CN102728303B - A kind of porous active storage ammonia active mixture of magnesium salts and preparation - Google Patents
A kind of porous active storage ammonia active mixture of magnesium salts and preparation Download PDFInfo
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- CN102728303B CN102728303B CN201210238810.1A CN201210238810A CN102728303B CN 102728303 B CN102728303 B CN 102728303B CN 201210238810 A CN201210238810 A CN 201210238810A CN 102728303 B CN102728303 B CN 102728303B
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Abstract
The present invention relates to a kind of porous active storage ammonia mixture and preparation of magnesium salts, it is characterized in that: the powder adopting the anhydrous chlorination magnesium salts of industry, mix appropriate molecular sieve, Ludox, deionized water and industrial alcohol, the Homogeneous phase mixing wet feed of mechanical agitation furnishing semi-drying, be filled in tank body, make Integrate porous solid block, ammonia conveying hole in this solid block is enriched, macroscopically possess some macropores, possess and fill ammonia faster and store up ammonia performance preferably, ammonia can be discharged fast, can recycle not broken, possess efficient adsorption and conciliate characterization of adsorption, be applicable to the adsorption storage of ammonia, for SCR and FCEV system, meet the application demand of future automobile industry.
Description
Technical field
The present invention relates to a kind of porous storage ammonia active mixture and preparation of magnesium salts, be applied to SCR aftertreatment system and the FCEV fuel cell system of vehicle exhaust.
Background technology
Current, the whole world faces the integration challenges of the energy and environment.In the technological means selection of the emission compliance of orthodox car, and the fuel supply technical elements people of new-energy automobile still face many difficult problems.
SCR aftertreatment system relies on the accurate supply of carbamide reducing agent and resolves into ammonia De NO X hazardous material afterwards in the front end of catalyst, reach the object of cleaning of off-gas, the standard of the state 4 realizing vehicle or more up to standard, but, in actual use, this dependence urea decomposition becomes the metered injection of the liquid area of ammonia to there is many deficiencies and difficult point, such as, the problem of urea liquid icing blocking under-11 DEG C of environment, needs extra pipeline heating system to solve, could decompose under the temperature environment of urea liquid more than 135 DEG C, and many vehicles of public transit system loiter, urea liquid stable decomposition temperature cannot be reached at all, cannot output ammonia, predetermined NOX composition cannot be eliminated, finally cause the accumulation of liquid area in blast pipe, produce the polymer of melamine, blocking urea nozzle and the exhaust pipe of engine, vehicle is caused to produce fault, impact is normal to be used, in addition, if the main flow vehicle of state more than 4 uses SCR system comprehensively, relate to the problem of about 150,000, whole nation oiling website Innovation Construction liquid area filling infrastructure, huge owing to investing, still do not see that Government and enterprise starts to improve this infrastructure at present, become SCR use in a potential huge problem,
For breakthrough energy dilemmas, solve the new-energy automobile development problem of future source of energy problem, it is a very important technology path that hydrogen fuel cell is recognized, but, how stable acquisition hydrogen source is a no small difficult problem for restriction this area development, likely in adopted hydrogen source mode, gas cylinder is had to store up the technology path of hydrogen, there is the technology path of water electrolysis hydrogen production, there is the technology path of high-purity hydrocarbon petroleum fuels cracking hydrogen production, the presoma decomposition of the technology path of low molecule alcohols cracking hydrogen production and the hydrogeneous of other H-N or the technology path of cracking hydrogen production, in above-mentioned technology path, all there is some problem and deficiency, such as, hydrogen production efficiency and cost, hydrogen manufacturing precision and speed, also the problem of system aspects is comprised, in a word, the source of hydrogen is the bottleneck of fuel-cell vehicle development, people's idea is needed to solve,
The presoma of hydrogen one of them be the hydrogeneous compound of H-N, wherein, what hydrogen-storage density was the highest is ammonia.Ammonia is a kind of modal industrial chemicals, and ammonia molecule belongs to active polar molecule, and the diameter dimension of molecule is about 3 ~ 4A, and therefore, very active under normal temperature, very easily spreads, and have toxic, its toxic is embodied in has corrosion and spread effect to the skin histology of contact, can absorb the moisture in skin histology, make histone sex change, and make tissue fat saponification, destroys membrane structure, ammonia in water solubility high, so mainly have stimulation and corrosiveness to the upper respiratory tract of animal or human's body, often be attracted on mucocutaneous and eye conjunctiva, thus produce stimulation and inflammation, in addition, ammonia sucks human body usually in gaseous form, easily blood is entered by alveolar after ammonia is inhaled into lung, be combined with hemoglobin, destroy fortune oxygen function, enter IA ammonia, small part is neutralized by carbon dioxide, remainder is absorbed into blood, there will be after sucking a large amount of ammonia in a short time and shed tears, pharyngalgia, cough, uncomfortable in chest, expiratory dyspnea, dizzy, vomiting, weak etc., if the long-term ammonia sucked is too much, cause ammonia density in blood too high, will cause heart stop fight and breathe stopping, threat to life safety, therefore, the maximum hidden danger of the use of ammonia is safety problem.
