JPH0748559A - Water repellent material and manufacturing method thereof - Google Patents

Abstract

(57) [Summary] [Object] To provide a water-repellent material having excellent water repellency and durability by a simple method and applicable to a wide range of applications, and a method for producing the same. Further, it provides a water-repellent material capable of controlling the movement of water in the soil extremely efficiently, which is caused by a capillary phenomenon that occurs in voids formed between particles of the soil such as a sandy beach and a dune. ## STR1 ## RnSiX4-n (R represents a monovalent hydrocarbon group having 2 or more carbon atoms or a phenyl group or a monovalent hydrocarbon group having a substituent. X is chlorine. N is an integer of 3 or less.) A water-repellent material obtained by dissolving a silane compound represented by the formula (3) in an organic solvent, mixing this with a granular inorganic material, and then filtering, washing with water, and drying. is there.

Description

Detailed Description of the Invention

[0001]

The present invention relates to a novel water repellent material,
More specifically, it relates to a novel water repellent material obtained by producing a specific silane compound and an inorganic material by a specific method, and a method for producing the same.

This water-repellent material can efficiently control the water content in the soil when it is used to improve the soil. Therefore, it is necessary to protect the soil from desertification, desert greening, forest protection, and other environmental protection industries and various agriculture. It is particularly effectively used in industrial fields such as horticulture, and in the field of ground structure such as civil engineering and construction.

[0003]

2. Description of the Related Art In recent years, cultivation of agricultural products has been actively attempted in so-called dry areas such as beaches and dunes. Irrigation farming, for example, is carried out in these areas,
In sandy beaches and dunes, it is extremely difficult to control the movement of water in the soil because the water is taken up or discharged by the capillary phenomenon that occurs in the voids formed between the sand particles. Therefore, in the cultivation of agricultural products on sandy beaches and dunes, it is extremely important to control the movement of water in the soil to maintain the soil environment suitable for the agricultural products.

Conventionally, as a method for controlling the water content in the soil, there is known a method in which a waterproof sheet is put on a certain section of an agricultural land or an asphalt layer is formed in the soil.

On the other hand, although water-repellent materials and their manufacturing methods are different for each purpose of use, for example, a method of water-repellently treating sand using a commercially available waterproofing agent (Japanese Patent Laid-Open No. 179588/1987). Kaihei 2-171126)
Alternatively, a method of treating sand with silicone oil or alkoxysilane (US Pat. No. 4,036,658, JP-A-1-31)
9585) and the like are known.

[0006]

However, any of the methods for controlling the water content in the soil by placing a waterproof sheet on a certain section of the farmland or forming an asphalt layer in the soil is a large-scale work. And enormous cost is required. Furthermore, in dry areas such as sandy beaches and dunes, the asphalt layer may become extremely soft or the waterproof sheet may deteriorate due to the rise in temperature, resulting in lack of durability under severe environmental conditions. .

Further, a method for treating sand with water repellent using the above-mentioned commercially available waterproofing agent (JP-A-62-179588, JP-A-2-171126) or a method for treating sand with silicone oil or alkoxysilane ( US Pat. No. 4,036,658
The water repellent obtained by Japanese Patent Laid-Open No. 1-319585) is used for controlling the water content of farmland in dry areas such as sandy beaches and dunes, and the water repellent property is caused by long-term use under severe environmental conditions. However, the function of controlling the movement of water caused by the capillary phenomenon was not always satisfactory.

Further, in order to produce these water repellent materials, a lot of processing time is required, and the raw materials are expensive and the water content of farmland in dry areas such as sandy beaches and dunes, which are used in large quantities, is required. It was not practical from the purpose of controlling.

[0009]

In view of the above-mentioned problems, the present inventors have earnestly studied various water repellent materials, and as a result, surprisingly, a specific silane compound and an inorganic material were specified. The water-repellent material obtained by the method described above has excellent water repellency and durability by a simple method. Furthermore, when it is used in the soil of agricultural land such as a sandy beach or a dune, especially the particles of sand. The inventors have found that the movement of water in the soil, which is caused by a capillary phenomenon generated in voids formed between them, can be controlled extremely efficiently, and have completed the present invention.

