南工大化工复试英语

文献阅读： PATENT SPECIFICATION GB851,690 NO DRAWINGSDate of Application and filing Complete Specification:June 26, 1959 No. 22094/59.Application made in Germany on Aug. 21, 1958.Complete Specification Published: Oct. 19, 1960. Index at Acceptance: -Class 1(3), Ain46A.International Classification: -C01f. COMPLETE SPECIFICATIONMethod of Dehydrating Barium Hydroxide Hydrate We, Kali-CHEMIE AKTIENGESELLSCHAFT, of Hans Bckler Allee 20, Hannover, Germany, a body corporate organized under the laws of Germany, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement:-This invention relates to a method of dehydrate barium hydroxide 氢氧化钡hydrates. 水和Barium hydroxide octahydrate八水合, monohydrate, and anhydrous barium hydroxide are known as well defined compounds. Products having varying contents含量 water of crystallization结晶水 between the mono- and the octahydrate are also industrially used. Barium hydroxide octahydrate congruently 一致的melts in its own water of crystallization. The water cannot be removed from this solution otherwise than by prolonged heating at temperatures up to 300. The process is accompanied by troublesome spattering飞溅 and incrustation结壳 phenomena. An improvement can be achieved by dehydrating under reduced pressure at a temperature of about 130 . The barium hydroxide octahydrate will then, when slowly heated, lose part of its water of crystallization at temperature below its congruent同成分 melting point of 78, so that the solid state is preserved throughout the dehydrating process. A drawback of this method is the long time the process of dehydration takes to perform, the water of crystallization being released extremely slowly. In both cases it is impossible quantitatively定量的 to control the degree of dehydration attained in the course of the process.It has now been found that the water of crystallization can be withdrawn除去 from the barium hydroxide hydrate either by heating the same in an organic solvent, the water being azeotropically 共沸distilled off with the solvent, or by removing it from the barium hydroxide hydrate merely by digestion浸提 in a suitable solvent at elevated temperature升温. It is, however, necessary to select a solvent which is chemically inert to化学惰性的barium hydroxide, but the selected solvent may be a solvent mixture.Organic solvents which, in the liquid phase, are not miscible 可混合的with water in any proportion比例 have been found to be especially useful for performing the azeotropic distillation共沸精馏, so that the continuous and complete separation of the water can be effected实现 in a receiver接收器 fitted with an overflow溢流口. It is then possible to dehydrate relatively large quantities of barium hydroxide hydrate with the aid of a constant quantity 一定量的of solvent. In the case of barium hydroxide octahydrate a solvent must be selected which has a boiling point 沸点near the congruent melting point 同成分熔点of 78，and an azeotropic boiling point共沸点 which below this melting point. The process of dehydration can be discontinued中断 when a desired期望的 quantity of water has been removed so that barium hydroxides in any desired stage of hydration期望的结合水含量 can thus be obtained. For lower hydrates of barium hydroxide the selection of a suitable solvent is not determined in the above manner, and the boiling point of pure solvent and of the azeotropic mixture共沸混合物 should be above and as close as possible respectively相应的 to the boiling point of