CN114604826A - Hydrogen production method based on fine silicon powder and sodium silicate - Google Patents
Hydrogen production method based on fine silicon powder and sodium silicate Download PDFInfo
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- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 79
- 239000001257 hydrogen Substances 0.000 title claims abstract description 78
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000011863 silicon-based powder Substances 0.000 title claims abstract description 60
- 229910052911 sodium silicate Inorganic materials 0.000 title claims abstract description 45
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 42
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000004115 Sodium Silicate Substances 0.000 title claims abstract description 40
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000003756 stirring Methods 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 229910001868 water Inorganic materials 0.000 claims abstract description 17
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims description 65
- 239000000243 solution Substances 0.000 claims description 48
- 238000000034 method Methods 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 239000011734 sodium Substances 0.000 claims description 12
- 229910020489 SiO3 Inorganic materials 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 5
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000000843 powder Substances 0.000 description 19
- 229910003243 Na2SiO3·9H2O Inorganic materials 0.000 description 15
- PHIQPXBZDGYJOG-UHFFFAOYSA-N sodium silicate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-][Si]([O-])=O PHIQPXBZDGYJOG-UHFFFAOYSA-N 0.000 description 13
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 8
- 238000003760 magnetic stirring Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000003345 natural gas Substances 0.000 description 5
- 239000003245 coal Substances 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000003034 coal gas Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- -1 fossil fuel-chemical Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000000629 steam reforming Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Classifications
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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
Abstract
The invention relates to a hydrogen production method based on fine silicon powder and sodium silicate. The hydrogen production method comprises the following steps: mixing Na2SiO3·9H2Dissolving O in water to prepare a sodium silicate aqueous solution; and mixing and stirring the obtained sodium silicate aqueous solution and the silicon powder, and starting to react to form hydrogen.
Description
Technical Field
The invention relates to a clean hydrogen production method based on fine silicon powder and sodium silicate, and belongs to the field of hydrogen preparation.
Background
Hydrogen is a clean secondary energy with high energy density, and is studied by a large number of researchers in countries around the world. The preparation of hydrogen is an important technical link for utilizing hydrogen. There are a variety of methods for producing hydrogen, including: fossil fuel-chemical, biological, electrolytic, photocatalytic, and alkaline catalytic methods.
In industry, fossil fuels such as coal and natural gas are used as hydrogen production raw materials, so that the method has the characteristics of economy, easiness in large-scale production and the like, and occupies a leading position in the hydrogen industry at present. The specific flow of the coal gasification hydrogen production is that coal is gasified at high temperature to prepare coal gas (the main component is H)2CO, etc.) then at highReacting CO and H under warm conditions2O reaction, impurity gas CO in the product2、SO2And reaction and removal are carried out in subsequent processes, and finally, hydrogen with different purities is prepared through purification processes with different degrees. Coal is dominant in energy structures in China, and largely determines the main position of coal gasification hydrogen production in the hydrogen production industry, but the method has large investment, large water consumption and serious pollution, and is not suitable for operation under the current economic and green industrial large background. The hydrogen production by natural gas is a widely adopted hydrogen production method in North America, middle east and other regions. The main technology comprises a steam reforming method, a partial oxidation method and a catalytic cracking method, and the principle is that natural gas reacts with water vapor or oxygen in the presence of a catalyst to be converted into hydrogen. The reaction process needs to be carried out under the high-temperature condition of special equipment, the investment is large, the energy consumption is high, and the method is not suitable for running under the industrial background of deficient natural gas resources in China.
The water electrolysis hydrogen production method is commonly used for preparing high-purity hydrogen, and the principle is that water molecules are subjected to decomposition reaction on an electrode electrified with direct current, and hydrogen is generated on a cathode electrode. The energy utilization rate of the hydrogen production process by water electrolysis is about 80%, the equipment is simple, the process is clean, but the electric quantity consumption is large, and the reaction rate is limited by the surface area of an electrolysis electrode, so that the method is not suitable for preparing hydrogen in large quantity.
