WO2016072885A2 - Procédé de production de cellulose - Google Patents

Procédé de production de cellulose Download PDF

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Publication number
WO2016072885A2
WO2016072885A2 PCT/RU2015/000869 RU2015000869W WO2016072885A2 WO 2016072885 A2 WO2016072885 A2 WO 2016072885A2 RU 2015000869 W RU2015000869 W RU 2015000869W WO 2016072885 A2 WO2016072885 A2 WO 2016072885A2
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WIPO (PCT)
Prior art keywords
cellulose
solution
hydrolysis
vacuum
water
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PCT/RU2015/000869
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English (en)
Russian (ru)
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WO2016072885A3 (fr
Inventor
Яков Кузьмич АБРАМОВ
Владимир Михайлович ВЕСЕЛОВ
Виктор Михайлович ЗАЛЕВСКИЙ
Виталий Григорьевич ТАМУРКА
Вениамин Сергеевич ВОЛОДИН
Владимир Дмитриевич ЕВДОКИМОВ
Борис Иванович МИРОНОВ
Ольга Борисовна ВАТУЕВА
Николай Александрович ГУКАСОВ
Людмила Михайловна МАРШАННИКОВА
Татьяна Михайловна МОРДВИНОВА
Наталья Александровна САЛОМАТИНА
Дмитрий Константинович САРЫЧЕВ
Александр Иванович ПИЛЬГУН
Валентина Ивановна БИРЮКОВА
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Общество с ограниченной ответственностью "Твин Технолоджи Компани"
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Application filed by Общество с ограниченной ответственностью "Твин Технолоджи Компани" filed Critical Общество с ограниченной ответственностью "Твин Технолоджи Компани"
Priority to KR1020177015098A priority Critical patent/KR20180083251A/ko
Priority to US15/522,990 priority patent/US20170314196A1/en
Priority to JP2017543700A priority patent/JP2017535690A/ja
Priority to EP15857573.8A priority patent/EP3216917A4/fr
Priority to PCT/RU2015/000869 priority patent/WO2016072885A2/fr
Priority to CN201580067873.7A priority patent/CN107075799B/zh
Publication of WO2016072885A2 publication Critical patent/WO2016072885A2/fr
Publication of WO2016072885A3 publication Critical patent/WO2016072885A3/fr

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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C1/00Pretreatment of the finely-divided materials before digesting
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C1/00Pretreatment of the finely-divided materials before digesting
    • D21C1/02Pretreatment of the finely-divided materials before digesting with water or steam
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C5/00Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/001Modification of pulp properties
    • D21C9/007Modification of pulp properties by mechanical or physical means