water. In an alternative procedure备选过程 of heating the barium hydroxide hydrates with an organic solvent, the water of crystallization is removed by digestion浸提 in an anhydrous organic solvent or solvent mixture which is chemically inert with respect to考虑到 barium hydroxide but miscible可混合的 in the liquid phase with water in any proportion, the process being performed at a temperature above the congruent同成分 melting point of the barium hydroxide octahydrate and below the boiling point of the solvent or solvent mixture. It has been proposed to dry pastes糊状物 or sludges 烂泥状consisting of fine particles of hydrophobic憎水的 solids, by a method which consists in mixing the pastes with a second liquid which is substantially immiscible完全不能与之混合 with water and which has a greater adhesive粘合性的 affinity 亲和力with solid than water, and then separating the solid from its water by the displacement置换 of the water, the second liquid being then removed by evaporation蒸馏 until the paste糊状物 is dry. Suitable displacing liquid are for instance toluene甲苯 or other benzene homologues苯同系物, as well as various chloro-hydrocarbons氯代烃. The major proportion of the adhesively bound 粘附的water is removed from the aqueous pastes 含水糊状物after their flowability 流动性has possibly first been improved by the addition of further water, the water being displaced by the second liquid and separated without the application应用 of heat, for instance by filtration过滤. Small residues残留物 of water still attached by the hydrophobic solid are azeotropically distilled off together with the second liquid. The object 目的of the method is to dry otherwise原来 difficultly drying aqueous pastes consisting of fine particles of hydrophobic solids by utilising the higher wetting strength 润湿能力of the second liquid in relation to water与水相比, the method at the same time affording economies in the consumption of thermal energy.In contradistinction区别 thereto另外, the present method relates to dehydration脱水, that is to say to the removal of water of crystallisation from barium hydroxide hydrates, which is bound by covalent bonds共价键 and in practice实际上 produces compounds of distinctive独特的 properties. Dehydration is performed whilst同时的 heating the dry hydrated initial substance, either by azeotropic distillation of water of crystallisation with a solvent known to be suitable for such a purpose, or by digestion at a given temperature in an anhydrous organic solvent which is miscible with water in any proportions, and then filtering. The object as well as the manner of performing the two methods are therefore different.The present invention will now be illustrated by the following examples:-EXAMPLE 1.150g Ba(OH)2.8H2O were slowly heated, whilst同时 being stirred, with 500cc. benzene under reflux 回流with a receiver fitted with an overflow溢流管. At the boiling temperature viz.即 69.3 of the azeotropic mixture of benzene and water, the first distillate蒸馏物 appeared. At the end of 90 minutes a quantity of water representing 相当于7 molecules of water of crystallisation had collected in the receiver. In the course of further heating the temperature rose to 80.2. Not until 直至fresh Ba(OH)2.8H2O had been added did the temperature drop and the process of dehydration continue. Finally the benzene suspension悬浮物 of the barium hydroxide which had been dehydrated to the monohydrate was drained排出 and filtered, adhering benzene being removed from the substance by brief 简单的evacuation抽空. The benzene filtrate was immediately re-used for further dehydration.EXAMPLE 2.100 g. of barium manohydrate obtained in accordance与。