KR101877018B1 - Preparing method for hydrophobic-granted inorganic binder using silane-treatment and inorganic binder by preparing method thereof - Google Patents

Abstract

The present invention relates to a method for producing an inorganic binder and an inorganic binder produced thereby, which comprises the steps of adding a silane to a mixture of alcohol and water and reacting the silane to hydrolyze the silane, mixing the silicate solution to be mixed with the hydrolyzed silane Preheating the silicate solution to adjust the viscosity, mixing for reaction of the hydrolyzed silane with the preheated silicate solution, heat treating the silane to remove impurities of the reacted silicate, and heat treating the heat treated silicate mixture To a solution state. The present invention relates to a method for producing an inorganic binder having hydrophobicity imparted through a silane treatment, and an inorganic binder produced by the method. The inorganic binder can improve corrosion resistance against water, It can be used for insulation, refractory, and heat-resistant material. And an inorganic binder produced by the method.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an inorganic binder having hydrophobicity through silane treatment, and an inorganic binder prepared by the method. BACKGROUND ART < RTI ID = 0.0 >

The present invention relates to a method for producing an inorganic binder having hydrophobicity imparted by a silane treatment and an inorganic binder produced by the method. More particularly, the present invention relates to a method for producing an inorganic binder by bonding a hydrophobic functional group to a hydroxyl group of a silicate by silane, The present invention relates to a method for improving corrosion durability against water and realizing high thermal properties compared with existing inorganic binders.

Recently, interest in the production of functional composite materials using various inorganic materials is increasing. Today, light inorganic materials are used as building materials because they are high temperature, fireproof, insulation, and low cost materials. In addition, heat insulating boards and the like using lightweight inorganic materials are used in fire doors and are applied to heat insulating materials such as automobile exhaust pipes.

It is well known that such lightweight inorganic materials use binders to combine inorganic materials. However, inorganic materials have limited applications due to their high water uptake rate, and research for securing these problems is increasing.

Glass wool, ceramic wool, perlite, and inorganic materials, which are conventional commercial thermal insulation products, have a problem that the heat insulation performance is drastically deteriorated when moisture is absorbed, and maintenance or replacement is inevitable in case of such a problem.

Therefore, there has been a demand for development of a manufacturing method for lowering the water absorption rate in the production of lightweight inorganic materials and expanding the application field by manufacturing an inorganic binder imparted with hydrophobicity through silane treatment instead of the existing inorganic binder.

The object of the present invention is to provide a method for producing an inorganic binder to which hydrophobicity is imparted by using silane so that an inorganic binder having a higher moisture resistance than an existing inorganic binder can be produced.

Another object of the present invention is to provide a hydrophobic inorganic binder produced by using silane.

(A) adding silane to a mixture of alcohol and water and reacting the silane to hydrolyze the silane; (b) preheating the silicate solution to match the mixed viscosity of the silicate solution to be mixed with the hydrolyzed silane; (c) mixing the hydrolyzed silane for reaction with the preheated silicate solution; (d) heat treating the silane to remove impurities of the silicate reacted therewith; And (e) converting the heat-treated silicate mixture to a solution state.

In step (a), the mixing ratio of the alcohol and water may be 95 wt.%: 5 wt.% To 85 wt.%: 15 wt.%.

The mixing ratio of the alcohol-water mixture and the silane-containing silane solution may be 100 wt%: 1 wt% to 100 wt%: 6 wt%.

The silane solution may be any one selected from 3-aminopropyl-triethoxysilane (APES), 3-chloropropyl-triethoxysilane (CPES), 3-glycidoxypropyl-triethoxysilane (GPES) and 3-mercaptopropyl-triethoxysilane (MPES).

In the step (a), the stirring temperature for hydrolysis of the silane may be 50 to 80 ° C.

The step (c) is preferably carried out at a temperature of 50 to 80 캜 for stirring the hydrolyzed silane and the silicate solution.

When the impurities are removed in step (d), an inorganic binder in a gel state may be formed.

The mixing ratio of the inorganic binder in the gel state to the distilled water may be from 20 wt.%: 80 wt.% To 50 wt.%: 50 wt.% In the gel state inorganic binder. have.

In addition, the present invention can provide the hydrophobic inorganic binder produced by the above method.

The inorganic binder prepared through the method of producing an inorganic binder having hydrophobicity through the silane treatment according to the embodiment of the present invention can realize higher moisture resistance and thermal characteristics than conventional inorganic binders.

