公开(公告)号：CH666038A5

公开(公告)日：1988-06-30

申请号：CH238585

申请日：1985-06-05

Applicant: KAO CORP

Inventor： KUROSAKI TOMIHIRO ,  WAKATSUKI JUNYA ,  FURUGAKI HISAKAZU ,  KOJIMA KATSUTOSHI

IPC: C07F9/02 ,  C07F9/09 ,  C07F9/11 ,  C07F9/113

公开(公告)号：DE3520053C2

公开(公告)日：1994-09-08

申请号：DE3520053

申请日：1985-06-04

Applicant: KAO CORP

Inventor： KUROSAKI TOMIHIRO ,  WAKATSUKI JUNYA ,  FURUGAKI HISAKAZU ,  KOJIMA KATSUTOSHI

IPC: C07F9/02 ,  C07F9/09 ,  C07F9/11 ,  C07F9/113

Abstract: A novel process for producing a phosphoric monoester which comprises reacting per 1 mole of a linear or branched, saturated or non-saturated aliphatic alcohol having from 8 to 36 carbon atoms, from 2 to 10 moles of a polyphosphoric acid at 100 to 116% concetration converted as orthophosphoric acid in (a) one or more solvents selected from the group consisting of linear or branched saturated aliphatic hydrocarbons having from 4 to 8 carbon atoms and saturated cycloaliphatic hydrocarbons having from 5 to 7 carbon atoms, then adding (b) a lower alcohol having from 1 to 4 carbon atoms and water to the reaction mixture, transferring the orthophosphoric acid to the lower alcohol-aqueous phase to separate it from the phosphoric monoester, and concentrating the thus recovered orthophosphoric acid for reuse. The process reaction proceeds smoothly, separation and purification can be carried out readily and very effectively and the recovered phosphoric acid can be re-used.

公开(公告)号：DE3520053A1

公开(公告)日：1985-12-19

申请号：DE3520053

申请日：1985-06-04

Applicant: KAO CORP

Inventor： KUROSAKI TOMIHIRO ,  WAKATSUKI JUNYA ,  FURUGAKI HISAKAZU ,  KOJIMA KATSUTOSHI

IPC: C07F9/02 ,  C07F9/09 ,  C07F9/11 ,  C07F9/113

Abstract: A novel process for producing a phosphoric monoester which comprises reacting per 1 mole of a linear or branched, saturated or non-saturated aliphatic alcohol having from 8 to 36 carbon atoms, from 2 to 10 moles of a polyphosphoric acid at 100 to 116% concetration converted as orthophosphoric acid in (a) one or more solvents selected from the group consisting of linear or branched saturated aliphatic hydrocarbons having from 4 to 8 carbon atoms and saturated cycloaliphatic hydrocarbons having from 5 to 7 carbon atoms, then adding (b) a lower alcohol having from 1 to 4 carbon atoms and water to the reaction mixture, transferring the orthophosphoric acid to the lower alcohol-aqueous phase to separate it from the phosphoric monoester, and concentrating the thus recovered orthophosphoric acid for reuse. The process reaction proceeds smoothly, separation and purification can be carried out readily and very effectively and the recovered phosphoric acid can be re-used.

公开(公告)号：DE3334523A1

公开(公告)日：1984-03-29

申请号：DE3334523

申请日：1983-09-23

Applicant: KAO CORP

Inventor： TSUTO KEIICHI ,  KUNIKAWA KENZO ,  KOJIMA KATSUTOSHI

IPC: C07C309/20 ,  C07C67/00 ,  C07C301/00 ,  C07C303/00 ,  C07C303/02 ,  C07C303/06 ,  C07C143/16 ,  C07C139/00

Abstract: The invention relates to a process for the sulphonation of alpha -olefins with an SO3-containing gas by means of thin-layer sulphonation while maintaining the following process conditions: 5 d)(WC)

公开(公告)号：JPS60258191A

公开(公告)日：1985-12-20

申请号：JP11530584

申请日：1984-06-05

Applicant: KAO CORP

Inventor： KUROSAKI TOMIHIRO ,  WAKATSUKI JIYUNYA ,  FURUGAKI HISAKAZU ,  KOJIMA KATSUTOSHI

IPC: C07F9/11 ,  C07F9/09

Abstract: PURPOSE:A mixture containing phosphoric acid ester and orthophosphoric acid is subjected to extraction with a solvent consisting of a specific aliphatic hydrocarbon, lower alcohol and water, to remove orthophosphoric acid to enable high- efficiency purification of the titled compound, which is used as a cleaning solution. CONSTITUTION:In the extraction from a mixture containing a phosphoric acid ester such as lauryl phosphate and orthophosphoric acid with a solvent, the mixture is mixed with (A) solvent 1 which is a mixture of 4-8C aliphatic hydrocarbon such as n-hexane, 5-7C alicyclic hydrocarbon and (B) solvent 2 consisting of 1-4C lower alcohol such as isopropanol and water, in the mixer 3, then sent to the separation tank 4. Then, the upper phase which flows out of the upper part of the separation tank 4 is continuously mixed with aqueous isopropanol 5 in the mixing tank 6 and separated in the separation tank 7 whereby phosphoric acid ester 8 is obtained from the upper part of the separation tank 7, the lower phases 9, 10 containing orthophosphoric acid are obtained from the lower part of the separation tanks 4, 7.

