CN100439245C

CN100439245C - Preparation method of acid swellable mica

Info

Publication number: CN100439245C
Application number: CNB2006100650414A
Authority: CN
Inventors: 周明辉
Original assignee: Individual
Current assignee: Individual
Priority date: 2006-03-15
Filing date: 2006-03-15
Publication date: 2008-12-03
Anticipated expiration: 2026-03-15
Also published as: CN101037209A

Abstract

The present invention relates to a method of preparing swelling mica in acid solution, which comprises the steps of mixing the mica powder with alkaline matter, heating to execute ion exchange, and then diluting and scrubbing with water to lower the temperature of the mica solid, separating the mica solid from the alkaline solution, adding acid to the mica solid to neutralize, and separating the mica solid from the acid solution. In the present invention, the heating reaction having a long reaction time and a high reaction temperature of more than 260 DEG C is not needed, so that the manufacturing cost is reduced and the market competitive power is improved.

Description

Mica method for making that can swelling in acid

Technical field

The invention provides a kind of mica method for making that can swelling in acid, especially refer to a kind of micaceous of swelling cheaply method for making.

Background technology

In the prior art, with lamellar aluminosilicate (polynite, mica) as nanometer (how rice) matrix material be present industry one of the extensive technology of knowing, comparatively general with polymer-clay (polynite) nano composite material at present, mica is the lamellar aluminosilicate mineral, be generally non-swelling MICA, its many characteristics that do not have practicality, only can use as stopping composition merely, therefore how converting non-swelling mica to the swelling mica is the direction that present material industry is studied.

Further investigation reveals that about non-swelling mica being converted to swelling micaceous research document, at first come from people's such as Japanese Ikazaki research, it carries out mechanical mill with lithium nitrate, SODIUMNITRATE, saltpetre and rubidium nitrate to sericite, can obtain the sericite powder of a high surface area, point out in its article of delivering that sericite interlayer potassium ion content is relevant with the variation of specific area, sericite can destroy its crystalline structure after grinding, and making potassium ion to exchange, its result of study also shows that rubidium nitrate is best grinding aid.

In addition, just make swelling micaceous method for making aspect in detail, No. 460427 " method for making of swelling sericite and uses thereof " middle disclosure of tw Taiwan invention bulletin has the sericite of use lithium nitrate and powder to carry out ion-exchange, to obtain the swelling mica.

Yet the lithium nitrate of use that above-mentioned patent documentation is put down in writing, or the disclosed SODIUMNITRATE of Japanology document, saltpetre or rubidium nitrate are neutral treatment agent, the lithium nitrate of being put down in writing with the tw Taiwan patent documentation, temperature required when it carries out ion-exchange up to 260 ℃～420 ℃, and embodiment need reach 40 hours 1 disclosed heat-up time, embodiment is respectively 16 2 disclosed heat-up times, 40,96 hours, need the very long time of cost to heat, though therefore can produce the swelling mica, but because for the required temperature height of ion-exchange, and the treatment time is of a specified duration, will cause the raising of cost, in addition, lithium nitrate as ion-exchanger costs an arm and a leg, be similarly one of reason that causes the cost raising, swelling mica with the disclosed method making of this patent documentation, price is very high, if, will help swelling mica popularizing on market so can work out a kind of method for making that does not need to expend so a large amount of energy and use expensive raw material.

Summary of the invention

In view of this inventor actively sets about being engaged in research and development, in the hope of improving the shortcoming of above-mentioned existing making swelling mica method, through constantly research and effort, develops the present invention finally.

The object of the present invention is to provide the low swelling micaceous method for making of a kind of required cost.

