CN115609000A - Preparation method of high-dispersion nickel nano dispersion liquid - Google Patents
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Abstract
The invention discloses a preparation method of a high-dispersion nickel nano dispersion liquid, which is characterized in that a weak reducing agent is compounded to reduce Ni salt into metal ions under a hydrothermal condition, the metal ions are highly dispersed in a solution under the action of a complexing agent and a compounded surfactant, and then the metal ions with proper particle size are screened through ions, so that the metal ions have uniform crystal grain size and excellent dispersion stability.
Description
Technical Field
The invention relates to the technical field of magnetic nano materials, in particular to a Ni magnetic material, and particularly relates to a preparation method of a high-dispersion, high-stability and high-uniformity nickel nano dispersion liquid, wherein the dispersion liquid is mainly used in the fields of electroplating and catalytic media and is used as an additive.
Technical Field
The preparation of nano powder with high purity, high uniformity and high chemical composition precision, and the solution and dispersion thereof are the prerequisite of nano material research. Nano metal is an important material in nano materials, and is increasingly widely applied together with dispersion liquid thereof.
Metal nanoparticles differ greatly from bulk materials in terms of grain size, surface to bulk atomic ratio, grain shape, etc., thus creating the special effects of nanomaterials: including small-scale effects, surface interface effects, quantum size effects, macroscopic quantum tunneling and mechanical properties, thermal properties, electrical properties (including piezoelectric effects, etc.), magnetic properties, etc.
CN 1513591A institute of Metal research, national academy of sciences of China, a nanometer metal powder dispersion and its preparation method, in weight ratio, this composite is by nanometer metal powder 5-80% of the average particle size under 150nm of primary particle, dispersant 0.3-18%, stabiliser 0.3-7%, dispersion medium of the surplus makes up; the preparation method comprises the steps of adding a dispersing agent into a dispersing medium, adding the nano metal powder and a stabilizing agent, dispersing for 15-60 minutes by using a high-speed dispersion machine at 600-3500rpm, and grinding the obtained nano metal powder dispersion liquid for 20 minutes-18 hours to prepare the nano metal powder dispersion liquid. The nano metal powder dispersion liquid of the invention is a dispersion liquid with high solid content and low viscosity, has good monodispersity and high stability, and can be widely applied to the fields of paint, printing ink, electronic industry and the like.
Similarly, CN 101015774A nano metal dispersion liquid and its preparation method provide a nano metal dispersion liquid and its preparation method, which are simple and convenient, and can be used for industrial production of high-purity, high-uniformity, and high-precision chemical composition nano metal dispersion liquid with high efficiency and low cost. The nano metal dispersion liquid has the advantages of high purity, high solid content, excellent conductivity, stable storage, good monodispersity, no agglomeration, no sedimentation and the like, can be widely applied to the fields of coatings, printing ink, electronic industry and the like, and also faces the same technical problem.
The invention discloses a controllable preparation method of multi-morphology iron-cobalt alloy magnetic nanoparticles with high saturation magnetic induction intensity, which belongs to the field of magnetic nanomaterial preparation, and is disclosed by CN 108723383A institute of metals of Chinese academy of sciences. According to the invention, hydrazine hydrate is used for reducing ferrous iron and cobalt under an alkaline condition at a certain temperature and time by using a hydrothermal method, and iron-cobalt nanoparticles with uniform components and structures and different morphologies can be obtained by controlling the amount of cyclohexane and PEG and other reaction conditions, especially the molar ratio of ferrous iron to cobalt. The method has the characteristics of rich raw material sources, simple process, lower reaction temperature, less energy consumption, environmental friendliness and the like. The nano particles can be used for preparing high-performance iron-cobalt-based composite soft magnetic materials, are suitable for various complex, miniaturized and multifunctional high-power soft magnetic devices, and have wide application prospects. Under the combined action of polyethylene glycol and cyclohexane, hydrazine hydrate is utilized to reduce Fe < 2+ > and Co < 2+ > in a salt solution of iron and cobalt under an alkaline condition by adopting a hydrothermal method, and due to the strong reducibility of the hydrazine hydrate, alloy particles of 170nm in example 1, 175nm in example 4, 550nm in example 5 and 600nm in example 6 are obtained, so that the particle size is obviously far beyond the nanometer range in practice (in a mesoscopic system, a system with the grain size range of 1 to 100nm is generally called a nanometer system).
