CN105680045A - Preparation method of high-stability amorphous manganous silicate - Google Patents
Preparation method of high-stability amorphous manganous silicate Download PDFInfo
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- CN105680045A CN105680045A CN201610237316.1A CN201610237316A CN105680045A CN 105680045 A CN105680045 A CN 105680045A CN 201610237316 A CN201610237316 A CN 201610237316A CN 105680045 A CN105680045 A CN 105680045A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a preparation method of high-stability amorphous manganous silicate. The method comprises the steps that sodium silicate and manganese chloride are used as raw materials, and amorphous manganous silicate powder is obtained through boiling water processing; the amorphous manganous silicate powder and glucose are mixed to be subjected to a reaction under the temperature of 600-700 DEG C. According to the preparation method of the amorphous manganous silicate, the reaction time is short, the reaction temperature is low, the production efficiency is high, and the method is suitable for mass production. The obtained amorphous manganous silicate is high in purity and amorphous structural stability.
Description
Technical field
The preparation method that the present invention relates to a kind of high stability amorphous manganous silicate, belongs to technical field of preparation for inorganic material.
Background technology
Non-crystalline material has the features such as longrange disorder, shortrange order and macroscopically isotropic, show some special physical and chemical performances, mechanical performance as bigger, good in loose structure, specific surface area and soft magnet performance, and optical characteristics etc., it is widely used to numerous areas, such as solaode, permanent magnet film material, superconductor, sensitization functional material etc.
Report in the light of recent researches, non-crystalline material is owing to having uniformly loose structure, be conducive to lithium ion diffusive migration, and the volumetric expansion in charge and discharge process can be held, relaxed stress, also can produce capacitive character energy storage simultaneously, therefore cause great concern in the application of the new energy field such as lithium ion battery, ultracapacitor.
Manganous silicate material rich reserves in nature, environmental friendliness, and industrial applications are extensive, as provided the oxygen of decoupled conjunction for burning chemistry chains as the carrier of oxygen, improve the reactivity with methane; As the parachloronitrobenzene in ozone catalyst degraded drinking water; Catalyst as general-purpose platform synthesis nano; As lithium ion battery negative material etc.
But the preparation process of non-crystalline material is complicated at present, synthesis difficulty is big, the cycle is long, and not only cost is high, and is easily generated other impurity. Therefore such as how low cost, simply and efficiently preparing non-crystalline material in a large number is the challenge faced at present. And prior art is not also related to report prepared by high stability amorphous manganous silicate, therefore, a kind of method developing efficient preparation high stability amorphous silicic acid manganese material, the application further for manganous silicate material has great importance.
Summary of the invention
For above-mentioned prior art, the preparation method that it is an object of the invention to provide a kind of high stability amorphous manganous silicate. The course of reaction of this preparation method is simple, and efficiency is high, and the amorphous silicic acid manganese material purity of preparation is high, and non crystalline structure is stable.
For achieving the above object, the present invention adopts following technical proposals:
The preparation method of a kind of high stability amorphous manganous silicate, including with sodium silicate and manganese chloride for raw material, prepares the step of amorphous silicic acid manganese powder body through boiling water treating; And amorphous silicic acid manganese powder body is mixed with glucose, the 600-700 DEG C of step reacted.
In above-mentioned preparation method, the mol ratio of sodium silicate and manganese chloride is 1:1.
In above-mentioned preparation method, the time of boiling water treating is 2-8 hour.
In above-mentioned preparation method, the mass ratio of amorphous silicic acid manganese powder body and glucose is 1:0.3-1.
In above-mentioned preparation method, as preferred scheme, boiling water treating prepares amorphous silicic acid manganese powder body method particularly includes: with deionized water dissolving, sodium silicate and manganese chloride are obtained homogeneous solution respectively; Under stirring, manganese chloride solution is slowly added in sodium silicate solution, forms mixed liquor; By mixed liquor heated and boiled, keep 2-8 hour, washed product, dry, obtain amorphous silicic acid manganese powder body.
In above-mentioned preparation method; as preferred scheme; amorphous silicic acid manganese powder body and glucose hybrid reaction method particularly includes: by glucose deionized water dissolving; then mix homogeneously with amorphous silicic acid manganese powder body; through 120 DEG C dry after put in tube furnace nitrogen atmosphere be protected in 600～700 DEG C reaction 5 hours after, naturally cool to room temperature.
Amorphous silicic acid manganese material prepared by said method, non crystalline structure stability is high, even if without producing crystalline phase under 700 DEG C of hot conditionss.