The solar cell is a reliable and environment-friendly energy acquisition technology, mainly based on a semiconductor material silicon wafer, and the annual market demand is about tens of thousands of tons. However, more than about 40% of silicon powder is generated during the sawing process for slicing single crystal or polycrystalline silicon ingots into wafers, and with the continuous development of the solar cell industry, the recycling or reusing of waste silicon is very important.
Therefore, in order to solve the technical problems in the industry, a hydrogen production method with simple preparation process, no pollution and high efficiency is needed.
Disclosure of Invention
In order to solve the problem that a large amount of waste silicon is generated in the solar cell industry, the invention provides a clean hydrogen production method based on fine silicon powder and sodium silicate, which comprises the following steps:
mixing Na2SiO3·9H2Dissolving O in water to prepare a sodium silicate aqueous solution; and mixing and stirring the obtained sodium silicate aqueous solution and the silicon powder, and starting to react to form hydrogen.
In the invention, sodium silicate solution with specific concentration is used as reaction solvent and catalyst, and the catalytic action of sodium silicate is utilized to promote the reaction of fine silicon powder and water to prepare hydrogen. The hydrogen production method does not involve adopting coal gas or natural gas, and the whole process is carried out at room temperature, the hydrogen production yield can reach 98.22 percent of the theoretical yield, and the reaction rate can reach 1.72 multiplied by 10-4gH2/(s·gSi) The reaction by-product is amorphous SiO2And the preparation process is green and pollution-free. The reaction equation is as follows:
and (3) hydrolysis process:
the reaction process comprises the following steps: si + (4-n) H2O+nOH-→SiOn(OH)4-n n-+2H2↑
When Na is present2SiO3·9H2The molar ratio of the O powder to the Si powder is more than 2:1, the exothermic heat of reaction is reduced, the system temperature is low, resulting in a low reaction rate and a low degree of reaction progress. When Na is present2SiO3·9H2The molar ratio of the O powder to the Si powder is less than 1:2, the exothermic quantity of the reaction is increased, the temperature of the system is high, and the reaction rate is high; however, since the reaction is continuously carried out, OH generated by hydrolysis in the system-Is continuously consumed, Si (OH)4The solution is accumulated continuously, the pH value of the solution is reduced continuously, and the silicon powder cannot be completely reacted, so that the yield is reduced.
Preferably, Na in the sodium silicate aqueous solution2SiO3·9H2The mass fraction of O is not less than 6wt%, preferably 6 to 14wt%, more preferably 8 to 14 wt%.
When Na is contained in sodium silicate aqueous solution2SiO3·9H2When the mass fraction of O is less than 6wt%, the reaction proceeds slowly, and the temperature of the suspension increases slowly, so that the reaction does not proceed completelyBottom, resulting in a decrease in yield and reaction rate.
Preferably, the resulting aqueous sodium silicate solution is allowed to stand to room temperature before the silicon powder is added. The endothermic standing of the sodium silicate dissolved in water increases the temperature of the solution and thus the rate of its initial phase of reaction.
Preferably, the time required for standing is 1 to 3 minutes, such as 2 minutes. Na (Na)2SiO3·9H2The process of dissolving O in water absorbs heat, so that the temperature of the obtained sodium silicate aqueous solution is slightly reduced, and the solution can be returned to the room temperature by standing for 1-3 minutes to absorb heat.
Preferably, said Na2SiO3·9H2The molar ratio of O to silicon powder is 4: 1-1: 4, preferably 2: 1-1: 2.
preferably, the particle size of the silicon powder is D502.5 to 25 μm. Controlling the median particle diameter of the silicon powder to be D50The reaction rate is moderate and the reaction process is controllable, wherein the reaction rate is 2.5-25 mu m. If the particle diameter is too large, the reaction initiation temperature is required to be high (D)50At 25 μm, the initial reaction temperature is set to>50 deg.C) and the reaction does not proceed completely. If the particle size is too small, the hydrogen production rate is too high, and the experimental risk is extremely high.