CN 110655827A national institute of Chinese academy of sciences Qingdao bioenergy and Process research discloses a micron or nanometer liquid metal water-based dispersion and its preparation method, add liquid metal into soluble natural macromolecule dispersion, mix, ultrasonic cavitation of low temperature, get the uniform dispersed dispersion of particle size; wherein the soluble natural polymer dispersion liquid consists of soluble polymers and water-based solution; wherein the soluble polymer is one or more of Sodium Alginate (SA), hyaluronic Acid (HA), sodium carboxymethylcellulose (CMC), and quaternized chitosan (Qch). The liquid metal dispersion liquid prepared by the method has the characteristics of high preparation efficiency, adjustable particle size, stable dispersion, long-term storage, high biocompatibility and the like, but the direct method is only limited to liquid metals with the melting point within the range of 0-100 ℃, such as gallium (Ga), indium (In), mercury (Hg) or alloys of the metals.
Disclosure of Invention
Based on the technical problems in the prior art, the invention provides the nano-particles which are simple to operate and low in cost, have adjustable sizes and are obtained by a hydrothermal method, and the nano-particles are highly dispersed in a solution, are stored for a long time and are convenient for industrial production.
A preparation method of high-dispersion nickel nano dispersion liquid comprises the following preparation methods:
(1) Taking dipropylene glycol and glucose as reducing agents, and sequentially adding the reducing agents into deionized water at normal temperature;
(2) Adding 2-mercaptothiazole complexing agent, P123 and fatty alcohol acyl sodium sulfate AES surfactant into the solution obtained in the step (1) in sequence, and reacting with 40-50 o C, magnetically stirring at 150-200rpm for 10-15min, standing, cooling to normal temperature, adding ammonia water to regulate pH value,
(3) And slowly adding nickel salt into the solution to obtain the nickel nano dispersion liquid precursor.
(4) Placing the precursor solution in a Teflon hydrothermal reaction kettle, sealing the reaction kettle, evacuating nitrogen, and performing vacuum distillation at 30 deg.C o Stirring for 5-10min under C, closing nitrogen valve, and heating to 105-110 deg.C o And C, continuously stirring, fully reacting for 12-15h, and naturally cooling to room temperature.
(5) Pouring out the hydrothermal reaction solution, carrying out primary centrifugal separation, taking the upper solution of the solution, discarding the lower solution, carrying out secondary centrifugal separation, and taking the lower solution of the solution, wherein the lower solution of the secondary centrifugal separation is the high-dispersion nickel nano dispersion solution.
Further, 50-60ml of dipropylene glycol is used in the step (1); 3-5g of glucose and 20-30ml of deionized water.
Further, 1-1.2g of 2-mercaptothiazole in the step (2); 0.1-0.15g of P123; sodium fatty alcohol acyl sulfate AES 0.05-0.1g.
Further, the pH value in the step (2) is 7.5-7.8
Further, 0.8g to 0.9g of nickel salt is used in the step (3).
Further, the temperature rise of the step (4) is increased to 105-110 o The time of C is 20-30min.
Further, the primary centrifugation parameters of step (5): 2500rpm,4-5min; secondary centrifugal separation parameters: 6000rpm,1-2min;
furthermore, the elementary substance size of Ni obtained from the nano dispersion liquid is 20-40nm.
Further, the high-dispersion nickel nano dispersion liquid has a stable time of more than 90 days at normal temperature and normal pressure.
