Boron phenolic resin is a polymer with good heat resistance and low cost, and its initial decomposition temperature can reach more than 350 ℃. The synthesis methods, properties and modification methods of boron phenolic resin were reviewed. The results show that the synthesis of boron phenolic resin by blending method has the problems of incomplete reaction of boron source and unstable modification effect. The salicyl alcohol method has the problem of low yield, but the preparation process is easy to control and the product quality is stable. The modification effect of solid phase synthesis is relatively good, but the reaction conditions are higher. The modification of boron phenolic resin mainly includes toughening modification, water resistance modification and heat resistance modification. The future development trend of boron phenolic resin is prospected in order to provide some reference for the research in this field.

锰矿中有毒有害元素对锰提纯工艺、生产环境和产品质量的影响,一直是困扰锰行业发展的技术难题,也是实验测试亟需解决的质量基础共性技术问题.目前,国内外现有的锰矿石成分分析标准物质共有10个,定值成分有Mn、Fe、Al2 O3和SiO2等17种,均缺乏Cl、F、Pb、Cd、Co、Cr、Hg和As等有害成分的定值,从而无法满足锰提纯工艺研发、环境监测评估、锰矿进口监督、检测方法评价等需要.本文研制了2个锰矿石成分分析标准物质(GBW07139、GBW07140),候选物样品采自湖南省和新疆自治区的3个大型锰矿区,根据矿床类型采用单独或组合方式进行样品制备,样品全部通过97μm标准筛和均匀性初检,并分装为最小包装单元.通过对随机抽取的2×30瓶样品进行均匀性检验,F实测值均小于F0.05(29,60)=1.59,且相对标准偏差为0.45％～6.44％,表明样品的均匀性好.在一年时间内进行长期和短期稳定性检验,采用线性模型/平均值一致性数据统计,未发现统计学意义的明显差异,表明样品的稳定性好.通过10家实验室对Mn、MnO2、SiO2、Al2 O3、Fe、CaO、MgO、K2 O、Na2 O、TiO2、S、P、Cu、Co、Zn、Ni、Pb、Cd、Hg、Cr、As、Cl、F共23种成分进行协作定值,2个锰矿石成分分析标准物质中Mn质量分数分别为21.63％和41.55％,Cl质量分数为38×10-6和1214×10-6,Ni质量分数为1075×10-6和30.9×10-6,具有较宽泛的含量范围和代表性.该批锰矿石成分分析标准物质实现了锰矿石成分分析标准物质中Cl、F、Pb、Cd、Cr、Co、Hg和As成分的定值,适用于锰相关分析检测质量控制.

以过硫酸钾为引发剂,壬基酚聚氧乙烯醚(NP-10)和烯丙基聚乙氧基磺酸盐(SE-1ON)为复合乳化剂,水溶性低分子有机脲为链转移剂,乙酸乙烯(VAC)、丙烯酸丁酯(BA)、丙烯酸-2-乙基己酯(2-EHA)和甲基丙烯酸(MAA)为主要原料,采用种子乳液聚合法合成塑料瓶用新型标签黏合剂.考察了单体用量、引发剂用量、乳化剂用量和链转移剂用量对产物性能的影响.研究结果表明:当w(单体)=20％[m(VAC)∶m(BA)∶m(2-EHA)∶ m(MAA)=1∶12∶3∶4]、w(引发剂)=0.2％、w(乳化剂)=0.6％、w(链转移剂)=0.25％(均相对于体系总质量而言),该条件下黏合剂的综合性能最佳.