To achieve the above object of the invention, the present invention takes following technique means, comprising following steps:

Mixing step mixes the powdery mica with the metal alkaline material, its blended part by weight is 1: 1～1: 20;

Heating steps is heated to 150 ℃～230 ℃ with mixed powdery mica and alkaline matter, keeps this temperature and continues 30 minutes to carry out ion diffusion, allows the metal ion in the alkaline matter be dispersed in the micaceous interlayer matrix;

The cooling washing step with powdery mica after the heating end and the washing of alkaline matter dilute with water, makes the cooling of mica solid;

Solid-liquid separation step for the first time: with alkaline matter by water dilute formed basic solution and mica solids constituent from;

Add sour neutralization procedure, be adjusted to mica solid pH-value less than 7;

Solid-liquid separation step for the second time, thin up adds the acidic solution after the acid neutralization, acidic solution after will diluting again and mica solids constituent from, the mica solid of gained is product.

Above-mentioned steps of the present invention does not need high temperature, long reacting by heating, can reach production swelling micaceous purpose, has therefore reduced cost of manufacture.

The water of dilution usefulness is preferably cold water in the described cooling washing step; The acidic solution that adds sour neutralization procedure and be thin up re-uses on the mica solid, with the alkaline matter on the residual mica solid that neutralizes.

Metal alkaline material in the above-mentioned mixing step is strong alkaline substance or its mixtures such as lithium hydroxide, sodium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide or hydrated barta; Described heating steps is for to be heated to 150 ℃～230 ℃ with mixed powdery mica and strong alkaline substance, and keeps continuing under this temperature 30 minutes to carry out ion diffusion again, allows the metal ion in the strong alkaline substance be uniformly diffuse in the micaceous interlayer matrix; Powdery mica and strong alkaline substance that described cooling washing step will heat after finishing preferably utilize cold water to dilute washing, and purpose is to make the cooling of mica solid.

Above-mentioned first time solid-liquid separation step be utilize basic solution after water extracter will dilute and mica solids constituent from, get the mica solid thin up washing again after the dehydration, solid-liquid separation to the alkaline components in the mica solid of going again is less than 1wt% and carries out subsequent step again;

It is above-mentioned that to add sour neutralization procedure be to add acidic solutions such as sulfuric acid, hydrochloric acid, nitric acid, acetic acid or oxalic acid, re-use on the mica solid after in this acidic solution, adding the cold water dilution, will residue in the alkaline matter neutralization on the mica solid, to be adjusted to mica solid pH-value less than 7 o'clock, mica promptly can produce the swelling phenomenon;

Above-mentioned second time, solid-liquid separation step was first thin up acidic solution, acidic solution after will diluting with water extracter again and mica solids constituent from, the mica solid of gained is product.

Via above-mentioned steps, the present invention need not use up to the high temperature more than 260 ℃ and carry out long reacting by heating, can reach production swelling micaceous purpose, therefore can reduce the cost when making, and increases the swelling micaceous market competitiveness.

Description of drawings

Fig. 1: schema of the present invention.

Embodiment

Describe the present invention in detail below in conjunction with accompanying drawing, but do not limit practical range of the present invention.

Please referring to shown in Figure 1, the present invention's swelling micaceous method for making includes:

Mixing step (1): with powdery mica and lithium hydroxide, sodium hydroxide, potassium hydroxide, rubidium hydroxide, the alkaline matter of cesium hydroxide or hydrated barta mixes, the blended weight ratio is 1: 1～1: 20, preferred sodium hydroxide of employed alkaline matter and/or lithium hydroxide, the mixture of sodium hydroxide and lithium hydroxide most preferably, this sodium hydroxide and lithium hydroxide account for more than the 80wt% of alkaline matter, all the other compositions highly basic that uses other solubilities (potassium hydroxide for example of can arranging in pairs or groups, rubidium hydroxide, cesium hydroxide or hydrated barta) so that total amount reaches 100%, above-mentioned employed mica comprises white mica, coloured mica, sericite, fluorine mica and pyrophyllite etc.;