Preferably, the stirring is magnetic rotor stirring, the stirring speed is 500rpm, and the stirring time is 1-3 minutes.
Preferably, the reaction temperature is 25-40 ℃, and the reaction time is 30-60 minutes.
Preferably, the produced hydrogen gas is filled with CaCl2The washing bottle absorbs the water vapor therein, and the water vapor is collected after being dried.
Preferably, the water is deionized water.
The invention has the beneficial effects that:
for the preparation of hydrogen, the fossil fuel has the problems of serious pollution, large investment and the like; the water electrolysis method has the problems of high energy consumption, limited reaction rate and the like; although a great deal of research is carried out on biological hydrogen production and photolytic hydrogen production, the hydrogen production rate is greatly limited. At present, the research at home and abroad needs to consume strong alkali liquor as a reactant, and the invention prepares hydrogen through silicon powder, and the preparation process is simple, pollution-free and efficient; sodium silicate is used as a catalyst, so that the loss is avoided in the whole reaction process, and the reaction is stable.
Drawings
Fig. 1 shows the steps of a specific embodiment of the hydrogen production method of the present invention.
Fig. 2 shows a scanning electron micrograph of Si powder in the starting material for the preparation of the present invention.
FIG. 3 is a photograph showing the reaction product at 3min from the start of the reaction in example 5; the experimental state can be read from the figure, i.e., that there are many bubbles generated and the reaction is proceeding.
FIG. 4 shows a photograph of a reaction product at 6min from the start of the reaction in comparative example 1; the experimental state can be read from the figure, i.e., a large amount of bubbles are generated and the reaction is proceeding.
FIG. 5 shows the XRD profile of the remaining black film on the surface of the solution (reaction by-products are shown in FIG. 4) after the reaction of example 5 is over (30 min is started); as can be seen from the graph, the broad peak around 22 ℃ corresponds to amorphous SiO2The glass phase, the remaining three peaks correspond to silicon powder which is not completely reacted in the suspension.
Detailed Description
The following detailed description of the present invention will be made in conjunction with the accompanying drawings and examples. It is to be understood that the following drawings and examples are illustrative of the invention and are not to be construed as limiting the invention.
The invention provides a clean hydrogen production technology based on fine silicon powder and sodium silicate. It comprises the following steps, as shown in figure 1:
(1) using Si powder and Na2SiO3·9H2O powder and water (preferably deionized water) are used as reaction raw materials;
(2) by using Na2SiO3·9H2Preparing sodium silicate solution by using O, wherein magnetic stirring and mixing can be carried out in the preparation process;
(3) mixing and stirring the raw material Si powder and the sodium silicate solution for 1-3 minutes, stopping stirring, and preparing hydrogen after the reaction.
The resulting aqueous sodium silicate solution is preferably allowed to stand to room temperature before step (3).
The yield of the mixed solution can reach 98.22 percent of the theoretical yield at room temperature, and the reaction rate can reach 1.72 multiplied by 10- 4gH2/(s·gSi)。
The Si powder and Na2SiO3·9H2O powder and deionized water are used as reaction raw materials, wherein the Na is2SiO3·9H2The molar ratio of O to silicon powder is 4: 1-1: 4, preferably 2: 1-1: 2. na in the sodium silicate aqueous solution2SiO3·9H2The mass fraction of O is not less than 6wt%, preferably 6 to 14wt%, more preferably 8 to 14 wt%. The grain diameter of the Si powder is D50＝2.5～25 μm as shown in FIG. 2.
The stirring is magnetic rotor stirring, the stirring speed is 500rpm, and the stirring time is 1-3 minutes. The reaction temperature is 25-40 ℃, and the reaction time is 30-60 minutes.
The prepared hydrogen gas is filled with CaCl2The wash bottles are dried and collected.
The produced hydrogen is collected by a drainage method, and the yield of the hydrogen is indirectly measured by measuring the volume of drainage.