As can be seen here, resolve in the use of ammonia and store and safety problem, just can open up the technology path of a new ammonia utilization.
Traditional ammonia storing mode is gas cylinder, or realizes with the water-soluble formation ammoniacal liquor of high concentration ammonia.If adopt gas cylinder to store ammonia, there is the potential safety hazard of operating aspect and seal aspect in commercial Application in enormous quantities, if in the mode of high concentrated ammonia liquor, there is again serious etching problem.
At China national patent information net, to be the theme word and search to store up ammonia, ' composite functional ammonia storage device ' that the patent No. is ' a kind of Urotropine tail gas ammonia recovery device with gas phase method ' of CN201120099229.7, the patent No. is CN201020677361.7 ' the Pei An bindiny mechanism for machine room of refrigerated warehouse ', the patent No. are CN201020269811.9, the patent No. are ' a kind of ammonia steaming device ' of CN200520057558.X, be that a class carries out to ammonia nitrogen industrial wastewater the environment protection treating device that ammonia nitrogen gets rid of process, also do not relate to the characteristic component in the present invention.Uncorrelated with the present invention;
These 2 inventions of the patent No. to be ' method and system for testing to the work of SCR catalyst ' of CN201010244091.5 and the patent No. be ' operation method of SCR exhaust after treatment system and the diagnostic method ' of CN200880104697.X provide a kind of for SCR (SCR) catalytic converter and traditional liquid ureaclastic ammonia dispensing module and control system, do not relate to the characteristic component of compound;
The patent No. is that the invention of ' a kind of preparation method of efficient low-temperature ammonia-storing material ' of CN200910197860.8 is applied to SCR aftertreatment system, feature is that amino borane compound is placed in closed container, vacuumize, at 0-4 DEG C of temperature, contact with ammonia, at 0-4 DEG C of temperature, keep 30-60 minute, prepare required product amino borane ammino-complex NH3BH3 (NH3) n (n=1-3); The maximum storage ammonia amount of room temperature can reach 62.4wt.%, room temperature supply gas pressure about 2.0bar, room temperature is moderate for ammonia pressure, ammonia completely reversibility is put in suction, but the extraordinary material amino borane of this patent is expensive, there is higher explosion danger and burning grade, be not suitable for applying in enormous quantities of general industry field;
The patent No. is that the invention of the solid material of delivering ammonia ' store and ' of CN200580026626.9 relates to and storing and the solid material of delivering ammonia.The solid material of this storage ammonia comprises a kind of ammonia and absorbs salt, and wherein this ammonia absorption salt is general formula is M
a(NH
3)
nx
zionic salt, wherein M is one or more cations being selected from alkaline-earth metal and/or one or more transition metal such as Mn, Fe, Co, Ni, Cu and/or Zn, X is one or more anion, a is the cation number that each molecules of salt comprises, z is the anion number that each molecules of salt comprises, n is the ligancy of 2 ~ 12, and wherein M is Mg, and it is that auto industry ammonia provides a kind of safety, lightweight, cheap and fine and close storage that this ammonia absorbs salt.This patent is that electric heating adds Thermal desorption ammonia direct for solid material compression molding, more lays particular emphasis on the control strategy of system, does not relate to modification and the optimization of mixture;
The patent No. is that ' purposes of ammonia storage device in energy production ' invention of CN200580009219.7 relates to a kind of generator unit, and this unit comprises the ammonia storage device of (i) container (2) form, and comprising general formula is M
a(NH
3)
nXzammonia absorb with release salt, wherein M is one or more cations, be selected from alkali metal, alkaline-earth metal and transition metal are as Li, K, Mg, Ca, V, Cr, Mn, Fe, Co, Ni, Cu or Zn, X is one or more anion, be selected from fluorine root, chlorine root, bromine root, iodine root, nitrate anion, thiocyanate radical, sulfate radical, molybdate, phosphate radical and chloranion, a is the cation number of each molecules of salt, z is the anion number of each molecules of salt, and n is the ligancy of 2-12, (ii) for heating described container (2) and ammonia absorption and release salt to discharge the device (3a) of ammonia, (iiia) for ammonia being converted into the fuel cell of electrical power, or (iiib1) for ammonia being dissociated into the reactor (6) of hydrogen and nitrogen, (iiib2) for hydrogen being converted into the fuel cell (4) of electrical power, this patent is mainly used in fuel cell, refer to property material in claim 4 for such salt or be positioned on porous carrier materials, which kind of material statement is not,
