低成本有机硅生产法获发明专利

吉林石化公司研究院近日开发出一种低成本有机硅生产方法，并获得国家发明专利。 二甲基二氯硅烷水解是有机硅生产过程中的重要环节，直接关系到有机硅生产原料中氯的回收，是降低生产成本的关键技术之一。目前，国内主要采取活性炭吸附法、聚苯乙烯基树脂吸附等方法降低酸水中硅氧烷的含量，但效果均不理想。     

国内信息

国内信息二甲基二氯硅烷恒沸酸水解工艺技术开发成功吉化集团公司研究院开发成功的二甲基二氯硅烷恒沸酸水解工艺技术成果，日前正式通过专家验收。二甲基二氯硅烷恒沸酸水解技术经全面系统的小试工艺研究和百吨级中试，确定了有关参数，完成了１８ｋｔ／ａ有机硅生产装置...     

二甲基二氯硅烷浓酸与恒沸酸水解方法比较

聚二甲基硅氧烷主要由二甲基二氯硅烷水解制得,介绍了二甲基二氯硅烷水解的两种方法,即浓酸水解法与恒沸酸水解法,以60 kt/a二甲基二氯硅烷水解为例,对两种水解工艺过程的用能、设备投资、占地投资等进行了计算分析。结果表明,浓酸水解方法具有成本低、能耗低、流程短等优点,将逐渐取代恒沸酸水解方法成为聚硅氧烷生产的新的发展趋势。     

浅谈沉降时间对二甲基二氯硅烷水解产物收率的影响

介绍了二甲基二氯硅烷水解反应机理及恒沸酸水解工艺,探讨了恒沸酸水解工艺生产过程中沉降时间对水解物收率的影响。     

中国专利

纳米级可固化硅树脂印模材料／CN101617994 浓盐酸环路水解二甲基二氯硅烷工艺／CN101619072 热固性硅氧烷树脂-环氧树脂组合物和由其模制的预制包装体／CN101619169     

二甲基二氯硅烷水解工艺研究进展

综述了二甲基二氯硅烷水解工艺的研究进展,包括恒沸酸水解工艺、饱和酸水解工艺和浓酸水解工艺.着重介绍了各种水解工艺在氯化氢回收利用上的改进,通过对各水解工艺优缺点的探讨,展望了二甲基二氯硅烷水解工艺的发展方向.     

过滤-吸附法回收废盐酸的技术研究

采用过滤-吸附法对含高浓度有机物废盐酸进行回收处理的实验研究,实验分别考察了纤维球、活性炭、树脂的物理性质,探究了废液过滤吸附流速、吸附剂质量及废液浓度对过滤吸附效果的影响。结果表明,实验最佳工艺参数为:纤维球柱与活性炭柱、树脂柱串联;纤维球柱填充纤维球质量50 g,活性炭柱填充质量130 g,流速0.25 BV/h;树脂柱填充床层体积50 m L,流速2 BV/h,实验得到油含量低于10 mg/L的洁净盐酸50 BV,回收率较高,实现了废盐酸的再生循环利用。     

浓酸水解法制备硅氧烷工艺条件探索

通过实验研究了二甲基二氯硅烷浓酸水解过程中盐酸浓度、反应温度、时间、原料配比对反应的影响,并对产物硅氧烷的水洗过程进行了研究,为开发二甲基二氯硅烷浓酸水解的新工艺提供了基础数据。结果表明,针对二甲基二氯硅烷浓酸水解过程,反应时间不应超过15 min,反应温度控制在35℃左右,原料二甲基二氯硅烷与浓盐酸的体积比为1∶12~1∶17。水洗过程中,碱液为6%的Na2CO3溶液,碱洗后再进行两次水洗,水洗温度为80℃以上,水洗过程中水相与有机相的体积比为5∶1,最终产物硅氧烷中氯离子含量为6.5 mg/kg,透明度为93%。在保证产品质量的前提下,浓酸水解在工艺和节能方面更具有优越性。     

过滤-吸附法回收废盐酸的技术研究

采用过滤-吸附法对含高浓度有机物废盐酸进行回收处理的实验研究,实验分别考察了纤维球、活性炭、树脂的物理性质,探究了废液过滤吸附流速、吸附剂质量及废液浓度对过滤吸附效果的影响。结果表明,实验最佳工艺参数为:纤维球柱与活性炭柱、树脂柱串联;纤维球柱填充纤维球质量50 g,活性炭柱填充质量130 g,流速0.25 BV/h;树脂柱填充床层体积50 m L,流速2 BV/h,实验得到油含量低于10 mg/L的洁净盐酸50 BV,回收率较高,实现了废盐酸的再生循环利用。     

