The method of microcrystalline cellulose

 

(57) Abstract:

The method relates to the manufacture of cellulose derivatives and relates to a method of microcrystalline cellulose (MCC), which can be used as filler in pharmaceutical and food industries, sorbent and filter material in the technique, the raw material for producing low-viscosity cellulose derivatives. The technical result is achieved by the fact that the processing of the original pulp whiteness of not more than 65% is carried out in two stages with intermediate extraction with alkali solution. The first stage involves the simultaneous hydrolysis and bleaching of raw materials. The second subsequent dabelko of the material obtained by the chlorine dioxide in the presence of sodium hydrogen carbonate solution. The present invention allows to obtain cells from the pulp whiteness of not more than 65%. table 1.

The invention relates to the manufacture of cellulose derivatives and relates to a method of microcrystalline cellulose, which can be used as filler in pharmaceutical and food industries, sorbent and filter material in the technique, the raw material for nisavaski is C) by processing the original pulp whiteness of 65% and above in one step, combining hydrolysis and bleaching, a solution of sulfuric and proximodorsal acid with a concentration of 2.5-10% 0,48-3%, respectively, at atmospheric pressure and the boiling point of the mixture for 0.5 to 3.0 h (RF patent 2119986). The resulting product being dried and, if necessary, grind.

However, this method can only be used for MCC production of pulp with a high initial whiteness.

The present invention is to develop a method of producing microcrystalline cellulose from unbleached pulp.

The present invention allows to obtain cells from the pulp whiteness of not more than 65%.

The technical result is achieved by the fact that the processing of the original pulp whiteness of not more than 65% is carried out in two stages with intermediate extraction with alkali solution, the first step involves the simultaneous hydrolysis and bleaching of raw materials, and the second subsequent dabelko of the material obtained by the chlorine dioxide in the presence of sodium hydrogen carbonate solution.

The essential features of the invention: method of microcrystalline cellulose, including simultaneous hydrolysis and bleaching of the original pulp whiteness of not more than 65% in RA is AI and a temperature of 100-105oC for 30-180 min processing of semi-finished product with alkali solution at elevated temperature and subsequent dabelko of the material obtained by the chlorine dioxide with a flow rate of 1.5 to 2.5% by weight of the abs. dry material when the temperature of 20-40oC for 30-90 min, in the presence of a solution of sodium bicarbonate (NaHCO3) a concentration of 0.5-1.0 mol/cm3.

The method is as follows.

The first step involves the simultaneous hydrolysis and bleaching the original unbleached pulp with a solution of sulfuric and proximodorsal acid concentration of 2.5-10% 0,48-3%, respectively. The treatment is carried out at atmospheric pressure and the boiling temperature of the mixture within 30-180 minutes Then the semi-finished product is washed with water until neutral and treated with 1% NaOH solution at 70oC and the mass concentration of 5-10% within 60 minutes and then the microcrystalline cellulose is washed with water until neutral.

The second step involves dabelko of the material obtained by the chlorine dioxide with a flow rate of 1.5 to 2.5% by weight of the abs. the dry material at 20-40oC for 30-90 min in the presence of a solution of sodium bicarbonate (NaHCO3), with an initial concentration of 0.5-1.0 mol/cm3.

Example. 200 cm3and pour the sulfuric acid solution containing proximodorsal acid to a total volume of 100 cm3. After mixing the components with stirring suspension of cellulose concentration equivalent to 10% of sulfuric acid and 1% hydrogen peroxide (equivalent to 3% proximodorsal acid). The flask is heated to boiling temperature and incubated for 90 min, then removed from the heater, cooled to 60-80oC. the Obtained cellulose material is washed with warm water until neutral (by decantation), pour 50 cm31% NaOH solution and carry out the alkaline extraction at 70oC within 60 minutes After extraction, the resulting intermediate product is transferred to a Buchner funnel and washed with warm water until neutral. The obtained semi-product is a powder material with a degree of polymerization of 350 and white 41%. To increase white cake mix (MCC) is subjected to dobelle as follows.

A portion of MCC of mass 2 g (abs. dry. material) is transferred into the flask at 100 cm3pour 55,18-63,10 cm3solution of NaHCO3with an initial concentration of 0.5-1.0 mol/DM3and under stirring suspension add 6,90-14,82 cm3solution of chlorine dioxide concina porous filter obtained microcrystalline cellulose is washed with water until neutral and dried at a temperature of 60oC.

The table below shows examples 1-5, made by the above method.

Example 6 instead of sodium bicarbonate used 57,65 cm3distilled water, the whiteness of the obtained material was 57.6 per cent. The use of sodium hydrogen carbonate solution allows to increase the whitening ability of chlorine dioxide in the temperature range 20-40oC minor influence on the degree of polymerization of the cellulose, and also allows you to use the effect of swelling of lignocellulosic material in a basic environment that provides the best desorption products of oxidation of residual lignin.

The method of microcrystalline cellulose, including simultaneous hydrolysis and bleaching source of cellulose in the solution of sulfuric and proximodorsal acid at a concentration of 2.5 - 10% 0,48 - 3.0% respectively at atmospheric pressure and temperatures of 100 - 105oC for 30 to 180 min, characterized in that the feedstock used unbleached pulp, which after hydrolysis and bleaching is subjected to extraction with alkali solution and zabelivajut solution of chlorine dioxide with a flow rate of 1.5 to 2.5% by weight of the abs. the dry material at a temperature of 20 - 40oC for 30 - 90 min

 

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3 cl, 34 ex, 4 tbl

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