A kind of amido complex compound of the disclosure of the invention of CN200710156866.1 ' a kind of amido complex compound and its production and use ' and its production and use.The composition of this amido complex compound is MX
m(NH
3)
n, in formula, M is one or more in Li, Mg, Al, Ca, Sc, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Sr, Ba, Sn; X is F, Cl, Br, NO
3, SO
4in one or more; M determines according to chemical valence, 1≤m≤5; N determines according to ligancy, 1≤n≤15.Using the amido complex compound after deamination as the absorbent of ammonia, inhale ammonia by low temperature, high temperature puts ammonia and realize the separation of ammonia, purification, storage and transport.This patent only relates to preparation technology and the process of this amido complex compound itself;
The patent No. is that the solid ammonia that ' high-density city of ammonia ' patent of CN200680005886.2 comprises ammonia absorption/desorption solid material stores and conveying material, the described density that has been compacted to is greater than the storage of 50% of theoretic skeleton density and carries material to provide solid ammonia storage material, this storage medium is easily prepared and is processed and have the storage ammonia of very high-density, described storage ammonia easily discharges under controlled conditions, even if the porosity of described material is very low still like this, and this storage medium is safe for storage and delivering ammonia, does not need special safety measure.This patent adopts the direct compression molding of solid material, adopt binding agent, only stating may be silicon dioxide fibre binding agent, not dosage ratio, also only state that solid material may comprise granular materials, porous material, crystalline material, amorphous materials or their bond composition in other claim and embodiment, do not have the thin item of clear and definite claim, industry technology personage almost cannot implement.Create the present invention therefrom.
Summary of the invention
The object of the present invention is to provide a kind of porous storage ammonia active mixture preparation of magnesium salts, in order to improve the hole of storage ammonia active material solid block, increasing ammonia transmission channel, weaken or avoid repeatedly MgCl in sorption and desorption additive process
2the efflorescence fragmentation of the caking occurred and solid block, what meet industrial occasions repeatedly recycles requirement, possesses efficient adsorption and conciliates characterization of adsorption, be applicable to the adsorption storage of ammonia, for SCR and FCEV system, meet the application demand of future automobile industry.
Technical scheme of the present invention is achieved in that a kind of porous storage ammonia active mixture of magnesium salts, it is characterized in that: by the powder of mass fraction by anhydrous for the industry of 45 ~ 90 parts chlorination magnesium salts, mix the Ludox of 2 ~ 15 parts, 1 ~ 8 part of molecular sieve, mix with the deionized water of 4 ~ 17 parts and the industrial alcohol of 3 ~ 15 parts.
The preparation method of described mixture is as follows: by the powder of the anhydrous chlorination magnesium salts of industry, mix appropriate molecular sieve, Ludox, deionized water and industrial alcohol, through mechanical agitation uniformly mixture wet feed, be filled in tank body, addition is no more than 80% of tank volume, and machinery concussion 5 ~ 10min eliminates the air gap; Whole tank body is put in vacuum drying oven, slowly heats under normal pressure, and temperature controls at 65 ~ 160 DEG C, eliminating water and ethanol are to mixture constant weight, and substep is evacuated to 550mbar, constant temperature and pressure 0.5 ~ 3h, take out tank body, sealing charge door, make storage ammonia active mixture Integrate porous solid block; Ammonia is filled in tank body under 0.05 ~ 0.8MPa pressure, saturated to mixture absorbing ammonia.
Described molecular sieve bore diameter scope is at 2 ~ 30nm, and specific area is greater than 300m
2/ g.
Described industrial clay particle diameter is less than 2um, and in water, disperse becomes suspension.
Described tank body is the withstand voltage tank body of stainless steel, inner tank wall thermal spraying nylon heat-insulation layer.
