CN105214615B - A kind of moulding process of composite absorbent material - Google Patents
A kind of moulding process of composite absorbent material Download PDFInfo
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- CN105214615B CN105214615B CN201510742656.5A CN201510742656A CN105214615B CN 105214615 B CN105214615 B CN 105214615B CN 201510742656 A CN201510742656 A CN 201510742656A CN 105214615 B CN105214615 B CN 105214615B
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- absorbent material
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Abstract
The invention discloses a kind of moulding process of composite absorbent material, takes porous carrier, amine modifying agent and alcohols solvent to be uniformly mixed, and dries, and the powder that gained is dried is through being granulated the graininess composite absorbent material being molded.The technological forming Particles dispersed absorbent material is high to the adsorption capacity of water, and intensity is high.
Description
Technical field
The present invention relates to the preparation method of composite absorbent material, more particularly to a kind of moulding process of composite absorbent material.
Background technology
SF6Gas insulation electric appliance equipment has that floor space is few, electromagnetic pollution is small, the advantage such as safe and reliable, in city electricity
It is widely used in net, but the minor amount of water being inevitably present inside it, usually 20 ~ 200ppm, can form insulation defect
And further deteriorated in shelf depreciation, it is consequently formed equipment safety hidden danger.Therefore to ensure SF6Electrical equipment safety and stability is transported
OK, a certain amount of adsorbent is generally placed in equipment air chamber, as 4A types, 5A types, 13X types, KDHF-03 equimoleculars sieve and in
Property aluminum oxide etc..But SF6Insulating gas can be in SF6Decomposing during shelf depreciation occurs in device interior, and it decomposes the spy of generation
The order of severity and type of sign constituent content and growth rate and shelf depreciation have close contact.Therefore, can be by monitoring SF6
Decomposition components are simultaneously analyzed its feature content, can find the sign of insulation degradation in time, and understand insulation defect and serious
Degree, to ensure the safe operation of equipment.This is a kind of for GIS insulating monitorings and the non-electrical monitoring method of fault diagnosis, is had
Antijamming capability and easily quantitative, the extensive concern just gone together both at home and abroad.Therefore, it is necessary to develop new selectivity water suction
Material, its suction-operated to feature decomposition gas is greatly reduced while efficient absorption moisture.Related research both at home and abroad
Work is still rare.
Adsorbent typically becomes the particle of definite shape and size after being molded or loading and fix, and is seated in adsorption tower, inhales
Used in attached tank, adsorption column.But conventional such as molecular sieve bad adhesion, its shaped granule is in active forces such as the deadweights of adsorption bed
Under be easily broken so that system can not effectively be run for a long time.Binding agent is added in forming process（Such as cement, silica gel）It can improve
The intensity of adsorbent, but and forming process often results in a part of duct blocking and great adsorption capacity is lost, its absorption appearance
Amount and mechanical strength can not be taken into account（Tang Maohui, the preparation research of ammonia compound adsorbent, academic dissertation, Sichuan University, 2008）.
So needing to develop the body formed method of suitable adsorbent powder, ensure that shaped granule has sufficient intensity and toughness, and use
Material safety, longtime running can ensure that absorbent particles do not crush, non-swelling, not leach, securely and reliably.
The content of the invention
Object of the present invention is to provide a kind of moulding process of composite absorbent material, and the technique is using porous carrier as load
Body, simultaneously high to the adsorption capacity of water as modifying agent and binding agent, shaped granule using organic amine, intensity is high.
The purpose of the present invention is achieved through the following technical solutions：A kind of moulding process of composite absorbent material, takes porous
Carrier, amine modifying agent and alcohols solvent are uniformly mixed, and are dried, and the powder that gained is dried is through being granulated the graininess being molded
Composite absorbent material.
