没食子酸的制备及应用

<正> 没食子酸又名五倍子酸,化学名为3,4,5-三羟基苯甲酸。广泛用于有机合成、制药、染料、轻工、国防和食品等部门。没食子酸一般是由林产资源——五倍子加工制得的。五倍子是我国的特产,其产量     

没食子酸生产技术(上)

没食子酸因原料不同,有天然与合成之分。天然没食子酸的生产有酸法和生物法,在我国以酸法生产为主,因为以酸法生产历史最长、技术成熟。本文着重介绍以五倍子为原料的工业没食子酸的酸法水解技术。没食子酸是利用五倍子或刺云实荚等原料,用酸(或碱)法、生物法水解制成的产     

HPLC法测定五倍子油膏中没食子酸的含量

采用高效液相色谱法测定五倍子油膏中没食子酸的含量。结果表明,五倍子油膏中没食子酸在0.1136~0.6816μg范围内线性良好(R=0.9998),回归方程为y=3217x+25.747,平均回收率为99.54%(RSD=0.75%)。该方法准确可靠、简便易行,可用于五倍子油膏中没食子酸的含量测定。     

中药五倍子中没食子酸甲酯的含量测定研究

建立有关中药五倍子中主要活性物质没食子酸甲酯的含量测定方法。通过超声波提取法从五倍子中提取活性物质没食子酸甲酯,并采用高效液相色谱法测定其含量。结果表明,没食子酸甲酯的线性范围为0.02～0.20μg,三批不同产地的五倍子药材中没食子酸甲酯的含量为0.36～0.63 mg/g。上述结果表明,本文所建立的基于高效液相色谱的含量测定方法简单有效,可作为五倍子药材的质量控制。     

没食子酸生产技术(中)

二、五倍子单宁的水解水解是没食子酸生产的主要工序,也是决定产品收率、成本高低的关键。 1.水解的原理及其影响因素五倍子单宁由没食子酰基与β-D-葡萄糖以酯键连接而成。在酸或酶的作用下,酯键很容易断裂分解成没食子酸和葡萄糖。     

酶法没食子酸工业化试产成功

由中国林科院林化所研制的发酵法五倍子或倍花制没食子酸生产技术于1988年8月20日通过工业化试产验收,年内将投入正常生产。微生物法制没食子酸工艺技术的研究成功,填补了我国发酵工业领域空白。没食子酸的用途,除人们熟知的常用于     

五倍子制备没食子酸的研究进展

没食子单宁是没食子酸与多元醇制成的酯,易在酸、碱、酶的催化作用下水解,由此可制备多种与没食子酸相关的衍生物.以五倍子为原料提取没食子酸的方法有化学法和生物法两种,与化学水解法相比,生物法最显著的特点是水解完全,水解副产物葡萄糖可作为能源与碳源被生物催化剂代谢,不仅提高了资源的有效利用率,而且发酵废液易于处理,有利于环境保护.     

没食子酸发酵新工艺(简报)

没食子酸发酵经1853年Van Tieghem,1913年Kundson,1926年Thom等研究知是黑曲霉(Asp.niger)和青霉作用的结果。我国三十～四十年代时,方心芳等前辈也曾选出黑曲霉No.316以五倍子的浸液进     

高转化率生物法制没食子酸研究

本文介绍由倍花上分离的１株黑曲霉酶解五倍子单宁生物转化制没食子酸试验结果。     

没食子酸标准样品的制备与定值研究

研究了没食子酸标准样品的制备、均匀性和稳定性检验及其定值方法。用五倍子单宁酸水解得到的没食子酸为原料,经精制得到高纯度的没食子酸标准样品。通过红外光谱、核磁共振、热重分析证实该标准样品的化学结构式。标准样品含量测定采用高效液相色谱面积归一化法,并通过了均匀性检验和稳定性检验(15个月)。经6个实验室的联合定值,没食子酸标准样品的含量值为99.96%±0.10%。     

转盘塔内甲基异丁基酮萃取湿法磷酸实验研究

溶剂萃取法是一种经济有效的湿法磷酸净化方法。在转盘塔中,以甲基异丁基酮（MIBK）为萃取剂,开展了净化湿法磷酸的实验研究。考察了搅拌转速、相比对磷酸萃取率、杂质离子选择性、洗涤效果和反萃效果的影响。研究结果表明：萃取过程适宜的相比（溶剂与磷酸的体积比）为4,搅拌转速为200~400 r/min,在此条件下磷酸萃取率为85%;洗涤过程的搅拌转速不应大于100 r/min,适宜的洗涤酸用量为溶剂相体积的10%~15%,在此条件下铁离子（Ⅲ）和镁离子脱除率均在90%以上、铝离子脱除率大于70%、硫酸根脱除率为50%~60%;反萃过程搅拌转速不应大于200 r/min,适宜的反萃水用量为溶剂相体积的9%~15%。MIBK对阳离子的脱除效果较好,但是对阴离子的脱除效果不佳。经过萃取、洗涤和反萃3个过程,磷酸收率为57.8%~70.3%,磷酸中铁离子（Ⅲ）含量可以达到工业级磷酸标准,但是硫酸根的含量无法达标,需要结合其他方法进一步脱除。     