Definitions

  • the invention relates to the chemical industry, namely to the production of cellulose from all types of plant cellulose-containing material, chemically and structurally homogeneous, bleached and unbleached, for paper, textile, medical, nitrocellulose (hereinafter - SC) industry, paint and varnish, powder technology, which can be used for further processing in various industries: SC for gunpowders, varnishes, enamels, textile, paper, medical, pharmaceutical, food, etc.
  • SC nitrocellulose
  • SC nitrocellulose
  • the most common method for producing various pulps is currently the sulfate method. In the world pulp and paper industry, this method produces up to 90-95% of all types of pulp.
  • the use of high (up to 1.5 MPa) pressure for large reactor boilers (up to 400 m 3 or more) with high temperatures complicates the process and its hardware design.
  • the lignin separation process at 145 ° C takes place in 12 hours, at 160-180 ° C in 4-6 hours, and only at 200 ° C for 30 minutes.
  • the introduction of additional components into the reagent causes the emission of gases that worsen the ecology of the air basin, complicates the regeneration of solutions and washing of cellulose with the use of a large amount of water and complicating the organization of their circulation.
  • Sulfite belongs to the group of acidic methods for producing celluloses, inorganic (HNO 3 , ⁇ 1), organic (acetic, monochloroacetic and other) acids, as well as ethylene glycol, phenol, butyl and other alcohols, as well as a calcium base, are used as reagents containing Ca (HS0 3 ) 2 with an excess of S0 2 , supporting the pH of the solution at a level of 1.2-1.5. Gaseous S0 2 having strongly acidic properties, penetrates into wood chips faster than the solution, therefore, the heating of the solution is slower, otherwise incomplete delignification of wood occurs.
  • the temperature of the solution in the manufacture of paper pulp lies in the range 125-135 ° C, and pulp for the chemical industry 145 ° C, the duration of the process is up to 12 hours.
  • the application of this method leads to a deterioration in the sorption properties of the obtained cellulose, its structural and chemical heterogeneity, a reduced degree of crystallinity, and a decreased stability of properties during storage.
  • the cellulose obtained especially when obtained by the sulfate method, cellulose is molecularly heterogeneous.
  • the output characteristics of celluloses have increased scatter in viscosity, ⁇ -cellulose content, etc.
  • a known method of producing fibrous cellulose from cellulose-containing raw materials using an aqueous solution of nitric acid as a delignifying agent (RF patent N ° 2353626, IPC ⁇ 08 ⁇ 1 / 04; D01F2 / 00, dated October 25, 2007).
  • the treatment solution contains surfactants, an ammonium inorganic salt or potassium or sodium nitrate.
  • the oxidative treatment is carried out in an alkaline peroxide solution containing sodium carboxymethyl cellulose and a nonionic water-soluble cellulose ether.
  • a known method of producing cellulose by cooking wood chips from hardwood in sulphite cooking solution and subsequent washing (RF patent N ° 2010069, IPC D21C3 / 06 from 08.07.1992).
  • This method is used to obtain cellulose from wood chips from hardwood or from low-resinous species of wood: spruce, fir.
  • the disadvantage of this method is the use of reagents that degrade the ecological environment of air and water pools. The resulting cellulose does not have sufficient chemical and structural homogeneity.
  • a known method of producing cellulose from non-wood plant materials with a content of native cellulose of not more than 50% and an aqueous solution of caustic soda (RF patent No. 2448118, IPC ⁇ 08 ⁇ 11/12, 1/00, 1/02, dated 09.11.2010).
  • the raw materials are washed with hot water at a temperature of 40-75 ° C at atmospheric pressure for 0.5-4.0 hours, delignification is carried out at a temperature of 90-95 ° C with an aqueous solution of nitric acid at a concentration of 2-8% for 4-20 hours.
  • the cellulose is subjected to additional processing with a solution of caustic soda 1-4% at a temperature of 60-95 ° C for 1-6 hours, which increases the duration of the process. This stage reduces the degree of polymerization and leads to a deterioration in the quality of cellulose, in particular, to a decrease in the strength index.
  • miscanthus or fruit shells of cereal crops, or straw of cereal crops are used to obtain cellulose, however, the resulting cellulose does not have sufficient chemical and structural homogeneity.
  • the output characteristics of the cellulose obtained by the considered methods have increased scatter in viscosity, alpha-cellulose content and other indicators.
  • the aim of the invention is to provide a method for producing cellulose of high quality, with chemical and structural homogeneity from various cellulose-containing raw materials, while simplifying and cheapening the process.
  • the goal is achieved by processing cellulose-containing raw materials, including the impregnation and hydrolysis of the raw materials in a hydrolysis solution, filtering the resulting cellulose, subsequent washing with water, filtering and drying, in which, according to the invention, the impregnation and hydrolysis of raw materials in a hydrolysis solution medium, filtering the resulting cellulose, subsequent washing with water, filtering and drying are carried out with the simultaneous use of cycles including heating the material to a temperature of 115 ° C or less, high-speed pulse exposure to vacuum with pressure ranging up to 5 mmHg Art., in less than 10 seconds, followed by exposure to vacuum, for example, until a constant temperature is reached and the vacuum is released.
  • a solution of nitric or sulfuric acids, or a mixture of nitric and sulfuric acids with a concentration of solutions of not more than 15.0% can be used with a ratio of cellulose-containing raw materials to the hydrolysis solution (module) of not more than 1: 15.