石煤钒矿资源的开发和合理利用需要对其成分进行准确的分析测试和质量控制.目前,国内外尚未有石煤钒矿成分分析的标准物质,现有钒成分分析标准物质无论是其五氧化二钒含量,还是定值成分都无法满足我国对石煤钒矿勘查、开发和研究需要.本文对采自湖北省崇阳县小源冲钒矿、湖南省芷江县牛牯坪钒矿、湖南省古丈县岩头寨钒矿和湖南省凤凰县黑冲钒矿等4个大型石煤钒矿区样品开展了标准物质研制工作,研制了4个石煤钒矿成分分析标准物质(GBW07875、GBW07876、GBW07877、GBW07878).将矿层样品、顶底板岩石和人工剥离高品位样品,经过颚式初碎、对辊中碎、粗粒过筛混匀、配矿混匀、盘式细磨、细粒过筛、灭活混匀等加工处理,经初检合格后,装瓶和编号.随机抽取的4×35瓶样品进行均匀性检验,F实测值均小于F0.05(34,70)=1.60,且相对标准偏差(RSD)在0.31％～7.48％之间,表明样品的均匀性好.对随机抽取样品进行长期稳定性检验和短期稳定性检验,结果没有发现统计学意义的明显差异,表明样品的稳定性良好.通过9家实验室参加协作定值研究,定值成分包括V2 O5、C和SiO2等共16种成分,其中4个石煤钒矿成分分析标准物质中的V2O5的质量分数分别为0.63％、0.86％、1.55％、3.99％,涵盖边界品位0.50％、工业品位0.70％、富矿品位≥1％,碳含量分别为2.40％、3.46％、5.60％、7.27％.本批次4个标准物质的研制成功,可为石煤钒矿的科学利用和研究提供参考和借鉴.

N-氰乙基-N-羟乙基苯胺是一种具有广泛用途的染料中间体,针对传统合成方法中的缺陷,以1-丁基-3-甲基咪唑硫酸氢盐([BMIM]HSO4)为催化剂,丙烯腈和N-羟乙基苯胺为原料,建立了N-氰乙基-N-羟乙基苯胺的绿色合成新工艺.系统考察了离子液体种类、离子液体用量、底物比例等因素的影响规律,结果表明,[BMIM]HSO4用量为0.8 mmol,n(N-羟乙基苯胺):n(丙烯腈)=1:1.2,反应温度为90℃,反应时间为12 h时,N-氰乙基-N-羟乙基苯胺产率最高(89％),离子液体循环使用5次后,催化活性基本保持不变.

以过量甲苯二异氰酸酯和聚乙二醇为主要原料制备预聚物;以三乙烯二胺为催化剂,聚乙二醇二丙烯酸酯为交联剂,预聚物和巯基乙醇反应制备巯基聚醚聚氨酯橡胶.考察了催化剂用量和交联剂用量对产物性能的影响,采用变温红外光谱和拉曼光谱对其温敏性进行了研究.结果 表明:催化剂用量0.8％,交联剂用量1.0％,产物性能最佳;200℃以下样品的红外吸收峰受温度变化影响不大;200℃时,样品在2 273 cm-1处出现-N=C=O特征吸收峰,同时2 583 cm-1处的—SH特征伸缩振动吸收峰消失.

以桐油和二乙醇胺为主要原料,反应制备桐油酰胺.采用傅里叶变换红外光谱(FTIR)和拉曼光谱对桐油的结构进行表征,并进行了谱带归属;用傅里叶变温红外光谱(temperature-dependent FTIR)对合成产物的温敏性、谱带变化和双键变化进行了研究.结果表明:1630 cm-1和991 cm-1为桐油的红外和拉曼特征吸收峰;25～225℃范围内,桐油酰胺变温红外光谱在1737 cm-1(—C=O—)处吸收峰的吸光度随着温度升高而逐渐增大;温度高于125℃,991 cm-1处的—CH=CH2键断裂,产物发生分解;找出了桐油酰胺应用的温度条件.

在小试试验基础上,对合成AA/AMPS/DMDAAC阻垢分散剂进行了半吨级中试研究,并进行了反渗透水处理剂的中试研究.中试产品反渗透水处理剂和美国King Lee公司PTP-0150反渗透水处理剂进行了应用对比实验.结果表明:中试阶段AA/AMPS/DMDAAC共聚物阻垢分散剂的阻垢率数据略低于小试阶段;两种反渗透水处理剂的阻垢、分散性能相当;中试产品反渗透水处理剂应用于反渗透水处理系统时,系统脱盐率在97.57％以上,水的回收率在86.5％以上,满足工业应用需求.

研究了水解法制备α,ω-二羟基聚二甲基硅氧烷的过程,通过傅里叶变换红外光谱学(FTIR)、氢核磁共振(H1 NMR)对水解产物的结构进行了严格的归属,表明二甲基二乙氧基硅烷(DMDES)水解后可生成α,ω-二羟基聚二甲基硅氧烷.此外,产物结构受水含量的影响较大,过量水解有利于形成端羟基聚硅氧烷,含水量不足则生成端乙氧基聚硅氧烷.通过黏均分子量测试,发现由于可逆的解聚反应的存在,聚合度受反应温度和反应时间等因素的影响不大,不同反应条件下分子量稳定适中,均处于1 500～3 000范围,可作为改性剂使用,改善聚合物的耐热性和耐水性.

