CN111573621B - Method for preparing hydrogen by hydrolysis - Google Patents
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- CN111573621B CN111573621B CN202010506496.5A CN202010506496A CN111573621B CN 111573621 B CN111573621 B CN 111573621B CN 202010506496 A CN202010506496 A CN 202010506496A CN 111573621 B CN111573621 B CN 111573621B
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000001257 hydrogen Substances 0.000 title claims abstract description 67
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 67
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 56
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 15
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 22
- 230000007935 neutral effect Effects 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 33
- 238000000498 ball milling Methods 0.000 claims description 25
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 13
- 239000011780 sodium chloride Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 2
- 239000003575 carbonaceous material Substances 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000011777 magnesium Substances 0.000 abstract description 53
- 238000004519 manufacturing process Methods 0.000 abstract description 33
- 238000006243 chemical reaction Methods 0.000 abstract description 21
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000000446 fuel Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000010970 precious metal Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000012300 argon atmosphere Substances 0.000 description 14
- 230000035484 reaction time Effects 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 239000010419 fine particle Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- JQMFQLVAJGZSQS-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-N-(2-oxo-3H-1,3-benzoxazol-6-yl)acetamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)NC1=CC2=C(NC(O2)=O)C=C1 JQMFQLVAJGZSQS-UHFFFAOYSA-N 0.000 description 2
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910019440 Mg(OH) Inorganic materials 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- -1 but not limited to Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
- C01B3/08—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents with metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
- C01B3/065—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents from a hydride
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical Kinetics & Catalysis (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention provides a method for preparing hydrogen by hydrolysis, which utilizes water solution of neutral salt and Mg-Mg 2 NiH 4 The composite material is hydrolyzed to produce hydrogen. The present invention providesThe hydrolysis hydrogen production method improves the comprehensive hydrogen production performance of the magnesium-based composite material, particularly remarkably improves the hydrolysis kinetic performance, can directly react with the aqueous solution of neutral salt at normal temperature, can produce hydrogen in 20 seconds up to 845.1mL, has the conversion rate up to 94.7 percent and the maximum hydrogen production rate of 6391mL g ‑1 min ‑1 The device can realize rapid and real-time hydrogen production and real-time hydrogen supply, and is suitable for providing high-purity hydrogen sources for hydrogen consumption equipment such as hydrogen fuel cells and the like. Meanwhile, the hydrolysis hydrogen production method provided by the invention does not need precious metal elements, has the advantages of low raw material price, simple and convenient operation and high hydrogen production efficiency, and is beneficial to industrialization.
Description
The technical field is as follows:
the invention relates to the field of hydrogen production by hydrolysis, in particular to a method for producing hydrogen by hydrolysis of a magnesium-based composite material.
Background art:
in the field of new energy, hydrogen energy has the advantages of high calorific value, zero pollution, recyclability and the like, is considered to be the energy with the most potential to replace fossil fuels, and particularly, the development of hydrogen consumption equipment such as hydrogen fuel cells and the like puts more strict requirements on hydrogen production technology. The development of safe, efficient, cheap and rapid hydrogen production technology becomes a research hotspot. Among a plurality of hydrogen production technologies, the light metal for hydrogen production by hydrolysis is a research hotspot of scholars at home and abroad in recent years.
In light metal, metal magnesium is rich in resources, low in price, high in theoretical hydrogen production amount (921 mL/g), mild in reaction conditions, and environment-friendly in hydrolysis by-products, so that the method has great development potential and research value. But as the reaction proceeds, a dense passivation layer Mg (OH) is formed 2 The film is coated on the surface of the unreacted magnesium particles, so that water molecules are prevented from further diffusing into the particles, and the hydrolysis kinetic performance and the conversion rate are reduced sharply.
The current research aiming at the problems of the magnesium-based material mainly focuses on the introduction of additives to prepare the composite hydrolysis material.For example Huang et al (J.Power Sources 365 (2017) 273-281) report a Mg-10wt.% MoS 2 The hydrogen production amount in 1min of the composite hydrogen production agent is 759.1mL/g, and the maximum hydrogen production rate is 3258mL g -1 min -1 (ii) a Liu et al (Energy 68 (2014) 548-554) in Mg-LiBH 4 Introducing AlCl into the system 3 The hydrolysis kinetic performance of the material is enhanced; xiao et al (int.j. Hydrogen Energy 44 (2019) 1366-1373) introduce In to catalyze Mg hydrolysis during ball milling, and the conversion rate reaches 93.0% within 20 min. The relevant reports at home and abroad are summarized in a table 1, and the method is characterized in that the hydrolysis kinetic performance of magnesium is promoted on the premise of sacrificing the theoretical hydrogen production amount of a system. A more ideal scheme is how to obviously improve the hydrolysis kinetic performance of magnesium under the condition of not obviously reducing the theoretical hydrogen production amount of a system, and the method has very important research value and practical significance.
