JPH0341149A - Production of mica-containing polyester composition - Google Patents

Abstract

PURPOSE:To obtain the title composition containing mica in a state of a good dispersion of micaceous particles and excellent in stability in melt forming into a fiber, a film, a resin molding or the like by adding mica under specified conditions in the production of the title composition. CONSTITUTION:Mica and a dispersant (e.g. polyethylene glycol) are added to the reaction system in the stage before the completion of the esterification or transesterification in the production of the title composition.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing a mica-containing polyester composition containing mica in a well-dispersed state of scaly particles.

[Conventional technology]

Polyester has many excellent properties and is therefore widely used in clothing and industrial fibers, films, resin molded products, and other fields.

Mica-containing polyester is used in the textile field as polyester tin, which has far-infrared radiation properties, and in the resin field, as polyester resin with improved mechanical properties such as elastic modulus! It has been proposed to use each A as a packaging polyester film with improved gas barrier properties.

However, when mica is incorporated into polyester, the dispersibility of mica particles in the polyester is generally not good. For example, when used as a yarn, the stability during the spinning process is extremely reduced and the spinning pressure increases. It had drawbacks such as frequent occurrence of defects such as interrupted threads and fuzz.

Conventionally, in order to incorporate mica into polyester, it has been common practice to mix them using a suitable mixer at normal pressure and at a temperature above the melting point of the polyester.

This method was adopted because it was easy to operate, and because it was thought that the dispersion state B of mica particles in the resulting polyester composition would be hardly affected by differences in the mixing method. be.

[Problem to be solved by the invention]

In the present invention, mica is well dispersed in the form of particles in polyester, and has excellent stability in the melt-forming process into transverse fibers, films, resin molded products, etc. The object of the present invention is to provide a polyester composition containing x-matrix.

[Means to solve the problem]

The present invention is a method for producing a mica-containing polynisder, which is characterized in that mica and a dispersant are added to the reaction system at a stage before the esterification reaction or transesterification reaction is completed when producing the mica-containing polyester.

In the present invention, the content of the ox mother in the produced polyester is α5-251i, which is excellent! 〈 is 1 to 15% by weight. If the content exceeds 25 weights t4, the stability of the composition in the melt shaping process will be significantly reduced. ! trl, quintuple i-
If it is less than 4, the fibers and films obtained by melt shaping will not have the effects of far-infrared radiation properties, gas barrier properties, and mechanical properties that resin molded products have.

The mica used in the present invention is preferably sericite whose main components are silicon dioxide and aluminum oxide. Also,
The dispersant used in the present invention is a surfactant that changes the properties of the particle surface by penetrating into the gaps between the primary mica particles and adsorbing onto the particle surface, or has a protective colloid effect by forming an electric double layer. They are inorganic electrolytes and polymer compounds. Specifically, the nonionic surfactant potassium metaphosphate, the anionic surfactant sodium dode V rubenzene sulfonate, sodium alkyl sulfonate, the inorganic electrolyte dipotassium hydrogen phosphate, and the terminal capping of the polymer compound. It is preferable to use polyethylene glycol as a dispersant, and the content of the B6 dispersant is cL 5 to 2 weight (relative to mica), and if it exceeds 2 weight, the acid value of the polyester polymer will increase. Thermal decomposition is likely to occur during the single polycondensation reaction. On the other hand, if the weight ratio is less than LL5, the dispersibility effect will be extremely reduced.

The polyester of the present invention contains an ester-forming derivative of terephthal #kataba as a dicarboxylic acid component, and at least one ester-forming derivative of glycol tobacco selected from ethylene glycol and 1,4-butanediol. A polyester containing a glycol component is typical, but a part of the dicarboxylic acid component may be replaced with another dicarboxylic acid component, and a part of the glycol component may be replaced with another glycol component.

Other dicarboxylic acid components include isophthalic acid, naphthalene dicarboxylic acid, diphenyldicarboxylic acid, diphenylsulfonic acid carboxylic acid, adipic acid, and sepacic acid%1
．． 4-5/Dicarboxylic acids such as clohexanedicarboxylic acid or their esters, p-oxybenzoic acid, p-β
-olll-sy x ) Oxycarboxylic acids such as xybenzoic acid or esters thereof, and the like.

