of Li+For Sr (OH)2-Mg(OH)2The coprecipitation has a stabilizing effect, so if the amount of lithium salt is less than 0.1 part, Li+the/Sr-Mg-O trioctahedral is unstable, and thus a layered structure is difficult to form smoothly; if the amount of the lithium salt is more than 0.5 part, Li is excessively contained+Aggregate in the interlayer region, resulting in interlayer structure susceptible to Li during high temperature firing+Collapse.
Then adding zinc salt, aluminum salt and silica sol into the reaction system, and Zn under the salting-out action2+-Al3+/SiO2Sol particles with Li+/Sr(OH)2-Mg(OH)2The coprecipitation is the stacking and ordered arrangement of templates, and then a layered structure is gradually formed under the high-temperature hydrothermal condition (the heat preservation reaction is carried out for 30-60 min at the temperature of 120-150 ℃). After the high-temperature hydrothermal reaction is finished, roasting the fully washed filter cake at the high temperature of 200-300 ℃ for 30-60 min, and completely crystallizing and aging the layered structure to obtain the modified magnesium lithium silicate. In the present invention, Li must be generated first+/Sr(OH)2-Mg(OH)2Coprecipitation, post-formation of Zn2+-Al3+/SiO2The former is used as a template to be gradually stacked, and a layered structure can be formed in a high-temperature hydrothermal reaction stage. In addition, if the amount of the zinc salt or the aluminum salt is less than 0.2 part, the amount of negative charges of Zn-Al/Si-O tetrahedrons is too small, so that the magnesium silicate lithium cannot absorb enough water molecules through a hydration process due to insufficient amount of interlayer cations, the bonding force between platelets is difficult to break through, and the expansion and the flaking capability of the magnesium silicate lithium in a salt solution are rapidly weakened; if the amount of the zinc salt or the aluminum salt is more than 0.8 part, only Zn (OH) is generated in the subsequent high-temperature hydrothermal reaction stage2、Al(OH)3And SiO2Three kinds of precipitates. Meanwhile, if the high-temperature hydrothermal reaction temperature is lower than 120 ℃ or the high-temperature hydrothermal reaction time is shorter than 30min, the layered structure is immature and unstable; if the high-temperature hydrothermal reaction temperature is higher than 150 ℃ or the reaction time is more than 60min, the lattice structure of the magnesium lithium silicate is over mature, the bonding force between platelets is large, and therefore the high-temperature hydrothermal reaction temperature is remarkably reducedSwelling in saline solution and flaking.
The modified magnesium lithium silicate prepared by the invention has a brand new lattice structure which is quite different from the conventional magnesium lithium silicate: the upper and lower layers are Zn-Al/Si-O tetrahedron (small amount of Al in tetrahedron)3+And trace amount of Zn2+By substitution of part of Si4+And therefore exhibit a negative charge); ② the middle layer is Li/Sr-Mg-O trioctahedral (Mg and a small amount of Sr and O form the trioctahedral, and a small amount of Li+By substitution of part of Mg2+And therefore also exhibits a negative charge); obviously, the overall modified magnesium lithium silicate lattice prepared by the invention is negative in charge. It is known that the upper and lower layers of conventional magnesium lithium silicate are zero charge Si-O tetrahedra, the middle layer is negatively charged Li/Mg-O trioctahedral, and the whole lattice structure thereof exhibits negative charges.
The Zn-Al/Si-O tetrahedron and the Li/Sr-Mg-O trioctahedron of the modified magnesium lithium silicate prepared by the invention both present negative charges, but because Zn2+、Al3+And Li+The substitution amount is small, so the negative charge amount is small (the cell layer charge amount is only about 0.35-0.40), which is obviously smaller than that of the conventional magnesium lithium silicate (the cell layer charge amount is about 0.50-0.60), when the lithium magnesium silicate is dissolved in water and fully expanded and peeled, the lithium magnesium silicate platelets have little negative charge amount, so the lithium magnesium silicate platelets and Na in water+、Ca2+、Mg2+、Al3 +The affinity of the polyvalent metal cations is quickly weakened, so that the interference and attack of high-concentration salt solution and the polyvalent metal cations on the formation of a 'card house' structure of the lamella are effectively avoided, namely the viscosity performance of the magnesium lithium silicate is still excellent. The method has the advantages of being the most core innovation point, and thoroughly solving the key technical bottleneck that the viscosity performance of the existing smectite minerals such as bentonite, montmorillonite, magnesium lithium silicate and the like is rapidly deteriorated in high-salt concentration and polyvalent metal salt solutions.
