Способы Получения Микрокристаллической Целлюлозы (Обзор)

Болтовский, Валерий Станиславович

doi:10.52065/2520-2669-2021-241-1-40-50

Cited by 4 publications

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“…В качестве материала для гидролиза использовали произведенную из хвойных пород древесины листовую сульфатную [1] беленую целлюлозу Братского целлюлозно-бумажного комбината. целлюлозу измельчали на шредере до размера частиц 3×30 мм.…”

Section: объекты и методы исследованияunclassified

Cellulose Hydrolysis Using Hydrogen Chloride Gas-Air Mixtures

Pimenov¹,

Mzokov²,

Sizov³

2022

Lesnoy Zhurnal (Forestry Journal)

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Abstract. Microcrystalline cellulose (MCC) is a common product used in pharmaceutical, food and other industries. MCC is obtained by liquid-phase hydrolysis of cotton or wood bleached pulp with diluted 0.5–10.0 % mineral acids at a temperature of 100–140 °C. This process requires significant consumption of acid, water, and heat energy. Production of MCC in general is very expensive, which determines its high cost and the need to find alternative methods of cellulose hydrolysis. It is proposed to hydrolyze cellulose with concentrated hydrochloric acid produced by absorption of hydrogen chloride. We studied the processes of hydrogen chloride adsorption by bleached wood pulp with 8–18 % humidity. It is shown that adsorption of hydrogen chloride is determined by pulp humidity and is 3–5 % of the dry pulp mass. The sorption of hydrogen chloride leads to the formation of hydrochloric acid with a concentration of 25–40 % in the raw material moisture, significant heating of the mass and rapid hydrolysis of the amorphous cellulose fraction. It has been found that the use of pure hydrogen chloride for saturation causes strong darkening and humification of pulp. We recommend the use of hydrogen chloride gas-air mixtures to saturate the pulp, which will significantly reduce the sorption temperature and eliminate the strong darkening of the pulp during hydrolysis. The adsorption of hydrogen chloride by cellulose proceeds at an extremely high rate and is accompanied by the formation of a clearly visible sorption front at a temperature of 45–60 °C. Hydrolysis occurs for 15–30 min at 40–60 °C until the amorphous cellulose fraction is completely decomposed. A very small amount of monosaccharides is formed (4 % of dry pulp). The yield of MCC is high, more than 95 %. These circumstances are probably related to the recrystallization of a part of the amorphous fragments of cellulose macromolecules, which is a characteristic of hydrolysis with concentrated acids. The product obtained by cellulose hydrolysis is identical to MCC according to the data of IR spectroscopy, X-ray diffraction and viscometry. The article shows the high efficiency of cellulose hydrolysis with hydrogen chloride gas-air mixtures compared to traditional methods of MCC production.

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Section: объекты и методы исследованияunclassified

Cellulose Hydrolysis Using Hydrogen Chloride Gas-Air Mixtures

Pimenov¹,

Mzokov²,

Sizov³

2022

Lesnoy Zhurnal (Forestry Journal)

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Preparation of microcrystalline cellulose from industrial hemp trusts

