JPH05301969A - Production of resin particle - Google Patents

Abstract

PURPOSE:To obtain a method for producing resin particles in which components of inner layer and surface layer of these particles are formed of different resins. CONSTITUTION:The objective method for producing resin particles different in resin composition between their inner layer and surface layer is characterized by dissolving the first resin and the second resin in the first solvent, adding the second solvent to the solution to deposit the first resin particles and then adding the third solvent thereto to deposit the second resin particles on the surface of the first resin particles.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing resin particles used in paints, adhesive materials, electronic materials, optical materials and the like. The present invention relates to a method for producing resin particles.

[0002]

2. Description of the Related Art A method for producing resin particles (composite particles) made of resins in which the inner layer and surface layer of the particles have different components
(1) Particles II ′ formed of resin I and particles II ′ formed of resin I, the particle size of which is smaller than that of particles I ′.
And (2) are brought into contact with each other in an air stream to form the particle inner layer with the resin I, and the particle surface layer is formed with the resin II (high-speed air stream impact method), (2) polymerization of the monomer raw material 1 in a solvent To produce particles I ′ having an inner layer formed of resin I,
Next, there is a method of polymerizing the monomer raw material 2 on the surface of the particle I ′ to form a surface layer of the resin II (seed polymerization method).

[0003]

Among the above-mentioned conventional methods, (1) the high-speed air current impact method has the troublesome handling of handling solid powder particles in the air,
(2) Since the seed polymerization method is manufactured by suspending in a specific solvent (limited to a solvent that does not dissolve the polymerized precipitation particles),
In order to newly suspend it in a solvent according to any purpose and use, there is a drawback that it is necessary to separate and remove the specific solvent.

In view of the above-mentioned state of the art, the present invention has no drawbacks as in the conventional method, and produces resin particles (particle diameter is about 0.1 to 10 μm) suspended in a solvent according to any purpose and application. It is intended to provide a new method of doing so.

[0005]

According to the present invention, a first resin and a second resin are dissolved in a first solvent, and a second solvent is added to this solution to precipitate first resin particles, Next, a third solvent is added to deposit the second resin particles on the surface of the first resin particles, which is a method for producing resin particles having different resin compositions in the inner layer and the surface layer.

Hereinafter, the present invention will be described in more detail with reference to FIGS. The present invention includes the following Step 1, Step 2, and Step 3
Composed of.

Step 1: Two kinds of resin (Resin I,
Resin II) is added, and the resin I and the resin II are dissolved in the solvent A by means such as stirring or heating (see FIG. 1).
"I" in FIG. 1 shows a state in which the resins I and II are both dissolved in the solvent A, that is, the final state of the dissolving step. At this time, a crystal precipitation nucleus material and a crystal dispersant can be added at the same time, if necessary.

Step 2: Next, the solvent B is gradually added to the mixed solution obtained in Step 1 while cooling the mixed solution, if necessary, to precipitate fine particles I ′ consisting of the resin I only.
At this time, the solvent B is the solvent A, the solvent B, the resin I, the resin II.
The dissolution characteristics of the above are selected from those satisfying the state diagram shown in FIG. Solvent B is added to the final state "a" of the dissolution process of FIG.
It is shown in FIG. 1 that the resin I is precipitated and that the resin II is not precipitated when the is added.
1 and 2 indicate the final state of the resin I deposition step. Further, "d" indicates a solubility curve in the absence of solvent C.

Step 3: Next, the solvent C is added to the mixed solution obtained in Step 2 while cooling the mixed solution, if necessary, to precipitate the resin II, and at the same time, to form the resin I. The fine particles I ′ are attached to the surface. At this time, the solvent C is selected from those in which the solubility characteristics of the solvent A, the solvent B, the solvent C, the resin I, and the resin II satisfy the state diagrams shown in FIGS. 3 and 4. FIG. 3 and FIG. 4 are diagrams showing a state change when the solvent C is added after the completion of the precipitation step of the resin I. FIG. 3 relates to the resin I and the resin C is added even if the solvent C is added. I
FIG. 4 is a diagram showing that the deposited state is maintained, and FIG. 4 is a diagram showing that the resin II in the dissolved state changes to the deposited state when the solvent C is added. "Indicates the final state when solvent C is added.