  • an alkaline solution with a solution concentration of less than 30 grams / liter can be used with a ratio of cellulose-containing raw materials to hydrolysis solution (module) of not more than 1: 15.
  • the impurities dissolved in it such as lignin, hemicellulose, pectins, pentosans, etc., are separated from the spent hydrolysis solution from the cellulose fiber, followed by their planting and production of fertilizers based on them in a simpler way than in the production of sulfate cellulose.
  • the wash water After washing and filtering the cellulose, the wash water is regenerated with the organization of water circulation for subsequent use.
  • the pulp is bleached using cycles that include heating the material to a temperature of 115 ° C or less, high-speed pulse exposure to vacuum with a pressure change in the range up to 5 mm Hg. Art., in a time less than 30 seconds, followed by exposure to vacuum, for example, until a constant temperature is reached and the vacuum is released.
  • some types of cellulose after washing with water and filtering, squeeze the vacuum on a mesh or fabric filter by pulsed suction of water with a pull of air coolant through a layer of fibrous cellulose and a mesh until the desired moisture content is reached, followed by loosening of the compacted cellulose.
  • the technical result is achieved due to the fact that all stages of the process are accompanied by cycles, including heating the material to a temperature of 115 ° C or less, high-speed pulsed exposure to vacuum with a change in pressure in the range up to 5 mm RT. Art. in less than 10 seconds, followed by exposure to vacuum and vacuum relief. High-speed pulsed exposure to vacuum is carried out using a receiver and pipelines equipped with high-speed valves. This leads to the intensification of mass transfer with the acceleration of the process of hydrolysis of the material and other advantages.
  • Impregnation in a hydrolysis solution Impregnation in a hydrolysis solution.
  • the impregnation of cellulose-containing raw materials with simultaneous exposure to cycles, including high-speed pulsed vacuum is carried out in a hydrolysis solution.
  • the impact of a high-speed pulsed vacuum during the impregnation improves the wettability, degasses the treated mixture, facilitating the penetration of the hydrolysis solution into the fibers of the raw material, reduces the duration of the impregnation, accelerating the dissolution of lignin, freeing the cellulosic part of the raw material from other impurities.
  • the raw material is subjected to hydrolysis.
  • capillaries of heated cellulosic material during pulsed evacuation remove moisture vapor, air and gases dissolved in moisture, rupture of part of the membrane walls, and when the vacuum is released, not only capillaries are impregnated with the hydrolysis solution, but also the structure of the cellulosic material.
  • the destruction of cellulosic material by high-speed pulsed vacuum ensures the rapid penetration of the hydrolysis solution into the cellulosic material with the dissolution of lignin, hemicellulose and other impurities from destructible cellulose with the formation of chemically and structurally homogeneous cellulose from all known types of cellulose-containing materials with bast fibers.
  • the hydrolysis of various cellulose-containing raw materials can be carried out in an alkaline or acidic environment. Hydrolysis in an alkaline medium proceeds more slowly than in an acidic medium, in which the wettability of the material and the diffusion of the solution into the material are improved. With high-speed pulsed exposure to vacuum, the wettability of materials improves, therefore, the hydrolysis of cellulose-containing materials can be carried out both in alkaline and in acidic environments. Given the versatility of the developed process, preference is given to hydrolysis with acidic solutions, both from the standpoint of simplifying the composition of the hydrolysis solution, and from the standpoint of intensifying the hydrolysis process, lowering the process temperature, as well as obtaining high-quality low-viscosity cellulose. See examples 1 and 2 below.
  • the cellulose-containing raw material is impregnated and hydrolyzed in a hydrolysis solution medium, where a solution of nitric, sulfuric acids, or a mixture of nitric and sulfuric acids with a concentration of solutions of not more than 15.0% is used as a hydrolysis solution with a ratio of cellulose-containing raw materials to hydrolysis solution of not more than 1:15.
  • a solution of nitric, sulfuric acids, or a mixture of nitric and sulfuric acids with a concentration of solutions of not more than 15.0% is used as a hydrolysis solution with a ratio of cellulose-containing raw materials to hydrolysis solution of not more than 1:15.
  • the combined effect of acids favorably affects hydrolysis, improving the uniformity of cellulose from wood and annual plants.
  • Lignin is subsequently converted to organic fertilizer, increasing crop yields.
  • the impregnation and hydrolysis of cellulose-containing raw materials is also carried out in an environment where an alkaline solution with a concentration of less than 30 grams / liter is used as the hydrolysis solution with a ratio of cellulose-containing raw materials to the hydrolysis solution of not more than 1:15.
  • the impregnation and hydrolysis of cellulose-containing raw materials can be carried out with a solution of waste acids from the production of cellulose nitrates, which are a mixture of nitric, sulfuric acids and water.
  • waste acids from the production of cellulose nitrates, which are a mixture of nitric, sulfuric acids and water.
  • spent acid depending on the composition of the initial working acid mixture, the content of nitric acid reaches 20-28%, sulfuric acid up to 60% and water up to 20%, which allows you to create the necessary hydrolysis solution.
