CN105680045B - A kind of preparation method of high stability amorphous manganous silicate - Google Patents
A kind of preparation method of high stability amorphous manganous silicate Download PDFInfo
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- CN105680045B CN105680045B CN201610237316.1A CN201610237316A CN105680045B CN 105680045 B CN105680045 B CN 105680045B CN 201610237316 A CN201610237316 A CN 201610237316A CN 105680045 B CN105680045 B CN 105680045B
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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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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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Abstract
The invention discloses a kind of preparation method of high stability amorphous manganous silicate, including using sodium metasilicate and manganese chloride as raw material, the step of amorphous silicic acid manganese powder body is prepared through boiling water treating；And mix amorphous silicic acid manganese powder body with glucose, reacted for 600 700 DEG C the step of.The preparation method of the amorphous manganous silicate of the present invention, the reaction time is short, and reaction temperature is low, and production efficiency is high, suitable for a large amount of productions.The amorphous silicic acid manganese material of preparation, its purity is high, and non crystalline structure stability is high.
Description
Technical field
The present invention relates to a kind of preparation method of high stability amorphous manganous silicate, belong to technical field of preparation for inorganic material.
Background technology
Non-crystalline material has the characteristics that longrange disorder, shortrange order and macroscopically isotropic, and it is special to show some
Physical and chemical performance, such as loose structure, the mechanical performance that specific surface area is larger, good and soft magnet performance, and optical characteristics etc.,
It is widely used to numerous areas, such as solar cell, permanent magnet film material, superconductor, sensitization functional material.
Report in the light of recent researches, non-crystalline material is due to uniform and loose structure, being advantageous to lithium ion diffusion
Migration, and the volumetric expansion in charge and discharge process can be accommodated, relaxed stress, while capacitive character energy storage can be also produced, therefore in lithium
The application of the new energy fields such as ion battery, ultracapacitor causes great concern.
Silicic acid manganese material rich reserves in nature, it is environment-friendly, and industrial applications are extensive, are such as the carrier of oxygen
Burning chemistry chains provide the oxygen of decoupled conjunction, improve the reactivity with methane；As pair in ozone catalyst degraded drinking water
Chloronitrobenzene；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, cycle length, and not only cost is high, and easily produces
Raw other impurity.Therefore such as how low cost, it is the challenge faced at present simply and efficiently largely to prepare non-crystalline material.
And it is not related to the report of high stability amorphous manganous silicate preparation also in the prior art, therefore, it is high to develop a kind of efficiently preparation
The method of stability amorphous silicic acid manganese material, the further application for silicic acid manganese material have great importance.
The content of the invention
For above-mentioned prior art, it is an object of the invention to provide a kind of preparation method of high stability amorphous manganous silicate.
The course of reaction of the preparation method is simple, efficiency high, and the amorphous silicic acid manganese material purity of preparation is high, and non crystalline structure is stable.
To achieve the above object, the present invention uses following technical proposals：
A kind of preparation method of high stability amorphous manganous silicate, including using sodium metasilicate and manganese chloride as raw material, at boiling water
The step of amorphous silicic acid manganese powder body is prepared in reason；And mix amorphous silicic acid manganese powder body with glucose, enter at 600-700 DEG C
The step of row reaction.
In above-mentioned preparation method, the mol ratio of sodium metasilicate and manganese chloride is 1:1.
In above-mentioned preparation method, the time of boiling water treating is 2-8 hours.
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 preferable scheme, the specific method that boiling water treating prepares amorphous silicic acid manganese powder body is：
Sodium metasilicate and manganese chloride are obtained into homogeneous solution with deionized water dissolving respectively；Under stirring, it is manganese chloride solution is slow
It is added in sodium silicate solution, forms mixed liquor；Mixed liquor heating is boiled, kept for 2-8 hours, washed product, drying, is produced
Amorphous silicic acid manganese powder body.
In above-mentioned preparation method, as preferable scheme, the specific side of amorphous silicic acid manganese powder body and glucose hybrid reaction
Method is：By glucose deionized water dissolving, then it is well mixed with amorphous silicic acid manganese powder body, pipe is put into after 120 DEG C of drying
In formula stove 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 the above method, non crystalline structure stability is high, under 700 DEG C of hot conditions
Crystalline phase will not be produced.
