CN107640742B - Silicon-based efficient solid hydrogen production agent - Google Patents
Silicon-based efficient solid hydrogen production agent Download PDFInfo
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- CN107640742B CN107640742B CN201711141166.5A CN201711141166A CN107640742B CN 107640742 B CN107640742 B CN 107640742B CN 201711141166 A CN201711141166 A CN 201711141166A CN 107640742 B CN107640742 B CN 107640742B
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- 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
Abstract
A silicon-based efficient solid hydrogen production agent is prepared by cleaning and recovering sawdust mud generated during cutting of a silicon wafer by a diamond wire saw, mechanically mixing the recovered silicon powder with a certain proportion of special reaction auxiliary agents, molding into blocks, and packaging with a plastic film. The reaction auxiliary agent consists of one or more of sodium hydroxide, sodium chloride, calcium oxide and sodium ethoxide. The obtained hydrogen production agent can directly react with water to generate hydrogen, 0.3-0.6 liter of hydrogen can be produced by each gram of hydrogen production agent, and the maximum hydrogen production rate can be regulated and controlled along with the water addition proportion and the hydrogen production agent formula within the range of 0.1-0.5 liter/min. The products of the reaction are harmless silica and silicate. The hydrogen production agent can produce hydrogen immediately after being put into water, and can provide a convenient hydrogen source for hydrogen energy utilization.
Description
Technical Field
The invention belongs to the field of hydrogen energy, provides a solid hydrogen source convenient for storage and transportation for hydrogen energy utilization, and relates to a design and preparation method of an efficient solid hydrogen production agent.
Background
Hydrogen power generation is clean power with great complementary advantages to other new energy power such as solar photovoltaic and the like, but the development of hydrogen power generation is limited by the basic limitation that hydrogen is difficult to store and transport in large quantities. The high-pressure storage and transportation has great potential safety hazard and higher cost; various hydrogen storage material technologies have not yet achieved practical requirements so far; the high-efficiency solid hydrogen production agent can be conveniently stored and transported to a use site, and a large amount of rapid hydrogen production is provided for use, so that the high-efficiency solid hydrogen production agent can become a practical option for solving the difficult problem of hydrogen storage and transportation.
The conventional solid hydrogen production agent is an aluminum-based hydrogen production agent based on the reaction of aluminum and water to generate hydrogen, and has limited raw material sources and higher cost. The silicon-based hydrogen production agent based on the reaction of silicon and water to generate hydrogen can reduce the cost and expand the raw material range of the solid hydrogen production agent. Chenxin et al disclose a preparation method of silicon/alkali metal hydrogen production material (CN 107188123A); yi Tianchu et al disclose a preparation method of hydrogen production material based on magnesium-silicon, aluminum-silicon and zinc-silicon alloy (CN 107188124A). Both methods involve alloy preparation and high-temperature treatment requirements, the cost is high, and the hidden danger of passivating the hydrogen production material by high-temperature oxidation exists. Paul Brack et al reported an experimental study of hydrogen production from ferrosilicon (International Journal of Energy Research (2017, open access)), and showed that it was less efficient in producing hydrogen. Hsing-Yu Tuan et al reported a study of hydrogen production by reacting recycled silicon wafer-cutting sawdust powder with a potassium hydroxide solution and providing hydrogen production efficiency by adding silicic acid and sodium silicate (Journal of Materials Chemistry A, vol.4 (2016), 12921); they further disclose an apparatus for preparing a reaction solution, heating and reacting with silicon powder and water to produce hydrogen. This method can realize low-cost and high-efficiency hydrogen production, but has two problems in view of application requirements. 1. The system reacts to form a large amount of potassium silicate precipitates which are insoluble in water, and the potassium silicate precipitates are difficult to discharge from a reaction kettle in time and are not beneficial to large-scale continuous application; 2. the user needs to prepare the reaction solution each time, which is very inconvenient in many field applications.
Disclosure of Invention
The invention aims to provide a low-cost high-efficiency solid hydrogen production agent. The operation and the use are convenient, a large amount of hydrogen can be produced by putting the hydrogen into water, and heating is not needed; and a large amount of solid-phase precipitation products are not generated in the hydrogen production.
The invention is realized by the following technical scheme.
The invention relates to a silicon-based efficient solid hydrogen production agent, which comprises the following steps: cleaning and recovering silicon powder from sawdust mud generated by cutting a silicon wafer by a diamond wire saw, wherein the recovery method comprises the following steps of: 3-6, putting hydrofluoric acid aqueous solution with the concentration of 0.2-1.2 mol/L, stirring for 0.5-4 hours at 35-55 ℃, and then filtering and drying; and then stirring and cleaning the obtained powder in an organic solvent for 0.5-1 hour, filtering and drying to obtain the recovered silicon powder. The silicon powder and the reaction auxiliary agent are mechanically mixed, pressed into blocks and packaged to obtain the high-efficiency solid hydrogen production agent.