AlCl3/活性炭催化甲基三氯硅烷与低沸物再分配反应研究

甲基三氯硅烷(M1)与低沸物(LBR)是工业上"直接法"生产二甲基二氯硅烷单体过程中产生的副产物,两者之间通过再分配反应可转化为高价值的有机硅单体.以活性炭为载体,采用浸渍蒸发煅烧法制备了负载型AlCl3固体酸催化剂,在固定床反应器中进行甲基三氯硅烷与低沸物的再分配反应,制得二甲基二氯硅烷和三甲基氯硅烷.考察了活性炭载体预处理方式及反应条件对再分配反应的影响.结果表明,经过高温扩孔处理的活性炭载体负载的AlCl3催化剂具有较好的反应活性;优化的反应条件为:W(M1/LBR)为2.0～3.0,反应温度为310℃,LHSV为1.5 h-1;该催化剂的制备过程简单,催化反应条件温和且表现出良好的催化稳定性.     

改性活性炭吸附脱除二氧化碳中微量乙烷

我国对食品级二氧化碳要求较高,在其生产过程中乙烷的脱除是难点。文章首先考察了市售的不同吸附剂,包括Y型、X型、A型等分子筛类,椰壳和煤基活性炭以及吸附树脂等吸附剂对CO2中微量C2H6的吸附效果,之后考察了不同浓度盐酸酸改性与氢氧化钠碱改性、双氧水氧化改性、氨水还原改性等改性条件对吸附剂吸附性能的影响。研究表明,具有高比表面积、丰富微孔和适量中孔结构的活性炭更有益于二氧化碳中微量乙烷的吸附;浓度为1%的盐酸溶液浸渍活性炭3 h后,能增强其对CO2中微量C2H6的吸附能力;浓度3%、浸渍时间6 h为氢氧化钠碱溶液改性活性炭的最佳条件;弱氧化剂双氧水改性能略微提高活性炭对二氧化碳中乙烷的吸附能力,弱还原剂氨水改性对吸附效果无明显影响。     

稻秸半纤维素水解条件和水解液脱毒的研究

为了充分利用稻秸半纤维素,并提高水解液发酵性能,对稻秸半纤维素的水解条件和水解液脱毒进行了研究。考察了酸浓度、温度、时间和固液比对稻秸半纤维素水解率的影响;通过正交实验设计确定水解的最优条件为:硫酸质量分数3%,温度120℃,时间1.5h,固液比(W/V)1∶10;在此条件下得到水解液,通过对有机溶剂萃取、大孔树脂吸附和活性炭吸附多种脱毒方法的比较,确定用Ca(OH)2+S-8型树脂进行水解液脱毒。     

γ-(2,3-环氧丙氧)丙基硅氧烷耐高温树脂的合成及热性能

以γ-(2,3-环氧丙氧)丙基三甲氧基硅烷(GPTS)、酸催化剂和混合溶剂等为原料,采用水解-缩合法合成了含环氧基的硅氧烷杂化树脂。以黏度和环氧值为衡量指标,采用单因素试验法优选出制备该杂化树脂的较佳工艺条件,并对其热性能进行了表征。结果表明:在酸性介质中,当n(GPTS)∶n(水)∶n(酸催化剂)∶n(溶剂)=1∶3.0∶0.5∶7.7时,GPTS经水解、缩合反应后,可以获得黏度为1 270～1 320 mPa.s、环氧值为0.183的硅氧烷杂化树脂;该杂化树脂的起始分解温度为270.1℃,800℃时的残炭率(43.0%)相对较高,说明其热稳定性较好。     

Comparison of different procedures for the detoxification of eucalyptus hemicellulosic hydrolysate for use in fermentative processes

Eucalyptus (Eucalyptus grandis) shavings were submitted to an acid hydrolysis process with the aim of obtaining a hemicellulosic hydrolysate rich in fermentable sugars. However, the hydrolysate obtained contained, in addition to sugars, several compounds that are toxic to microorganisms, namely furfural, hydroxymethylfurfural, acetic acid and phenolics. In order to produce a hydrolysate suitable for use in fermentative processes, several procedures were evaluated for hydrolysate detoxification, including concentration by vacuum evaporation and adsorption on activated charcoal, diatomaceous earths, ion‐exchange resin or adsorbent resin. Hydrolysate concentration was especially effective for furfural removal, whereas the adsorbent resin was efficient in removing hydroxymethylfurfural, phenolics and acetic acid. Combination of this resin with activated charcoal was better than with diatomaceous earths for removal of acetic acid and phenolics. The best detoxification procedure evaluated was based on hydrolysate concentration followed by adsorption on activated charcoal and adsorbent resin. By this treatment, removal rates of 82.5, 100, 100 and 94% were attained for acetic acid, furfural, hydroxymethylfurfural and phenolics, respectively. Copyright © 2005 Society of Chemical Industry     