Further, the dispersion is used in an electroplating solution as metal particles.
The preparation process of the present invention is explained as follows:
(1) According to the invention, dipropylene glycol and glucose are used as a compound reducing agent, in the prior art, reduction is usually carried out by strong reducing property such as hydrazine hydrate, the stronger the reducing property of the reducing agent is, the faster the metal ions are reduced in a solution, and finally, metal particles are larger and agglomerate or take a non-directional growth shape, so that 50-60ml of dipropylene glycol is reduced by adopting dipropylene glycol and glucose; 3-5g of glucose, under the normal temperature condition, the reducibility of the reducing agent is too weak, and is insufficient to reduce metal salt, so that the invention adopts a hydrothermal condition, pure hydroxyl and aldehyde group of glucose can present obvious reducibility under the hydrothermal condition, and are slowly and uniformly reduced and nucleated to aggregate into nano metal, and in addition, the reduction effect of the compounded dipropylene glycol and glucose is greater than that of the dipropylene glycol used alone.
(2) Regarding the solvent, 50-60ml of dipropylene glycol and 20-30ml of deionized water are used, i.e. the main solvent is dipropylene glycol, and theoretically the effect of using pure dipropylene glycol is best, but since glucose, a complexing agent and a surfactant are required to be added subsequently, the viscosity of the solution is too high, the centrifugal effect is extremely poor during subsequent centrifugal separation, and therefore, a proper amount of water needs to be added to balance the viscosity of the solution, so as to improve the separation effect.
(3) Regarding ammonia and pH: the pH value is adjusted by adding ammonia water, and the pH value is 7.5-7.8.
In a hydrothermal process, the following reactions may occur
CH 2 OH-(CHOH) 4 -CHO+Ni 2+ +2OH - →CH 2 OH-(CHOH) 4 -COOH+Ni↓+H 2 O, if added with a transitional OH-, under high pH conditions, shifts the equilibrium significantly to the right, accelerating the formation of Ni, and, in addition, at high pH, ni 2+ Oxidation with OH-to form nickelThis is not a requirement of the present invention.
(4) With respect to the complexing agent(s),
in the above process, if the 2-mercaptothiazole complexing agent (M) is added, the reduction process becomes
CH 2 OH-(CHOH) 4 -CHO+M(Ni) 2+ +2OH - →CH 2 OH-(CHOH) 4 -COOH+M+Ni↓+H 2 O
The N atom and the S atom in the polar amino group in the 2-mercaptothiazole have lone pair electrons, and can form covalent bonds with nickel ions to form nickel complex ions, so that the alleged rate of silver particles is effectively controlled.
(4) With respect to the temperature: hydrothermal temperature of 105-110 deg.c o C, the hydrothermal temperature is not too high, the reduction carbonization reaction is avoided, in addition, the generated metal atoms are more, the hydrothermal reaction temperature is high, the Brownian motion is violent, the growth of the crystal is more random, and the crystal growth is caused by the facts that the hydrothermal temperature is not too high, and the reduction carbonization reaction is avoided
This does not result in a single shaped metal particle. Specific hydrothermal ceiling, not material to the present invention, is 105-110 o C does not cause any carbonization reaction, and the metal particles are uniform and do not affect the purity of the dispersion, and is a preferred temperature.
(5) With respect to the surfactant: p123 and fatty alcohol acyl sodium sulfate, as known by technicians in the field, when metal ions are reduced by dipropylene glycol and glucose to obtain metal crystal nuclei, the crystal nuclei grow slowly, because the surface energy of the just-generated metal particles is extremely high and has extremely strong adsorption performance, the same metal ions can be adsorbed and agglomerated, the surfactant has strong adsorption capacity, the generated metal particles and the surfactant have mutual competitive reaction and are preferentially adsorbed by the surfactant, and the surfactant P123 is 0.1-0.15g; 0.05-0.1g of fatty alcohol sodium acyl sulfate AES, the concentration cannot be too low, if the concentration of the surfactant is too low, the competition reaction can be deviated, namely when the surfactant is completely coated on the surface of the metal ion, due to the low concentration of the surfactant, the metal is reasonable, the surfactant is not adsorbed in a certain direction, other metal particles with higher surface energy are adsorbed, and the metal particles grow into nanowires or nanorods, so that the phenomenon similar to that in CN201810411717 is a linear structure.
