JP3235864B2 - Inorganic oxide colloid particles - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an inorganic oxide colloid particle modified with a chain polymer silane coupling agent.

[0002]

2. Description of the Related Art Conventionally, surface-modified inorganic oxide particles have been in high demand for use as fillers for improving the surface lubricity of synthetic resin films such as magnetic tapes. Development is taking place. For example, Japanese Patent Publication No. 2-1090 proposes powdery silica which is treated with a silylating agent such as a silane of a low molecular weight chain compound or aromatic compound and can be uniformly dispersed in an organic solvent. Japanese Patent Application Laid-Open No. 3-271114 proposes silica particles modified with a multipoint-bonding polymer silylating agent and capable of being uniformly redispersed in an organic solvent.

[0003] However, silica particles treated with the above-mentioned multipoint-bonding type polymer silylating agent or a silylating agent having a low molecular weight and a short molecular chain have an adhesive property with a synthetic resin when used as a filler of a synthetic resin film. However, there is a problem that the silica particles are easily dropped. Attempts have also been made to modify inorganic oxide particles with long chain polymer silane coupling agents, but inorganic oxide colloid particles that are monodispersible in organic solvents are not yet known. .

[0004]

An object of the present invention is to provide an inorganic oxide colloidal particle modified with a single-point chain type chain polymer silane coupling agent which is homogeneously monodispersible in an organic solvent and has excellent stability. Is to do.

[0005]

SUMMARY OF THE INVENTION The inorganic oxide colloid particles of the present invention are modified with a single-point silane coupling agent represented by the following general formula.

Embedded image [Wherein, m and n are integers of 0 to 2, l is an integer of 1 to 3, and a value satisfying 1 + m + n = 3. R ¹ ,
R ² and R ³ are hydrogen or an alkyl group having 1 to 4 carbon atoms. X
It is the copolymerization of a polymerizable or different monomers of the same monomer
Thus, the obtained number average molecular weight is 1,000 to 200,
An atomic group mainly comprising a 000 chain polymer compound. ]

[0006]

DETAILED DESCRIPTION OF THE INVENTION In the general formula of the silane coupling agent for modifying the inorganic oxide colloid particles of the present invention, the number average molecular weight of the chain high molecular compound which is a main component of the atomic group X is 1, 5,000 to 150,000, especially 10,000 to 200,000.
It is preferably in the range of 000 to 100,000.
When the number average molecular weight is smaller than 1,000, the atomic group X
When the inorganic compound colloid particles modified with such a silane coupling agent are used as fillers in a synthetic resin because of their short molecular chains, the adhesion to the synthetic resin is poor, and a so-called anchor effect is obtained. I can't. On the other hand, if the number average molecular weight is larger than 200,000, the modified inorganic oxide colloid particles are not preferred because monodispersibility in an organic solvent is deteriorated and aggregated particles are increased.

The atomic group X has --Si at the other terminal and side chain.
(OR) ₃ groups, wherein R represents hydrogen or an alkyl group. ]. That is, the silane coupling agent is of a single-point bond type. There is no particular limitation on the chain polymer compound which is the main constituent element of the atomic group X other than the above, and a general chain polymer obtained by polymerization of the same monomer or copolymerization of different monomers. Compounds, for example, polyethylene,
Polypropylene, polystyrene, polyvinyl chloride, polyvinylidene chloride, polyvinyl acetate, polyvinyl acetal, polymethyl methacrylate, polyacrylic acid, polymethyl acrylate, polyacrylonitrile, polyacrylamide, polytetrafluoroethylene, polychlorotrifluoroethylene, Polyvinylidene fluoride, polybutadiene, polybutene, polyisoprene, polychloroprene, propylene / ethylene copolymer, ethylene / vinyl acetate copolymer, vinylidene chloride / vinyl chloride copolymer, aliphatic polyamide, aromatic polyamide, polycarbonate, polyacrylate, polyethylene terephthalate, aromatic Examples thereof include polyester, polyethylene oxide, and polypropylene oxide.

