SYNTHESIS OF NANO-NI BY LIQUID REDUCTION METHOD IN A

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SYNTHESIS OF NANO-NI BY LIQUID REDUCTION METHOD IN A COMBINED REACTOR OF ROTATING PACKED BED AND STIRRED TANK REACTOR Kun Dong, Yong Yang, Yong Luo, Liangliang Zhang, GuangWen Chu, Haikui Zou, Bao-Chang Sun, and Jian-Feng Chen Ind. Eng. Chem. Res., Just Accepted Manuscript • DOI: 10.1021/acs.iecr.7b04875 • Publication Date (Web): 28 Feb 2018 Downloaded from http://pubs.acs.org on March 1, 2018

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Industrial & Engineering Chemistry Research

SYNTHESIS OF NANO-NI BY LIQUID REDUCTION METHOD IN A COMBINED REACTOR OF ROTATING PACKED BED AND STIRRED TANK REACTOR

Kun Dong †,‡, Yong Yang§, Yong Luo§, Liangliang Zhang †,§, Guangwen Chu†,§, Haikui Zou†,§, Baochang Sun†,§*, Jianfeng Chen†,§ †

State Key Laboratory of Organic-Inorganic Composites, Beijing University of

Chemical Technology, Beijing 100029, China ‡

BUCT-CWRU International Joint Laboratory, College of Energy, Beijing University

of Chemical Technology, Beijing 100029, China §

Research Center of the Ministry of Education for High Gravity Engineering and

Technology, Beijing University of Chemical Technology, Beijing 100029, China

1

ACS Paragon Plus Environment

Industrial & Engineering Chemistry Research 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

ABSTRACT This work presented a novel process of nano-Ni preparation by liquid reduction method without surfactant in a combined reactor of rotating packed bed (RPB) and stirred tank reactor (STR). The reaction mechanism of this process was studied, and the effects of different operating conditions including rotation speed, NaBH4 concentration, liquid volumetric flow rate and liquid circulation time on the characteristics of the nano-Ni were systematically investigated in the RPB to control the morphology and average particle size of the prepared nano-Ni. The average particle size of the prepared nano-Ni can be adjusted from 42 to 130 nm by changing operating conditions, and the prepared nano-Ni with a face centered cubic (FCC) structure, an average particle size of 42 nm and a particle size distribution of 30-60 nm was obtained under the optimal operating conditions. This research provides a novel pathway and theoretical basis for controllable preparation production of nano-Ni. KEYWORDS:

nano-Ni; controllable preparation; liquid reduction method; rotating

packed bed

2


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1. INTRODUCTION Nano-Ni has been widely used for the industrial applications such as in catalysis, biosensors, photovoltaic technology, optoelectronics, information storage, etc. due to its excellent magnetic, catalytic properties and inexpensive.1-4 Therefore, research on its preparation has still intense interests. The preparation method of nano-nickel (nano-Ni) includes physical and chemical methods. Although there are some advantages including easy operating process and mass production for the physical methods, their applications usually exhibit high equipment and operating cost, and wide particle size distribution (PSD). While the chemical methods, including sol-gol,5 hydrothermal,6-7 microemulsion,8-11 liquid phase reduction,12-14 with advantages of easier controlling of PSD and low cost, have been received considerable attention in the recent times. Among the chemical methods, liquid phase reduction method is desired owing to its relatively low cost and environmentally benign nature.15,16 Generally, the studies on the preparation of nano-Ni by reduction method have been reported by many researches. Li Lei et al have investigated synthesis of nano-Ni using the nickel sulfate and hydrazine hydrate as raw materials and reductant respectively in a stirred reactor (STR), and the results showed that the average particle size of the prepared nano-Ni with face-centered cubic structure is about 400 nm.17 Yu Ying et al have explored the synthesis of nano-Ni by liquid reduction method in STR, and the results showed the prepared nano-Ni with particle size of 180 nm.18 Li Zhiyu

