阅读说明：本技术 一种剥离滑石片层的方法 (Method for stripping talc lamella ) 是由 钟力 邹正光 于 2021-10-04 设计创作，主要内容包括：本发明公开了一种剥离滑石片层的方法。本方法将合适的有机物溶液与滑石粉混合并油浴加热,先制备出有机插层的滑石复合材料,然后将有机插层的滑石复合材料在合适条件下煅烧,使其层间的有机物完全分解进而从滑石层间逸出,从而使滑石粉片层之间相互剥离,得到最终产品。本发明制备出的产物,不仅剥离效果良好,使滑石的比表面积有了显著的提高,而且还可以保持滑石良好的晶体结构,提高滑石的使用价值。(The invention discloses a method for stripping a talc sheet layer. The method mixes a proper organic solution with talcum powder and heats the mixture in an oil bath to prepare the talc composite material with the organic intercalation, and then calcines the talc composite material with the organic intercalation under proper conditions to ensure that the organic matters between layers of the talc composite material are completely decomposed and then escape from the layers of the talc, thereby mutually stripping the talcum powder layers to obtain the final product. The product prepared by the invention not only has good stripping effect and obviously improves the specific surface area of the talc, but also can keep the good crystal structure of the talc and improve the use value of the talc.)

1. A method of exfoliating a talc platelet characterized by: the method comprises the following specific steps:

(1) preparing a certain amount of organic cation solution, adding into a beaker, adding a proper amount of talcum powder, and stirring under the condition of oil bath to prepare a suspension;

(2) after the mixed liquid prepared in the step (1) is filtered, the mixed liquid is placed into a forced air drying oven to be dried and then taken out, and the dried mixed liquid is ground to obtain organic cation modified talcum powder;

(3) preparing a certain amount of active organic matter solution, adding the active organic matter solution into a beaker, adding the powder obtained in the step (2), and stirring under the oil bath condition to prepare suspension;

(4) after the mixed liquid prepared in the step (3) is filtered, the mixed liquid is put into a blast drying oven to be dried and then taken out, and the mixed liquid is ground to obtain the talc powder with the active organic matter intercalation;

(5) preparing a certain amount of easily-decomposed organic matter solution, adding the easily-decomposed organic matter solution into a beaker, adding the powder obtained in the step (4), and stirring at normal temperature to prepare a suspension;

(6) after the mixed liquid prepared in the step (5) is subjected to suction filtration, the mixed liquid is placed into a blast drying oven for vacuum drying and then taken out, and talc powder easy to decompose the organic matter intercalation is obtained by grinding;

(7) putting the powder prepared in the step (6) into a porcelain boat, and calcining in a muffle furnace to obtain talc powder from which the interlaminar organic matters are removed;

(8) and (4) grinding the powder prepared in the step (7) to obtain the exfoliated talc.

2. The method of claim 1, wherein the organic cation intercalator inserted between the layers of the talc is any one of quaternary ammonium cations, such as triethanolamine cation solution, cetyltrimethylammonium bromide, and tetradecyltrimethylammonium chloride.

3. The method according to claim 1, wherein the first drying temperature is 70 to 90 ℃ and the time is 12 to 36 hours.

4. The method of claim 1, wherein the active organic intercalant inserted between the talc layers is any active small molecule organic substance, such as dimethyl sulfoxide, methanol, etc.

5. The method according to claim 1, wherein the second drying temperature is 70 to 90 ℃ and the time is 24 to 48 hours.

6. The process according to claim 1, wherein the easily decomposable organic intercalator inserted between the talc layers is any organic substance decomposable into a gas, and may be hydrazine, urea, ammonium acetate or the like.

7. The method according to claim 1, wherein the third drying temperature is 40 to 50 ℃ and the time is 24 to 48 hours.

8. The preparation method according to claim 1, wherein the calcination temperature is 400 to 600 ℃, the temperature rise rate is 5 to 10 ℃/min, and the time is 3 to 5 hours.

9. The invention discloses and states the purpose of peeling the talcum sheet layer by using organic intercalation for the first time.

Technical Field

The invention relates to a method for stripping a talc lamella, belonging to the field of preparation of inorganic superfine lamella materials.

Background

The talc is hydrated magnesium silicate with a special layered structure, has good adsorbability, chemical stability, strong acid and strong alkalinity resistance and larger specific surface area, can be physically or chemically connected with a polymer to improve the thermodynamic performance of the material, and has abundant natural reserve. The talcum powder can be widely applied to various fields of paper making, coating, medicine, sewage treatment, plastic products and the like, and has a very wide application prospect. In the production of many high-grade products in the above industries, the requirements for the particle size and dispersibility of raw materials are higher and higher, so that the peeling of the talc material is particularly important.