一致 with Example 1 was treated with 300 cc. of toluene in the same manner as that described above. Dehydration could now be continued to completion完全 and the anhydrous barium hydroxide obtained. The boiling temperature of the azeotropic toluene and water mixture was 84.1 .EXAMPLE 3.50 g. Ba(OH)2.8H2O were digested浸提 in 1000 cc. of anhydrous dioxane无水二氧杂环乙烷 at 80 , the mixture being vigorously剧烈的 stirred. At the end of one hour the mixture was filtered. The barium hydroxide appeared in the form of the monohydrate.WHAT WE CLAIM IS: 1. A method of dehydrating barium hydrates, where the water of crystallisation is extracted by heating in an organic solvent or solvent mixture which is chemically inert to barium hydroxide.2. A method as claimed in Claim 1, wherein在其中 the water of crystallisation is removed by azotropic distillation with an organic solvent or solvent mixture that is chemically inert to barium hydroxide.3. A method as claimed in Claim 1, wherein the water of crystallisation is removed by digestion in an organic solvent or solvent mixture which is chemically inert to barium hydroxide but is miscible with water on any proportions, the process being performed at a temperature above the congruent melting point of barium hydroxide octahydrate and below the boiling point of solvent or solvent mixture.4. A method of dehydrating barium hydrates substantially 充分地as hereinbefore以上 described in any one of the foregoing examples.W.H.A. THEIMANN,Prestige House,14 to 18 Holbone,London, E.C.1,Agent for the Applicants我们德国法律下组织的一个法人团体，据此宣布一项发明以及本发明的实施方法，希望能够批准我们的专利。以下相关的描述和声明。本发明是有关水和氢氧化钡脱水的方法。八水合，一水合及无水氢氧化钡都是定义明确的化合物。结晶水含量在一到八之间的氢氧化钡也是工业上常用的。八水合氢氧化钡同成份熔融于其结晶水中。这些水只有通过长时间的在300以上加热才能从溶液中除去。这个工艺伴随着讨厌的飞溅和结壳现象。对该方法的改进措施是在大约130时减压条件下脱水。当缓慢加热时，八水合氢氧化钡将在温度低于其同成份熔点即78时失去部分结晶水，从而在整个脱水过程中固态物质得以保存下来。这种方法的一个缺点是所进行的脱水过程时间长，结晶水释放非常缓慢。两种情况下都不可能在过程工艺中定量控制脱水的程度。现在发现有两种方法可以从水合氢氧化钡中除去水：将其在某一有机溶剂中加热，通过共沸蒸馏水可以与溶剂一起除去；或在升温条件下用合适的溶剂从水合氢氧化钡中浸提出去。所选择的溶剂必须对氢氧化钡是化学惰性的，且可能是一种混合溶剂。液相时以任意比例都不能和水混合的有机溶剂在进行共沸蒸馏时是特别有用的，因此使用装有溢流口的接收器可以连续的并完全将水分离出去。因此使用一定量的溶剂就可能使大量的水和氢氧化钡脱水，对于八水合氢氧化钡，所选择的溶剂其沸点应与同成份熔点即78相近，共沸点必须低于此熔点。当一定量的水被除去时，脱水过程可以随时中止，因此可以获得所希望结晶水数目的氢氧化钡。对与结晶水数目较少的氢氧化钡，合适溶剂的选择与上述不同：纯溶济和共沸混合物的沸点应分别高于及尽量接近水的沸点。在另一个把水合氢氧化钡与有机溶剂一起加热的过程中，结晶水是通过一种无水的有机溶剂从溶剂混合物浸提除去，这种有机溶剂对于氢氧化钡是化学惰性的，且在液相可以与水以任意比例互溶，脱水过程的温度高于八水合氢氧化钡的同成份熔点而低于溶剂或溶剂混合物的沸点。一种干燥由微小的憎水颗粒组成的糊状物或淤泥状物的方法是将其与第二种液体混合，该液体完全不能与水混溶，而且与固体之间的胶粘亲和力大于水，通过置换水的方法把水与固体分开，第二种液体可以通过蒸馏的方法移去，直至糊状物干燥。合适的置换液体如甲苯或其它苯的同系物，以及各种氯代烃。大部分的粘附的水可以通过这种方法由含水糊状物中除去：进一步加入水后，其流动性可能得到改进，水被第二种液体取代后无需通过加热，可由简单的方法如过滤分离出去。少量仍然粘附在憎水固体的水可以与第二种液体共沸蒸馏除去。这种方法的目的是通过使用一种与水相比润湿能力较强的液体来干燥一些难以干燥的。由憎水固体的细小颗粒组成的糊状物。同时本方法从消耗热能的角度来说是较为经济的。与以上方法的区别是，本方法是与脱水相关，即从水和氢氧化钡中除去结晶水，这些水是通过具有不同性质的共价键结合的。脱水是与加热干燥的水合初始底物同时进行；或者通过与一种满足此目的的溶剂共沸蒸馏除去结晶水，或者在一定温度下用一种可与水以任意比例互溶的无水有机溶剂浸提，然后过滤。其目的和两种方法的操作方式是不同的。本发明可以通过以下例子加以阐明。例1：150g八水合氢氧化钡和500cc苯一起缓慢加热回流，装置带有一配有溢流管的接收器。在苯和水共沸混合物的沸点即69. 3时，第一个蒸馏物出现，90分钟后接收器中收集到相当于7摩尔结晶水量的水。继续加热温度将升高到80.2，直至加入新的八水合氢氧化钡，温度下降，脱水过程继续进行。最后取出所形成的一水合氢氧化钡的苯的悬浮液并过滤，粘附的奔可以通过简单的蒸馏方法从底物中除去。过滤得到的苯可以马上用于进一步的脱水。例2：100g例1得到的一水合氢氧化钡按上面描述的方法用300cc甲苯处理。脱水过程进行完全，获得无水氢氧化钡。甲苯和水混合物的共沸温度是84.1。例3：50g八水合氢氧化钡用1000cc浸提，剧烈搅拌混合物。一小时后过滤混合物，氢氧化钡以一水合物的形式出现。我们要求的权限是：1、一种水合氢氧化钡的脱水方法，通过在一种对氢氧化钡惰性的有机溶剂或混合溶剂中加热抽提去结晶水。2、按权限1的要求，通过与一种对氢氧化钡惰性的有机溶剂或混合熔剂中共沸除去结晶水。