Synthesis and modification of Nickel /SAPO-34 Nanocatalyst for MTO Process via ultrasound and impregnation and hydrothermal methods

doi:10.21203/rs.3.rs-1648459/v1

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Synthesis and modification of Nickel /SAPO-34 Nanocatalyst for MTO Process via ultrasound and impregnation and hydrothermal methods

https://doi.org/10.21203/rs.3.rs-1648459/v1

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In this paper, to research the effect of Ni on the structure and performance of the SAPO-34 catalyst, seven samples were synthesized. 3 samples were prepared via ultrasound, impregnation, and hydrothermal methods and with 2% Ni, the characteristics and performance of those samples were compared with SAPO-34 and was choosing the sole method. Then three samples were synthesized with a ratio of 3, 5, 7% Nickel then the optimized method. These catalysts were characterized by BET, NH3-TPD techniques. Cooperation of the performance of the catalysts showed that catalysts prepared by using ultrasound are more appropriate because of smaller particle size, Reduction of the expansion of the crystal, and uniform distribution of particles within the catalyst structure than the catalysts prepared by impregnation and hydrothermal method. Catalyst synthesized by ultrasound and 5% nickel, due to high crystallinity, the little size of crystals, high expanse, and suitable acid power showed the most effective possible selectivity for ethylene and propylene. The utmost ethylene and propylene selectivity for this sample was 47.89% and 35.16%. The sample was synthesized by using ultrasound and seven nickel, that possessed strong and high density of acidic sites thanks to the increasing amount of nickel, despite the reduction of particle size, was deactivated rapidly. Pure SAPO-34 was the underside selectivity to light olefins.

Asphalting

Nano

Gas Injection

Water Injection

Crystallinity

The production of ethylene and propylene has received wide attention in recent years because of the increasing demand for these products [1–3]. In percent, light olefins production isn't guilty for world demand. Light olefins typically were produced with steam cracking or catalyst cracking of naphtha. Recently, because the instability in crude prices then the limitation of crude sources, the international market of olefins has faced a big challenge. SAPO-34 is most promising catalysts for the methanol to light olefins process [4–7, 51–55]. the foremost important characteristics of those catalysts are shape selectivity and moderate acidity. The SAPO-34 catalyst is well-known because the foremost effective catalyst for the MTO process. it's a CHA structure with an 8-membered ring cage-type and cage entrance diameter of 0.38 nm. SAPO-34 catalyst has beyond 90% light olefins selectivity and complete methanol conversion at mild conditions. Si/Al ratio might be an important factor for determining the acidity and catalytic performance of SAPO-34 [8–10]. Synthesized SAPO-34 by higher Si/Al ratio has moderate acidity and lightweight olefins are main products but at lower Si/Al ratio due to more strong acid sites, aromatics are major products[56–63]. So, the subsequent Si/Al ratio of about 200 is proper for the MTO process. Synthesized SAPO-34 at the subsequent Si/Al ratio has a longer lifetime and lower light olefins selectivity in comparison with SAPO-34 [11–13]. Therefore, a mix of SAPO-34 catalysts finally lands up within the formation of an optimal catalyst within the angle of optimum light olefins selectivity and lifelong. Light olefins are basic materials in chemical industries and are accustomed make polyethylene and polypropylene and other important products [14–20]. Traditionally, light olefins are produced by steam creaking units and fluid catalytic cracking units, where the foremost feedstock is petroleum. The methanol to olefins (MTO) process provides another approach to supply light olefins from non-oil resources like coal and fuel [21–27]. to induce an honest mechanical strength to resist the abrasion during fluidization, the binder was commonly used as a cross-link additive [28]. SAPO-34 are of poor self-binding property and can be bound with a binder like silica, alumina, or clay to convey a desired physical shape and mechanical strength for industrial application. For catalytic applications of SAPO-34, silica, and alumina as a binder are the foremost widely utilized commercially [29–32]. Until now, there has been no published work that systemically discusses the results of binders on the spray-dried SAPO-34 physiochemical properties and also the potential effects of binder’s materials on catalytic performance seem to possess been largely neglected within the tutorial literature [33–35]. The aim of this text to check the effect of metal and its different methods in placing it within the composition of the SAPO-34 catalyst, Samples with different ratios of nickel-metal are visiting be prepared and their performance within the methanol to olefin process are examined [36–40]. the employment of nickel-metal within the synthesis of the SAPO-34 catalyst increases the precise area of the catalyst, creating strong acidic centers suitable for pure SAPO-34 and improving the catalyst's performance [41–50].

