Assistant professor, Karshi Institute of Engineering and Economics, Republic of Uzbekistan, Karshi
METHOD FOR SEPARATING NICKEL FROM INDUSTRIAL WASTE AND ITS USE IN PRODUCTION
ABSTRACT
The article describes the process of nickel extraction from the used waste of the GIAP-8 catalyst in the form of nickel nitrate, in which it not only does not affect the environmental environment, but is also a cost-effective solution for the production of nickel catalysts. The obtained catalysts were tested under laboratory conditions, andthe reactivity of the catalyst in this convertedresidual methane was 35.7% at T=500 °C and 6.5% at T=700°C.
АННОТАЦИЯ
В статье описан процесс извлечения никеля из состава используемых отходов катализатора ГИАП-8 в виде нитрата никеля, в котором он не только не влияет экологическую среду, но и является экономически эффективным решением для производства никелевых катализаторов. Полученные катализаторы апробировано в лабораторных условиях, активность катализатора в этом преобразованном остаточном метане составляла 35,7% при T=500 °C и 6,5% при T=700°C.
Keywords: industrial waste, nickel oxide, catalyst, nickel nitrate, GIAP-8, activity.
Ключевые слова: промышленные отходы, оксид никеля, катализатор, нитрат никеля, GIAP-8, активность.
The development of modern science and technology leads to the fact that the need for non-ferrous and rare metals increases from year to year. Processing of non-ferrous metals leads to a reduction in deposits of rare earth metals. One of the most pressing problems at present is the development and implementation of energy-saving technologies for processing rare metals contained in secondary raw materials into finished or semi-finished products. Rational integrated use of raw materials, transitionto production is one of the most urgent problems of waste-free technologies for its processing and recycling of technogenic formations. Processing of raw materials is of great economic and environmental importance.
According to numerous studies, the best catalyst for the methane conversion process is a nickelcatalyst. And in the catalyst in the form of nickel oxide. The catalyst accelerates the conversion of methane. Therefore, in the process before starting the conversion, hydrogen together with the catalyst is reduced to nickel oxide for 2-4 hours at a temperature of 300-400 °C, NiO +H2O = Ni +H2O. The process can also be anhydrous, in which it is carried out with a working mixture (methane and water vapor) at 700-800 °C.
If nickel is not in the form of oxides, but in the form of their compounds with aluminum oxide (spinel), then its reduction requires a high temperature (800-900 °C). In this case, the recovery process is slow.H2 formation when the nickel-aluminum catalyst is heated above 600 °C.
The GIAP-8 catalyst is designed for the conversion of natural gas. The composition of the catalyst is nickel and aluminum oxide. The mass fraction of NiO in the catalyst is 6-10%.
And in the catalyst used, the nickel oxide content is 5.5-6.5% of the total mass of the catalyst. Given that nickel is purchased abroad at a high price, it is undesirable to throw it away. As a result of scientific research, Ni(NO3)2 with nitric acid was extracted from the GIAP-8 catalyst used. As a result, the acid concentration, its norm, and the ratio of liquid phases are determined.
The resulting Ni(NO3)2 solution was impregnated with a catalyst carrier (alumina-calcium-manganese alloy) CHKR-06 (improved). To extract из отработанныхGIAP-8 from spent catalysts, the central laboratory of JSC “Maksam-Chirchik” used the method of dissolution in nitric acid. GIAP development catalyst-8 20%, 30%, 40%, 50% it is soluble in concentrated nitric acid [4]. The results shown in Table1show that washing with boiling water after separation in a 40% nitric acid solution for 4 hours is achieved by converting 90-95% nickel into solution (Table 1).
The GIAP-8 catalyst that was originally used for the process was ground and placed in a 1: 4 ratio glass of distilled water and evaporated by boiling the water. History 20%, 30%, 40%, 50% in concentrated nitric acid, insist, stirring for 4 hours. Gives color, slowly turning into a solution for 4 hours. The mixture was then separated into liquid and solid phases in a vacuum filter. Ni(NO3)2 forming the composition of the liquid phase was analyzed by titration.
Table 1.
Spent GIAP-8 catalyst for 4 hours 20%, 30%, 40%, 50% dissolution in concentrated nitric acid
Mass of spent catalyst GIAP-8, g |
Concentration of HNO3, % |
Amount of acid, ml amount of water, ml |
Amount of water, ml |
Amount of NiO remaining in the solid phase, % |
Amount remaining in acid, g/dm3 |
Degree of extraction of Ni, % |
|
100 norm |
|||||||
10 |
20 |
106.75 |
40 |
0.967 |
16.42 |
82.84 |
|
10 |
30 |
71,16 |
40 |
0,6716 |
26,53 |
91,6 |
|
10 |
40 |
53,375 |
40 |
0,42 |
43,824 |
95,12 |
|
110 the norm |
|||||||
25 |
20 |
266,87 |
- |
1,6 |
14,15 |
78,27 |
|
25 |
30 |
178-1 |
- |
,56 |
21,45 |
79,537 |
|
25 |
40 |
101,34 |
- |
1,02 |
40,172 |
88,75 |
|
25 |
50 |
106,75 |
- |
0,93 |
43,824 |
90,05 |
|
25 |
20 |
293,56 |
100 |
2,328 |
12,1 |
72,036 |
|
25 |
30 |
195,8 |
100 |
0,827 |
21,4 |
90,33 |
|
25 |
40 |
146,74 |
100 |
0.714 |
35.38 |
92.43 |
|
The solid phase was also analyzed for its NiO content. The rate of nickel recovery from the catalyst was calculated by the formula:
gde, S-macca of nickel oxide isolated from the catalyst (NiO), g;
C1is the mass of nickel oxide (NiO) remaining in the solid phase after filtration of the used GIAP-8, g.