Beneficial effects of the present invention:
(1) preparation method of the amorphous manganous silicate of the present invention, course of reaction is simple, and by-product easy cleaning is removed.
(2) preparation method of the amorphous manganous silicate of the present invention, the response time is short, and reaction temperature is low, and production efficiency is high, is suitable to a large amount of production.
(3) the amorphous silicic acid manganese material that prepared by the present invention, its purity is high, and non crystalline structure stability is high.
Accompanying drawing explanation
Fig. 1 is the x-ray diffraction pattern that embodiment 1,8,10 prepares amorphous manganous silicate;
Fig. 2 is the x-ray diffraction pattern that embodiment 2 prepares crystalline phase complex silicate manganese;
Fig. 3 embodiment 3 prepares the x-ray diffraction pattern of amorphous manganous silicate;
Fig. 4 embodiment 4,9,11 prepares the x-ray diffraction pattern of amorphous manganous silicate;
Fig. 5 embodiment 5 prepares the x-ray diffraction pattern of crystallization manganous silicate;
Fig. 6 embodiment 12 prepares the x-ray diffraction pattern of amorphous manganous silicate;
Fig. 7 embodiment 13 prepares the x-ray diffraction pattern of crystalline phase manganous silicate.
Detailed description of the invention
The present invention is further illustrated in conjunction with the embodiments, it should explanation, and its content, merely to explain the present invention, is not defined by the description below.
Embodiment 1:
Amorphous manganous silicate is prepared by sodium silicate and manganese chloride reaction. Take 7.55g manganese chloride and 10.85g sodium silicate water dissolution in 50mL deionization respectively. Under stirring, manganese chloride solution is slowly added in sodium silicate solution, mix homogeneously. By mixed liquor heated and boiled, keep 4 hours, be cooled to room temperature, by deionized water wash products 3 times, then 120 DEG C of drying, it is thus achieved that 5.0g dark brown powder, productivity and purity are close to 100%. According to X-ray diffracting spectrum analysis (as shown in Figure 1), product is amorphous manganous silicate.
Embodiment 2:
Weigh the dark brown powder 1.0g of preparation in embodiment 1 in tube furnace, under nitrogen atmosphere, be heated to 600 DEG C of insulations 5 hours, be cooled to room temperature, it is thus achieved that black powder. According to X-ray diffracting spectrum analysis (as shown in Figure 2), product is crystalline phase complex silicate manganese Mn2+Mn3+ 6SiO12(JCPDS41-1367)。
Embodiment 3:
Weigh dark brown powder 1.5g and the 1.05g glucose of preparation in embodiment 1; add deionized water dissolving glucose and be uniformly mixed; put into after 120 DEG C dry in tube furnace and naturally cool to room temperature after nitrogen atmosphere is protected in 600 DEG C of reactions 5 hours, it is thus achieved that black powder. According to X-ray diffracting spectrum analysis (as shown in Figure 3), product is amorphous manganous silicate.
Embodiment 4:
Weigh dark brown powder 1.5g and the 1.05g glucose of preparation in embodiment 1; add deionized water dissolving glucose and be uniformly mixed; put into after 120 DEG C dry in tube furnace and naturally cool to room temperature after nitrogen atmosphere is protected in 700 DEG C of reactions 5 hours, it is thus achieved that black powder. According to X-ray diffracting spectrum analysis (as shown in Figure 4), product is amorphous manganous silicate.
Embodiment 5:
Weigh dark brown powder 1.5g and the 1.05g glucose of preparation in embodiment 1; add deionized water dissolving glucose and be uniformly mixed; put into after 120 DEG C dry in tube furnace and naturally cool to room temperature after nitrogen atmosphere is protected in 800 DEG C of reactions 5 hours, it is thus achieved that black powder. According to X-ray diffracting spectrum analysis (as shown in Figure 5), product is crystallization manganous silicate (MnSiO3,JCPDS29-0895)。
Embodiment 6:
Weigh dark brown powder 1.5g and the 1.5g glucose of preparation in embodiment 1; add deionized water dissolving glucose and be uniformly mixed; put into after 120 DEG C dry in tube furnace and naturally cool to room temperature after nitrogen atmosphere is protected in 700 DEG C of reactions 5 hours, it is thus achieved that black powder is amorphous manganous silicate.
Embodiment 7:
Weigh dark brown powder 1.5g and the 0.45g glucose of preparation in embodiment 1; add deionized water dissolving glucose and be uniformly mixed; put into after 120 DEG C dry in tube furnace and naturally cool to room temperature after nitrogen atmosphere is protected in 700 DEG C of reactions 5 hours, it is thus achieved that black powder is amorphous manganous silicate.
