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1. 发明公开

US20240076261A1 METHOD FOR PREPARING HIGH-BULK-DENSITY IBUPROFEN SPHERICAL CRYSTAL AND PRODUCT THEREOF 审中-公开
公开(公告)号：US20240076261A1
公开(公告)日：2024-03-07
申请号：US18270725
申请日：2022-03-24
申请人： ZHEJIANG NHU COMPANY LTD.
发明人： JINLONG LIU , SHUMIN LV , RUIJUN HU , XUEZHONG HE , MENGLIANG DU , XIAOCHUN WANG , ZIYU WANG , LANYING LIANG
IPC分类号： C07C51/43
CPC分类号： C07C51/43 , C07B2200/13
摘要： The present invention discloses a method for preparing an ibuprofen spherical crystal having high bulk density and a product thereof. The method includes: (1) heating ibuprofen until a molten liquid state is reached; and (2) pressurizing the molten liquid state of ibuprofen, dropping the molten liquid state of ibuprofen into a crystallizer filled with water through a liquid distributor for crystallization under stirring conditions until the molten liquid state of ibuprofen is completely dropped, lowering the rotation speed of stirring to allow crystal growing, and finally, subjecting a resulting crystal slurry to post-treatment to obtain the ibuprofen spherical crystal having high bulk density. The ibuprofen spherical crystal has a bulk density of 0.50-0.70 g/mL, a tap density of 0.63-0.89 g/mL, a median particle size of 300-1,000 μm and an angle of repose of 22-29°. The method of the present invention features that the process thereof is simple, and that no additives are used, such that the method is suitable for industrial production. The ibuprofen spherical crystal prepared has regular crystal habit, smooth crystal surface, good fluidity, high bulk density and high product purity. The quality of a product meets requirements of CP2020, EP9.8, USP41 and other pharmacopoeias.

2. 发明授权

US11632970B2 Vitamin and carotenoid powder and its preparation method and application 有权
公开(公告)号：US11632970B2
公开(公告)日：2023-04-25
申请号：US16067528
申请日：2016-12-08
申请人： ZHEJIANG NHU COMPANY LTD. , ZHEJIANG UNIVERSITY
发明人： Jiandong Li , Zhirong Chen , Hong Yin , Xiaoyong Zhu , Dan Qiu , Lifang Shi , Dongming Shi , Yong Qi
IPC分类号： A23K20/174 , A23K40/30 , A23P10/30 , A23L33/15 , A61K9/14 , A61K31/015
摘要： The present invention discloses a method for preparation of vitamin and carotenoid powder; the vitamin and carotenoid powder comprises vitamin, carotenoid microcapsule and physical gel protection film covered on the surface of the vitamin and carotenoid microcapsule; the physical gel protection film is made from super-molecular system; the super-molecular system comprises the following constituents of parts in weight: vegetable oil: 6-30 parts; gel: 0.5-3 parts and antioxidant: 0.5-3 parts. The hot super-molecular solution is sprayed on the surface of cold vitamin and carotenoid microcapsule during preparation to form a specific 3D network structure that is used to bind the liquefied vegetable oil to form a physical gel protection film; the physical gel protection film has improved product storage stability as well as the its stability for application in feedstuff, food and health care products.

3. 发明授权

US09567440B2 Fiber grade polyphenylene sulfide resin synthesis method 有权
标题翻译：纤维级聚苯硫醚树脂合成方法
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
IPC分类号： C08G75/16 , C08G75/00 , 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/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。

4. 发明申请

US20160374375A1 METHOD FOR PREPARING OIL-DISPERSIBLE CAROTENOID PREPARATION 审中-公开
标题翻译：用于制备油分散的卡培他滨制剂的方法
公开(公告)号：US20160374375A1
公开(公告)日：2016-12-29
申请号：US14902553
申请日：2014-06-03
申请人： ZHEJIANG NEW WEIPU ADDITIVE CO., LTD. , ZHEJIANG UNIVERSITY , ZHEJIANG NHU COMPANY LTD.
发明人： DAN QIU , LIFANG SHI , JIANDONG LI , ZHIRONG CHEN , JIACHAO ZHOU
IPC分类号： A23L5/44 , A23L33/105
CPC分类号： A23L5/44 , A23L33/105 , A23V2002/00
摘要： Disclosed in the present invention is a method for preparing an oil-dispersible carotenoid preparation, comprising (by weight parts): mixing 100 parts of carotenoid microcapsule, 100-400 parts of vegetable oil and 0.1-1 part of oil-soluble antioxidant; and grinding the mixture in a colloid mill in a nitro—gen atmosphere and at 10-30° C. to obtain a uniform oil-dispersible carotenoid preparation, wherein the preparation contains 2%-14% carotenoid with an average particle size of up to 0.1-1 μm, and 100 parts of carotenoid microcapsule contains 10.5-35.8 parts carotenoid, 0.1-1 part of water-soluble antioxidant, and the remainder is a water-soluble colloid. The advantages of the present invention lie in that the oil-dispersible form has a high stability as the surface of the carotenoid particles is still protected with a dense water-soluble colloid, and that an oil-dispersible carotenoid preparation containing carotenoid with a content of up to 2%-14% and an average particle size of only 0.1-1 μm can be prepared.
摘要翻译：本发明公开了一种制备油分散类胡萝卜素制剂的方法，其包含（重量份）：混合100份类胡萝卜素微胶囊，100-400份植物油和0.1-1份油溶性抗氧化剂; 并在硝基气氛中和10-30℃下在胶体磨中研磨混合物，得到均匀的油分散类胡萝卜素制剂，其中制备物含有2％-14％的类胡萝卜素，其平均粒度可达 0.1-1μm，100份类胡萝卜素微胶囊含有10.5-35.8份类胡萝卜素，0.1-1份水溶性抗氧化剂，其余为水溶性胶体。本发明的优点在于，油分散形式具有高的稳定性，因为类胡萝卜素颗粒的表面仍然被致密的水溶性胶体保护，并且含有含有类胡萝卜素的类胡萝卜素的油分散类胡萝卜素制剂高达2％-14％，平均粒径仅为0.1-1μm。

