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公开(公告)号：US20150284323A1
公开(公告)日：2015-10-08
申请号：US14425310
申请日：2013-01-06
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。
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公开(公告)号：US09206120B2
公开(公告)日：2015-12-08
申请号：US14425310
申请日：2013-01-06
发明人： Zhirong Chen , Cunchao Wang , Chuqiu Zhao , Sujuan Wang , Chengfeng Zhang , Tao Long , Xinhong Liu
IPC分类号： C07C323/00 , C07C321/00 , C07C45/00 , 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, neutralizing 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。
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公开(公告)号：US11632970B2
公开(公告)日：2023-04-25
申请号：US16067528
申请日：2016-12-08
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.
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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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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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6.发明申请公开(公告)号：US20210147350A1
公开(公告)日：2021-05-20
申请号：US17263362
申请日：2019-08-27
发明人： Zhirong Chen , Hong Yin , Baishan Hu , Zhengjiang Wang , Zhixuan Wang , Cong Chen , Guisheng Qiu , Qichuan Li , Qingai Shi
IPC分类号： C07C319/20 , C07C319/28 , C07C323/52 , B01J19/24
摘要： Provided by the present disclosure are a method and a device for preparing 2-hydroxy-4-methylthiobutyric acid and intermediates thereof; the intermediates for preparing 2-hydroxy-4-methylthiobutyric acid comprise 3-methylthiopropionaldehyde and 2-hydroxy-4-methylthiobutyronitrile. The method for preparing 2-hydroxy-4-methylthiobutyric acid provided by the present disclosure comprises: step (1), a step of reacting acrolein with methyl mercaptan to prepare 3-methylthiopropionaldehyde; step (2), a step of reacting 3-methylthiopropionaldehyde with hydrocyanic acid to prepare 2-hydroxy-4-methylthiobutyronitrile; and step (3), a step of hydrating 2-hydroxy-4-methylthiobutyronitrile by using sulfuric acid and then hydrolyzing to prepare 2-hydroxy-4-methylthiobutyric acid; wherein in steps (1), (2) and (3), the reaction status of the materials is detected online, and the proportions of the materials are controlled according to the detection results such that reactions are performed completely
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公开(公告)号：US10212957B2
公开(公告)日：2019-02-26
申请号：US14902553
申请日：2014-06-03
发明人： Dan Qiu , Lifang Shi , Jiandong Li , Zhirong Chen , Jiachao Zhou
IPC分类号： A23L5/44 , A23L33/105
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.
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公开(公告)号：US10065901B2
公开(公告)日：2018-09-04
申请号：US15565133
申请日：2016-11-29
发明人： Yougui Zhou , Ming Yu , Jintao Yuan , Lei Zhao , Xiandong Zhu , Guangxiong Yu , Weiwei Su , Weikang Shao , Xingxing Shi , Yin Zhang , Ming Feng , Zhirong Chen , Haoran Li , Yuhong Zhang
IPC分类号： C07C45/62 , C07B53/00 , B01J31/02 , B01J23/46 , C07D333/22 , C07C47/225 , C07C47/232 , C07C49/21 , C07C49/217 , C07D307/46 , C07C47/21
摘要： The present invention discloses a method for preparing optically active carbonyl compound, comprising the following steps: under the catalysis of chiral amine salt and transition metal catalysts, with hydrogen and catalytic amount of dihydropyridine compound as hydrogen source, use α, β-unsaturated aldehydes or α, β-unsaturated troponoid compounds to conduct asymmetric catalytic reaction to obtain the optically active carbonyl compound. This method comes in moderate reaction condition, simple operation, and catalytic amount of dihydropyridine compounds usage, the target product is easy to be separated and purified from the reaction system, and the metal catalyst can be recycled, it is economical.
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9.发明授权公开(公告)号：US10668460B2
公开(公告)日：2020-06-02
申请号：US16669524
申请日：2019-10-31
申请人： ZHEJIANG NHU COMPANY LTD. , ZHEJIANG UNIVERSITY , SHANDONG NHU PHARMACEUTICAL CO., LTD. , SHANDONG NHU VITAMIN CO., LTD.
发明人： Yong Wang , Lili Yu , Xiao Ma , Jianyong Mao , Zhe Wang , Shanjun Mao , Jingsi Tang , Haoran Li , Zhirong Chen
IPC分类号： B01J37/02 , B01J37/04 , B01J35/10 , C07D495/04 , C07C5/05 , B01J37/16 , B01J23/42 , B01J23/44 , B01J23/46 , B01J37/08 , B01J21/18
摘要： A composite catalyst includes a carrier and noble metal particles supported by the carrier, wherein the carrier is a nitrogen-doped porous carbon composite material having a plurality of passages. The nitrogen-doped porous carbon composite material can include a nitrogen-doped porous carbon material and a plurality of metal oxide particles. The plurality of metal oxide particles can be uniformly distributed in the nitrogen-doped porous carbon material. The plurality of metal oxide particles can be partially exposed through the plurality of passages. The noble metal particles can be tightly combined with the exposed metal oxide particles to achieve recombination. And the noble metal particles can be at least one of Pd metal particles, Pt metal particles, Ru metal particles, Rh metal particles, Ir metal particles, Au metal particles, or a combination thereof.
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10.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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