Embodiment 8:
Amorphous manganous silicate is prepared by sodium silicate and manganese chloride reaction. Take 7.55g manganese chloride and 10.85g sodium silicate water dissolution in 50mL deionization respectively. Under stirring, manganese chloride solution is slowly added in sodium silicate solution, mix homogeneously. By mixed liquor heated and boiled, keep 2 hours, be cooled to room temperature, by deionized water wash products 3 times, then 120 DEG C of drying, it is thus achieved that 5.0g dark brown powder, according to X-ray diffracting spectrum analysis (as shown in Figure 1), product is amorphous manganous silicate.
Embodiment 9:
Weigh dark brown powder 1.5g and the 1.05g glucose of preparation in embodiment 8; add deionized water dissolving glucose and be uniformly mixed; put into after 120 DEG C dry in tube furnace and naturally cool to room temperature after nitrogen atmosphere is protected in 700 DEG C of reactions 5 hours, it is thus achieved that black powder. According to X-ray diffracting spectrum analysis (as shown in Figure 4), product is amorphous manganous silicate.
Embodiment 10:
Amorphous manganous silicate is prepared by sodium silicate and manganese chloride reaction. Take 7.55g manganese chloride and 10.85g sodium silicate water dissolution in 50mL deionization respectively. Under stirring, manganese chloride solution is slowly added in sodium silicate solution, mix homogeneously. By mixed liquor heated and boiled, keep 8 hours, be cooled to room temperature, by deionized water wash products 3 times, then 120 DEG C of drying, it is thus achieved that 5.0g dark brown powder, according to X-ray diffracting spectrum analysis (as shown in Figure 1), product is amorphous manganous silicate.
Embodiment 11:
Weigh dark brown powder 1.5g and the 1.05g glucose of preparation in embodiment 10; add deionized water dissolving glucose and be uniformly mixed; put into after 120 DEG C dry in tube furnace and naturally cool to room temperature after nitrogen atmosphere is protected in 700 DEG C of reactions 5 hours, it is thus achieved that black powder. According to X-ray diffracting spectrum analysis (as shown in Figure 4), product is amorphous manganous silicate.
Embodiment 12:
Amorphous manganous silicate is prepared by sodium silicate and manganese chloride reaction. Take 7.55g manganese chloride and 10.85g sodium silicate water dissolution in 50mL deionization respectively.Under stirring, manganese chloride solution is slowly added in sodium silicate solution, mix homogeneously, do not carry out decocting in water process, by deionized water wash products 3 times, then 120 DEG C of drying, it is thus achieved that 5.0g dark brown powder, productivity and purity are close to 100%. According to X-ray diffracting spectrum analysis (as shown in Figure 6), product is amorphous manganous silicate.
Embodiment 13:
Weigh dark brown powder 1.5g and the 1.05g glucose of preparation in embodiment 12; add deionized water dissolving glucose and be uniformly mixed; put into after 120 DEG C dry in tube furnace and naturally cool to room temperature after nitrogen atmosphere is protected in 600 DEG C of reactions 5 hours, it is thus achieved that black powder. According to X-ray diffracting spectrum analysis (as shown in Figure 7), product is crystalline phase Mn2SiO4(JCPDS35–0748)。
As can be seen from the above-described embodiment, with sodium silicate and manganese chloride for raw material, after boiling water treating, although drying the dark-brown powder body obtained is amorphous manganous silicate, but its structure is still unstable. Even if having nitrogen as protective atmosphere, this dark-brown powder body being heated to 600 DEG C and will be changed into crystalline phase, as shown in embodiment 2 and Fig. 2.
The dark-brown powder body prepared after boiling water treating, only further with glucose solution Homogeneous phase mixing after, in heating process, just can keep its non crystalline structure until 700 DEG C of high temperature, as shown in embodiment 3, embodiment 4, embodiment 9, embodiment 11 and Fig. 3, Fig. 4.
With sodium silicate and manganese chloride for raw material, if not carrying out boiling water treating, though the dark-brown powder body then prepared further with glucose solution Homogeneous phase mixing after, also converted into crystalline phase in heating process, as shown in embodiment 13 and Fig. 7.
