CN102730716A - Preparation of porous active ammonia-storing mixture containing molecular sieve - Google Patents
Preparation of porous active ammonia-storing mixture containing molecular sieve Download PDFInfo
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- CN102730716A CN102730716A CN201210238807XA CN201210238807A CN102730716A CN 102730716 A CN102730716 A CN 102730716A CN 201210238807X A CN201210238807X A CN 201210238807XA CN 201210238807 A CN201210238807 A CN 201210238807A CN 102730716 A CN102730716 A CN 102730716A
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- 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
- Y02E60/50—Fuel cells
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Abstract
The invention relates to preparation of a porous active ammonia-storing mixture containing molecular sieve. The preparation is characterized by comprising the following steps: adopting industrial anhydrous calcium chloride salt powders; adding a right amount of the molecular sieve, clay, de-ionized water and industrial spirit; mechanistically stirring to obtain the uniform half-dried mixed wet material; and filling the mixed wet material in a tank to prepare integral porous solid blocks. The solid blocks are provided with multiple ammonia gas conveying channels and a plurality of large holes on macroscopic scale, so that the ammonia can be quickly filled, the performance for storing ammonia is good, and the ammonia gas can be quickly released and can be cycled without breakage. The high-efficiency absorption and desorption prosperities are provided, so that the mixture is suitable for adsorbing and storing the ammonia, and can be applied to SCR (selective catalyst reduction) and FCEV (fuel cell electric vehicle) systems to meet the application needs of car industry in the furture.
Description
Technical field
The present invention relates to a kind of porous active storage ammonia mixture preparation that contains molecular sieve, be applied to the SCR after-treatment system and the FCEV fuel cell system of vehicle exhaust.
Background technology
Current, the whole world faces the comprehensive challenge of the energy and environment.Aspect the technique means selection of the emission compliance of orthodox car, and the fuel feed technical elements people of new-energy automobile still face many difficult problems.
The SCR after-treatment system is to rely on the accurate supply of carbamide reducing agent and after the front end of catalyzer resolves into ammonia, remove the NOX hazardous material, reaches the purpose of cleaning of off-gas, realizes state 4 or above standard up to standard of vehicle; But; In actual use, this dependence urea decomposition becomes the meter injection of the liquid area of ammonia to have many deficiencies and difficult point, for example; Urea soln is icing blocking problem under-11 ℃ of environment, needs extra pipeline heating system to solve; Urea soln could decompose under the temperature environment more than 135 ℃, and many vehicles of public transit system loiter, and can't reach urea soln stable decomposition temperature at all; Can't the output ammonia, can't eliminate predetermined NOX composition, cause the accumulation of liquid area in vapor pipe at last; Produce the polymkeric substance of trimeric cyanamide, stop up the urea nozzle and the exhaust pipe of engine, cause vehicles produces fault; Influence is normal to be used, in addition, if the main flow vehicle of state more than 4 uses the SCR system comprehensively; Relate to the whole nation about 150,000 oiling websites innovation and build the problem of liquid area filling Infrastructure; Because investment is huge, do not see still that at present government and enterprise start to improve this Infrastructure, become a huge problem of potential in the SCR use;
For breaking through energy predicament, solve the new-energy automobile development problem of future source of energy problem, hydrogen fuel cell is a very important techniques route by generally acknowledging; But how stable acquisition hydrogen is originated is a no small difficult problem of restriction this area development, in institute's possible adopted hydrogen source mode; Technological line and the hydrogenous presoma decomposition of other H-N or the technological line of cracking hydrogen production that the technological line of gas cylinder storage hydrogen, the technological line that water electrolysis hydrogen production is arranged, the technological line that high-purity hydro carbons oil fuel cracking hydrogen production is arranged, low mass molecule alcohol class cracking hydrogen production are arranged; In the above-mentioned technological line, all there are some problem and shortage, for example; Hydrogen production efficiency and cost; Hydrogen manufacturing precision and speed also comprise the problem of system aspects, in a word; The source of hydrogen is the bottleneck of fuel-cell vehicle development, needs people's idea to solve;
One of them is the hydrogenous compound of H-N for the presoma of hydrogen, and wherein, what hydrogen-storage density was the highest is ammonia.Ammonia is a kind of modal industrial chemicals, and the ammonia molecule belongs to active polar molecule, and the diameter dimension of molecule is about 3 ~ 4A, therefore, very active under the normal temperature, very easily diffusion, and have toxic; The skin histology that its toxic is embodied in contact all has corrosion and hormesis, can absorb the moisture in the skin histology, makes the tissue protein sex change, and makes the tissue fat saponification, destroys membrane structure; Ammonia in water solubleness high, stimulate and corrosive nature so mainly the upper respiratory tract of animal or human's body is had, often be attracted on mucocutaneous and the eye conjunctiva; Stimulate and inflammation thereby produce, in addition, ammonia sucks human body with gas form usually; Ammonia gets into blood through alveolar after being inhaled into lung easily, combines with oxyphorase, destroys fortune oxygen function; Get into IA ammonia; Few part is neutralized by carbonic acid gas, and remainder is absorbed into blood, suck in a short time can occur shedding tears behind a large amount of ammonias, pharyngalgia, cough, uncomfortable in chest, expiratory dyspnea, dizziness, vomiting, weak etc.; If the long-term ammonia that sucks is too much, cause ammonia excessive concentration in the blood, will cause heart stop fight and breath stopped threat to life safety; Therefore, the maximum hidden danger of the use of ammonia is safety-problems.