5. 发明申请

US20150284323A1 CLEAN METHOD FOR PREPARING D,L-METHIONINE 有权
标题翻译：用于制备D，L-甲硫氨酸的清洁方法
公开(公告)号：US20150284323A1
公开(公告)日：2015-10-08
申请号：US14425310
申请日：2013-01-06
申请人： ZHEJIANG NHU COMPANY LTD. , ZHEJIANG UNIVERSITY , SHANDONG NHU AMINO ACIDS CO., LTD.
发明人： Zhirong Chen , Cunchao Wang , Chuqiu Zhao , Sujuan Wang , Chengfeng Zhang , Tao Long , Xinhong Liu
IPC分类号： C07C319/20 , C07D207/38
CPC分类号： C07C319/20 , C07D207/38 , C07C323/58
摘要： The present invention discloses a clean method for preparing a D,L-methionine comprising the steps of: preparing a potassium cyanide solution using a crystallized mother solution containing potassium carbonate as an absorbing liquid to absorb hydrocyanic acid, then reacting the potassium cyanide solution with 3-methylthio propionaldehyde and an ammonium bicarbonate solution at 50-150° C. for 3-15 minutes so as to obtain a 5-(β-methylthioethyl)glycolyurea solution, then bring the 5-(β-methylthioethyl)glycolyurea solution to a temperature of 140-220° C. and subjecting to a saponification reaction for 2-5 minutes, after the completion of the saponification, reducing the temperature to 0-40° C., extracting with an organic solvent, neutralising the water phase with CO2 and crystallizing, then filtering, washing, and drying to obtain an acceptable D,L-methionine product; bring the crystallized D,L-methionine mother solution from filtration to a temperature to 110-160° C. to remove CO2, which are all then circulated and used as a hydrocyanic acid-absorbing liquid. The process route of the present invention is a route suitable for a continuous and clean production, substantially without producing waste water and waste gas.
摘要翻译：本发明公开了一种制备D，L-甲硫氨酸的清洁方法，包括以下步骤：使用含有碳酸钾的结晶的母液作为吸收液体吸收氰氰酸，然后使氰化钾溶液与3 - 甲硫基丙醛和碳酸氢铵溶液在50-150℃下反应3-15分钟，得到5-（叔丁基硫代乙基）糖醇脲溶液，然后将5 - （（R） - 甲硫基乙基）糖醇脲溶液温度为140-220℃，皂化反应2-5分钟，皂化完成后，将温度降至0-40℃，用有机溶剂萃取，中和水相用 CO 2并结晶，然后过滤，洗涤和干燥，得到可接受的D，L-甲硫氨酸产物; 将结晶的D，L-甲硫氨酸母液过滤至110-160℃，除去二氧化碳，然后循环使用，并用作氢氰酸吸收液。本发明的工艺路线是适合连续清洁生产的路线，基本上不产生废水和废气。

6. 外观设计

USD1013533S1 Bag packaging 有权
公开(公告)号：USD1013533S1
公开(公告)日：2024-02-06
申请号：US35515274
申请日：2022-09-13
申请人： ZHEJIANG NHU COMPANY LTD. , HEILONGJIANG NHU BIOTECHNOLOGY COMPANY LTD. , SHANGYU NHU BIO-CHEM CO., LTD. , SHANDONG NHU FINE CHEMICAL SCIENCE AND TECHNOLOGY COMPANY LTD. , XINCHANG NHU VITAMINS COMPANY LTD.
设计人： Liangang Shi , Xiujuan Lei
摘要： 1. Bag packaging
1.1 : Front;
1.2 : Back;
1.3 : Left;
1.4 : Right;
1.5 : Top;
1.6 : Bottom;
1.7 : Reference view (unfolded status);
The broken lines showing of portions of the bag packaging is included for the purpose of illustrating environmental structure and forms no part of the claimed design.