The exfoliation techniques of layered silicates include mechanical abrasive exfoliation and chemical exfoliation. The mechanical grinding method has the defects that: the phyllosilicate material can be subjected to an additional shearing force in the grinding process to damage the crystal structure of the phyllosilicate material, so that the product performance is poor. The principle of the chemical stripping method is that organic molecules are inserted between layers of a layered silicate material through intercalation reaction, so that the distance between the layers is increased, Van der Waals acting force and bonding force between the layers are damaged, and after organic intercalation substances are removed, the layers which are originally tightly stacked can naturally peel off from each other, thereby achieving the purpose of natural stripping. But the application of the chemical stripping method on the talc material faces huge technical challenges, and the talc has strong Van der Waals force and extremely small distance between layers, so that most organic matters are difficult to directly enter the layers of the talc through intercalation. Therefore, how to obtain exfoliated talc powder by organic intercalation is an urgent problem to be solved.

Disclosure of Invention

The invention aims to provide a method for stripping a talc sheet layer. Provides effective experimental basis for researching the application of the chemical stripping method in the research field of the talc stripping.

In order to realize the purpose, the invention firstly selects proper organic molecules and technology to prepare the talc composite material with organic intercalation, the organic molecules are inserted to prop open the talc sheet layer so as to enlarge the interlayer space, and then the subsequent heat treatment is carried out on the product so as to realize the interlayer stripping of the talc powder sheet layer. The talc flake peeled by the method has larger specific surface area, the thickness of the flake layer is greatly reduced, and the flake shape of the original talc powder can be completely reserved.

The method comprises the following specific steps:

(1) preparing a certain amount of organic cation solution, adding into a beaker, adding a proper amount of talcum powder, and stirring under the condition of oil bath to prepare suspension.

(2) And (2) carrying out suction filtration on the mixed liquid prepared in the step (1), drying the mixed liquid in a blast drying oven, taking out the dried mixed liquid, and grinding the dried mixed liquid to obtain the organic cation modified talcum powder.

(3) Preparing a certain amount of active organic matter solution, adding the active organic matter solution into a beaker, adding the powder obtained in the step (2), and stirring under the condition of oil bath to obtain a suspension.

(4) And (4) after the mixed liquid prepared in the step (3) is filtered, the mixed liquid is placed into a blast drying oven to be dried and then taken out, and the active organic matter intercalated talcum powder is obtained by grinding.

(5) Preparing a certain amount of easily decomposed organic matter solution, adding the organic matter solution into a beaker, adding the powder obtained in the step (4), and stirring at normal temperature to prepare suspension.

(6) And (5) after the mixed liquid prepared in the step (5) is filtered, the mixed liquid is placed into a blast drying oven for vacuum drying and then taken out, and the talc powder easy to decompose the organic intercalation is obtained after grinding.

(7) And (4) putting the powder prepared in the step (6) into a porcelain boat, and calcining in a muffle furnace to obtain the talc powder without the interlaminar organic matters.

(8) And (4) grinding the powder prepared in the step (7) to obtain the exfoliated talc.

Preferably, the organic cation intercalator inserted between the talc layers may be any quaternary ammonium cation, such as triethanolamine cation solution, cetyltrimethylammonium bromide, tetradecyltrimethylammonium chloride, and the like.

Preferably, the first drying temperature is 70-90 ℃, and the time is 12-36 h.

Preferably, the active organic intercalation compound inserted between the talc layers can be any active small molecule organic compound, such as dimethyl sulfoxide, methanol and the like.

Preferably, the second drying temperature is 70-90 ℃ and the time is 24-48 h.

Preferably, the easily decomposable organic intercalator inserted between the talc layers may be any organic substance decomposable into a gas, and may be hydrazine, urea, ammonium acetate, or the like.

Preferably, the third drying temperature is 40-50 ℃ and the time is 24-48 h.

Preferably, the calcining temperature is 400-600 ℃, the heating rate is 5-10 ℃/min, and the time is 3-5 h.

According to the invention, the talc is peeled by a chemical peeling method, so that an effective experimental basis is provided for researching the application of the chemical peeling method in the talc peeling research field, the thickness of the prepared talc sheet layer is greatly reduced, and the specific surface area of the product is from 4-6 m²The/g is increased to 30-32 m²/g。

Drawings

FIG. 1 is an SEM photograph at 5000 magnification of talc platelets produced according to example 1 of the present invention.

FIG. 2 is an SEM photograph at 5000 magnification of the talc platelet layer obtained in comparative example 1 of the present invention.