Александров,

Момзякова,

Дебердеев

et al. 2024

Известия СПбЛТА

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Получение микрокристаллической целлюлозы (МКЦ), как одного из широко востребованных продуктов переработки целлюлозы, из альтернативных источников целлюлозосодержащего сырья является актуальнейшей задачей на сегодняшний день. В качестве альтернативного источника микрокристаллической целлюлозы рассматривается техническая конопля, которая имеет ряд преимуществ по сравнению с другим растительным сырьем, таких как большой объём ежегодного воспроизведения биомассы; невысокие затраты на её возделывание; высокая урожайность по стеблю; содержание лигнина значительно ниже по сравнению с древесиной; упрощённая делигнификация. Техническая конопля перед началом варки размалывалась до размеров 10-20 мм. Из-за высокого содержания костры в размолотой технической конопле разработан многостадийный технологический режим получения микрокристаллической целлюлозы. Многостадийный технологический режим получения микрокристаллической целлюлозы состоит из предгидролиза (натронной варки), пероксидно-молибдатной делигнификации, кислотного гидролиза и отбелки. Натронная варка, по сравнению с сульфатной или сульфитной варкой, обусловлена экологичностью из-за отсутствия соединений серы. Пероксидно-молибдатная делигнификация выбрана из-за более полного удаления остаточного лигнина из растительного сырья. Гидролиз полученного полупродукта минеральными кислотами обусловлен тем, что это самый распространенный и доступный способ получения микрокристаллической целлюлозы. Отбелка необходима для придания окончательных свойств, так как полученная МКЦ представляет собой мелкодисперсные частицы кремового цвета. Применение раствора серной кислоты для кислотного гидролиза тресты технической конопли по предлагаемой технологической схеме получения МКЦ приводит к уменьшению степени полимеризации на 55-60 единиц по сравнению с применением раствора соляной кислоты при этой же технологической схеме получения МКЦ. Микрокристаллическая целлюлоза из тресты технической конопли, полученная с использованием более высоких температур при натронной варке, при одинаковых режимах на других стадиях характеризуется более низкой белизной, из чего следует, что более оптимальным технологическим режимом получения МКЦ из тресты технической конопли является применение низкотемпературной натронной варки при начальной стадии. The production of microcrystalline cellulose (MCC), as one of the widely popular products of cellulose processing, from alternative sources of cellulose-containing raw materials is a pressing task today. Industrial hemp is considered as an alternative source of microcrystalline cellulose, which has a number of advantages compared to other plant raw materials, such as a large volume of annual biomass reproduction; low costs for its cultivation; high yield per stem; lignin content is significantly lower compared to wood; simplified delignification. Before cooking, industrial hemp was ground to a size of 10-20 mm. Due to the high content of buds in ground industrial hemp, a multi-stage technological regime for the production of microcrystalline cellulose has been developed. The multi-stage technological regime for the production of microcrystalline cellulose consists of pre-hydrolysis (sodium cooking), peroxide-molybdate delignification, acid hydrolysis and bleaching. Soda cooking, compared to sulfate or sulfite cooking, is environmentally friendly due to the absence of sulfur compounds. Peroxide-molybdate delignification was chosen due to the more complete removal of residual lignin from plant materials. Hydrolysis of the resulting intermediate product with mineral acids is due to the fact that this is the most common and accessible method for producing microcrystalline cellulose. Bleaching is necessary to impart final properties, since the resulting MCC is fine, cream-colored particles. The use of a sulfuric acid solution for the acid hydrolysis of industrial hemp trusts according to the proposed technological scheme for the production of MCC leads to a decrease in the degree of polymerization by 55-60 units than the use of a hydrochloric acid solution with the same technological scheme for the production of MCC. Microcrystalline cellulose from industrial hemp trust, obtained using higher temperatures during soda cooking, under the same conditions at other stages is characterized by lower whiteness, which means that the more optimal technological mode for obtaining MCC from industrial hemp trust is the use of low-temperature soda cooking at the initial stages.

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The role of prehydrolysis refining in obtaining microcrystalline cellulose: case of biodamage wood from Picea abies, Larix sibirica and Populus tremula species

Yurtaeva,

Alashkevich,

Kaplyov

et al. 2024

Forestry Engineering Journal

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The ability of grinding equipment in the production of microcrystalline cellulose (MCC) to separate plant polymers into fibers, grind and develop certain properties in them can be used if it is impossible to minimize the concentration of acid. To obtain microcrystalline cellulose, samples (N = 6) of dry wood Picea abies (L.) H.KARST., Larix sibirica LEDEB., Populus tremula L. species were used. The samples were cooked in a laboratory autoclave, prehydrolysis grinding was carried out in a centrifugal grinding machine at a fibrous mass concentration of 6% and varying the degree of grinding from 15 to 85 degrees of Schopper Riegler (°SR). Chemical treatment of cellulose samples with different degrees of grinding was carried out with varying hydrolysis temperatures from 80 to 100 °C, hydrochloric acid concentrations from 54.75 to 91.25 g/l, and hydrolytic degradation time from 60 to 120 minutes. The dependences of the degree of polymerization (R2 = 0.93) and the degree of crystallinity (R2 = 0.99) on these factors are approximated by second-order regression equations and visualized as three-dimensional response surfaces. The optimal values of the hydrolysis variables are: hydrochloric acid concentration – 54.75 g/l, hydrolytic degradation time – 60 min, hydrolysis temperature – 80 °C, grinding degree – 85 °C. The degree of grinding of the fibrous mass has the greatest influence on the quantitative values of the degree of polymerization and the degree of crystallinity, the lowest is the temperature of hydrolysis. With an increase in the degree of grinding, a significant 2.7-fold decrease in the degree of polymerization occurs in MCC samples from P. abies and P. tremula wood. An increase in the degree of crystallinity (17%) and bulk density (20%) is observed to a greater extent in MCC samples from P. abies and L. sibirica wood. The use of prehydrolysis milling of cellulose in the process of obtaining MCC reduces the cost of chemical treatment by 1.7 times.

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Способы Получения Микрокристаллической Целлюлозы (Обзор)

Cited by 4 publications

References 0 publications

Cellulose Hydrolysis Using Hydrogen Chloride Gas-Air Mixtures

Cellulose Hydrolysis Using Hydrogen Chloride Gas-Air Mixtures

Preparation of microcrystalline cellulose from industrial hemp trusts

The role of prehydrolysis refining in obtaining microcrystalline cellulose: case of biodamage wood from Picea abies, Larix sibirica and Populus tremula species

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