Good effect of the present invention optionally adds Ludox, and particle diameter is herein at 10 ~ 20nm, and density is at 1.15g/cm
3, dioxide-containing silica 25%, pH value 8 ~ 10, in water, disperse becomes suspension, by means of mechanical agitation and MgCl
2and other fillers fully mix, at MgCl
2bridging between particle, forms mechanical strength higher " integrated solid block " after dry, can effectively weaken or avoid the efflorescence fragmentation that the dilation of solid block in sorption and desorption additive process causes; The water added and ethanol dissolve and differential falls apart MgCl
2and other fillers, improve the wetting and spreading between liquid-solid two-phase, in addition, the hole that process is formed deviate from by water and ethanol, enriched the transmission channel of ammonia; The molecular sieve added, facilitates MgCl
2dispersion, can effectively weaken or avoid the generation of caking phenomenon, improve the richness of microscopic void, add the transmission channel of ammonia, greatly improve the permeance property of ammonia, promote the formation of ammoniation magnesium chloride complex compound, the loose structure of molecular sieve itself, possesses certain absorption and memory function to ammonia simultaneously; The pore diameter range herein selected is at 2 ~ 30nm, and specific area is greater than 300m
2/ g; The molecular sieve added is dispersed in MgCl
2in particle, can effectively weaken or eliminate the generation of caking phenomenon, improve the richness of microscopic void, add the internal transmission passage of ammonia, greatly improve the permeance property of ammonia, promote the formation of ammoniation magnesium chloride complex compound; In order to ensure security at elevated pressures, tank body used is the withstand voltage tank body of stainless steel, inner tank wall thermal spraying nylon heat-insulation layer.
To sum up, the molecular sieve added improves the richness of microcosmic nano-pore, add the quantity of macroscopic pores, the Ludox added and molecular sieve weaken or avoid the phenomenon of the ammonia gas absorption desorption that caking, fragmentation etc. cause, improve the richness of microscopic void, add the quantity of macroscopic pores, improve the mechanical strength of composition sample block, there is very high practical value, be suitable for SCR post processing or the FCEV system of automobile industry.
Accompanying drawing explanation
The thermogravimetric curve of the active mixture of the absorbing ammonia of Fig. 1 embodiment of the present invention 1.
Detailed description of the invention
Further describe the present invention below by embodiment, embodiment, for illustrate feature of the present invention further, is not equal to restriction the present invention, for the change that those skilled in the art carries out according to the present invention, all should be included within protection scope of the present invention.
embodiment 1
By the water of the magnesium chloride of 71 parts, 3 parts of molecular sieves, 6 parts of Ludox and 12 parts, in homogenizer, mix 1h, add 8 parts of ethanol, continue mechanical agitation 3h, make uniform mixture wet feed, be filled in tank body, be added into 80% of tank volume, machinery concussion 10min eliminates the air gap;
Whole tank body is put in vacuum drying oven, rises to 120 DEG C as shown in Figure 1 under normal pressure with the heating rate of 2 DEG C/min, constant temperature 6h, get rid of water and ethanol, substep is evacuated to 550mbar, constant temperature and pressure 1h, take out tank body, sealing charge door, make storage ammonia active mixture Integrate porous solid block.
embodiment 2
By the water of 2 parts of molecular sieves, 18 parts of Ludox and 15 parts, 1h is mixed in homogenizer, add the magnesium chloride mixing 1h of 55 parts, add 10 parts of ethanol, continue mechanical agitation 3h, make uniform mixture wet feed, be filled in tank body, be added into 75% of tank volume, machinery concussion 10min eliminates the air gap;
Whole tank body is put in vacuum drying oven, rises to 120 DEG C under normal pressure with the heating rate of 2 DEG C/min, constant temperature 6h, get rid of water and ethanol, substep is evacuated to 550mbar, constant temperature and pressure 1h, take out tank body, sealing charge door, make storage ammonia active mixture Integrate porous solid block.
embodiment 3
By the water of 4 parts of Ludox and 6 parts, 1h is mixed in homogenizer, add the magnesium chloride mixing 1h of 81 parts, add 3 parts of molecular sieve mixing 1h, add 6 parts of ethanol, continue mechanical agitation 3h, make uniform mixture wet feed, be filled in tank body, be added into 80% of tank volume, machinery concussion 10min eliminates the air gap;
Whole tank body is put in vacuum drying oven, rises to 100 DEG C under normal pressure with the heating rate of 5 DEG C/min, constant temperature 8h, get rid of water and ethanol, substep is evacuated to 550mbar, constant temperature and pressure 2h, take out tank body, sealing charge door, make storage ammonia active mixture Integrate porous solid block.