The content of the silicon powder is 20-80 percent by weight, and the rest is reaction auxiliary agent.
The reaction auxiliary agent is composed of one or more of sodium hydroxide, sodium chloride, calcium oxide and sodium ethoxide. The composition comprises the following components in percentage by mass: sodium hydroxide: sodium chloride: calcium oxide: sodium ethoxide = 40-100: 0 to 10:0 to 10:0 to 60.
The pressing block package is formed by pressing a metal mold under the pressure of 0.1-1.5 MPa and is immediately packaged by a plastic film.
The hydrogen production agent can rapidly generate oxidation-reduction reaction for replacing hydrogen in water with silicon after being put into water to generate hydrogen, and theoretically, at most two moles of hydrogen can be generated in each mole of silicon.
The hydrogen production rate can be regulated and controlled by the proportion of water added and the composition proportion of the hydrogen production agent per gram, and the maximum hydrogen production rate per gram of the hydrogen production agent is 0.1-0.5 liter/min. The hydrogen production agent does not need to heat water in advance to control water temperature, and has good hydrogen production effect in normal-temperature water. The hydrogen production of the reaction can be tracked and measured by a drainage method. Fig. 1 is a typical curve of hydrogen production amount of hydrogen production agents with different sodium hydroxide contents in normal temperature water obtained in a group of experiments along with time change. The accumulated maximum gas production rate of the hydrogen production agent and the gas production rate at each moment in the reaction process, including the maximum gas production rate can be measured and calculated by the curve.
Table 1 shows the gas production effect data of the high-efficiency solid hydrogen production agent with different compositions obtained by the method, including the maximum gas production rate and the maximum gas production rate. Under the condition of certain maximum gas production rate, the gas production rate is high, a large amount of gas can be supplied in a short time, and the gas production rate is low, so that the gas can be supplied for a long time in one-time charging application, and different application occasions are provided respectively.
Drawings
FIG. 1 is a curve showing the change of hydrogen production with time (sodium chloride content 1.5%, calcium oxide content 1.5%, and the balance silicon powder) of high-efficiency solid hydrogen production agents with different sodium hydroxide contents in normal temperature water.
Detailed Description
The present invention will be described in further detail with reference to examples. The adopted silicon wafer sawdust mud cut by the diamond wire saw comes from factory discharge materials, and the silicon content is higher than 80%; if not stated otherwise, all the chemical reagents and solvents used are chemically pure, with a purity of greater than 99%.
Example 1.
Taking 100 g of silicon wafer cutting sawdust mud, adding 400 ml of 0.2 mol/L hydrofluoric acid aqueous solution, stirring for 2 hours at 40 ℃, filtering and drying; and then stirring the obtained powder in ethanol for 0.5 hour, filtering and drying to obtain the recovered silicon powder. Taking 25 g of recycled silicon powder, mechanically mixing with 20 g of sodium hydroxide, 1 g of sodium chloride, 1 g of calcium oxide and 3 g of sodium ethoxide, and then pressing into blocks in a metal die under the pressure of 1.5 MPa to obtain the high-efficiency solid hydrogen production agent. The hydrogen production block is put into normal temperature (20 ℃) water with the mass 10 times of that of the hydrogen production block, the hydrogen production amount of the reaction is tracked and measured by a drainage method, and the hydrogen production effect is shown in table 1.
Example 2.
Taking 100 g of silicon wafer cutting sawdust mud, adding 400 ml of 0.7 mol/L hydrofluoric acid aqueous solution, stirring for 2 hours at 40 ℃, filtering and drying; and then stirring the obtained powder in ethanol for 0.5 hour, filtering and drying to obtain the recovered silicon powder. Taking 25 g of recycled silicon powder, mechanically mixing with 20 g of sodium hydroxide, 1 g of sodium chloride, 1 g of calcium oxide and 3 g of sodium ethoxide, and then pressing into blocks in a metal mold under the pressure of 1.5 MPa to obtain the high-efficiency solid hydrogen production agent. The hydrogen production block is put into normal temperature (20 ℃) water with the mass 10 times of that of the hydrogen production block, the hydrogen production amount of the reaction is tracked and measured by a drainage method, and the hydrogen production effect is shown in table 1.
Example 3.