Some exemplary embodiments are further set forth below to better illustrate the invention. It should be understood that the above detailed description of the present invention and the following examples are intended to illustrate rather than limit the scope of the present invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art in light of the foregoing description are intended to be included within the scope of the present invention. In addition, the specific formulation, time, temperature, etc. of the process parameters described below are also merely exemplary, and those skilled in the art can select appropriate values within the above-defined ranges.
Example 1
Si powder (0.6720g), Na2SiO3·9H2O powder (3.3333g) and deionized water (30ml), sodium silicate nonahydrate was prepared into a solution having a concentration of 10 wt%, magnetic stirring was carried out using a magnetic rotor for 2min, and then the solution was allowed to stand at room temperature (25 ℃ C.) for 2min to obtain sodium silicateThe solution is mixed with silicon powder, magnetic stirring is carried out for 2min by using a magnetic rotor, and the stirring is stopped until the reaction is finished. The yield of the prepared hydrogen is 97.60 percent, and the 70 percent hydrogen production rate is 1.72 multiplied by 10-4gH2/(s·gSi)。
Example 2
Si powder (0.3407g), Na2SiO3·9H2O powder (3.4090g) and deionized water (25ml), preparing sodium silicate nonahydrate into a solution with the concentration of 12 wt%, magnetically stirring for 2min by using a magnetic rotor, standing for 2min at room temperature, mixing the obtained sodium silicate solution with silicon powder, magnetically stirring for 2min by using the magnetic rotor, and stopping stirring until the reaction is finished. The yield of the prepared hydrogen is 97.20 percent, and the 70 percent hydrogen production rate is 1.50 multiplied by 10-4gH2/(s·gSi)。
Example 3
Si powder (0.1652g), Na2SiO3·9H2O powder (3.3333g) and deionized water (30ml), preparing sodium silicate nonahydrate into a solution with the concentration of 10 wt%, magnetically stirring for 2min by using a magnetic rotor, standing for 2min at room temperature, mixing the obtained sodium silicate solution with silicon powder, magnetically stirring for 2min by using the magnetic rotor, and stopping stirring until the reaction is finished. The yield of the prepared hydrogen is 90.29 percent, and the 70 percent hydrogen production rate is 1.26 multiplied by 10-4gH2/(s·gSi)。
Example 4
Si powder (0.4078g), Na2SiO3·9H2O powder (4.0700g) and deionized water (25ml), preparing sodium silicate nonahydrate into a solution with the concentration of 14wt%, magnetically stirring for 2min by using a magnetic rotor, standing for 2min at room temperature, mixing the obtained sodium silicate solution with silicon powder, magnetically stirring for 2min by using the magnetic rotor, and stopping stirring until the reaction is finished. The yield of the prepared hydrogen is 98.22 percent, and the 70 percent hydrogen production rate is 1.51 multiplied by 10-4gH2/(s·gSi)。
Example 5
Si powder (0.6646g), Na2SiO3·9H2O powder (6.6666g) and deionized water (60ml), sodium silicate nonahydrate was used as a 10 wt% solutionAnd magnetically stirring the solution for 2min by using a magnetic rotor, standing the solution for 2min at room temperature to obtain a sodium silicate solution, mixing the sodium silicate solution with the silicon powder, magnetically stirring the solution for 2min by using the magnetic rotor, and stopping stirring until the reaction is finished. The yield of the prepared hydrogen is 95.33 percent, and the 70 percent hydrogen production rate is 1.55 multiplied by 10-4gH2/(s·gSi)。
Example 6
Si powder (0.3323g), Na2SiO3·9H2O powder (3.3333g) and deionized water (30ml), preparing sodium silicate nonahydrate into a solution with the concentration of 10 wt%, magnetically stirring for 2min by using a magnetic rotor, standing for 2min at room temperature, mixing the obtained sodium silicate solution with silicon powder, magnetically stirring for 2min by using the magnetic rotor, and stopping stirring until the reaction is finished. The yield of the prepared hydrogen is 95.33 percent, and the 70 percent hydrogen production rate is 1.39 multiplied by 10-4gH2/(s·gSi)。