An object of the present invention is to provide a water-repellent material capable of efficiently controlling the water content in soil to solve the above-mentioned problems, and at the same time, to prevent soil from becoming desertified, desert greening,
Not limited to the environmental protection industry such as forest protection and various industrial fields such as agriculture and horticulture, for example, civil engineering,
It is an object of the present invention to provide a wide range of water repellent materials for controlling water content in the technical fields such as ground structures such as construction work.

[0011]

That is, the present invention has the general formula [Chemical Formula 1] as described in claim 1 of the appended claims.

[Chemical 1] (R represents a monovalent hydrocarbon group having 2 or more carbon atoms, a phenyl group or a monovalent hydrocarbon group having a substituent. X
Represents chlorine. n is an integer of 3 or less. ) Is dissolved in an organic solvent, a granular inorganic material is mixed with the silane compound, and the water-repellent material is obtained by filtering, washing with water and drying.

Further, according to the present invention, as described in claim 2 of the claims, the granular inorganic material is sand or silica having an average particle diameter of 10 μm to 10 mm. The water repellent material described above is provided.

Further, according to the present invention, as described in claim 3 of the invention, 0.05 parts of the silane compound represented by the general formula [Chemical Formula 1] is added to 100 parts by weight of the organic solvent.
The water repellent material according to claim 1 or 2, wherein the water repellent material is dissolved in an amount of 1.0 to 1.0 part by weight.

According to the present invention, the silane compound represented by the general formula [Chemical Formula 1] is hexyltrichlorosilane, octyltrichlorosilane or decyltrichlorosilane, as described in claim 4 of the claims. The water repellent material according to claim 1, wherein the water repellent material is provided.

Next, according to the present invention, as described in claim 5 of the claims, the following general formula:

[Chemical 1] (R represents a monovalent hydrocarbon group having 2 or more carbon atoms, a phenyl group or a monovalent hydrocarbon group having a substituent. X
Represents chlorine. n is an integer of 3 or less. The present invention provides a method for producing a water-repellent material obtained by dissolving a silane compound represented by (4) in an organic solvent, mixing the inorganic material in the form of particles, and then filtering, washing with water and drying.

Further, according to the present invention, as described in claim 6 of the claims, the granular inorganic material is sand or silica having an average particle diameter of 10 μm to 10 mm. The present invention provides a method for producing the described water repellent material.

Further, according to the present invention, as described in claim 7 of the invention, 0.05 to 1 of the silane compound represented by the general formula [Chemical Formula 1] is added to 100 parts by weight of the organic solvent. The present invention provides a method for producing a water repellent material according to claim 5 or 6, wherein the water repellent material is dissolved in an amount of 0.0 part by weight.

Further, according to the present invention, the silane compound represented by the general formula [Chemical Formula 1] is hexyltrichlorosilane, octyltrichlorosilane or decyltrichlorosilane. The present invention provides a method for producing the described water repellent material.

Next, the present invention provides a water repellent material for soil improvement comprising the water repellent material according to any one of claims 1 to 4, as described in claim 9 of the claims. Is provided.

Further, the present invention provides the water repellent material for soil improvement according to claim 9, wherein the soil to be improved is a soil formed of sand as described in claim 10 of the claims. To do.

The present invention will be described below. In the present invention, a silane compound satisfying the general formula [Chemical Formula 1] must be used, and this is the first point of the invention found by the present inventor.

In the general formula [Chemical Formula 1] RnSiX4-n, R represents a monovalent hydrocarbon group having 2 or more carbon atoms or a phenyl group or a monovalent hydrocarbon group having a substituent,
X represents chlorine. n is an integer of 1, 2 or 3.

Specific examples of the silane compound represented by the general formula [Chemical Formula 1] include C ₄ H ₉ SiCl ₃ , C ₆ H ₁₃ SiCl
₃ , C ₈ H ₁₇ SiCl ₃ , C ₁₀ H ₂₁ SiC
_{l 3, C 6 H 5 -SiCl} 3, CH 2 = CHSiC
_{l 3, CH 2 = CH (} CH 3) COOC 3 H 6 SiCl
₃ , CF ₃ (CH ₂ ) ₂ SiCl _{3 and the} like.

In particular, when hexyltrichlorosilane, octyltrichlorosilane or decyltrichlorosilane is used, extremely favorable water repellency is exhibited.