Taking 100 g of silicon wafer cutting sawdust mud, adding 400 ml of 1.2 mol/L hydrofluoric acid aqueous solution, stirring for 2 hours at 40 ℃, filtering and drying; and then stirring the obtained powder in acetone for 0.5 hour, filtering and drying to obtain the recovered silicon powder. Taking 25 g of recycled silicon powder, mechanically mixing with 20 g of sodium hydroxide, 1 g of sodium chloride, 1 g of calcium oxide and 3 g of sodium ethoxide, and then pressing into blocks in a metal mold under the pressure of 1.5 MPa to obtain the high-efficiency solid hydrogen production agent. The hydrogen production agent block is put into normal temperature (20 ℃) water with the mass 10 times of that of the hydrogen production agent block, the hydrogen production amount of the reaction is tracked and measured by a drainage method, and the hydrogen production effect is listed in table 1.
Example 4.
Taking 100 g of silicon wafer cutting sawdust mud, adding 400 ml of 0.7 mol/L hydrofluoric acid aqueous solution, stirring for 2 hours at 40 ℃, filtering and drying; and then stirring the obtained powder in ethanol for 0.5 hour, filtering and drying to obtain the recovered silicon powder. Taking 25 g of recycled silicon powder, mechanically mixing with 10 g of sodium hydroxide, 1.5 g of sodium chloride, 1.5 g of calcium oxide and 12 g of sodium ethoxide, and then pressing into blocks in a metal die under the pressure of 1.5 MPa to obtain the high-efficiency solid hydrogen production agent. The hydrogen production block is put into normal temperature (20 ℃) water with the mass 10 times of that of the hydrogen production block, the hydrogen production amount of the reaction is tracked and measured by a drainage method, and the hydrogen production effect is shown in table 1.
Example 5.
Taking 100 g of silicon wafer cutting sawdust mud, adding 400 ml of 0.7 mol/L hydrofluoric acid aqueous solution, stirring for 2 hours at 40 ℃, filtering and drying; and then stirring the obtained powder in ethanol for 0.5 hour, filtering and drying to obtain the recovered silicon powder. Taking 25 g of recycled silicon powder, mechanically mixing with 22 g of sodium hydroxide, 1.5 g of sodium chloride and 1.5 g of calcium oxide, and then pressing the mixture into blocks in a metal mold under the pressure of 1.5 MPa to obtain the high-efficiency solid hydrogen production agent. The hydrogen production agent block is put into normal temperature (20 ℃) water with the mass 10 times of that of the hydrogen production agent block, the hydrogen production amount of the reaction is tracked and measured by a drainage method, and the hydrogen production effect is listed in table 1.
Example 6.
Taking 100 g of silicon wafer cutting sawdust mud, adding 400 ml of 0.7 mol/L hydrofluoric acid aqueous solution, stirring for 2 hours at 40 ℃, filtering and drying; and then stirring the obtained powder in ethanol for 0.5 hour, filtering and drying to obtain the recovered silicon powder. Taking 25 g of recycled silicon powder, mechanically mixing with 23.5 g of sodium hydroxide and 1.5 g of sodium chloride, and then pressing the mixture into blocks in a metal mold under the pressure of 1.5 MPa to obtain the high-efficiency solid hydrogen production agent. The hydrogen production block is put into normal temperature (20 ℃) water with the mass 10 times of that of the hydrogen production block, the hydrogen production amount of the reaction is tracked and measured by a drainage method, and the hydrogen production effect is shown in table 1.
Example 7.
Taking 100 g of silicon wafer cutting sawdust mud, adding 400 ml of 0.7 mol/L hydrofluoric acid aqueous solution, stirring for 2 hours at 40 ℃, filtering and drying; and then stirring the obtained powder in ethanol for 0.5 hour, filtering and drying to obtain the recovered silicon powder. Taking 25 g of recycled silicon powder, mechanically mixing the recycled silicon powder with 25 g of sodium hydroxide, and then pressing the mixture into blocks in a metal mold under the pressure of 1.5 MPa to obtain the high-efficiency solid hydrogen production agent. The hydrogen production block is put into normal temperature (20 ℃) water with the mass 10 times of that of the hydrogen production block, the hydrogen production amount of the reaction is tracked and measured by a drainage method, and the hydrogen production effect is shown in table 1.
Example 8.
Taking 100 g of silicon wafer cutting sawdust mud, adding 400 ml of 0.7 mol/L hydrofluoric acid aqueous solution, stirring for 2 hours at 40 ℃, filtering and drying; and then stirring the obtained powder in ethanol for 0.5 hour, filtering and drying to obtain the recovered silicon powder. And taking 12.5 g of the silicon powder, mechanically mixing the silicon powder with 40 g of sodium hydroxide, 2 g of sodium chloride, 2 g of calcium oxide and 6 g of sodium ethoxide, and pressing the mixture into blocks in a metal die under the pressure of 1.5 MPa to obtain the high-efficiency solid hydrogen production agent. The hydrogen production agent block is put into normal temperature (20 ℃) water with the mass 10 times of that of the hydrogen production agent block, the hydrogen production amount of the reaction is tracked and measured by a drainage method, and the hydrogen production effect is listed in table 1.
