›› 2019, Vol. 50 ›› Issue (11): 56-60.

• 油品与添加剂 • 上一篇    下一篇

低碱值聚异丁烯硫膦酸钙的研制

刘依农,段庆华   

  1. 中国石化石油化工科学研究院
  • 收稿日期:2019-03-26 修回日期:2019-07-05 出版日期:2019-11-12 发布日期:2019-11-29
  • 通讯作者: 刘依农 E-mail:liuyinong.ripp@sinopec.com

DEVELOPMENT OF LOW BASIC CALCIUM POLYISOBUTYLENE THIOPHOSPHONATE

Liu Yinong,Duan Qinghua   

  • Received:2019-03-26 Revised:2019-07-05 Online:2019-11-12 Published:2019-11-29
  • Contact: Liu Yinong E-mail:liuyinong.ripp@sinopec.com

摘要: 探索了聚异丁烯硫膦酸钙(简称硫膦酸钙)的合成工艺,重点考察了聚异丁烯硫膦酸(简称硫膦酸)、硫膦酸钙的合成条件。在硫膦酸合成中,考察了反应温度、反应时间、五硫化二磷(P2S5)加入量、催化剂加入量和水的加入量等工艺条件的影响,得到优化的工艺条件为:反应温度为T0,反应时间为10 h,P2S5加入量(与聚异丁烯质量比)为21%,催化剂加入量(与聚异丁烯质量比)为0.5%,水加入量(与聚异丁烯硫膦酸酐质量比)为0.10%;并通过钙化工艺得到低碱值硫膦酸钙。中型放大试验结果表明:合成硫膦酸、硫膦酸钙的工艺条件稳定,试验重复性好,所合成的硫膦酸钙碱值在40~50 mgKOH/g之间,磷质量分数大于0.9%,硫质量分数大于3.0%;产品具有良好的清净、分散、抗氧化性能,可以用于内燃机油中。

关键词: 聚异丁烯硫膦酸, 聚异丁烯硫膦酸钙, 发动机油, 低碱值

Abstract: The preparation process of calcium polyisobutylene thiophosphonate,including polyisobutylene thiophosphonic acid and calcium polyisobutylene thiophosphonate were developed. The reaction parameters for synthesis of polyisobutylene thiophosphonic acid, such as reaction temperature,reaction time,the dosage of P2S5 and catalyst,the dosage of water for hydrolysis were investigated. The optimized reaction parameters covered a reaction temperature of T0,a reaction time of 10 h,a mass ratio of P2S5 to polyisobutylene of 21%,a mass ratio of catalyst to polyisobutylene of 0.5% and a mass ratio of water to polyisobutylene thiophosphonic anhydride of 0.1%. The low basic calcium polyisobutylene thiophosphonate were synthesized by calcification process. The synthesis of polyisobutylene thiophosphonate in pilot reactor indicated that the preparation conditions were controllable with good test repeatability. The product, calcium polyisobutylene thiophosphonate, has a base value of 40-50mgKOH/g,while the mass fractions of P and S are greater than 0.9% and 3.0%, respectively. The product has good cleaning, dispersion and oxidation resistance, and can be used in internal combustion engine oil.

Key words: polyisobutylene thiophosphonic acid, calcium polyisobutylene thiophosphonate, engine oil, low basic