Heating steps (2): mixed powdery mica and alkaline matter are heated to 150 ℃～230 ℃, and (for example 150 ℃～230 ℃) continue 30 minutes to carry out ion diffusion under the maintenance certain temperature, allow the metal ion in the alkaline matter evenly be spread in the micaceous interlayer matrix;

Cooling washing step (3): the powdery mica and the alkaline matter that will heat after finishing utilize cold water to dilute, and make mica solid temperature fall;

Solid-liquid separation step (4) for the first time: utilize basic solution after water extracter will dilute and mica solids constituent from, get the mica solid thin up washing again after the dehydration, go solid-liquid separation sodium hydroxide and lithium hydroxide composition to the mica solid again and be less than 1wt% and carry out subsequent step again;

Add sour neutralization procedure (5): add re-using on the mica solid after acidic solutions such as sulfuric acid, hydrochloric acid, nitric acid, acetic acid or oxalic acid dilute with cold water, will residue in the alkaline matter neutralization on the mica solid, to be adjusted to mica solid pH-value less than 7 o'clock, the preferred acid base number was less than 4 o'clock, mica promptly can produce the swelling phenomenon, again, aforementioned acidic solution is preferably nitric acid;

Solid-liquid separation step (6) for the second time: first thin up acidic solution, acidic solution after will diluting with water extracter again and mica solids constituent from, the mica solid of gained is product.

Embodiment 1

Getting 1 kilogram of powdery mica mixes with sodium hydroxide and 1 kilogram of lithium hydroxide of 5 kilograms, be heated to 220 ℃ with molten sodium hydroxide, and continue 30 minutes to carry out ion diffusion, treat that the cold water that finished in 30 minutes 2 liters of room temperatures adds in the molten sodium hydroxide to dilute its basicity, simultaneously mica is lowered the temperature, sodium hydroxide solution and mica solid after will lowering the temperature afterwards carry out solid-liquid separation with water extracter again, the nitric acid that add about 100 grams are in adding on the mica solid that cold water dilutes the alkaline matter that is attached to dilution on the mica solid again, mica solid acid base number after the dilution is 7, the cold water that adds room temperature once again is with dilute acid solution, this moment, the mica solid promptly began to produce the swelling phenomenon, utilize acidic solution after water extracter will dilute again and mica solids constituent from, the mica solid of gained is product, and its weight is 0.85 kilogram.

Via the swelling mica of the inventive method made, therefore its manufacturing cost can effectively increase the swelling micaceous market competitiveness far below existing manufacture method.

Claims

1, a kind of mica method for making that can swelling in acid, comprising following steps:

Solid-liquid separation step for the first time: will by water-reducible basic solution and mica solids constituent from;

2, method for making as claimed in claim 1, wherein the employed metal alkaline material of mixing step is lithium hydroxide, sodium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide or hydrated barta or its mixture.

3, method for making as claimed in claim 1, wherein adding the employed acidic solution of sour neutralization procedure is sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, acetic acid or oxalic acid.

4, as claim 1 or 2 or 3 described method for makings, wherein adding sour neutralization procedure is to be adjusted to mica solid pH-value less than 7 by adding acidic solution.

5, method for making as claimed in claim 4, wherein the solid-liquid separation step and second solid-liquid separation step are to utilize water extracter or pressure filter to carry out solid-liquid separation for the first time.

6, as claim 1 or 2 or 3 described method for makings, wherein employed alkaline matter comprises sodium hydroxide and lithium hydroxide in the mixing step, and described sodium hydroxide and lithium hydroxide account for more than the 80wt% of this alkaline matter.

7, method for making as claimed in claim 6 comprises also wherein and uses other solubility highly basic materials so that the alkaline matter total amount reaches 100% that these other solubility highly basic materials comprise potassium hydroxide, rubidium hydroxide, cesium hydroxide or hydrated barta.

8, method for making as claimed in claim 1, wherein said mica comprise white mica, coloured mica, sericite and fluorine mica.