CN107473183A - The application of phosphating sludge catalyzing manufacturing of hydrogen in alkaline formaldehyde solution - Google Patents

The application of phosphating sludge catalyzing manufacturing of hydrogen in alkaline formaldehyde solution Download PDF

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CN107473183A
CN107473183A CN201710715999.1A CN201710715999A CN107473183A CN 107473183 A CN107473183 A CN 107473183A CN 201710715999 A CN201710715999 A CN 201710715999A CN 107473183 A CN107473183 A CN 107473183A
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hydrogen
formaldehyde
phosphating sludge
moll
manufacturing
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CN107473183B (en
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李越湘
彭惠琛
彭绍琴
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Nanchang University
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Nanchang University
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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
    • C01B3/22—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/14—Phosphorus; Compounds thereof
    • B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
    • B01J27/19—Molybdenum
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/02—Processes for making hydrogen or synthesis gas
    • C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
    • C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/10—Catalysts for performing the hydrogen forming reactions
    • C01B2203/1041—Composition of the catalyst
    • C01B2203/1088—Non-supported catalysts

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The application of phosphating sludge catalyzing manufacturing of hydrogen in alkaline formaldehyde solution.Its catalytic reaction condition is：Carried out under room temperature and heating condition, naoh concentration is in 0.01 ~ 10 molL in formalin‑1Between, formalin concentration is in 0.1 ~ 3 molL‑1Between, molybdenum phosphide catalyst dosage is between 5 ~ 30 mg in 100 mL formalins.The hydrogen that the present invention is prepared under inert gas atmosphere can be directly used for fuel cell, it is not necessary to separate oxygen.Alkaline formaldehyde solution hydrogen manufacturing is effectively catalyzed with can under heating condition at room temperature, hydrogen source is provided for fuel cell.At room temperature, phosphating sludge catalysis alkaline formaldehyde solution hydrogen production rate of the present invention has reached 150 mLmin‑1·g‑1, it is precious metals pd catalysis 2 times of formaldehyde hydrogen manufacturing, is 7 times of Ni metal catalysis formaldehyde hydrogen manufacturing.In a heated condition, phosphating sludge catalysis formaldehyde hydrogen production rate can exponentially increase.

