The method of obtaining this highly oxidised cellulose and this highly oxidised cellulose "bookselling"

 

(57) Abstract:

The invention relates to the field of chemical technology, in particular to methods for this highly oxidised cellulose, which can be used to retrieve highly toxic substances, such as strontium, antimony, mercury, lead, rare earth elements. Describes how to obtain this highly oxidised cellulose, including two-stage oxidation of cellulose consistently iodine-containing compound and nitrogen oxides, washing with purified water, ethyl alcohol and drying, in the first stage, the process is carried out in 5-11% solution of periodate sodium with a pH of 2.5 to 4.5 at 40-60C, followed by washing with purified water and sulfuric acid solution, in the second stage oxidation spend 15-30% solution of oxides of nitrogen in carbon tetrachloride for 30-40 minutes at a temperature of 2-10C and a pressure of 0.2 to 2.0 MPa, then the obtained intermediate product is separated from the solution and incubated for 3-5 h at a temperature of 25-40C and a pressure of 3.2 to 5.0 MPa. The technical result - obtaining this highly oxidised cellulose, used as non-toxic radioprotective, hemostatic, antimicrobial and wound healing agents. 1 C.p. f-crystals, 4 PL.

what th cellulose, which can be used to retrieve highly toxic substances, such as strontium, antimony, mercury, lead, rare earth elements.

A method of obtaining this highly oxidised cellulose sequential oxidation of cellulose by periodate sodium and nitrogen oxides. By carboxycellulose with the content of carboxyl groups of up to 50% (Ed. St. USSR N 451710, CL MKI6C 08 B 15/04 1974)

The disadvantage of this method is the length of the process and contamination of the final product nitrogen compounds.

Closest to the proposed invention is a method in which the oxidation is carried out in two stages: in the first stage oxidation of cellulose carried out with a mixture of periodate sodium and periodate potassium in a weight ratio of periodate sodium: periodate potassium equal to (10-15): 1, medium 10-12% aqueous solution of sulfuric acid at a pH of 2.6-4.4 and a temperature of 50-55oC, in the second stage oxidation is carried oxides of nitrogen at a pressure of from 1.5 to 3.0 MPa, followed by washing with distilled water under vibration with a frequency of 5-10 Hz, followed by drying in vacuum at a temperature of 80-90oC. (Patent RF N 2095369 class. MKI6C 08 B 15/04 B. I. N 31, 1997).

The disadvantages of the prototype OI the result is to reduce processing time, reducing it costs, improving the quality of the final product, by improving the uniformity of oxidation.

To achieve a technical result in the production method of this highly oxidised cellulose, including two-stage oxidation of cellulose consistently iodine-containing compound and nitrogen oxides, washing with purified water, ethyl alcohol and drying, in the first stage, the process is carried out in 5-11% solution of periodate sodium with a pH of 2.5 to 4.5 at 40-60oC, followed by washing with purified water and sulfuric acid solution, in the second stage oxidation spend 15-30% solution of oxides of nitrogen in carbon tetrachloride for 30-40 minutes at a temperature of 2 to 10oC and a pressure of 0.2 to 2.0 MPa, after which the intermediate product is separated from the solution and incubated for 3-5 hours at a temperature of 25-40oC and a pressure of 3.2 to 5.0 MPa. While on the second stage oxidation spend 15-30% solution of nitrogen oxides in 1,1,2,2-tetrachlorethane, or in dichloromethane. In the proposed method turns out this highly oxidised cellulose, used as non-toxic radioprotective, hemostatic, antimicrobial and wound healing agent.

The essence of izaberete is 5-11% solution periodate sodium with a pH of 2.5 to 4.5 at a temperature of 40-60oC for 4-5 hours, which contributes to the specificity of its oxidation by OH-groups at C2and C3atoms of elementary links with the formation of aldehyde groups (AG) and the flow of this process without decomposition of the oxidizer with a maximum speed up of the content of AG - 32-34%.

Subsequent washing of the obtained valdecaballeros (DAC) successively with water treated with 0.5% solution of sulfuric acid and purified water leads to thoroughly remove from it periodate and Iodate ions, affecting the toxicity of the final product. Received DAC dried by pulling air with a temperature of 60-70oC, until the residual moisture 8-12%.

