Научная статья на тему 'Research of process of washing of fluorine from phosphor gypsum'

Research of process of washing of fluorine from phosphor gypsum Текст научной статьи по специальности «Фундаментальная медицина»

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Ключевые слова
phosphorite / extraction phosphoric acid / phosphor gypsum / defluorination / filtration / degree of washing

Аннотация научной статьи по фундаментальной медицине, автор научной работы — Shamshidinov Israiljon Turgunovich, Mirzakulov Kholtura Chorievich

Results of clearing of phosphor gypsum from fluoric compounds by washing by its solutions a chamois, a mix of sulfuric and phosphoric acids, 30 % a solution of ammonium nitrate and water are resulted. The maximum degree of washing phosphor gypsum from fluorine is observed at use of 60 % of sulfuric acid, a mix of sulfuric and phosphoric acid, 30 % by a solution of ammonium nitrate. Thus degree of washing makes 95.0–97.0 %, and the fluorine contents in phosphor gypsum decreases to 0.10–0.17 %.

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Текст научной работы на тему «Research of process of washing of fluorine from phosphor gypsum»

unpicking agent at initial temperatures of boiling 158 °C was allocated 5 % of fraction, and at decontamination from light naphtha this indicator made 164 °C. The boiling end with water vapor made 225 °C, and about the ferry of light naphtha made 209°C. At the end of technological process the exit ofhydrocarbonic fractions when using by water vapor made 98 %, the rest of 1.1 %, and with use of light naphtha as the unpicking agent the exit of fractions made 98.0 %, the rest of 1.2 %. From the conducted pilot researches it is visible that kerosene decontamination Jet

A-1 with hydrocarbonic couples proves to the advantages at their use as the unpicking agent.

Thus, uses of light naphtha as the unpicking agent for kerosene decontamination Jet A-1 to the advantages, after decontamination of their density, temperature of flash increases and acidity decreases this results from the fact that as a part of ready to production doesn't remain easy fractions and is absent an amount of water, besides temperature too decreases, this indicator it is possible will see their temperatures of flash.

References:

1. Skoblo A. I., Molokanov Yu. K., Vladimirov A. I., Shchelkunov V. A. Processes and devices of a neftegazoper-abotka and petrochemistry. 3rd prod. reslave. and additional. - M: JSC Businesstsentr-Nedra, 2000. - P. 5-7.

2. Technology of oil refining. In 2 parts. Part one. Primary oil refining/Under the editorship of O. F. Glagoleva and V. M. Kapustin. - M.: Chemistry, Colossus, 2006. - P. 331-345.

3. Manovyan A. K. Technology of primary oil refining and natural gas. Manual for higher education institutions. 2nd prod. - M.: Chemistry, 2001. - P. 138-140.

4. Salimov Z. S., Saydakhmedov Sh. M., Khudoyberganov A. A., Khurmamatov A. A., Hudayberdiyev A. A. Studying of process of an decontamination of kerosene fraction by hydrocarbonic couples//Oil processing Magazine and petrochemistry. - Moscow, 2012. - No. 9. - P. 10-13.

DOI: http://dx.doi.org/10.20534/AJT-17-1.2-107-111

Shamshidinov Israiljon Turgunovich, Candidate of technical science, associate professor, Associate professor of cathedral «Professional education (Chemical technology)»,

Namangan engineering-pedagogical institute, Uzbekistan

E-mail: [email protected]

Mirzakulov Kholtura Chorievich, Doctor of technical science, professor, Professor of cathedral «<Chemical technology of inorganic substances»

E-mail: [email protected]

Research of process of washing of fluorine from phosphor gypsum

Abstract: Results of clearing of phosphor gypsum from fluoric compounds by washing by its solutions a chamois, a mix of sulfuric and phosphoric acids, 30 % a solution of ammonium nitrate and water are resulted. The maximum degree of washing phosphor gypsum from fluorine is observed at use of 60 % of sulfuric acid, a mix of sulfuric and phosphoric acid, 30 % by a solution of ammonium nitrate. Thus degree of washing makes 95.0-97.0 %, and the fluorine contents in phosphor gypsum decreases to 0.10-0.17 %.

Keywords: phosphorite, extraction phosphoric acid, phosphor gypsum, defluorination, filtration, degree of washing.

Introduction fluorine. At achievement of full satisfaction of require-

At the average contents in extraction phosphoric ment of agriculture of Republic Uzbekistan in phosphor-acid (EPA) 1.2 % is fluorine, received of 716 thousand ic fertilizers (the requirement for phosphoric fertilizers t washed burnt phosphor concentrate of Central Kyzyl- makes 518 thousand t. 100 % of P2 05) on fields will be kum (CK), annually in soil is brought 8.59 thousand t of brought 34.36 thousand t fluorine.