Other glycol components include carbon atoms of 2 to 101.
7) Flukylene glycol, 1,4-cyclohexane dimetatool, neopentyl glycol, i,4-bis(
(β-oxyethoxy)benzene, bisglycol ether polyalkylene glycol of bisphenol A, and the like.

Furthermore, to the extent that the polyester is substantially linear, polycarboxylic acids such as trimellitic acid and pyromellitic acid, polyols such as pentaerythritol, trimethylolpropane, and glycerin, monohydric polyalkylene oxides, phenylacetic acid, etc. A polymerization terminator may also be used.

Such polyester can be synthesized by any known method.

For example, explain polyethylene terephthalate.
Terephthalic acid is produced by directly esterifying terephthalic acid and ethylene glycol, by transesterifying lower alkyl ester of terephthalic acid such as dimethyl terephthalate with ethylene glycol, or by adding ethylene oxide to terephthalic acid. A common method is to synthesize a glycol ester of an acid and a low polymer of tobacco, and then polycondense it by a conventional method.

According to the present invention, it is necessary to add mica and a dispersant during the polyester synthesis process at a stage before the esterification reaction or transesterification reaction of the polyester is completed. Specific timings for addition include the polyester raw material preparation stage, during the esterification or transesterification reaction, or at the latter stage of the reaction. Addition of mica and dispersant to the reaction system completes the esterification reaction or transesterification reaction.

If carried out in subsequent steps, the dispersion state of mica particles in the resulting polyester will be poor. As a result, the stability of the polyester during melt shaping is extremely reduced.

In the present invention, mica may be added in the form of powder (11), or may be added in the form of a slurry by dispersing it in ethylene glycol or the like.

Furthermore, in carrying out the present invention, known catalysts, antioxidants, coloring inhibitors, ultraviolet stabilizers, ether bond by-product inhibitors, lubricants, mold release agents, dispersion aids, flame retardants, etc. are used as appropriate. be able to.

! 9. The mica-containing polyester composition obtained according to the present invention may be melt-formed by itself, or may be melt-formed by blending or using other polymers as appropriate. There is no problem.

〔Effect of the invention〕

In the mica-containing polyester composition produced according to the present invention, mica has a maximum length of 10 μWL and a thickness of CL05 to 8 μm.
It is contained in polyester in a well-dispersed state of scale-like particles, and it has extremely excellent stability when melting and shaping this polyester into fibers, films, resin molded products, etc., and as a result, it has far-infrared radiation effects and gas barrier properties. - The excellent effects originally possessed by mica, such as the effect of improving physical properties and mechanical properties, can be exhibited without impairing the physical properties of polyester.

〔Example〕

Hereinafter, the present invention will be explained in more detail with reference to Examples.

In the examples, "part" and "excellent" mean "part by weight" and "weight" respectively.

The melt-forming stability of the prepared polyester is determined by chipping the polyester using a conventional method, drying it, and performing a melt-spinning test at 285°C through a spinneret having 24 circular spinning holes with a diameter of a3. Good quality is indicated by ○, somewhat good quality is indicated by Δ, and poor quality is indicated by ×.

Examples 1 to 5 100 parts of terephthalic acid, 0 parts of ethylene di-1-nocolf,
Salient mica Z-2O (mica manufactured by Salary Mining Co., Ltd.) 6.1 part, 1st
1 part of the dispersant shown in the table (for mica), 0.0 parts of sodium hydroxide.
012 parts were charged into the esterification reaction and the esterification reaction was carried out at 260°C under a pressure of 4 kg/z''.Subsequently, trimethyl phosphite and antimony dioxide were added to the resulting reaction product. (LO
1 and 11,104% as ethylene glycol dispersions, transferred to a polymerization tank, and heated at 285°C under high vacuum.
A polymerization reaction was carried out for a predetermined period of time to obtain a bo1-noester polymer.

Table 1 shows the size of dispersed mica particles in the obtained polyester and the melt-forming stability of the polyester.

Among these, polyesters obtained in Comparative Examples 1 to 4 in the same manner as in the Examples except that no dispersant was used and the timing of mica addition was changed are also listed in Table 1.

/ No. 1 table *Molecular weight 2 00 polyethylene glycol

Claims (1)

[Claims] A method for producing a mica-containing polyester composition, which comprises adding mica and a dispersant to a reaction system at a stage before the esterification reaction or transesterification reaction is completed when producing the mica-containing polyester.