  • the use of spent acids minimizes the cost of the hydrolysis solution.
  • the resulting cellulose is filtered to separate from the spent hydrolysis solution while using the above cycles, including high-speed pulsed vacuum.
  • a large pressure drop across the filter material increases the productivity of the process of separating the hydrolysis solution with the impurities dissolved in it from the cellulose fiber.
  • the dissolved impurities in the spent hydrolysis solution are subsequently precipitated together with lignin.
  • washing is carried out with the simultaneous use of the above cycles, including high-speed pulsed exposure to vacuum, with water heated to 50-70 ° C, then with a temperature of 15-25 ° C in order to remove residual hydrolysis solution adsorbed on the surface of lignin fiber, etc.
  • Impurities and low molecular weight hydrolysis products are intensifying mass transfer processes, especially when boiling water with pulsed evacuation throughout the volume of the solution. Cellulose is washed to a neutral environment.
  • Bleaching is carried out mainly with hydrogen peroxide using cycles that include heating the material to a temperature of 115 ° C or less, high-speed pulsed exposure to vacuum with a pressure change in the range up to 5 mm RT. Art., in a time less than 30 seconds, followed by exposure to vacuum and vacuum discharge.
  • the cellulose After washing the cellulose with water, it is filtered using high-speed pulsed vacuum, similar to filtration after hydrolysis. The separated wash water is sent for regeneration for reuse.
  • Cellulose is dried using the above cycles, including high-speed pulsed exposure to vacuum, which makes it possible to obtain cellulose with less than 10% moisture, due to better desorption of surface moisture and positively directed gradients of pressure, temperature and humidity of cellulose. Deeper and more uniform drying occurs at a cellulose temperature of less than 100 ° C.
  • the cellulose washed and filtered from rinsing water is squeezed on a mesh or fabric filter using a high-speed pulsed vacuum suction of water with an air heat carrier through a layer of fibrous cellulose and a mesh to not more than 10% humidity. Subsequently, the densified pulp is loosened.
  • the use of high-speed pulse effects of vacuum at all stages of the process of producing cellulose gives the following advantages of the method: reducing the duration of the process of hydrolysis of cellulose by an order of magnitude, the possibility of creating a closed cycle of water circulation, as well as hydrolyzing and bleaching solutions, lowering the temperature of the processes to obtain the required chemical and structural uniformity material, with the achievement of greater conservation of the crystalline part of the cellulose with faster destruction of the amorphous part of the cellulose oses, the possibility of obtaining the desired grade of pulp from any cellulose-containing raw material.
  • the exclusion of additional chemicals from the hydrolysis solution improves the ecology of not only the air basin, but also the water basin by reducing the volume of washing water with the organization of their regeneration.
  • the regeneration of used hydrolysis, bleaching solutions and wash water is greatly simplified. Simplified pulp separation technology lignin and other impurities and the process of obtaining high-quality homogeneous cellulose.
  • Cotton lint is impregnated with high-speed pulsed vacuum
  • cotton hydrolysis is carried out using cycles in all processes, including high-speed pulsed exposure to vacuum, a 2.5% melange solution at 60 ° C and a 1: 7.5 module for 50 minutes. Impregnation of cotton is carried out with a change in pressure by high-speed pulse effects of vacuum up to 10 mm RT. Art.
  • the hydrolysis solution is filtered from cotton. Hydrolysis the solution is regenerated and put back into circulation. The fiber is washed with water at a temperature of 60 ° C and then with water at a temperature of 20 ° C with a module of 1: 7.5 to a neutral environment. Wash water after two-stage (10 and 5 ⁇ m) filtration and pH adjustment are reused.
  • the washed fiber is bleached with a mixture of aqueous solutions of alkali with a concentration of 3 grams / liter and hydrogen peroxide with a concentration of 8 grams / liter at a temperature of 70 ° C for 30 minutes with high-speed pulsed vacuum. Then, the bleaching solution is separated from cellulose, the solution is filtered twice, regenerated and returned to the technological cycle. This is followed by washing the cellulose with water under high-speed pulsed exposure to vacuum. Water at high-speed pulsed effects of vacuum is also filtered, adjusted by pH and reused.
  • Bleached, washed cellulose is squeezed on a continuous, conveyor screen or fabric filter with pressure rolls and then dried by drawing in an air coolant with a temperature of 100-115 ° C through a layer of cellulose and a mesh to 5-10% moisture by high-speed pulsed vacuum, followed by loosening of the compacted pulp.
  • the resulting medical cotton wool is soft and meets the requirements of TU in terms of parameters and has increased wettability. Humidity - 8%, whiteness - 80%.
  • hemp stalks like flax
  • cycles including high-speed pulsed vacuum to preliminary hydrolysis at a temperature of 95 ° ⁇ with a 3.0% melange solution at a module of 1: 7.5.
  • the impregnated fiber is subjected to hydrolysis, where it is brought to the required viscosity standards.
  • the washed fiber is bleached with an alkaline peroxide solution, the solution is separated, the fiber is washed and subjected to extraction and drying on a continuous conveyor screen apparatus with pressure rollers and suction of an air coolant with a temperature of 98 ° C and high-speed pulse effects of vacuum through the fiber layer and the net. Fiber drying is carried out up to 10% humidity, loosens roll machine and then packaged in bales. Achieved the degree of polymerization of flax fiber - 10000, the degree of polymerization of hemp - 8000.