Beneficial effects of the present invention：
(1) preparation method of amorphous manganous silicate of the invention, course of reaction is simple, and accessory substance easy cleaning removes.
(2) preparation method of amorphous manganous silicate of the invention, the reaction time is short, and reaction temperature is low, and production efficiency is high, is suitable to
A large amount of productions.
(3) amorphous silicic acid manganese material prepared by the present invention, its purity is high, and non crystalline structure stability is high.
Brief description of the drawings
Fig. 1 is the x-ray diffraction pattern that amorphous manganous silicate is made in embodiment 1,8,10；
Fig. 2 is the x-ray diffraction pattern that crystalline phase complex silicate manganese is made in embodiment 2；
The x-ray diffraction pattern of amorphous manganous silicate is made in Fig. 3 embodiments 3；
The x-ray diffraction pattern of amorphous manganous silicate is made in Fig. 4 embodiments 4,9,11；
The x-ray diffraction pattern of crystallization manganous silicate is made in Fig. 5 embodiments 5；
The x-ray diffraction pattern of amorphous manganous silicate is made in Fig. 6 embodiments 12；
The x-ray diffraction pattern of crystalline phase manganous silicate is made in Fig. 7 embodiments 13.
Embodiment
The present invention is further illustrated in conjunction with the embodiments, it should which explanation, the description below is merely to explain this
Invention, is not defined to its content.
Embodiment 1：
Amorphous manganous silicate is prepared by sodium metasilicate and manganese chloride reaction.7.55g manganese chlorides and 10.85g sodium metasilicate is taken to distinguish
Dissolved in 50mL deionizations reclaimed water.Under stirring, manganese chloride solution is slowly added into sodium silicate solution, mixing is equal
It is even.Mixed liquor heating is boiled, is kept for 4 hours, is cooled to room temperature, is dried with deionized water wash products 3 times, then at 120 DEG C,
5.0g dark brown powders, yield and purity are obtained close to 100%.(as shown in Figure 1), product are analyzed according to X-ray diffracting spectrum
For amorphous manganous silicate.
Embodiment 2：
Weigh the dark brown powder 1.0g prepared in embodiment 1 and be heated to 600 DEG C of insulations 5 under nitrogen atmosphere in tube furnace
Hour, room temperature is cooled to, obtains black powder.Analyzed (as shown in Figure 2) according to X-ray diffracting spectrum, product is that crystalline phase is compound
Manganous silicate Mn2+Mn3+ 6SiO12(JCPDS 41-1367)。
Embodiment 3：
Dark brown powder 1.5g and the 1.05g glucose prepared in embodiment 1 is weighed, adds deionized water dissolving glucose simultaneously
Be uniformly mixed, through 120 DEG C drying after be put into tube furnace nitrogen atmosphere be protected in 600 DEG C reaction 5 hours after it is naturally cold
But to room temperature, black powder is obtained.Analyzed (as shown in Figure 3) according to X-ray diffracting spectrum, product is amorphous manganous silicate.
Embodiment 4：
Dark brown powder 1.5g and the 1.05g glucose prepared in embodiment 1 is weighed, adds deionized water dissolving glucose simultaneously
Be uniformly mixed, through 120 DEG C drying after be put into tube furnace nitrogen atmosphere be protected in 700 DEG C reaction 5 hours after it is naturally cold
But to room temperature, black powder is obtained.Analyzed (as shown in Figure 4) according to X-ray diffracting spectrum, product is amorphous manganous silicate.
Embodiment 5：
Dark brown powder 1.5g and the 1.05g glucose prepared in embodiment 1 is weighed, adds deionized water dissolving glucose simultaneously
Be uniformly mixed, through 120 DEG C drying after be put into tube furnace nitrogen atmosphere be protected in 800 DEG C reaction 5 hours after it is naturally cold
But to room temperature, black powder is obtained.Analyzed (as shown in Figure 5) according to X-ray diffracting spectrum, product is crystallization manganous silicate
(MnSiO3,JCPDS 29-0895)。
Embodiment 6：
Dark brown powder 1.5g and the 1.5g glucose prepared in embodiment 1 is weighed, adds deionized water dissolving glucose simultaneously
Be uniformly mixed, through 120 DEG C drying after be put into tube furnace nitrogen atmosphere be protected in 700 DEG C reaction 5 hours after it is naturally cold
But to room temperature, acquisition black powder is amorphous manganous silicate.
