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Process for production of polyamideimide resin microparticles, and polyamideimide resin microparticles

A polyamide-imide resin and particle technology, which is applied in the preparation of polyamide-imide resin particles and the field of polyamide-imide resin particles, can solve the problems of lack of reproducibility and large particle size variation, and achieves The effect of increasing the degree of freedom, simple and stable preparation

Inactive Publication Date: 2012-07-18
TORAY IND INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although polyamide-imide resin particles below 1 μm can be obtained by this method, the particle size depends on the concentration of the surfactant, the number of stirring revolutions, and the time until the polyamide-imide resin solution is dropped into the surfactant aqueous solution. The variation is large, so there is a lack of reproducibility, and it is not always possible to obtain polyamide-imide resin particles below 1 μm
In addition, in this method, since the solvent for dissolving PAI resin is limited to 1,3-dimethyl-2-imidazolidinone, and high-speed stirring at 1000~4000rpm is required, there are various problems in industrialization

Method used

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  • Process for production of polyamideimide resin microparticles, and polyamideimide resin microparticles
  • Process for production of polyamideimide resin microparticles, and polyamideimide resin microparticles
  • Process for production of polyamideimide resin microparticles, and polyamideimide resin microparticles

Examples

Experimental program
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preparation example Construction

[0039] As the preparation method of PAI resin, the following methods are known: the isocyanate method using trimellitic anhydride and diisocyanate as raw materials (for example, Japanese Patent Publication No. 50-33120 communique); making chlorinated trimellitic anhydride and diamine in N,N-dimethyl Acyl chloride method polymerized in acetamide (for example, Japanese Patent Publication No. 42-15637); in the presence of 3-valent or 5-valent inorganic or even organic phosphorus compounds, aromatic tricarboxylic acid, its anhydride or its ester and di A direct polymerization method in which amines react in a solution (for example, Japanese Patent Publication No. 49-4077); the PAI resin in the present invention can be prepared by any method.

[0040] As said polyamide-imide resin, a commercial item can also be selected suitably and used, Specifically, the polyamide-imide resin TI-5013P by Toray Co., Ltd., Toron by Solbey, etc. can be used.

[0041] [Preparation of PAI resin microp...

Embodiment 1

[0116] [Dissolution process] (b1)

[0117] A 1000ml autoclave of a dissolution tank was equipped with a stirrer, a temperature measuring device, and an extraction pipe for an internal solution. A connecting pipe that can be opened and closed by a valve is installed on the extraction pipe. In addition, as a receiving tank for flash crystallization, install a stirrer, a condenser, and a gas vent pipe on a 1000ml autoclave, and install the other end of the connection pipe (flash crystallization outlet) from the above-mentioned dissolution tank on the immersion receiving tank. position in the bath.

[0118] 12 g of PAI resin (manufactured by Toray Co., Ltd., TI-5013P, the powder used in the following examples) and 338 g of NMP (manufactured by Kanto Chemical Co., Ltd.) (PAI resin concentration: 3% by mass) were placed in a dissolution tank, and nitrogen replacement was performed. It was sealed and the internal temperature was raised to 240° C. while stirring, and then stirred fo...

Embodiment 2

[0123] Example 2 (dissolution process: b1, precipitation process: b2)

[0124] It implemented similarly to Example 1 except having set the temperature of the dissolution tank of Example 1 to 50 degreeC, and pressurized it to 0.5 MPa with nitrogen. The average particle size of the flash liquid is 12.4 μm. In addition, the average primary particle size of the PAI microparticles was 110 nm, and the coefficient of variation was 40%. Observed with a scanning electron microscope (SEM) at 30,000 magnifications, the particles are roughly spherical.

[0125] In order to confirm the reproducibility, the same operation as above was carried out. As a result, the average primary particle size of the PAI microparticles was 112 nm, and the coefficient of variation was 38%, confirming reproducibility.

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Abstract

Disclosed are: a process for producing polyamideimide (PAI) resin microparticles with high reproducibility in a simple manner, which can be achieved on an industrial scale; and PAI resin microparticles which are extremely fine and have uniform particle sizes. Specifically disclosed is a process for producing PAI resin microparticles, which comprises the dissolution step and the precipitation step mentioned below. [Dissolution step] A step selected from items (a1) and (b1): (a1) a step of dissolving a PAI resin in an organic solvent so as to produce a PAI resin-dissolved solution (A1) having a PAI resin concentration of less than 5 mass%; and (b1) a step of dissolving a PAI resin in an organic solvent so as to prepare a PAI resin-dissolved solution (B1) having a PAI resin concentration of less than 10 mass%. [Precipitation step] (a2) A step of adding the PAI resin-dissolved solution (A1) to a solvent that can cause the precipitation of PAI resin microparticles that contain substantially no surfactant to cause the precipitation of the PAI resin microparticles; and (b2) a step of subjecting the PAI resin-dissolved solution (B1) to flash crystallization to cause the precipitation of PAI resin microparticles.

Description

technical field [0001] The invention relates to a preparation method of polyamide-imide resin particles and polyamide-imide resin particles. Background technique [0002] Polyamide-imide resins are excellent in heat resistance, chemical resistance, abrasion resistance, etc., and are used in industrial machinery parts, films, electrical and electronic parts, automobile parts, and aerospace-related components. In addition, when coating polyamide-imide, it is usually used as a varnish by dissolving it in an organic solvent. However, in recent years, the problem of reducing volatile organic compounds (VOC) has arisen, so it is strongly desired not to use VOC. As one of the methods, there is a means of pulverizing polyamide-imide resin. By micronization, it is possible to directly spray the member, or apply its aqueous dispersion to the member and then remove the water for coating. In addition, polyamide-imide resin fine particles are mixed with other resins or composite mater...

Claims

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Application Information

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IPC IPC(8): C08J3/14C08G73/14
CPCC08J2379/08C08J3/14C08G73/14Y10T428/2982
Inventor 赤阪宽章大野孝卫高桥俊也
Owner TORAY IND INC
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