Next, the silane compound of the general formula [Formula 1] is dissolved in an organic solvent. Specific examples of the organic solvent include aliphatic hydrocarbons such as hexane and octane, aromatic hydrocarbons such as benzene and toluene, halogenated hydrocarbons such as dichloromethane and carbon tetrachloride, and the like. It is appropriately selected depending on the intended use of the water material.

The mixing ratio of the silane compound of the general formula [Chemical Formula 1] and the organic solvent is such that in order to obtain the water repellent material of the present invention, the silane compound is 0.0 with respect to 100 parts by weight of the organic solvent.
It may be 1 to 3 parts by weight. If the amount is less than 0.01 parts by weight, sufficient water repellency cannot be uniformly given when a large amount of water repellent material is produced, and if the amount is more than 3 parts by weight, it is uneconomical and the gel material floats in water. Is generated in a large amount, which is not preferable.

Particularly, when the silane compound represented by the general formula [Chemical Formula 1] is dissolved in 0.05 to 1.0 parts by weight with respect to 100 parts by weight of the organic solvent, extremely preferable water repellency is exhibited.

Next, the inorganic material is treated using the organic solvent in which the silane compound is dissolved. The inorganic material mixed with the organic solvent is a granular material, and specifically, sand or silica powder having an average particle diameter of 10 μm to 10 mm is preferable.

The method of treating the inorganic material is represented by the general formula:
After mixing with the organic solvent in which the silane compound is dissolved, it may be filtered, washed with water, and dried. More specifically, an inorganic material may be put in a container, an organic solvent may be put in the container to such an extent that the inorganic material is sufficiently dipped, and the mixture may be left standing for a short time.

It is also possible to stir and mix for a short time, preferably using a container equipped with a stirrer.

It is also possible to place the inorganic material to be treated in the filter medium and to flow the above-mentioned organic solvent over the whole inorganic material to perform the treatment. It is also possible to use equipment such as spraying and fluidized beds. The filtration may be appropriately determined depending on the silane compound, organic solvent and inorganic material used.

After filtration, washing is carried out with water in order to surely fix the silane compound of the general formula [Chemical Formula 1] to the surface of the inorganic material and to remove the generated hydrochloric acid and the remaining organic solvent. For washing with water, it is possible to wash the inorganic material on the filter medium with water as it is, or to separate the inorganic material from the filter medium once and wash it separately.

Finally, the washed inorganic material is dried to obtain the water repellent material of the present invention. As a drying method, it is possible to dry in the sun, or it is also possible to perform heat drying by using a blow dryer. The degree of drying may be appropriately determined according to the purpose of use.

The water-repellent material obtained by the present invention is an excellent water-repellent material exhibiting a high degree of water repellency and its purpose of use is not particularly limited, but it is formed of sand such as a beach, a dune, or a desert. It has been confirmed by the present inventor that when used in soil of agricultural land, the movement of water in the soil caused by the capillary phenomenon generated in the voids formed between the sand particles can be controlled very efficiently.

In particular, when the water repellent material obtained by the present invention is used as a water repellent layer in soil, it exerts an extremely excellent function as a waterproof layer and can control the movement of water.

[0036]

EXAMPLES Next, the present invention will be described in more detail by way of examples, but the present invention is not limited thereto.

Example 1 0.3 part by weight of decyltrichlorosilane was dissolved in 100 parts by weight of hexane to prepare a treatment liquid. 1 kg of silica sand having an average particle size of 0.1 mm was placed in a beaker, and 250 g of the prepared decyltrichlorosilane-hexane solution was poured,
It was left for about 1 hour. After standing, it was filtered and washed with about 1 liter of tap water. After draining, the product was dried at 80 ° C. for 24 hours to obtain the water repellent material of the present invention.

Example 2 1.0 part by weight of decyltrichlorosilane was dissolved in 100 parts by weight of hexane to prepare a treatment liquid. 1 kg of silica sand having an average particle size of 0.1 mm was placed in a beaker, and 250 g of the prepared decyltrichlorosilane-hexane solution was poured,
It was left for 1 hour. After standing, it was filtered and washed with about 1 liter of tap water. After draining, the product was dried at 80 ° C. for 24 hours to obtain the water repellent material of the present invention.