Example 7
Si powder (0.1583g), Na2SiO3·9H2O powder (1.6059g) and deionized water (25ml), preparing sodium silicate nonahydrate into a solution with the concentration of 10 wt%, magnetically stirring for 2min by using a magnetic rotor, standing for 2min at room temperature, mixing the obtained sodium silicate solution with silicon powder, magnetically stirring for 2min by using the magnetic rotor, and stopping stirring until the reaction is finished. The yield of the prepared hydrogen is 89.54 percent, and the 70 percent hydrogen production rate is 1.09 multiplied by 10-4gH2/(s·gSi)。
Example 8
Si powder (0.2162g), Na2SiO3·9H2O powder (2.1927g) and deionized water (25ml), preparing sodium silicate nonahydrate into a solution with the concentration of 10 wt%, magnetically stirring for 2min by using a magnetic rotor, standing for 2min at room temperature, mixing the obtained sodium silicate solution with silicon powder, magnetically stirring for 2min by using the magnetic rotor, and stopping stirring until the reaction is finished. The yield of the prepared hydrogen is 91.04 percent, and the 70 percent hydrogen production rate is 1.12 multiplied by 10-4gH2/(s·gSi)。
Comparative example 1
Si powder (0.3323g), Na2SiO3·9H2O powder (3.3333g) toPreparing sodium silicate nonahydrate into a solution with the concentration of 10 wt% by using ionized water (30ml and 50 ℃), performing magnetic stirring for 2min by using a magnetic rotor, standing at room temperature until the temperature of the solution is cooled to 40 ℃, mixing the obtained sodium silicate solution with silicon powder, performing magnetic stirring for 2min by using the magnetic rotor, and stopping stirring until the reaction is completed. The yield of the prepared hydrogen is 81.77 percent, and the 70 percent hydrogen production rate is 3.33 multiplied by 10-4gH2/(s·gSi). At high reaction initiation temperatures, the reaction rate is greatly increased, but the SiO is too fast2Film formation causes part of the unreacted Si to be carried out of the solution, resulting in a decrease in yield, as shown in fig. 4.
Comparative example 2
Si powder (0.1108g), Na2SiO3·9H2O powder (1.1111g) and deionized water (10ml), preparing sodium silicate nonahydrate into a solution with the concentration of 10 wt%, magnetically stirring for 2min by using a magnetic rotor, standing for 2min at room temperature, mixing the obtained sodium silicate solution with silicon powder, magnetically stirring for 2min by using the magnetic rotor, and stopping stirring until the reaction is finished. The yield of the prepared hydrogen is 74.28 percent, and the 70 percent hydrogen production rate is 9.35 multiplied by 10-5gH2/(s·gSi). When the overall water consumption is too low, also due to the SiO formed2The unreacted Si is carried out of the solution, resulting in incomplete reaction and a decrease in yield. Meanwhile, the amount of Si powder is small, and the heat release in the reaction process is small, so that the solution temperature is low, and the reaction rate is greatly reduced.
Comparative example 3
Si powder (0.0825g) and Na2SiO3·9H2O powder (3.3333g) and deionized water (30ml), preparing sodium silicate nonahydrate into a solution with the concentration of 10 wt%, magnetically stirring for 2min by using a magnetic rotor, standing for 2min at room temperature, mixing the obtained sodium silicate solution with silicon powder, magnetically stirring for 2min by using the magnetic rotor, and waiting for the reaction. The yield of the prepared hydrogen is 72.15 percent, and the 70 percent hydrogen production rate is 9.8 multiplied by 10-5gH2/(s·gSi). When Na is present2SiO3·9H2When the molar ratio of the O powder to the Si powder is too large (> 2:1), the reaction heat generation is small, the system temperature is low, and the reaction rate and the reaction progress degree are low.