Compared with the prior art, the invention has the beneficial effects that: the method completely solves the biggest key technical problem that the viscosity performance of the magnesium lithium silicate is rapidly deteriorated in high-concentration salt solution and multivalent metal salt solution by effectively reducing the quantity of negative charges of the magnesium lithium silicate, fills up the technical blank at home and abroad, and can be widely applied to occasions involving the high-concentration salt solution (especially the high-concentration multivalent metal salt solution) in the industries of aqueous coating ink adhesives, detergents, cosmetics, pharmacy and the like.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
A preparation method of high-salt-resistance high-performance modified lithium magnesium silicate is characterized by comprising the following steps: the preparation method comprises the following steps of:
(1) firstly, 1 part of strontium chloride, 30 parts of magnesium chloride, 0.1 part of lithium chloride, 5 parts of sodium carbonate and 500 parts of pure water are added into a hydrothermal reaction kettle and fully stirred for 10 min;
(2) then adding 0.2 part of zinc chloride, 0.2 part of aluminum chloride and 20 parts of silica sol, fully and uniformly stirring, then hermetically heating to 120 ℃, and carrying out heat preservation reaction for 30 min;
(3) and then stopping reaction discharging, filtering and fully washing the reaction solution, and roasting the collected filter cake at the high temperature of 200 ℃ for 30min to obtain the modified lithium magnesium silicate No. 1.
Example 2
A modified magnesium lithium silicate with strong salt resistance and high performance and a preparation method thereof are characterized in that: the preparation method comprises the following steps of:
(1) firstly, 2.5 parts of strontium chloride, 2.5 parts of strontium nitrate, 30 parts of magnesium sulfate, 30 parts of magnesium nitrate, 0.25 part of lithium sulfate, 0.25 part of lithium nitrate, 5 parts of sodium carbonate and 500 parts of pure water are added into a hydrothermal reaction kettle and fully stirred for 30 min;
(2) then adding 0.4 part of zinc sulfate, 0.4 part of zinc nitrate, 0.4 part of aluminum sulfate, 0.4 part of aluminum nitrate and 50 parts of silica sol, fully and uniformly stirring, then raising the temperature to 150 ℃ in a closed manner, and carrying out heat preservation reaction for 60 min;
(3) and then stopping reaction discharging, filtering and fully washing the reaction solution, and roasting the collected filter cake at the high temperature of 300 ℃ for 60min to obtain the modified lithium magnesium silicate No. 2.
Example 3
A modified magnesium lithium silicate with strong salt resistance and high performance and a preparation method thereof are characterized in that: the preparation method comprises the following steps of:
(1) firstly, 1 part of strontium chloride, 1 part of strontium nitrate, 15 parts of magnesium chloride, 10 parts of magnesium sulfate, 15 parts of magnesium nitrate, 0.1 part of lithium sulfate, 0.1 part of lithium nitrate, 0.1 part of lithium hydroxide, 5 parts of sodium carbonate and 500 parts of pure water are added into a hydrothermal reaction kettle and fully stirred for 15 min;
(2) then adding 0.2 part of zinc chloride, 0.2 part of zinc sulfate, 0.1 part of zinc nitrate, 0.1 part of aluminum chloride, 0.1 part of aluminum sulfate, 0.2 part of aluminum nitrate and 30 parts of silica sol, fully and uniformly stirring, then raising the temperature to 120-150 ℃ in a closed manner, and carrying out heat preservation reaction for 40 min;
(3) and then stopping reaction discharging, filtering and fully washing the reaction solution, and roasting the collected filter cake at the high temperature of 240 ℃ for 40min to obtain the modified lithium magnesium silicate No. 3.
Example 4
A modified magnesium lithium silicate with strong salt resistance and high performance and a preparation method thereof are characterized in that: the preparation method comprises the following steps of:
(1) firstly, 2.2 parts of strontium chloride, 1.7 parts of strontium nitrate, 20 parts of magnesium chloride, 13 parts of magnesium sulfate, 18 parts of magnesium nitrate, 0.15 part of lithium chloride, 0.06 part of lithium sulfate, 0.13 part of lithium nitrate, 0.09 part of lithium hydroxide, 5 parts of sodium carbonate and 500 parts of pure water are added into a hydrothermal reaction kettle and fully stirred for 25 min;
(2) then adding 0.14 part of zinc chloride, 0.23 part of zinc sulfate, 0.21 part of zinc nitrate, 0.2 part of aluminum chloride, 0.2 part of aluminum sulfate, 0.2 part of aluminum nitrate and 40 parts of silica sol, fully and uniformly stirring, then raising the temperature to 145 ℃ in a sealed manner, and carrying out heat preservation reaction for 45 min;
(3) and then stopping reaction discharging, filtering and fully washing the reaction solution, and roasting the collected filter cake at the high temperature of 270 ℃ for 50min to obtain the modified lithium magnesium silicate No. 4.
Comparative example 1
The amount of strontium chloride was changed to 0.5 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
Strontium chloride is replaced by strontium sulfate which is insoluble in water, the other reaction parameters and process conditions are completely the same as those in example 1, and the prepared modified lithium magnesium silicate is denoted as No. 6.
Comparative example 3
The amount of strontium chloride 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 denoted as No. 7.
Comparative example 4
The amount of lithium chloride was changed to 0.03 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. 8.
Comparative example 5
The amount of lithium chloride was changed to 0.62 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. 9.