The average contents of fluorine in phosphor contents the fertilizers made in Republic, such as ammophos, su-prephos, makes superphosphate from 2.0 to 4.0 %. One of perspective methods of decrease the fluorine contents in fertilizers is its extraction from EPA by its manufacture as 70-80 % offluorine at acid decomposition ofphosphat-ic raw materials remain in EPA. It can achieve introduction in process sulfuric acid decomposition of phosphates of connections of alkaline metals with simultaneous reception fluorosilicate or by evaporation acid [1; 2]. These ways demand the additional equipment and are connected with the big expense of power resources.

Many researches are devoted to defluorination of EPA from phosphorites of Central Kyzylkum, which distinctive feature are low (0.13 %) the contents of acid-soluble compounds of silicon [3-5].

We develop a way of clearing of EPA from fluorine in a work cycle of manufacture of acid, by introduction of a carbonate of calcium before a filtration of extraction pulps [6]. Thus from 68.4 % to 82.5 % of fluorine it is besieged in the form of fluoride of calcium and remains in structure phosphor sypsum depending on norm of a carbonate of calcium (60-100 % on the fluorine content). At norm of 100-150 % of a calcium carbonate in phosphor gypsum passes 82.5-86.8 % of fluorine from available in phosphorite.

Fluorine is the necessary chemical element for manufacture of anticorrosive preparations, extraction

of precious metals, serves mineralizator at reception of cements. Therefore researches directed on extraction of fluorine from phosphor gypsum are very actual.

Objects and methods

On purpose allocation of fluorine from phosphor gypsum researches on washing of phosphor gypsum with sulfuric acid and phosphoric acid are carried out by solutions of various concentration, and also solutions of ammonium nitrate.

For this purpose received phosphor gypsum by introduction in sulfuric acid pulp of contents of EPA of a calcium carbonate in quantity providing norm of calcium on contents of fluorine of 100 %. After 30 minute hashing at temperature 80 °C, a pulp divided on funnel of Buxner, using lavsan fabric. The area of a filtering fabric of 131.8 sm 2.

Received phosphor gypsum contained 3.37 % of fluorine. Washing of phosphor gypsum was carried out by 5-60 % solutions of sulfuric acid, a mix of sulfuric acid with EPA, containing from 2.28 % to 6.97 % P2O5 , the temperature was supported 60 °C.

The first washing phosphor gypsum spent washing solutions, and the second and third washing carried out hot water (60 °C).

Results of the residual contents of fluorine in phosphor gypsum and technological indicators reception EFA and washing of phosphor gypsum are resulted in table 1.

Table 1. - Technological indicators of washing phosphor gypsum from fluorine sulfuric- and sulfuric-phosphoric acid solutions

№ experiments Washing solution The contents of fluorine after washing phosphor gypsum Technological indicators of reception of EPA Degree of washing phosphor gypsum from fluorine, %

Concentration H2SO4, % on SO3 Concentration EPA, % on P2O5 K , p. % K , otm/ % K t , out ' %

1. 60 — 0.42 99.80 99.30 99.20 87.54

2. 30 - 0.50 98.70 98.90 97.61 85.11

3. 20 — 0.55 98.48 98.60 97.11 83.68

4. 10 - 0.61 98.09 98.40 96.52 81.90

5. 5 — 0.77 97.87 98.21 96.12 77.15

6. 60 2.28 0.15 99.60 99.99 99.59 95.55

7. 30 4.29 0.30 98.60 99.99 98.58 91.10

8. 20 5.96 0.21 98.53 99.76 98.29 87.83

9. 10 6.97 0.10 98.38 99.70 98.08 97.03

With increase in concentration ofsulfuric acid with 5 to 60 % the fluorine content in phosphor gypsum decreases from 3.37 % to 0.42-0.77 %. Degree of extraction of fluorine makes 77.15-87.54 %. The best results are received at use ofsulfuric acid with concentration of60 %. Thus the decomposition factor ofphosphor raw material makes 99.8 %, factor washing 99.3 % and factor of an exit of 99.2 %.