The silane coupling agent represented by the above general formula is prepared by introducing a low-molecular-weight silane coupling agent into the chain polymer compound. The introduction can be performed by a known method.For example, a compound having a functional group such as a carboxyl group is introduced to one end of a chain polymer compound, and then a low-molecular-weight silane coupling agent having an amino group is added. Prepare by reacting. Therefore,
The chain high molecular compound is bonded to the silicon atom via the low molecular compound having the above functional group, and the atomic group X is composed of the chain high molecular compound and the low molecular compound. In the above general formula, R ¹ , R ² and R ³ specifically represent hydrogen or a methyl group, an ethyl group, a propyl group or a butyl group.

In the present invention, as the inorganic oxide colloid particles to be modified, generally known inorganic oxide colloid particles can be used, and SiO ₂ , Al ₂ O ₃ ,
In addition to colloidal oxide particles such as TiO ₂ , ZrO ₂ and Fe ₂ O ₃ , SiO ₂ .Al ₂ O ₃ , SiO ₂ .B ₂ O
₃ , TiO ₂ · CeO ₂ , SnO ₂ · Sb ₂ O ₃ , Si
O ₂ · Al ₂ O ₃ · TiO ₂ , TiO ₂ · CeO ₂ · S
Examples thereof include composite inorganic oxide colloid particles such as iO ₂ . Further, inorganic colloid particles such as MgF ₂ and CaF ₂ can be used.

[0010] The average particle diameter of the inorganic oxide colloidal particles is desirably 1000 nm or less, preferably in the range of 7 to 800 nm. It is also desirable to use the composite oxide sol described in Japanese Patent Application No. 3-83578 previously filed by the applicant of the present application.

Next, a method for modifying the inorganic oxide colloid particles with the above-mentioned chain polymer silane coupling agent will be described. The silane coupling agent is dissolved in a suitable organic solvent to form a dispersion of 1 to 20% by weight,
This solution is added to a 1 to 40% by weight inorganic oxide colloid solution using an organic solvent prepared as a dispersion medium by a usual method. If necessary, a catalyst such as an acid or an alkali is added to the solution, and the solution is heated to room temperature to 200 ° C.,
Let react for hours.

Thereafter, the solvent of the colloid solution is evaporated,
If removed, it can be a powder of inorganic oxide colloid particles modified with a chain polymer silane coupling agent, or, if solvent replacement is performed by a commonly used method,
A colloid solution containing inorganic oxide colloid particles modified with a chain polymer silane coupling agent using a desired organic solvent as a dispersion medium can also be prepared. The modified inorganic oxide colloid particles of the present invention include colloid particles modified with a low molecular weight silane coupling agent together with a chain polymer silane coupling agent.

When binding the silane coupling agent to the surface of the inorganic oxide colloid particles, a solubility parameter (hereinafter referred to as SP value) δ _S of an organic solvent which is a dispersion medium of the inorganic oxide colloid solution, between the SP values [delta] _P of the main components of the atomic group X of the silane coupling agent chain polymer compound, be a combination of organic solvent and a silane coupling agent which satisfies the following relationship preferable. However, the unit of each SP value is [cal / cm ³ ]
^Use a value represented by ^1/2 . 1 ≦ │δ _S −δ _P │ ≦ 5

If the above relational expression is satisfied, the chain polymer silane coupling agent becomes a poor solvent for the dispersion medium of the colloid solution and becomes unstable. Therefore, if the chain polymer silane coupling agent is hydrolyzed, even if the amount of the coupling agent with respect to the colloid particles is small, it is deposited on the surface of the colloid particles. it can. Further, the stability of the colloidal particles is not impaired, which is preferable.

When the difference in SP value is smaller than 1, the silane coupling agent becomes a good solvent for the dispersion medium of the colloid solution, and is dispersed in a stable state. At this time,
Even when the chain polymer silane coupling agent is hydrolyzed, it is hydrolyzed in the dispersion medium and does not precipitate on the surface of the colloid particles, and the ratio of reacting with the surface of the colloid particles is extremely small. Therefore, in order to bond the silane coupling agent to the surface of the colloid particles, a large amount of the silane coupling agent must be used for the colloid particles, and
In a dispersion medium containing a large amount of a silane coupling agent,
If the ratio of the modified silane coupling agent is small, adverse effects such as impairment of the stability of the colloid particles occur, which is not preferable.