This shows, resolve in the use of ammonia storing and safety-problems, just can open up the technological line of a new ammonia utilization.
Traditional ammonia storing mode is a gas cylinder, or realizes with the water-soluble formation ammoniacal liquor of high density ammonia.If adopt gas cylinder to store ammonia, there is the potential safety hazard of operating aspect and seal aspect in the industrial application in enormous quantities, if, have serious etching problem again with the mode of high strong aqua.
At China national patent information net; With the storage ammonia word and search that is the theme; The patent No. is that CN201120099229.7's ' a kind of urotropine by using gas phase method tail gas ammonia recovery unit ', the patent No. is that ' be used for freezer machine room join ammonia connection mechanism ' of CN201020677361.7, ' complex function type storage ammonia device ', the patent No. that the patent No. is CN201020269811.9 are CN200520057558.X ' a kind of ammonia steaming device '; Be one type the ammonia nitrogen trade effluent carried out the environment protection treating device that ammonia nitrogen is got rid of processing, also do not relate to the characteristic component among the present invention.Uncorrelated with the present invention;
The patent No. is that CN201010244091.5's ' be used for method and system that the work of SCR catalyzer is tested ' and the patent No. is that this 2 inventions of CN200880104697.X ' operation method of SCR exhaust after treatment system and diagnostic method ' provide a kind of SCR (SCR) catalytic converter and traditional liquid ureaclastic ammonia dispensing module and system of being used for, and does not relate to the characteristic component of compound;
The patent No. is that CN200910197860.8's the invention of ' a kind of preparation method of efficient low-temperature ammonia-storing material ' is applied to the SCR after-treatment system; Characteristic is to place encloses container to the amino borane compound; Vacuumize, under 0-4 ℃ of temperature, contact with ammonia; Under 0-4 ℃ of temperature, kept 30-60 minute, prepare required product amino borane ammonia complex NH
3BH
3(NH
3) n (n=1-3); The maximum storage of room temperature ammonia amount can reach 62.4wt.%; About room temperature supply gas pressure 2.0bar; Room temperature supplies ammonia pressure moderate, inhales to put the ammonia completely reversibility, but the costing an arm and a leg of the extraordinary material amino borane of this patent; Have higher explosion hazard and burning grade, be not suitable for applying in enormous quantities of general industry field;
The patent No. is that CN200580026626.9's the invention of ' storage and carry the solid material of ammonia ' relates to storage and carries the solid material of ammonia.The solid material of this storage ammonia comprises that a kind of ammonia absorbs salt, and wherein this ammonia absorption salt is that general formula is M
a(NH
3)
nX
zIonic salt; Wherein M is selected from for example one or more positively charged ions of Mn, Fe, Co, Ni, Cu and/or Zn of earth alkali metal and/or one or more transition metal, and X is one or more negatively charged ion, and a is the positively charged ion number that comprises in each molecules of salt; Z is the negatively charged ion number that comprises in each molecules of salt; N is 2～12 ligancy, and wherein M is Mg, and it is automotive industry that this ammonia absorbs salt provides a kind of safety, lightweight, cheap and fine and close storage with ammonia.This patent is the direct compression molding of solid material, and ammonia is resolved in the electric heating heating, more lays particular emphasis on the control strategy of system, does not relate to the modification and the optimization of mixture;
The patent No. be CN200580009219.7's ' purposes of ammonia storage device in energy generation ' invention relate to a kind of generator unit, this unit comprises the ammonia storage device of (i) container (2) form, comprising general formula is M
a(NH
3)
NXzAmmonia absorb and discharge salt; Wherein M is one or more positively charged ions, is selected from basic metal, earth alkali metal and transition metal such as Li, K, Mg, Ca, V, Cr, Mn, Fe, Co, Ni, Cu or Zn, and X is one or more negatively charged ion; Be selected from fluorine root, chlorine root, bromine root, iodine root, nitrate radical, thiocyanate ion, sulfate radical, molybdate, phosphate radical and chloranion; A is the positively charged ion number of each molecules of salt, and z is the negatively charged ion number of each molecules of salt, and n is the ligancy of 2-12; (ii) being used to heat said container (2) and ammonia absorbs and discharges the fuel cell that salt with the device (3a) that discharges ammonia and (iiia) is used for ammonia is converted into electric power; Perhaps (iiib1) is used for ammonia is dissociated into the reactor drum (6) of hydrogen and nitrogen; (iiib2) be used for hydrogen is converted into the fuel cell (4) of electric power; This patent is mainly used in fuel cell; Mentioned property material in the claim 4 and be such salt or be positioned on the porous carrier materials, which kind of material statement is not;