公开(公告)号：JPS5955865A

公开(公告)日：1984-03-31

申请号：JP16606482

申请日：1982-09-24

Applicant: Kao Corp

Inventor： DEN KEIICHI ,  KUNIKAWA KENZOU ,  KOJIMA KATSUTOSHI

IPC: C07C309/20 ,  C07C67/00 ,  C07C301/00 ,  C07C303/00 ,  C07C303/02 ,  C07C303/06

CPC classification number: C07C309/00

Abstract: PURPOSE: In sulfonating an α-olefin with a SO
3 -containing gas in a thin film state in a parallel flow continuously, to obtain a sulfonated substance having hue not requiring bleaching process, carrying out the reaction under defined specific conditions of gas line speed, diameter of a reaction tube, etc.
CONSTITUTION: In a method wherein an α-olefin and a SO
3 -containing gas are introduced to a vertically supported reaction tube of cylinder or double cylinder so that it is sulfonated in a thin film state in a parallel flow continuosuly, the reaction is carried out under conditions shown by the formula[v is gas line speed(m/sec); d is diameter of corresponding diameter of reaction tube (4× cross-sectional area of flow÷wet side length)(m); w is feed rate of raw material per unit wet side length(kg-mol/m.hv); c is SO
3 average gas concentration at inlet of reaction tube (vol%)]. A sulfonated substance having low coloring is obtained by selecting balanced values of v, d, w, and c(preferably, d is 0.014W 0.022m, v is 25W38/sec., and c is ≥3%).
COPYRIGHT: (C)1984,JPO&Japio

Abstract translation: 目的：在连续的平行流动下，用薄膜状态的含SO 3的气体将α-烯烃磺化，得到不需要漂白处理的色相的磺化物质，在规定的气体线速度的特定条件下进行反应， 反应管的直径等。结构：在其中将α-烯烃和含SO 3的气体引入到圆柱体或双圆柱体的垂直支撑的反应管中以使其以平行的薄膜状态磺化的方法 反应在式[v为气体管线速度（m / sec）所示的条件下进行。 d是反应管的相应直径的直径（4倍横截面积由湿边长度分散）（m）; w是每单位湿侧长度（kg-mol / m.hv）的原料进料速率; c为反应管入口处SO3平均气体浓度（体积％）]。 通过选择v，d，w和c的平衡值（优选d为0.014-0.022m，v为25-38 / sec，c为> = 3％）获得具有低着色的磺化物质。

公开(公告)号：JPS6117593A

公开(公告)日：1986-01-25

申请号：JP13777784

申请日：1984-07-03

Applicant: Kao Corp

Inventor： KUROSAKI TOMIHIRO ,  WAKATSUKI JIYUNYA ,  FURUGAKI HISAKAZU ,  KOJIMA KATSUTOSHI

IPC: C07F9/11 ,  C07F9/09 ,  C07F9/113

Abstract: PURPOSE: To purify the titled compound useful as a detergent, etc., economically in an industrial scale, by adding a hydrocarbon, a lower alcohol and water to a mixture of a phosphoric acid ester and orthophosphoric acid, removing the lower alcohol and water from the extract by azeotropic distillation, and carrying out the recrystallization of the residue.
CONSTITUTION: A mixture containing a phosphoric acid ester and orthophosphoric acid is mixed with solvents consisting of (A) one or more kinds of 4W8C saturated aliphatic hydrocarbons (e.g. n-hexane) and 5W7C saturated alicyclic hydrocarbons, etc. and (B) a 1W4C alcohol (e.g. isopropanol) and water to effect the extraction and separation of the phosphoric acid ester to the hydrocarbon layer. The lower alcohol and water mixed in the hydrocarbon layer is removed by the azeotropic distillation, and the objective compound is produced from the residue by recrystallization or topping.
COPYRIGHT: (C)1986,JPO&Japio

Abstract translation: 目的：通过向磷酸酯和正磷酸的混合物中加入烃，低级醇和水，以经济的方式纯化用作洗涤剂等的标题化合物，将低级醇和水从 通过共沸蒸馏提取提取物，并进行残余物的再结晶。 构成：将含有磷酸酯和正磷酸的混合物与（A）一种或多种4-8C饱和脂族烃（例如正己烷）和5-7C饱和脂环烃等组成的溶剂混合，和 B）1-4C醇（例如异丙醇）和水，以便将磷酸酯萃取和分离成烃层。 通过共沸蒸馏除去混合在烃层中的低级醇和水，并且通过重结晶或顶部由残余物产生目标化合物。

