Process of preparing alkylhydroxyalkylcellulose
    3.
    发明授权
    Process of preparing alkylhydroxyalkylcellulose 有权
    制备烷基羟烷基纤维素的方法

    公开(公告)号:US07402668B2

    公开(公告)日:2008-07-22

    申请号:US10197070

    申请日:2002-07-17

    CPC classification number: C08B11/193

    Abstract: A process of preparing alkylhydroxyalkylcellulose (e.g., methylhydroxyethylcellulose and methylhydroxypropylcellulose) by reaction of cellulose in the presence of alkali metal hydroxide with an alkylating agent and a hydroxyalkylating agent is described. The process includes: (a) alkalizing cellulose by means of 0.9 to 2.9 equivalents of an alkali metal hydroxide I/AGU of the cellulose in the form of an aqueous alkali metal hydroxide solution, in the presence of a suspension medium containing at least 0.2 equivalents of an alkylating agent I/AGU of the cellulose; (b) reacting the alkalized cellulose of step (a) with alkylating agent I and a hydroxyalkylating agent at a temperature above 65° C.; (c) adding additional alkali metal hydroxide 11 in the form of an aqueous alkali metal hydroxide solution; and (d) adding additional alkylating agent 11 in an amount of at least the absolute value of the difference between (i) the number of equivalents of alkylating agent I/AGU of the cellulose already added, and (ii) the total number of equivalents of alkali metal hydroxide/AGU of the cellulose added. Additional alkylating agent 11 is not added in step (d) if (i) the number of equivalents of alkylating agent I/AGU of the cellulose already added exceeds (ii) the total number of equivalents of alkali metal hydroxide/AGU of the cellulose already added. In a further step (e), the alkylhydroxyalkylcellulose is isolated from the reaction mixture. The isolated alkylhydroxyalkylcellulose may be optionally purified.

    Abstract translation: 描述了通过在碱金属氢氧化物存在下纤维素与烷基化剂和羟烷基化剂反应来制备烷基羟烷基纤维素(例如甲基羟乙基纤维素和甲基羟丙基纤维素)的方法。 该方法包括:(a)在含有至少0.2当量的悬浮介质存在下,通过0.9至2.9当量的碱金属氢氧化物I / AGU将纤维素碱化为碱金属氢氧化物水溶液形式的纤维素碱化纤维素 的纤维素的烷基化剂I / AGU; (b)在高于65℃的温度下使步骤(a)的碱化纤维素与烷基化剂I和羟烷基化剂反应; (c)加入碱金属氢氧化物水溶液形式的另外的碱金属氢氧化物11; 和(d)添加额外的烷基化剂11,其量至少为(i)已经加入的纤维素的烷基化剂I / AGU的当量数之间的差异的绝对值,和(ii)总当量数 的碱金属氢氧化物/ AGU的纤维素加入。 如果(i)已经加入的纤维素的烷基化剂I / AGU的当量数超过(ii)已经在纤维素中的碱金属氢氧化物/ AGU的当量的总数,则在步骤(d)中不加入另外的烷基化剂11 添加。 在另外的步骤(e)中,从反应混合物中分离烷基羟烷基纤维素。 分离的烷基羟烷基纤维素可以任选地纯化。

    Process for preparing alkylhydroxyalkyl cellulose
    6.
    发明授权
    Process for preparing alkylhydroxyalkyl cellulose 有权
    制备烷基羟烷基纤维素的方法

    公开(公告)号:US06891034B2

    公开(公告)日:2005-05-10

    申请号:US09923011

    申请日:2001-08-03

    CPC classification number: C08B11/193

    Abstract: Described is a process of preparing alkylhydroxyalkyl cellulose, e.g., methylhydroxypropyl cellulose (MHPC). The process includes: (a) alkylating cellulose with an aqueous caustic solution containing from 1.5 to 5.5 equivalents of alkali metal hydroxide, e.g., NaOH, per anhydroglucose unit (AGU) of said cellulose, in the presence of a suspension agent, e.g., dimethyl ether, which contains alkyl halide, e.g., methyl chloride, in an amount of from (equivalents of alkali metal hydroxide per AGU minus 1.4) to (equivalents of alkali metal hydroxide per AGU plus 0.8); (b) reacting the alkalised cellulose of step (a) with one or more alkylene oxides, e.g., propylene oxide, at a temperature higher than 65° C., e.g., 85° C.; (c) adding alkyl halide, to the product of step (b), in an amount of at least the difference between (i) the equivalents of alkyl halide per AGU in step a) and (ii) the equivalents of alkali metal hydroxide added per AGU in step (a), provided that the amount of additionally added alkyl halide is at least 0.2 equivalents per AGU; and (d) isolating alkylhydroxyalkyl cellulose from the reaction mixture of step (c). Optionally the isolated alkylhydroxyalkyl cellulose may be purified.

    Abstract translation: 描述了制备烷基羟烷基纤维素的方法,例如甲基羟丙基纤维素(MHPC)。 该方法包括:(a)在悬浮剂例如二甲基甲酰胺存在下,用含有1.5至5.5当量碱金属氢氧化物(例如NaOH)的所述纤维素的每个脱水葡萄糖单元(AGU)的含水苛性碱溶液对纤维素进行烷基化 醚,其含有(每当AGU的碱金属氢氧化物的当量减去1.4)的烷基卤化物,例如甲基氯,(每个AGU的碱金属氢氧化物加上0.8当量); (b)使步骤(a)的碱化纤维素与一种或多种环氧烷如环氧丙烷在高于65℃,例如85℃的温度下反应; (c)将步骤(b)中的烷基卤添加至(i)步骤a)中每个AGU的烷基卤的当量与(ii)加入的碱金属氢氧化物的当量之间的至少差异的量 步骤(a)中的每个AGU,条件是额外添加的烷基卤化物的量为每个AGU至少0.2当量; 和(d)从步骤(c)的反应混合物中分离出烷基羟烷基纤维素。 任选地,分离的烷基羟烷基纤维素可以被纯化。

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