CN101961644B - Chloride-carbonaceous skeleton composite adsorbent and preparation method thereof - Google Patents
Chloride-carbonaceous skeleton composite adsorbent and preparation method thereof Download PDFInfo
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- CN101961644B CN101961644B CN2010102929423A CN201010292942A CN101961644B CN 101961644 B CN101961644 B CN 101961644B CN 2010102929423 A CN2010102929423 A CN 2010102929423A CN 201010292942 A CN201010292942 A CN 201010292942A CN 101961644 B CN101961644 B CN 101961644B
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Abstract
The invention belongs to the fields of adsorptive refrigeration/heat pumps, adsorptive separation purification and hydrogen storage, and particularly relates to a chloride-carbonaceous skeleton composite adsorbent and a preparation method thereof. The adsorbent is characterized by comprising the following raw materials: based on a carbonaceous precursor, 0.5 to 2 percent of chloride, 0 to 25 percent of adhesive and 0 to 50 percent of heat conducting material. The preparation method for the chloride-carbonaceous skeleton composite adsorbent is characterized by comprising the steps of crushing of the carbonaceous precursor, preparation of impregnation liquid, impregnation of the carbonaceous precursor, forming, air-blasting drying, carbonization and activation and the like. The adsorbent prepared by the method fully solves the problem of mass transfer coefficient decline caused by filling the chloride and pressing a plugging micropore at the same time of ensuring efficient heat transfer, and obviously improves the loading strength and the utilization rate of the chloride.
Description
Technical field
The invention belongs to absorption refrigeration/heat pump, the purification of transformation adsorbing separation and hold the hydrogen technical field.Be particularly related to a kind of chloride-carbonaceous skeleton compound adsorbent and preparation method thereof.
Background technology
Along with people's is to the intensification of energy-conserving and environment-protective understanding, and low-carbon economy will progressively become global awareness form and international mainstream values, and low-carbon economy has become the focus of development of world economy with its special advantages and huge market.The main body refrigeration modes is the electricity refrigeration at present, needs the high-grade electric energy of labor.Absorption refrigeration/heat pump techniques is because it utilizes regenerative resources such as low-grade heat source and solar energy as drive energy; And the natural materials that makes environmentally friendly property such as water, ammonia and alcohols is as cold-producing medium; Become a focus of refrigerating field research and development, the adsorbent of wherein researching and developing superior performance is very big for this The Application of Technology influence.The adsorbent of absorption refrigeration/heat pump employing mainly contains physical absorbent, chemosorbent and mixing/compound adsorbent at present.Wherein the physical absorbent adsorbance is little, and luming can appear in chemosorbent, expansion causes adsorbent mass-and heat-transfer difference and performance degradation is serious.For solving these shortcomings, the advantage of comprehensive physical absorbent and chemosorbent is all over the body, and the mixing/compound adsorbent of exploitation superior performance becomes one of important process of current absorption refrigeration research.Study more calcium chloride-active carbon mixed adsorbent at present; Utilize cement or gypsum to cohere curing molding after adopting simple the mixing; Better solve chemosorbent because of the obvious difficult problem that descends of adsorption capacity that the caking that expands causes, improved its antidamping ability greatly.But simple mix the just mixing of macroscopic view, can not overcome chloride particulate caking phenomenon fully, be easy to cause chloride to sinter piece in micropore inside near reaching vitrification point such as heat source temperature, adsorption capacity sharply descends.Simultaneously, can cause a large amount of micropores to stop up when the chloride load capacity is too high, can reduce, reduce mass-transfer efficiency with the adsorbance under the operating mode.Solidify adsorbent through adding cement or gypsum, can improve heat exchange efficiency, but reduce the unit mass refrigerating capacity of adsorbent, increased resistance to mass tranfer.Other in the world at present a kind of general adsorbent preparation method is the porous media infusion process, is published in the Isothermal sorptioncharacteristics of the BaCl on " Applied Thermal Engineering " like Y.Zhong
2-NH
3Advantages such as the barium chloride/vermiculite compound adsorbent preparation method in pair in a vermiculite host matrix one literary composition, its result of study show that compound adsorbent that this method is made has that mass-transfer performance is good, barium chloride utilization rate height and chloride are not scattered.Excessive or when adopting the adhesive cures moulding when load capacity, also exist blocking microporous, influence adsorbent mass transfer ability force phenomenon.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned prior art, provide that a kind of chloride utilization rate is high, mass transfer effect is good and can significantly reduce chloride-carbonaceous skeleton compound adsorbent of heat exchanger and adsorbent thermal contact resistance and preparation method thereof.
