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公开(公告)号：US20240336560A1
公开(公告)日：2024-10-10
申请号：US17800452
申请日：2022-06-21
申请人： ZHEJIANG UNIVERSITY , ZHEJIANG NHU CO., LTD. , ZHEJIANG NHU SPECIAL MATERIALS CO., LTD. , ZHEJIANG NHU NYLON MATERIALS CO., LTD.
发明人： Zhirong Chen , Wenbin Wu , Hong Yin , Zengshi Zha , Keyan Wang , Li Ma , Guodong Huang , Guiyang Zhou , Yong Xu
IPC分类号： C07C253/10 , B01J31/18 , B01J37/04 , C07F9/06 , C07F9/6571
CPC分类号： C07C253/10 , B01J31/185 , B01J37/04 , C07F9/062 , C07F9/6571 , B01J2231/322 , B01J2231/52 , B01J2531/004 , B01J2531/847
摘要： A multidentate phosphite ligand is used in the catalytic synthesis of adiponitrile. The ligand is represented by the following general formula (I). The method of catalytic synthesis of adiponitrile comprises primary hydrocyanation, isomerization, and secondary hydrocyanation reactions, wherein the catalyst adopted each comprises a phosphite ligand-nickel complex composed of a nickel precursor and a multidentate phosphite ligand. The ligand molecule has a higher electron cloud density, and the phosphorus content capable of participating in coordination in the ligand molecule per unit mass is higher, so that the catalytic activity of the catalyst is improved, and the amount of the catalyst is reduced.
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公开(公告)号：US20220025120A1
公开(公告)日：2022-01-27
申请号：US17416587
申请日：2019-11-20
发明人： Zhirong Chen , Hong Yin , Hangjun Deng , Guiyang Zhou , Danqi Zhu , Xiaoxiao Wu , Wengang Hong , Guisheng Qiu , Qichuan Li
摘要： The present disclosure discloses a semi-aromatic polyamide and a preparation method therefor. The semi-aromatic polyamide is obtained by polymerization reaction using a diamine, a dibasic acid and a monoacid as main raw materials while adding a special end-capping agent. The semi-aromatic polyamide prepared according to the present disclosure has good thermal stability, a yellowness index of less than 20, a glass transition temperature of 90° C. or above, and a melting point of 300° C. or above, and can be applied to spare parts for fuel pipelines in automobiles, and electronic and electrical industries such as LED panels.
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3.发明申请公开(公告)号：US20230094350A1
公开(公告)日：2023-03-30
申请号：US17795838
申请日：2021-09-16
申请人： ZHEJIANG UNIVERSITY , ZHEJIANG NHU CO., LTD. , SHANDONG NHU AMINO ACID CO., LTD. , ZHEJIANG NHU SPECIAL MATERIALS CO., LTD.
发明人： Zhirong Chen , Wenbin Wu , Hong Yin , Yaqing Liu , Zengshi Zha , Zhichao Feng , Tinglan Zhang , Guodong Huang
IPC分类号： B01J31/06 , C08F30/02 , C08J9/14 , B01J23/755 , B01J31/28 , B01J35/10 , B01J35/00 , C07C253/10
摘要： A porous polymer has a pore volume of 0.3 to 2.5 cm3/g and comprises a pore having a first pore diameter and a pore having a second pore diameter. A ratio of pore volume of the pore having a first pore diameter to pore volume of the pore having a second pore diameter is 1 to 10:1. The porous polymer is obtained by self-polymerization or copolymerization of at least one of the phosphorus ligands, and phosphorous content of the porous polymer is 1 to 5 mmol/g. The porous polymer-nickel catalyst made of the porous polymer has a significant increase in water resistance, which may reduce the consumption of phosphorus ligands, eliminating the steps of removing water from raw materials and reaction system water control, which greatly saves process equipment investment. When used in the preparation of adiponitrile from butadiene, it has high catalytic activity, high reaction selectivity, and high linearity.
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公开(公告)号：US09567440B2
公开(公告)日：2017-02-14
申请号：US14655326
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： Zhirong Chen , Woyuan Li , Haoran Li , Ming Lian , Hong Yin , Guiyang Zhou , Xinfeng Zheng
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/10 min, weight-average molecular weight as measured by GPC is over 4.2×104, 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，将N-甲基吡咯烷酮作为溶剂和通过脱水形成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。 鉴于MFR低于125g / 10min，通过GPC测得的重均分子量超过4.2×104，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，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。
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5.发明授权公开(公告)号：US11440996B2
公开(公告)日：2022-09-13
申请号：US16957934
申请日：2018-07-12
发明人： Woyuan Li , Hong Yin , Zhirong Chen , Baishan Hu , Guiyang Zhou , Hangjun Deng , Ming Lian , Xiongwei Zhang , Qichuan Li , Jiang Zhao
IPC分类号： C08G75/0254 , C08G75/0213 , C08G75/029
摘要： A preparation method of a polyphenylene sulfide resin, and a polyphenylene sulfide resin prepared by the method using a sulfur-containing compound, an alkaline substance and p-dichlorobenzene as raw materials, a fatty acid as a polycondensation aid to carry out a polycondensation reaction. After purification treatment, a primary polyphenylene sulfide is obtained, which then reacts with a terminal-group adjusting agent at a high temperature to generate the polyphenylene sulfide resin resulting in high yield and low cost. The prepared polyphenylene sulfide resin has high reactivity, high melting crystallization temperature and excellent thermal stability. The resulting polyphenylene sulfide resin can be directly used for extrusion and injection molding.