Embodiment 7：
Dark brown powder 1.5g and the 0.45g glucose prepared in embodiment 1 is weighed, adds deionized water dissolving glucose simultaneously
Be uniformly mixed, through 120 DEG C drying after be put into tube furnace nitrogen atmosphere be protected in 700 DEG C reaction 5 hours after it is naturally cold
But to room temperature, acquisition black powder is amorphous manganous silicate.
Embodiment 8：
Amorphous manganous silicate is prepared by sodium metasilicate and manganese chloride reaction.7.55g manganese chlorides and 10.85g sodium metasilicate is taken to distinguish
Dissolved in 50mL deionizations reclaimed water.Under stirring, manganese chloride solution is slowly added into sodium silicate solution, mixing is equal
It is even.Mixed liquor heating is boiled, is kept for 2 hours, is cooled to room temperature, is dried with deionized water wash products 3 times, then at 120 DEG C,
5.0g dark brown powders are obtained, are analyzed (as shown in Figure 1) according to X-ray diffracting spectrum, product is amorphous manganous silicate.
Embodiment 9：
Dark brown powder 1.5g and the 1.05g glucose prepared in embodiment 8 is weighed, adds deionized water dissolving glucose simultaneously
Be uniformly mixed, through 120 DEG C drying after be put into tube furnace nitrogen atmosphere be protected in 700 DEG C reaction 5 hours after it is naturally cold
But to room temperature, black powder is obtained.Analyzed (as shown in Figure 4) according to X-ray diffracting spectrum, product is amorphous manganous silicate.
Embodiment 10：
Amorphous manganous silicate is prepared by sodium metasilicate and manganese chloride reaction.7.55g manganese chlorides and 10.85g sodium metasilicate is taken to distinguish
Dissolved in 50mL deionizations reclaimed water.Under stirring, manganese chloride solution is slowly added into sodium silicate solution, mixing is equal
It is even.Mixed liquor heating is boiled, is kept for 8 hours, is cooled to room temperature, is dried with deionized water wash products 3 times, then at 120 DEG C,
5.0g dark brown powders are obtained, are analyzed (as shown in Figure 1) according to X-ray diffracting spectrum, product is amorphous manganous silicate.
Embodiment 11：
Dark brown powder 1.5g and the 1.05g glucose prepared in embodiment 10 is weighed, adds deionized water dissolving glucose
And be uniformly mixed, it is put into after 120 DEG C of drying in tube furnace natural after nitrogen atmosphere is protected in 700 DEG C of reactions 5 hours
Room temperature is cooled to, obtains black powder.Analyzed (as shown in Figure 4) according to X-ray diffracting spectrum, product is amorphous manganous silicate.
Embodiment 12：
Amorphous manganous silicate is prepared by sodium metasilicate and manganese chloride reaction.7.55g manganese chlorides and 10.85g sodium metasilicate is taken to distinguish
Dissolved in 50mL deionizations reclaimed water.Under stirring, manganese chloride solution is slowly added into sodium silicate solution, mixing is equal
It is even, handled without boiling, with deionized water wash products 3 times, then in 120 DEG C of drying, obtain 5.0g dark brown powders, yield
With purity close to 100%.Analyzed (as shown in Figure 6) according to X-ray diffracting spectrum, product is amorphous manganous silicate.
Embodiment 13：
Dark brown powder 1.5g and the 1.05g glucose prepared in embodiment 12 is weighed, adds deionized water dissolving glucose
And be uniformly mixed, it is put into after 120 DEG C of drying in tube furnace natural after nitrogen atmosphere is protected in 600 DEG C of reactions 5 hours
Room temperature is cooled to, obtains black powder.Analyzed (as shown in Figure 7) according to X-ray diffracting spectrum, product is crystalline phase Mn2SiO4
(JCPDS35–0748)。
As can be seen from the above-described embodiment, using sodium metasilicate and manganese chloride as raw material, after boiling water treating, obtained depth is dried
Although brown powder is amorphous manganous silicate, its structure is still unstable.Even if there is nitrogen as protective atmosphere, by the dark-brown
Powder, which is heated to 600 DEG C, will be changed into crystalline phase, as shown in embodiment 2 and Fig. 2.