Detailed Description

Example 1:

24ml of triethanolamine, 6ml of phosphoric acid and 210ml of deionized water are weighed and added into a beaker, the beaker is placed on a constant temperature heating magnetic stirrer, 3g of talcum powder is added while stirring, and the mixture is stirred for 24 hours in an oil bath at 80 ℃. And (3) after the mixed solution is subjected to suction filtration, the mixed solution is placed into a forced air drying oven to be dried for 12 hours at the temperature of 80 ℃, and then the dried mixed solution is taken out and ground to obtain the organic cation modified talcum powder. 180ml of dimethyl sulfoxide and 20ml of deionized water are weighed and added into a beaker, and then the talc powder modified by organic cations is added and stirred for 24 hours in an oil bath at the temperature of 80 ℃. And after the prepared mixed solution is subjected to suction filtration, the mixed solution is placed into a blast drying oven to be dried for 12 hours at the temperature of 80 ℃, and then the dried mixed solution is taken out and ground to obtain the talc powder with the active organic matter intercalation. 150g of ammonium acetate and 100g of deionized water are weighed and added into a beaker, and then the talc powder of the active organic matter intercalation is added and stirred for 24 hours at normal temperature. And (3) performing suction filtration on the prepared mixed solution, putting the mixed solution into a blast drying oven, performing vacuum drying at 40 ℃ for 24 hours, taking out the mixed solution, and grinding the dried mixed solution to obtain the talcum powder with the intercalation of the organic matters easy to decompose. And putting the prepared powder into a porcelain boat, calcining in a muffle furnace at the temperature of 300 ℃, at the heating rate of 5 ℃/min for 4h, and grinding to obtain the peel-off talc. The thickness of the prepared talc tablet is greatly reduced, and the specific surface area is measured from 5m²The/g is increased to 30m²/g。

Example 2:

180ml of dimethyl sulfoxide and 20ml of deionized water are weighed and added into a beaker, the beaker is placed on a constant temperature heating magnetic stirrer, 3g of talcum powder is added while stirring, and the mixture is stirred for 24 hours in an oil bath at 80 ℃. And after the prepared mixed solution is subjected to suction filtration, the mixed solution is placed into a blast drying oven to be dried for 12 hours at the temperature of 80 ℃, and then the dried mixed solution is taken out and ground to obtain the talc powder with the active organic matter intercalation. 150g of ammonium acetate and 100g of deionized water are weighed and added into a beaker, and then the talc powder of the active organic matter intercalation is added and stirred for 24 hours at normal temperature. And (3) performing suction filtration on the prepared mixed solution, putting the mixed solution into a blast drying oven, performing vacuum drying at 40 ℃ for 24 hours, taking out the mixed solution, and grinding the dried mixed solution to obtain the talcum powder with the intercalation of the organic matters easy to decompose. And putting the prepared powder into a porcelain boat, calcining in a muffle furnace at the temperature of 300 ℃, at the heating rate of 5 ℃/min for 4h, and grinding to obtain the peel-off talc.

Example 3:

weighing 5g of octadecyl trimethyl ammonium bromide into a beaker, weighing 2.5ml of hydrochloric acid and 340ml of deionized water, adding into the beaker to prepare a mixed solution, then putting the beaker on a constant-temperature heating magnetic stirrer, adding 3g of talcum powder while stirring, and carrying out oil bath stirring on the mixture at 80 ℃ for 24 hours. And (3) after the mixed solution is subjected to suction filtration, the mixed solution is placed into a forced air drying oven to be dried for 12 hours at the temperature of 80 ℃, and then the dried mixed solution is taken out and ground to obtain the organic cation modified talcum powder. 180ml of dimethyl sulfoxide and 20ml of deionized water are weighed and added into a beaker, and then the talc powder modified by organic cations is added and stirred for 24 hours in an oil bath at the temperature of 80 ℃. And after the prepared mixed solution is subjected to suction filtration, the mixed solution is placed into a blast drying oven to be dried for 12 hours at the temperature of 80 ℃, and then the dried mixed solution is taken out and ground to obtain the talc powder with the active organic matter intercalation. 150g of ammonium acetate and 100g of deionized water are weighed and added into a beaker, and then the talc powder of the active organic matter intercalation is added and stirred for 24 hours at normal temperature. And (3) performing suction filtration on the prepared mixed solution, putting the mixed solution into a blast drying oven, performing vacuum drying at 40 ℃ for 24 hours, taking out the mixed solution, and grinding the dried mixed solution to obtain the talcum powder with the intercalation of the organic matters easy to decompose. And putting the prepared powder into a porcelain boat, calcining in a muffle furnace at the temperature of 300 ℃, at the heating rate of 5 ℃/min for 4h, and grinding to obtain the peel-off talc.

Comparative example 1:

talc powder from a company was used as the talc raw material of example 1.

SEM pictures of comparative example 1 at 5000 x magnification were tested according to the test method of example 1 to observe the change in morphology.