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RU2013138168A - METHOD FOR REGENERATING THE COMPLEX SALT OF LITHIUM CHLORIDE - DIMETHYLACETAMIDE IN THE PRODUCTION OF HIGH-STRENGTH ARAMID THREADS - Google Patents

METHOD FOR REGENERATING THE COMPLEX SALT OF LITHIUM CHLORIDE - DIMETHYLACETAMIDE IN THE PRODUCTION OF HIGH-STRENGTH ARAMID THREADS Download PDF

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Publication number
RU2013138168A
RU2013138168A RU2013138168/04A RU2013138168A RU2013138168A RU 2013138168 A RU2013138168 A RU 2013138168A RU 2013138168/04 A RU2013138168/04 A RU 2013138168/04A RU 2013138168 A RU2013138168 A RU 2013138168A RU 2013138168 A RU2013138168 A RU 2013138168A
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Russia
Prior art keywords
lithium chloride
dimethylacetamide
rectification
complex salt
crystals
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RU2013138168/04A
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Russian (ru)
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RU2542367C1 (en
Inventor
Владимир Юрьевич Лакунин
Владимир Викторович Ведехин
Галина Борисовна Склярова
Александр Семенович Шрайфель
Сергей Владимирович Комиссаров
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Открытое акционерное общество "Каменскволокно"
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Priority to RU2013138168/04A priority Critical patent/RU2542367C1/en
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Publication of RU2542367C1 publication Critical patent/RU2542367C1/en
Publication of RU2013138168A publication Critical patent/RU2013138168A/en

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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

Способ регенерации комплексной соли хлорид лития - диметилацетамид в производстве высокопрочных арамидных нитей, включающий нейтрализацию исходных растворов, ректификацию раствора пластификационной ванны в двух колоннах, вакуумную выпарку смеси кубового остатка второй колонны и осадительной ванны, ректификацию кубового остатка вакуум-выпарного аппарата, вакуумную ректификацию отгонного продукта вакуум-выпарного аппарата и третьей колонны с получением растворителя, кристаллизацию концентрированного раствора хлорида лития в диметилацетамиде, выделение кристаллов из раствора, сепарирование кристаллов на центрифугах и растворение кристаллов в растворителе с получением целевого продукта, отличающийся тем, что, с целью повышения качества конечного продукта, многокомпонентные исходные смеси, содержащие от 0 до 60% диметилацетамида (ДМАА), от 0 до 70% изобутилового спирта (ИБС), а также хлорид лития (LiCl), хлорид водорода, воду и примеси - остальное до 100%, вначале разделяют на содержащие хлорид лития и не содержащие его, затем разделяют смеси, не содержащие хлорид лития, на содержащие ДМАА и не содержащие его, жидкий поток, состоящий из ИБС и воды, выводят из системы, поток концентрированного хлорида лития последовательно направляют на гетероазеотропную ректификацию, кристаллизацию и центрифугирование, где отделяют комплексную соль хлорид лития - диметилацетамид или в твердой фазе и получают чистую комплескную соль.A method for the regeneration of a complex salt of lithium chloride - dimethylacetamide in the production of high-strength aramid yarns, including the neutralization of initial solutions, rectification of the plasticization bath solution in two columns, vacuum evaporation of the mixture of the bottom residue of the second column and the precipitation bath, rectification of the bottom residue of the vacuum evaporator, vacuum rectification of the stripping product a vacuum evaporator and a third column to obtain a solvent, crystallization of a concentrated solution of lithium chloride in dimethylacetamide, separation of crystals from solution, separation of crystals in centrifuges and dissolution of crystals in a solvent to obtain the target product, characterized in that, in order to improve the quality of the final product, multicomponent initial mixtures containing from 0 to 60% dimethylacetamide (DMAA), from 0 to 70% isobutyl alcohol (IBS), as well as lithium chloride (LiCl), hydrogen chloride, water and impurities - the rest up to 100%, are first divided into containing chl lithium orid and not containing it, then the mixtures that do not contain lithium chloride are separated into those containing DMAA and not containing it, the liquid flow consisting of IBS and water is removed from the system, the concentrated lithium chloride flow is sequentially sent to heteroazeotropic rectification, crystallization and centrifugation , where the complex salt of lithium chloride - dimethylacetamide is separated or in the solid phase and a pure complex salt is obtained.