The present invention realizes in the following manner:
A kind of chloride-carbonaceous skeleton compound adsorbent, it is characterized in that its raw material and each set of dispense are such as following: with the carbonaceous predecessor is benchmark, and chloride is 0.5～2 times of its quality, and binding agent is 0～25% of its quality, and Heat Conduction Material is 0～50% of its quality.Wherein the carbonaceous predecessor is to being used for making the raw material general designation of carbon or absorbent charcoal material.
Above-mentioned chloride-carbonaceous skeleton compound adsorbent is characterized in that: described carbonaceous predecessor be shell, fruit stone, timber, stalk, mud, bituminous coal, anthracite, brown coal, carbonized material, paper pulp at least a; Said chloride is CaCl
2, MnCl
2, SrCl
2, FeCl
2, BaCl
2, PbCl
3One of; Said binding agent is at least a in starch and starch ether, polyvinyl alcohol, cellulose ether (like methylcellulose, ethyl cellulose, CMC, hydroxyethylcellulose, hydroxypropyl cellulose), secondary stock, the coal tar; Said Heat Conduction Material be copper, iron, aluminium, carborundum etc. not with powder or the silk screen of absorption working pair to strong Heat Conduction Material that chemical reaction takes place.
The preparation method of above-mentioned chloride-carbonaceous skeleton compound adsorbent is characterized in that may further comprise the steps:
(1) fragmentation
It is 20～400 purpose particles that the carbonaceous predecessor is ground into particle diameter;
(2) preparation maceration extract
As solvent, chloride prepares maceration extract as solute with the solution (like water and alcohols) with higher solubility; Said maceration extract, its chloride quality concentration is 10～65%;
(3) dipping
The particle of the carbonaceous predecessor that step (1) is made is put into the made maceration extract dipping of step (2), and the duration is 2～24h, and its dipping temperature scope is normal temperature～120 ℃;
(4) moulding
Oven dry or the air-dry carbonaceous predecessor that is made by step (3) dipping add Heat Conduction Material and binding agent, insert mould compression moulding or insert the extruder extrusion modling after mixing evenly; Briquetting pressure is 2～20MPa;
(5) drying
Forced air drying; The forced air drying temperature is 60～140 ℃, until solvent less than 3%;
(6) carbonization-activation
Carbonization-activation under anaerobic or anaerobic environment; Its temperature is 350～800 ℃, and the carbonaceous predecessor burns the mistake rate less than 85%.
The preparation method of above-mentioned a kind of chloride-carbonaceous skeleton compound adsorbent makes powdery or granular adsorption agent if it is characterized in that said adsorbent, then crosses step (4), directly carries out step (5) and step (6).
Said adsorbent is used for absorption refrigeration/heat pump, adsorbing separation is purified and hold the hydrogen field, low temperature exhaust heat capable of using, used heat and solar energy regeneration, and regeneration temperature is 65 ℃～450 ℃.
The present invention is directed to chemosorbent, simply mix and the shortcoming of immersion-type compound adsorbent; The chloride that immerses the carbonaceous predecessor during in conjunction with high temperature has stronger water separation capability; Make H atom and O atom in the high-carbon raw material combine with the alkali metal ion coordination than generating water, then as the H of part with 2: 1 atom number
2O overflows through moving of coordination ionic dissociation equilibrium again, and at high temperature reacts with carbon, forms CO and H
2, whole process has been accomplished the erosion dissolving to carbonaceous predecessor inner cellulose, thereby reaches the activation purpose, forms the flourishing carbonaceous skeleton structure of micropore; Because microcellular structure is to be formed centrally in being with each chloride molecule; And according to spontaneous individual layer dispersion theory; In high temperature carbonization activation process, chloride can evenly form the individual layer dispersed structure at microcellular structure, with respect to the compound adsorbent of simple mixing or immersion-type; Improved micropore surface and muriatic utilization rate greatly, high temperature heat source can cause chloride in micropore sintered defective in can effectively overcoming; The formed absorbent that this method makes is that micropore forms preceding briquet, when guaranteeing efficient heat transfer, has overcome the mass transfer ability drop problem that the dipping chloride is blocking microporous and compression moulding destruction pore structure causes fully; High temperature carbonization activation process can make carbon intensive around muriatic, thereby has improved the intensity of load; Because adhesive is higher starch of phosphorus content or fiber substance, identical through after the carbonization-activation with the resulting product of carbonaceous predecessor carbonization-activation, can not influence mass transport process, can not reduce the unit mass adsorbance yet.
