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    • 4. 发明授权
    • Process for the preparation of tetrachloro-1,4-benzoquinone
    • 制备四氯-1,4-苯醌的方法
    • US5525744A
    • 1996-06-11
    • US327033
    • 1994-10-21
    • Otto ArndtHans Schubert
    • Otto ArndtHans Schubert
    • B01J27/128C07B61/00C07C46/00C07C46/06C07C46/10C07C50/24C10M131/10
    • C10M131/10C07C46/06C07C46/10C10M2211/042C10M2211/06
    • A process for the preparation of tetrachloro-1,4-benzoquinone of high purity by the action of chlorine and concentrated hydrochloric acid on hydroquinone, by introducing a part of the hydroquinone to be employed into an initially introduced 4- to 6-fold molar amount--based on the total amount of hydroquinone--of 20 to 37 % aqueous hydrochloric acid containing catalytic amounts of iron(III) ions and an anionic dispersant, introducing 1.5 to 2.0 times the molar amount--based on total hydroquinone--of chlorine as a gas into this solution at a temperature of 20.degree. to 90.degree. C., then adding the residual amount of hydroquinone as a solid or in dissolved form, introducing 1.5 to 2.0 times the molar amount of chlorine as a gas, keeping the concentration of the hydrochloric acid here at 23-25% by addition of water and finally raising the temperature to 100.degree. to 107.degree. C. with further introduction of chlorine as a gas (1.7 to 2.5 times the molar amount) and dilution with water to a hydrochloric acid concentration of 20 to 22%.
    • 通过将氯和浓盐酸作用于氢醌的作用制备高纯度四氯-1,4-苯醌的方法,通过将待使用的一部分氢醌引入最初引入的4至6倍摩尔量 - 基于氢醌的总量 - 含有催化量的铁(III)离子和阴离子分散剂的20至37%盐酸水溶液,引入基于总氢醌的1.5至2.0倍摩尔量的氯作为气体 在20〜90℃的温度下加入到该溶液中,然后加入残留量的氢醌作为固体或溶解形式,引入作为气体的氯的摩尔量的1.5-2.0倍,保持浓度的盐酸 酸加入水中,最后升温至100〜107℃,再加入氯气作为气体(1.7〜2.5倍摩尔量),用水稀释至盐酸 酸浓度为20〜22%。
    • 5. 发明授权
    • Process for the preparation of naphthostyril
    • 制备萘普生的方法
    • US4824962A
    • 1989-04-25
    • US170065
    • 1988-03-14
    • Otto ArndtTheodor Papenfuhs
    • Otto ArndtTheodor Papenfuhs
    • C07D209/92
    • C07D209/92
    • Process for the preparation of naphthostyril by dissolving 1,8-naphthalimide in an aqueous solution of lithium hydroxide and potassium hydroxide while heating at 40.degree. C. to 80.degree. C., cooling the solution obtained to 14.degree. C. and seeding it at said temperature with a maximum of 1 mol-% of sodium 1,8-naphthalimide per 1 mol of 1,8-naphthalimide used, then adding chlorine bleaching liquor at 10.degree. C. to 20.degree. C., reductively removing excess active chlorine after the reaction has taken place, adjusting the alkaline aqueous solution produced of the alkali-metal salt of the 1-aminonaphthal-ene-8-carboxylic acid formed to a pH of 2.0 by adding acid and isolating the naphthostyril which precipitates in this process.