On the other hand, if the difference in SP value is larger than 5, the silane coupling agent does not dissolve in the colloid solution, so that micelles of the silane coupling agent are formed and reacted with the surface of the colloid particles. Have difficulty. Further, even if it can be modified, the dispersion stability of the colloid particles is significantly impaired, which is not preferable. The SP values of organic solvents and chain polymer compounds are those of Po.
Since these are described in the Polymer Handbook (Wiley Interscience), a combination of a desired organic solvent and a chain polymer silane coupling agent can be obtained by using these values.
In addition, a colloid solution using a desired organic solvent as a dispersion medium is
It can be prepared by a known method such as solvent replacement using an ultrafiltration membrane.

In the present invention, the amount of the silane coupling agent that modifies the inorganic oxide colloid particles is preferably in the range of 0.5 to 30 parts by weight based on 100 parts by weight of the colloid particles. If the amount of the coupling agent is less than 0.5 part by weight, a desired anchor effect cannot be obtained even if the modified inorganic oxide colloid particles are added as a filler to a synthetic resin or the like. On the other hand, when the amount exceeds 30 parts by weight, only the chain polymer compound layer formed on the surface of the colloid particles becomes dense, and the anchor effect is not changed, which is not economical.

[0018]

【Example】

1. Synthesis of chain polymer silane coupling agent [Synthesis Example 1] Number average molecular weight 5.0 × 1 in a four-necked flask
0 ³ polyoxyethylene ether (POE) 2
After adding 0 g and 8 g of succinic anhydride and degassing to make a nitrogen atmosphere, 120 g of 1,2-dichloroethane was used as a solvent.
And 1 g of pyridine as a catalyst were added, followed by stirring at 80 ° C. for 72 hours. After stirring, perform suction filtration, collect the filtrate,
Subsequently, pyridine and 1,2-dichloroethane in the filtrate were removed by evaporation using an evaporator. The obtained white powder was dissolved by adding 40 g of water, and then washed by adding diethyl ether. The reaction product in the aqueous phase was extracted with chloroform, separated from the aqueous phase, and then evaporated to remove chloroform.Then, benzene was added and dissolved, diethyl ether was added, and ice-cooled white precipitate was purified. I got
The precipitate was filtered by suction and dried under reduced pressure to obtain polyoxyethylene methyl succinate having a carboxyl group.

10 g of polyoxyethylene methyl succinate obtained by the above operation was added to an eggplant-shaped flask together with 1.06 g of dicyclohexylcarbodiimide (catalyst) using 400 g of chloroform as a solvent, and stirred for 2 hours while cooling with ice. After stirring, 1.36 g of aminopropyltriethoxysilane was added, and the mixture was allowed to react at 5 ° C. for 24 hours. Next, chloroform was removed by evaporation, and benzene was added to the reaction product to dissolve it. Further, diethyl ether was added and the mixture was cooled with ice to obtain a purified white precipitate. This precipitate was dissolved in ethyl acetate, and the undissolved precipitate was removed by suction filtration. Then, ethyl acetate in the filtrate was removed by evaporation using an evaporator, and the POE coupling agent was obtained by drying under reduced pressure.

[Synthesis Example 2] A three-necked flask was degassed and then made into a nitrogen atmosphere.
-0.4 g of mercaptopropionic acid and 0.82 g of 2,2'-azobisisobutyronitrile and 40 g of tetrahydrofuran dried by a conventional method were charged as solvents,
After stirring for 6 hours while maintaining the temperature at 70 ° C., the reaction was continued, and the solvent was removed by evaporation to obtain a white powder. Benzene was added to this white powder to dissolve it, and methanol was further added thereto, followed by cooling on ice to produce a purified white precipitate. The precipitate was suction-filtered and dried under reduced pressure, and 16.3 g of polystyrene (PSt) having a carboxyl group at the terminal.
I got As a result of measuring the obtained PSt by gel permeation chromatography (GPC), the number average molecular weight was 1.2.
× 10 ⁴ .

