公开(公告)号：US3959449A

公开(公告)日：1976-05-25

申请号：US456717

申请日：1974-04-01

申请人： Motoo Shigeyasu ,  Takeo Ozaki ,  Nobuo Kusano

发明人： Motoo Shigeyasu ,  Takeo Ozaki ,  Nobuo Kusano

IPC分类号： B01J37/22 ,  B01J37/30 ,  B01J39/04 ,  C07C51/487 ,  C01B7/12 ,  B01D11/02 ,  C01G45/06 ,  C01G51/08

CPC分类号： B01J39/043 ,  B01J37/22 ,  B01J37/30 ,  C07C51/487

摘要： A method of recovering in highly pure states heavy metals such as cobalt, manganese, etc., and bromine without the contamination of organic impurities and heavy metal impurities from the residue of the reaction mother liquor, which is obtained by removing a solvent from the reaction mother liquor remained after recovering terephthalic acid from the oxidation reaction product obtained in the method of producing terephthalic acid by subjecting an alkylbenzene such as p-xylene to a liquid phase oxidation with oxygen or oxygen-containing gas in the presence of a catalyst containing the heavy metals and bromine using a lower aliphatic monocarboxylic acid as the solvent, said method comprising: stirring the residue of the reaction mother liquor with water as solvent in the presence of molecular oxygen and a sulfur compound, removing solid impurities from the extracted mixtures thus treated by solid-liquid separation to provide an aqueous catalyst extract solution, passing the aqueous solution through a column packed with a strongly acidic cation-exchange resin to adsorb thereon the heavy metal catalyst, distilling the solution thus passed through the ion-exchange resin to recover bromine contained in the aqueous extract solution as hydrobromic acid, and, on the other hand, passing hydrobromic acid through the column of the ion exchange resin having adsorbed thereon the heavy metal catalyst to desorb the heavy metal catalyst, whereby the heavy metal catalyst is recovered as the bromide of it.

摘要翻译： 在高纯度状态下回收重金属如钴，锰等的方法和溴，而不会从反应母液的残留物中除去有机杂质和重金属杂质，这是通过从反应中除去溶剂而获得的 在从对苯二甲酸生产方法中得到的氧化反应产物中回收对苯二甲酸后，母液在含有重氢的催化剂存在下，用对二甲苯等烷基苯进行液相氧化 使用低级脂族一元羧酸作为溶剂的金属和溴，所述方法包括：在分子氧和硫化合物的存在下，用水作为溶剂搅拌反应母液的残余物，从如此处理的提取的混合物中除去固体杂质， 固液分离以提供含水催化剂提取液，通过水溶液 n通过填充有强酸性阳离子交换树脂的柱以吸附重金属催化剂，蒸馏由此通过离子交换树脂的溶液以回收含水提取物溶液中的溴作为氢溴酸，另一方面 将氢溴酸通过其上吸附有重金属催化剂的离子交换树脂的柱，使重金属催化剂解吸，由此重金属催化剂作为其溴化物被回收。

公开(公告)号：US4160108A

公开(公告)日：1979-07-03

申请号：US770145

申请日：1977-02-18

申请人： Motoo Shigeyasu ,  Nobuo Kusano

发明人： Motoo Shigeyasu ,  Nobuo Kusano

IPC分类号： C07C63/26 ,  B01J27/00 ,  C07B61/00 ,  C07C51/00 ,  C07C51/265 ,  C07C67/00 ,  C07C51/33

CPC分类号： C07C51/265 ,  Y02P20/52

摘要： In a process for producing terephthalic acid which comprises subjecting p-xylene to a liquid-phase oxidation in a lower aliphatic carboxylic acid solvent in the presence of a cobalt compound-manganese compound-bromine or bromine compound catalyst and molecular oxygen, the improvement which comprisesThe % by weight based on the weight of said lower aliphatic carboxylic acid solvent of the cobalt component (as cobalt) in the catalyst being within the range of-6.00.times.10.sup.-4 t+1.65.times.10.sup.-1 to -2.50.times.10.sup.-3 t+6.25.times.10.sup.-1 wherein t is the reaction temperature in .degree. C.;the weight ratio of the manganese component (as manganese) in the catalyst to the cobalt component in the catalyst ranges from 0.25:1 to 1:1 and also the amount of the manganese component in the catalyst is 0.05% by weight or less based on the weight of said lower aliphatic carboxylic acid solvent; andThe % by weight based on the weight of said lower aliphatic carboxylic acid solvent of the bromine component (as atomic bromine) in the catalyst is within the range of-4.40.times.10.sup.-3 t+1.08 to -1.00.times.10.sup.-2 t+2.50 wherein t is as defined above.