KR100491118B1 - Layered Na-Silicate for Strength Reinforcement of Polymer Composites and its production method - Google Patents

Abstract

    The present invention relates to an intercalated organic layered silicate used as a strength reinforcing agent of a polymer composite and a method of manufacturing the same, and more particularly, to a polymer composite by intercalating amine, cationic and neutral templates into the layered silicate. The present invention relates to an intercalated organic layered silicate that allows a polymer material to be smoothly inserted between layers to act as a strength enhancer, and a method of manufacturing the same.

Description

Layered Na-Silicate for Strength Reinforcement of Polymer Composites and its production method}

The present invention relates to an organic layered silicate for strength reinforcement of a polymer composite and a method of manufacturing the same, and more particularly, to a layered silicate by intercalating amines, cationic and neutral templates to expand the interlayers, thereby increasing the interlayer. The present invention relates to an organic layered silicate for strength reinforcement of a polymer composite that is smoothly inserted between the polymer composites and serves as a strength reinforcing agent, and a method of manufacturing the same.

As a synthesis method of mesoporous silica, the following three synthesis methods are known by the combination of a silica source and a template, for example. The first method is a method described in US3556725, Japanese Patent Application Laid-open No. Hei 5-503499, Japanese Patent Application Laid-open No. Hei 8-34607, and the like, wherein the amorphous silica powder or aqueous alkali silicate solution and active silica are described. It is a method synthesize | combined in an alkaline region using as a silica source the quaternary ammonium salt or phosphonium salt which has a long-chain alkyl group as a template. The second method is a method described in Japanese Patent Application Laid-open No. Hei 4-238810 and the like, which is obtained by using a layered silicate such as kaneite as a silica source and a long chain alkylammonium cation as a template, It is a method of synthesis. The third method is a method described in US5672556 and the like, wherein alkoxides such as tetraethoxysilane and the like are used as silica sources, and alkylamine and the like are used as templates.

The first method is performed in an alkaline region using strong cationic surfactants such as quaternary ammonium salts as templates. Mesoporous silica is obtained by removing these templates, wherein any one of the methods of oxidative decomposition in air or proton exchange with an acid and a solvent is essential for removing the template. In the second method, in addition to this, it is necessary to synthesize canemate or the like which is a starting material. The third method is advantageous for the removal of the template because amine is used as the template, but is not advantageous for industrial mass production because alkoxides such as tetraethoxysilane and the like are expensive.

Thus, the synthesis of mesoporous silica was inevitably carried out in the alkaline region using a strong cationic surfactant such as quaternary ammonium salt as a template or using expensive raw materials such as alkoxides. The mesoporous silica synthesized under such conditions had a poor hydrophobic surface, which was disadvantageous for absorption of aqueous solutions and the like.

Therefore, the present invention is to insert the amine, cationic and neutral template in the layered silicate to widen the interlayer of the layered silicate, so that the polymer material is smoothly inserted between the layers in the production of the polymer composite having the effect of strengthening the strength of the polymer material It is an object of the present invention to provide an organic layered silicate for strength reinforcement and a method of manufacturing the same.

The above object of the present invention is achieved by an intercalation method of an organic ring layered silicate for strength reinforcement of a polymer composite, characterized by mixing and reacting a layered sodium silicate and a template used as a column and synthesizing an organicized layered silicate.

The intercalated organic layered silicate according to the present invention forms a layer, and the interlayer spacing by X-ray diffraction is 2.0 to 4.6 nm.

Although it does not specifically limit as a neutral template used by this invention, A long-chain alkylamine oxide etc. can be used.

The amine used in the present invention is preferably represented by the structural formula RNH2 (wherein R represents an alkyl group having 8 to 20 carbon atoms), and specifically, dodecylamine, tetradecylamine, hexadecylamine, octadecylamine, or the like. Can be mentioned.

As a nonionic surfactant used by this invention, what is represented by structural formula R (OCH2CH2) nOH (where R represents a C12-20 alkyl group and n represents 2-30) is specifically poly Oxyethylene lauryl ether, polyoxyethylene cetyl ether, polyoxyethylene stearyl ether and the like.

Examples of the cationic surfactant used in the present invention include hexadecyltrimethylammonium bromide, hexadecyltrimethylammonium chloride, and the like.

The composition used for these reactions is 1-20, Preferably the range of 1-10 is used as molar ratio of layered sodium silicate / template.