If the amount of the surfactant used is excessive, the solution may be significantly bubbled, especially, fine bubbles may be present, which is disadvantageous to uniform reduction of metal ions.
The compound nonionic surfactant and the anionic surfactant are compounded, so that the surface tension of the solution is improved, the use amount of the surfactant is reduced, and the formation of bubbles caused by excessive use is avoided.
If example 2 is taken as the standard, the difference is that no surface activity is added, the obtained nickel metal can be 1-20 microns in size, is agglomerated and settled, has no suspension capacity, and the obtained solution has low transparency.
(6) Regarding nitrogen evacuation: sealing the reaction kettle, evacuating nitrogen gas at 30 DEG o C, stirring for 5-10min, closing a nitrogen valve, and introducing air inevitably in the solution preparation process, wherein the air is inevitably exhausted in time, so that the tiny metal particles and oxygen are easily oxidized on the surfaces of the metal particles with high surface activity particularly under the hydrothermal condition, and the emptying operation can relieve the oxidation of the metal ions to a certain extent.
(7) Regarding centrifugation: in the hydrothermal process, as the reaction solution contains part of water, and nitrogen cannot be completely exhausted to remove air in the liquid, oxidation of metal nickel can be inevitably generated, so that metal oxide is formed, after hydrothermal reaction of the metal oxide is finished, a little black and green deposit can be found at the bottom of the hydrothermal reaction kettle, besides the oxide, some agglomerated metal particles exist, the particles are nanowires or nanorods or amorphous state, centrifugal separation is needed for 2500rpm for one time and 4-5min, the upper solution of the solution is taken, the lower solution is discarded, namely one-time centrifugation is carried out, and the discarded lower solution mainly contains nickel oxide and agglomerated metal particles.
And (3) secondary centrifugation: secondary centrifugal separation parameters: 6000rpm,1-2min; the method mainly aims to screen nickel metal with a proper particle size, the size of the metal particle size which is not subjected to secondary screening is 1-40nm, solution stability is not facilitated for some excessively fine metal particles, and the surface activity energy of the fine nano metal is very high, so that fine and macroscopic sediments exist in the dispersion liquid which is not subjected to secondary separation for 50-60 days at normal temperature and normal pressure.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, a weak reducing agent is compounded to reduce Ni salt into metal ions under a hydrothermal condition, and the metal ions are highly dispersed in a solution under the action of a complexing agent and a compounded surfactant.
2. The invention obtains nickel metal particles with uniform size by secondary centrifugation.
3. The nickel metal particle dispersion liquid obtained by the invention has excellent stability.
4. The reaction condition has no strong alkali, the process is simple, and the obtained dispersion can be used in the fields of magnetic recording material, catalytic material and electroplating material.
Drawings
FIG. 1 is an optical picture of a highly dispersed nickel nanodispersion prepared according to the present invention.
Fig. 2 is a TEM image of metal ions in the highly dispersed nickel nanodispersion of the present invention.
FIG. 3 is a [111] lattice HR-TEM image of a nickel metal of the present invention.
Fig. 4 is an SEM image of the highly dispersed nickel nanoparticles of the present invention.
Fig. 5 is a size distribution diagram of the highly dispersed nickel nanoparticles of the present invention.
Detailed Description
Example 1
A preparation method of high-dispersion nickel nano dispersion liquid comprises the following preparation methods:
(1) 50ml of dipropylene glycol and 3g of glucose are used as reducing agents, and 20ml of deionized water is sequentially added into the reducing agents at normal temperature.