  • the fiber is pulverized by hydrolysis in a solution with a temperature of 95-98 ° C with a 1: 5 module to 50-100 ⁇ m, the viscosity of cellulose decreases to 5-10 cPs.
  • the hydrolysis solution is also separated from the fiber.
  • the hydrolysis solution is filtered off, lignin and impurities are precipitated, after regeneration, the solution is returned to the technological cycle.
  • the cellulose used to make SCs for nitro-lacquers and enamels is bleached in an aqueous alkaline peroxide solution.
  • the solution is filtered, regenerated and returned to the technological cycle. Bleached pulp is washed, squeezed and dried.
  • Cellulose fibers are washed to a neutral medium, squeezed in a centrifuge or screw press under high-speed pulsed vacuum.
  • cellulose is pressed through a heated cone press tool with dies and squeezed to a moisture content of 15-20%.
  • the cellulose is vacuum-packed in a dense layer into a vacuum-pulse continuous dryer and dried at a temperature of 110 ° C for 30 minutes to a moisture content of not more than 10% and is packed.
  • cellulose is impregnated with high-speed pulsed vacuum in a particular solution and dissolves into fibers.
  • Wood chips with a thickness of 5 mm, a width of 10 mm and a length of 14 mm are subjected to impregnation at high-speed pulsed exposure to vacuum with a solution of sodium hydroxide and sodium sulfide at a concentration of 10 grams / liter at 95 ° C, a module of 1: 7.5 with a pressure change of up to 10 mm RT. Art. within 30 minutes.
  • the grinding of chips with an alkaline hydrolysis solution is carried out on a laboratory grinder to a particle size of 50-100 microns.
  • the hydrolysis of crushed wood chips in an alkaline medium is brought to 10-15 cPs for 1 hour.
  • the hydrolysis solution with dissolved lignin and other impurities is filtered through woven metal mesh with mesh sizes of 50, 10 and 5 microns.
  • Cellulose fiber after separation of hydrolysis the solution is washed with water at a temperature of 60 ° C and water at a temperature of 20 ° C to a neutral environment.
  • Washed cellulose, for better purification from impurities and finely dispersed finely divided amorphous cellulose is subjected to additional acid hydrolysis with a 3.0% solution of mixture at 90-95 ° C using high-speed pulsed exposure to vacuum for 60 minutes, reducing the viscosity of the pulp to 9-10 cps.
  • the hydrolysis solution is filtered.
  • the fiber is washed, squeezed in a laboratory centrifuge and dried to 8-10% moisture.
  • it is bleached with a mixture of alkali solution (NaOH) of concentration - 4-5 grams / liter and hydrogen peroxide - 10 grams / liter at 70-75 ° C for 15 minutes, followed by filtration of the bleaching solution, washing, pressing and drying at a temperature of 115 ° C to a moisture content of 10% cellulose.
  • NaOH alkali solution
  • alpha-cellulose reaches 96-97%, wettability - 150-160 g, humidity - 8-10%, viscosity - 6-9 cps, degree of polymerization - 260.
  • wood chips are subjected to impregnation with a solution of melange with a concentration of 2.5% at 95-98 ° C and a module of 1: 7.5 with the simultaneous use at this and subsequent stages of cycles involving high-speed pulsed exposure to vacuum with a pressure change of up to 10 mm Hg. Art. within 30 minutes. Chips are crushed in a hydrolysis solution to a particle size of 50-100 microns. The required viscosity of the pulp is achieved in the grinding process.
  • the required viscosity indices are achieved by high-speed pulsed vacuum influences.
  • the hydrolysis solution is filtered by high-speed pulsed vacuum through a stainless steel mesh with cells of 10 and 5 ⁇ m, and is regenerated by chemical composition with the organization of the circulation of the solution in a closed cycle.
  • the separated cellulose is washed twice with water at a temperature of 50-60 ° C and then with water at a temperature of 20 ° C.
  • Wash water by high-speed pulsed vacuum is filtered through a stainless steel mesh with mesh sizes of 10 and then 5 microns.
  • the waters are regenerated by launch vehicle with the organization of a closed water circulation.
  • the washed cellulose is bleached with a mixture of aqueous solutions of alkali NaOH with a concentration of 3-6 grams / liter and hydrogen peroxide with a concentration of at least 8 grams / liter at a temperature of 50-75 ° C for 30 minutes, followed by stepwise filtration and regeneration of the solution, washing water, s the organization of the turnover of the solution and water.
  • Cellulose bleaching is necessary only for transparent nitro lacquers and enamels.
  • the resulting cellulose is squeezed in a centrifuge using a suction of squeezed water by high-speed pulsed vacuum.
  • On the screw press cellulose through heated a cone-shaped press with a cowl is pressed through dies with a moisture content of 15-20%.
  • Cellulose drying is carried out in a continuous vacuum dryer using high-speed pulse effects of vacuum at a temperature of 110 ° C to a moisture content of 10%.
  • wood chips are impregnated with nitric acid at a concentration of 8.0%, without the use of Ca (HS0 3 ) 2 solution, without S0 2 penetrating the wood chips faster than the solution, and also without the use of alcohols (butyl and others), as well as without phenol, ethylene glycol and organic acids (acetic, monochloroacetic and other acids).
  • the hydrolysis solution is separated in a centrifuge with the planting of dissolved impurities.
  • the fiber is washed to a neutral medium, squeezed in a centrifuge and dried to 10% humidity.
  • the cellulose is bleached with a NaOH solution mixed with hydrogen peroxide to separate, regenerate the solution, rinse and dry the cellulose to 10% moisture.
  • Alpha cellulose content reaches up to 97%, wettability up to 150g, degree of polymerization - 240, humidity - 10%.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Paper (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