Comparative example 4
Si powder (1.0080g) and Na2SiO3·9H2O powder (3.3333g) and deionized water (30ml), preparing sodium silicate nonahydrate into a solution with the concentration of 10 wt%, magnetically stirring for 2min by using a magnetic rotor, standing for 2min at room temperature, mixing the obtained sodium silicate solution with silicon powder, magnetically stirring for 2min by using the magnetic rotor, and waiting for the reaction. The yield of the prepared hydrogen is 75.38 percent, and the 70 percent hydrogen production rate is 2.38 multiplied by 10-4gH2/(s·gSi). When Na is present2SiO3·9H2When the molar ratio of the O powder to the Si powder is too small (less than 1:2), the reaction heat release is large, and the system temperature is high, so that the reaction rate is high; however, since the reaction is continuously carried out, OH generated by hydrolysis in the system-Is continuously consumed, Si (OH)4The solution is accumulated continuously, the pH value of the solution is reduced continuously, and the silicon powder cannot be completely reacted, so that the yield is reduced.
Comparative example 5
Si powder (0.3323g), Na2SiO3·9H2O powder (3.3333g) and deionized water (30ml), preparing sodium silicate nonahydrate into a solution with the concentration of 10 wt%, carrying out magnetic stirring for 2min by using a magnetic rotor, directly mixing the obtained sodium silicate solution with silicon powder without standing, carrying out magnetic stirring for 2min by using the magnetic rotor, and stopping stirring until the reaction is finished. The yield of the prepared hydrogen is 95.98 percent, and the 70 percent hydrogen production rate is 1.28 multiplied by 10-4gH2/(s·gSi)。
TABLE 1
Claims (9)
1. A hydrogen production method based on fine silicon powder and sodium silicate is characterized by comprising the following steps:
mixing Na2SiO3·9H2Dissolving O in water to prepare a sodium silicate aqueous solution;
and mixing and stirring the obtained sodium silicate aqueous solution and the silicon powder, and starting to react to form hydrogen.
2. The method for producing hydrogen according to claim 1, wherein Na is contained in the aqueous sodium silicate solution2SiO3·9H2The mass fraction of O is not less than 6wt%, preferably 6 to 14 wt%.
3. The method for producing hydrogen according to claim 1 or 2, characterized in that the obtained aqueous sodium silicate solution is allowed to stand to room temperature before the silicon powder is added.
4. Process for producing hydrogen according to any of claims 1 to 3, characterized in that Na is added2SiO3·9H2The molar ratio of O to silicon powder is 4: 1-1: 4, preferably 2: 1-1: 2.
5. the hydrogen production method according to any one of claims 1 to 4, wherein the silicon powder has a median particle diameter D50=2.5～25μm。
6. The method according to any one of claims 1 to 5, wherein the mixing and stirring is magnetic rotor stirring, the stirring rate is 500 to 3000rpm, and the time is 1 to 3 minutes.
7. The method for producing hydrogen according to any one of claims 1 to 6, wherein the reaction temperature is 25 to 40 ℃ and the reaction time is 30 to 60 minutes.
8. Process for producing hydrogen as claimed in any of claims 1 to 7, characterized in that the hydrogen produced is passed through a system containing CaCl2The wash bottles are dried and collected.
9. The method for producing hydrogen as claimed in any one of claims 1 to 8, wherein the water is deionized water.
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| CN107640742A (en) * | 2017-11-17 | 2018-01-30 | 江西硅辰科技有限公司 | A kind of silica-based high-efficiency solid-state hydrogen production agent |
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| JP2001213609A (en) * | 2000-01-28 | 2001-08-07 | Sugino Mach Ltd | Process of producing hydrogen and apparatus therefor |
| JP2006240935A (en) * | 2005-03-04 | 2006-09-14 | Sharp Corp | Method for producing hydrogen gas |
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| CN107640742A (en) * | 2017-11-17 | 2018-01-30 | 江西硅辰科技有限公司 | A kind of silica-based high-efficiency solid-state hydrogen production agent |
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