The disclosure of the Invention of CN200710156866.1 ' a kind of amido complex compound ' a kind of amido complex compound.The composition of this amido complex compound is MX
m(NH
3)
n, M is one or more among Li, Mg, Al, Ca, Sc, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Sr, Ba, the Sn in the formula; X is F, Cl, Br, NO
3, SO
4In one or more; M decides according to valency, 1≤m≤5; N decides according to ligancy, 1≤n≤15.With the absorption agent of the amido complex compound behind the deamination, put separation, purification, storage and the transportation that ammonia is realized ammonia through low temperature suction ammonia, high temperature as ammonia.This patent only relates to the preparation technology and the process of this amido complex compound itself;
The patent No. is solid ammonia storage and the conveying material that CN200680005886.2's the high-density of the ammonia ' storage ' patent comprises ammonia absorptions/desorb solid material; The said density that has been compacted to is greater than 50% storage of theoretical skeletal density with carry material that the solid ammonia storage medium is provided; The storage ammonia that this storage medium prepares and handles and have very high-density easily; Said storage ammonia discharges under controlled condition easily; Even the porosity of said material is very low still like this, and this storage medium does not need special security measures for storage with to carry ammonia be safe.This patent is to adopt the direct compression molding of solid material; Adopt sticker; Only stated it possibly is the silica fiber sticker, do not had the dosage ratio, the solid material of also only stating among other claim item and the embodiment possibly comprise particulate material, porous material, crystalline material, amorphous material or their binding substances composition; Do not have thin of clear and definite claim, industry technology personage almost can't implement.Produced the present invention therefrom.
Summary of the invention
The object of the present invention is to provide a kind of porous active storage ammonia mixture preparation that contains molecular sieve, it increases the ammonia transmission path in order to improve the hole of storage ammonia active substance solid piece, weaken or avoid adsorbing repeatedly with desorption process in CaCl
2The caking that takes place and the efflorescence of solid piece are broken, and that satisfies industrial occasions repeatedly recycles requirement, possesses efficient absorption and conciliates characterization of adsorption, and the absorption that is fit to ammonia stores, and is used for SCR and FCEV system, satisfies the application demand of following automotive industry.
Technical scheme of the present invention is achieved in that a kind of porous active storage ammonia mixture preparation that contains molecular sieve; It is characterized in that the preparation method is following: press the powder of mass fraction with 45 ~ 90 parts industrial anhydrous calcium chloride salt; Mix industrial ball clay and 1 ~ 8 part of molecular sieve of 2 ~ 15 parts; Become uniform mixture wet feed with 4 ~ 17 parts deionized water with 3 ~ 15 parts industrial alcohol mechanical stirring again; Be filled in the tank body, addition is no more than tank body volumetrical 80%, and machinery concussion 5 ~ 10min eliminates the clearance; Whole tank body is put in the vacuum drying oven, and normal pressure is slowly heating down, and temperature is controlled at 65 ~ 160 ℃; Get rid of water and ethanol to mixture constant weight, substep is evacuated to 550mbar, constant temperature and pressure 0.5 ~ 3h; Take out tank body, the sealing charging opening is processed the whole porosu solid piece of storage ammonia activated mixture; Ammonia is filled in the tank body under 0.05 ~ 0.8MPa pressure, saturated to the mixture absorbing ammonia.
Described molecular sieve bore diameter scope is at 2 ~ 30nm, and specific surface area is greater than 300m
2/ g.
Described tank body is the withstand voltage tank body of stainless steel, inner tank wall thermospray nylon thermal insulation layer.
