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    1-Aminoalkane-1,1-diphosphonic acids and their salts
    41.
    发明授权
    1-Aminoalkane-1,1-diphosphonic acids and their salts 失效
    1-氨基链烷-1,1-二膦酸及其盐

    公开(公告)号：US3979385A

    公开(公告)日：1976-09-07

    申请号：US475207

    申请日：1974-05-31

    申请人： Klaus Wollmann ,  Walter Ploger ,  Karl-Heinz Worms

    发明人： Klaus Wollmann ,  Walter Ploger ,  Karl-Heinz Worms

    IPC分类号： C07F9/38 ,  C07D295/04

    CPC分类号： C07F9/3873

    摘要： A process for the production of 1-aminoalkane-1,1-diphosphonates of the formula ##SPC1##Wherein R.sub.1 is a member selected from the group consisting of hydrogen, lower alkyl and phenyl, R.sub.2 and R.sub. 3 are members selected from the group consisting of hydrogen, alkyl having 1 to 22 carbon atoms, cycloalkyl having 5 to 6 carbon atoms, phenyl, alkylphenyl having 7 to 18 carbon atoms, phenylalkyl having 7 to 18 carbon atoms and together with the nitrogen atom, piperidino, pyrrolidino and morpholino, and X is a member selected from the group consisting of hydrogen, alkali metal, ammonium, pyridinium, guanidinium and mono-, di-, and tri-lower-alkanol-ammonium with the proviso that at least one of R.sub.1, R.sub.2 and R.sub.3 is other than hydrogen, which consists essentially in reacting a phosphorus trihalide selected from the group consisting of phosphosus trichloride and phosphorus tribromide with a monocarboxylic acid amide of the formula ##SPC2##wherein the molecular weight of said carboxylic acid amide is over 46 and R.sub.1, R.sub.2 and R.sub. 3 have the above assigned meanings, at a temperature of from 0.degree. to 75.degree.C, subjecting the resultant reaction product to hydrolysis, and recovering said 1-aminoalkane-1,1-diphosphonates. The 1-aminoalkane-1,1-diphosphonates, some of which are novel, are capable of forming complexes with heavy metals.

    摘要翻译： 制备式WHEREIN R1的1-氨基烷烃-1,1-二膦酸盐的方法是选自氢，低级烷基和苯基的成员，R 2和R 3是选自氢， 具有1至22个碳原子的烷基，具有5至6个碳原子的环烷基，苯基，具有7至18个碳原子的烷基苯基，具有7至18个碳原子的苯基烷基以及氮原子，哌啶子基，吡咯烷子基和吗啉代，X是 选自氢，碱金属，铵，吡啶鎓，胍和单 - ，二 - 和三 - 低级 - 链烷醇 - 铵的成员，条件是R 1，R 2和R 3中的至少一个不是氢， 其主要在于使选自三磷化磷和三溴化磷的三卤化磷与下式的一元羧酸酰胺反应，其中所述羧酸酰胺的分子量超过46且R1，R2 和R 3具有上述含义，在0℃至75℃的温度下，使所得反应产物水解，并回收所述1-氨基烷烃-1,1-二膦酸盐。 其中一些是新型的1-氨基烷烃-1,1-二膦酸盐能够与重金属形成络合物。

    Use of a hydrophilic plasticizer for plastic dispersions and pastes
    43.
    发明授权
    Use of a hydrophilic plasticizer for plastic dispersions and pastes 失效
    使用亲水性增塑剂用于塑料分散体和糊剂

    公开(公告)号：US3957712A

    公开(公告)日：1976-05-18

    申请号：US498998

    申请日：1974-08-20

    申请人： Rudi Heyden ,  Michael Eckelt ,  Karl Mahall ,  Wilfried Kuper

    发明人： Rudi Heyden ,  Michael Eckelt ,  Karl Mahall ,  Wilfried Kuper

    IPC分类号： C08G65/332 ,  C08K5/103 ,  C08L71/02 ,  C08K5/11

    CPC分类号： C08K5/103 ,  C08G65/3322 ,  C08L71/02

    摘要： In the process of plasticizing hardenable plastics in the form of dispersions and pastes, the use of fatty acid esters of polyoxyalkylene glycol having the formulaR.sub.1 --A--R.sub.2wherein R.sub.1 and R.sub.2 are acyls of the fatty acids having from 12 to 22 carbon atoms and A is a bivalent polyoxyalkylene glycol radical having a molecular weight of from 2000 to 4000 and a content of 40 to 50% by weight of ethylene oxide units and 50 to 60% by weight of propylene oxide units, as hydrophilic plasticizers for said plastic dispersions and pastes.