以聚乙二醇单甲醚衣康酸酯、聚乙二醇单甲醚甲基丙烯酸酯、N-[4-(磺酰胺)苯基]丙烯酰胺为聚合单体,采用大单体直接共聚法,合成早强型聚羧酸系高分子减水剂.对单体摩尔分数、引发剂用量、反应温度等反应条件进行系统考察,得到最佳合成工艺参数:聚乙二醇单甲醚衣康酸酯、聚乙二醇单甲醚甲基丙烯酸酯、N-[4-(磺酰胺)苯基]丙烯酰胺的摩尔分数分别为35％,35％,30％,引发剂用量为3％(占单体总量),反应温度80℃,反应时间5 h.与传统聚羧酸系高分子减水剂进行对比的实验结果显示,所合成的早强型聚羧酸系高分子减水剂在减水率及抗压强度等方面都有更好的效果.

压裂技术是提高低渗透油气藏生产能力和油气井采收率的重要手段,而压裂液是影响压裂效果的关键因素.相较于水基植物胶压裂液和以单链表面活性剂为稠化剂的传统清洁压裂液,双子表面活性剂类清洁压裂液在耐温、携砂和保护油气层等使用性能上更具优势,是新一代清洁压裂液发展重点.本文综述了双子表面活性剂类清洁压裂液制备、性能及应用的研究进展,分析比较了阳离子双子表面活性剂类清洁压裂液、阴离子双子表面活性剂类清洁压裂液、两性双子表面活性荆类清洁压裂液等的优缺点,讨论了双子表面活性剂类清洁压裂液在油田领域的应用现状:阳离子双子表面活性剂类清洁压裂液的制备方法成熟,耐温性能较好,可以应用于中高温油田,但是其生产成本较高;阴离子双子表面活性剂类清洁压裂液能有效减少表面活性剂在地层的吸附损失,降低储层渗透率伤害,但是其合成条件苛刻,耐温性不高,适用于中低温油田;两性双子表面活性剂类清洁压裂溶液的耐温性好,但是其制备过程繁琐、成本高,难以大规模推广应用.对双子表面活性剂类清洁压裂液的研究前景进行了展望:发展低成本的合成方法及耐高温双子表面活性剂类清洁压裂液的制备及应用.

According to the study on the technological mineralogy of a medium-high temperature fluid fissure filling metasomatic type tin-polymetallic ore from Hunan province, the mineral com-positions of the ore are complex. The main valuable elements are tin and bismuth,followed by cop-per,fluorite and silver. The primary minerals for these elements are cassiterite,bismuthinite,chal-copyrite and isomorphism minerals in a variety of sulfide ore,respectively. Therefore,the valuable minerals are mainly cassiterite,bismuthinite and a small amount of natural bismuth, chalcopyrite, fluorite,and chalcocite,etc. Except for the fluorite,the useful minerals have fine dissemination si-zes and closely symbiotic relationships,which makes the ore refractory. Based on this study,some suggestions for the utilization of this tin-polymetallic ore are put forward.

我国现行国家标准GB 5009.5—2016《食品中蛋白质的测定》中的杜马斯(Dumas)燃烧法是先将样品燃烧测出含氮量,然后根据氮元素与蛋白质换算系数计算蛋白质的含量,如果添加含氮量高的物质,如三聚氰胺,就可以测出较高的"蛋白质含量".采用普通FTIR光谱定性鉴别出奶粉的主要组成成分,然后用杜马斯燃烧法准确测出奶粉中的氮元素和碳元素含量,通过蛋白质换算系数计算出蛋白质含量,可以避免上述由于添加违规化学物质造成测定蛋白质含量虚高的结果;同时通过C/N元素含量比,进一步印证奶粉中的营养成分组成.

