Overbased sulfurized alkaline earth metal alkylphenate having excellent water tolerance properties in lubricant formulations is prepared by charging into a reactor a preheated (280-380°F) mixture of alkaline earth metal base and alkylphenol (preferably in oil), while simultaneously, but separately, charging a promoter solvent such as a glycol. Then a controlled amount of molten sulfur is charged at a rate that controls the reaction exotherm and off-gas evolution, while maintaining the 280-380°F temperature. Upon completing the sulfur charge, the reactor contents are allowed to interact at 280-380°F long enough to form the sulfurized alkylphenate. While keeping the temperature at 280-380°F, the sulfurized alkylphenate is overbased by charging the reactor simultaneously with controlled amounts of alkaline earth metal base, promoter solvent, and carbon dioxide gas, at a controlled charge rate not much greater or less than the rate at which the reactants undergo reaction to form the overbased phenate. Upon completing the charging of the alkaline earth metal base and promoter solvent, the carbon dioxide charge is continued until completion of the carbonation reaction. Unreacted alkylphenol and promoter solvent are stripped off under vacuum with inert gas purge at 400-480°F, and the resultant reaction product is filtered and the filtered product recovered. The reaction cycle time is no more than about 6 hours, and the filtered product has water tolerance properties normally associated with a batch preparation of the same product requiring a reaction cycle time of at least 8 hours.
                            过基
硫化碱土
金属烷基
酚酯在润滑油配方中具有优异的耐
水性能,其制备方法是将碱土
金属碱和烷基
酚(最好在油中)的预热(280-380°F)混合物装入反应器,同时但单独装入
促进剂溶剂(如
乙二醇)。然后,在保持 280-380°F 温度的情况下,以控制反应放热和废气产生的速率,加入一定量的熔融
硫磺。完成
硫磺充填后,让反应器内容物在 280-380 华氏度下相互作用足够长的时间,以形成
硫化烷基
酚酸盐。当温度保持在 280-380 华氏度时,
硫化烷基
苯甲酸酯通过同时向反应器充入受控量的碱土
金属碱、
促进剂溶剂和
二氧化碳气体进行过基反应,其充入速率不大于或小于反应物发生反应以形成过基
苯甲酸酯的速率。碱土
金属碱和
促进剂溶剂充填完成后,
二氧化碳充填继续进行,直至碳化反应完成。未反应的烷基
酚和
促进剂溶剂在 400-480°F 下用惰性气体吹扫抽真空脱除,过滤反应产物并回收过滤产物。反应周期不超过约 6 小时,过滤后的产品具有耐
水特性,而批量制备相同产品通常需要至少 8 小时的反应周期。