公开(公告)号：EP4289855A1

公开(公告)日：2023-12-13

申请号：EP22755062.1

申请日：2022-06-29

申请人： Zhejiang NHU Company Ltd. ,  Zhejiang University ,  Zhejiang NHU Special Materials Co., Ltd. ,  ZHEJIANG NHU NYLON MATERIALS CO., LTD.

发明人： ZHA, Zengshi ,  CHEN, Zhirong ,  WU, Wenbin ,  ZHANG, Tinglan ,  YIN, Hong ,  WANG, Keyan ,  ZHOU, Litao ,  LI, Haoran ,  HUANG, Guodong ,  XU, Yong

IPC分类号： C07F9/141 ,  C07F9/145 ,  C07F9/572 ,  C07F9/6506 ,  C07F9/6584 ,  B01J31/02 ,  B01J31/06 ,  B01J35/08

摘要： A method for preparing a phosphorus-containing ligand is provided, which includes: mixing a phosphorus chloride compound, polypyridine ionic liquid-loaded porous microspheres with a first organic solvent to obtain a first mixture, and mixing a compound in Formula (2) with a second organic solvent to obtain a second mixture,

wherein Z is a multivalent aliphatic hydrocarbon group or a multivalent aromatic hydrocarbon group comprising at least one substituent group, wherein the substituent group is selected from hydrogen atom, halogen atom, C 1 -C 10 alkyl group, C 1 -C 10 alkoxy group, C 1 -C 10 alkanoyl group, aryl group, heteroaryl group, cyano group, or nitro group, and n is an integer from 1 to 8; and mixing the first mixture with the second mixture to make the first mixture react with the second mixture to obtain a reaction mixture, removing generated HCl, filtrating to obtain a filter liquor, and treating the filter liquor to obtain the phosphorus-containing ligand.

公开(公告)号：EP2940061A1

公开(公告)日：2015-11-04

申请号：EP13867285.2

申请日：2013-10-29

申请人： Zhejiang Nhu Special Materials Co., Ltd. ,  Zhejiang University ,  Shangyu Nhu Biological Chemical Co., Ltd. ,  Zhejiang Nhu Company Ltd

发明人： CHEN, Zhirong ,  LI, Woyuan ,  LI, Haoran ,  LIAN, Ming ,  YIN, Hong ,  ZHOU, Guiyang ,  ZHENG, Xinfeng

IPC分类号： C08G75/02

CPC分类号： C08G75/16 ,  C08G75/02

摘要： The present invention discloses a fiber-grade polyphenylene sulfide resin synthesis method, taking sodium bisulfide and p-dichlorobenzene as raw materials, N-methyl pyrrolidone as the solvent and C5-C6 fatty acid salt formed through dehydration to C5-C6 fatty acid and sodium hydroxide as the polymerization additive for synthesis through polymerization. White polyphenylene sulfide resin is obtained through acidification and washing of reaction slurry. In view of the fact that MFR is below 125 g/10min, weight-average molecular weight as measured by GPC is over 4.2×10 4 , and whiteness is over 90, it can satisfy requirements for fiber polyphenylene sulfide resin. C5-C6 fatty acid salt according to the method of the present invention has a higher solubility in NMP, which can better promote polymerization. It is to be fully diverted into the filtrate after filter prior to conversion into free fatty acid again through acidification with hydrochloric acid. C5-C6 fatty acid is available for azeotropy with water, which has a limited solubility in water. Therefore, it is applicable to recycle C5-C6 fatty acid from the filtrate through azeotropy with water, and thereby solve the problem with separation of additive and sodium chloride that are soluble in water.

摘要翻译： 本发明公开了以二硫化二钠和对二氯苯为原料的纤维级聚苯硫醚树脂的合成方法，以N-甲基吡咯烷酮为溶剂，通过脱水形成C5-C6脂肪酸和 氢氧化物作为通过聚合合成的聚合添加剂。 白色聚苯硫醚树脂通过反应浆液的酸化和洗涤得到。 考虑到MFR低于125g / 10min，通过GPC测定的重均分子量超过4.2×10 4，白度超过90，可以满足纤维聚苯硫醚树脂的要求。 根据本发明方法的C5-C6脂肪酸盐在NMP中的溶解度较高，这可以更好地促进聚合。 过滤后将其全部转入滤液，然后再用盐酸酸化再转化成游离脂肪酸。 C5-C6脂肪酸可与水共沸，其在水中的溶解度有限。 因此，适用于通过与水共沸从滤液中回收C5-C6脂肪酸，从而解决了可溶于水的添加剂和氯化钠的分离问题。

公开(公告)号：EP3677566A1

公开(公告)日：2020-07-08

申请号：EP18890918.8

申请日：2018-11-30

申请人： Zhejiang NHU Company Ltd. ,  Zhejiang University ,  Shandong Nhu Amino Acid Co., Ltd. ,  Shandong Nhu Fine Chemical Science and Technology Company Ltd.

发明人： CHEN, Zhirong ,  MAO, Jianyong ,  HU, Baishan ,  LI, Guanbing ,  LI, Haoran ,  WANG, Yu ,  YANG, Yingkuo ,  LIU, Qing ,  TANG, Jiyu ,  CHEN, Weiyong

IPC分类号： C07C209/52 ,  C07C209/48 ,  C07C211/36 ,  B01J8/02

摘要： The present disclosure relates to a method for preparing isophorone diamine by means of a hydrogenation reduction of isophorone nitrile imine. The hydrogenation reduction is continuously carried out in a multi-stage bubble column reactor loaded with a supported alkaline cobalt-based catalyst, wherein isophorone nitrile imine is successively in countercurrent contact with hydrogen in each stage of the reactor to carry out a hydrogenation reduction reaction, so as to obtain the isophorone diamine. The preparation method solves the problem of back-mixing, and further improves the conversion rate and the cis/trans ratio of the product.

公开(公告)号：EP3456728A1

公开(公告)日：2019-03-20

申请号：EP17870452.4

申请日：2017-05-18

申请人： Zhejiang Nhu Company Ltd

发明人： DENG, Fuxiang ,  DING, Yu ,  XUE, Wei ,  SHENG, Yu ,  YAN, Wenwu ,  YU, Ming ,  ZHOU, Yougui ,  LI, Haoran

IPC分类号： C07H13/06 ,  C07H1/00

摘要： The present invention discloses a method for preparing sucralose-6-acetate in a biphasic liquid-liquid system. The method comprises slowly dropwise adding an inert non-polar solvent containing a chlorinating agent to an N,N-dimethyl formamide (DMF) solution of sucrose-6-acetate; then reacting the biphasic liquid-liquid mixture at a certain temperature for 9-20 hours; cooling the system to room temperature after stopping heating, and settling the solution to form layers, an upper layer being an inert non-polar solvent layer, and a lower layer being a DMF solution layer containing the product; hydrolyzing, neutralizing, and filtering the lower layer to obtain a filtrate, and then concentrating the filtrate to obtain a concentrate; dissolving the concentrate in water, and obtaining the product by extraction using ethyl acetate and crystallization, the inert non-polar solvent being an alkane solvent containing 8-18 carbon atoms that is not mutually soluble with DMF. The method has a high product yield, and can significantly reduce the decomposition of DMF, thereby reducing costs.