The obtained dark-brown powder after boiling water treating, after only further uniformly being mixed with glucose solution, is being heated
During can just keep its non crystalline structure until 700 DEG C of high temperature, such as embodiment 3, embodiment 4, embodiment 9, embodiment 11 and figure
3rd, shown in Fig. 4.
Using sodium metasilicate and manganese chloride as raw material, if without boiling water treating, even if obtained dark-brown powder enters one
After step uniformly mixes with glucose solution, 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 need to mix sodium metasilicate and manganese chloride
Close liquid and carry out boiling water treating；Product after boiling water treating is also needed to after being well mixed with glucose solution, amorphous silicic acid manganese material
Stability can just bring up to more than 700 DEG C without produce crystalline phase.Therefore, the step of boiling water treating and mixed with glucose solution
The step of be the critical process step for preparing high stability amorphous silicic acid manganese material, Neither of the two can be dispensed.
Although above-mentioned the embodiment of the present invention is described with reference to accompanying drawing, model not is protected to the present invention
The limitation enclosed, one of ordinary skill in the art should be understood that on the basis of technical scheme those skilled in the art are not
Need to pay various modifications or deformation that creative work can make still within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of amorphous manganous silicate, it is characterised in that including using sodium metasilicate and manganese chloride as raw material, by manganese chloride
It is dissolved in deionization reclaimed water respectively with sodium metasilicate, under stirring, manganese chloride and sodium silicate solution is well mixed, by mixed liquor
The step of heating boils to obtain amorphous silicic acid manganese powder body；And mix amorphous silicic acid manganese powder body with glucose, at 600-700 DEG C
The step of being reacted；
The specific method that the boiling water treating prepares amorphous silicic acid manganese powder body is：Sodium metasilicate and manganese chloride are used into deionized water respectively
Dissolving obtains homogeneous solution；Under stirring, manganese chloride solution is slowly added into sodium silicate solution, forms mixed liquor；
Mixed liquor heating is boiled, kept for 2-8 hours, washed product, drying, produces amorphous silicic acid manganese powder body.
2. preparation method as claimed in claim 1, it is characterised in that the mol ratio of sodium metasilicate 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 hours.
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 amorphous silicic acid manganese powder body and the tool of glucose hybrid reaction
Body method is：By glucose deionized water dissolving, then it is well mixed with amorphous silicic acid manganese powder body, is put after 120 DEG C of drying
Enter in tube furnace nitrogen atmosphere be protected in 600~700 DEG C reaction 5 hours after, naturally cool to room temperature.
6. the amorphous manganous silicate that the preparation method described in any one of claim 1 to 5 is prepared.
7. use of the amorphous manganous silicate in as the carrier of oxygen, catalyst or lithium ion battery negative material described in claim 6
On the way.
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| CN107758676B (en) * | 2017-11-16 | 2020-01-10 | 北京化工大学 | Method for preparing double-layer hollow nano manganese silicate based on bell-shaped structure template |
| CN109824056B (en) * | 2019-04-04 | 2022-04-19 | 河北工业大学 | Method for preparing nano flaky manganese silicate composite selective adsorbent by using iron tailings |
| 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 |
| 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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| CN1839099A (en) * | 2003-05-15 | 2006-09-27 | 卡奴母鲁·拉乌·拉居 | Functional transition metal silicates (FTMS) |
| CN102659126A (en) * | 2012-05-18 | 2012-09-12 | 哈尔滨工业大学 | Preparation method and application of iron-manganese composite silicate |
| CN103263931A (en) * | 2013-06-07 | 2013-08-28 | 哈尔滨工业大学 | Preparation method and application of modified cobalt-manganese compound silicate |
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|---|---|---|---|---|
| US3962523A (en) * | 1970-07-09 | 1976-06-08 | Blythe Colours (Australia) Proprietary Limited | Vitreous coating composition |
| CN1839099A (en) * | 2003-05-15 | 2006-09-27 | 卡奴母鲁·拉乌·拉居 | Functional transition metal silicates (FTMS) |
| CN102659126A (en) * | 2012-05-18 | 2012-09-12 | 哈尔滨工业大学 | Preparation method and application of iron-manganese composite silicate |
| CN103263931A (en) * | 2013-06-07 | 2013-08-28 | 哈尔滨工业大学 | Preparation method and application of modified cobalt-manganese compound silicate |
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