(2) Adding 1g of 2-mercaptothiazole complexing agent, 0.1g of P123 and 0.05g of fatty alcohol sodium acyl sulfate AES surfactant into the solution obtained in the step (1) in sequence, and mixing with 40 g of o And C, magnetically stirring at 150rpm for 10min, standing, cooling to normal temperature, and adding ammonia water to adjust the pH value to 7.5.
(3) 0.8g of nickel salt was slowly added to the above solution to obtain a nickel nanodispersion precursor solution.
(4) Placing the precursor solution in a Teflon hydrothermal reaction kettle, sealing the reaction kettle, evacuating nitrogen, and performing vacuum distillation at 30 DEG o Stirring for 5min under C, closing nitrogen valve, and rising to 105 in 20min o And C, continuously stirring, fully reacting for 12 hours, and naturally cooling to room temperature.
(5) Pouring out the hydrothermal reaction solution, and performing primary centrifugal separation: 2500rpm,4min, taking solution supernatant, abandoning supernatant, performing secondary centrifugal separation: 6000rpm,1min, and taking the solution lower liquid, wherein the lower liquid of the secondary centrifugal separation is the high-dispersion nickel nano dispersion liquid.
Example 2
A preparation method of high-dispersion nickel nano dispersion liquid comprises the following preparation methods:
(1) 55ml of dipropylene glycol and 4g of glucose are taken as reducing agents, and 25ml of deionized water is sequentially added into the reducing agents at normal temperature.
(2) Adding 1.1g of 2-mercaptothiazole complexing agent, 0.125g of P123 and 0.075g of fatty alcohol sodium acyl sulfate AES surfactant into the solution in the step (1) in sequence, and mixing with 45 g of o And C, magnetically stirring at 200rpm for 12.5min, standing and cooling to normal temperature, and adding ammonia water to adjust the pH value to 7.7.
(3) 0.85g of nickel salt was slowly added to the above solution to obtain a nickel nanodispersion precursor solution.
(4) Placing the precursor solution in a Teflon hydrothermal reaction kettle, sealing the reaction kettle, evacuating nitrogen, and performing vacuum distillation at 30 DEG o Stirring for 5-10min under C, closing nitrogen valve, and increasing to 108 in 25min o C, continuing stirring and filling
The reaction is carried out for 14h, and the reaction product is naturally cooled to room temperature.
(5) Pouring out the hydrothermal reaction solution, and performing primary centrifugal separation: 2500rpm,4.5min, getting the upper solution of the solution, discarding the lower solution, performing secondary centrifugal separation: 6000rpm,1.2min, taking the solution underflow, wherein the underflow obtained after the secondary centrifugal separation is the high-dispersion nickel nano dispersion liquid.
Example 3
1. A preparation method of high-dispersion nickel nano dispersion liquid comprises the following preparation methods:
(1) 60ml of dipropylene glycol and 5g of glucose are taken as reducing agents, and 30ml of deionized water is sequentially added into the reducing agents at normal temperature.
(2) Adding 1.2g of 2-mercaptothiazole complexing agent, 0.15g of P123 and 0.1g of fatty alcohol acyl sodium sulfate AES surfactant into the solution in the step (1) in sequence, and mixing with 50 o And C, magnetically stirring at 200rpm for 15min, standing, cooling to the normal temperature, and adding ammonia water to adjust the pH value to 7.8.
(3) 0.9g of nickel salt was slowly added to the above solution to obtain a nickel nanodispersion precursor solution.
(4) Placing the precursor solution in a Teflon hydrothermal reaction kettle, sealing the reaction kettle, evacuating nitrogen, and performing vacuum distillation at 30 DEG o Stirring for 10min under C, closing nitrogen valve, and increasing to 110 in 30min o And C, continuously stirring, fully reacting for 15 hours, and naturally cooling to room temperature.