Description

The application of phosphating sludge catalyzing manufacturing of hydrogen in alkaline formaldehyde solution
Technical field
The invention belongs to chemical application technology field, it is related to the new application of phosphating sludge.
Background technology
The progress of human society is developed rapidly so that energy resource consumption sharp increase and increasing environmental pollution with industry.Therefore, people Seeking new sustainable, cleaning the energy always.And Hydrogen Energy is pursued with the characteristics of its clean environment firendly by people.Through Ji, safe, environment-friendly hydrogen manufacturing and hydrogen storage are key technologies urgently to be resolved hurrily.Hydrogen fuel cell energy transformation ratio is up to 60% ~ 80%, it is to utilize the optimal mode of Hydrogen Energy.Purity requirement of the fuel cell to hydrogen is very high, it is impossible to containing CO, Pt otherwise can be made electric It is poisoned pole.
Formaldehyde is the chemicals of low cost, being capable of large-scale industry preparation.Formaldehyde can produce in sodium hydrate aqueous solution Raw a small amount of hydrogen.In the presence of a catalyst, formaldehyde, being capable of highly effective hydrogen yield in alkaline solution.Hydrogen caused by this method It is very pure, without CO and CO2, it is particularly suitable for the hydrogen storage of hydrogen fuel cell.Hu et al. has prepared palladium nanotube, urges at room temperature Choline formalin hydrogen manufacturing, at 25 DEG C, hydrogen output is up to 80 mL after reacting 1 h；Li et al. has found that silver nano-grain also can Enough to be catalyzed alkaline formaldehyde solution hydrogen manufacturing at room temperature, under the conditions of 25 DEG C and pure oxygen, 1 h hydrogen outputs have reached 20 mL, are nitrogen 10 times under atmosphere.Formaldehyde production hydrogen reaction unit is simple, but the noble metal catalyst used at present is expensive, and resource has Limit.It is relatively low using base metal and compound price, there is good actual application prospect.
Phosphorus arranges first 10 in earth's crust rich content.Although content of the molybdenum in the earth's crust is not very high, it easily into ore deposit, So it, which exploits and prepared cost, is less than noble metal.By the use of phosphating sludge substitute noble metal as the hydrogen manufacturing of catalyst decomposing formaldehyde with into This advantage and resources advantage.In the document reported in the past, phosphating sludge is mainly used in the hydrodesulfurization processing of oil product, or is used as and helps Catalyst is used for water electrolysis hydrogen production and photocatalysis hydrogen production.
The content of the invention
It is an object of the invention to provide a kind of new application of phosphating sludge, i.e. phosphating sludge catalyzing manufacturing of hydrogen in alkaline formaldehyde solution New application.
The present invention is achieved by the following technical solutions.
The chemical composition of phosphating sludge of the present invention is MoP.
The application of phosphating sludge of the present invention catalyzing manufacturing of hydrogen in alkaline formaldehyde solution, be in inert gas-nitrogen or Under argon atmosphere and in alkaline solution, phosphating sludge catalytic decomposition formaldehyde hydrogen manufacturing.
Described catalytic reaction can be carried out under room temperature and heating condition, and the reaction temperature of optimization is more than 45 DEG C.Formalin Naoh concentration is in 0.01 ~ 10 molL in solution-1Between, the concentration of optimization is in 1 ~ 4 molL-1Between.Formalin Concentration is in 0.1 ~ 3 molL-1Between, the concentration of optimization is in 1 ~ 3 molL-1Between.Phosphating sludge is urged in 100 mL formalins Agent dosage is between 5 ~ 30 mg, and the dosage of optimization is in 20 ~ 30 mg.
The invention provides a kind of new application of phosphating sludge hydrogen manufacturing in formalin under atmosphere of inert gases.In indifferent gas The hydrogen prepared under body atmosphere can be directly used for fuel cell, it is not necessary to separate oxygen.At room temperature with can under heating condition Alkaline formaldehyde solution hydrogen manufacturing is effectively catalyzed, hydrogen source is provided for fuel cell.At room temperature, phosphating sludge catalysis of the present invention Alkaline formaldehyde solution hydrogen production rate has reached 150 mLmin-1·g-1, it is precious metals pd catalysis 2 times of formaldehyde hydrogen manufacturing, is gold Belong to 7 times of Cu catalysis formaldehyde hydrogen manufacturing.In a heated condition, phosphating sludge catalysis formaldehyde hydrogen production rate can exponentially increase.
Brief description of the drawings
Fig. 1 is with the Na of different mol ratio in embodiment 12MoO4And NaH2PO2The X of the phosphating sludge prepared for reactant spreads out Penetrate figure.
Fig. 2 is with the Na of different mol ratio in embodiment 12MoO4And NaH2PO2For reactant prepare phosphating sludge in alkalescence The contrast of catalysis production hydrogen activity in formalin.
Fig. 3 is to work as Na in embodiment 22MoO4And NaH2PO2Mol ratio is 1:The phosphating sludge prepared when 7 is in different alkali concns Lower catalysis formalin production hydrogen activity.
Fig. 4 is to work as Na in embodiment 32MoO4And NaH2PO2Mol ratio is 1:The phosphating sludge prepared when 7 is in various concentrations Catalysis production hydrogen activity in formalin.
Fig. 5 is to work as Na in embodiment 42MoO4And NaH2PO2Mol ratio is 1:The addition of the phosphating sludge prepared when 7 is to alkali Property catalysis of solution of formaldehyde production hydrogen activity influence.
