CN104743562A - Preparation method of sericite nanosheets - Google Patents
Preparation method of sericite nanosheets Download PDFInfo
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- CN104743562A CN104743562A CN201510123384.0A CN201510123384A CN104743562A CN 104743562 A CN104743562 A CN 104743562A CN 201510123384 A CN201510123384 A CN 201510123384A CN 104743562 A CN104743562 A CN 104743562A
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Abstract
The invention relates to a preparation method of sericite nanosheets. The preparation method comprises the steps of carrying out hydrothermal reaction in a reaction kettle by taking inorganic salt as an intercalator, and carrying out ultrasonic treatment, so as to finally obtain sericite nanosheets with thin sheet layers, complete crystal structures and high quality. According to the preparation method, sericite is stripped by virtue of a lithium ion intercalation method; compared with an existing mechanical stripping manner, the operation is simple the yield is high, the crystal forms of the stripped sericite nanosheets are relatively good; and the preparation method is applicable to industrial production.
Description
Technical field
The invention belongs to chemical technology field, relate to a kind of preparation method of sericite nano micro-flake.
Background technology
Sericite is under the jurisdiction of monoclinic crystal, its crystal is flakey, there is tiffany smooth (white mica is vitreous luster), pure piece of gray, purple rugose rose look, white etc., radius-thickness ratio >80, proportion 2.6-2.7, mole hardness is 2-3, full of elasticity, flexible, resistance to abrasion and wear resistance good; High temperature insulation, is insoluble in acid-base solution, stable chemical nature.The chemical constitution of sericite, structure, structure are close with kaolin, and have again some characteristic of clay mineral, namely in water medium and organic solvent, dispersion suspension is good, and look white grain is thin, toughness etc.Therefore, sericite has the various features of mica mineral and clay minerals concurrently.Sericite Young's modulus is 1505-2134 MPa, thermal stability 500-600 DEG C, thermal conductivity 0.419-0.670 W. (m.K)
-1, electrical insulating property 200kv/mm, radioresistance 5 × 10
14thermal neutron/cm
2to illumination.Sericite structural sheet does unordered accumulation usually, so be difficult to be linked to be large stretch of existence on plane of structure, therefore, sericite is lamellar structure crystalline structure, and { 001} face cleavage is extremely complete, can peel off into very thin sheet along cleavage surface.The nano flake of sericite can improve resistance to abrasion and wear resistance, shielding ultraviolet rays and the microwave absorbing function of sericite better, enables sericite better be applied in rubber, papermaking and paint field.In addition, the chorion of sericite, absorptivity and tack can also be improved, be better applied in the fields such as makeup.
At present, prior art (1) Baudet G, Perrotel V, Seron A.Two dimensions comminution of kaolinite clay particles.Powder Techn01.1999,105:125-134; (2) Sanchez.Soto P J, Jimenez de Haro M c.Effects ofdry grinding on the structural changes ofkaolinite powders.J.Am.Ceram.Soc.2000,83 (7): 1649-1657; (3) Suraj G, Iyer CSP, Pugmini S.The effect ofmicronization Oll kaolinites and their sorption behabiour.Appl.Clay Sci.1997,12:111-130, in the preparation method that above-mentioned document provides, the tradition of the silicate minerals of stratiform is peeled off, most employing be mechanically peel and grinding: as wet method and dry grinding, this shortcoming depending merely on the method for mechanical mill is the crystalline structure of destruction silicate minerals that can be excessive, causes the performance of product not good.
Summary of the invention
The present invention is directed to the sericite that exists in prior art peel off exist yield poorly, quality is not good, be difficult to the technical problems such as industrialization, a kind of preparation method of sericite nano micro-flake is provided, the sericite powder of wet-layer preparation is acted on by lithium ion intercalation and supersound process, obtain lamella thin, crystalline structure is complete, the sericite nano micro-flake that quality is high.
The preparation method of sericite nano micro-flake of the present invention, comprises the following steps:
1) lithium chloride to be added to the water and after fully dissolving, add sericite by sericite and lithium chloride mass ratio 1:3 ~ 20, ultrasonic mixing 15 min ~ 1 h, then seals, be warming up to 80 ~ 150 DEG C, and continuously stirring reacts 4 ~ 24 h;
2) after reaction terminates, the reaction solution that step 1) is obtained, ultrasonic disperse 0.5 ~ 2 h, washing, dry, obtain sericite nano micro-flake.