To investigate the effect of nickel metal on the synthesis of SAPO-34 catalysts, 3 catalyst samples were prepared using hydrothermal, impregnation, ultrasonic methods with 2% nickel, and a catalyst sample without nickel. Then, from these three methods, the optimal method was selected. Then 3 samples were synthesized with a ratio of 3, 5, and 7 Nickel. Samples were prepared by combining the following molar ratios. Table 1 was placed on the SAPO-34 catalyst using different methods[36–41].

Table 1

.synthesis SAPO-34 catalyst using different methods.
Sample	Methods synthesis Ni/SAPO-34	NiO/ Al₂O₃
S1	hydrothermal	0.02
S2	hydrothermal	0.02
S3	impregnation	0.02
S4	ultrasonic	0.02
S5	ultrasonic	0.03
S6	ultrasonic	0.05
S7	ultrasonic	0.07

1Al₂O₃: 1P₂O₅: 0.4SiO₂: 1TEAOH:0.5MOR:0.5TEA:70H₂O: 0.02 NiO

1Al₂O₃: 1P₂O₅: 0.4SiO₂: 1TEAOH:0.5MOR:0.5TEA:70H₂O: 0.03 NiO

1Al₂O₃: 1P₂O₅: 0.4SiO₂: 1TEAOH:0.5MOR:0.5TEA:70H₂O: 0.05 NiO

1Al2O3: 1P2O5: 0.4SiO2: 1TEAOH:0.5MOR:0.5TEA:70H2O: 0.07NiO.

3.1. Investigate the surface area and size of the catalyst cavity (BET).

The results of the BET analysis are given in Table 2 the extent, size, and volume of the catalyst cavities. These results show that by changing the synthesis methods and different ratios of nickel metal, the size of the cavities, the volume, and area of their surface changes, which can affect the acceptability and efficiency of sunshine olefins production. Comparing the extent of the catalysts, it's concluded that the S6 catalyst prepared by ultrasound and with a ratio of fifty nickel has the simplest extent and cavity volume compared to other samples. The presence of ultrasonic energy is an honest consideration controlling the particle size within the ultrasonic method and its effect on increasing the zeolite level is over the impregnation and hydrothermal method. As a result, the extent of the S6 catalyst was over the rest of the samples. Sample S6 the ratio of sample S5 is higher due to having more nickel and better crystallinity and a better specific extent. it's expected that this process will have better activity within the method of methanol to olefin. additionally, per Table 2, Sample S1 has the underside expanse because of the larger crystal size [25].

Table 2

BET for prepared catalyst
Sample	Surface area, m²/g	Pore volume, cm³/g	Pore size, Å
S1 (SAPO-34 pure)	511.24	0.29	22.13
S2(Hydrothermal method and 2% nickel)	541.18	0.33	23.40
S3(impregnation method and 2% nickel )	532.58	0.31	21.90
S4 (ultrasound method and 2% nickel )	563.91	0.38	27.67
S6 (ultrasound method and 5% nickel )	645.07	0.40	24.82

3.2. Temperature Programmed Desorption (TPD).

The temperature-programmed desorption of ammonia (NH₃-TPD) analysis to research the acidic properties and catalytic behavior and distinguish of acid strength and so the amounts of acid sites of three samples of S1, S6, and S7 are shown in Figs. 1 Sample was selected for TPD analysis to provide comparative conditions for the acidic behavior of pure SAPO-34 catalyst and a nickel-modified metal catalyst. the first strong peak in TPD charts is sometimes related to weak acidic locations because of T–O–H bonds within the middle of tetragonal structure that are only capable of converting methanol to dimethyl ether and can't convert methyl ether to light olefins. the large area under this peak is because the presence of incomplete structures within the catalytic composition and thus the reduction of sample crystallization. Sample S6 modified by nickel metal is relatively less crystallized than sample S1, and as is also seen within the TPD diagram, the globe of the realm below the first peak in sample S6 is larger than that of sample S1. The second peak appeared in sample S6 at a higher temperature (425°C) than sample S1, that the acidity of acidic places is higher during this sample. On the other hand, the intensity of the second peak indicates the number of acidic sites and is proportional to the amount of ammonia excreted, which is larger than the intensity of the second peak for sample S6.