Fig. 6 is to work as Na in embodiment 52MoO4And NaH2PO2Mol ratio is 1:The phosphating sludge prepared when 7 is at different temperatures It is catalyzed alkaline formaldehyde solution production hydrogen activity.
Embodiment
The present invention will be described further by following examples.But present disclosure is not limited to this.
Embodiment 1.
（1）The preparation of molybdenum phosphide catalyst.It is 1 in molar ratio:3~1:9 weigh Na2MoO4And NaH2PO2（Na2MoO4Thing Quality is 1 mM）, it is dissolved in 15 mL water, stirring and dissolving, 60 DEG C of drying obtain solid reactant presoma, after grinding In N2In the tubular type Muffle furnace of atmosphere 1 h is calcined at 300 DEG C.Deionized water, ethanol washing are multiple, and 60 DEG C are dried to obtain phosphatization Molybdenum.
Fig. 1 is the Na with different mol ratio2MoO4And NaH2PO2The X diffraction patterns of the phosphating sludge prepared for reactant（XRD）. It can be seen that with NaH2PO2Amount increase, crystal formation do not change, and is MoP, but diffraction maximum in XRD Slowly die down.
（2）The evaluation of formalin hydrogen production activity is catalytically decomposed in phosphating sludge.Phosphating sludge decomposing formaldehyde hydrogen production reaction is at one Carried out in about 500 mL Pyrex flasks, bottleneck silicone rubber seal.The phosphating sludge of the above-mentioned different compositions of 20 mg is weighed, is added Into 100 mL formaldehyde alkaline solution.The concentration of sodium hydroxide and formaldehyde is 1.0 molL in the solution-1.Fill N2 20 Oxygen in min fully exclusion systems, the h of stirring reaction 1 at 25 DEG C, reaction gas phase hydrogen product pass through bottleneck silicon rubber gap and sampled Analysis, uses chromatographic（Detector is TCD, carrier gas N2, splitter is NaX molecular sieve columns, quantified by external standard method）.
As shown in Fig. 2 the phosphating sludge decomposing formaldehyde production hydrogen activity prepared is with preparing NaH in catalyst process2PO2Addition Increase and increase, work as Na2MoO4And NaH2PO2Mol ratio is 1:Hydrogen output increase is slow after 7, considers cost of material, preferably Na2MoO4And NaH2PO2Mol ratio is 1:7.
Embodiment 2.
（1）The preparation of molybdenum phosphide catalyst.Weigh 1 mmol Na2MoO4With 7 mmol NaH2PO2, it is dissolved in 15 ml water In, lower dissolving is stirred, 60 DEG C of drying obtain solid reactant presoma.In N after grinding21 h is calcined at 300 DEG C of atmosphere.Go Ionized water, ethanol washing are multiple, and 60 DEG C are dried to obtain phosphating sludge.
（2）The influence of naoh concentration PARA FORMALDEHYDE PRILLS(91,95) hydrogen production reaction activity.The evaluation of hydrogen production reaction activity is the same as in embodiment 1 Step（2）.The phosphating sludge for weighing 20 mg preparations is added to 1 molL-1In the reaction solution of formalin, hydroxide in the solution The concentration of sodium is in 0.01-4 molL-1Between scope.Room temperature（20℃）The lower min of stirring reaction 30.As shown in figure 3, low Under alkali concn（Less than 0.5 mol.L-1）, production hydrogen activity is very low, but when naoh concentration is more than 1.0 molL-1Afterwards, alkali is dense Spend the influence very little to producing hydrogen activity.The naoh concentration of optimization is in 1-3 molL-1Between.
Embodiment 3.
（1）The preparation of catalyst is the same as the step 1 of embodiment 2.
（2）The influence of concentration of formaldehyde PARA FORMALDEHYDE PRILLS(91,95) hydrogen production reaction activity.The evaluation of hydrogen production reaction activity is the same as step in embodiment 1 2.The phosphating sludge for weighing 20 mg preparations is added to 1 molL-1In the reaction solution of sodium hydroxide solution, the reaction solution formaldehyde it is dense Degree is in 0.1-3 molL-1Between scope.Room temperature（20℃）The lower min of stirring reaction 30.As shown in figure 4, production hydrogen activity is with first The increase of aldehyde concentration and increase, be 2 molL in concentration of formaldehyde-1When reach optimal.The concentration of formaldehyde of optimization is in 1-3 mol L-1Between.
Embodiment 4.
（1）The preparation of catalyst is the same as the step 1 of embodiment 2.
（2）The influence of the amount PARA FORMALDEHYDE PRILLS(91,95) hydrogen production reaction activity of phosphating sludge.The evaluation of hydrogen production reaction activity in embodiment 1 the same as walking Suddenly（2）.The phosphating sludge for weighing 5-30 mg preparations is added in 100 mL formaldehyde alkaline solution, formaldehyde and sodium hydroxide it is dense Degree is 1.0 molL-1.Room temperature（20℃）The lower min of stirring reaction 30.As shown in figure 5, production hydrogen activity is with the phosphatization of addition The amount of molybdenum increases and increased, and when the amount of phosphating sludge reaches 20 m g, production hydrogen is optimal, slightly declines higher than hydrogen output after 20 mg. The amount of the phosphating sludge of optimization is between 20-30 mg.
Embodiment 5.
（1）The preparation of catalyst is the same as the step 1 of embodiment 2.
（2）The influence of reaction temperature PARA FORMALDEHYDE PRILLS(91,95) hydrogen production activity.The evaluation of hydrogen production reaction activity is the same as step in embodiment 1（2）. The phosphating sludge for weighing 20 mg preparations is added in 100 mL formaldehyde alkaline solution, and the concentration of formaldehyde and sodium hydroxide is 1.0 mol·L-1.Reaction temperature is controlled between 5-65 DEG C, the min of stirring reaction 10.As shown in fig. 6, production hydrogen activity is with reaction temperature Increase and increase, after temperature is higher than 45 DEG C, production hydrogen activity increases sharply.It is low in view of that should be used as far as possible in practical application Temperature, the reaction temperature of optimization should be higher than that 45 DEG C.