5.75 g of PSt obtained by the above operation was added to an eggplant-shaped flask together with 0.1 g of dicyclohexylcarbodiimide (catalyst) using 100 g of chloroform as a solvent, and stirring was continued for 2 hours while cooling with ice. After stirring, 0.13 g of aminopropyltriethoxysilane was added thereto, and the mixture was allowed to react at 5 ° C. for 24 hours. Next, after removing tetrahydrofuran by evaporation, benzene was added to the reaction product to dissolve it, and then methanol was added thereto, followed by cooling with ice to obtain a purified white precipitate. This precipitate was dissolved in ethyl acetate, and the undissolved precipitate was removed by suction filtration. Then, the ethyl acetate in the filtrate was removed by evaporation using an evaporator, and dried under reduced pressure to obtain a PSt coupling agent.

[Synthesis Example 3] A three-necked flask was degassed and then made into a nitrogen atmosphere. Distilled under reduced pressure, 5 g of methyl methacrylate, 0.14 g of 3-mercaptopropionic acid and 0.2 g of 2,2'-azobisisobutyronitrile. 07g,
10 g of tetrahydrofuran dried by a conventional method was charged as a solvent, and the reaction was continued by stirring for 3 hours while maintaining the temperature at 60 ° C. Then, the solvent was removed by evaporation to obtain a white powder. Benzene was added to this white powder to dissolve it, hexane was further added, and the mixture was ice-cooled to produce a purified white precipitate. The precipitate was filtered by suction and dried under reduced pressure to obtain 3.3 g of polymethyl methacrylate (PMMA) having a carboxyl group at a terminal. As a result of measuring the obtained PMMA by gel permeation chromatography (GPC),
The number average molecular weight was 8.5 × 10 ³ .

2 g of PMMA obtained by the above operation was added to an eggplant-shaped flask together with 0.049 g of dicyclohexylcarbodiimide (catalyst) using 100 g of chloroform as a solvent, and stirring was continued for 2 hours while cooling with ice. After stirring, 0.13 g of aminopropylethoxysilane was added thereto and added at 5 ° C.
For 24 hours. Next, chloroform was removed by evaporation, and benzene was added to the reaction product to dissolve it, and hexane was further added, followed by cooling with ice to obtain a purified white precipitate. This precipitate was dissolved in ethyl acetate, the undissolved precipitate was removed by suction filtration, and the ethyl acetate in the filtrate was removed by evaporation using an evaporator.
The PMMA coupling agent was obtained by drying under reduced pressure.

[Synthesis Example 4] After degassing the three-necked flask, the atmosphere was changed to a nitrogen atmosphere, and 15 g of vinyl acetate distilled under reduced pressure and 0.15 of 4,4'-azobis (4-cyanoisovaleric acid) were added.
and 5 g of methanol as a solvent.
After the reaction was continued for 4 hours while maintaining the temperature at 0 ° C., the solvent was removed by evaporation to obtain a white powder. Dioxane was added to this white powder to dissolve it, and diethyl ether was further added thereto, followed by cooling with ice to produce a purified white precipitate.
The precipitate is suction-filtered and dried under reduced pressure to obtain 12.1 g of polyvinyl acetate (PVAc) having a carboxyl group at the terminal.
I got As a result of measuring the obtained PVAc by gel permeation chromatography (GPC), the number average molecular weight was 1.3.
× 10 ⁵ .