The inorganic binder prepared by the method of producing an inorganic binder through hydrophilicity through the silane treatment according to the embodiment can realize higher moisture resistance and thermal characteristics than conventional inorganic binders, and therefore can be applied to heat insulating materials, refractory materials, heat resistant materials, coating materials And the effect of providing high performance is expected.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flowchart sequentially showing an inorganic binder manufacturing method imparted with hydrophobicity through a silane treatment according to an embodiment of the present invention; FIG.
FIG. 2 is a photograph of the solution state viscosity change of the hydrophobic inorganic binder prepared in Examples 1, 7, and 8. FIG.
3 is a photograph of the surface contact angle of the hydrophobic inorganic binder prepared in Comparative Examples and Examples 1, 5, and 6. FIG.

Hereinafter, the description of the present invention with reference to the drawings is not limited to a specific embodiment, and various transformations can be applied and various embodiments can be made. It is to be understood that the following description covers all changes, equivalents, and alternatives falling within the spirit and scope of the present invention.

In the following description, the terms first, second, and the like are used to describe various components and are not limited to their own meaning, and are used only for the purpose of distinguishing one component from another component.

Like reference numerals used throughout the specification denote like elements.

As used herein, the singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. It is also to be understood that the terms " comprising, "" comprising, "or" having ", and the like are intended to designate the presence of stated features, integers, And should not be construed to preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, or combinations thereof.

Hereinafter, embodiments of the present invention will be described in detail with reference to FIGS. 1 to 3 attached hereto.

FIG. 1 is a flowchart sequentially showing an inorganic binder manufacturing method imparted with hydrophobicity through a silane treatment according to an embodiment of the present invention.

Referring to FIG. 1, a method for producing an inorganic binder having hydrophobicity according to the present invention comprises the steps of adding silane to a mixture of alcohol and water to react the silane to hydrolyze the silane (S100), mixing the hydrolyzed silane (S200) to adjust the mixed viscosity of the silicate solution (S200), mixing (S300) for the reaction of the hydrolyzed silane with the preheated silicate solution, the impurity in the silicate mixture reacted with the silane (S400), and converting the heat-treated silicate mixture to a solution state (S500).

Specifically, the step (S100) of adding silane to the mixture of alcohol and water to react the silane to thereby silane is carried out by adding a silane solution to the mixture of alcohol and water and stirring to induce the hydrolysis reaction.

Here, the hydrolysis reaction can be performed at a higher temperature than the normal temperature. At this time, when the mixture of the mixture of alcohol and water and the silane solution is stirred, the temperature may be 50 ° C or higher, and preferably 50 to 80 ° C. If the temperature at the time of stirring exceeds 80 캜, there may arise a problem that only alcohol is vaporized before the hydrolysis reaction of the silane is induced.

If the temperature is less than 50 캜 during stirring, the hydrolysis may take a long time or hydrolysis may not occur.

Here, the silane may be an organosilane-based silane, and may be at least one selected from triethoxysilane, trimethoxysilane, and the like.

The hydrolysis reaction of silane can be carried out by adding alcohol and water to a suitable vessel and adding a silane solution thereto. The ratio of alcohol to water is 95 wt.%: 5 wt.% To 85 wt.%: 15 wt.% .

At this time, the hydrolysis reaction may not occur when the alcohol ratio exceeds 95 wt.% Or the water ratio is less than 5 wt.%. Therefore, when mixing alcohol and water, alcohol should not exceed 95 wt.% And water should be more than 5 wt.%.

The ratio of the mixture of alcohol and water to the silane solution may be from 100 wt.%: 1 wt.% To 100 wt.%: 6 wt.%. For example, the mixture may be mixed with all of the above-mentioned mixture in a container, followed by stirring for 30 to 60 minutes.

Here, the silane solution may be any one selected from 3-aminopropyl-triethoxysilane (APES), 3-chloropropyl-triethoxysilane (CPES), 3-glycidoxypropyl-triethoxysilane (GPES) and 3-mercaptopropyl-triethoxysilane (MPES).

Next, the step (S200) of preheating the silicate solution to match the mixed viscosity of the silicate solution to be mixed with the hydrolyzed silane is carried out by mixing the silicate solution in a suitable vessel to match the mixed viscosity of the hydrolyzed silane mixture with the silicate solution And then heated to the same temperature as the mixture.

The heating temperature at this time may be 50 ° C or higher, preferably 50 to 80 ° C.