Compare with the prior art achievement; Beneficial effect of the present invention is specific as follows: according to muriatic high dehydrated; Carbonaceous predecessor behind the high temperature carbonization activation dipping; With after the carbonaceous predecessor is processed active carbon earlier again dip forming compare, reduced operations such as pickling, later stage drying, thereby reduced the generation of energy resource consumption and waste liquid and waste gas; High temperature carbonization activation process chloride forms uniform individual layer to be disperseed, and has improved micropore surface and muriatic utilization rate; Along with the carrying out of carbonization-activation, the carbon molecule is that the center is gathered with the chloride molecule, has strengthened the chloride intensity of load, has overcome the chemosorbent expansion, lumps and has dusted a difficult problem; Because of the briquetting process prior to micro molding, when guaranteeing heat transfer efficiency, solved mass transfer problem, and solved a difficult problem that causes a large amount of micropores to stop up behind the active carbon dip forming; Carbonaceous predecessor behind the dipping adopts the higher adhesive of carbon content to cohere moulding, the two is carbonization-activation simultaneously, has overcome the problem that adhesive hinders mass transfer, blocking microporous, the decrease of power density; If with the whole compression moulding of heat exchanger, carry out the activation charing then, can significantly reduce heat exchanger and adsorbent thermal contact resistance.
Specific embodiments
Provide five embodiment of the present invention below, but protection scope of the present invention is not limited to subordinate's embodiment.
Embodiment 1
Be ground into paulownia wood 200 grams less than 100 purpose particles earlier; In the beaker of a 1000ml, be dissolved in 200 gram calcium chloride in 90 ℃ the 200ml water, and add the paulownia wood powder that has made and stir, put into the oil bath case, keep constant temperature 12h; Scatter macerate in the beaker and put into air dry oven, 120 ℃ of baking temperatures, drying time 6h; Add 20 gram starch in the beaker, 60ml water stirs, and is heated to 90 ℃, till starch gelatinization finishes; Mix macerate and gelatinized starch that drying finishes evenly, form stiff mud shape thing, evenly put into mould then; Pressing pressure is 10MPa; After the compression moulding, put into the vacuum Muffle furnace and be heated to 500 ℃, keep this temperature 1h; Take out after being cooled to normal temperature, obtain calcium chloride-carbonaceous skeleton compound adsorbent.
The cavernous structure of the calcium chloride-carbonaceous skeleton compound adsorbent of present embodiment preparation be mesoporous be main loose structure, can be used for absorbing ammonia, methyl alcohol and ethanol etc.According to the absorption of ammonia test, the calcium chloride mass fraction is about 80%, and maximum ammonia adsorbance is about 0.97kg/kg, and the thermal conductivity factor maximum can reach 0.6W/ (mK).According to XRD analysis, calcium chloride forms even monolayer at micropore surface.In view of cost; This process has reduced pickling, finished product dry run and active carbon and the calcium chloride hybrid infusion dry run of making active carbon; Greatly reduce energy consumption, production process does not have harmful waste and produces, if its manufacturing cost of large-scale production should be about 1/2 of direct mixed type.
Embodiment 2
Stalk 100 grams and anthracite 100 grams mix and are ground into less than 100 purpose powder; In the beaker of a 1000ml, be dissolved in 200 gram manganese chlorides in 90 ℃ the 200ml water, add the stalk that made and the mixed-powder of bituminous coal and stir, put into constant temperature water tank, keep constant temperature 12h; Scatter macerate in the beaker and put into air dry oven, 120 ℃ of baking temperatures, drying time 4h; The macerate and the 30 gram ethyl cellulose powder mixes that finish drying are even, put into mould with an iron plate that has burr then, and are hot-forming; Together put into the vacuum Muffle furnace to obtained sample and iron plate and be heated to 500 ℃, keep this temperature 1h, take out after being cooled to normal temperature, obtain manganese chloride---carbonaceous skeleton compound adsorbent.