3、按权限1的要求，通过一种对氢氧化钡惰性、且可与水以任意比例互溶的有机溶剂或混合溶剂浸提除去结晶水，操作温度高于八水合氢氧化钡的同成份熔点，低于溶剂或溶剂混合物的沸点。4、一种水合氢氧化钡完全脱水的方法，如上文描述的所有例子。文献阅读： Designation：D46582 ( Reapproved 1997)1 Standard Test Methods for Acid Number of RosinThis standard is issued under the fixed designation D 465: the number immediately followed the designation indicate the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval.Note: Section 7 was changed editorially in November 1987.1 These test methods are under the jurisdiction of ASTM Committee D-1 on Paint and Related Coating and Materials and are the direct responsibility of Subcommittee D01.34 on Naval Stores.Current edition approved March 26, 1982. Published June 1982. Originally published as D465-37T. Last previous edition D 465-59(1981).1. Scope1.1 These test methods are intended for determining the acid number酸值 of rosin松香. Two methods are covered, as follows:1.1.1 Internal indicator method内标法, and1.1.2 Potentiometric method电位法.1.2 The internal indicator method is suitable for use only with light- and medium-colored rosin. The potentiometric method is suitable for use with both light- and dark-colored resin.1.3 This standard方法，标准 may involve hazardous有害的 materials, operation, and equipment. This standard does not purport to旨在 address声明 all of safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability适用的 of regulatory limitations 规章限制prior to在。之前 use.2. Referenced Document2.1 ASTM Standard:美国材料实验协会标准E 70 Test Method for pH of Aqueous Solutions水溶液 with the Glass Electrode22Annual Book of ASTM Standards, Vol 15.053. Preparation of Specimen样品3.1 The specimen taken for analysis shall consist of small pieces of rosin chipped切 from a freshly exposed part of a lump or lumps, and thereafter crushed to facilitate方便 weighing and solution. The specimen shall be so prepared the same day on which the test is begun, in order to avoid changes in properties due to surface oxidation, which is very pronounced显著 on ground rosin having a large surface area exposed to the air.4. Purity of Reagents and Water4.1 Unless otherwise另外的 indicated, it is intended that all reagents shall conform to the specifications established by the Committee on Analytical Reagents of the American Chemical Society美国化学会分析试剂委员会, where such specifications are available3. References to water shall be understood to mean普通的 distilled water.3 “Regent Chemical, American Chemical Society Specification, ”Am. Chem. Soc., Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical, see “Reagent Chemicals and Standards,” by Joseph Rosin, D. Van Nastrand Co., Inc., New York, NY, and the “United States Pharmacopeia”INTERNAL INDICATOR METHOD5. Reagents5.1 Alkali碱, Standard Solution (0.5N)Dissolve either 22 g of sodium hydroxide (NaOH) or 33 g of potassium hydroxide (KOH) (pellets or sticks) in water or in alcohol conforming to 5.2, and dilute 稀释to 1L with the same solvent. Standardize to 0.001 N.5.2 Ethyl Alcohol乙醇Neutral methanol中性甲醇, neutral isopropanol中性异丙醇(91 to 99%), neutral denatured alcohol 中性改变本质的醇conforming to Formula No. 30 or No 3A of the U. S. Bureau of Internal Revenue. 