Example 9.
Taking 100 g of silicon wafer cutting sawdust mud, adding 400 ml of hydrofluoric acid water solution with the concentration of 0.7 mol/L, stirring for 2 hours at 40 ℃, filtering and drying; and then stirring the obtained powder in ethanol for 0.5 hour, filtering and drying to obtain the recovered silicon powder. And taking 20 g of silicon powder, mechanically mixing the silicon powder with 24 g of sodium hydroxide, 1.2 g of sodium chloride, 1.2 g of calcium oxide and 3.6 g of sodium ethoxide, and pressing the mixture into blocks in a metal mold under the pressure of 1.5 MPa to obtain the high-efficiency solid hydrogen production agent. The hydrogen production block is put into normal temperature (20 ℃) water with the mass 10 times of that of the hydrogen production block, the hydrogen production amount of the reaction is tracked and measured by a drainage method, and the hydrogen production effect is shown in table 1.
Example 10.
Taking 100 g of silicon wafer cutting sawdust mud, adding 400 ml of hydrofluoric acid water solution with the concentration of 0.7 mol/L, stirring for 2 hours at 40 ℃, filtering and drying; and then stirring the obtained powder in ethanol for 0.5 hour, filtering and drying to obtain the recovered silicon powder. And taking 40 g of the silicon powder, mechanically mixing the silicon powder with 8 g of sodium hydroxide, 0.4 g of sodium chloride, 0.4 g of calcium oxide and 1.2 g of sodium ethoxide, and pressing the mixture into blocks in a metal mold under the pressure of 1.5 MPa to obtain the high-efficiency solid hydrogen production agent. The hydrogen production block is put into normal temperature (20 ℃) water with the mass 10 times of that of the hydrogen production block, the hydrogen production amount of the reaction is tracked and measured by a drainage method, and the hydrogen production effect is shown in table 1.
Example 11.
Taking 100 g of silicon wafer cutting sawdust mud, adding 400 ml of 0.7 mol/L hydrofluoric acid aqueous solution, stirring for 2 hours at 40 ℃, filtering and drying; and then stirring the obtained powder in ethanol for 0.5 hour, filtering and drying to obtain the recovered silicon powder. And taking 20 g of silicon powder, mechanically mixing the silicon powder with 24 g of sodium hydroxide, 1.2 g of sodium chloride, 1.2 g of calcium oxide and 3.6 g of sodium ethoxide, and pressing the mixture into blocks in a metal mold under the pressure of 1.5 MPa to obtain the high-efficiency solid hydrogen production agent. The hydrogen production agent block is put into normal temperature (20 ℃) water with the mass 5 times of that of the hydrogen production agent block, the hydrogen production amount of the reaction is tracked and measured by a drainage method, and the hydrogen production effect is listed in table 1.
TABLE 1 gas generation capacity of high efficiency solid hydrogen production agents of different compositions prepared by the present invention
Note: naOH, naCl, caO and CHONa in the table represent, in order, chemically pure (purity > 99%) sodium hydroxide, sodium chloride, calcium oxide and sodium ethoxide.
Claims (1)
1. A silicon-based efficient solid hydrogen production agent is characterized by comprising the following steps: cleaning and recovering silicon powder from sawdust mud generated by cutting a silicon wafer by a diamond wire saw, wherein the recovery method comprises the following steps of: 3-6, putting hydrofluoric acid aqueous solution with the concentration of 0.2-1.2 mol/L, stirring for 0.5-4 hours at 35-55 ℃, and then filtering and drying; then, stirring and cleaning the obtained powder in an organic solvent for 0.5 to 1 hour, filtering and drying to obtain recycled silicon powder; mechanically mixing the silicon powder and a reaction auxiliary agent, and pressing and packaging;
the content of the silicon powder is 20-80 percent by weight, and the rest is reaction auxiliary agent;
the reaction auxiliary agent consists of sodium hydroxide, sodium chloride, calcium oxide and sodium ethoxide, wherein the weight ratio of the sodium hydroxide: sodium chloride: calcium oxide: the sodium ethoxide comprises the following components in percentage by mass: 80;
and the pressed block is packaged, is pressed and molded by a metal mold under the pressure of 1.5 MPa, and is immediately packaged by a plastic film.
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| CN114604826A (en) * | 2020-12-09 | 2022-06-10 | 中国科学院上海硅酸盐研究所 | Hydrogen production method based on fine silicon powder and sodium silicate |
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