聚醚酮新型精制工艺的研究

为解决聚醚酮(PEK)生产过程中反应产物、溶剂及副产物等难分离,以及工艺流程较长、设备分散、物料需多次转移、耗时、耗能、耗水等问题,对其工艺进行了重新设计。将分散的、单一功能设备综合在一起,先经丙酮浸取,除去溶剂二苯砜;再经水洗除去氟盐等水溶性物质;最后经过真空、气流干燥得到纯物料。新工艺投产后,聚醚酮精制时间由原来的22 h降为18h,干燥后物料含水质量分数≤0.02%,物料的粉化率仅为1.68%,丙酮损失量由300 kg/t降为62 kg/t。新工艺设备集中,占用场地面积小,操作简化,能耗降低,节约超纯水用量,含氟水零排放。     

BP-Amoco精对苯二甲酸生产工艺技术分析

介绍了精对苯二甲酸生产BP-Amoco工艺及Dupont工艺的技术特点,并按照两种工艺进行了技术对比分析。结果表明:与Dupont工艺相比,BP-Amoco工艺进行了技术改进,包括采用溶剂置换技术除去粗对苯二甲酸中的醋酸、采用多功能高压脱水塔回收氧化溶剂、取消精制母液处理系统、取消精制单元污水排放、降低尾气膨胀机入口温度等。BP-Amoco工艺简化了工艺流程,其装置综合能耗降低约60%,污水排放量减少约75%,装置投资成本节省约30%。     

纳微结构聚醚酮结晶物生产工艺及设备的开发

为缩短聚醚酮精制时间、降低能耗,将试验中间歇操作获得纳微结构聚醚酮结晶物的制备方法,改进成一种连续的工艺并应用于生产。运行结果表明:160℃左右结晶的聚醚酮在混合物中的晶型全部类似海绵状,晶体间孔隙较大、空隙率高,其精制时间是12.3h,为原传送带水冷精制时间的65.4%。对同批次结晶的聚醚酮进行物性检测对比,未见发生变化。此工艺较大程度的降低了聚醚酮精制的能耗,提高了生产效率。     

聚醚酮合成产物中二苯砜的浸取工艺

以二苯砜为溶剂合成聚醚酮时,反应结束后,产物、溶剂、副产物、原料等掺杂在一起,常温下形成固体混合物。为了将产物与其它物料分离,通常将混合固体粉碎,首先用溶剂将二苯砜浸出,然后再经蒸馏、干燥,回收二苯砜。本研究从脂肪提取工艺、抽提工艺、蒸煮工艺及循环等工艺出发,探索了聚醚酮合成产物中二苯砜的浸出过程。试验结果表明改进脂肪提取工艺是浸出二苯砜的最适宜工艺,其过程简单,控制容易,整批物料处理周期为2.16 h,丙酮消耗量为0.03 L,物料粉化率为零。同时,明确了浸取过程的机理,为二苯砜浸出的工业生产过程的工艺设计奠定了基础。     

混合溶剂法精制双酚S的工艺研究

研究了醇-四氯乙烷或醇-苯甲醚混合溶剂法精制粗品双酚S。将粗品双酚S在醇中溶解,加入四氯乙烷或苯甲醚,加热条件下活性炭脱色,蒸馏除去醇,过滤得到高质量分数的双酚S精制产品。醇-四氯乙烷精制的最佳工艺条件为:10 g粗品于40 g异戊醇中溶解,加入100 g四氯乙烷,1 g活性炭,50℃搅拌脱色1 h,过滤得滤液,蒸馏除去醇,降温、过滤、干燥,所得精制产品中双酚S的质量分数为99.50%,收率为82%;醇-苯甲醚精制的最佳工艺条件为:10 g粗品于40 g异丁醇或异戊醇中溶解,加入60 g苯甲醚,1 g活性炭。50℃搅拌脱色1 h,过滤,滤液蒸馏除去醇,降温、过滤、干燥,所得精制产品质量分数达99.80%以上,收率在83%左右。     

聚醚酮合成产物中二苯砜回收工艺的改进

针对现行生产工艺中,采用丙酮浸取回收聚醚酮反应溶剂二苯砜存在的问题及后续工艺要求,依据分析及实验结果对现行工艺进行改进,将原有的循环工艺和抽提工艺改为改进脂肪提取式工艺,即将待浸取物料作为溶剂冷凝介质。实际生产运行证明,改进后工艺较大程度地提高了生产效率。处理时间是原来的1/3～1/4,丙酮溶液使用量是原来的1/2～1/5,丙酮溶液消耗量是原来的1/4～1/8,物料粉化率是原来的1/10～1/16。     