Adipic acid was synthesized by catalytic oxidation using NO2 as oxidant and homemade absorption tower for reaction to the generator.The product was characterized by FTIR.The results show that the synthetic product is adipic acid.The effects of reaction temperature,reaction time and the velocity of NO2 etc.factors on the yield of adipic acid were studied by single-factor method for optimizing the synthesis conditions.The optimal experimental conditions are the velocity of NO2 0.3 L/min,the reaction temperature 50-60 ℃,the reaction time 6 h.Under this condition,the yield of adipic acid can reach 87.4 ％,and the absorption of cyclohexanol to NO2 is 98.9 ％ on average.In addition,this experimental method provides a new way for the recovery and utilization of NO2.

Acetic acid bacteria are the core microbes in vinegar industry,and the most commonly used strain is Acetobacter.Results showed that many acetic acid bacteria,which were tolerant to high ethanol and temperature,could also keep high production of acetic acid.The discovery of these acetic acid bacteria had brought new insights into the modern brewing industry,and it was advantageous to the characteristics of acetic acid bacteria mining with different growth and metabolism and new brewing process development.This paper reviewed the current application progress on the properties and application of acetic acid bacteria with high tolerance of ethanol and temperature in the brewing industry.It would be of great significance for screening more acetic acid bacteria with high tolerance and improving the brewing technology.

利用专利实验炉,研究了氧化锰矿石还原焙烧过程中铁还原率的评价方法.该方法可用于指导氧化锰矿石还原焙烧过程中铁还原的控制,具有实用性.

In order to obtain fracturing fluid with high temperature resistance,a gemini surfactant was synthesized with stearic acid,oxalic acid,N,N-dimethylbenzene-1,4-diamine,N,N'-(ethane-1,2-diyl)diethane-1,2-diamine and 1,3-dichloro-2-propanol as the materials. Using this gemini surfactant as viscosifier,a cleaning fracturing fluid was prepared by mixing ammonium chloride solution and gemini surfactant. The performance of cleaning fracturing fluid(3％gemini surfactant+1％NH4C1),such as heat and shear resistance,sand-carrying property,gel-breaking property and so on,was investigated. The results showed that comparing with guargum fracturing fluid,this cleaning fracturing fluid was thermally stable and had good temperature and shear resistance. The viscosity of cleaning fracturing fluid was 88 mPa·s at 120℃,which could meet the requirement of high temperature oil and gas field. The sedimentation rate of seed in cleaning fracturing fluid was 0.79 mm/s at 120℃,which indicated that the cleaning fracturing fluid had a good sand-carrying performance. The compatibility between cleaning fracturing fluid and formation fluid was good. The cleaning fracturing fluids would break automatically when it encountered lamp kerosene,without adding gel breaker, which was very convenient to use.

某金矿石金品位1.98 g/t,嵌布粒度较粗,79.00%的金以裸露及半裸露金的形式存在.为合理开发利用该金矿资源,进行选矿试验研究.结果表明,矿石适宜采用尼尔森选矿机先回收粗粒金、重选尾矿采用丁基黄药+丁铵黑药作组合捕收剂进行浮选提金.在磨矿细度-0.074 mm 69.8%的条件下,原矿1粗2精重选—重选尾矿1粗3精2扫闭路浮选试验可获得重选金精矿品位5250.00 g/t、回收率53.03%和混合金精矿(重选中矿与浮选精矿合并)品位41.26 g/t、回收率42.52%的良好指标,实现了该金矿资源的高效回收利用.

湖南某低品位硫化铜矿铜品位0.603%,铜主要以硫化铜的形式存在.为有效回收利用其中的铜,采用浮选法进行选矿试验.结果表明,原矿磨矿至-0.074 mm 70.82%,以碳酸钠为矿浆pH调整剂、丁胺黑药+丁基黄药为组合捕收剂,经1粗1精1扫、中矿顺序返回闭路浮选流程选别,可获得铜品位23.56%、回收率88.34%的铜精矿,达到铜精矿三级品要求,可供最终工艺流程的选择参考.

Using the ionic liquid as the catalyst,the gemini surfactant is synthesized by multicomponent domino reaction with the materials palmitic acid,erucic acid,N,N-dimethyl-1,3-propane diamine and 1,3-dichloro-2-propanol.Comparing with the traditional methods,the new procedure is fitter for industrial production,because of the atom economy,simple preparation process,lower energy consumption and cost.A cleaning fracturing fluid is prepared by using this gemini surfactant as viscosifier.This cleaning fracturing fluid is thermally stable and has a good temperature resistant capacity which has the shearing resistance and good sand-carrying performance.