As can be seen here, to obtain the amorphous silicic acid manganese material of high stability, both needed the mixed liquor of sodium silicate and manganese chloride is carried out boiling water treating; After product after boiling water treating also needs to mix homogeneously with glucose solution, the stability of amorphous silicic acid manganese material just can bring up to more than 700 DEG C and not produce crystalline phase. Therefore, step and the step mixed with glucose solution of boiling water treating are to prepare the critical process step of high stability amorphous silicic acid manganese material, and Neither of the two can be dispensed.
The specific embodiment of the present invention is described in conjunction with accompanying drawing although above-mentioned; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme, those skilled in the art need not pay various amendments or deformation that creative work can make still within protection scope of the present invention.
Claims (8)
1. the preparation method of a high stability amorphous manganous silicate, it is characterised in that include, with sodium silicate and manganese chloride for raw material, preparing the step of amorphous silicic acid manganese powder body through boiling water treating; And amorphous silicic acid manganese powder body is mixed with glucose, the 600-700 DEG C of step reacted.
2. preparation method as claimed in claim 1, it is characterised in that the mol ratio of sodium silicate and manganese chloride is 1:1.
3. preparation method as claimed in claim 1, it is characterised in that the time of boiling water treating is 2-8 hour.
4. preparation method as claimed in claim 1, it is characterised in that the mass ratio of amorphous silicic acid manganese powder body and glucose is 1:0.3-1.
5. preparation method as claimed in claim 1, it is characterised in that boiling water treating prepares amorphous silicic acid manganese powder body method particularly includes: with deionized water dissolving, sodium silicate and manganese chloride are obtained homogeneous solution respectively; Under stirring, manganese chloride solution is slowly added in sodium silicate solution, forms mixed liquor; By mixed liquor heated and boiled, keep 2-8 hour, washed product, dry, obtain amorphous silicic acid manganese powder body.
6. preparation method as claimed in claim 1; it is characterized in that; amorphous silicic acid manganese powder body and glucose hybrid reaction method particularly includes: by glucose deionized water dissolving; then mix homogeneously with amorphous silicic acid manganese powder body; through 120 DEG C dry after put in tube furnace nitrogen atmosphere be protected in 600～700 DEG C reaction 5 hours after, naturally cool to room temperature.
7. the amorphous manganous silicate that the preparation method described in any one of claim 1 to 6 prepares.
8. the amorphous manganous silicate described in claim 7 is as the purposes in the carrier of oxygen, catalyst or lithium ion battery negative material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107758676A (en) * | 2017-11-16 | 2018-03-06 | 北京化工大学 | A kind of method that double layer hollow nanometer manganous silicate is prepared based on shape stay in place form of ringing a bell |
| CN109824056A (en) * | 2019-04-04 | 2019-05-31 | 河北工业大学 | The method for preparing the compound selective absorbent of nano-sheet manganous silicate using iron tailings |
| CN110482560A (en) * | 2019-08-25 | 2019-11-22 | 山东理工大学 | A kind of preparation method of two dimension manganous silicate nanometer sheet |
| CN110510621A (en) * | 2019-08-25 | 2019-11-29 | 山东理工大学 | A kind of preparation method of high stability amorphous silicic acid cerium |
| CN116889857A (en) * | 2023-07-11 | 2023-10-17 | 四川农业大学 | Film gradient diffusion method for in-situ selective monitoring lead effective state |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107758676A (en) * | 2017-11-16 | 2018-03-06 | 北京化工大学 | A kind of method that double layer hollow nanometer manganous silicate is prepared based on shape stay in place form of ringing a bell |
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| CN109824056A (en) * | 2019-04-04 | 2019-05-31 | 河北工业大学 | The method for preparing the compound selective absorbent of nano-sheet manganous silicate using iron tailings |
| CN110482560A (en) * | 2019-08-25 | 2019-11-22 | 山东理工大学 | A kind of preparation method of two dimension manganous silicate nanometer sheet |
| CN110510621A (en) * | 2019-08-25 | 2019-11-29 | 山东理工大学 | A kind of preparation method of high stability amorphous silicic acid cerium |
| CN110510621B (en) * | 2019-08-25 | 2022-11-08 | 山东理工大学 | Preparation method of high-stability amorphous cerium silicate |
| CN110482560B (en) * | 2019-08-25 | 2022-11-08 | 山东理工大学 | Preparation method of two-dimensional manganese silicate nanosheet |
| CN116889857A (en) * | 2023-07-11 | 2023-10-17 | 四川农业大学 | Film gradient diffusion method for in-situ selective monitoring lead effective state |
| CN116889857B (en) * | 2023-07-11 | 2024-04-02 | 四川农业大学 | Film gradient diffusion method for in-situ selective monitoring lead effective state |
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