美国国内税收局NOTE 1In case of disagreement between purchaser and seller, aqueous alkali solution shall be used.5.3 Phenolphthalein Indicator Solution酚酞指示剂Dissolve 1 g of phenolphthalein in 100 mL methanol.5.4 Thymol Blue Indicator Solution百里酚蓝指示剂Dissolve 0.1 g of thymol blue in 100 mL methanol.6. Procedure6.1 Transfer 3.95 to 4.05g of the sample, weighed to the nearest 0.001 g, to a 250 mL Erlenmeyer flask厄仑美厄烧瓶, and add 100 mL of neutral alcohol.6.2 Heat, if necessary, to dissolve the rosin, cool to room temperature (Note 2), and titrate滴定 the solution with the standard alkali solution using 1mL of either phenolphthalein or thymol blue indicator solution. With phenolphthalein, titrate to the first persistent不变的（不变色） faint pink color浅粉红色, with thymol blue, titrate to a distinct blue.Note 2 If the rosin does not remain in solution when it cools, use 200 mL of alcohol instead of 100 mL.7. Calculation and Report7.1 Calculate the acid number of the rosin, expressed as milligrams毫克 of KOH per gram of sample, as follow, and report to the nearest whole number取整数:Acid number = (AN56.1)/Bwhere:A = alkali solution required for titration of the specimen, mL,N = normality当量浓度 of the alkali solution and B = specimen weight, g.POTENTIOMETRIC METHOD8. Apparatus仪器8.1 Glass-Electrode pH Meter 璃电极pH计conforming to the requirements of Test Method E 70. Use either standard or alkali-resistant electrodes 标准或耐碱的电极for this test. Alternatively另外, an automatic potentiometric电位 titrator测定仪 may be used.8.2 Stirrer, variable-speed with a glass propeller-type stirring paddle.搅拌桨9. Reagents9.1 Prepare the reagents described in 4.1 and Borax Buffer硼砂缓冲液. Standard Solution (0.01M, pH 9.18 at 25)Dissolve 3.810.01 g of disodium tetraborate四硼酸二钠 (Na2B4O710H2O) in water and dilute to 1L in a volumetric flask容量瓶. Use the special grade4 of borax硼砂 prepared specifically for use as a pH standard.4The National Bureau of Standards standard sample of borax No. 187 is satisfactory for this purpose.10. Standardization of Apparatus10.1 Adjust the pH meter with the standard borax buffer solution, following essentially本质上 the same procedure as described in Test Method E 70.11. Procedure11.1 Transfer 3.95 to 4.05g of the sample, weighed to the nearest 0.001 g, to a 400-mL tall-form beaker 高脚烧杯and add 200 mL of neutral alcohol. Heat, if necessary, to dissolve the rosin and cool to room temperature.11.2 Adjust the beaker so the lower half of each electrode of the pH meter is immersed in the specimen. Start the stirrer and adjust the speed so that there is vigorous stirring without spattering.11.3 Titrate滴定 with the standard alkali solution, recording the buret滴定管 and pH meter readings. Sufficient alkali may be added initially to bring the pH of the solution to about 8.0. Allow sufficient time for the electrode system to reach equilibrium. Add alkali in 1.0-mL portions分量 until the change in pH per increment 增量added amounts to about 0.3 pH unit. Reduce the additions of alkali to 0.1 mL until the end point has been passed, as indicated by a significant decrease in pH per 0.1mL added. Continue the titration with 1.0-mL portions until it becomes apparent that the inflection point拐点 has been well defined.11.4 Determine测定 the inflection point拐点 (point of maximum change in pH millilitre毫升 of alkali solution) to the nearest 0.1 mL by plotting作图 the pH readings against the millilitres of alkali used. For great accuracy, a plot may be made of the change in pH per millilitre of alkali, against the pH. The peak of this curve will indicate the exact inflection point突变点. The inflection point shall be taken as the end of the titration滴定. Alternatively另外, if an automatic titrator is used, the end point shall be taken either as t