To calculate the degree of dissociation, taking into account that the mass fraction of NiO in the GIAP-8 catalyst used is 6.5%, a mass fraction of 6% NiO was isolated in it. The mass concentration of Ni (NO3)2 in solution is (200-550) g /dm3. The mass of nickel oxide remaining in the solid phase is (20-30) g /dm3. The nickel nitrate solution was evaporated and the nickel nitrate content Ni(NO3)2 was adjusted to 2-490 g /dm3. This solution was immersed twice in the support, and the catalyst was dried and cooled in the control mode.
The mass fraction of NiO is 10%, and the mass fraction of SO3 is 0.004%. B) The CHCR-21 catalyst was obtained. The catalyst test is performed in Figure 1.
Figure 1. Scheme for testing the catalyst in the laboratory
1,1", 1" - cylinders with H2, N2, CH4 2,2\ 2 "- reducers on the line with H2, N2, CH4 3, 3', 3", 12 - odnoshnekovoy crane 4,4", 4 " - manostats 5-flask Tishchenko (drexel6 ,6 " - rheometers 7-column with scavenger CP-And 8 - column with desulfurizing mass 9,20,22 electric furnace 10, 29- 10,29-scavenger flask with Ca(CH3COOCH3COO)solution)2 solution2 11 - chromell-alumel thermocouple 13-pressure flask 14-bottle (50-100) cm3 15-water supply capillary
|
16-mercury diphmanometer 17-xylene coil evaporator 18 - xylene thermostat 19-xylene vapor condensation pipe ксилола 21, 28, 31-three-way tap 23-quartz reactor 24- selected pipette 25-thermocouple 26-water cooler 27-collection steam condensate collector 30- gas meter 32- asbestos cord-winding 33, 36-two- way tap 34- cotton water supply thread 35, 35', 35 " - three-way tap on a comb |
The results of testing the catalyst obtained in the central laboratory of the enterprise JSC "Maksam-Chirchik" are shown in Table 2.
Table of test results of the CHKR-06 catalyst (advanced) test units were tested and put into operation. Prepared to work with nitrogen. They gave out hydrogens and the temperature began to rise to 500 °C.
Tsh 0020368-15: 2014 according to the enterprise standard, the test result of the CHCR-06 (improved) catalyst should not exceed 37% of the residual methane content, which does not decompose at a temperature of 500 °C. At a temperature of 700 °C, the content of non-decomposed residual methane should not exceed 8%. Based on the test results of the CHKR-06 (advanced) catalyst, the test result indicators showed that at a temperature of 500 °C, the content of non-decomposed residual methane was 35.7%, and at a temperature of 700 °C, the content of non-decomposed residual methane was 6.5%.
Table 2
Results показателей активности of catalyst activity indicators
Time |
Temperature mode, °C |
Water mode |
Gas mode |
Note |
||||
in the reactor |
Purification sulfur |
in xylene strain gauge |
pressure, mm |
Water level measurement in the burette, ml |
Water flow rate, ml |
CH4 |
|
|
1030 |
500 |
250 |
180 |
61 |
19 |
17 |
30 |
Output №1-35,3% |
1100 |
500 |
250 |
180 |
84,5 |
23,5 |
20 |
30 |
Output №2-36,1% |
1130 |
500 |
250 |
180 |
100/6,5 |
22 |
17 |
30 |
Output №3-35,8% |
1200 |
600 |
250 |
190 |
25 |
18,5 |
11,5 |
30 |
|
1230 |
675 |
250 |
190 |
48,5 |
23,5 |
13,5 |
30 |
|
1300 |
700 |
250 |
190 |
70 |
21,5 |
13,5 |
30 |
|
1330 |
700 |
250 |
185 |
96 |
26 |
15 |
30 |
|
1400 |
700 |
250 |
185 |
100/21 |
25,5 |
13 |
30 |
Output №1-5,6% |
1430 |
700 |
250 |
185 |
44,5 |
24 |
14 |
30 |
Output №2-6,8% |
1500 |
700 |
250 |
185 |
70 |
24,5 |
14 |
30 |
Output №3-7,2% |
1530 |
700 |
250 |
185 |
93 |
23 |
13 |
30 |
Output №4-6.5% |
Conclusion. NiO contained in the GIAP-8 catalyst separated with nitric acid was separated. To do this, water is placed in the catalyst in a ratio of 1: 4 and boiled water is evaporated, then nitric acid is added and infused, stirring for 4 hours. The solid phase was then separated from the liquid phase in a vacuum filter, and the solid phase was analyzed for Ni(NO3)2 g/dm3 in the liquid phase. In the case of Ni(NO3)2 the resulting solution was evaporated and brought to Ni (NO3)2=490 g /dm3, and a CHCR-06 (improved) catalyst was installed on the support. NIO impregnation meets the requirements of GOST. The level of operation of the resulting catalyst in laboratory testing equipment was checked. As a result, the indicators meet the requirements of the enterprise standard.
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