    摘要翻译： 在分散体和糊剂形式的可硬化塑料的增塑过程中，使用具有式R1-A-R2的聚氧亚烷基二醇的脂肪酸酯，其中R1和R2是具有12-22个碳原子的脂肪酸的酰基，和 A是分子量为2000〜4000，含量为40〜50重量％的氧化乙烯单元和50〜60重量％的环氧丙烷单元的二价聚氧亚烷基二醇基，作为所述塑料分散体的亲水增塑剂， 糊状物

    Method for production of hydroxyalkylglycol ethers
    47.
    发明授权
    Method for production of hydroxyalkylglycol ethers 失效
    羟烷基乙二醇醚的制备方法

    公开(公告)号：US3931338A

    公开(公告)日：1976-01-06

    申请号：US458752

    申请日：1974-04-08

    申请人： Wolfgang Rupilius

    发明人： Wolfgang Rupilius

    IPC分类号： C07C43/13 ,  C07C20060101 ,  C07C41/00 ,  C07C41/02 ,  C07C43/04 ,  C07C43/10 ,  C07C67/00

    摘要： A method for the production of hydroxyalkyl glycol ethers comprises reacting non-terminal epoxides with ethylene glycol in the presence of an alkoxylation catalyst and saturated hydrocarbons, in particular, saturated aliphatic hydrocarbons, as solvents.

    摘要翻译： 用于制备羟烷基二醇醚的方法包括在烷氧基化催化剂和饱和烃，特别是饱和脂族烃作为溶剂的存在下使非末端环氧化物与乙二醇反应。

    Process for the production of secondary alcohol ether sulfates
    48.
    发明授权
    Process for the production of secondary alcohol ether sulfates 失效
    二醇醇硫酸盐生产工艺