The cavernous structure of the manganese chloride of present embodiment preparation---carbonaceous skeleton compound adsorbent be mesoporous be main loose structure, can be used for absorbing ammonia, methyl alcohol and ethanol etc.The maximum characteristics of this kind preparation method are the whole compactings of adsorbent and heat exchanger and form by a firing, greatly reduce the thermal contact resistance between adsorbent and the heat exchanger.Find that according to test the hot coefficient of slug type complex heat transfer can reach 200-500W/ (m
2K), apparently higher than existing 100-150W/ (m
2K).
Embodiment 3
Coconut husk 100 grams are ground into less than 100 purpose particles, and almond carbonized material 100 grams are ground into less than 100 purpose particles; In the beaker of a 1000ml, be dissolved in 150 gram strontium chlorides in 90 ℃ the 100ml water, and add completed coconut husk and almond carbonized material powder stirs, put into the oil bath case, keep constant temperature 24h; Scatter macerate in the beaker and put into air dry oven, 120 ℃ of baking temperatures, drying time 2h; Add 30 gram secondary stocks and 50 gram carborundum powders in the beaker, mix macerate, secondary stock and carborundum powder that drying finishes evenly, form stiff mud shape thing; Evenly put into mould then, pressing pressure is 15MPa, after the compression moulding; Put into the vacuum Muffle furnace and be heated to 600 ℃; Keep this temperature 1h, take out after being cooled to normal temperature, obtain strontium chloride---carbonaceous skeleton compound adsorbent.
Present embodiment preparation strontium chloride---carbonaceous skeleton compound adsorbent can be used for absorbing ammonia.According to test, its thermal conductivity factor maximum can reach 5W/ (mK), and according to electron-microscope scanning, strontium chloride is uniformly dispersed in carbon skeleton inside.This kind adsorbent can be used for the circulation of air cooling absorption refrigeration because the adsorption-desorption temperature is higher.
Embodiment 4
Municipal sludge 200 grams that drying finishes are ground into less than 100 purpose particles; In the beaker of a 1000ml, be dissolved in 150 gram barium chlorides in 30 ℃ the 100ml ethanol, and add completed mud powder and stir, put into the oil bath case, keep constant temperature 24h; Scatter macerate in the beaker and put into air dry oven, 70 ℃ of baking temperatures, drying time 1h; Add 60ml water and 30 gram starch ethers guar gum ether powder in the beaker, mix macerate, guar gum ethereal solution and 50 gram aluminium wires that drying finishes evenly, form stiff mud shape thing; Evenly put into mould then, pressing pressure is 5MPa, after the compression moulding; Put into the vacuum Muffle furnace and be heated to 450 ℃; Keep this temperature 2h, take out after being cooled to normal temperature, obtain barium chloride---carbonaceous skeleton compound adsorbent.
Present embodiment preparation barium chloride---carbonaceous skeleton compound adsorbent can be used for absorbing ammonia.According to test, its thermal conductivity factor maximum can reach 4W/ (mK), and according to electron-microscope scanning, barium chloride is uniformly dispersed in carbon skeleton inside.This kind adsorbent can be used for the low temperature level adsorbent of multistage absorption refrigeration circulation because the adsorption-desorption temperature is lower.
Embodiment 5
In the beaker of a 1000ml, be dissolved in 127 gram iron chloride in 60 ℃ the 100ml water, and add 300ml paper pulp and stir, put into the oil bath case, keep constant temperature 24h; Put into air dry oven to macerate in the beaker, 120 ℃ of baking temperatures are dried to mixture and become the stiff mud shape; Take out and evenly put into mould, pressing pressure is 5MPa, after the compression moulding, puts into micro-wave oven and secluding air, and power 700W continues 12 minutes, takes out after being cooled to normal temperature, obtains iron chloride---carbonaceous skeleton compound adsorbent.