In step 1), described lithium chloride and the mass ratio of water are: 1:10 ~ 100;
In step 1), described sericite is wet method sericite in powder, and granularity is 325 ~ 1000 orders;
Step 2) in, described washing, method is for be added to the water reaction solution, and reaction solution and water volume ratio are 1:4, stir 20 min, washes 3 ~ 5 times;
Step 2) in, described drying, condition is 50 ~ 80 DEG C of vacuum-drying 3 ~ 5 h.
Step 1) and step 2) in ultrasonic power be 200 W.
At present, sericite is in the application in the fields such as coating, papermaking, rubber, plastics, and mainly by using after simple mineral primary election and mechanical workout and grinding, these application can not fully play the physical and chemical performance of the excellence of sericite.Preparation method of the present invention adopts inorganic salt as intercalator, carries out hydro-thermal reaction in a kettle., then carries out supersound process, and finally obtain lamella thin, crystalline structure is complete, the sericite nano micro-flake that quality is high.
The preparation method of sericite nano micro-flake of the present invention, compared with prior art its beneficial effect is: by the method for lithium ion intercalation, sericite is peeled off, compared with existing mechanically peel, simple to operate, output is high, and the crystal formation peeling off the sericite nano micro-flake obtained is better, is suitable for suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram sheet of the sericite nano micro-flake of embodiment 1;
Fig. 2 is the sericite nano micro-flake scanning electron microscope diagram sheet of comparative example;
Fig. 3 is the X-ray diffraction spectrogram of wet method sericite in powder raw material;
Fig. 4 is the X-ray diffraction spectrogram of embodiment 1 sericite nano micro-flake.
Embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail, and without departing from the idea case in the present invention described above, the various replacement made according to ordinary skill knowledge and customary means or change, include within the scope of the invention.
Embodiment of the present invention sericite used is wet method sericite in powder, and the model of sericite in powder is (HY-TM6), and granularity is 325 ~ 1000 orders.
Embodiment 1
1) 500 ml water and 50 g lithium chloride powder are added in beaker successively, be stirred to lithium chloride fully to dissolve, add 5 g wet method sericites in powder, ultrasonic mixing 15 min, then mixing solutions is proceeded in 1 L reactor, sealing, adopts blowing-type thermostatic drying chamber to be heated to 150 DEG C, reacts 24 h;
2), after having reacted, reaction solution step 1) obtained takes out, and 200 W ultrasonic disperse 2 h, reaction solution joins deionized water for stirring 20 min of 2L, repeated washing 4 times, and 80 DEG C of vacuum-drying 3 h, obtain the present embodiment sericite nano micro-flake.
The present embodiment sericite nano micro-flake is carried out analysis to measure, record microplate thickness and be reduced to about 10 ~ 65 nm(as shown in Figure 1 by tens microns).
Embodiment 2
1) 500 ml water and 25 g lithium chloride powder are added in beaker successively, be stirred to lithium chloride fully to dissolve, add 5 g wet method sericites in powder, ultrasonic mixing 15 min, then mixing solutions is proceeded in 1 L reactor, sealing, adopts blowing-type thermostatic drying chamber to be heated to 150 DEG C, reacts 24 h;
Step 2) with embodiment 1.
The present embodiment sericite nano micro-flake is carried out analysis to measure, recording microplate thickness is about 82 ~ 175 nm.
Embodiment 3
Similar to Example 1, be 80 DEG C unlike the Heating temperature in step 1), the present embodiment sericite nano micro-flake is carried out analysis and measure, recording microplate thickness is about 150 ~ 280 nm.
Embodiment 4
Similar to Example 1, be 120 DEG C unlike the Heating temperature in step 1), the present embodiment sericite nano micro-flake is carried out analysis and measure, recording microplate thickness is about 100 ~ 230 nm.
Embodiment 5
Similar to Example 1, unlike step 2) in ultrasonic time be 0.5h, the present embodiment sericite nano micro-flake is carried out analysis and measure, recording microplate thickness is about 70 ~ 200 nm.
Embodiment 6
Similar to Example 1, the quality unlike the wet method sericite added in step 1) is 20g, and the present embodiment sericite nano micro-flake is carried out analysis and measure, recording microplate thickness is about 220 ~ 355 nm.
