The method of microcrystalline cellulose

 

(57) Abstract:

The method concerns of microcrystalline cellulose from straw herbaceous plants of the family of grasses that can be used in chemical, cosmetics, pharmaceutical, food industries and medicine. Of air-dried plant materials produce pulp of Kurshner by well-known methods or subjected to delignification in alkaline solution. Then the pulp is subjected to acid hydrolysis. The method allows to obtain microcrystalline cellulose, containing no admixture of aromatic character in the form of lignin. 3 table.

The invention relates to the manufacture of cellulose derivatives, namely to obtain microcrystalline cellulose (MCC), which can be used in chemical, cosmetics, pharmaceutical, food industries and medicine.

A method of obtaining ICC (RF patent 2147057), chosen for the prototype, a pre-hydrolysis subjected to mechanical grinding to a powder air-dried oat straw in sulfuric and proximodorsal acids. MCC has the following indicators: degree of polymerization (SP) 87-210 the C lignin Komarova, that, depending on the purpose for use, MCC, is not always desirable indicator.

The present invention is to obtain ICC straw herbaceous plants of the family cereal that does not contain impurities of aromatic character in the form of lignin.

This is a technical result.

Straw of cereals refers to the waste of agricultural production. In Russia annually collects more than 200 million tons of straw. From the straw of cereals can produce two types of fibrous semi-finished products: coarse straw mass (yield about 70% of raw material) for use in the production of cardboard and paper for corrugation and pulp (yield from raw materials 35-45%), which is unbleached and white-washed the form can be used for the production of quality paper and cardboard. For industrial processing, it is preferable to use the straw of wheat and rye, which are more durable pulp, paper and cardboard, than other types of straw (C. E. Moskaleva and other Diagnostic signs of non-timber plant and chemical fibers. M : the Forest industry here, 1981. - S. 46). There is information about the use of straw as the Russian is their use as a coarse low-value food (the degree of digestibility of biomass straw does not exceed 15-20%) and bedding material. However, according to our data, the component composition of the biomass straw herbaceous plants of the family cereal similar plant tissue of coniferous and deciduous wood - the main components are cellulose and lignin (table 1). High cellulose content, comparable with the content of cellulose in wood (40-50%), shows the principal possibility of using straw herbaceous plants of the family of cereals as a raw material source for MCC production. The elemental composition of drugs dioxane lignin isolated from straw are presented in table 2. Functional composition of dioxane lignin preparations are presented in table 3.

It should be noted that the straw of cereals contains almost no resins, i.e. has a clean environment, is an affordable, renewable raw materials.

Xylem herbaceous plants much easier may be subject to physical and chemical processing than wood of coniferous and deciduous species. This can be explained by the following reasons. Wood of coniferous species has a relatively simple structure, so as to 90-95% consists of tracheids are long, thin cells with a flat or spindle-shaped closed ends of the mechanical tissue consists of fibers libriform and fiber tracheids. The main anatomical elements herbaceous plants are fiber, then the vascular, parenchymal, and epithelial cells. The xylem density is determined by the number and diameter of vessels, number parenchyma cells, as well as the wall thickness of the fibers libriform or tracheids. Due to the anatomical structure of the xylem, the greater the density of its forming cells and less significativamente, herbaceous plants are easily amenable to physical and chemical influences.

The main components of plant tissue are the polysaccharides (cellulose and lignin. The rest are mecellose polysaccharides, ash components and extractives. Pulp of wood and other plant materials is a linear homopolysaccharide built from elementary units-D-glucopyranose. As in the cell wall lignin is not simply deposited between polysaccharides and is in close Association and forms a so-called lignin-carbohydrate complex, then to explain the mechanisms of chemical transformation of plant tissue are essential differences in the chemical structure of the lignin of wood and herbaceous plants. Lignin softwood tree units vallromanas, siegerrebe and n-coumaric. Softwood and hardwood lignins are characterized by a high degree of kondensirovannoi. For lignin herbaceous plants characterized by a high content of n-Kumarovich units and the large number of easy-hydrolyzed in acidic and alkaline environment of ester groups.

Thus, features of the anatomical and chemical structure of herbaceous plants explain them easier physico-chemical processing compared to wood. Note the similarity of the chemical composition of the straw of various herbaceous plants of the family graminaceae, and show the same approach to the processing of these raw sources.