3



et al have studied the reaction kinetics of Ni2+ reduction by hydrazine in solution. The study indicated that the Ni2+ reduction process belongs to reaction precipitation process, which includes nucleation, crystal growth, coalescence and agglomeration in the liquid phase.19 The nucleation process with a fast nucleation rate required a fast micromixing process to achieve the homogeneous nucleation and control the crystal growth.20 However, the conventional reactor exhibits poor micromixing, easily resulting into wide PSD and difficult controlling of average particle size. It is therefore desirable to develop an innovation technique for controllable preparation of nano-Ni. A rotating packed bed (RPB) is a novel high gravity device, which can greatly enhance micromixing and mass transfer efficiency.21-29 Previous studies have shown that RPBs can yield nanoparticles with good morphology, small particle size and narrow particle size distribution.30 Also, it has been reported that the micromixing, which can be obtained in RPB, can greatly affect the nucleation process and has little effect on crystal growth in the reactive precipitation process, while a uniform crystal growth process can be obtained just in a macro homogeneous mixing state (STR).31 However, to the best of our knowledge, the application of RPB in the synthesis of nano-Ni is still scarce. This study therefore employed a combined reactor of RPB and STR in an attempt to prepare high quality nano-Ni particles without adding surfactant by liquid reduction method. The effects of different operating conditions such as rotation speed,

4


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NaBH4 concentration, liquid volumetric flow rate and liquid circulation time on the characteristic of the nano-Ni were systematically investigated in an attempt to obtain the effect law.

2. MECHANISM OF THE NANO-NI PREPARATION PROCESS During the liquid reduction process, the Ni2+ is reduced by hydrazine hydrate in the solution to prepare nano-Ni. The reaction between nickel sulfate and hydrazine hydrate can be written as: NiSO4 + nN2H4 = Ni(N2H4)nSO4 (n = 2,3)

(1)

Ni(N2H4)nSO4 + 2OH- = Ni(OH)2 + nN2H4 + SO42–

(2)

2Ni(OH)2 + N2H4 = 2Ni + N2 + 4H2O

(3)

The nickel sulfate firstly reacts with hydrazine hydrate to generate a complex compound (Ni(N2H4)nSO4), and then the complex, which is unstable, can form nickel hydroxide under the alkaline condition.32 The nickel hydroxide furtherly reacts with hydrazine hydrate to form nano-Ni. Therefore, it is difficult to generate Ni in this process, leading to an excessive N2H4 consumption without precipitating aid agent. While a small amount of NaBH4 was added into the above reaction system initially, Ni-B and Ni will be produced, and these two productions can catalyze the reaction between nickel sulfate and hydrazine hydrate to form Ni: NaBH4 + 4NiSO4 + 8NaOH = 4Ni↓ + NaBO2 + 4Na2SO4 + 6H2O

(4)

2NaBH4 + 4NiSO4 + 6NaOH = 2Ni2B↓ + 4Na2SO4 + 6H2O + H2↑

(5)

5



Therefore, the mixture of hydrazine hydrate and NaBH4 with a certain proportion was adopted as the reductant in this work. As mentioned in the introduction, although the nucleation process is fast in this process, but the yield of Ni particles is little in first 2 min (as shown in figure 1). Then the yield of nano-Ni was increased obviously with an increase of time from 4 to 10 min under the catalysis of Ni-B and Ni. While the reaction time is above 14 min, the yield has little change. Based on this, the reaction time of 15 min was adopted in this process. 100 90 80

nano-Ni yield (%)

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70 60 50 40 30 20 10 0

0

2

4

6

8

10

12

14

16

time (min)

Figure 1. Nano-Ni yield at different reaction time

3. EXPERIMENTAL SECTION 3.1. Materials and Procedure All chemical reagents used in this study were AR grade without further treatment. Nickel Sulfate Hexahydrate (A. R.) was purchased from Beijing Lark Prestige