6 g of PVAc obtained by the above operation was added to an eggplant-shaped flask together with 100 g of chloroform, and stirring was continued for 2 hours while cooling with ice. After stirring, 0.026 g of aminopropyltriethoxysilane was added thereto, and the mixture was allowed to react at 5 ° C. for 24 hours. Then, after removing chloroform by evaporation, dioxane was added to the reaction product to dissolve it,
Further, diethyl ether was added thereto, and the mixture was cooled with ice to obtain a purified white precipitate. This precipitate was dissolved in ethyl acetate, the undissolved precipitate was removed by suction filtration, and the ethyl acetate in the filtrate was removed by evaporation using an evaporator.
The PVAc coupling agent was obtained by drying under reduced pressure.

2. Modification of Inorganic Oxide Colloidal Particles with Silane Coupling Agent Example 1 Average Particle Diameter of 50 Using Ethanol as Dispersion Medium
4 g of the POE silane coupling agent obtained in Synthesis Example 1 was dissolved in 32 g of methanol while stirring at room temperature 200 g of a colloid solution (oxide concentration: 20% by weight) containing 0 nm silica-alumina composite oxide colloid particles. The solution was added over 1 hour. Next, this colloid solution was kept at 30 ° C., and 40 g of 28% by weight aqueous ammonia was added over 30 minutes while stirring, and further stirred for 1 hour. Thereafter, the colloid solution was heated to 60 ° C. and aged for 1 hour to obtain a colloid solution in which silica-alumina composite oxide colloid particles modified with a POE silane coupling agent were monodispersed.

Next, 100 g of ethylene glycol was added to the colloid solution, and the solvent was evaporated by heating at 80 ° C. with a rotary evaporator to replace the solvent. POE having a solid concentration of 30% by weight using ethylene glycol as a dispersion medium was used. A stable colloid solution containing silica-alumina composite oxide colloid particles modified with a silane coupling agent was obtained.

The properties of the colloid solution thus prepared were measured and observed as follows. (1) Average particle diameter of inorganic oxide colloid particles Measured by an ultracentrifugal automatic particle size distribution analyzer. (2) Modification Amount of Chain Polymeric Silane Coupling Agent The colloid solution was subjected to a small centrifuge to separate colloid particles, and the obtained particles were dried at 150 ° C. for 20 hours.
Subsequently, the sample was subjected to thermogravimetric analysis for 150 minutes.
The weight loss at １０００1000 ° C. was determined as a percentage of the amount of the silane coupling agent.

(3) Stability of Colloid Solution The colloid solution was allowed to stand for one week and visually observed.・ ・ ・: No precipitate was observed △: A slight precipitate was observed ×: A large amount of precipitate was observed (4) Redispersibility Colloid particles obtained by drying the colloid solution under reduced pressure were It was again dispersed in the original solvent to prepare a colloidal solution having a concentration of 10% by weight, and the stability was similarly visually observed.

Table 1 shows the conditions for preparing the colloid solution and the silane coupling (coupler), and Table 2 shows the properties of the colloid solution such as the above measurement results and evaluation results.
FIG. 1 shows a scanning electron micrograph of the colloid particles modified with the chain polymer silane coupling agent obtained in Example 1, and FIG. 2 shows a scanning electron micrograph of the colloid particles before modification. Show. In FIG. 1, colloidal particles modified with a chain polymer silane coupling agent that appeared to be aggregated were redispersed in a solvent to obtain a stable colloidal solution in which the colloidal particles were monodispersed.

Example 2 Colloidal solution containing silica colloidal particles having an average particle diameter of 180 nm using N, N-dimethylformamide as a dispersion medium (oxide concentration: 40% by weight)
In the same manner as in Example 1, except that POE was used, POE having an ethylene concentration of 25% by weight and a dispersion medium of ethylene glycol was used.
A colloid solution containing silica colloid particles modified with a silane coupling agent was prepared. Tables 1 and 2 show the preparation conditions and properties of the colloid solution.