Present embodiment preparation iron chloride---carbonaceous skeleton compound adsorbent can be used for absorbing ammonia.According to the absorption of ammonia test, the iron chloride mass fraction is about 75%, and maximum ammonia adsorbance is about 0.61kg/kg, and the thermal conductivity factor maximum can reach 0.63W/ (mK).This kind adsorbent can be used for the high temperature level adsorbent of multistage absorption refrigeration circulation because the adsorption-desorption temperature is higher.
Claims (2)
1. the preparation method of chloride-carbonaceous skeleton compound adsorbent; It is characterized in that its raw material and each set of dispense are such as following: with the carbonaceous predecessor is benchmark; Chloride is 0.5～2 times of its quality, and binding agent is 0～25% of its quality, and Heat Conduction Material is 0～50% of its quality; Described carbonaceous predecessor is at least a of shell, fruit stone, timber, stalk, mud, bituminous coal, anthracite, brown coal, carbonized material, paper pulp; Said chloride is CaCl
2, MnCl
2, SrCl
2, FeCl
3, BaCl
2, PbCl
3One of; Said binding agent is at least a in starch and starch ether material, polyvinyl alcohol, cellulose ether and derivative thereof, secondary stock, the coal tar; Said Heat Conduction Material is the powder or the silk screen of copper, iron, aluminium, carborundum; The preparation method may further comprise the steps:
(1) fragmentation
It is 20～400 purpose particles that the carbonaceous predecessor is ground into particle diameter;
(2) preparation maceration extract
Water or alcohols are as solvent, and chloride prepares maceration extract as solute; Said maceration extract, its chloride quality concentration is 10～65%;
(3) dipping
The particle that step (1) makes the carbonaceous predecessor is put into the made maceration extract dipping of step (2), and the duration is 2～24h, and its dipping temperature scope is normal temperature～120 ℃;
(4) moulding
Oven dry or air-dry step (3) dipping make the carbonaceous predecessor, add Heat Conduction Material and binding agent, insert mould compression moulding or insert the extruder extrusion modling after mixing evenly; Briquetting pressure is 2～20MPa;
(5) drying
Forced air drying; The forced air drying temperature is 60～140 ℃, is dried to solvent less than 3%;
(6) carbonization-activation
Carbonization-activation under oxygen-free environment, its temperature are 350～800 ℃, and the carbonaceous predecessor burns the mistake rate less than 85%.
2. the preparation method of a kind of chloride carbonaceous skeleton compound adsorbent according to claim 1 makes powdery or granular adsorption agent if it is characterized in that said adsorbent, then crosses step (4), directly carries out step (5) and step (6).
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| CN102698712A (en) * | 2012-05-14 | 2012-10-03 | 北京工业大学 | Surface modification method of sludge-activated carbon for treating dyeing wastewater |
| CN102895957B (en) * | 2012-11-11 | 2014-05-14 | 桂林理工大学 | Preparation method of moso bamboo biomorphic Fe2O3/Fe3O4 compound heavy metal absorbent |
| CN104138748A (en) * | 2014-08-07 | 2014-11-12 | 黄山学院 | Compound biosorbent capable of greatly improving capability of adsorbing heavy metal by waste biomasses and preparation method thereof |
| CN105948435A (en) * | 2016-06-29 | 2016-09-21 | 南安泰达工业设计有限公司 | Acetone pollution sludge treatment agent and preparation method thereof |
| CN106085455A (en) * | 2016-07-01 | 2016-11-09 | 苏加强 | A kind of vinyl chloride Contaminated Sewage Sludge inorganic agent and preparation method thereof |
| CN106007281A (en) * | 2016-07-11 | 2016-10-12 | 许祚员 | Phenol polluted sludge treatment agent and preparing method thereof |
| CN106007301A (en) * | 2016-07-29 | 2016-10-12 | 张凯悦 | Petroleum-hydrocarbon-polluted sludge treating agent and preparation method thereof |
| CN106994331A (en) * | 2017-04-24 | 2017-08-01 | 李志全 | The method that paper-making industrial waste water sludge prepares shale charcoal sorbing material |
| CN108467171B (en) * | 2018-05-11 | 2020-07-28 | 广东溢达纺织有限公司 | Method for recycling sludge containing ferrous iron |
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