The essential features of the invention: method of microcrystalline cellulose from straw herbaceous plants of the family of cereals containing cellulose 40-50%, lignin 18-23%, mecellose polysaccharides, ash components and extractives - the rest, by acid hydrolysis of air-dried plant materials, while before hydrolysis pre-allocate the pulp of Kurshner by well-known methods or subjected feedstock delignification saloon what about the dry straw of herbaceous plants in the family cereal is subjected to mechanical grinding in a vibrating mill to a powder. Then, to obtain the ICC used two approaches: 1) extraction from milled feedstock cellulose as individual substances with subsequent hydrolysis; 2) delignification milled feedstock and subsequent hydrolysis. The first option of receiving MCC associated with the separation of cellulose from plant tissue by the method of Kurshner (A. C. Obolenskaya and other Laboratory work on chemistry of wood and cellulose. M. : Ecology, 1991) and subsequent hydrolysis of cellulose to limit the degree of polymerization proximodorsal acid (PMS) and the classical way. PMS is formed during the reaction with sulfuric acid (H2SO4and hydrogen peroxide H2ABOUT2. This method of obtaining MCC has worked well from an environmental point of view, and, in addition, PMS causes oxidation of residual lignin and has a cellulose destructible action (V. A. Demin, L. S. Kocheva, A. P. Karmanov. Srtucture and properties of microcristalline cellulose received by different methods //Fifth European Workshop on Lignocellulosics and Pulp. Proceedings. Portugal, 1998. - P. 157-159. ). The classical way of obtaining MCC is considered to be the hydrolysis of 2.5 N. hydrochloric acid HCl at 105oC for 2 hours.

The second option for the ICC is that the original straw after grinding on vibration is x raw water is used to obtain the ICC by treating PMS and classic way.

The use of these two approaches to processing the original plant materials allows to obtain not contain lignin Komarova MCC, because in the first case, the hydrolysis is subjected to the preparation of the pulp, and in the second case, the product from which previously removed lignin. Lignin Komarov was determined by standard method (A. C. Obolenskaya and other Laboratory work on chemistry of wood and cellulose. M. : Ecology, 1991).

As the characteristics of the samples obtained MCC used the degree of polymerization (SP). JV samples was determined by the viscosity of their solutions in catocene [Cd(en)3] (OH)3the method error is 1-2% (HP Bolotnikov and other Method of determining the viscosity and degree of polymerization of cellulose // Russian journal of applied chemistry, 1966. - So 39. Vol. 1. - S. 176-180). As an example, annual herbaceous plants of the family cereal examined oats, as an example of perennial herbaceous plants of the family cereal considered meadow fescue.

Example 1. Pulp of Kurshner get from the ground to a powder, straw oat in accordance with the following method. A portion of the air-dry straw weight of about 1 g is placed in a conical flask with a capacity of 250 cm3and the nitric acid (density 1.4 g/cm3) and four volumes of 95% ethanol. To the flask and attach the reflux condenser and boil the straw with the mixture on a water bath for 1 hour This treatment is carried out three or four times. After the last treatment, the pulp is sucked dried to constant weight glass Frit, applying suction, washed with 10 cm3fresh nitrogen-alcohol mixture, and then hot water. The filter pulp dried in a drying Cabinet at a temperature of (1032)oC to constant weight. Thus obtained air-dry cellulose of Kurshner transferred into a flask and pour a solution containing PMS. After mixing the components with stirring suspension of straw oats concentration equivalent to 10% of sulfuric acid and 1% hydrogen peroxide (equivalent to 3% of PMS). The water ratio of 1: 50. Flask with reflux condenser heated to the boiling point of the mixture and incubated for 120 min, then removed from the heater, cooled to room temperature and vortex separating the hydrolysate. The resulting ICC washed with water until neutral wash water, and dried. Indicators: lignin Komarova: no; SP: original oat straw - catocene not dissolving pulp of Kurshner of straw oat - 766; M is ovat suspension and handle, as in example 1. Indicators: lignin Komarova: no; SP: original straw of meadow fescue in catocene not dissolving pulp of Kurshner of straw meadow fescue - 1184; MKC-326.

Example 3. A portion of air-dried pulp of Kurshner obtained from milled to a powder, straw, oats, transferred into a flask and pour a solution of 2.5 N. HCl. The water ratio of 1: 50. Further treatment is carried out as in example 1. Indicators: lignin Komarova: no; SP 422.

Example 4. As a source of raw materials use air-dry straw of meadow fescue. Preparing a suspension and are processed as in example 3. Indicators: lignin Komarova: no; SP 636.

Example 5. A portion of the air-dry straw of oats, ground to a powder, transferred into a flask and pour a solution of 2 N. NaOH. The water ratio 1: 5. Flask with reflux condenser heated to the boiling point of the mixture and incubated for 120 min, then removed from the heater, cooled to room temperature and vortex separating the hydrolysate. The resulting product is washed with water until neutral wash water, dried to air-dry state. Further treatment is carried out as in example 1. Indicators: lignin Komarova: who are the product of alkaline delignification, as in example 5. Further treatment is carried out as in example 3. Indicators: lignin Komarova: no; SP 384.

Evidence suggests that the straw herbaceous plants of the family cereal serves as a raw material source for the production of MCC. Ecological purity of raw materials and final products can be recommended MCC straw herbaceous plants of the family of grasses for use not only in the chemical industry, but also in medicine, pharmacy, perfumery and food production.

The method of microcrystalline cellulose from straw herbaceous plants of the family of cereals containing cellulose 40-50%, lignin 18-23%, mecellose polysaccharides, ash components and extractives - the rest, by acid hydrolysis of air-dried plant material, characterized in that before hydrolysis pre-allocate the pulp of Kurshner by well-known methods or subjected feedstock delignification alkaline solution Paon.

 

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