Example 3 A colloid solution containing colloidal particles of titania / ceria composite oxide having an average particle diameter of 90 nm using N, N-dimethylformamide as a dispersing medium (manufactured by Catalyst Chemical Industry Co., Ltd .; Optics, oxides) 100 g (concentration 10% by weight) was stirred at room temperature, and
A solution obtained by dissolving 0.85 g of the PSt silane coupling agent obtained in 2 above in 27.5 g of xylene was added over 30 minutes. This colloid solution was kept at 50 ° C., and 60 g of 0.5% by weight hydrochloric acid was added over 1 hour while stirring, and the mixture was further stirred for 2 hours, and then cooled to room temperature. Next, while adding styrene to the colloid solution, the solvent is replaced with an ultrafiltration membrane, and a colloid containing titania-ceria composite oxide colloid particles modified with a PSt silane coupling agent using styrene as a dispersion medium is used. A solution was prepared. Tables 1 and 2 show the preparation conditions and properties of the colloid solution.

[Example 4] A colloid solution containing titania colloid particles having an average particle diameter of 200 nm using N-methylpyrrolidone as a dispersion medium (manufactured by Catalyst Chemical Industry Co., Ltd .; Queen Ti
tanic, oxide concentration 20% by weight) and P obtained in Synthesis Example 3
A colloid containing titania colloid particles modified with a PMMA silane coupling agent after treating in the same manner as in Example 3 except that 0.4 g of an MMA silane coupling agent was used, followed by solvent replacement with terahydrofuran A solution was prepared. Tables 1 and 2 show the preparation conditions and properties of the colloid solution.

Example 5 The procedure of Example 5 was repeated except that 100 g of a colloidal solution (oxide concentration: 10% by weight) containing silica-alumina composite oxide colloidal particles having an average particle diameter of 300 nm using normal propyl alcohol as a dispersion medium was used. 4
After treating in the same manner as in
A colloid solution containing silica-alumina composite oxide colloid particles modified with an MMA silane coupling agent was prepared. Tables 1 and 2 show the preparation conditions and properties of the colloid solution.

Example 6 To 300 g of a colloidal solution (oxide concentration: 10% by weight) containing silica colloid particles having an average particle diameter of 400 nm using methyl alcohol as a dispersion medium, 30 g of 1% by weight ammonia water was added. While maintaining the colloid solution at 25 ° C. and stirring, a solution obtained by dissolving 7.3 g of the PVAc silane coupling agent obtained in Synthesis Example 4 in 50 g of acetone was mixed with a solution of 5 wt% ammonia water 40%.
g and 2.2 g of tetraethoxysilane (manufactured by Tama Chemical; SiO ₂ concentration: 28% by weight) were simultaneously added over 30 minutes.

Next, the colloid solution was aged at 50 ° C. for 4 hours, and then cooled to room temperature. Subsequently, 128 g of ethylene glycol was added to the colloid solution, and the mixture was heated to 100 ° C. with a rotary evaporator to replace the solvent.
A colloid solution containing silica colloid particles modified with a PVAc silane coupling agent using ethylene glycol as a dispersion medium was prepared. Tables 1 and 2 show the preparation conditions and properties of the colloid solution.

[0037]

Table 1 Preparation Conditions colloidal solution mosquitoes flops la over S P value particle size dispersion medium type M _n ratio δ _P δ _S Δδ Example ^{1 500nm Et POE 5 × 10 3} 0.100 14.6 12.7 1.9 Example 2 180 DMF POE 5 × 10 ³ 0.125 14.6 12.1 2.5 Example 3 90 DMF PSt 1.2 × 10 ⁴ 0.085 9.3 12.1 2.8 Example 4 200 NMP PMMA 8.5 × 10 ³ 0.020 9.3 11.3 2.0 Example 5 300 Pr PMMA 8.5 × 10 ³ 0.040 9.3 11.9 2.6 Example 6 400 Me PVAc 1.3 × 10 ⁵ 0.243 9.6 14.5 4.9

(Remarks of Table 1) In the column of "dispersion medium",
Me: methanol, Et: ethanol, DMF: N, N-dimethylformamide, NMP: N-methylpyrrolidone, Pr:
Indicates propanol. In the "coupler" column,
M _n : number average molecular weight of chain polymer compound, ratio: weight ratio of silane coupling agent to colloid particles.
The unit of the SP value is a value represented by [cal / cm ³ ] ^1/2 .