The preheating of the silicate solution not only allows the temperature to be close to the temperature of the alcohol, water and silane mixture, but also lowers the viscosity of the silicate solution to facilitate mixing of the alcohol, water and silane mixture solution and silicate solution.

Next, the step (S300) for mixing the hydrolyzed silane mixture with the preheated silicate solution is carried out by mixing the hydrolyzed silane mixture and the preheated silicate solution in a vessel and mixing them.

At this time, it is preferable to use an agitator capable of stirring the silane mixture and the silicate solution at a constant temperature.

The heating temperature or stirring temperature of the stirrer may be in the range of 50 to 80 ° C, preferably 55 to 75 ° C. If the agitation temperature is lower than 50 ° C, the degree of bonding between the hydrolyzed silane and the silicate solution becomes insufficient, which is not suitable for imparting an even hydrophobicity. If the mixing temperature is higher than 80 ° C, the reaction may be completely non-uniform due to rapid water evaporation and rapid partial reaction of the mixture. Further, the stirring time may be 30 to 120 minutes, preferably 60 to 90 minutes, and the mixing speed may be 250 to 500 rpm for an even reaction.

If the mixing speed, that is, the number of revolutions per minute (rpm) of the stirrer is lower than 250 [rpm], the mixing of the hydrolyzed silane with the silicate solution may be uneven.

Next, the heat treatment (S400) for removing the impurities of the silicate reacted with the silane (S400) is performed in a range of less than 100 ° C to remove impurities except for the silicate reacted with the silane, that is, the inorganic binder. Alcohol or water acting as an impurity can react with the silane and the reacted silicate over time. Therefore, the impurities are removed by heating the stirrer to remove impurities such as alcohol and water.

When the impurities are removed, an inorganic binder in a gel state is produced.

Here, a heat treatment process is performed for a predetermined time at a constant temperature of less than 100 캜 in an agitator. At this time, the heat treatment time may be 30 to 120 minutes, preferably 50 to 100 minutes.

Next, the step of converting the silicate reacted with the silane into the solution state (S500) converts the silicate reacted with the silane, that is, the gel-state inorganic binder into the solution state.

The impurity-free inorganic binder is in a gel state, and distilled water is used to convert the gel-state inorganic binder into a solution-state inorganic binder.

At this time, the ratio of the inorganic binder in the gel state to the distilled water may be 20 wt.%; 80 wt.% To 50 wt.%: 50 wt.%.

If the ratio of the distilled water to the distilled water is lower than 20 wt.%, There is a problem that the reaction mixture remains in a gel state.

The contact angle of the wetting liquid (water) of the inorganic binder produced by the hydrophobic-imparted inorganic binder manufacturing method according to the embodiment of the present invention is 30 DEG or more, preferably 40 to 100 DEG, more preferably 40 To 90 degrees.

[Example]

Hereinafter, the present invention will be described in more detail with reference to Examples and Experimental Examples, but the present invention is not limited by these Examples and Experimental Examples. The embodiments according to the present invention can be modified into various other forms, and the scope of the present invention should not be construed as being limited to the embodiments described below. The embodiments of the present invention are provided to enable those skilled in the art to more fully understand the present invention.

85 ml of ethanol, 15 ml of distilled water and 1 ml of silane APES were mixed and stirred. Then, 300 ml of the preheated silicate solution was mixed and stirred, and then mixed with 100 ml of distilled water. The applied inorganic binder was manufactured.

An inorganic binder having hydrophobicity imparted thereto was prepared in the same manner as in Example 1, except that silane CPES was used instead of APES.

An inorganic binder having hydrophobicity imparted thereto was prepared in the same manner as in Example 1, except that silane GPES was used instead of APES.

An inorganic binder having hydrophobicity was prepared in the same manner as in Example 1, except that silane MPES was used instead of APES in Example 1.

An inorganic binder having hydrophobicity was prepared in the same manner as in Example 1, except that the silane ratio in Example 1 was changed to 3 wt.% Instead of 1 wt.%.

An inorganic binder having hydrophobicity imparted thereto was prepared in the same manner as in Example 1, except that the silane ratio in Example 1 was changed to 6 wt.% Instead of 1 wt.%.

An inorganic binder having hydrophobicity was prepared in the same manner as in Example 1, except that the distillation yield in Example 1 was changed to 200 ml instead of 100 ml.

An inorganic binder having hydrophobicity was prepared in the same manner as in Example 1, except that the distillation yield in Example 1 was changed to 300 ml instead of 100 ml.

[Comparative Example 1]

Only the silicate solution used in Example 1 was used.