As you'll see, to work out the activity of the synthesized catalysts, 2 g (catalyst + silicon carbide) was subjected to the equality reaction conditions. The reaction temperature is 410°C and gas pressure, and also the spatial velocity of 8 h^− 1 and also the mixture of 30 wt. you look after methanol in water with a rate of 0.4 ml/min has been missed out the catalyst[1–3]. Comparison of the performance of catalysts in Figs. 2 (S1-S7) shows that the catalyst prepared using the ultrasonic method thanks to the smaller size, reduced growth of crystals and uniform distribution of particles within the structure compared to catalysts prepared by impregnation and hydrothermal method has more suitable activity are. As are often seen, the samples S4–S7 that were synthesized using the ultrasonic method have higher selectivity than the sample S1–S3. Sample S1 incorporates a faster selectivity drop than olefins than other samples. the rationale for this will be associated with the presence of huge crystals during this catalyst[35–42]. Large crystals increase the penetration resistance and forestall reactions from reaching the catalyst center. Therefore, the extent used for catalytic activity in coarse crystals is low and this catalyst is quickly inactivated. Maximizing the efficiency of ethylene indicates the onset of catalytic inactivity and also the reduction of free space within the catalytic cavities, after which the ethylene efficiency decreases and bigger hydrocarbons occupy the cavities. thanks to all kinds of selectivity, propylene drop occurs faster than ethylene. this can be because the vacuum within the structure of the catalytic cavities must be reduced because of the formation of larger hydrocarbon species like methylnaphthalene, phenanthrene, and pyrene. These species then act as organic centers, rather than producing propylene, it produces ethylene. In sample S7, after about 200 min, there's a small decrease within the production of olefins, which might be attributed to the strong and high acidity during this sample. Large amounts of acidic sites increase the probability of hydrogen transfer reactions to olefins, the formation of hydrocarbons and aromatics, and also the formation of coke at the catalyst level[42]. This article was conducted in an MTO unit located in the Iranian Olefin Research Laboratory and most of them, the reactor conditions, Product production methods, catalyst weight, feed flow type. The operating conditions, the type of catalyst, and the results of the studies are presented in Table 3[42–45].

Table 3

Research on MTO unit
	yield wt.%			temperature operating	feed	References
catalysts	Ethylene + propylene	propylene	Ethylene	temperature operating	feed	References
SAPO-34	70.45	20.55	49.9	410⁰C	Methanol + water	[42]
SAPO-34	76.39	24.56	51.83	410⁰C	Methanol + water	[43]
Ni/SAPO-34	74	22	52	410⁰C	Methanol + water	[44]
Ni/SAPO-34	73	28	45	410⁰C	Methanol + water	[45]
Ni/SAPO-34	83.05	35.16	47.89	410⁰C	Methanol + water	In work

during this article, to check the effect of metal and its different methods in placing it within the composition of the SAPO-34 catalyst, Samples with different ratios of nickel-metal are going to be prepared and their performance within the methanol to olefin process is going to be examined. the utilization of nickel-metal within the synthesis of the SAPO-34 catalyst increases the precise expanse of the catalyst, creating strong acidic centers suitable for pure SAPO-34 and improving the catalyst's performance.
the employment of the ultrasonic method within the analysis of Ni/SAPO-34 has had excellent effects on the properties and performance of this catalyst within the process of methanol to olefin. The decreased growth of crystals and uniform distribution of particles within the catalyst structure have resulted Compared to the impregnation and hydrothermal method. Evaluating the performance of catalysts showed that catalysts produced by the ultrasound method have higher activity.
Sample S6 features a high crystallization percentage, also with the best extent and high acidity, it's the very best selectivity to light olefins. After that, sample S5, with alittle difference, creates the very best selectivity of sunshine olefins.
Sample S7, thanks to the rise in nickel content, despite the reduction in particle size, the presence of impurities within the catalyst structure reduces the crystallization percentage. And an excessive amount of acidity makes it less durable than other catalysts.
Sample S7, despite the pure catalyst structure, thanks to the massive crystal size and low acidity, it's very cheap selectivity compared to light olefins and a shorter lifetime.

S1 (SAPO- 34 pure)

S2 (Hydrothermal method and 2% nickel)

S3 (Impregnation method and 2% nickel )

S4 (Ultrasound method and 2% nickel)

S5 (Ultrasound method and 3% nickel)

S6 (Ultrasound method and 5% nickel )

S7 (Ultrasound method and 7% nickel )

OCT Olefins Conversion Technology

MTO Methanol to olefin

NH₃-TPD NH₃ temperature-programmed Desorption

WHSV weight hourly space velocity

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Department of Chemical Engineering, Arak Branch, Islamic Azad University, Arak, Iran

Young Researchers and Elite Club, Gachsaran Branch, Islamic Azad University, Gachsaran, Iran

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Ehsan kianfar

Department of Chemical Engineering, Arak Branch, Islamic Azad University, Arak, Iran

Young Researchers and Elite Club, Gachsaran Branch, Islamic Azad University, Gachsaran, Iran

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Synthesis and modification of Nickel /SAPO-34 Nanocatalyst for MTO Process via ultrasound and impregnation and hydrothermal methods

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Abstract

Figures

1. Introduction

2. Catalyst Preparation Ni/sapo-34

3. Results And Discussion

3.1. Investigate the surface area and size of the catalyst cavity (BET).

3.2. Temperature Programmed Desorption (TPD).

4. Catalyst Performance

5. Conclusions

Nomenclature

Declarations

References

Additional Declarations

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