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1. 发明公开

EP4361132A1 PURIFICATION METHOD AND SYSTEM FOR N-METHYLMORPHOLINE-N-OXIDE, AND OBTAINED N-METHYLMORPHOLINE-N-OXIDE 审中-公开
公开(公告)号：EP4361132A1
公开(公告)日：2024-05-01
申请号：EP22830362.4
申请日：2022-06-23
申请人： B-FCTL Co., Ltd.
发明人： LU, Wanli , MA, Jie
IPC分类号： C07D295/24 , D01F11/00 , D01F13/00
CPC分类号： Y02P70/62
摘要： The invention discloses a purification method and system of N-methylmorpholine N-oxide (NMMO), and a N-methylmorpholine N-oxide obtained thereof. The invention is used for recovering and purifying NMMO in a lyocell fiber coagulation bath. The method comprises: performing flocculation, microfiltration, ultrafiltration and nanofiltration membrane separation process to the lyocell fiber coagulation bath to remove macromolecular impurities such as suspending substance, heavy metal ions, heavy metal complexes, polysaccharides, etc., and then performing cooling crystallization between -20°C and 78°C to obtain NMMO hydrate crystals. The NMMO hydrate crystals obtained by the method provided in the invention do not contain PG, PG oxidation products, cellulose breakdown products such as various carbohydrates, sugar ketones, sugar acid, furans, furfurals, phenols, and NMMO decomposition products, which are present in the coagulation bath. The NMMO hydrate crystals do not contain various metal ions and anions as well. The NMMO hydrate crystals are added with water to prepare a NMMO aqueous solution with a concentration of 19.8%, and the electrical conductivity is about 14.8µs/cm. The crystalline NMMO obtained by a first crystallization is added with water to perform crystallization again, and a crystalline NMMO with higher purity can be obtained. The crystalline NMMO with higher purity is added with water to prepare a NMMO aqueous solution with a concentration of 19.8% and the electrical conductivity is reduced to less than 12.4µs/cm.

2. 发明公开

EP4335842A1 PURIFICATION METHOD, SYSTEM AND DETECTION METHOD FOR N-METHYLMORPHOLINE N-OXIDE AND OBTAINED N-METHYLMORPHOLINE-N-OXIDE 审中-公开
公开(公告)号：EP4335842A1
公开(公告)日：2024-03-13
申请号：EP22803748.7
申请日：2022-04-24
申请人： B-FCTL Co., Ltd.
发明人： LU, Wanli , MA, Jie
IPC分类号： C07D295/24 , B01D1/22
摘要： Disclosed are a purification method, system and detection method for N-methylmorpholine N-oxide (NMMO) and an obtained NMMO. The NMMO is derived from a crude product of NMMO prepared by reacting N-methylmorpholine with hydrogen peroxide. The mass concentration of NMMO in the crude NMMO product is 50-60%. The purification method comprises: cooling a crude NMMO product to -20°C-78°C for crystallization so as to obtain a crystal of NMMO. The NMMO purification method of the present invention has low costs. The obtained NMMO product has high purity and almost no "three wastes" are generated. Different from current NMMO purification process, the purification method of the present invention does not require an ion exchange resin; therefore, environmental problems such as large amounts of high-salt and high-COD wastewater and waste ion exchange resin brought about by the regeneration of an ion exchange resin are completely solved.

3. 发明公开

EP4357337A1 METHOD AND SYSTEM FOR PURIFYING NMMO AND OBTAINED NMMO HYDRATE CRYSTAL 审中-公开
公开(公告)号：EP4357337A1
公开(公告)日：2024-04-24
申请号：EP22830365.7
申请日：2022-06-23
申请人： B-FCTL Co., Ltd.
发明人： LU, Wanli , MA, Jie
IPC分类号： C07D295/24 , D01F13/02 , C02F9/00
CPC分类号： Y02P70/62
摘要： Disclosed in the present invention are a purification method and system of NMMO and a NMMO hydrate crystal obtained thereof. The purification method is suitable for purifying NMMO in a coagulating bath of a cellulose product, and by means of the method, almost all impurities including carbohydrate impurities can be removed from the NMMO solution of the coagulating bath of the cellulose product and a high-purity NMMO hydrate crystal is obtained. The purification method comprises the following steps: performing a cooling crystallization to the coagulating bath of the cellulose product between -20°C and 78°C to obtain NMMO hydrate crystals. According to the method for purifying and recovering NMMO in the coagulating bath of the cellulose product in the invention, ion-exchange resins are not needed, and acid and alkali are not needed for resin regeneration. High-salt wastewater is not generated, and almost no discharge of waste gas, waste water, and solid waste. Environmental protection problems caused by a large amount of high-salt and high-COD waste water generated by ion-exchange resin regeneration and spent ion-exchange resins are solved. The preparation process for the cellulose product truly becomes a low-cost and green production process, and the method can be applied to a wider field of cellulose product production.

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