In the second stage DAC for 40 minutes, treated with 15-30% solution of oxides of nitrogen in carbon tetrachloride (or 1.1, 2,2-tetrachlorethane, or dichloromethane) at 2-10oC. as a result, she absorbs this amount of nitrogen oxides, which is sufficient for subsequent oxidation to the desired degree. So, after sorption processing, merge the oxidizer solution, and further oxidation DAC carried out only at the expense of sorbed by nitrogen oxides within 3-5 hours when in 25-40oC and a pressure of 3.2 to 5.0 MPa. When observed is ilenia DAC to C2OOH - and C3OOH-groups throughout its volume with maximum speed.

Formed during oxidation of the intermediate product (this highly oxidised cellulose - oxides of nitrogen) purge with dry air, then washed with water purified from related oxides of nitrogen to achieve a pH value of wash water of 3.0 to 4.0. Subsequent washing of the product with ethyl alcohol is carried out with the aim of dehydration this highly oxidised cellulose and remove traces of low molecular weight fractions, which increases its toxicity.

Washed this highly oxidised cellulose is dried at 40-50oC and a residual pressure of 0.2-0.4 MPa.

The final product - this highly oxidised cellulose is non-toxic agent with radioprotective, kroveostanavlivajushchimi, antimicrobial and wound healing properties.

Described in the claims the settings selected on the basis of numerous experiments and are optimal. This is confirmed by the data of tables 1, 2, 3 and 4.

The method is as follows:

In a glass reactor load 5-11% solution of periodate sodium with a pH of 2.5-4.5 and heated to 40-60oC. Then charged to the reactor of the original cellulose and vidnym sulfuric acid solution, again with purified water and dried by air heated to 60-70oC.

In the second stage the resulting valdecaballeros (DAC) is loaded into the reactor with an oxidant - 15 - 30%-s ' solution of oxides of nitrogen in carbon tetrachloride, or 1,1, 2,2-tetrachloroethane, or dichloromethane and seal it. Cooling the reaction mass to 2-10oC, carry out the adsorption of nitrogen oxides on DAC for 30-40 min, then poured the oxidizer solution. The subsequent oxidation is carried out at 25-40oC and a pressure of 3.2 to 5.0 MPa within 3-5 hours Received this highly oxidised cellulose blown off with air, washed with purified water and ethanol, then dried in vacuum at 40-50oC to a residual moisture content of not more than 12%.

Example 1. In a reactor equipped with a jacket and a reflux condenser, download from the measuring device to 9.0 l of 10% aqueous solution of periodate sodium and heated to 50oC. Then a solution of oxidant load 580 g of cotton cellulose in the form of medical bandages size 0,h,0 m, pre-wound into skeins length of 0.25-0.30 m, consisting of 15 to 16 layers, after which the reaction mass is allowed to stand 5 hours, stirring occasionally, at a temperature of 55oC.

After the oxidation is drained exhaust R is again purified water.

Drying DAC spend in the dryer heater type at a temperature of 60-70oC to a residual moisture content of 8-12%. Gets 600 g DAC. The output is 98% by weight of the loaded cellulose 100% basis.

In the second stage of obtaining this highly oxidised cellulose was charged to the reactor 600 g DAC and 8 l of a 20% aqueous solution of oxides of nitrogen in carbon tetrachloride, pre-cooled to 4oC. Then the reactor is sealed and give exposure at a specified temperature for 40 minutes. Then merge the oxidizer solution from the reactor in the collection, and further oxidation DAC carry adsorbed oxides of nitrogen at 40oC and a pressure of 3.5 MPa for 4 h

Upon completion of the oxidation release the pressure in the system neutralization of nitrogen oxides, then blow the reactor and this highly oxidised cellulose compressed air for 1 h Received this highly oxidised cellulose is washed with purified water until no traces of nitric acid in the wash water. The last washing is carried out with ethyl alcohol.

Washed and well wrung a lot this highly oxidised cellulose is dried for 3 h at 40oC and a residual pressure of 0.4 MPa.

The dried product is cooled to 2 is ihod on stage is 90%.

The total yield of this highly oxidised cellulose - 70-75%, counting on the original cellulose in 100% basis. The content of carboxyl groups is 45-50%; the loss in weight on drying to 10%.

This highly oxidised cellulose "BOOKSELLING" granular white powder without odor and sour taste, practically insoluble in water, alcohol 95%, chloroform, diluted hydrochloric acid; sparingly soluble in 1% solutions of Kali caustic and caustic soda with the formation of small opalescence with the content of carboxyl groups 45-55%.

Received this highly oxidised cellulose "BOOKSELLING" can be used as effects for cation-exchanger with high exchange capacity, stable when in an acidic environment. "BOOKSELLING" absorbs radioactive nuclide and removes them from the body. Effective BOOKSELLING with the excretion of heavy metals.