embodiment 4
The tank body that the storage ammonia active mixture completed for embodiment 1 installs additional, adopt high-purity industrial ammonia bottle by pipe valve for subsequent use, slowly carry out filling ammonia in the inlet pressure ranges of 0.4Mpa, filling the ammonia time is 3h, and filling tank body quality before and after ammonia increases by 42%;
Complete the tank body after filling ammonia to be connected with automobile SCR system, when NH_3 leakage amount is less than 10ppm, Mass lost 38% before and after test tank body desorption.
embodiment 5
The tank body that the storage ammonia active mixture completed for embodiment 2 installs additional, adopt high-purity industrial ammonia bottle by pipe valve for subsequent use, slowly carry out filling ammonia in the inlet pressure ranges of 0.2Mpa, filling the ammonia time is 6h, and filling tank body quality before and after ammonia increases by 37%;
Complete the tank body after filling ammonia to be connected with automobile SCR system, when NH_3 leakage amount is less than 10ppm, Mass lost 33% before and after test tank body desorption.
embodiment 6
The tank body that the storage ammonia active mixture completed for embodiment 3 installs additional, adopt high-purity industrial ammonia bottle by pipe valve for subsequent use, slowly carry out filling ammonia in the inlet pressure ranges of 0.5Mpa, filling the ammonia time is 5h, and filling tank body quality before and after ammonia increases by 38%;
Complete the tank body after filling ammonia to be connected with automobile SCR system, when NH_3 leakage amount is less than 10ppm, Mass lost 34% before and after test tank body desorption.
Claims (2)
1. the porous storage ammonia active mixture of a magnesium salts, it is characterized in that: by the powder of mass fraction by anhydrous for the industry of 45 ~ 90 parts chlorination magnesium salts, mix the Ludox of 2 ~ 15 parts, 1 ~ 8 part of molecular sieve, with the deionized water of 4 ~ 17 parts and the industrial alcohol of 3 ~ 15 parts, mechanical agitation is mixture wet feed uniformly, be filled in tank body, addition is no more than 80% of tank volume, and machinery concussion 5 ~ 10min eliminates the air gap; Whole tank body is put in vacuum drying oven, slowly heats under normal pressure, and temperature controls at 65 ~ 160 DEG C, eliminating water and ethanol are to mixture constant weight, and substep is evacuated to 550mbar, constant temperature and pressure 0.5 ~ 3h, take out tank body, sealing charge door, make storage ammonia active mixture Integrate porous solid block; Ammonia is filled in tank body under 0.05 ~ 0.8MPa pressure, saturated to mixture absorbing ammonia.
2. the porous storage ammonia active mixture of a kind of magnesium salts according to claim 1, it is characterized in that described molecular sieve bore diameter scope is at 2 ~ 30nm, specific area is greater than 300m
2/ g; Tank body is the withstand voltage tank body of stainless steel, inner tank wall thermal spraying nylon heat-insulation layer.
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Citations (5)
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| GB9810387D0 (en) * | 1998-05-15 | 1998-07-15 | Crosfield Joseph & Sons | Process for adsorbing gas |
| JP2003305461A (en) * | 2002-04-16 | 2003-10-28 | Nippon System Products Kk | Element for removing ammonia-nitrogen in liquid and method for manufacturing the same |
| CN101128394A (en) * | 2005-02-03 | 2008-02-20 | 氨合物公司 | High density storage of ammonia |
| CN101584999A (en) * | 2008-05-20 | 2009-11-25 | 揖斐电株式会社 | Honeycomb structure |
| CN101982232A (en) * | 2010-10-29 | 2011-03-02 | 烟台大学 | Deaminizing agent and preparation method thereof |
-
2012
- 2012-07-11 CN CN201210238810.1A patent/CN102728303B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB9810387D0 (en) * | 1998-05-15 | 1998-07-15 | Crosfield Joseph & Sons | Process for adsorbing gas |
| JP2003305461A (en) * | 2002-04-16 | 2003-10-28 | Nippon System Products Kk | Element for removing ammonia-nitrogen in liquid and method for manufacturing the same |
| CN101128394A (en) * | 2005-02-03 | 2008-02-20 | 氨合物公司 | High density storage of ammonia |
| CN101584999A (en) * | 2008-05-20 | 2009-11-25 | 揖斐电株式会社 | Honeycomb structure |
| CN101982232A (en) * | 2010-10-29 | 2011-03-02 | 烟台大学 | Deaminizing agent and preparation method thereof |
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