As shown in FIG. 2, the viscosity of Example 1, Examples 7 and 8 was changed according to the amount of distilled water.

The following experiments were carried out on the hydrophobic-imparted inorganic binders prepared in Examples 1 to 8 and the silicate solutions of the comparative examples.

[Experimental Example 1: Measurement of Heat Resistance of Hydrophobic Inorganic Binder]

The heat resistance of the inorganic binder and the silicate solution of the comparative example prepared in Examples 1 to 4 were measured. For the measurement of heat resistance, inorganic binder samples prepared by completely drying the inorganic binder with hydrophobicity prepared in Examples 1 to 4 and the silicate solution of Comparative Example using an oven at 120 DEG C for 24 hours.

The inorganic binder samples thus prepared were measured for decomposition temperature by a thermogravimetric analyzer (TGA), and the results are shown in Table 1 below.

yield(%) Integral thermal decomposition progress temperature [IPDT] (℃) Example 1 77.18 157894.90 Example 2 77.77 161237.60 Example 3 76.85 174885.10 Example 4 82.94 440876.40 Comparative Example 69.28 60903.78

As shown in Table 1, it can be seen that the yield of the hydrophobic inorganic binder produced by reacting with the silane is better than that of the silicate inorganic binder.

In addition, it was confirmed that the starch pyrolysis progress temperature (IPDT), which is the theoretical temperature at which complete pyrolysis of the material can occur, is about twice as much as that of the pure silicate of the comparative example in all the hydrophobic inorganic binders produced by reacting with silane , And in the case of Example 4 using the silane MPES, it was possible to confirm a superior integrated pyrolysis progress temperature (IPDT).

[Experimental Example 2: Measurement of contact angle of hydrophobic inorganic binder]

The contact angle measurement of the hydrophobic inorganic binder prepared in Examples 1 to 6 and the silicate solution of the comparative example was carried out. For the contact angle measurement, the inorganic binder samples prepared by the hydrophobic inorganic binders prepared in Examples 1 to 6 and the silicate solutions of the comparative examples were thoroughly dried at 120 DEG C for 24 hours using an oven.

Contact Angle (°) Example 1 53.79 Example 2 36.32 Example 3 37.63 Example 4 53.43 Example 5 60.83 Example 6 97.25 Comparative Example Not measurable

As can be seen from Table 2 and FIG. 3, it can be seen that the contact angle of all of the inorganic binders having hydrophobicity produced by reacting with the silane was higher than that of the inorganic binders made only of silicate.

3 (a) is a photographic view of an inorganic binder of a comparative example, (b) is a photographic image of Example 1, (c) is Example 5, and (d) is a photographic image of Example 6. FIG.

Claims (9)

(a) adding silane to a mixture of alcohol and water and reacting the silane to hydrolyze the silane;
(b) preheating the silicate solution to match the mixed viscosity of the silicate solution to be mixed with the hydrolyzed silane;
(c) mixing the hydrolyzed silane for reaction with the preheated silicate solution;
(d) heat treating the silane to remove impurities of the silicate reacted therewith; And
(e) converting the heat treated silicate mixture to a solution state,
The step (a)
The mixing ratio of the alcohol and water is 95 wt.%: 5 wt.% To 85 wt.%: 15 wt.%,
Wherein the mixing ratio of the alcohol-water mixture to the silane-containing silane solution is 100 wt.%: 1 wt.% To 100 wt.%: 6 wt.%.
delete delete The method according to claim 1,
Wherein the silane solution is any one selected from the group consisting of 3-aminopropyl-triethoxysilane (APES), 3-chloropropyl-triethoxysilane (CPES), 3-glycidoxypropyl-triethoxysilane (GPES), and 3-mercaptopropyl-triethoxysilane A method of manufacturing an applied inorganic binder.
The method according to claim 1,
The step (a)
Wherein the stirring temperature for hydrolysis of the silane is 50 to 80 ° C.
The method according to claim 1,
The step (c)
Wherein the hydrolyzed silane is reacted with the silicate solution at a temperature of 50 to 80 DEG C under agitation.
The method according to claim 1,
In the step (d)
Wherein when the impurities are removed, an inorganic binder in a gel state is formed.
8. The method of claim 7,
The step (e)
Distilled water is mixed with the inorganic binder in the gel state,
Wherein the mixing ratio of the inorganic binder in the gel state to the distilled water is 20 wt.%: 80 wt.% To 50 wt.%: 50 wt.%.
An inorganic binder produced by the production method of any one of claims 1 to 8,

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