[0039]

[Table 2] Properties of colloid solution Dispersion medium solids concentration modification amount stability redispersibility Example 1 Eg 30 wt% 10.2 wt% ○ ○ Example 2 Eg 25 12.3 ○ ○ Example 3 St 20 8.2 ○ ○ Example 4 THF 15 2.3 ○ ○ Example 5 Tol 20 3.6 ○ ○ Example 6 Eg 20 23.1 ○ ○

(Remarks in Table 2) In the column of "dispersion medium",
Eg: ethylene glycol, St: styrene, THF: tetrahydrofuran, Tol: toluene.

[0041]

[Effect] The colloidal particles of inorganic oxide modified with the chain polymer silane coupling agent of the present invention include alcohols, ketones, ethers, aromatic hydrocarbons, and aliphatic hydrocarbons.
Since it is homogeneously dispersed in most organic solvents, it can be used as a filler for modifying various resins, a reactant with various resins, and the like.

In particular, since the inorganic oxide colloid particles have a long molecular chain, when used as an additive (filler) to a synthetic resin, they exhibit an excellent anchor effect in the synthetic resin, Can be improved to the utmost. In addition, antistatic, blocking prevention,
Supporting fillers for organic substances, pigments or metals, cosmetics,
Additives for improving the feeling of toner and fiber, waterproofness or anti-friction, auxiliary agents such as lubricants, smoothing agents, defoamers, fillers for paints, hard coating agents for resins, and imparting slip to steel plates Agent,
It is also suitable for use in applications such as.

[Brief description of the drawings]

FIG. 1 is a scanning electron micrograph of colloid particles modified with a chain polymer silane coupling agent obtained in Example 1.

FIG. 2 is a scanning electron micrograph of colloid particles before being modified.

──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Hiroyasu Nishida 13-2 Kitaminato-cho, Wakamatsu-ku, Kitakyushu-shi, Fukuoka Prefecture Inside the Wakamatsu Plant (72) Inventor Toshiro Komatsu Kita-Kyushu-shi, Fukuoka 13-2 Minatomachi Inside the Wakamatsu Plant of Catalysts and Chemicals Co., Ltd. (56) References JP-A-3-271114 (JP, A) JP-A-60-219288 (JP, A) JP-A-60-120703 (JP, A) JP-A-3-70778 (JP, A) JP-B-57-1483 (JP, B2) U.S. Pat. No. 4,759,866 (US, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) C09C 3 / 12 C01B 33/149 C08K 9/06 B01J 13/00

Claims (2)

(57) [Claims] 1. An inorganic oxide colloid particle modified with a single-point bond type silane coupling agent represented by the following general formula. Embedded image [Wherein, m and n are integers of 0 to 2, l is an integer of 1 to 3, and a value satisfying 1 + m + n = 3. R ¹ , R ² and R ³ are hydrogen or an alkyl group having 1 to 4 carbon atoms. X represents the polymerization of the same monomer or the copolymerization of different monomers.
Number average molecular weight obtained by polymerization is 1,000 to 2
An atomic group mainly composed of a 000 chain polymer compound. ] 2. The method according to claim 1, wherein the chain polymer compound is polyethylene, polypropylene, polystyrene, polyvinyl chloride,
Polyvinylidene chloride, polyvinyl acetate, polyvinyl acetal, polymethyl methacrylate, polyacrylic acid, polymethyl acrylate, polyacrylonitrile, polyacrylamide, polytetrafluoroethylene, polychlorotrifluoroethylene, polyvinylidene fluoride, polybutadiene, polybutene, Polyisoprene, polychloroprene, propylene / ethylene copolymer, ethylene / vinyl acetate copolymer, vinylidene chloride / vinyl chloride copolymer, aliphatic polyamide, aromatic polyamide, polycarbonate, polyacrylate, polyethylene terephthalate, aromatic polyester, polyethylene oxide,
The inorganic oxide colloid particles according to claim 1, which are any of polyvinylene oxide.