Comparative example 6
The amounts of zinc sulfate and zinc nitrate were changed to 0.05 parts, 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 aluminum sulfate and aluminum nitrate were changed to 0.05 parts, 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 0.4 part and 0.5 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. 12.
Comparative example 9
The amounts of aluminum sulfate and aluminum nitrate were changed to 0.6 part and 0.3 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. 13.
Comparative example 10
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. 14.
Comparative example 11
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. 15.
Comparative example 12
The high-temperature hydrothermal reaction temperature was changed to 155 ℃ 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 denoted as No. 16.
Comparative example 13
The high temperature hydrothermal reaction time was changed to 70min, 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. 17.
Comparative example 14
Firstly generating Zn in a reaction kettle2+-Al3+/SiO2Regeneration of Li+/Sr(OH)2-Mg(OH)2The coprecipitation was carried out, 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. 18.
The results of negative charge numbers (measured as number of charges per unit cell layer) of modified magnesium lithium silicate Nos. 1 to 18 prepared in the above examples, imported magnesium lithium silicate (model: RD, BYK, Germany) and their viscosity comparison tests in various salt solutions 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 1: X-No stable suspension, rapid demixing after standing, no measurement of the plastic viscosity.
Note 2: XXX-since there is almost no layered structure, it has no practical meaning of the number of layer charges, and the number of cell layer charges cannot be measured.
As can be seen from table 1 comparing the test data: (1) reaction parameters and process conditions must be strictly limited within the technical requirement range of the invention, otherwise, on one hand, most products (such as No. 3-No. 9 and the like) almost have no layered structure, cannot expand in water, and completely disappear in viscous property, and have no practicability; on the other hand, partial products (such as No.10 and No. 11) have a layered structure, but have poor salt resistance. (2) The modified magnesium lithium silicate prepared by the invention has low negative charge quantity (the charge number of a unit cell layer is in the range of 0.35-0.40), the affinity between the lamellar crystal and metal ions after fully stripping in water is weak, and the interference and attack of the metal ions on the formation of a card house structure on the lamellar crystal are effectively eliminated, so that the tackifying and thickening effects of the modified magnesium lithium silicate in various high-concentration salt solutions are obviously better than those of similar products imported from abroad, the excellent tackifying and thickening capabilities are maintained in a saturated sodium chloride solution, and the tackifying and thickening effects in high-concentration divalent metal salt (10% calcium chloride) and trivalent metal salt (5% aluminum sulfate) are also very ideal (basically close to the viscosity of imported RD in pure water), so that the application prospect in the industries of aqueous coating adhesive, medicine, washing, daily chemicals and the like is extremely bright.
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-salt-resistance high-performance modified lithium magnesium silicate is characterized by comprising the following steps: the preparation method comprises the following steps of:
(1) firstly, adding 1-5 parts of strontium salt, 30-60 parts of magnesium salt, 0.1-0.5 part of lithium salt, 5 parts of sodium carbonate and 500 parts of pure water into a hydrothermal reaction kettle and fully stirring for 10-30 min;
(2) then adding 0.2-0.8 part of zinc salt, 0.2-0.8 part of aluminum salt and 20-50 parts of silica sol, fully and uniformly stirring, then raising the temperature to 120-150 ℃ in a closed manner, and carrying out heat preservation reaction for 30-60 min;
(3) and stopping reaction discharging, filtering and fully washing the reaction solution, and roasting the collected filter cake at the high temperature of 200-300 ℃ for 30-60 min to obtain the modified magnesium lithium silicate.
2. The method for preparing the high-salt-resistance high-performance modified lithium magnesium silicate according to claim 1, wherein the method comprises the following steps: the strontium salt is one or two of strontium chloride and strontium nitrate which are combined randomly.
3. The method for preparing the high-salt-resistance high-performance modified lithium magnesium silicate according to 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.
4. The method for preparing the high-salt-resistance high-performance modified lithium magnesium silicate according to claim 1, wherein the method comprises the following steps: the lithium salt is one or any combination of lithium chloride, lithium sulfate, lithium nitrate and lithium hydroxide.
5. The method for preparing the high-salt-resistance high-performance modified lithium magnesium silicate according to 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-salt-resistance high-performance modified lithium magnesium silicate according to claim 1, wherein the method comprises the following steps: the aluminum salt is one or any combination of aluminum chloride, aluminum sulfate and aluminum nitrate.
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| CN108847355A (en) * | 2018-06-20 | 2018-11-20 | 江苏海明斯新材料科技有限公司 | A kind of preparation method of lithium magnesium silicate modified manganese dioxide based super capacitor electrode material |
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| FR2292027A1 (en) * | 1974-11-20 | 1976-06-18 | Ryan John | Aqueous colloidal hectorite gels - consisting of a solution of a humectant in an aqueous colloidal solution of hectorite |
| KR20180054058A (en) * | 2016-11-14 | 2018-05-24 | 주식회사 엘지화학 | Method for producing synthetic hectorite at low temperature and atmospheric pressure |
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