TABLE 1 comparison of hydrolysis Properties of different magnesium-based materials
a Volume of hydrogen obtained by 1g compound hydrogen production
The invention content is as follows:
the invention aims to provide a method for preparing hydrogen by hydrolysis aiming at the defects of the prior art. The hydrogen production method has the advantages of short reaction time, high hydrogen production amount, high hydrogen production rate, high efficiency, simplicity, no need of complex equipment and procedures, low cost, safety and environmental protection.
The technical scheme of the invention is as follows: a method for preparing hydrogen by hydrolysis comprises the following specific steps:
1) Weighing Mg and Mg 2 NiH 4 Mixing with grinding aid to obtain composite material, and ball milling to obtain Mg-Mg 2 NiH 4 Compounding a solid powder; wherein the Mg accounts for 80 to 98.8 percent of the total mass of the mechanical mixed composite material, and the Mg accounts for 2 NiH 4 0.2-15 percent of grinding aid and 1-5 percent of grinding aid;
2) Mixing the composite solid powder with water solution of neutral salt, and hydrolyzingShould be (Mg + 2H) 2 O→Mg(OH) 2 +H 2 ,Mg 2 NiH 4 +4H 2 O→2Mg(OH) 2 +Ni+4H 2 ) Hydrogen gas is produced.
Preferably, the ball mill used for the mechanical ball milling comprises a planetary ball mill; the ball milling is carried out in an inert atmosphere, including an argon atmosphere; grinding aids are carbon materials including, but not limited to, graphite; the ball mass ratio of the ball-milled material is 20-40; the rotating speed of the ball milling is 250-500 r/min; the ball milling time is 0.5-5 h.
Preferably, the aqueous solution of the neutral salt is NaCl solution, KCl solution or K 2 SO 4 Solution, etc., the mass concentration of the water solution of the neutral salt is 2 to 5 percent.
The mass-to-volume ratio of the composite solid powder to the aqueous solution of the neutral salt is preferably 1 (50-200) g/mL.
The temperature of the hydrolysis reaction is preferably 10 to 50 ℃.
Has the advantages that:
1) The invention provides a portable online hydrolysis hydrogen production method with low price and excellent performance, which has the advantages of short reaction time, high hydrogen production amount and high hydrogen production rate, wherein the hydrogen production amount can reach 845.1mL/g in 20 seconds, the conversion rate is 94.7%, and the maximum hydrogen production rate is 6391mL g -1 min -1 . It can be easily found through comparing the relevant research data at home and abroad in table 1 that the hydrolysis hydrogen production performance obtained by the hydrogen production method provided by the invention has significant competitive power internationally.
2) The prepared high-purity hydrogen can be directly introduced into other hydrogen consumption equipment such as a hydrogen fuel cell and the like without other processing, can be rapidly prepared anytime and anywhere as required, can be produced and used, and solves a plurality of problems in the hydrogen storage and transportation process.
Description of the drawings:
FIG. 1 is Mg-10wt.% Mg prepared in example 1 2 NiH 4 An XRD pattern of the composite material;
FIG. 2 is Mg-10wt.% Mg obtained in example 1 and comparative example 2 NiH 4 Composite material and without addition of Mg 2 NiH 4 3.5% by weight of Mg in a NaCl solution at 30 ℃;
FIG. 3 is Mg-10wt.% Mg from example 2 2 NiH 4 SEM backscattered electron imaging of the composite material;
FIG. 4 is Mg-10wt.% Mg from example 2 2 NiH 4 3.5% by weight of NaCl solution at 30 ℃ for the composite material;
FIG. 5 is Mg-10wt.% Mg from example 5 2 NiH 4 Graph of the hydrolysis kinetics of the composite in 3.5% NaCl solution at different temperatures (10 ℃ to 40 ℃);
FIG. 6 Mg-10wt.% Mg prepared in example 5 2 NiH 4 Arrhenius curve of composite material.
The specific implementation mode is as follows:
the technical solution of the present invention will be further described in detail with reference to the following specific embodiments and accompanying drawings, but the present invention is not limited thereto.