Catalytic ozonation of phenolic compounds: The case of gallic acid

The catalytic ozonation of gallic acid has been carried out in the presence of a perovskite type material (LaTi_0.15Cu_0.85O₃). Some of the main operating parameters like temperature, catalyst and ozone doses exerted a positive influence in the ozonation rate. Contrarily, initial gallic acid concentration showed a negative effect in terms of conversion while the optimum working pH was found to be around 2 (3.5 if deactivation is avoided). Addition of tert-butyl alcohol (free radical scavenger) had no effect on the catalytic removal of gallic acid, although its presence decreased the mineralization degree achieved. The catalyst demonstrated a high stability in terms of the acid removal, however, a partial deactivation was experienced in terms of organic carbon elimination if compared the first and second reuses. The catalyst kept its activity after further reutilisations. Due to the moderate regime developed in the homogeneous phase, the process was better simulated by an empirical expression rather than using a detailed model.     

Solvent Extraction of Cyclohexanecarboxylic Acid From Waste Fluid by Using a Mixture of Toluene and 1-Octanol

Solvent extraction studies have been carried out for the recovery of cyclohexanecarboxylic acid (CCA) from simulated waste fluid. Influences of various parameters including extractant types, pH of the solution, equilibration time, and initial concentrations of CCA, etc., were studied. A mixture of toluene and 1-octanol (90:10, v/v) was found suitable for the extraction. The results showed that solution pH had a great effect on the distribution ratio, and CCA could be efficiently extracted when the pH was lower than 3.5. The extraction was found quite rapidly. The distribution ratio decreased as the initial concentration of CCA increased. The stripping rate of CCA using sodium hydroxide as stripping agent was found to be increased with the increase of alkali concentration. After back extraction once, more than 98% stripping efficiency was achieved with 0.8 mol/L sodium hydroxide solution at aqueous to organic phase (A/O) ratio 1:1 when CCA concentration was lower than 38.3 g/L. The practical extraction process was carried out for the waste fluid (concentration of CCA 36.5 g/L) discharged in the production of caprolactam from toluene. After four extraction stages at A/O ratio 1:1, the cumulative extraction recovery reached 99.3%. The practical stripping efficiency from loaded organic phase reached 98.2% in one single stage.     

Study of lactic acid extraction with higher molecular weight aliphatic amines

Lactic acid extraction was studied with two extractants, trioctyl amine (TOA) and Aliquat 336, in three diluents (methylisobutyl ketone (MIBK), octanol and paraffin liquid). The effects of organic phase extractant concentration and aqueous phase pH on the extraction process were examined. Among the extractants, TOA was found to be a better extractant than Aliquat 336 in all the diluents. In experiments with 50% (v/v) TOA in methylisobutyl ketone, 79% lactic acid could be extracted (initial lactic acid concentration 86·96 g dm⁻³). MIBK had a profound effect on the extraction behaviour of TOA in comparison with octanol and paraffin liquid while none of the diluents affected the extraction with Aliquat 336. The extraction of lactic acid was favoured at low pH. The toxicities of TOA and the diluents to Lactobacillus rhamnosus NRRL B445 were also studied. While TOA was found to be highly toxic at the molecular and the phase level, the paraffin liquid was totally non-toxic. The extraction of glucose and yeast extract by TOA and the diluents used was found to be low, which thus enables the selective extraction of lactic acid. © 1998 SCI     

用磷酸三丁酯萃取分离硫酸铵母液中的HCN

研究了磷酸三丁酯(TBP)-磺化煤油体系从重庆某企业甘氨酸生产副产物硫酸铵母液中萃取分离HCN的工艺,考察了萃取体系、TBP体积分数、母液初始pH值、相比(Vorg∶Vaq)对萃取HCN的影响以及氢氧化钠浓度、相比(Vaq∶Vorg)和平衡pH值对HCN反萃的影响。结果表明:选用TBP作为萃取剂能够对硫酸铵母液中的HCN进行快速有效的萃取;TBP体积分数、母液初始pH值及相比对HCN萃取率影响显著;以含体积分数35%TBP的有机相作萃取剂,在相比(Vorg∶Vaq)为2∶1的条件下,pH值为2.92的含氰1.71 g/L的硫酸铵母液经3级错流萃取,萃余液中含氰低于0.5 mg/L,氰的萃取率接近100%;在相比(Vaq∶Vorg)为1∶1条件下,以0.6 mol/L的氢氧化钠为反萃液,控制反萃液平衡pH值大于13.0,氰的单级反萃率大于96%;含氰0.78 g/L的有机相在相比为1∶1条件下,经过2级错流反萃,氰基本上被反萃完全,贫有机相不经过处理可循环使用。     

Recovery of Fumaric Acid from Industrial Wastewater by Chemical Extraction and Stripping