The present invention considers that absorbent material should not introduce aqueous solvent in preparation process, and amine is modified composite absorbent material not
Suitable high-temperature calcination, non-slurry pelletizing is used in forming process, i.e., raw material thing powder direct weighting is compressed into larger tablet, then weigh
Newly it is ground into a certain size particle.Need to make to produce adhesion between particle by compression stress in the method, this causes the selection of binding agent
It is particularly important.The species and dosage of binding agent, for the size of particle after granulation, uniformity, hardness, collapse elasticity and be compressed into
Type will produce material impact.The stickiness of binding agent is larger, or binding agent concentration it is higher when, the hardness of particle is larger, granularity
Skewness, disintegration are slower；In turn, during consumption of binder deficiency, particle is loose, intensity is insufficient.Select in the present invention
Amine modifying agent and the modifying agent as adsorbent, when the load capacity of amine modifying agent is sufficiently large or even is tied beyond porous carrier duct
The receiving limit of structure, organic amine is adhered to duct port and outer surface, therefore also serves as binding agent simultaneously.It is former according to similar compatibility
Reason, bond agent molecule and the active group of porous carrier surface（Hydroxyl, the carboxyl oxygen-containing functional group of such as activated carbon surface）It is logical
Shared electron forms covalent bond or hydrogen bond between crossing atom, and dispersion force may also be produced between nonpolar molecule.After dry solidification, bond
Agent produces engagement force at interface, the attraction between powder grain is effectively increased, so as to improve the intensity of shaped granule.At this
In order to control production cost in invention, the load capacity of amine modifying agent is 40-65%, i.e. matter between amine modifying agent and porous carrier
It is 40-65% to measure ratio, preferably 40-60%.
From porous carrier 3 beneficial effects can be produced as carrier：（1）Often specific surface area is big for porous carrier, duct
It is abundant, there is certain pipeline enrichment effect to hydrone.（2）The unique pore passage structure of porous carrier also carries for further modification
Sufficient confinement space has been supplied, has introduced the water absorption capacity that the scattered amino of height space further improves composite.（3）
Amine modifying agent at room temperature tends to intramolecule and reunited, sticky to be not easy to flow, this divergent contour to molecule in its network structure
Into great resistance, the effective rate of utilization of amino reduces.Porous carrier can from be sufficiently spatially separated subsequently load it is organic
Amine, so as to expose more hydrophilic radicals, improve the water absorption capacity of composite.Specifically, described porous carrier is charcoal
Combination more than one or both of sill, silica gel, zeolite molecular sieve and stratified material.The carbon based material is activity
Charcoal, activated coke or carbon fiber, layered material include magnalium hydrotalcite, kaolin etc..The zeolite molecular sieve includes 5A points
Sub- sieve, 13X molecular sieves, mesoporous silica molecular sieve etc..
The abundant amino contained in described amine modifying agent provides main hydrophilic radical for composite, significantly
Improve its water absorption character.Specifically, described amine modifying agent is MEA, diethanol amine, TEPA, pentaethylene hexamine
With combination more than one or both of polyethyleneimine.
The granulation can use extruding pelletization, such as use rotary-type dry press；20- can also be ground into after the tabletting of powder elder generation
The particle of 60 mesh, such as use roller concora crush granulator.
Described alcohols solvent is methanol or ethanol.The dosage of the alcohols solvent is 5 ~ 20ml/g- carrier materials.
Described porous carrier, amine modifying agent and alcohols solvent at room temperature be stirred 4-6h.
The beneficial effects of the present invention are：
(1) sorbing material water adsorption capacity of the invention is big, and intensity is high, non-breakable.
(2) preparation process is simple and easy：Amine modifying agent in adsorbent be used as binding agent simultaneously, saved preparation and into
Operating procedure during type.
Embodiment
Embodiment 1
Take 500 g mesoporous silica molecular sieves MCM-41 to be mixed with 5000 ml methanol and be made into carrier alcoholic solution, by TEPA
Add in carrier alcoholic solution, TEPA and MCM-41 mass ratio are 40%.4 h are stirred at room temperature, are then dried, and are dried
20 ~ 40 mesh particles are made in crushing after gained powder uses roller concora crush granulator tabletting, produce TEPA (40%)/MCM-
41 composite absorbent materials.The composite absorbent material is 122mg/g to the adsorbance of minor amount of water, and breaking strength is more than 38N, and 24h shakes
Bottle test Particle Breakage rate is less than 1%.
Embodiment 2
Take 1000 g mesoporous silica molecular sieves SBA-15 to be mixed with 15000 ml methanol and be made into carrier alcoholic solution, by diethanol amine
Add in carrier alcoholic solution, diethanol amine and SBA-15 mass ratio are 65%.6h is stirred at room temperature, is then dried, and dries gained
Powder is extruded through rotary-type dry press, and diethanol amine (65%)/SBA-15 composite absorbent materials that diameter is 1.5mm are made.