7. 发明申请

US20230063291A1 STABLE CAROTENOID MICROCAPSULE HAVING HIGH BIOAVAILABILITY AND PREPARATION METHOD THEREFOR 有权
公开(公告)号：US20230063291A1
公开(公告)日：2023-03-02
申请号：US17793937
申请日：2021-04-29
申请人： ZHEJIANG NHU COMPANY LTD. , ZHEJIANG UNIVERSITY , XINCHANG NHU VITAMINS COMPANY LTD.
发明人： Jiandong LI , Zhirong CHEN , Lifang SHI , Guodong HUANG , Lishuang PAN , Hong YIN , Dan QIU , Qilei ZHANG , Xiaoyong ZHU , Xiang LIU , Lidan QI
IPC分类号： A23K40/30 , A23K20/105 , A23K20/147 , A23K20/158 , A23K20/163
摘要： A stable carotenoid microcapsule having high bioavailability and a preparation method therefor. The method includes the following steps: a) mixing carotenoid crystals with an organic solvent, and dissolving the mixture to obtain a carotenoid solution; b) introducing the carotenoid solution and a grease into a dispersion system to fully disperse carotenoid into the grease, and vaporizing the organic solvent to obtain a carotenoid-containing dispersion liquid; c) mixing the carotenoid-containing dispersion liquid and a protective colloid aqueous solution, and emulsifying the mixture to obtain an emulsion; and d) performing spray granulation and drying to obtain a carotenoid microcapsule.

8. 发明申请

US20220080400A1 HYDROFORMYLATION CATALYST, PREPARATION METHOD THEREFOR AND USE THEREOF 有权
公开(公告)号：US20220080400A1
公开(公告)日：2022-03-17
申请号：US17258439
申请日：2019-11-06
申请人： ZHEJIANG NHU COMPANY LTD. , ZHEJIANG UNIVERSITY , SHANDONG NHU PHARMACEUTICAL CO., LTD. , SHANDONG NHU VITAMIN CO., LTD.
发明人： Yong WANG , Zhe WANG , Yutong GONG , Lei WU , Lili YU , Haoran LI , Zhirong CHEN , Xiao MA , Jianyong MAO
IPC分类号： B01J31/22 , B01J37/04
摘要： A hydroformylation catalyst, a preparation method thereof and a use thereof. The hydroformylation catalyst including an active component and a carrier carrying the active component, wherein the active component includes a transition metal as a center atom, and a polyhydroxy aromatic ring group bonded to the transition metal; and the transition metal and the polyhydroxy aromatic ring groups are bonded by at least one of metal-hydroxyl coordination bond and at least one of metal-oxygen covalent bond, and the active component has at least one of the metal-hydroxyl coordination bond and at least one of the metal-oxygen covalent bond.

9. 发明申请

US20210009514A1 PREPARATION METHOD FOR 4-PHENYLTHIO-BENZENETHIOL 有权
公开(公告)号：US20210009514A1
公开(公告)日：2021-01-14
申请号：US16955511
申请日：2018-07-12
申请人： ZHEJIANG NHU COMPANY LTD. , ZHEJIANG UNIVERSITY , ZHEJIANG NHU SPECIAL MATERIALS CO., LTD.
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： C07C319/06
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.

10. 发明申请

US20210002317A1 METHOD FOR SYNTHESIZING SUCROSE-6-ESTER 有权
公开(公告)号：US20210002317A1
公开(公告)日：2021-01-07
申请号：US16981986
申请日：2019-04-24
申请人： Zhejiang Nhu Company Ltd. , Shandong Nhu Fine Chemical Science and Technology Company Ltd.
发明人： Yougui ZHOU , Jiang CAI , Kaifeng MA , Yugang WANG , Xiaoqiao WEI , Yunhan YANG
IPC分类号： C07H1/06
摘要： A method for synthesizing sucrose-6-ester includes: (a) in the presence of a polar aprotic solvent, contacting an organic phosphine compound represented by formula I with sucrose and an organic tin compound; (b) removing water to obtain a reaction liquid containing a tin-sucrose adduct; and (c) contacting the reaction liquid containing the tin-sucrose adduct with an acid anhydride compound to prepare a sucrose-6-ester. In formula I, R1, R2, and R3 each are a linear or branched alkyl having 1 to 20 carbon atoms, a cycloalkyl having 3 to 10 carbon atoms, or an aryl having 6 to 10 carbon atoms; moreover, the R1, R2, and R3 are identical groups, partially identical groups, or different groups from each other. According to the method, the reaction conversion rate and selectivity are greatly improved; moreover, it is easy to realize industrial application.

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