6


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Science and technology Limited company while sodium borohydride (A. R.) was supplied by China National Biotec Group. Hydrazine hydrate was purchased from Beijing Quanta Hengyi technology co., whereas sodium hydroxide was purchased from Beijing Tong Guang chemical company. Alcohol (A. R.) was supplied by Beijing Tong Guang chemical company. And Deionized Water was used through all the experiments. The specifications of the used RPB in this work are given in Table 1. The liquid distributor of the RPB has a circular titanium alloy nozzle with a diameter of 3 mm to maintain a certain initial speed of the liquid flow. In order to maintain a certain high gravity level, the rotation speed was varied from 400 to 2800 rpm. In this process, the mixed reducing liquid was induced into the circulating solution containing Ni(SO4)2, and the schematic diagram of experimental setup is shown in Figure 2. The mixed reducing liquid (50 ml) comprised 4.8 M N2H4, 1 M NaOH and 0.06 M NaBH4 while the other solution (50 ml) contained 0.8 M Ni(SO4)2 (aq). Both solutions were introduced into the RPB through separate liquid inlets where they merged into a single stream and flowed to the outer edge of the rotor under the action of centrifugal force generated by the rotating packing. The exiting liquid stream was maintained under circulation at 6 ml/s between the RPB and a circulation tank (the liquid holdup in RPB and tank were about 0.5 ml and 99.5 ml respectively). After about 2-4 min of circulation time, the exiting liquid was released into a STR where the reaction continued for about 8-13 min after which the resultant mixture was filtered to obtain a

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precipitate. The precipitate was washed for several times by deionized water and alcohol successively, and then dried at 333 K for 4 h.

Table 1. Specifications of the RPB item

unit

value

inner radius of the packing, ri

mm

20

outer radius of the packing, ro

mm

45

axial length of the packing, h

mm

25

volume of the rotor, vb

mL

51

surface area of the dry packing per unit

m2/m3

812

packing material

stainless wire mesh

voidage of the dry packing, ε

m3/m3

8


0.85

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Figure 2. Schematic diagram of experimental setup (1) circulation tank (2) pump (3) reductant inlet (4) RPB (5) STR (6) packing (7) motor (8) temperature control system (9) pump

3.2. Characterization The as-prepared nano-Ni were characterized by X-ray diffraction (XRD) on a Siemens D500 diffractometer using Cu Kα radiation source (λ =0.154 nm) with graphite monochromator. The samples’ XRD patterns were collected at a scanning rate of 2o/min in the range of 5-90o. The size and morphology analyses of the prepared Ni particles were performed by transmission electron microscopy (TEM) using an H-800 electron microscope (Hitachi, Japan). The average particle size of nano-Ni was obtained by measuring more than 1000 particles in the TEM image of the product. The

surface

area

(SA)

of

the

Ni

particles

was

calculated

by

the

Brunauer-Emmett-Teller (BET) equation. The purity of the prepared nano-Ni was analyzed by X ray fluorescence and ion chromatography. The amount of the prepared nano-Ni was measured by the EDTA titration method. Also, the nano-Ni yield percentage is estimated in the following equation. nano-Ni yield =

actual mass of nano-Ni (g.ml-1 ) theoretically mass of nano-Ni (g.ml-1 )

9


× 100%


4. RESULTS AND DISCUSSIONS 4.1.Effect of Rotation Speed Figure 3 shows the effect of the rotation speed on the average particle size of the nano-Ni in the RPB. It was noted that the average particle size of the nano-Ni first gradually decreased from 96 to 53 nm with an increase in rotation speed from 800 to 2000 rpm, and thereafter increased with further increase in rotation speed. And there is a critical point at which the average particle size is minimal. In this process, a higher rotation speed in the RPB can obtain a better micromixing to achieve a higher level homogenous nucleation process and more crystal nucleus,31,33 resulting in a smaller particle size and narrower PSD. However, a further increase in rotation speed results in the change of morphology from multi-aspect spherical structure to the barbed sphere structure which is instability and easier to coalescence and grow, resulting in the increase of particle size, as shown in Figure 4. However, a further increase in rotation speed can leads to the decrease of liquid residence time in the packing (e.g. mixing time) and then the decrease of mixing effect, 34 resulting in the change of the crystal growth direction. Thus, a higher rotation speed may lead to the change of nano-Ni’s morphology and increase in average particle size of nano-Ni. The similar phenomenon has been also found in the preparation of nano-Ni in the STR and the preparation of other particle in STR.35,36