Example 3 A treating solution was prepared by dissolving 0.05 part by weight of decyltrichlorosilane in 100 parts by weight of hexane. 1 Kg of silica sand having an average particle diameter of 0.01 mm was placed in a beaker, 250 g of the prepared decyltrichlorosilane-hexane solution was poured, and the mixture was left for about 1 hour. After standing, it was filtered and washed with about 1 liter of tap water. After draining, 80 ℃, 2
It was dried for 4 hours to obtain the water repellent material of the present invention.

Example 4 1.0 part by weight of decyltrichlorosilane was dissolved in 100 parts by weight of hexane to prepare a treatment liquid. Average particle size 1
1 kg of quartz sand of mm was placed in a heker, 250 g of the prepared decyltrichlorosilane-hexane solution was poured, and the mixture was left for about 1 hour. After standing, it was filtered and washed with about 1 liter of tap water. After draining, the product was dried at 80 ° C. for 24 hours to obtain the water repellent material of the present invention.

Example 5 0.5 part by weight of octyltrichlorosilane was dissolved in 100 parts by weight of hexane to prepare a treatment liquid. 1 Kg of silica sand having an average particle diameter of 0.1 mm was placed in a beaker, 250 g of the prepared octyltrichlorosilane-hexane solution was poured, and the mixture was left for about 1 hour. After standing, it was filtered and washed with about 1 liter of tap water. After draining, 80 ℃, 2
It was dried for 4 hours to obtain the water repellent material of the present invention.

Example 6 0.3 parts by weight of hexyltrichlorosilane was dissolved in 100 parts by weight of hexane to prepare a treatment liquid. 1 Kg of silica sand having an average particle diameter of 0.1 mm was placed in a beaker, 250 g of the prepared hexyltrichlorosilane-hexane solution was poured, and the mixture was left for about 1 hour. After standing, it was filtered and washed with about 1 liter of tap water. After draining, 80 ℃, 2
It was dried for 4 hours to obtain the water repellent material of the present invention.

Example 7 0.5 part by weight of decyltrichlorosilane was dissolved in 100 parts by weight of hexane to prepare a treatment liquid. Average particle size 1
1 mm of 0 mm gravel was placed in a beaker, 250 g of the decyltrichlorosilane-hexane solution prepared was poured, and about 1
Left for hours. After standing, it was filtered and washed with about 3 liters of tap water. After draining, the product was dried at 80 ° C. for 24 hours to obtain the water repellent material of the present invention.

Comparative Example 1 0.3 part by weight of decyltrichlorosilane was dissolved in 100 parts by weight of hexane to prepare a treatment liquid. Average particle size 1
Put 1 kg of 5 mm gravel in a beaker and pour 250 g of the prepared decyltrichlorosilane-hexane solution to about 1
Left for hours. After standing, it was filtered and washed with about 1 liter of tap water. After draining, it was dried at 80 ° C. for 24 hours to obtain a water repellent material for comparison.

Comparative Example 2 A treatment liquid was prepared by dissolving 5.0 parts by weight of decyltrichlorosilane in 100 parts by weight of hexane. 1 kg of silica sand having an average particle diameter of 0.1 mm was placed in a beaker, and 250 g of the prepared decyltrichlorosilane-hexane solution was poured,
It was left for about 1 hour. After standing, it was filtered and washed with about 1 liter of tap water. After draining, it was dried at 80 ° C. for 24 hours to obtain a water repellent material for comparison.

Comparative Example 3 0.3 parts by weight of methyltrichlorosilane was dissolved in 100 parts by weight of hexane to prepare a treatment liquid. 1 kg of silica sand having an average particle diameter of 0.1 mm was placed in a beaker, 250 g of the prepared methyltrichlorosilane-hexane solution was poured,
It was left for about 1 hour. After standing, it was filtered and washed with about 1 liter of tap water. After draining, it was dried at 80 ° C. for 24 hours to obtain a water repellent material for comparison.

[Waterproofness Test] Using the water repellent materials produced in the above examples, a waterproofness test in soil was conducted to test the function of controlling the movement of water in the soil. Two
Silica sand 150 with an average particle size of 0.1 mm in a beaker of 00 ml
40 g of tap water was poured into this to form a wet sand layer. On this wet sand layer, 150 g of the water-repellent material of the present invention produced in the above-mentioned example was placed, and allowed to stand in a thermostatic chamber at 25 ° C. and a humidity of 50% for 98 hours, and the weight reduction was measured. It was judged that the better the waterproofness in the soil, the better.