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公开(公告)号：US11220478B2
公开(公告)日：2022-01-11
申请号：US16955511
申请日：2018-07-12
发明人： Zhirong Chen , Woyuan Li , Hong Yin , Guíyang Zhou , Haoran Li , Shuaifeng Pan , Ming Lian , Guangde Qin , Qichuan Li
IPC分类号： C07C319/20 , C01D5/02
摘要： The present disclosure discloses a preparation method for 4-phenylthio-benzenethiol. The preparation method comprises the following steps: subjecting phenyl sulfide as a raw material to a halogenation reaction to obtain 4-halophenyl sulfide; subjecting the 4-halophenyl sulfide to a sulfhydrylation reaction to obtain a 4-phenylthio-phenylthiolate; and subjecting the 4-phenylthio-phenylthiolate to acidification. The preparation method of the present disclosure avoids the use of materials such as thiophenol which pollutes the environment, and realizes efficient recycling of the reaction materials, solvents, water and the like. The preparation method of the present disclosure is a green process for the synthesis of 4-phenylthio-phenylthiol without organic waste, waste acid and waste water discharge.
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公开(公告)号：US20200055985A1
公开(公告)日：2020-02-20
申请号：US15779414
申请日：2017-06-29
发明人： Zhirong Chen , Hong Yin , Qin Zhang , Xiaoxiao Wu , Wengang Hong , Hangjun Deng , Guiyang Zhou , Changze Wang
摘要： The present disclosure provides a production method of a semi-aromatic polyamide, and a semi-aromatic polyamide. Said production method of a semi-aromatic polyamide includes: step 1 of subjecting an initial charge of a diamine and a binary acid in an amine/acid molar ratio of less than 1.0 to form a slurry together with water and a catalyst, and subjecting the slurry to heating and dissolution to form a saline solution; step 2 of dehydrating said saline solution after detecting the composition thereof, detecting the content of diamine in a steam condensate from a dehydration unit, adjusting the amine/acid molar ratio to be larger than 1.0 by a molten diamine and a monoacid as a molecular weight regulator, and performing pre-polymerization; and step 3 of subjecting a pre-polymerization solution to post-polycondensation after vacuum flashing. The semi-aromatic polyamide of the present disclosure has a low gel content, excellent performance and extensive scope of application.
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公开(公告)号：US20180043281A1
公开(公告)日：2018-02-15
申请号：US15549833
申请日：2015-12-23
发明人： Zhirong Chen , Zhixuan Wang , Cong Chen , Zhengjiang Wang , Cunchao Wang , Yin Li , Zhixiang Zhang
IPC分类号： B01D9/00 , C07C319/28 , C07C323/58
CPC分类号： B01D9/0036 , B01D9/0013 , B01D9/0027 , B01D9/0054 , B01D2009/0086 , C07C319/28 , C07C323/58
摘要： The present disclosure relates to a method for continuous preparation of high bulk density methionine crystals. The process of the method is as follows: a hydrolysate solution, which is obtained from a reaction of 5-(β-methylmercaptoethyl) hydantoin and a potassium carbonate solution, is mixed with an external circulation material from a DTB neutralization crystallizer having a gas phase neutralization section; after being cooled, the mixture enters a liquid distributor of a neutralization region in the upper part of the crystallizer and is sprayed in the form of liquid droplet or trickle into carbon dioxide gas for neutralization reaction, and then naturally falls into a crystallization region in the lower part to be mixed with a material in the region; the obtained mixture grows on fine crystals in a system to form crystals having larger particle diameters, and meanwhile new crystal nucleuses are formed; in a deposition area in the middle part of the crystallization region, the crystals having larger particle diameters deposits into an elutriation leg, while the fine crystals circulate with the external circulation material, and a part of the external circulation material is used to elutriate the crystals in the elutriation leg, while another part of the same is used to be mixed with the hydrolysate solution; and the crystals in the elutriation leg are separated, washed and dried to obtain the high bulk density methionine product.
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公开(公告)号：US10293273B2
公开(公告)日：2019-05-21
申请号：US15549833
申请日：2015-12-23
发明人： Zhirong Chen , Zhixuan Wang , Cong Chen , Zhengjiang Wang , Cunchao Wang , Yin Li , Zhixiang Zhang
IPC分类号： B01D9/00 , C07C319/28 , C07C323/58
摘要： The present disclosure relates to a method for continuous preparation of high bulk density methionine crystals. The process of the method is as follows: a hydrolysate solution, which is obtained from a reaction of 5-(β-methylmercaptoethyl) hydantoin and a potassium carbonate solution, is mixed with an external circulation material from a DTB neutralization crystallizer having a gas phase neutralization section; after being cooled, the mixture enters a liquid distributor of a neutralization region in the upper part of the crystallizer and is sprayed in the form of liquid droplet or trickle into carbon dioxide gas for neutralization reaction, and then naturally falls into a crystallization region in the lower part to be mixed with a material in the region; the obtained mixture grows on fine crystals in a system to form crystals having larger particle diameters, and meanwhile new crystal nucleuses are formed; in a deposition area in the middle part of the crystallization region, the crystals having larger particle diameters deposits into an elutriation leg, while the fine crystals circulate with the external circulation material, and a part of the external circulation material is used to elutriate the crystals in the elutriation leg, while another part of the same is used to be mixed with the hydrolysate solution; and the crystals in the elutriation leg are separated, washed and dried to obtain the high bulk density methionine product.
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10.发明授权公开(公告)号：US11180440B2
公开(公告)日：2021-11-23
申请号：US16954774
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： Zhirong Chen , Jianyong Mao , Baishan Hu , Guanbing Li , Haoran Li , Yu Wang , Yingkuo Yang , Qing Liu , Jiyu Tang , Weiyong Chen
IPC分类号： C07C209/52 , B01J23/78 , B01J35/04 , C07C209/48
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.
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