玉米秸秆水解及水解液的净化处理

对玉米秸秆水解和水解液的净化处理进行了研究。结果表明,在水解温度为120℃时,半纤维素水解率为93.7%,纤维素水解率为19.7%。温度为160℃时,半纤维素水解率为98.1%,纤维素水解率为73.4%。采用CR系列大孔吸附树脂、阴离子交换树脂和阳离子交换树脂3种混合树脂床对水解液进行净化处理,能除掉水解液中96%的多酚类物质和94%的阳离子以及96%的弱酸根及无机酸根离子。     

水解蛋白作为酸洗缓蚀剂的缓蚀性能研究

以发酵工业废水为原料提出菌体，将其部分水解后，所得水解蛋白液作为酸洗缓蚀剂，采用失重法研究了它在盐酸、硫酸溶液中对钢、铝的缓蚀效率，认定其在盐酸、硫酸溶液中对钢有较好的缓蚀作用，以及同六次甲基四胺复配后良好的缓蚀协同作用。     

甲苯法生产己内酰胺水溶液的吸附精制工艺试验研究

以活性炭、活性炭纤维及离子交换树脂作为吸附剂，在甲苯法己内酰胺水溶液中试验了不同吸附剂对己内酰胺水溶液中杂质的吸附能力。结果表明，当光密度均降低30％时，采用活性炭吸附，对己内酰胺中有机杂质的动态吸附容量为26．7mL／g；活性炭纤维杂乱填充时的动态吸附容量为67．48mL／g；强碱性离子交换树脂IAR900的动态吸附容量为46．66mL／mL。提出了活性炭纤维与离子交换树脂组合吸附工艺，当光密度均降低50％时，动态吸附容量为36．67mL／g，该组合工艺能有效去除己内酰胺水溶液中的杂质，提高了产品的质量。     

ZH-01吸附树脂对苯甲酸的吸附性能研究

比较了超高交联吸附树脂ZH-01与大孔吸附树脂AmberliteXAD-4对苯甲酸的静态吸附和动态吸附行为,并探讨了温度和起始浓度对平衡时间和吸附速率的影响.从静态平衡吸附行为及其热力学性质讨论吸附机理,动态吸附进一步验证聚苯乙烯超高交联吸附树脂对苯甲酸的吸附能力比AmberliteXAD-4强.结果表明:在288～3...     

The conditions of cationic exchange with the use of recycling polystyrene derivative,the product of sulfonation by silica sulfuric acid

Growing amount of waste plastics has become an environmental problem on a global scale. This study presents an investigation of the conditions of cleaning water from heavy metal ions using chemically recycled polystyrene. To get effective ion exchangers, the sulfonation of virgin polystyrene and expanded polystyrene wastes were obtained using silica sulfuric acid. As it turned out, the use of this solid sulfonating agent simplifies the separation of the polymeric product from the acid and the solvent in comparison to conventional sulfonation methods. The ion exchange behavior of copper and zinc cations in the yielded sulfonated derivatives of polystyrene was studied. Batch shaking adsorption experiments depending on contact time, pH, temperature, and dosage of adsorbate were carried out. The stability of resin to cyclical adsorption and regeneration (column experiment) was also investigated. We report that resins have a high adsorption efficiency with total ion exchange capacity (IEC) about 2.6 meq g^?1, which drops with decreasing pH owing to competition between protons H⁺ and metal cations, whereas with the increasing resin doses the removal of cations rises for a constant initial metal concentration. The speed of cation exchange for yielded adsorbents was even better than for commercial resins. After 360 cyclical adsorption and regeneration in column, resin had working IEC of about 2.3 meq g^?1. The study shows that cation exchange resin from polystyrene wastes can be used as an efficient adsorbent for the removal of heavy metal ions from water. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Preparation of trioctylamine-impregnated polystyrene–divinylbenzene porous resins for the collection of precious metals from water

A water-insoluble extracting solvent, trioctylamine (TOA), was solubilized in the aqueous micellar solution of a polyoxyethylene-type nonionic surfactant, polyethyleneglycol (10)-mono-4-nonylphenyl ether (PONPE-10). By mixing the solution and a polystyrene–divinylbenzene porous resin (Amberlite XAD-4), TOA was successfully impregnated into the resin. Gold(III), platinum(II), and palladium(II) were well extracted from hydrochloric acid to the TOA-impregnated resins. The extents of the extraction of platinum(II) and palladium(II) increased with increasing the amount of TOA impregnated. The TOA-impregnated filter disk was also prepared by passing aqueous mixture of PONPE-10 and TOA through an Empore disk involving polystyrene–divinylbenzene. The disk was useful for concentrating precious metals in water prior to their graphite furnace atomic absorption spectrometric analysis.