    公开(公告)号：US3931271A

    公开(公告)日：1976-01-06

    申请号：US118549

    申请日：1971-02-24

    申请人： Horst Baumann ,  Wilfried Umbach ,  Werner Stein

    发明人： Horst Baumann ,  Wilfried Umbach ,  Werner Stein

    IPC分类号： C07C309/65 ,  C07C29/52 ,  C07C303/24 ,  C07C303/28 ,  C11D1/29 ,  C07C139/00 ,  C07C139/10 ,  C07C141/00

    CPC分类号： C07C29/52 ,  C07C303/24 ,  C11D1/29

    摘要： A process for the production of secondary alcohol ether sulfates which consists essentially of reacting adducts of secondary alkanols having from 6 to 22 carbon atoms adducted with 1 to 10 mols of an alkylene oxide selected from the group consisting of ethylene oxide and propylene oxide, said adduct having at least 1 mol of oxypropylene per mol of alcohol, with at least a molecular equivalent of a sulfating agent stronger than concentrated sulfuric acid at temperatures of from 0.degree.C to 50.degree.C and recovering said secondary alcohol ether sulfate.THE PRIOR ARTAt present secondary alcohols can be prepared from inexpensive raw materials, such as by oxidation of paraffins, substantially simpler than the preparation of primary alcohols. However, up to now the practical use of secondary alcohols is limited to non-ionic products prepared from them. Surface-active sulfates derived from secondary alcohols are used only in small amounts since the preparation of such raw materials for washing agents is very difficult, because of the instability of the secondary alkylsulfates. Primary alcohols, on the contrary, can be converted simply and with good yields into surface-active sulfates. In the sulfation of secondary alcohols, the conversion rates are low. In order to obtain somewhat usable products, expensive procedures have to be introduced, such as working with solvents and adduct formers, use of special sulfating agents, such as, for example, amidosulfonic acid, etc., as well as the addition of ethylene oxide adducts of primary alcohols. On the other hand, there is the possibility that by reaction of secondary alcohols with ethylene oxide, adducts with primary hydroxyl groups can be prepared, the sulfation products of which could be expected to have greater stability.It is, however, very difficult to prepare ethoxylates of secondary alcohols with a high conversion rate and small amounts of by-products. A higher conversion rate of the secondary alcohols with ethylene oxide can only be attained by relatively cumbersome procedures, such as, for example, a two-step ethoxylation in which in the first step an acidic catalyst is used and, after distilling off the unreacted secondary alcohol, in the second step an alkaline catalyst is utilized. However, the ethoxylated secondary alcohols obtained by this expensive procedure are also unsatisfactorily sulfated and can only be sulfated by the application of special procedures. This is difficult to explain since by the ethoxylation of secondary alcohols, adducts with primary hydroxyl groups were formed.OBJECTS OF THE INVENTIONAn object of the present invention is the development of a simple process for the production of secondary alcohol ether sulfates utilizing conventional strong sulfating agents to give products with a high degree of sulfation.Another object of the invention is the development of a process for the production of secondary alcohol ether sulfates which consists essentially of reacting adducts of secondary alkanols having from 6 to 22 carbon atoms adducted with 1 to 10 mols of an alkylene oxide selected from the group consisting of ethylene oxide and propylene oxide, said adduct having at least 1 mol of oxypropylene per mol of alcohol, with at least a molecular equivalent of a sulfating agent stronger than concentrated sulfuric acid at temperatures of from 0.degree.C to 50.degree.C and recovering said secondary alcohol ether sulfate.These and other objects of the invention will become more apparent as the description thereof proceeds.DESCRIPTION OF THE INVENTIONIt has now been surprisingly found that alkylene oxide adducts of secondary alcohols which contain at least one propylene glycol ether group can be sulfated simply with a high conversion rate. This result was the more unexpected since, as is known, on the introduction of propylene glycol ether groups by propoxylation, adducts with predominately secondary hydroxyl groups are formed. Therefore, the same difficulties in the further reaction of these adducts, especially in sulfation, would be expected as in the sulfation of secondary alcohols themselves. With this expectation, the sulfation of secondary alcohol propoxylates would appear to the expert as having little prospect of good yields.The invention relates, therefore, to a process for the preparation of surface-active ether and polyether sulfates which is characterized in that adducts of secondary alkanols having 6 to 22 carbon atoms adducted with 1 to 10 mols of alkylene oxide, possessing in the average at least 1 mol of propylene oxide per mol of alcohol, are reacted in a known manner at temperatures between 0.degree.C and 50.degree.C, particularly from 10.degree.C and 30.degree.C, with strong sulfating agents in at least stoichiometric amounts.As starting materials those adducts may be used that were obtained (1) by ethoxylation of secondary alcohols in the first step and subsequent propoxylation of the reaction mixtures, or (2) by reaction of secondary alcohols with ethylene oxide/propylene oxide mixtures, or (3) by the ethoxylation of reaction mixtures of secondary alcohols with propylene oxide, or (4) by pure propoxylation of secondary alcohols. The preferred starting materials are the adducts of propylene oxide to secondary alcohols or secondary alkanol propoxylates having 6 to 22 carbon atoms in the alkanol and 1 to 10 oxypropylene units.The mixed alkoxylates to be used contain preferably 1 to 4, particularly 2 to 3, oxyethylene groups. Of particular advantage among the pure propylene oxide adducts are those substance mixtures which were obtained by reaction of 1.5 to 5 mols of propylene oxide with 1 mol of secondary alcohol.The starting materials can be obtained by conventional alkoxylation methods. The alkoxylation can be carried out both anionically, in the presence of alkaline alkoxylation catalysts, such as alkali metal hydroxides or alkali metal alcoholates, particularly sodium, potassium and lithium lower alkanolates, and cationically in the presence of acidic catalysts, such as BF.sub.3, or in the presence of the tertiary oxonium salts described as alkoxylation catalysts in Belgian Pat. No. 715,048.If mixed adducts are used which have been obtained by propoxylation of ethylene oxide adducts of secondary alcohols as starting materials, such mixed adducts are preferred in which the alkoxylation in the first step was carried out by a cationic catalyst and in the second step with an anionic catalyst.Among the mixed adducts which are obtained by simultaneous addition of ethylene oxide and propylene oxide, or by propoxylation in the first step and ethoxylation in the second step, as well as in the pure propoxylation products, these are preferably prepared by reaction with an anionic catalyst.The secondary alcohols utilized to prepare the alkoxylation mixtures can be either compounds of uniform chain length or mixtures of homologs. Of particular economic advantage are those alcohol mixtures which have been obtained by the oxidation of paraffins in the presence of boron compounds, such as, for example, boric acid, boron trioxide, borates, boric acid esters, as well as other known reagents for the formation of secondary alcohols, such as arsenic acid, arsenic acid esters, arsenic trioxide, and others.The alkoxylation mixtures utilizable for the subsequent sulfation can be used as crude products, that is, without intervening purification or processing operations. This is of essential importance for the technical execution of the process. These crude alkoxylation mixtures contain, therefore, in addition to the desired alkylene oxide adducts of secondary alcohols, as secondary constituents, the corresponding alkylene and/or polyalkylene glycols as well as, possibly, non-reacted secondary alcohol. The sulfation of the alkoxylate mixture is preferably carried out in the temperature range of from 10.degree.C to 30.degree.C.By "strong sulfating agents" are meant those which are stronger than concentrated sulfuric acid, for example, SO.sub.3 or SO.sub.3 /air mixtures, oleum, chlorosulfonic acid, and the like. The addition of adduct formers for the sulfating agent or the presence of solvents are not required in the process. The preferred sulfating agent is chlorosulfonic acid. The mol ratio between the alkoxylate and the sulfating agent is advantageously chosen in the range of from 1:1.0 to 1:1.2, particularly in the range of from 1:1.02 to 1:1.1.The sulfation reaction can be carried out continuously or discontinuously. The reaction times lie between fractions of seconds to about 20 minutes, depending upon the sulfating agent and/or sulfating apparatus used. Particularly short reaction times are attained if the reaction is carried out with very strong sulfating agents, such as SO.sub.3 /air mixtures, in modern short-time sulfation reactors which operate by the split-ring or falling film principle.The products of the process have a substantially higher degree of sulfation than the products obtained by the sulfation of technical ethylene oxide adducts of secondary alcohols. They have, without further processing, very good surface-active properties and are superior, particularly in regard to their wetting action, to the known commercial sulfated adducts of ethylene oxide to primary alcohols.The advantages attainable with the invention consist primarily in that as a raw material source for surface-active, water-soluble sulfates, secondary alcohols have been made available. Particularly those secondary alcohols which are easily obtainable by paraffin oxidation in the presence of the above-named oxidation catalysts to produce secondary alcohols with statistically distributed hydroxyl groups. These alcohols are converted by alkoxylation to the substances suitable for sulfation. Thus, these petrochemical raw materials can form the basis for the desired surface-active substances. Anionic active derivatives of secondary alcohols were up to now technically not producible by a simple way although secondary alcohols have been produced for some time on a large scale. The use of secondary alcohols was, therefore, until now limited to the production of non-ionic substances.A further advantage of the process according to the invention can be seen in that the necessary alkoxylation may be carried out without a large expense in regard to catalysts and/or equipment.The following examples are illustrative of the invention without being deemed limitative in any respect.