As a result, in a comparative test in which 150 g of the inorganic material silica sand was directly placed on the wet sand layer without using the water repellent material of the present invention, the average particle diameter of the inorganic material silica sand was 0.1 mm, 0. The weight loss of the comparative test example of 0.01 mm was 25.4 g and 31.6 g, respectively, whereas the waterproof property using the water repellent material produced in Examples 1, 2, 3, 4, 5, 6, and 7 was used. In the test, each weight loss was 4.
9g, 4.2g, 5.6g, 5.4g, 4.3g, 4.
It was 7 g and 8.5 g, and exhibited extremely good waterproofness.

In the waterproof test using the water repellent material produced in Comparative Example 1, the weight loss was 28.3 g, which was a bad result. In Comparative Example 2, the weight loss was 6.
2g was relatively good, but when washing with tap water,
The workability was poor because of the formation of a large amount of gel, the adhesion of silica sand and stickiness. In Comparative Example 3,
The weight loss was 10.3 g, which was relatively bad.

[0050]

According to the present invention, a water repellent material having excellent water repellency and durability, which can be applied to a wide range of applications, is provided by a simple method.

In addition, when the water-repellent material of the present invention is used for the soil of agricultural land such as sandy beach and dunes, the migration of water in the soil caused by the capillary phenomenon particularly in the voids formed between the sand particles is extremely reduced. It can be controlled efficiently.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Takao Oshima Daikaku, Nakakubiki-gun, Niigata Pref. 28, Nishi-Fukushima 1 Shin-Etsu Kasei Co., Ltd. Naoetsu Plant (72) Inventor Shirataki Takumi, Nakakubiki-gun, Niigata Pref. No. 28, Nishi-Fukushima 1 Shin-Etsu Chemical Co., Ltd. Naoetsu factory

Claims (10)

[Claims] 1. RnSiX4-n (R represents a monovalent hydrocarbon group having 2 or more carbon atoms or a phenyl group or a monovalent hydrocarbon group having a substituent.
Represents chlorine. n is an integer of 3 or less. ) The water-repellent material obtained by dissolving the silane compound represented by the formula (1) in an organic solvent, mixing this with a granular inorganic material, and then filtering, washing with water, and drying. 2. The water repellent material according to claim 1, wherein the granular inorganic material is sand or silica having an average particle diameter of 10 μm to 10 mm. 3. A silane compound represented by the general formula [Chemical Formula 1] in an amount of 0.05 to 1.0 with respect to 100 parts by weight of an organic solvent.
3. The water repellent material according to claim 1 or 2, wherein the water repellent material dissolves in parts by weight. 4. The water repellent according to any one of claims 1 to 3, wherein the silane compound represented by the general formula [Chemical Formula 1] is hexyltrichlorosilane, octyltrichlorosilane or decyltrichlorosilane. material 5. RnSiX4-n (R represents a monovalent hydrocarbon group having 2 or more carbon atoms or a phenyl group or a monovalent hydrocarbon group having a substituent.
Represents chlorine. n is an integer of 3 or less. The method for producing a water-repellent material obtained by dissolving the silane compound represented by the formula 1) in an organic solvent, mixing the inorganic material in the form of particles, and then filtering, washing with water and drying. 6. The method for producing a water repellent material according to claim 5, wherein the granular inorganic material is sand or silica having an average particle size of 10 μm to 10 mm. 7. A silane compound represented by the general formula [Chemical Formula 1] in an amount of 0.05 to 1.0 with respect to 100 parts by weight of an organic solvent.
7. The method for producing a water repellent material according to claim 5 or 6, characterized in that it is dissolved in parts by weight. 8. The water repellent according to claim 5, wherein the silane compound represented by the general formula [Chemical Formula 1] is hexyltrichlorosilane, octyltrichlorosilane or decyltrichlorosilane. Material manufacturing method 9. A water-repellent material for soil improvement comprising the water-repellent material according to claim 1. 10. The water repellent material for soil improvement according to claim 9, wherein the soil to be improved is a soil formed of sand.