Example 1
In a glove box with 0.1MPa argon atmosphere, mg powder and Mg 2 NiH 4 Uniformly mixing the powder and graphite according to the mass ratio of 88; after the ball milling is finished, the materials are taken in an argon atmosphere glove box to obtain sample powder with fine particles (Mg is recorded in the Mg-10 wt.%) 2 NiH 4 ，t0.5)。
The XRD pattern of the sample powder obtained by ball milling is shown in FIG. 1, and it can be seen from FIG. 1 that the curves contain Mg and Mg in addition 2 NiH 4 Diffraction peaks, no diffraction peaks of MgO and other substances, evidence of Mg and Mg during ball milling 2 NiH 4 No chemical reaction occurred.
Taking 0.1g of sample powder and 20mL of NaCl solution with the mass concentration of 3.5% to perform hydrolysis reaction at the temperature of 30 ℃, wherein the reaction time is 2.5 minutes, hydrogen is released to be 784.3mL/g, and the conversion rate is 87.9%; hydrogen 748.9mL/g evolved in 1 minute with 83.9% conversion, and the hydrolysis kinetics curve for the first 1 minute is shown in FIG. 2, curve (a).
Comparative example
In a glove box with 0.1MPa of argon atmosphere, uniformly mixing Mg powder and graphite according to the mass ratio of 98; and (3) taking materials in an argon atmosphere glove box after the ball milling is finished, and obtaining sample powder (Mg, t 1) with fine particles.
Taking 0.1g of sample powder and 20mL of 3.5% NaCl solution to perform hydrolysis reaction at 30 ℃, wherein the reaction time is 35 minutes, the hydrogen is discharged by 610.2mL/g, and the conversion rate is 67.6%; 117.5mL/g of hydrogen evolved in 1 minute, the conversion was 13.0%, and the hydrolysis kinetic curve for the first 1 minute is shown in FIG. 2 as curve (b).
The hydrolysis kinetics curve of the hydrolysis reaction of the composite solid powder in the NaCl solution is shown in the curve (a) in fig. 2, and as can be seen from the curve (a) in fig. 2, the hydrolysis performance is very excellent; the Mg-10wt.% Mg compared to the hydrolysis of magnesium powder by ball milling for 1h (curve (b)) 2 NiH 4 The hydrolysis performance of the composite material is greatly improved.
Example 2
In a glove box with 0.1MPa argon atmosphere, mg powder and Mg 2 NiH 4 Uniformly mixing the powder and graphite according to the mass ratio of 88; after the ball milling is finished, the materials are taken in an argon atmosphere glove box to obtain sample powder with fine particles (Mg is recorded in percentage by weight of 10 wt.%) Mg 2 NiH 4 ，t3)。
The SEM back scattering electron image of the sample powder obtained by ball milling is shown in FIG. 3, and it can be seen from FIG. 3 that the bright small particles are Mg 2 NiH 4 The gray flakes are Mg and Mg 2 NiH 4 The particles are embedded in the surface of the Mg sheet.
Taking 0.1g of sample powder and 10mL of NaCl solution with the mass concentration of 3.5 percent at 30 DEG CThe hydrolysis reaction is carried out for 20 seconds, the hydrogen gas 845.1mL/g is discharged, the conversion rate is 94.7 percent, and the maximum hydrogen production rate is 6391mL g -1 min -1 . The hydrolysis kinetics curve is shown in the curve in fig. 4, and it can be seen from the curve in fig. 4 that the amount of hydrogen produced by hydrolysis and the kinetics are further improved.
Example 3
In a glove box with 0.1MPa argon atmosphere, adding Mg powder and Mg 2 NiH 4 Uniformly mixing the powder and graphite according to a mass ratio of 94.8; and (4) taking materials in an argon atmosphere glove box after the ball milling is finished, so as to obtain sample powder with fine particles.
0.1g of sample powder and 5mL of NaCl solution with the mass concentration of 2% are taken to carry out hydrolysis reaction at 30 ℃, the reaction time is 4 minutes, the hydrogen 766.8mL/g is released, the conversion rate is 87.6%, the hydrogen 460.4mL/g is released within 1 minute, and the conversion rate is 52.6%. Compared with pure magnesium, only trace Mg needs to be added 2 NiH 4 The hydrolysis kinetic performance of Mg can be obviously improved.
Example 4
In a glove box with 0.1MPa argon atmosphere, mg powder and Mg 2 NiH 4 Uniformly mixing the powder and graphite according to the mass ratio of 80; and (4) taking materials in an argon atmosphere glove box after the ball milling is finished, so as to obtain sample powder with fine particles.
