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Title:
PURIFICATION METHOD AND SYSTEM FOR N-METHYLMORPHOLINE-N-OXIDE, AND OBTAINED N-METHYLMORPHOLINE-N-OXIDE
Document Type and Number:
WIPO Patent Application WO/2023/274038
Kind Code:
A1
Abstract:
Disclosed are a purification method and system for N-methylmorpholine-N-oxide (NMMO), and obtained NMMO. The present invention is used for recovering and purifying NMMO in a lyocell fiber coagulation bath. The method comprises: subjecting a lyocell fiber coagulation bath to flocculation, microfiltration, ultrafiltration, and nanofiltration membrane treatment; and removing macromolecular impurities such as suspended solids, heavy metal ions, heavy metal complexes and polysaccharide substances, and then performing cooling crystallization at -20°C to 78°C to obtain an NMMO hydrate crystal. The NMMO hydrate crystal obtained by means of the method of the present invention does not contain PG and PG oxidation products, cellulose decomposition products such as various sugars, sugar ketones, sugar acids, furans, furfurals and phenols, and NMMO decomposition products in the coagulation bath, and does not contain various metal ions and anions. Water is added to the crystal to prepare an NMMO aqueous solution having a concentration of 19.8%, and the conductivity is about 14.8 μs/cm. An NMMO crystal having higher purity can be obtained by adding water to the NMMO crystal subjected to primary crystallization and crystalizing again, 19.8% of NMMO aqueous solution is prepared by adding water, and the conductivity is reduced to 12.4 μs/cm or less.

Inventors:
LU WANLI (CN)
MA JIE (CN)
Application Number:
PCT/CN2022/100880
Publication Date:
January 05, 2023
Filing Date:
June 23, 2022
Export Citation:
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Assignee:
B FCTL CO LTD (CN)
XIAN SPIDE TECH ENVIRONMENTAL PROTECTION TECH CO LTD (CN)
International Classes:
C07D295/24; D01F11/00; D01F13/00
Domestic Patent References:
WO2020234330A12020-11-26
Foreign References:
CN114539186A2022-05-27
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CN112939281A2021-06-11
CN112876429A2021-06-01
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CN101088993A2007-12-19
CN101942712A2011-01-12
US9441318B22016-09-13
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US8633120B22014-01-21
US7938993B22011-05-10
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US10306919B22019-06-04
Other References:
YUE WENTAO: "Study on the Recycle Process and Mechanism of N-methylmorpholine-N-oxide(NMMO) as a Solvent for the Lyocell Fibers Production", CHINESE DOCTORAL DISSERTATIONS FULL-TEXT DATABASE, 1 December 2006 (2006-12-01), CN , pages 1 - 184, XP093019634, ISSN: 1674-022X
HAN ZENGQIANG ,WU ZHIYUN ,WANG SHAOPENG , CAI JIAN: "Recovery Process of Solvent NMMO for Producing Lyocell Fiber", SHANDONG TEXTILE SCIENCE & TECHNOLOGY, vol. 29, no. 6, 15 June 2007 (2007-06-15), pages 7 - 9, XP093019629, ISSN: 1009-3028
HU LINA: "Study on Recovery and Evaporation Process of New Organic Solvent NMMO", CHINA STRATEGIC EMERGING INDUSTRY, no. 18, 22 August 2019 (2019-08-22), pages 149, XP009542402, ISSN: 2095-6657
ROSENUA T.POTTHAST A.MILACHER W.ADORJAN I.HOFINGER AKOSMA P.: "Discoloration of cellulose solutions in N-methylmorpholine-N-oxide (Lyocell", CELLULOSE, vol. 12, 2005, pages 197 - 208, XP019234550, DOI: 10.1007/s10570-004-0210-3
ZHENG YU-CHENG: "Cause analysis of color change in lyocell fiber production", SYNTHETIC FIBER, vol. 47, no. 8, 2018, pages 17 - 23
Attorney, Agent or Firm:
LECOME INTELLECTUAL PROPERTY AGENT LTD. (CN)
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