Claims (4)

1. the application of phosphating sludge catalyzing manufacturing of hydrogen in alkaline formaldehyde solution.
2. application according to claim 1, it is characterized in that under inert gas-nitrogen or argon atmosphere and alkaline solution In, phosphating sludge catalytic decomposition formaldehyde hydrogen manufacturing.
3. application according to claim 1 or 2, the catalytic reaction condition described in its feature are：In room temperature and heating condition Lower progress, naoh concentration is in 0.01 ~ 10 molL in formalin-1Between, formalin concentration is 0.1 ~ 3 mol·L-1Between, molybdenum phosphide catalyst dosage is between 5 ~ 30 mg in 100 mL formalins.
4. application according to claim 1 or 2, the catalytic reaction condition described in its feature are：Reaction temperature is more than 45 DEG C, Naoh concentration is in 1 ~ 4 molL in formalin-1Between, formalin concentration is in 1 ~ 3 molL-1Between, 100 Molybdenum phosphide catalyst dosage is between 20 ~ 30 mg in mL formalins.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109499584A (en) * 2018-12-13 2019-03-22 安徽工业大学 With the method for NiPd/ porous C exCoyOz nanocatalyst catalysis formaldehyde dehydrogenation
CN109647435A (en) * 2018-12-17 2019-04-19 安徽工业大学 With the method for CuPd/ porous C exCoyOz nanocatalyst catalysis formaldehyde dehydrogenation
CN109665493A (en) * 2018-12-24 2019-04-23 安徽工业大学 With the method for NiPd/ porous C exCuyOz nanocatalyst catalysis formaldehyde dehydrogenation
CN109734051A (en) * 2019-01-10 2019-05-10 安徽工业大学 With the method for AgPd/ porous C exCuyOz nanocatalyst catalysis formaldehyde dehydrogenation
CN111167435A (en) * 2019-12-31 2020-05-19 南京环福新材料科技有限公司 Molybdenum-based titanium dioxide nano array catalyst and preparation method and application thereof

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WO2017042661A1 (en) * 2015-09-09 2017-03-16 Sabic Global Technologies B.V. Robust catalyst for hydrogen production from p-formaldehyde

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109499584A (en) * 2018-12-13 2019-03-22 安徽工业大学 With the method for NiPd/ porous C exCoyOz nanocatalyst catalysis formaldehyde dehydrogenation
CN109647435A (en) * 2018-12-17 2019-04-19 安徽工业大学 With the method for CuPd/ porous C exCoyOz nanocatalyst catalysis formaldehyde dehydrogenation
CN109665493A (en) * 2018-12-24 2019-04-23 安徽工业大学 With the method for NiPd/ porous C exCuyOz nanocatalyst catalysis formaldehyde dehydrogenation
CN109734051A (en) * 2019-01-10 2019-05-10 安徽工业大学 With the method for AgPd/ porous C exCuyOz nanocatalyst catalysis formaldehyde dehydrogenation
CN111167435A (en) * 2019-12-31 2020-05-19 南京环福新材料科技有限公司 Molybdenum-based titanium dioxide nano array catalyst and preparation method and application thereof
CN111167435B (en) * 2019-12-31 2023-02-03 南京环福新材料科技有限公司 Molybdenum-based titanium dioxide nano array catalyst and preparation method and application thereof

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