The composite absorbent material is 164mg/g to the adsorbance of minor amount of water, and breaking strength is more than 45N, 24h shaking flasks test Particle Breakage rate
Less than 1%.
Embodiment 3
Take 200 g mesoporous silica molecular sieves FDU to be mixed with 1000 ml methanol and be made into carrier alcoholic solution, by polyethyleneimine plus
Enter in carrier alcoholic solution, polyethyleneimine and FDU mass ratio are 45%.5h is stirred at room temperature, is then dried, and dries gained powder
40 ~ 60 mesh particles are made in crushing after end uses roller concora crush granulator tabletting, that is, obtain polyethyleneimine（45%）The compound suctions of/FDU
Water material.The composite absorbent material is 151mg/g to the adsorbance of minor amount of water, and breaking strength is more than 47N, the test of 24h shaking flasks
Grain percentage of damage is less than 2%.
Embodiment 4
Take the commercially available activated carbons of 2000 g to be mixed with 10000 ml methanol and be made into carrier alcoholic solution, MEA is added into carrier
In alcoholic solution, the mass ratio of MEA and activated carbon is 40%.4h is stirred at room temperature, is then dried, and dries gained powder through turning
Wheeled dry press extrusion, is made the MEA that diameter is 1.5mm（40%）/ activated carbon composite absorbent material.The compound suction
Water material is 54mg/g to the adsorbance of minor amount of water, and breaking strength is more than 40N, and 24h shaking flasks test Particle Breakage rate is less than 2%.
Embodiment 5
Take 1000 g 5A molecular sieves to be mixed with 15000 ml ethanol and be made into carrier alcoholic solution, diethanol amine is added into carrier
In alcoholic solution, the mass ratio of diethanol amine and 5A molecular sieves is 55%.4h is stirred at room temperature, is then dried, and dries gained powder warp
Rotary-type dry press extrusion, is made the diethanol amine that diameter is 2mm（55%）/ 5A molecular sieve composite absorbent materials.This is compound
Absorbent material is 41mg/g to the adsorbance of minor amount of water, and breaking strength is more than 42N, and 24h shaking flasks test Particle Breakage rate is less than 2%.
Embodiment 6
Take 2000 g 13X molecular sieves to be mixed with 40000 ml ethanol and be made into carrier alcoholic solution, pentaethylene hexamine is added and carried
In body alcoholic solution, the mass ratio of pentaethylene hexamine and 13X molecular sieves is 60%.5h is stirred at room temperature, is then dried, and dries gained
Powder is extruded through rotary-type dry press, and the pentaethylene hexamine that diameter is 2mm is made（60%）/ 13X molecular sieve composite water absorbing materials
Material.The composite absorbent material is 66mg/g to the adsorbance of minor amount of water, and breaking strength is more than 40N, 24h shaking flasks test Particle Breakage
Rate is less than 2%.
Embodiment 7
Take 100 g magnalium hydrotalcites to be mixed with 500 ml ethanol and be made into carrier alcoholic solution, MEA is added into carrier alcohol
In solution, the mass ratio of MEA and magnalium hydrotalcite is 40%.6h is stirred at room temperature, is then dried, and is dried gained powder and is adopted
20 ~ 40 mesh particles are made with being crushed after roller concora crush granulator tabletting, MEA is made（40%）The compound suction of/magnalium hydrotalcite
Water material.The composite absorbent material is 25mg/g to the adsorbance of minor amount of water, and breaking strength is more than 80N, 24h shaking flasks test particle
Percentage of damage is less than 1%.
Embodiment 8
Take 150 g kaolin to be mixed with 1500 ml methanol and be made into carrier alcoholic solution, TEPA is added into carrier alcohol
In solution, TEPA is 40% with kaolinic mass ratio.6h is stirred at room temperature, is then dried, and is dried gained powder and is used
Crushed after roller concora crush granulator tabletting and 40 ~ 60 mesh particles are made, TEPA is made（40%）/ kaolin composite water absorbing material
Material.The composite absorbent material is 27mg/g to the adsorbance of minor amount of water, and breaking strength is more than 76N, 24h shaking flasks test Particle Breakage
Rate is less than 1%.
The embodiment of the present invention is described above in association with example, it will be appreciated by those of skill in the art that
These are merely illustrative of, and protection scope of the present invention is that claims limit.Those skilled in the art without departing substantially from
On the premise of the principle and essence of the present invention, various changes or modifications can be made to these embodiments, but these changes and
Modification each falls within protection scope of the present invention.