The reaction proceeds easily even at room temperature, but may be carried out under heating up to 80 ° C as necessary. The reaction time is in the range of 0.5 to 24 hours, preferably 2 to 4 hours. The pH at the time of reaction becomes like this. Preferably it is the range of 6-12, and 8-9 are more preferable.

The template dispersion medium in the synthesis reaction is preferably a lower alcohol such as water, ethanol or methanol.

The synthesized organic layered silicate is filtered off by filtration or the like, washed, dried with water, ethanol or methanol to obtain an organic layered silicate powder.

Hereinafter, an interlayer insertion method of strength reinforcing layered sodium silicate (-Na 2 Si 2 O 5) of a polymer composite according to an exemplary embodiment of the present invention will be described in detail.

In the examples, powder X-ray diffractograms were measured using the RINT 2500 from Rig.

Example 1

500 ml of 0.1 mol hexadecyltrimethylammonium bromide solution dissolved in water and 26 g of layered sodium silicate (-Na2Si2O5) were added to a 1000 ml reactor, and the mixture was heated to 50 ° C while stirring for 4 hours. The organic layered silicate obtained after the reaction was filtered and washed with water, dried at 60 ° C. for 24 hours to obtain an organic layered silicate powder.

Example 2

500 ml of a 0.1 mole hexadecyltrimethylammonium bromide solution dissolved in ethanol and 26 g of layered sodium silicate (-Na2Si2O5) were added to a 1000 ml reactor, and the mixture was heated to 50 ° C and stirred for 4 hours. The organic layered silicate obtained after the reaction was filtered and washed with ethanol, dried at 60 ° C. for 24 hours to obtain an organic layered silicate powder. The X-ray diffractogram of this sample showed peaks at d value = 4.2 nm and d value = 3.8 nm.

Example 3

In a 1000 ml reactor, 500 ml of a 0.1 molar hexadecyltrimethylammonium bromide solution dissolved in a mixed solution of water and ethanol 2: 1 and 26 g of layered sodium silicate (-Na2Si2O5) were added thereto, and the mixture was heated to 50 ° C and stirred for 4 hours. The organic layered silicate obtained after the reaction was filtered, washed with a mixed solution of water and ethanol 2: 1, dried at 60 ° C. for 24 hours to obtain an organic layered silicate powder. The X-ray diffractogram of this sample showed a peak at d value = 3.8 nm.

Comparative Example 1

Instead of the reaction temperature of 50 ° C. in Example 1, a layered silicate powder obtained by reacting at room temperature was organicized.

In the X-ray diffractogram of this sample, a peak was found at a value d = 4.2 nm.

Comparative Example 2

Instead of the reaction temperature of 50 ° C. in Example 2, a layered silicate powder obtained by reacting at room temperature was organicized.

Comparative Example 3

Instead of the reaction temperature of 50 DEG C in Example 3, a layered silicate powder obtained by reacting at room temperature was organicized.

   The intercalated organic layered silicate according to the present invention and a method for preparing the same are used to widen the interlayers of layered silicates by intercalating amine, cationic and neutral templates into the layered sodium silicate to smoothly polymer materials between layers. Inserted to have the effect of strengthening the strength of the polymer material.

1 is a powder X-ray diffraction diagram of mesoporous silica synthesized in Example 1 according to the present invention.

2 is a powder X-ray diffraction diagram of mesoporous silica synthesized in Example 2 according to the present invention.

3 is a powder X-ray diffraction diagram of mesoporous silica synthesized in Example 3 according to the present invention.

4 is a powder X-ray diffraction diagram of mesoporous silica synthesized in Comparative Example 2 according to the present invention.

Claims (6)

As a method for producing a silicate, as a method for producing a silicate, a layered organic silicate is prepared by mixing and reacting a layered sodium silicate with a neutral, amine, nonionic or cationic surfactant at a pH of less than 10 and 40 to 80 ° C. for 2 to 4 hours. Method of producing a layered organic silicate for strength reinforcement of a polymer composite, characterized in that the synthesis. A layered organic silicate for strength reinforcement of a polymer composite, wherein a surfactant is intercalated into the layered sodium silicate to form a layer so that the polymer material is smoothly intercalated in the preparation of the polymer composite, and the interlayer spacing is 2 to 4.6 nm. delete delete delete delete