CN102728319B - A kind of porous active storage ammonia active mixture preparation containing expanded graphite - Google Patents
A kind of porous active storage ammonia active mixture preparation containing expanded graphite Download PDFInfo
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- CN102728319B CN102728319B CN201210238845.5A CN201210238845A CN102728319B CN 102728319 B CN102728319 B CN 102728319B CN 201210238845 A CN201210238845 A CN 201210238845A CN 102728319 B CN102728319 B CN 102728319B
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Abstract
The present invention relates to a kind of porous active storage ammonia mixture preparation containing expanded graphite, it is characterized in that: the powder adopting the anhydrous calcium chloride salt of industry, mix appropriate clay, expanded graphite, 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 active storage ammonia active mixture preparation containing expanded graphite, 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 NH
3bH
3(NH
3) 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 active storage ammonia mixture preparation containing expanded graphite, in order to improve the hole of storage ammonia active material solid block, increasing ammonia transmission channel, weaken or avoid repeatedly CaCl in sorption and desorption additive process
2the efflorescence fragmentation of the caking occurred and solid block, what meet industrial occasions repeatedly recycles requirement, it possesses and fills ammonia and good storage ammonia performance faster, 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.
Technical scheme of the present invention is achieved in that a kind of porous active storage ammonia mixture preparation containing expanded graphite, it is characterized in that preparation method is as follows: by the powder of mass fraction by anhydrous for the industry of 48 ~ 90 parts calcium chloride salt, mixing is industrial ball clay, 0.5 ~ 6 part of expanded graphite of 2.5 ~ 15 parts, with the deionized water of 4 ~ 16 parts and the industrial alcohol of 3 ~ 15 parts 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 industrial ball clay particle diameter is less than 2um, and in water, disperse becomes suspension.
The expansion multiplying power of described expanded graphite is 250 ~ 380ml/g, particle diameter≤15um.
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 expanded graphite, and expansion multiplying power is herein 250 ~ 380ml/g, particle diameter≤15um.The graphite plane layer of expanded graphite is polygon or slit shape and corresponding parallel cinclides thereof or wedge hole, expanded graphite is made to have excellent compression resilience and less thermal coefficient of expansion, for calcium chloride is in the volumetric expansion of sorption and desorption process with reduce and provide enough spaces, ensure that the performance of mixture can not change.High porosity makes gas easily via abundant pore structure, can carry out adsorption and desorption; Expanded graphite facilitates CaC1
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 ammino calcium chloride complex compound; The particle diameter added is less than the industrial ball clay of 2um, and in water, disperse becomes suspension, by means of mechanical agitation and CaC1
2and other fillers fully mix, at CaC1
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 CaC1
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; To sum up, the activity storage ammonia mixture that microcosmic nano pore containing expanded graphite is abundant, ensure that under the prerequisite that storage ammonia active material characteristic is constant, the clay added and expanded graphite weaken or eliminate 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 calcium chloride of 69 parts, 3 parts of expanded graphites, 8 parts of clays 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 expanded graphites, 18 parts of clays and 15 parts, 1h is mixed in homogenizer, add the calcium 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 5 parts of clays and 6 parts, 1h is mixed in homogenizer, add the calcium chloride mixing 1h of 80 parts, add 3 parts of expanded graphite 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 36%;
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 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 32%;
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 30% 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 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 32% before and after test tank body desorption.
Claims (3)
1. the porous active storage ammonia preparation method of mixture containing expanded graphite, it is characterized in that preparation method is as follows: by the powder of mass fraction by anhydrous for the industry of 48 ~ 90 parts calcium chloride salt, mixing is industrial ball clay, 0.5 ~ 6 part of expanded graphite that 2.5 ~ 15 parts of particle diameters are less than 2 μm, with the deionized water of 4 ~ 16 parts and the industrial alcohol of 3 ~ 15 parts 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.
2. a kind of porous active storage ammonia preparation method of mixture containing expanded graphite according to claim 1, is characterized in that described industrial ball clay disperse in water becomes suspension.
3. a kind of porous active storage ammonia preparation method of mixture containing expanded graphite according to claim 1, is characterized in that the expansion multiplying power of described expanded graphite is 250 ~ 380mL/g, particle diameter≤15 μm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1569324A (en) * | 2004-04-29 | 2005-01-26 | 上海交通大学 | Calcium chloride-active carbon mixed adsorbent |
| CN1613551A (en) * | 2004-09-29 | 2005-05-11 | 上海交通大学 | Calcium-expanding black lead mixed adsorbent |
| CN1899683A (en) * | 2006-07-05 | 2007-01-24 | 南京工业大学 | Attapulgite lay base composite adsorbent for ammonia adsorption refrigeration and its preparing and use |
| CN101128394A (en) * | 2005-02-03 | 2008-02-20 | 氨合物公司 | High density storage of ammonia |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20070057143A (en) * | 2004-08-03 | 2007-06-04 | 아미넥스 에이/에스 | A solid ammonia storage and delivery material |
| RU2395335C2 (en) * | 2005-02-03 | 2010-07-27 | Амминекс А/С | Storage of high-content ammonia |
-
2012
- 2012-07-11 CN CN201210238845.5A patent/CN102728319B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1569324A (en) * | 2004-04-29 | 2005-01-26 | 上海交通大学 | Calcium chloride-active carbon mixed adsorbent |
| CN1613551A (en) * | 2004-09-29 | 2005-05-11 | 上海交通大学 | Calcium-expanding black lead mixed adsorbent |
| CN101128394A (en) * | 2005-02-03 | 2008-02-20 | 氨合物公司 | High density storage of ammonia |
| CN1899683A (en) * | 2006-07-05 | 2007-01-24 | 南京工业大学 | Attapulgite lay base composite adsorbent for ammonia adsorption refrigeration and its preparing and use |
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