Embodiment 7
Similar to Example 1, be 4 h unlike the reaction times in step 1), the present embodiment sericite nano micro-flake is carried out analysis and measure, recording microplate thickness is about 300 ~ 650 nm.
Embodiment 8
Similar to Example 1, be 15 h unlike the reaction times in step 1), the present embodiment sericite nano micro-flake is carried out analysis and measure, recording microplate thickness is about 135 ~ 350 nm.
Comparative example
1) get 5 g sericites in powder and 50 g lithium chloride powder put into mortar, grind;
2), after grinding fully, the mixture in step 1) is put in ball grinder, at rotating speed be 300 r/min ball mill in ball milling 6h.
The sericite obtained is carried out analysis to measure, record thickness and be about hundreds of nanometer to (as shown in Figure 2) between several microns.
Claims (7)
1. a preparation method for sericite nano micro-flake, is characterized in that, comprises the following steps:
1) lithium chloride to be added to the water and after fully dissolving, add sericite by sericite and lithium chloride mass ratio 1:3 ~ 20, ultrasonic mixing 15min ~ 1h, then seals, and is warming up to 80 ~ 150 DEG C, and continuously stirring reacts 4 ~ 24 h;
2) after reaction terminates, the reaction solution that step 1) is obtained, ultrasonic disperse 0.5 ~ 2h, washing, dry, obtain sericite nano micro-flake.
2. preparation method according to claim 1, is characterized in that: in step 1), and described lithium chloride and the mass ratio of water are: 1:10 ~ 100.
3. preparation method according to claim 1, is characterized in that: in step 1), and described sericite is wet method sericite in powder.
4. the preparation method according to claim 1 or 3, is characterized in that: described sericite in powder granularity is 325 ~ 1000 orders.
5. preparation method according to claim 1, is characterized in that: step 2) in, described washing, method is for be added to the water reaction solution, and reaction solution and water volume ratio are 1:4, stir 20 min, washes 3 ~ 5 times.
6. preparation method according to claim 1, is characterized in that: step 2) in, described drying, condition is 50 ~ 80 DEG C of vacuum-drying 3 ~ 5 h.
7. preparation method according to claim 1, is characterized in that: step 1) and step 2) in ultrasonic power be 200 W.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105623315A (en) * | 2016-02-02 | 2016-06-01 | 安徽恒昊科技有限公司 | Preparation method of powder for new materials |
| CN105733312A (en) * | 2016-02-02 | 2016-07-06 | 安徽恒昊科技有限公司 | Preparation method of sericite nano micro-sheets |
| CN105731472A (en) * | 2016-02-02 | 2016-07-06 | 安徽恒昊科技有限公司 | Method for preparing natural mica powder |
| CN105733313A (en) * | 2016-02-02 | 2016-07-06 | 安徽恒昊科技有限公司 | Cosmetic sericite having easy dispersibility |
| CN105731473A (en) * | 2016-02-02 | 2016-07-06 | 安徽恒昊科技有限公司 | Preparation method of matte sericite powder |
| CN113583441A (en) * | 2021-09-07 | 2021-11-02 | 平江县盛盈云母工业有限公司 | Insulating material with mica as base material and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105623315A (en) * | 2016-02-02 | 2016-06-01 | 安徽恒昊科技有限公司 | Preparation method of powder for new materials |
| CN105733312A (en) * | 2016-02-02 | 2016-07-06 | 安徽恒昊科技有限公司 | Preparation method of sericite nano micro-sheets |
| CN105731472A (en) * | 2016-02-02 | 2016-07-06 | 安徽恒昊科技有限公司 | Method for preparing natural mica powder |
| CN105733313A (en) * | 2016-02-02 | 2016-07-06 | 安徽恒昊科技有限公司 | Cosmetic sericite having easy dispersibility |
| CN105731473A (en) * | 2016-02-02 | 2016-07-06 | 安徽恒昊科技有限公司 | Preparation method of matte sericite powder |
| CN113583441A (en) * | 2021-09-07 | 2021-11-02 | 平江县盛盈云母工业有限公司 | Insulating material with mica as base material and preparation method thereof |
| CN113583441B (en) * | 2021-09-07 | 2022-06-28 | 平江县盛盈云母工业有限公司 | Insulating material with mica as base material and preparation method thereof |
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Application publication date: 20150701 |