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Figure 3. Effect of rotation speed on the average particle size (NiSO4 concentration of 0.8 mol/L, NaOH concentration of 1 mol/L, NaBH4 concentration of 0.08 mol/L, reaction temperature of 80 oC, reactant molar ratio (N2H4:NiSO4) of 6:1, liquid volumetric flow rate of 6 ml/s, circulation time of 4 min)

(a) obtained at 2000 rpm

(b) obtained at 2800 rpm

Figure 4. TEM of the prepared nano-Ni at different rotation speed (a. 2000 rpm, b. 2800 rpm)

11



4.2. Effect of NaBH4 Concentration Figure 5 shows the effect of NaBH4 concentration on the average particle size of the nano-Ni. It was noted that the average particle size of the nano-Ni first gradually decreased from 203 to 45 nm with increase in NaBH4 concentration from 0 to 0.06 mol/L and then increased with further rise in NaBH4 concentration. As mentioned in the section 2, the products of Ni-B and Ni generated from the reaction between NaBH4 and NiSO4 can catalyze the reaction between NiSO4 and N2H4.19 This can intensify the nucleation process and form more crystal nucleus, leading to a smaller particle size in the RPB. In addition, it can be found that adding NaBH4 into the solution can make the nucleation of Ni easier than that without adding NaBH4. Therefore, it can be deduced that the Ni-B will be the main seed crystal at the beginning of the nucleation process. However, a further increase of NaBH4 concentration will lead to an easier formation of the secondary nucleation, resulting in producing the lager nanoparticle.

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Figure 5. Effect of NaBH4 concentration on the average particle size of nano-Ni (NiSO4 concentration of 0.8 mol/L, NaOH concentration of 1 mol/L, temperature of 80 oC, reactant molar ratio (N2H4:NiSO4) of 6:1, liquid volumetric flow rate of 6 ml/s, circulation time of 4 min, rotation speed of 2400 rpm)

4.3.Effect of Liquid Volumetric Flow Rate Figure 6 shows the effect of liquid volumetric flow rate on the average particle size of the nano-Ni. It was noted that the average particle size of the nano-Ni first decreased from 203 to 45 nm with increase in liquid volumetric flow rate from 2 to 6 ml/s and thereafter remained generally unchanged with further increase in liquid volumetric flow rate. The liquid turbulent degree, the relative velocity between liquid elements and the rotating packing and coalescence-redispersion frequency between droplets can be enhanced with an increase in the liquid volumetric flow rate, leading to a significant increase of micromixing effect in the RPB to form more nucleus.37 All of these results in the decrease of average particle size.

13



Figure 6. Effect of liquid volumetric flow rate on the average particle size of nano-Ni (NiSO4 concentration of 0.8 mol/L, NaOH concentration of 1 mol/L, NaBH4 concentration of 0.08 mol/L, temperature of 80 oC, reactant molar ratio (N2H4:NiSO4) of 6:1, circulation time on RPB of 4 min, rotation speed of RPB of 2400 rpm)

4.4.Effect of Circulation Time in the RPB Figure 7 shows the effect of liquid circulation time in the RPB on the average particle size of the nano-Ni. It was noted that the average particle size of the nano-Ni first decreased from 107 to 42 nm with increase in liquid circulation time in the RPB from 0 to 2 min and thereafter increased with further increase in liquid circulation time in the RPB. The increase of circulation time in the RPB will increase coalescence-redispersion times, and then intensify the micromixing effect in the RPB,34 which will increase the amount of generated nucleus, resulting in the decrease of average particle size.35 However, a further intensification of the micromixing effect caused by the further increase of circulation time, will leads to the easier formation of barbed sphere Ni (as shown in Figure 8), which is easier to coalescence and grow, resulting in the increase of particle size.