混合溶剂法精制双酚S的工艺研究

为减少废水排放及提高产品质量,研究了醇-四氯乙烷或醇-苯甲醚混合溶剂法精制粗品双酚S。将粗品双酚S在醇中溶解,加入四氯乙烷或苯甲醚,加热条件下活性炭脱色,蒸馏除去醇,过滤得到高质量分数的双酚S精制产品。醇-四氯乙烷精制的最佳工艺条件为：10g粗品于40g异戊醇中溶解,加入100g四氯乙烷,1g活性炭, 50℃~60℃搅拌脱色1h,过滤得滤液,蒸馏除去醇,降温、过滤、干燥,所得精制产品中双酚S的质量分数为99.50%,收率为82%;醇-苯甲醚精制的最佳工艺条件为：10g粗品于40g异丁醇或异戊醇中溶解,加入60g苯甲醚,1g活性炭。搅拌脱色1h,过滤,滤液蒸馏除去醇,降温、过滤、干燥,所得精制产品质量分数达99.80%以上,收率在83%左右。     

MES表面活性剂的工业化精制工艺

将α-磺基脂肪酸甲酯钠盐（MES）产品（含活性物质70%）在加热熔融的状态下滴加到50~55℃低沸点水溶性有机溶剂中,经冷却、结晶、过滤和干燥,得到高纯MES粉剂产品。考察了低沸点水溶性有机溶剂种类、原料与溶剂的投料质量比、冷却温度和结晶时间等工艺条件对产品回收率、活性物质量分数和过筛率的影响,得到了最佳纯化精制工艺：以甲醇为溶剂,5 kg MES,MES与溶剂的投料质量比为1：3,冷却温度为5℃,结晶时间为120 min,干燥时间60 min,干燥温度45℃,溶剂使用3次。本工艺条件下,所制得MES粉剂产品回收率大于98%,含活性物质量分数大于93.0%,产品在40℃密封保存12 h后,过0.850 mm筛孔的筛,过筛率达100%。     

联苯乙酸粗品的精制研究

精制了一种指定合成路线的联苯乙酸粗品.研究了溶剂类型、溶剂用量、结晶时间等因素对重结晶工艺的影响,确定适宜的工艺条件为:6∶4的95%乙醇-水为溶剂,溶剂和粗品体积质量比为15∶2(mL∶g),结晶时间为8 h,进行2次重结晶.得到精制联苯乙酸的纯度为99.6%.     

杜仲叶渣中杜仲胶提取工艺的研究

以提取过药用成分的杜仲叶渣为原料,提取杜仲胶。研究了分别用碱水解和酶解预处理杜仲叶渣,然后用溶剂提取杜仲胶,以及直接用溶剂提取杜仲胶的工艺。实验结果表明最佳工艺条件为:杜仲叶渣直接用正己烷作溶剂提取杜仲胶,原料与溶剂比例为1:20(g:mL),机械搅拌并加热回流浸提2h,趁热过滤,滤液放入冰箱在-20℃条件下冷却析晶1h,真空抽滤后自然干燥得到浅绿色杜仲胶产物,提取得率为4.42%。用丙酮多次精制得到白色的杜仲胶。对白色杜仲胶产物做红外光谱测定,确定为反式1,4-聚异戊二烯(TPI)。     

环己酮生产中碳酸钠回收干燥装置的设计与分析

针对环己酮生产过程中废碱碳酸钠回收利用的工艺特点,设计了一种新型干燥装置,对干燥器的干燥流程、干燥器的结构和工作原理进行了分析及计算。结果表明:循环自动干燥碳酸钠设备主要由干燥箱、供热风系统、抽湿系统、扩散系统和包装系统组成;通过温控由电烘箱进行碳酸钠干燥实验,得到了碳酸钠干燥设备的干燥曲线,该系统干燥能力达1～2 t/h,干燥后碳酸钠含水率小于2%;该系统利用工厂废烟气作热源,节省干燥成本,且无环境污染。该设备干燥能力大,热效率高,能耗低,调控性能好,很好的解决了环己酮工业中废碱处理的难题。     

甲基丙烯酸甲酯生产工艺及设备配置研究

以石油炼化企业炼油装置产生大量的副产物C4混合物为原料,经过精制后生产甲基丙烯酸甲酯,对该生产过程的工艺流程及设备配置进行优化设计,从而实现了提高了副产物c4馏分的利用率,大力发展循环经济,创造更多的经济价值,增强企业的竞争实力。     

Soft-sensing modeling and intelligent optimal control strategy for distillation yield rate of atmospheric distillation oil refining process

It is a challenge to conserve energy for the large-scale petrochemical enterprises due to complex production process and energy diversification. As critical energy consumption equipment of atmospheric distillation oil refining process, the atmospheric distillation column is paid more attention to save energy. In this paper, the optimal problem of energy utilization efficiency of the atmospheric distillation column is solved by defining a new energy efficiency indicator — the distillation yield rate of unit energy consumption from the perspective of material flow and energy flow, and a soft-sensing model for this new energy efficiency indicator with respect to the multiple working conditions and intelligent optimizing control strategy are suggested for both increasing distillation yield and decreasing energy consumption in oil refining process. It is found that the energy utilization efficiency level of the atmospheric distillation column depends closely on the typical working conditions of the oil refining process, which result by changing the outlet temperature, the overhead temperature, and the bottom liquid level of the atmospheric pressure tower. The fuzzy C-means algorithm is used to classify the typical operation conditions of atmospheric distillation in oil refining process. Furthermore, the LSSVM method optimized with the improved particle swarm optimization is used to model the distillation rate of unit energy consumption. Then online optimization of oil refining process is realized by optimizing the outlet temperature, the overhead temperature with IPSO again. Simulation comparative analyses are made by empirical data to verify the effectiveness of the proposed solution.     