At positively effect of the present invention is optionally to have added molecular sieve, has promoted CaC1
2Dispersion, can weaken or avoid the generation of caking phenomenon effectively, improved the richness of microscopic void; Increased the transmission path of ammonia; Improve the penetrating quality of ammonia greatly, promote the formation of ammino calcium chloride complex compound, simultaneously the vesicular structure of molecular sieve itself; Ammonia is possessed certain absorption and memory function, can weaken effectively or avoid adsorbing with desorption process in the expansion of solid piece to shrink the efflorescence cause broken; The diffusing CaC1 of water that adds and dissolve with ethanol and differential
2And other fillers, improve between the liquid-solid two-phase wetting with sprawl, in addition, water and ethanol are deviate from the hole of process formation, have enriched the transmission path of ammonia; To sum up, contain the abundant activity storage ammonia mixture of microcosmic nano pore of molecular sieve, guaranteeing under the constant prerequisite of storage ammonia active substance characteristic; Molecular sieve that adds and the phenomenon that clay weakens or the ammonia adsorption-desorption of having avoided caking, fragmentation etc. to cause attaches; Improve the richness of microscopic void, increased the quantity of macroscopic pores, improved the physical strength of mixture solid piece; Have very high practical value, be suitable for the SCR aftertreatment or the FCEV system of automobile industry.
Description of drawings
The thermogravimetric curve of the activated mixture of the absorbing ammonia of Fig. 1 embodiment of the invention 1.
Embodiment
Through embodiment the present invention is further described below, embodiment is not equal to restriction the present invention for further illustrating characteristics of the present invention,, all should be included within protection scope of the present invention according to the change that the present invention carries out for those skilled in the art.
Embodiment 1
Water with 71 parts calcium chloride, 3 parts of molecular sieves, 6 parts of clays and 12 parts mixes 1h in impeller, add 8 parts of ethanol; Continue mechanical stirring 3h, process uniform mixture wet feed, be filled in the tank body; Be added into tank body volumetrical 80%, machinery concussion 10min eliminates the clearance;
Whole tank body is put in the vacuum drying oven, and is as shown in Figure 1, and the temperature rise rate with 2 ℃/min under the normal pressure rises to 120 ℃, constant temperature 6h; Get rid of water and ethanol, substep is evacuated to 550mbar, constant temperature and pressure 1h; Take out tank body, the sealing charging opening is processed the whole porosu solid piece of storage ammonia activated mixture.
Embodiment 2
Water with 2 parts of molecular sieves, 18 parts of clays and 15 parts mixes 1h in impeller, add 55 parts calcium chloride mixing 1h; Add 10 parts of ethanol; Continue mechanical stirring 3h, process uniform mixture wet feed, be filled in the tank body; Be added into tank body volumetrical 75%, machinery concussion 10min eliminates the clearance;
Whole tank body is put in the vacuum drying oven, and the temperature rise rate with 2 ℃/min under the normal pressure rises to 120 ℃, constant temperature 6h; Get rid of water and ethanol, substep is evacuated to 550mbar, constant temperature and pressure 1h; Take out tank body, the sealing charging opening is processed the whole porosu solid piece of storage ammonia activated mixture.
Embodiment 3
Water with 4 parts of clays and 6 parts mixes 1h in impeller, add 81 parts calcium chloride mixing 1h; Add 3 parts of molecular sieve mixing 1h, add 6 parts of ethanol, continue mechanical stirring 3h; Process uniform mixture wet feed; Be filled in the tank body, be added into tank body volumetrical 80%, machinery concussion 10min eliminates the clearance;
Whole tank body is put in the vacuum drying oven, and the temperature rise rate with 5 ℃/min under the normal pressure rises to 100 ℃, constant temperature 8h; Get rid of water and ethanol, substep is evacuated to 550mbar, constant temperature and pressure 2h; Take out tank body, the sealing charging opening is processed the whole porosu solid piece of storage ammonia activated mixture.
Embodiment 4
The tank body that the storage ammonia activated mixture of accomplishing for embodiment 1 installs additional adopts high-purity industrial ammonia bottle through subsequent use pipe valve, in the top hole pressure scope of 0.4Mpa slowly fill ammonia, filling the ammonia time is 3h, fill ammonia before and after the tank body quality increase by 48%;
The tank body that completion is filled behind the ammonia is connected with automobile SCR system, and under the situation of ammonia spillage less than 10ppm, quality reduces 43% before and after the test tank body desorption.
