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A process for the degradation of polyethylene terephthalate - to dimethyl terephthalate

机译:将聚对苯二甲酸乙二醇酯降解为对苯二甲酸二甲酯的方法

摘要

A process for the degradation and conversion of polyethylene terephthalate to dimethyl terephthalate comprises treating the polyethylene terephthalate with steam at a temperature of substantially 400 DEG C. and preferably in counter-current, and thereafter forming a powder having a mean particle size of substantially 0.001 mm., forming an aerosol from this powder and methanol vapour and/or an inert gas, reacting the aerosol in a turbulent flow with an excess of methanol vapour at a temperature from 250-300 DEG C. without using pressure, separating the reaction products from constituents in solid or mist-like form, and cooling with fractionation. The reaction may be accelerated by adding a gaseous catalyst such as hydrogen chloride. Zinc oxide or zinc compounds with inorganic or organic oxides may be admixed with the polyethylene terephthalic before or after forming it into a powder. In an example polyethylene terephthalate was treated in a vertical tube with oppositely flowing superheated steam at a temperature of about 400 DEG C. which left the tube at a temperature of about 200 DEG C. The oily textile auxiliaries adhering to the polyethylene terephthalate waste distilled off with the steam, and the polyethylene terephthalate which accumulated as a melt beneath the tube, was continuously poured on to an endless steel band and solidified by cooling. It was ground by means of conventional mills into a powder having a mean particle size of 0.001 mm. which was stirred with methanol to form a suspension which was then sprayed by means of a known adjustable Nubilosa nozzle with simultaneous introduction of 0.1% by weight, calculated on introduced polyethylene terephthalate, of dry hydrogen chloride gas into turbulently flowing nitrogen. The aerosol of polyethylene terephthalate in the mixture of methanol vapour and nitrogen had a turbulent flow and was introduced tangentially at the bottom end of a heated reaction chamber. The reactants discharged tangentially at the upper end of the tube into a container heated to 250 DEG C. having a column with a dephlegmator mounted on it causing further cooling of the reaction products and so controlled that only reaction products passed over which were still in vapour form at a temperature from 165 to 175 DEG C. The separated products were cooled, again pulverized and reintroduced. The reaction products remaining in vapour form were cooled by means of a second cooling assembly to 65 DEG C. A liquid glycol and methanol mixture was formed and, after relatively slow crystallizing out, pure dimethyl terephthalate; which was removed by centrifuging and washed with methanol, was obtained.
机译:聚对苯二甲酸乙二醇酯的降解和转化为对苯二甲酸二甲酯的方法包括:在约400℃的温度下,优选在逆流下,用蒸汽处理聚对苯二甲酸乙二酯,然后形成平均粒径为约0.001mm的粉末。 ,由这种粉末和甲醇蒸气和/或惰性气体形成气溶胶,使该气溶胶与湍流与过量的甲醇蒸汽在250-300℃的温度下反应,而无需使用压力,将反应产物从固体或薄雾状的成分,并通过分馏冷却。可通过添加气态催化剂例如氯化氢来加速反应。可以将氧化锌或具有无机或有机氧化物的锌化合物与聚对苯二甲酸乙二醇酯在形成粉末之前或之后混合。在一个实施例中,聚对苯二甲酸乙二醇酯在垂直管中用约400℃的反向流动的过热蒸汽处理,该蒸汽在约200℃的温度下离开管。油性纺织品助剂粘附到蒸馏出的聚对苯二甲酸乙二醇酯废料上用蒸汽将聚对苯二甲酸乙二醇酯在管子下方以熔体的形式积累,然后将其连续倒在环形钢带上,并通过冷却使其固化。用常规研磨机将其研磨成平均粒径为0.001mm的粉末。将其与甲醇一起搅拌以形成悬浮液,然后将其通过已知的可调节Nubilosa喷嘴喷雾,同时将0.1重量%(按引入的聚对苯二甲酸乙二醇酯计)的干燥氯化氢气体引入湍流的氮气中。在甲醇蒸气和氮气的混合物中的聚对苯二甲酸乙二醇酯的气溶胶具有湍流,并且被切向地引入加热的反应室的底端。反应物在管的上端切向排放到加热到250℃的容器中,该容器的柱上装有分馏器,引起反应产物的进一步冷却,并控制只有通过的反应产物仍在蒸气中在165℃至175℃的温度下冷却。分离的产物冷却,再次粉碎并重新引入。残留的蒸气形式的反应产物通过第二冷却装置冷却至65℃。形成液体乙二醇和甲醇的混合物,并在相对缓慢的结晶后,得到纯的对苯二甲酸二甲酯。通过离心将其除去并用甲醇洗涤。

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