- Patent JPS5314599

Document Type and Number:

Japanese Patent JPS5314599

Kind Code:

B1

Abstract:

1336885 Zr- and Hf-modified amide-aldehyde polymers POLY-CHEM INDUSTRIES Inc 18 Jan 1971 [5 Feb 1970 22 Dec 1970] 2288/71 Headings C3R C3P and C3C A zirconium or hafnium-containing aminealdehyde polymer is obtained by heating a zirconium and/or hafnium halide with at least one amide having at least two labile H atoms, in the absence of water, mixing the product with at least one aldehyde, and adding water after the heating and before or with the aldehyde. Suitable amides include formamide, acetamide, propionamide, butyramide, adipamide, succinamide, maleamide, urea, thiourea, ethyleneurea, propyleneurea, guanidine and melamine; suitable aldehydes include formaldehyde, acetaldehyde, propionaldehyde, adipaldehyde, acrolein, cyclohexaldehyde, furfural and nicotinaldehyde. There may also be added during the reactions (i) a polyhydric polymer or phenol, (ii) an organic solvent, (iii) inert insoluble particles, e.g. glass beads, to assist heat transfer in the amide/ halide reaction, (iv) cyanuric acid, ammeline or ammelide, to stabilize the product. The hydrogen halide content of the hydrolysed amide/ halide product may be reduced by standing or by addition of a base, an ion-exchange resin, an oxidizing agent, e.g. O 2 , O 3 , H 2 O 2 or air, or conc. H 2 SO 4 , which displaces hydrogen halide and also becomes incorporated into the resin. Preferred proportions are 0À3-10 moles of water, 0À01-0À5 moles of halide and 0À01-1 mole of polyhydroxy benzene (if used) per mole of amide, and at least one mole of aldehyde per mole of amide plus phenol. In the examples urea is fused with ZrCl 4 , water is added, the product cooled and formalin added to give the polymer (molar ratios in Example 1: 0À15 : 0À0026- 0À01 : 0À17 : 0À2). In Examples 2 and 4 melamine, acetamide, thiourea or guanidine hydrochloride is used instead of urea; in Example 5 resorcinol is mixed with the urea; in Example 1 HfCl 4 is also used instead of ZrCl 4 ; in Example 5 dimethylformamide is added with the water; in Examples 3 and 4 polyvinyl alcohol is added with the formalin; in Example 6 the product is further polymerized with acrylic acid i.p.o. ammonium persulphate and sodium thiosulphate to give a foamed product; in Examples 7-10 the hydrolysed urea/ZrCl 4 product is treated with H 2 O 2 , urea is added, and the formalin is precondensed with urea or urea plus melamine or with biuret and optionally cyanuric acid; in Example 8 biuret is used instead of urea in the reaction with ZrCl 4 . Uses.-Casting resins, laminates, insulation, adhesives.

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