The shaded areas in FIGS. 1 to 4 indicate that the resin is deposited in this area, and the outside of the shaded areas is the area where the resin melts.

[0011]

The two layers of resin dissolved in the solvent are deposited in stages, whereby the inner layer and the surface layer of the particles can be formed of different resins. Further, the degree of heteromorphism of the particles can be adjusted by adjusting the ratio of the amount of the resin II to the resin I forming the inner layer or by adjusting the deposition rate of the resin II.

Further, as the solvent A, B, C, a solvent can be selected according to any purpose and application, so that the labor for separating and removing the specific solvent used for the above-mentioned polymerization or the like can be omitted. ..

[0013]

【Example】

(Example 1) ○ Step 1: Styrene-based resin 20 to 1,000 g of toluene
0 g and 210 g of acrylic acid ester-based resin were added, and this mixed solution was heated to 100 ° C. to dissolve these resins. Next, 80 g of carbon black as a crystal nucleus and 8 g of a nonionic dispersant (sorbitan) were added to this mixed solution, and after sufficiently stirring, the mixture was cooled to 25 ° C.

Step 2: Next, 470 g of isopropyl alcohol was gradually added to this mixed solution to deposit fine particles of styrene resin.

Step 3: Next, 1,300 g of isoparaffinic hydrocarbon was gradually added to this mixed solution to deposit an acrylic ester resin.

When the resin particles were separated from the mixed liquid finally obtained by the above operation, dried and observed with a scanning electron microscope, resin particles of about 1 μm were found.

Example 2 Step 1: To 1,000 g of toluene, 200 g of methacrylic acid ester resin and 200 g of acrylic acid ester resin
After adding g, it heated to 80 degreeC and these resins were dissolved. Next, to this liquid, carbon black 80
g and 8 g of a nonionic dispersant were added and sufficiently stirred to disperse, and then cooled to 20 ° C.

Step 2: Next, 700 g of isopropyl alcohol was gradually added to this mixed solution to deposit fine particles of a methacrylic ester resin.

Step 3: Next, 1,500 g of isoparaffinic hydrocarbon was gradually added to this mixed solution to deposit an acrylic ester resin.

As a result of observing the obtained particles with a scanning electron microscope in the same manner as in Example 1, resin particles of about 1.5 μm were observed.

[0021]

EFFECTS OF THE INVENTION (1) Non-spherical resin particles suspended in a solvent can be produced according to any purpose and application. (2) Physical properties (for example, the above-mentioned specific solvent) used for the surface shape of resin particles such as paints, adhesive materials, electronic materials, optical materials, etc. and a trace amount of other components contained in the solvent (for example, the above specific solvent). , Fluidity, cohesiveness, adhesiveness, chargeability, etc.).

[Brief description of drawings]

FIG. 1 is a view showing a dissolved state of resins I and II in a solvent A.

FIG. 2 is a diagram showing a state in which a resin I is deposited and a resin II is not deposited and is in a dissolved state when a solvent B is added to the state of FIG.

FIG. 3 is a view showing that resin I is deposited when solvent C is added to the state of FIG.

FIG. 4 is a diagram showing a state in which a dissolved resin II is deposited when solvent C is added to the state of FIG.

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[Procedure amendment]

[Submission date] March 26, 1992

[Procedure Amendment 2]

[Document name to be amended] Statement

[Correction target item name] 0008

[Correction method] Change

[Correction content]

[3] upon addition of solvent C in the state of FIG. 1, the resin I is analyzed
The figure which shows keeping an outgoing state .

Claims (1)

[Claims] 1. A first resin and a second resin are dissolved in a first solvent, a second solvent is added to this solution to precipitate first resin particles, and then a third solvent is added. A method for producing resin particles, wherein the second resin particles are added to deposit the second resin particles on the surface of the first resin particles, and the resin composition of the inner layer and the surface layer are different.