    • 通过在40℃至80℃下加热将1,8-萘二甲酰亚胺溶解在氢氧化锂和氢氧化钾的水溶液中而制备萘未斯特林的方法,将所得溶液冷却至14℃,并将其在所述 温度,每1摩尔1,8-萘二甲酰亚胺使用1,8-萘二甲酰亚胺钠最多1摩尔%,然后在10℃至20℃下加入氯漂白液,然后还原除去过量的活性氯 发生反应,通过加入酸调节形成pH为2.0的1-氨基萘-8-羧酸的碱金属盐产生的碱性水溶液,并分离出在该过程中析出的萘并三唑。
    • 6. 发明授权
    • Process for the preparation of 2,6-dichloro-4-nitroaniline
    • 2,6-二氯-4-硝基苯胺的制备方法
    • US4605767A
    • 1986-08-12
    • US734972
    • 1985-05-16
    • Otto ArndtTheodor Papenfuhs
    • Otto ArndtTheodor Papenfuhs
    • C07C209/74C07C67/00C07C209/00C07C211/52C07C85/24C07C87/60
    • C07C209/74
    • Process for the preparation of 2,6-dichloro-4-nitroaniline by chlorination of 4-nitroaniline with chlorine bleaching liquor in water using acids, which comprises chlorinating 1 mole of 4-nitroaniline in 3-6 moles of hydrochloric acid (HCl) or nitric acid (HNO.sub.3) in the form of a dilute, aqueous acid in the presence of a dispersing agent which is stable under the reaction conditions, the chlorination initially being carried out at 5.degree. to 10.degree. C. and then at 15.degree.-20.degree. C. and, finally, after 90-95% of the 2-chloro-4-nitroaniline intermediately formed has been converted into 2,6-dichloro-4-nitroaniline, the temperature of the aqueous suspension being increased from 15.degree.-20.degree. C. to 70.degree. C., without further addition of chlorine bleaching liquor, and then by post-chlorinating, by renewed addition of chlorine bleaching liquor, at temperatures between 20.degree. and 70.degree. C., bringing the pH of the aqueous suspension to 9.0 and filtering off the 2,6-dichloro-4-nitroaniline formed and washing it with dilute mineral acid.
    • 通过使用酸在氯水中用氯漂白液氯化4-硝基苯胺的方法制备2,6-二氯-4-硝基苯胺的方法,该方法包括将1-6摩尔盐酸(HCl)中的1摩尔4-硝基苯胺氯化,或 硝酸(HNO 3)为稀酸水溶液,在分散剂存在下,在反应条件下稳定,氯化最初在5〜10℃进行,然后在15〜-20℃ ℃,最后,90-95%的中间形成的2-氯-4-硝基苯胺已经转化为2,6-二氯-4-硝基苯胺,水悬浮液的温度从15°-20 在不进一步加入氯漂白液的情况下,通过后续氯化,通过在20℃至70℃的温度下再次加入氯漂白液,使水悬浮液的pH值达到70℃ 至9.0,滤出2,6-二氯-4-硝基苯胺 d用稀释的无机酸洗涤。
    • 7. 发明授权
    • Process for the preparation of 2,5-di-phenylamino-terephthalic acid and
its dialkyl esters
    • 制备2,5-二苯基氨基 - 对苯二甲酸及其二烷基酯的方法
    • US5616779A
    • 1997-04-01
    • US397733
    • 1995-03-02
    • Otto Arndt
    • Otto Arndt
    • C07C229/62B01J31/04C07B61/00C07C227/06C07C227/08C07C227/16C07C227/18C07C101/38C07C101/68C07C103/76
    • C07C227/08C07C227/16
    • The present invention relates to a process for the preparation of 2,5-di-phenylamino-terephthalic acid and its dialkyl esters of the formula ##STR1## in which R is a hydrogen atom or a methyl or an ethyl group, by reaction of a succinic acid dialkyl ester with a sodium alcoholate in xylene, treatment of the resulting 2,5-dihydroxy-cyclohexadiene-1,4-di-carboxylic acid dialkyl ester with acid and aniline, dehydrogenation of the resulting 2,5-di-phenylamino-dihydro-(3,6)-terephthalic acid dialkyl ester by means of oxygen, if appropriate hydrolysis of the 2,5-di-phenylamino-terephthalic acid dialkyl ester formed and liberation of the 2,5-di-phenylamino-terephthalic acid from the di-sodium salt formed. The 2,5-di-phenylamino-dihydro-(3,6)-terephthalic acid dialkyl ester is reacted with pure oxygen in the presence of an alkali metal ion and/or an alkaline earth metal ion. This significantly decreases undesirable impurities.
    • 本发明涉及通过琥珀酸二烷基酯与二甲苯醇钠反应制备2,5-二苯基氨基 - 对苯二甲酸及其通式为乙基的二烷基酯的方法,处理 的所得的2,5-二羟基 - 环己二烯-1,4-二羧酸二烷基酯与酸和苯胺,所得的2,5-二苯基氨基 - 二氢 - (3,6) - 对苯二甲酸二烷基酯 如果合适的水解形成的2,5-二苯基氨基 - 对苯二甲酸二烷基酯和形成的二钠盐释放2,5-二苯基氨基 - 对苯二甲酸,通过氧气。 2,5-二苯基氨基 - 二氢 - (3,6) - 对苯二甲酸二烷基酯在碱金属离子和/或碱土金属离子存在下与纯氧反应。 这显着降低了不需要的杂质。