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Figure 7. Effect of circulation time in the RPB on the average particle size of nano-Ni (NiSO4 concentration of 0.8 mol/L, NaOH concentration of 1 mol/L, NaBH4 concentration of 0.08 mol/L, temperature of 80 oC, reactant molar ratio (N2H4:NiSO4) of 6:1, circulation time of 4 min, rotation speed of 2400 rpm, liquid volumetric flow rate = 6 ml/s)

(a) obtained at 2 min

(b) obtained at 6 min

Figure 8. TEM of the prepared nano-Ni at different circulation time

4.5. Characterization of the Prepared Nano-Ni The prepared nano-Ni in the RPB under the operating conditions of initial NiSO4 15



concentration of 0.8 mol/L, reactant molar ratio (N2H4:NiSO4) of 6:1, NaOH concentration of 1 mol/L, NaBH4 concentration of 0.06 mol/L, temperature of 80 oC, rotation speed of 2000 rpm, stirring speed of 2400 rpm, liquid volumetric flow rate of 6 ml/s and circulation time in the RPB of 2 min were characterized by XRD and TEM analyses. Figure 9 shows the XRD pattern of the prepared nano-Ni in the RPB. It was noted that the nano-Ni has three plane diffraction peaks, (111), (200), (220), indicating the nano-Ni has a face-centered cubic (FCC) structure. No other species were clearly observed in the XRD pattern, indicating that the purity of nano-Ni is high. The TEM image of the prepared nano-Ni, as shown in Figure 10, revealed that the nano-Ni is multi-aspect spherical structure and have an average particle size of about 42 nm. Meanwhile, it was found that the prepared nano-Ni exhibit a narrow particle size distribution of 30-60 nm, and the particles in the size distribution from 35 to 45 nm accounted for about 68%. The surface area (SA) of the prepared nano-Ni was found to be about 17.2 m2/g. Also, the composition of the prepared nano-Ni is shown in table 2. It can be seen that the purity of nano-Ni can reach about 99.677%. Compared to the nano-Ni prepared in the STR in the reference ,13 the average particle size of the nano-Ni prepared in this study is smaller and its PSD is narrower.

16


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(111)

Intensity

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60


(200) (220)

10

20

30

40 50 2θ (deg)

60

70

80

90

Figure 9. XRD pattern of nano-Ni.

Figure 10. TEM image of nano-Ni. Table 2. The composition of the prepared nano-Ni Composition

Ni

B

S

Fe

Al

Cr

Content (%)

99.677

0.073

0.098

0.059

0.076

0.017

The comparison of average particle size and PSD of nano-Ni prepared in SRT, combined reactor of RPB and SRT, and commercial product (supplied by Beijng 17



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Flance Technology & Trade Co. Ltd) is shown in the table 3. It can be seen that the nano-Ni with a smaller average particle size and narrower PSD was prepared in the combined reactor of RPB and STR relative to those prepared in STR only and commercial product. Table 3. Comparisons of average particle size and PSD of nano-Ni prepared by different process STR

RPB and STR

commercial product

Average particle size (nm)

107

42

70

PSD (nm)

70-150

30-60

30-110

5. CONCLUSION This work herein presents the preparation of nano-Ni by liquid reduction method without adding surfactant in a combined reactor of RPB and STR. The reaction mechanism and single factor experimental were studied to obtain the effect law during the synthesis process. The average particle size can be adjustable from 42 to 130 nm by changing operating conditions. Also, nano-Ni with an FCC structure, an average particle size of 42 nm and a particle size distribution of 30 - 60 nm was obtained under the optimal operating conditions of initial NiSO4 concentration of 0.8 mol/L, reactant molar ratio (N2H4:NiSO4) of 6:1, NaOH concentration of 1 mol/L, NaBH4 concentration of 0.06 mol/L, temperature 80 oC, rotation speed of 2000 rpm, stirring speed of 2400 rpm, liquid volumetric flow rate of 6 ml/s and circulation time of 2 min.

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This research provides a novel pathway and theoretical basis for controllable preparation of nano-Ni.

AUTHOR INFORMATION Corresponding Author * E-mail: [email protected] Notes The authors declare no competing financial interest

ACKNOWLEDGMENTS This work was supported by the National Natural Science Foundation of China (No. 2140060589, U1607114, 21606010).

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SYNTHESIS OF NANO-NI BY LIQUID REDUCTION METHOD IN A

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