Efficiency evaluation of BOOKSELLING" as antidote tools in the treatment and prevention of lesions radioisotopes of strontium were performed as outpatients in 27 healthy volunteers - men aged 18-26 years.

"BOOKSELLING" was used once by 10 grams per day in the form dispersed in 100 ml of water powder for 4 hours before admission,

- therapeutic purposes - together with income,

one hour after the intake of radioactive strontium.

Duration of treatment was 1 day.

As a result, it was obtained the data indicating the absence of "BOOKSELLING" toxicity, its high specific efficiency in the intake of radioactive strontium.

"BOOKSELLING" well tolerated, weak and moderately strong side phenomenon when taking 10 g were recorded only in 33.3% of the subjects. "BOOKSELLING showed high specific efficiency in all tested variants. Preliminary application "BOOKSELLING" 4 hours prior to receipt of strontium-85 reduced the level of resorption of the isotope in the gut to 2.3%, while the introduction BOOKSELLING" isotope - 1.3%), the destination BOOKSELLING" one hour after receipt of the isotope to 4.8% at the level of this indicator in the control of 28.4%.

This protective effect was in the first version of 90.6% in the second - 95,4% and in the third - 81,3%. High protective effect BOOKSELLING" in a wide interval of time exceeds the available and currently recommended drugs (including adabar and alginate).

Solutions of radioactive isotopes activity of 5-100 mccure in 0.5 ml of distilled water, acidified with HCl to pH 3, was injected into the stomach of rats using a plastic probe. The data obtained show that "BOOKSELLING" has a high efficiency in a wide time interval. High preventive effect BOOKSELLING" is determined from the 6 hours prior to the introduction and one hour after the introduction of fresh fission products.

Also examined the effectiveness of "BOOKSELLING in the prevention and treatment of intoxication by heavy metals, particularly manganese and mercury.

Used white outbred female rats weighing 170-220, Learning efficiency "BOOKSELLING" conducted in three groups of experimental animals: 1 - oral intake of manganese - Mn54, 2 - parenteral intake of manganese, 3-intratracheal intake of manganese. "BOOKSELLING" was introduced simultaneously with the manganese in the amount of 100 mg per rat. Oral introduction Marg is and found the most heavily excretion of manganese occurs in the first day, then excretion is reduced. When intratracheal introduction of manganese "BOOKSELLING also effective, as with the introduction of oral manganese.

"BOOKSELLING" was tested as a prophylactic and as a therapeutic agent for a group of workers mercury plant. It was used in different dosages depending on the degree of intoxication in the form of a powder without the use of symptomatic means. It is noted that in the first days all workers number of discharge with urine mercury increased in 11-140 times or more. This effect of reducing mercury in the body is constant, despite the fact that the workers were in high concentrations of mercury vapor in the air.

During treatment all patients noted improvement in health: abate headaches, restored sleep, appetite, decreased intensity of pain in the extremities, decreased pathological changes of internal organs.

Of special interest "BOOKSELLER" is as draining, hemostatic and antimicrobial agent.

"BOOKSELLING" has bactericidal effect against Gram-negative and Gram-paleoshiblyak action promoting a faster healing of the affected surface, improves the structure of the dermal scar (prevents the development of keloid scars, especially burns)

When applied externally, "BOOKSELLING is applied in the form of fine powder on a permeable substrate, is applied on the skin surface and fixed with a bandage.

Strip with "BOOKSELLING" changes daily, and the duration of the healing depends on the extent of damage to the skin surface.

1. The method of obtaining this highly oxidised cellulose, including two-stage oxidation of cellulose consistent treatment of iodine-containing compound and nitrogen oxides, washing with purified water, ethyl alcohol and drying, characterized in that in the first stage, the treatment is carried out 5 - 11%-s ' solution of periodate sodium with a pH of 2.5 to 4.5 at a temperature of 40 - 60oC, followed by washing with purified water and sulfuric acid solution and drying air temperature of 60 - 70oC, in the second stage 15 - 30%-s ' solution of oxides of nitrogen in carbon tetrachloride or dichloromethane or 1,1,2,2-tetrachlorethane for 30 - 40 minutes at a temperature of 2 to 10oC and a pressure of 0.2 to 2.0 MPa, followed by the separation of the intermediate product from Rast is oxidized cellulose, obtained by the method according to p. 1, as a non-toxic radioprotective, hemostatic, antimicrobial and healing tools.

 

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