(5) Pouring out the hydrothermal reaction solution, and performing primary centrifugal separation: 2500rpm, 5min, taking the supernatant of the solution, discarding the supernatant, performing secondary centrifugal separation: and (4) taking the solution underflow after 2min at 6000rpm, wherein the underflow obtained after the secondary centrifugal separation is the high-dispersion nickel nano dispersion liquid.
As shown in FIG. 1, the highly dispersed nickel nanoparticles obtained by the invention are highly dispersed in the solution, and the transparency of the solution is extremely strong.
As shown in fig. 2 and 3, the nickel nanoparticles are highly dispersed, and the crystal lattice is shown as the [111] crystal plane of nickel, with a lattice spacing of 0.204nm.
As shown in figure 4, the particles have a spherical structure, uniform size and no agglomeration, and as shown in figure 5, the size is intensively distributed at 20-40nm.
Finally, it should be noted that the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A preparation method of high-dispersion nickel nano dispersion liquid is characterized by comprising the following preparation methods:
(1) Taking dipropylene glycol and glucose as reducing agents, and sequentially adding the reducing agents into deionized water at normal temperature;
(2) Adding 2-mercaptothiazole complexing agent, P123 and fatty alcohol acyl sodium sulfate AES surfactant into the solution obtained in the step (1) in sequence, and reacting with 40-50 o C, magnetically stirring at 150-200rpm for 10-15min, standing, cooling to normal temperature, adding ammonia water to adjust pH value,
(3) Slowly adding nickel salt into the solution to obtain a nickel nano dispersion liquid precursor;
(4) Placing the precursor solution in a Teflon hydrothermal reaction kettle, sealing the reaction kettle, evacuating nitrogen, and performing vacuum distillation at 30 DEG o Stirring for 5-10min under C, closing nitrogen valve, and heating to 105-110 deg.C o C, continuously stirring, fully reacting for 12-15h, and naturally cooling to room temperature;
(5) Pouring out the hydrothermal reaction solution, carrying out primary centrifugal separation, taking the upper solution of the solution, discarding the lower solution, carrying out secondary centrifugal separation, and taking the lower solution of the solution, wherein the lower solution of the secondary centrifugal separation is the high-dispersion nickel nano dispersion solution.
2. The method for preparing a highly dispersed nickel nanodispersion as claimed in claim 1, wherein in the step (1), 50-60ml of dipropylene glycol; 3-5g of glucose and 20-30ml of deionized water.
3. The method for preparing a highly dispersed nickel nanodispersion as claimed in claim 1, wherein the 2-mercaptothiazole in the step (2) is 1-1.2g; 0.1-0.15g of P123; sodium fatty alcohol acyl sulfate AES 0.05-0.1g.
4. The method for preparing a highly dispersed nickel nanodispersion as claimed in claim 1, wherein the pH in the step (2) is 7.5-7.8.
5. The method for preparing a highly dispersed nickel nanodispersion as claimed in claim 1, wherein the nickel salt is used in an amount of 0.8g to 0.9g in the step (3).
6. The method for preparing a highly dispersed nickel nano-dispersion according to claim 1, wherein the temperature of step (4) is raised to 105 to 110% o The time of C is 20-30min.
7. The method for preparing a highly dispersed nickel nanodispersion as claimed in claim 1, wherein the primary centrifugation parameter of the step (5): 2500rpm,4-5min; secondary centrifugal separation parameters: 6000rpm,1-2min.
8. The method for preparing a highly dispersed nickel nanodispersion as claimed in claim 1, wherein the size of Ni element obtained in the nanodispersion is 20-40nm.
9. The method of claim 1, wherein the highly dispersed nickel nanodispersion has a stabilization time of greater than 90 days at room temperature and pressure.
10. The method for preparing a highly dispersed nickel nano-dispersion according to claims 1 to 8, wherein the dispersion is used in an electroplating solution as metal particles.
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