Claims (5)
1. a kind of moulding process of composite absorbent material, it is characterized in that, take porous carrier, amine modifying agent and alcohols solvent stirring mixed
Close uniformly, dry, the powder that gained is dried is through being granulated, the graininess composite absorbent material being molded；The amine modifying agent with
Mass ratio between porous carrier is 40-60%；Described porous carrier is carbon based material, silica gel, zeolite molecular sieve and stratiform material
Combination more than one or both of material；The carbon based material includes activated carbon, activated coke or Carbon fibe, layered material
Including magnalium hydrotalcite or kaolin；The zeolite molecular sieve includes 5A molecular sieves, 13X molecular sieves or mesoporous silica molecular sieve；Institute
The amine modifying agent stated is one kind or two in MEA, diethanol amine, TEPA, pentaethylene hexamine and polyethyleneimine
The combination of the kind above.
2. the moulding process of composite absorbent material according to claim 1, it is characterized in that, it is described be granulated as extruding pelletization or
The particle of 20-60 mesh will be ground into after the tabletting of powder elder generation.
3. the moulding process of composite absorbent material according to claim 1, it is characterized in that, described alcohols solvent is methanol
Or ethanol.
4. the moulding process of composite absorbent material according to claim 1, it is characterized in that, the dosage of the alcohols solvent is
5 ~ 20 ml/g- carrier materials.
5. the moulding process of composite absorbent material according to claim 1, it is characterized in that, described porous carrier, amine change
Property agent and alcohols solvent at room temperature be stirred 4-6h.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105688872B (en) * | 2016-04-29 | 2018-09-11 | 广东电网有限责任公司电力科学研究院 | A kind of amino-functionalization adsorbent and preparation method thereof |
| CN105964186A (en) * | 2016-07-11 | 2016-09-28 | 滁州格锐矿业有限责任公司 | Granulation process for dry powder of mica powder |
| CN106237996B (en) * | 2016-09-19 | 2019-05-07 | 广东电网有限责任公司电力科学研究院 | A kind of porous ceramic matrix load type adsorbing agent and preparation method thereof |
| CN113694905A (en) * | 2021-09-07 | 2021-11-26 | 临沂三禾生物质科技有限公司 | Method for granulating nano porous calcium silicate |
| CN114392723A (en) * | 2021-12-27 | 2022-04-26 | 正大能源材料(大连)有限公司 | Carbon dioxide adsorbent, preparation method thereof, activation regeneration method and application |
| CN114210307A (en) * | 2022-01-05 | 2022-03-22 | 上海恒业微晶材料科技股份有限公司 | Preparation method and application of novel carbon-silicon material |
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| JP2000189794A (en) * | 1998-12-28 | 2000-07-11 | Nippon Shokubai Co Ltd | Production of water absorbing material |
| CN104324693A (en) * | 2014-11-03 | 2015-02-04 | 广东电网有限责任公司电力科学研究院 | Layered composite material with selective water adsorption property and preparation method and application thereof |
| CN104353433A (en) * | 2014-10-22 | 2015-02-18 | 广东电网有限责任公司电力科学研究院 | Stable efficient composite water absorbing material and preparation method thereof |
| CN104475060A (en) * | 2014-12-09 | 2015-04-01 | 成都信息工程学院 | Composite adsorbent, and preparation method and application thereof |
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2015
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Patent Citations (4)
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| JP2000189794A (en) * | 1998-12-28 | 2000-07-11 | Nippon Shokubai Co Ltd | Production of water absorbing material |
| CN104353433A (en) * | 2014-10-22 | 2015-02-18 | 广东电网有限责任公司电力科学研究院 | Stable efficient composite water absorbing material and preparation method thereof |
| CN104324693A (en) * | 2014-11-03 | 2015-02-04 | 广东电网有限责任公司电力科学研究院 | Layered composite material with selective water adsorption property and preparation method and application thereof |
| CN104475060A (en) * | 2014-12-09 | 2015-04-01 | 成都信息工程学院 | Composite adsorbent, and preparation method and application thereof |
Non-Patent Citations (1)
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| 有机胺改性MCM-41吸附富集CO2;侯洪蕾;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20121115;摘要、第14-15、22页 * |
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