Taking 0.1g of sample powder and 20mL of K with the mass concentration of 5% 2 SO 4 The solution is hydrolyzed at 30 ℃ for 50 seconds, hydrogen 757.6mL/g is released, and the conversion rate is 88.2%.
Example 5
In a glove box with 0.1MPa argon atmosphere, mg powder and Mg 2 NiH 4 Powder and graphite were mixed as in 88After uniformly mixing the components in the mass ratio of 2, putting the mixture into a ball-milling tank, putting the ball-milling tank into a high-energy planetary ball mill (QM-3 SP 2), alternately performing ball milling for 1 hour in an argon atmosphere at a ball-material ratio of 30; after the ball milling is finished, the materials are taken in an argon atmosphere glove box to obtain sample powder with fine particles (Mg is recorded in percentage by weight of 10 wt.%) Mg 2 NiH 4 ，t1)。
Taking 0.1g of sample powder and 10mL of NaCl solution with the mass concentration of 3.5 percent to carry out hydrolysis reaction at the temperature of 10 ℃,20 ℃, 30 ℃ and 40 ℃ respectively;
the hydrolysis reaction is carried out at the temperature of 10 ℃, the hydrolysis kinetic performance is excellent, the reaction time is 40 seconds, the hydrogen 830.3mL/g is released, and the conversion rate is 93.1%.
The hydrolysis reaction is carried out at the temperature of 20 ℃, the hydrolysis kinetic performance is excellent, the reaction time is 35 seconds, the hydrogen 834.9mL/g is released, and the conversion rate is 93.6%.
The hydrolysis reaction is carried out at the temperature of 30 ℃, the hydrolysis kinetic performance is excellent, the reaction time is 30 seconds, the hydrogen 832.8mL/g is released, and the conversion rate is 93.4%.
The hydrolysis reaction is carried out at the temperature of 40 ℃, the hydrolysis kinetic performance is excellent, the reaction time is 30 seconds, the released hydrogen is 850.2mL/g, and the conversion rate is 95.3 percent.
The hydrolysis kinetics curves of the hydrolysis reaction of the sample powder prepared in example 5 with the NaCl solution at 10 ℃,20 ℃, 30 ℃ and 40 ℃ are shown in the curves (a) to (d) of FIG. 5, respectively, and it is clear from the curves (a) to (d) of FIG. 5 that the hydrolysis kinetics performance is excellent; and Mg-10wt.% Mg 2 NiH 4 The hydrolysis performance of the composite material is further improved along with the improvement of the hydrolysis temperature.
The reaction activation energy of the hydrolysis system is calculated according to the Arrhenius equation, an Arrhenius curve is shown in FIG. 6, and as can be seen from FIG. 6, the reaction activation energy is only 19.8kJ/mol, which is remarkably reduced compared with pure magnesium, so that the hydrolysis hydrogen production method provided by the invention has the advantages of short reaction time, high hydrogen production quantity and high hydrogen production rate.
Claims (5)
1. A method for preparing hydrogen by hydrolysis comprises the following specific steps:
1) Weighing Mg and Mg 2 NiH 4 Mixing with grinding aid to obtain mixed composite material, and ball milling to obtain Mg-Mg 2 NiH 4 Compounding a solid powder; wherein the Mg accounts for 80 to 98.8 percent of the total mass of the mechanical mixed composite material, and the Mg accounts for 2 NiH 4 0.2-15 percent of grinding aid and 1-5 percent of grinding aid; wherein the grinding aid is a carbon material;
2) And mixing the composite solid powder with a water solution of neutral salt, and performing hydrolysis reaction to generate hydrogen.
2. The method of claim 1, wherein the mechanical ball milling is a planetary ball mill; the ball milling is carried out in an inert atmosphere; the mass ratio of ball materials subjected to ball milling is 20-40; the rotating speed of the ball milling is 250-500 r/min; the ball milling time is 0.5-5 h.
3. The method of claim 1, wherein the aqueous solution of neutral salt is NaCl solution, KCl solution or K 2 SO 4 The mass concentration of the solution and the water solution of neutral salt is 2-5%.
4. The method according to claim 1, wherein the feed liquid mass volume ratio of the composite solid powder to the neutral salt water solution is 1 (50-200) g/mL.
5. The method according to claim 1, wherein the temperature of the hydrolysis reaction is 10 to 50 ℃.
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