l'invention se rapporte au domaine de l'industrie chimique et concerne notamment un procédé de production de cellulose à partir de différentes matières premières contenant de la cellulose pour l'industrie du papier, textile et autres branches de l'industrie, y compris les technologies concernant les poudres. Le procédé comprend les étapes d'imprégnation et d'hydrolyse de la matière première dans une solution d'hydrolyse, de filtration de la cellulose, de rinçage à l'eau, de filtrage et de séchage, lesquelles s'accompagnent de cycles consistant à chauffer le matériau à une température de 115°C ou moins, et à appliquer une action rapide par impulsion sous vide avec une modification de pression dans une plage allant jusqu'à 5 mm de Hg en colonne pendant au moins 10 secondes, puis à maintenir le vide avant de l'annuler. Ce procédé est universel. La solution de pyrolyse peut consister en une d'acides nitrique ou sulfurique, en leur mélange ou en une solution alcaline. On peut également utiliser une solution d'acides usés issus de la production de nitrocellulose, ce qui est moins onéreux. Le résultat technique de ce procédé consiste en la production de cellulose d'une qualité voulue à partir d'une quelconque matière première contenant de la cellulose, en une réduction d'un ordre de la durée du processus d'hydrolyse de cellulose, en une diminution de la température des processus tout en obtenant une cellulose d'une uniformité chimique et structurelle voulue, et ceci sans utiliser d'équipement particulier. Le procédé donne la préférence à une hydrolyse par des solutions acides, ce qui simplifie la composition de la solution d'hydrolyse.
PCT/RU2015/000869 2014-11-05 2015-12-11 Procédé de production de cellulose WO2016072885A2 (fr)