Embodiment 5
The tank body that the storage ammonia activated mixture of accomplishing for embodiment 2 installs additional adopts high-purity industrial ammonia bottle through subsequent use pipe valve, in the top hole pressure scope of 0.2Mpa slowly fill ammonia, filling the ammonia time is 6h, fill ammonia before and after the tank body quality increase by 41%;
The tank body that completion is filled behind the ammonia is connected with automobile SCR system, and under the situation of ammonia spillage less than 10ppm, quality reduces 38% before and after the test tank body desorption.
Embodiment 6
The tank body that the storage ammonia activated mixture of accomplishing for embodiment 3 installs additional adopts high-purity industrial ammonia bottle through subsequent use pipe valve, in the top hole pressure scope of 0.5Mpa slowly fill ammonia, filling the ammonia time is 5h, fill ammonia before and after the tank body quality increase by 51%;
The tank body that completion is filled behind the ammonia is connected with automobile SCR system, and under the situation of ammonia spillage less than 10ppm, quality reduces 45% before and after the test tank body desorption.
Claims (3)
1. porous active storage ammonia mixture preparation that contains molecular sieve; It is characterized in that the preparation method is following: press the powder of mass fraction with 45 ~ 90 parts industrial anhydrous calcium chloride salt; Mix industrial ball clay and 1 ~ 8 part of molecular sieve of 2 ~ 15 parts, become uniform mixture wet feed with 4 ~ 17 parts deionized water with 3 ~ 15 parts industrial alcohol mechanical stirring again, be filled in the tank body; Addition is no more than tank body volumetrical 80%, and machinery concussion 5 ~ 10min eliminates the clearance; Whole tank body is put in the vacuum drying oven, and normal pressure is slowly heating down, and temperature is controlled at 65 ~ 160 ℃; Get rid of water and ethanol to mixture constant weight, substep is evacuated to 550mbar, constant temperature and pressure 0.5 ~ 3h; Take out tank body, the sealing charging opening is processed the whole porosu solid piece of storage ammonia activated mixture; Ammonia is filled in the tank body under 0.05 ~ 0.8MPa pressure, saturated to the mixture absorbing ammonia.
2. a kind of porous active storage ammonia mixture preparation that contains molecular sieve according to claim 1 is characterized in that described molecular sieve bore diameter scope at 2 ~ 30nm, and specific surface area is greater than 300m
2/ g.
3. a kind of porous active storage ammonia mixture preparation that contains molecular sieve according to claim 1 is characterized in that described tank body is the withstand voltage tank body of stainless steel, inner tank wall thermospray nylon thermal insulation layer.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108367268A (en) * | 2015-12-07 | 2018-08-03 | 国立大学法人广岛大学 | The manufacturing method of ammonia removal material, ammonia-removal method and hydrogen for fuel cell vehicle |
| CN114952203A (en) * | 2022-06-28 | 2022-08-30 | 重庆大学 | Magnesium-based alloy-molecular sieve composite hydrogen storage material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101128394A (en) * | 2005-02-03 | 2008-02-20 | 氨合物公司 | High density storage of ammonia |
| CN101149007A (en) * | 2006-09-18 | 2008-03-26 | 福特环球技术公司 | A method of managing ammonia vapour when engine in stop state |
| WO2009138296A2 (en) * | 2008-05-13 | 2009-11-19 | Robert Bosch Gmbh | Device, system and method for providing a reducing agent for a system for the selective catalytic reduction of nitrogen oxides |
-
2012
- 2012-07-11 CN CN201210238807.XA patent/CN102730716B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101128394A (en) * | 2005-02-03 | 2008-02-20 | 氨合物公司 | High density storage of ammonia |
| CN101149007A (en) * | 2006-09-18 | 2008-03-26 | 福特环球技术公司 | A method of managing ammonia vapour when engine in stop state |
| WO2009138296A2 (en) * | 2008-05-13 | 2009-11-19 | Robert Bosch Gmbh | Device, system and method for providing a reducing agent for a system for the selective catalytic reduction of nitrogen oxides |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108367268A (en) * | 2015-12-07 | 2018-08-03 | 国立大学法人广岛大学 | The manufacturing method of ammonia removal material, ammonia-removal method and hydrogen for fuel cell vehicle |
| CN114952203A (en) * | 2022-06-28 | 2022-08-30 | 重庆大学 | Magnesium-based alloy-molecular sieve composite hydrogen storage material and preparation method thereof |
| CN114952203B (en) * | 2022-06-28 | 2024-02-20 | 重庆大学 | Magnesium-based alloy-molecular sieve composite hydrogen storage material and preparation method thereof |
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