公开(公告)号：JPS57118522A

公开(公告)日：1982-07-23

申请号：JP412481

申请日：1981-01-14

Applicant: Kao Corp

Inventor： DEN KEIICHI ,  KOJIMA KATSUTOSHI

IPC: C07B45/02 ,  C07B31/00 ,  C07C67/00 ,  C07C301/00 ,  C07C303/06 ,  C07C309/17

Abstract: PURPOSE: To reduce the size of the pre- and the post-treatment facilities in the counter- current and continuous sulfonation of an organic compound with an SO
3 -containing gas, and to obtain the high quality objective product in high degree of conversion, by introducing the raw material compound to the waste gas produced by the reaction, and circulating the mixture of gas and liquid with a liquid ring pump.
CONSTITUTION: An organic compound is sulfonated countercurrently and continuously in the first reactor 2 with an SO
3 -containing gas sent through the pipe 13, and the sulfonated product separated by the vapor-liquid separtor 3 is taken out through the pipe 15. A part of the waste gas separated in the separator is exhausted through the pipe 12 and the waste gas treatment apparatus. The remaining part of the waste gas circulating through the pipe 11 is mixed with the organic compound raw material 4 sent through the pipe 14, and the organic compound and the waste gas are circulated in the form of a vapor-liquid mixture with a liquid ring pump 1. Pref. the second reactor 2' is placed at the upstream of the liquid ring pump 1, and a part of the SO
3 - containing gas is supplied to the reactor through the pipe 13'. Generation of waste gas mist in the recycling tube, carbonization of residence liquid, and accumulation of carbonized material can be prevented by this process.
COPYRIGHT: (C)1982,JPO&Japio

Abstract translation: 目的：为了减少含SO 3的气体的有机化合物的逆流和连续磺化的前处理设备和后处理设施的大小，并以高转化率获得高质量的目标产物，通过 将原料化合物引入到由反应产生的废气中，并用液环泵循环气体和液体的混合物。 构成：有机化合物在第一反应器2中以含有SO 3的气体通过管13反向和连续地磺化，并且由气液分离器3分离的磺化产物通过管15被取出。一部分 在分离器中分离的废气通过管12和废气处理装置排出。 通过管道11循环的废气的剩余部分与通过管14送出的有机化合物原料4混合，有机化合物和废气以液态环状的汽液混合物的形式循环 泵1。 第二反应器2'放置在液环泵1的上游，一部分含SO 3的气体通过管13'供给反应器。 通过该过程可以防止在回收管中产生废气雾，残留液的碳化和碳化材料的积聚。

公开(公告)号：JPH0246040B2

公开(公告)日：1990-10-12

申请号：JP13777784

申请日：1984-07-03

Applicant: KAO CORP

Inventor： KUROSAKI TOMIHIRO ,  WAKATSUKI JUNYA ,  FURUGAKI HISAKAZU ,  KOJIMA KATSUTOSHI

IPC: C07F9/11 ,  C07F9/09 ,  C07F9/113

公开(公告)号：JPS6117594A

公开(公告)日：1986-01-25

申请号：JP13882984

申请日：1984-07-04

Applicant: Kao Corp

Inventor： KUROSAKI TOMIHIRO ,  WAKATSUKI JIYUNYA ,  FURUGAKI HISAKAZU ,  KOJIMA KATSUTOSHI

IPC: C07F9/11

Abstract: PURPOSE: To obtain the titled substance economically, reutilizing the recovered phosphoric acid, and facilitating the separation and purification of the product, by reacting a specific (un)saturated aliphatic alcohol with a polyphosphoric acid in a hydrocarbon, and extracting the obtained reaction mixture with a solvent composed of a lower alcohol and water.
CONSTITUTION: 1mol of a 8W36C (un)saturated aliphatic alcohol (e.g. dodecyl alcohol) is made to react with 2W10mol of a polyphosphoric acid having a concentration of 100W116% in terms of orthophosphoric acid, in one or more solvents selected from 4W8C saturated aliphatic hydrocarbons (e.g. n-hexane) and 5W7C saturated alicyclic hydrocarbons (e.g. cyclohexane). A 1W4C alcohol and water are added to the reaction mixture to effect the migration of the orthophosphoric acid to the layer of the lower alcohol and water. The orthophosphoric acid separated efficiently from the monoalkylphosphoric acid by this process is concentrated and reused. The objective substance can be obtained by distilling off the solvent, the lower alcohol and water from the oil layer rich in the monoalkylphosphoric acid.
COPYRIGHT: (C)1986,JPO&Japio

Abstract translation: 目的：为了经济地获得标题物质，通过在烃中使特定的（未饱和的脂族醇与多磷酸）反应，将回收的磷酸再利用并促进产物的分离和纯化，并将所得的反应混合物用 由低级醇和水组成的溶剂。 构成：使1mol 8-36C（un）饱和脂族醇（例如十二烷醇）与2-10mol浓度为正磷酸的浓度为100-116％的多磷酸在一种或多种溶剂中反应 选自4-8C饱和脂族烃（如正己烷）和5-7C饱和脂环烃（如环己烷）。 向反应混合物中加入1-4C醇和水，以使正磷酸迁移到低级醇和水的层中。 通过该方法有效地从单烷基磷酸分离的正磷酸被浓缩并重新使用。 可以通过从富含单烷基磷酸的油层中蒸除溶剂，低级醇和水来获得目标物质。