JPH09263588A - Production of antimony glycolate and antimony glycol oxide - Google Patents

Abstract

PROBLEM TO BE SOLVED: To produce at a low cost a catalyst used in producing polyester resins such as polyethylene terephthalate by a polycondensation reaction. SOLUTION: Antimony glycolate and antimony glycol oxide are produced by heat-reacting antimony trichloride with >=1.5 molar equivalent of ethylene glycol and absorbing generated HCI gas with an aqueous solution of an alkali.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention proposes a method for producing a catalyst used in producing a polyester resin such as polyethylene terephthalate by a polycondensation reaction.

[0002]

2. Description of the Related Art As a polycondensation catalyst for polyester resins,
Various antimony compounds are known. Typical examples thereof include antimony trioxide, antimony acetate, antimony glycolate, antimony glycol oxide and antimony trichloride. Antimony trioxide is inexpensive, but somewhat poorly reactive, and antimony acetate is superior in reactivity to antimony trioxide, and as a result, the amount added in terms of metallic antimony can be reduced, but on the other hand, it is expensive, Further, it has a drawback that it reacts with moisture in the air to generate acetic acid and is easily transformed into antimony oxyacetate. Antimony glycolate and antimony glycol oxide, which are reaction products of antimony and ethylene glycol, are extremely effective catalysts, but have not been widely used because a method for producing them at low cost has not been known. In Japanese Patent Application No. 57-35840,
As a method of producing antimony glycol oxide, a method of reacting antimontris organic carboxylate with at least 15 equivalents of ethylene glycol has been proposed. However, according to this method, it is estimated that the antimontris organic carboxylate is easily converted into antimony glycolate or antimony glycol oxide under the polycondensation reaction condition, and it is meaningless to previously prepare antimony glycol oxide. In addition, since antimony tris organic carboxylate is used as a raw material, it is clear that antimony tris organic carboxylate is inferior in cost.

[0003]

DISCLOSURE OF THE INVENTION The present invention provides a method for inexpensively producing antimony glycolate or antimony glycol oxide and a mixture thereof produced from antimony and ethylene glycol, which has excellent catalytic performance. It is in.

[0004]

[Means for Solving the Problems] Antimony trichloride is industrially manufactured and sold by directly reacting metal antimony with chlorine. By removing this from the air with an inert gas and heating and stirring it with ethylene glycol, a de-HC1 reaction occurs and easily becomes antimony glycolate, and if excess ethylene glycol is removed, antimony glycol oxide can be removed. To generate.

[0005]

Example 1 228 parts of antimony trichloride and 186 parts of ethylene glycol were reacted in a boiling water bath under an inert atmosphere, the generated HCI gas was introduced into an alkaline aqueous solution, and the theoretical amount of gas was confirmed to react. Stopped. The reaction product was filtered to obtain uniformly transparent tris (β-hydroxyethoxy) antimony.

[Practical example 2] The tris (β-hydroxyethygi) antimony obtained in practical example 1 was heated under reduced pressure to remove excess ethylene glycol, and white antimony glycol oxide crystals were obtained.

[0006]

EFFECTS OF THE INVENTION According to the present invention, antimony glycolate and antimony glyoxide, which are useful as polycondensation catalysts for polyester resins, can be produced at low cost.

Claims (1)

[Claims] 1. A method for producing tris (β-hydroxyethoxy) antimony and / or antimony glycol oxide by reacting antimony trichloride with ethylene glycol in an amount 1.5 times or more that of antimony trichloride.