Priority Applications (6)

Application Number Priority Date Filing Date Title
KR1020177015098A KR20180083251A (ko) 2015-12-11 2015-12-11 셀룰로스의 제조 방법
US15/522,990 US20170314196A1 (en) 2014-11-05 2015-12-11 A cellulose production method
JP2017543700A JP2017535690A (ja) 2015-12-11 2015-12-11 セルロース生産方法
EP15857573.8A EP3216917A4 (fr) 2015-12-11 2015-12-11 Procédé de production de cellulose
PCT/RU2015/000869 WO2016072885A2 (fr) 2014-11-05 2015-12-11 Procédé de production de cellulose
CN201580067873.7A CN107075799B (zh) 2014-11-05 2015-12-11 纤维素的制备方法

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RU2014144224 2014-11-05
PCT/RU2015/000869 WO2016072885A2 (fr) 2014-11-05 2015-12-11 Procédé de production de cellulose

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WO2016072885A2 true WO2016072885A2 (fr) 2016-05-12
WO2016072885A3 WO2016072885A3 (fr) 2016-06-23

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JP (1) JP2017535690A (fr)
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RU2779000C1 (ru) * 2021-07-06 2022-09-09 Александр Геннадьевич Смыслов Способ получения целлюлозы

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US10287366B2 (en) 2017-02-15 2019-05-14 Cp Kelco Aps Methods of producing activated pectin-containing biomass compositions
CN116497465B (zh) * 2023-05-17 2024-05-07 中应国强安全科技(北京)有限公司 一种苋属植物纤维及其制备方法和烟花

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JP2017535690A (ja) 2017-11-30
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