At use of the sulfuric acid in addition containing EPA, technological indicators of process of washing improve, and the fluorine contents in phosphor gypsum decreases to 0.10-0.30 %, degree of extraction of fluorine makes 87.83-97.03 %. All factors — phosphorite decomposition, washing of phosphor gypsum and exit EPA raise also. Optimum techno-

logical parameters of washing fluorine from phosphor gypsum are: concentration of sulfuric acid of 60 % on SO3 , 60 % SO3 and with introduction of EPA in number of 2.28 % on P2O5 and 10 % on SO3 with introduction of 6.97 % EPA on P205

In fig. 1 the given changes of the content of fluorine in washed phosphor gypsum 30 % by a solution of ammonium nitrate, 11 % a solution of sulfuric acid on SO3 and hot water depending on temperature of washing solutions are cited.

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Fig. 1. Change of the contents of fluorine in phosphor gypsum at washing: 1) 30 % solution of ammonium nitrate; 2) 11 % solution of sulfuric acid on SO3; 3) hot water depending on temperature of process of washing

Table 2. - Influence of temperature of washing on the fluorine content in production EPA and washing solutions (the fluorine content in not washed phosphor gypsum 3.37 %)

№ experiments Washing temperature Th ie fluorine content, % The fluorine content in phosphor gypsum, % Degree of washing phosphor gypsum from fluorine, %

I ^-T II ^-T III ^-T IV ^-T

Counterflow washing by hot water

1 60 0.92 1.05 0.84 0.53 0.90 73.4

2 70 0.89 1.06 0.84 0.57 0.61 82.0

3 80 0.87 1.01 0.89 0.47 0.58 82.8

4 90 0.86 1.13 0.81 0.31 0.57 83.0

Washing of 30 % by solution NH4NO3

5 60 0.84 0.66 0.60 0.74 0.53 84.4

6 70 0.92 0.76 1.17 0.39 0.31 90.9

7 80 0.77 0.64 1.82 0.78 0.17 95.0

8 90 0.81 0.87 1.94 0.75 0.10 97.0

Washing of 11 % by a solution on SO3 su furic acid

9 60 0.59 0.94 1.04 0.83 0.54 83.9

10 70 0.47 0.95 1.13 0.83 0.47 86.1

11 80 — 0.94 1.18 0.67 0.44 87.0

12 90 0.69 1.07 1.24 0.57 0.43 87.1

From the resulted of data it is visible, that the best indicators ofwashing are reached at use of 30 % of a solution of ammonium nitrate. Rise in temperature of a washing solution essentially influences washing degree phosphor gypsum at application of a solution of ammonium nitrate

and water. At use of 11 % on SO3 a solution of sulfuric acid influence of temperature of a washing solution does not render appreciable influence. At temperature of a washing solution 80-90 °C washing degree of phosphor gypsum from fluorine a solution of ammonium nitrate

exceeds 97 %, 11 % sulfuric acid on SO3 exceeds 87 %, water makes more than 83 %.

In table 2 data on change of the content of fluorine in washing solutions are cited at use for water washing, 30 %

From the table it is visible, that rise in temperature with 60 °C to 90 °C promotes decrease in the content of fluorine in phosphor gypsum at washing by water from 0.90 % to 0.57 %, at washing of 30 % by a solution of am-

of a solution of ammonium nitrate and 11 % on SO a monium nitrate from 0.53 % to 0.10 % and 11 % on SO a

solution of sulfuric acid.

solution of sulfuric acid from 0.54 % to 0.43 '

Fig. 2. The basic technological scheme of washing phosphor gypsum from fluorine: 1 - extractor; 2 - carausel vacuum-filter; 2a - first zone of a filtration; 2b - second zone of a filtration; 2c - third zone of a filtration; 2d - fourth zone of a filtration; 3 - collection of the first filtrate; 4 - warehouse of extraction phosphoric acid; 5 - amalgamator; 6 - collection of the second filtrate; 7 - pressure head tank; 8 - collection of the third filtrate; 9 - collection of the fourth filtrate; 10 - sediment bowl.

In fig. 2 the washing scheme phosphor gypsum with use for washing of sulfuric acid is resulted. The pulp sulphur-phosphoric acid decomposition of phosphatic raw materials from an ex-tractor moves on 1st zone ofa filtration (poses. 2a) where occurs branch production EPA from phosphor gypsum. EPA arrives in the collection of 1st filtrate (poses. 3) and further in acid storehouse (poses. 4).

Phosphor gypsum at the first stage it is washed out by sulfuric acid (poses. 2b) also gathers in capacity (poses. 10). At the second and third stage it is washed out by hot water. A filtrate after the second stage (poses. 2c) also arrives in capacity (poses. 10), and after the third stage (poses. 2d) moves on the first stage of washing phosphor gypsum (poses. 2b),

In the second and third zones of washing (poses. 2c and 2d) occurs additional washing of fluorine from phosphor gypsum, passed under the influence of acid in the soluble form.

