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    • 2. 发明授权
    • Method for producing polyamide 6 of a low extract content, high viscosity stability and low remonomerization rate
    • 低提取物含量的聚酰胺6的制备方法,高粘度稳定性和低再聚合速率
    • US06525167B1
    • 2003-02-25
    • US09913122
    • 2001-08-09
    • Ralf MohrschladtVolker HildebrandtMotonori Yamamoto
    • Ralf MohrschladtVolker HildebrandtMotonori Yamamoto
    • C08G6904
    • C08G69/04C08G69/16
    • The continuous process for producing polyamides by reacting at least one aminonitrile with water comprises the following steps: (10) reacting at least one aminonitrile with water at a temperature of from 200 to 290° C. at a pressure of from 40 to 70 bar in a flow tube containing a Brönsted acid catalyst selected from a beta-zeolite, sheet-silicate or metal oxide catalyst in the form of a fixed bed, (11) diabatically or adiabatically expanding the reaction mixture from step (1) into a first separation zone to a pressure of from 20 to 40 bar, the pressure being at least 10 bar lower than the pressure in step (1), and to a temperature within the range from 220 to 290° C. by flash evaporation and removal of ammonia, water and any aminonitrile monomer and oligomer, (12) further reacting the reaction mixture from step (2) in the presence of water at a temperature of from 200 to 290° C. and a pressure of from 25 to 55 bar and in the presence or absence of a Brönsted acid catalyst selected from a beta-zeolite, sheet-silicate or metal oxide catalyst in the form of a fixed bed, (13) diabatically or adiabatically expanding the reaction mixture from step (3) into a second separation zone to a pressure of from 0.01 to 20 bar, the pressure being at least 20 bar lower than the pressure in step (3), and to a temperature within the range from 220 to 290° C. by flash evaporation and removal of ammonia, water and any aminonitrile monomer and oligomer.
    • 通过使至少一种氨基腈与水反应生产聚酰胺的连续方法包括以下步骤:(10)在200至290℃的温度下,在40至70巴的压力下使至少一种氨基腈与水反应, 含有布朗斯台德酸催化剂的流动管,其选自固体床形式的β-沸石,硅酸盐或金属氧化物催化剂,(11)将反应混合物从步骤(1)进行绝热或绝热膨胀到第一分离区 压力为20至40巴,压力比步骤(1)中的压力低至少10巴,并且通过闪蒸和除去氨,水的温度在220至290℃的范围内 和任何氨基腈单体和低聚物,(12)在水存在下,在200-290℃的温度和25至55巴的压力下,使步骤(2)的反应混合物进一步反应,并在 没有布朗斯台德酸催化剂选择f 以固定床形式的β-沸石,片状硅酸盐或金属氧化物催化剂(13)将步骤(3)的反应混合物从第二分离区中分离或绝热膨胀至压力为0.01至20巴 ,压力比步骤(3)中的压力低至少20巴,并通过闪蒸和氨,水和任何氨基腈单体和低聚物的除去而达到220-290℃的温度。
    • 5. 发明授权
    • Continuous method for producing polyamides from aminonitriles
    • 从氨腈生产聚酰胺的连续方法
    • US06288207B1
    • 2001-09-11
    • US09600958
    • 2000-07-25
    • Ralf MohrschladtDieter KraussVolker Hildebrandt
    • Ralf MohrschladtDieter KraussVolker Hildebrandt
    • C08G6904
    • C08G69/04C08G69/08C08G69/16
    • The continuous process for producing a polyamide by reacting at least one aminonitrile with water comprises the following steps: (1) reacting at least one aminonitrile with water at a temperature from 90 to 400° C. and a pressure from 0.1 to 15×106 Pa in a flow tube containing packing elements of a Brönsted acid catalyst selected from beta-zeolite, sheet-silicate or titanium dioxide packing elements and metallic packing elements to obtain a reaction mixture, (2) further reacting the reaction mixture at from 150 to 400° C. and a pressure which is lower than the pressure in step 1, the temperature and pressure being selected so as to obtain a first gas phase and a first liquid or a first solid phase or a mixture of first solid and first liquid phase, and the first gas phase is separated from the first liquid or first solid phase or the mixture of first liquid and first solid phase, and (3) admixing the first liquid or the first solid phase or the mixture of first liquid and first solid phase with a gaseous or liquid phase comprising water at a temperature from 150 to 370° C. and a pressure from 0.1 to 30×106 Pa to obtain a product mixture.