    摘要翻译： 一种生产仲醇醚硫酸盐的方法，其主要包括与6至22个碳原子的仲烷醇的加合物加成1至10摩尔选自环氧乙烷和环氧丙烷的环氧烷烃，所述加合物 每摩尔醇具有至少1摩尔氧化丙烯，至少在0℃至50℃的温度下至少分子当量的硫酸化剂比浓硫酸更强，并回收所述仲醇醚硫酸盐。

    Process for the production of a marbled or mottled soap cake and the product of such process
    50.
    发明授权
    Process for the production of a marbled or mottled soap cake and the product of such process 失效
    用于生产大理石或斑驳的肥皂饼的过程以及这种过程的产物

    公开(公告)号：US4036775A

    公开(公告)日：1977-07-19

    申请号：US589795

    申请日：1975-06-23

    申请人： Jutta Trautvetter ,  Albert Weingartz ,  Lothar Werner

    发明人： Jutta Trautvetter ,  Albert Weingartz ,  Lothar Werner

    IPC分类号： C11D13/08 ,  C11D13/22 ,  B29C9/00

    CPC分类号： C11D13/22 ,  C11D13/08 ,  Y10T83/0548 ,  Y10T83/06

    摘要： A process for the production of a marbled or mottled cake or bar, particularly of soap, comprising cutting an extruded rope having axially aligned section of different colors, into blanks of the desired dimension, at an angle .alpha. of 75.degree. to 15.degree. to the axis of said extruded rope, stamp molding said blanks with the direction of stamping at an angle .beta. of from 90.degree. to 30.degree. to the cut surfaces of said blank, and recovering a marbled or mottled cake or bar of soap.

    摘要翻译： 用于生产大理石或斑驳的蛋糕或条，特别是肥皂的方法，包括将具有不同颜色的轴向排列的部分的挤出的绳索切割成所需尺寸的坯料，角度α为75°至15° 所述挤压绳索的轴线，以与所述坯料的切割表面成90°至30°的角度β的冲压方向对所述坯料进行模压，并且回收大理石或斑驳的蛋糕或皂条。