For sedimentation of soluble forms of fluorine in sediment bowl (poses. 10) it is entered sodium sulphate

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for fluorine linkage in sodium fluorosilicate and its allocation for use to destination. Cleanliness sodium fluorosilicate makes not less than 96 %. Mother solution after branch sodium fluorosilicate comes back to a stage of decomposition of phosphorite.

Conclution

Thus, the carried out researches have shown possibility of reception of EPA partially cleared of fluorine by introduction in extraction pulp of a calcium carbonate and washing phosphor gypsum from fluorine solutions a chamois, a chamois and EPA acids, ammonium nitrate.

The best results of washing phosphor gypsum from fluorine are reached at use of 60 % on SO3 sulfuric acid, 60 and 10 % on SO3 a chamois and EPA acids with the contents of 2.28 % and 6.97 % P2O5, 30 % a solution of ammonium nitrate. Washing is desirable for carrying out at temperature 80-90 °C. Thus degree of washing makes 95.0-97.0 %, and the fluorine content in phosphor gypsum does not exceed 0.10-0.17 %.

Analysis of productive solutions and uranium sorption on anionits

References:

1. Kochetkov S. P., Smirnov N. N., Il'in A. I. Concentrating and clearing of extraction phosphoric acid/GOUV-PO Ivan. gov. chem.-technolog. ins. - Ivanova, 2007. - 308 p.

2. Khujamkulov S. Z., Melikulova G. E., Mirmusaeva K. S., Mirsaidov M. H., Mirzakulov Kh. Ch. Research ofprocesses of reception sodium fluorosilicate from extraction phosphoric acid on the basis of phosphorites of Central Kyzyl-kumov//Chemical technology. The control and management. - Tashkent: TGTU, 2016. - № 1 (67). - P. 34-40.

3. Khujamkulov S. Z., Asamov D. D., Bardin S. V., Mirzakulov Kh. Ch. Defluorination of extraction phosphoric acid with salts of sodium//Chemistry and chemical technology. - 2008. - № 2. - P. 16-19.

4. Khujamkulov S. Z., Asamov D. D., Bardin S. V., Mirzakulov Kh. Ch. Defluorination of extraction phosphoric acid of Central Kyzylkum in the presence of sodium silicate.//Chemistry and chemical technology. - 2008. -№ 4. - P. 8-11.

5. Khujamkulov S. Z., Asamov D. D., Bardin S. V., Mirzakulov Kh. Ch. Technology working out defluorination of extraction phosphoric phosphoric acid of Central Kyzylkum with recycling of sodium silicate//Chemical technology. The control and management. - Tashkent: TGTU, 2008. - № 4. - P. 41-45.

6. Arislanov A., Shamshidinov I., Gafurov K. Defluorination of EPA from phosphorites of KyzylKum in the process of decomposition//Scientific and technical journal FerPI. - Fergana: FerPI, 2006. - № 2. - P. 95-98.

DOI: http://dx.doi.org/10.20534/AJT-17-1.2-111-113

Sharipov Khasan T., Tashkent State Technical University, Professor, Doctor of Chemical Sciences, Deputy Chairman of the SUE "Fan va tarakkiet"

Sharafutdinov Ulugbek Z., Navoi Mining and Metallurgical Combinate, Chief of the technical control service of the MA. of the NMMC

E-mail: [email protected]

Rajabboev Ibodillo M., Navoi state mining Institute, researcher

Khujaev Jasur E., Navoi state mining Institute, researcher

Analysis of productive solutions and uranium sorption on anionits

Abstract: Currently of the uranium mined in Navoi Mining and Metallurgical Combinate is obtained by means of underground leaching in the Kyzyl-Kum open pits. This method allows to reduce the cost of uranium mining and ensure the environmentally clean production.

Keywords: uranium, underground leaching, sorption, extraction, rhenium, environmental protection.

Currently, mineral raw resources compound eco- of raw resources' basis consists of hydrogen mines

nomic roots of many developed countries therefore which are based on processing by boreholes of under-

advances of industry and agriculture depends on ratio- ground leaching.

nal and fruitful usage of them by means of creation of Uranium has had a severe impact on many aspects

new technologies which provide complex processing. of intergovernmental relations which are far from sci-

Especially it is about extraction of rare metals which ence, particularly on international politics. Develop-

composes interrelated and sophisticated cyclical pro- ment of mining the uranium in Kyzyl-Kum region on

cess and obtaining final ready products in their pure the basis of physicochemical technology inseparably

forms. Nowadays in uranium industry the main part tied together with common tendency of the global

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