    • 通过使至少一种氨基腈与水反应生产聚酰胺的连续方法包括以下步骤:(1)在90至400℃的温度和0.1至15×10 6 Pa的压力下使至少一种氨基腈与水反应, 含有选自β-沸石,片状硅酸盐或二氧化钛填料的布朗斯台德酸催化剂的填充元件和金属填充元素的流动管,以获得反应混合物,(2)使反应混合物在150-400℃下进一步反应 和低于步骤1中的压力的​​压力,选择温度和压力以获得第一气相和第一液体或第一固相或第一固体和第一液相的混合物,第一 气相与第一液体或第一固相或第一液体和第一固相的混合物分离,和(3)混合第一液体或第一固相或第一液体和第一固体p的混合物 在含有水的温度为150〜370℃,压力为0.1〜30×10 6 Pa的气相或液相中搅拌,得到产物混合物。
    • 7. 发明授权
    • Continuous preparation of polyamides from aminonitriles
    • 从氨基腈连续制备聚酰胺
    • US06316588B1
    • 2001-11-13
    • US09600957
    • 2000-07-25
    • Ralf MohrschladtVolker HildebrandtEberhard Fuchs
    • Ralf MohrschladtVolker HildebrandtEberhard Fuchs
    • C08G6900
    • C08G69/00C08G69/04C08G69/08C08G69/16C08G69/28C08K3/011
    • A continuous process for preparing a polyamide by reacting at least one aminonitrile with water comprises: (1) reacting at least one aminonitrile with water at a temperature from 90 to 400° C. and a pressure from 0.1 to 35×106 Pa in a flow tube containing a Brönsted acid catalyst selected from a beta-zeolite catalyst, a sheet-silicate catalyst or a titanium dioxide catalyst comprising from 70 to 100% by weight of anatase and from 0 to 30% by weight of rutile and in which up to 40% by weight of the titanium dioxide may be replaced by tungsten oxide to obtain a reaction mixture, (2) further reacting the reaction mixture at a temperature from 150 to 400° C. and a pressure which is lower than the pressure in step 1, in the presence of a Brönsted acid catalyst as in (1), the temperature and pressure being selected so as to obtain a first gas phase and a first liquid or a first solid phase or a mixture of first solid and first liquid phase, and the first gas phase is separated from the first liquid or the first solid phase or from the mixture of first liquid and first solid phase, and (3) admixing the first liquid or the first solid phase or the mixture of first liquid and first solid phase with a gaseous or liquid phase comprising water at a temperature from 150 to 370° C. and a pressure from 0.1 to 30×106 Pa to obtain a product mixture.
    • 通过使至少一种氨基腈与水反应制备聚酰胺的连续方法包括:(1)在90-400℃的温度和0.1至35×10 6 Pa的压力下使至少一种氨基腈与水反应, 选自β-沸石催化剂,片状硅酸盐催化剂或二氧化钛催化剂的布朗斯台德酸催化剂,其包含70至100重量%的锐钛矿和0至30重量%的金红石,其中至多40重量% 二氧化钛的重量可以被氧化钨代替以获得反应混合物,(2)使反应混合物在150-400℃的温度和低于步骤1的压力的压力下反应,在 存在如(1)中所述的布朗斯台德酸催化剂,选择温度和压力以获得第一气相和第一液体或第一固相或第一固体和第一液相的混合物,并且第一气体 相与杉木分离 第一液体或第一固相或第一液体和第一固相的混合物,和(3)将第一液体或第一固相或第一液体和第一固相的混合物与包含水的气相或液相混合 温度为150〜370℃,压力为0.1〜30×10 6 Pa,得到产物混合物。
    • 10. 发明授权
    • Method for producing polyamides from amino carboxylic acid compounds
    • 从氨基羧酸化合物制备聚酰胺的方法
    • US06362307B1
    • 2002-03-26
    • US09622337
    • 2000-08-16
    • Ralf MohrschladtVolker Hildebrandt
    • Ralf MohrschladtVolker Hildebrandt
    • C08G6900
    • C08G69/04C08G69/08
    • Polyamides are produced by reacting aminocarboxylic acid compounds of the general formula I H2N—(CH2)m—COR1  (I) where R1 is OH, O—C1-12-alkyl or NR2R3, where R2 and R3 are independently hydrogen, C1-12-alkyl or C5-8-cycloalkyl, and m is an integer from 3 to 12, optionally in a mixture with aminonitriles and their hydrolysis products and optionally in the presence of water, in a liquid phase at elevated pressure and elevated temperature in the presence of metal oxides as heterogeneous catalysts, the metal oxides being used in a form which permits mechanical removal from the reaction mixture and being removed from the reaction mixture during or after the polymerization.
    • 聚酰胺通过使通式I的氨基羧酸化合物反应来制备,其中R 1是OH,O-C 1-12 - 烷基或NR 2 R 3,其中R 2和R 3独立地是氢,C 1-12 - 烷基或C 5-8 - 环烷基,m是 在金属氧化物作为非均相催化剂的情况下,在升高的压力和升高的温度下,在液相中,任选地与氨基腈及其水解产物和其水解产物的混合物,任选地与氨基腈及其水解产物的混合物,任选地与氨基腈及其水解产物的混合物, 以允许从反应混合物机械除去并在聚合期间或之后从反应混合物中除去的形式。