Claims (1)

Способ регенерации комплексной соли хлорид лития - диметилацетамид в производстве высокопрочных арамидных нитей, включающий нейтрализацию исходных растворов, ректификацию раствора пластификационной ванны в двух колоннах, вакуумную выпарку смеси кубового остатка второй колонны и осадительной ванны, ректификацию кубового остатка вакуум-выпарного аппарата, вакуумную ректификацию отгонного продукта вакуум-выпарного аппарата и третьей колонны с получением растворителя, кристаллизацию концентрированного раствора хлорида лития в диметилацетамиде, выделение кристаллов из раствора, сепарирование кристаллов на центрифугах и растворение кристаллов в растворителе с получением целевого продукта, отличающийся тем, что, с целью повышения качества конечного продукта, многокомпонентные исходные смеси, содержащие от 0 до 60% диметилацетамида (ДМАА), от 0 до 70% изобутилового спирта (ИБС), а также хлорид лития (LiCl), хлорид водорода, воду и примеси - остальное до 100%, вначале разделяют на содержащие хлорид лития и не содержащие его, затем разделяют смеси, не содержащие хлорид лития, на содержащие ДМАА и не содержащие его, жидкий поток, состоящий из ИБС и воды, выводят из системы, поток концентрированного хлорида лития последовательно направляют на гетероазеотропную ректификацию, кристаллизацию и центрифугирование, где отделяют комплексную соль хлорид лития - диметилацетамид или в твердой фазе и получают чистую комплескную соль. The method of regeneration of the complex salt of lithium chloride - dimethylacetamide in the production of high-strength aramid yarns, including the neutralization of the initial solutions, rectification of a solution of a plasticization bath in two columns, vacuum evaporation of a mixture of bottoms of the second column and a precipitation bath, rectification of bottoms of a vacuum evaporation apparatus, vacuum distillation of a distant product vacuum evaporation apparatus and a third column to obtain a solvent, crystallization of a concentrated solution of lithium chloride in dimet of acetamide, isolating crystals from a solution, separating crystals in centrifuges and dissolving crystals in a solvent to obtain the target product, characterized in that, in order to improve the quality of the final product, multicomponent starting mixtures containing from 0 to 60% dimethylacetamide (DMAA), from 0 up to 70% of isobutyl alcohol (IHD), as well as lithium chloride (LiCl), hydrogen chloride, water and impurities - the rest is up to 100%, first they are divided into lithium chloride containing and not containing it, then mixtures not containing lithium chloride are divided into soda rusting DMAA and not containing it, the liquid stream consisting of IHD and water is removed from the system, the concentrated lithium chloride stream is sequentially directed to heterozeotropic distillation, crystallization and centrifugation, where the complex salt of lithium chloride - dimethylacetamide or in the solid phase is separated and a pure, complex phase is obtained salt.
RU2013138168/04A 2013-08-15 2013-08-15 Method of regenerating complex lithium chloride-dimethylacetamide salt in production of high-strength aramid fibres RU2542367C1 (en)

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RU2606118C1 (en) * 2015-12-22 2017-01-10 Акционерное общество "Каменскволокно" Method of removing water from process circuit in chemical production
RU2613438C1 (en) * 2015-12-22 2017-03-16 Акционерное общество "Каменскволокно" Method for lithium chloride regeneration in chemical industry

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SU531900A1 (en) * 1974-12-24 1976-10-15 Предприятие П/Я А-3193 Method of solvent regeneration in the production of chemical fibers
SU1707093A1 (en) * 1988-12-05 1992-01-23 Ленинградский научно-исследовательский институт химических волокон и композиционных материалов с экспериментальным заводом Method for dimethylacetamide regeneration
SE500113C2 (en) * 1992-07-09 1994-04-18 Kamyr Ab Method of bleaching pulp for disposal of released metals

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