Abstract

The study on chemical extraction and stripping for the recovery of fumaric acid from low concentration organic acid wastewater has been carried out. The parameters influencing the extraction efficiency were investigated, including extractant concentration, the initial pH, the volume ratio of water to oil (W/O), the extraction temperature, and the concentration of n‐octanol. The heat effect of the extraction process, the formation of acid‐amine complexes, and the corresponding equilibrium constant were determined. In the optimum condition that kerosene/N₇₃₀₁/n‐octanol was 2:2:1, pH was 0.5, W/O was 1:1, and the temperature was 303K, through chemical extraction and stripping, the COD_cr value of fumaric acid wastewater decreased from 71040 mg/l to 8411 mg/l, and the overall COD_cr removal rate reached 88.16%, and the extraction efficiency of fumaric acid was 70.67%. The extractant was regenerated by a stripping process with 2% NaOH, and the stripping rate almost arrived at 100%. The regenerated extractant was cycled seven times without decreasing extraction efficiency and the stripping rate. And fumaric acid was obtained by adjusting the pH of the salt from stripping. After extraction, the fumaric acid wastewater can be further treated by oxidation or biodegradation to environmentally acceptable levels.     

甲基异丁基酮净化湿法磷酸的研究

湿法磷酸含有较多杂质,通过净化可拓宽其用途。以甲基异丁基酮为溶剂,采用溶剂萃取法净化湿法磷酸。研究了相比、萃取时间、搅拌转速、反萃剂加入量对五氧化二磷分配系数、氟离子和硫酸根选择性的影响。实验结果表明：相比对五氧化二磷分配系数影响明显,但对硫酸根的选择性影响不明显;萃取时间、搅拌转速对五氧化二磷分配系数影响并不明显;甲基异丁基酮对氟离子和硫酸根均有良好的选择性。相比（有机相与水相的体积比）为4∶1、萃取时间为10 min、搅拌转速为200 r/min、反萃剂加入量为萃取后萃取剂体积的15%,净化效果较佳。     

Extraction and recovery of rhodamine B,methyl violet and methylene blue from industrial wastewater using D2EHPA as an extractant

The extraction behavior of cationic dyes namely rhodamine B (RB), methyl violet (MV) and methylene blue (MB) from industrial wastewater has been investigated using di-(2-ethylhexyl) phosphoric acid (D2EHPA) in hexane as a carrier. The extraction of cationic dyes increases with decreasing feed phase pH and increasing D2EHPA concentration in organic phase. The stripping percentage of dyes using acetic acid as the stripping agent from loaded D2EHPA was found to increase with increasing acid concentration. 98% stripping efficiency of dyes was achieved with 8.5 mol/L acetic acid solution at an organic:aqueous phase ratio (O/A) of 2:1. Parameters examined include D2EHPA concentration, effect of diluents, effect of pH, effect of initial dye concentration, equilibration time, and various stripping agents, aqueous to organic phase ratio in extraction and organic to aqueous phase ratio in stripping.     

络合萃取法对煤制气高浓度含酚废水的资源化处理

用磷酸三丁酯(TBP)为萃取剂和煤油为稀释剂,对煤制气过程中产生的高浓度含酚废水进行了络合萃取处理,并用氢氧化钠溶液为反萃取剂对负载有机相进行了反萃取。分别研究了废水pH、TBP体积分数对萃取及氢氧化钠溶液浓度对反萃取的影响,并对萃取和反萃取过程中有机相的重复使用问题进行了探讨。结果表明,当废水的pH为3～6时,萃取率可达90%以上,CODCr去除率达到80%以上;当氢氧化钠质量分数为4%～10%时,反萃取率可达80%以上;TBP-煤油有机相可在萃取和反萃的过程中多次重复使用。     

响应曲面法优化木薯酒精污泥基活性炭制备及对没食子酸的吸附性能

以木薯酒精厂生产过程中产生的脱水污泥为原料,采用响应曲面法 Box-Behnken模型优化了木薯酒精污泥基活性炭的制备工艺,同时对最优成品进行一系列表征分析,并将其应用于没食子酸废水的处理研究。活性炭的最优制备条件为活化温度489℃,浸渍时间14 h,活化时间51 min,氯化锌浓度21.53%,该条件下样品的碘吸附值达521.64 mg/g。表征分析显示其表面布有众多孔壁较薄、大小不一的孔洞,金属含量较小,BET比表面积达441.86 m²/g,平均孔径为2.50 nm,拥有丰富的微孔结构,表面富有较多的含氧官能团。考察了活性炭投加量、pH、接触时间、溶液温度对样品去除水中没食子酸的影响。结果表明,样品能够高效去除没食子酸,且随着投加量的增加和pH值降低,没食子酸的去除率呈增长趋势。木薯酒精污泥基活性炭对没食子酸的吸附符合pseudo second-order动力学模型和Freundlich等温模型,最大吸附量为126.72 mg/g。扩散机理显示除颗粒内扩散外也包含液膜扩散过程。热力学分析表明该吸附反应是自发进行的吸热且熵增的过程。本研究将为制备高性能污泥活性炭并应用于高浓度天然有机物废水处理提供理论基础。