分散红146合成工艺改进

文章着重对分散红146的缩合工艺进行了改进,采用1-氨基-2-溴-4-羟基蒽醌潮品直接缩合,不但省去了原来烦琐的干燥工序和干燥设备、节省能源、降低生产成本,而且由于使用了溶剂进行脱水,其脱水更为彻底,不但滤饼中的水份能够完全脱尽,同时还能将缩合反应产生的水及辅助原材料中带入的微量水份一并及时馏出,加快了缩合反应速度,缩短了缩合反应时间,缩合温度也适当降低,减少了物料的焦化,不但产品质量得到明显提升,而且缩合收率也得到一定程度的提高。     

碳酸镁生产中热解热能的回收与利用

碳酸镁属于高能耗产品,其生产过程中热解部分的能量消耗约占整个生产过程的50%,如何降低热解过程的能耗,对碳酸镁的生产具有极其重要的意义。对以白云石碳化法工艺生产碳酸镁产品的热解工艺进行了改进,回收热解后热解液中的热能并重新用于热解,使热解过程的能耗降低约15%。改进后的热解工艺不仅回收了热能,降低能耗,而且使热解液出口的温度降低,对过滤设备的要求降低,减少了设备投资。     

含氯高聚物干燥工艺、设备的状况及发展趋势

综述了国内外氯化聚乙烯、聚氯乙烯及其他含氯高聚物的生产工艺，尤其是干燥工艺及设备的进展情况和发展趋势。指出干燥工艺及设备的开发重点是组合干燥方法、设备的系统化、自动化、专业化以及降低能耗。     

氯气干燥系统氯中水含量控制

介绍了电石法聚氯乙烯生产装置中,浓硫酸在氯气干燥中系统中的作用。分析影响氯中水含量的因素。在保证生产正常运行的前提下,分析了氯气干燥中降低氯中水含量的措施。指出通过合理的设备选型,加强工艺控制,最终可以将氯中含水质量分数控制在0.02%以下,达到节能降耗的目的。     

Drying of Mushroom Slices Using Hot Air Combined with an Electrohydrodynamic (EHD) Drying System

In this study, hot air combined with EHD drying is examined as an improved method for drying mushroom slices. The effects of three levels of voltage (17, 19, and 21 kV) and electrode gap (5, 6, and 7 cm) on the drying kinetics, time, effective water diffusion coefficient, and energy consumption of the EHD, pure hot air (provided within a chamber), and hot air combined with EHD drying systems were investigated. ANOVA showed that there were significant differences between EHD treatments and control (pure hot-air-drying treatment) for all of the investigated responses. Voltage and electrode gap factors had significant effects on all investigated responses. The results confirmed that the combination of EHD and hot air can significantly reduce the drying period, resulting in a greater effective water diffusion coefficient and drying rate and reduced energy consumption. As such, this technique offers a promising solution to the considerable energy consumption of the drying industry.     

Freeze drying process: real time model and optimization

Freeze drying is a separation process based on the sublimation phenomenon. This process has the following advantages compared to the conventional drying process: the material structure is maintained, moisture is removed at low temperature (reduced transport rates), product stability during the storage is increased, the fast transition of the moisturized product to be dehydrated minimizes several degradation reactions. Freeze drying process has not been studied well enough. In order to put it to practice, a mathematical model based on fundamental mass and energy balance equations has been developed, based on a deterministic mathematical model proposed by Liapis and Sadikoglu [Drying Technol. 15 (3–4) (1997) 791], and used to calculate the amount of removed water and amount of residual water. The proposed model contains the freeze drying equations, which are solved by the orthogonal collocation and polynomial approximation—Jacobi method. The results show that the dynamic mathematical model represents well the process and is especially well suited for real time optimization. As a case study to illustrate the model utilization in a real time optimization procedure, the freeze drying process was optimized by the method of Successive Quadratic Programming (SQP) used for solution of non-linear equations, for skimmed milk and soluble coffee. The optimization procedure showed to be an important tool to improve the process performance since lower energy consumption and hence lower cost has been achieved to obtain the product with the same quality.     

内热式惰性粒子流化床中膏状物料干燥模型

通过对惰性粒子流化床中膏状物料干燥机理的分析,得到了干燥时间及单位面积床层水分汽化量的数学计算式,可对干燥器的性能进行预测。采用带浸没加热管的惰性粒子流化床对膏状钛白物料进行干燥中试研究,采用气流式喷嘴将膏状物料分散成200～400μm的小液滴喷洒在惰性粒子表面进行干燥,探索了适宜的干燥条件,测定和确定了最佳的干燥工艺参数、操作参数和设备参数。结果表明:该干燥工艺能强化床内传热传质,促进高黏性膏糊状物料很好地分散,床层温度分布均匀,干燥器的操作弹性大,热量消耗低,干燥强度高,传热系数可达300W·m-2·K-1以上。