CN101905145A - Molecular sieve cellular material and preparation method thereof - Google Patents
Molecular sieve cellular material and preparation method thereof Download PDFInfo
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- CN101905145A CN101905145A CN 201010215681 CN201010215681A CN101905145A CN 101905145 A CN101905145 A CN 101905145A CN 201010215681 CN201010215681 CN 201010215681 CN 201010215681 A CN201010215681 A CN 201010215681A CN 101905145 A CN101905145 A CN 101905145A
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Abstract
The invention relates to a molecular sieve cellular material and a preparation method thereof. The cellular material comprises the following components in percentage by mass: 80 to 70 percent of molecular sieve, 15 to 20 percent of binder and 5 to 10 percent of dilute acid. The cellular material prepared by using the molecular sieve can efficiently adsorb and purify harmful gases such as NO, NO2, VOCs, NH3, H2S, SO2 and the like and can be taken as a sewage purifying material and a catalyst carrier. The material has the advantages of simple processing procedure, low resistance, large specific surface area, large adsorption capacity, high stability, low cost, repeatability, reproducibility and the like. The molecular sieve cellular material can be taken as a material for purifying waste gas and waste liquid as well as the catalyst carrier and can be widely applied in the fields such as environmental protection, petrochemical industry, catalysis and the like.
Description
Technical field
The present invention relates to a kind of molecular sieve cellular material and preparation method thereof.
Background technology
Because molecular sieve has regular aperture structure, big characteristics such as specific area, advantages of excellent stability, high activity and ion exchangeable, is widely used in fields such as catalysis, petrochemical industry, chemical industry, environmental protection, natural gas, metallurgy and electronics.
Powder or particulate molecular sieve material range of application are wider, simultaneously also obtained bigger success, but, low pressure drop little at ask for something molecular screen material resistance, load are big, convenient filling and mechanical strength is high has limited its development and application than special industry industrial.Can satisfy above-mentioned requirements and molecular sieve is prepared into cellular material, have application promise in clinical practice.
Usually molecular sieve is prepared into cellular material and takes two kinds of methods.A kind of method is a dip coating, is about to business-like ceramic honey comb and is immersed in the slurry that contains molecular sieve, prepares thickness from several microns to tens microns molecular sieve coating through technologies such as purging, drying and roasting again.Patent JP 0418914 and JP 07132230 utilize the dip-coating technology at ceramic honey comb area load one deck Cu-ZSM-5 molecular sieve, are used for the catalytic purification vehicle exhaust.Advantages such as dip-coating is even though dip coating has, technology is simple and the molecular sieve kind is adjustable, but it has the molecular sieve coating and combines not firm with the ceramic honey comb surface, shortcomings such as thermal shock resistance is relatively poor, as under the operating mode of shock heating or quenching, the molecular sieve coating easily comes off from the ceramic honey comb surface, thereby causes catalyst performance to reduce greatly.Another kind method is the synthetic load molecular sieve technology of original position, has both carried out original position synthesis of molecular sieve coating on the ceramic honey comb surface.Patent USP 4800187 uses the original position synthetic technology to grow multiple molecular sieve at the ceramic honey comb surface crystallization.It is a kind of at multiple molecular sieves such as silicon chip surface original position hydro-thermal synthetic ZSM-5, ZSM-11 and ZSM-12 that patent USP 4904518 provides.Patent CN 1288781A and CN 1269262A disclose a kind of on lumpy cordierite honeycomb ceramic carrier the synthetic magnesium alkali SiO of original position
2The method of zeolite.At first with a certain proportion of Al
2O
3, SiO
2, Na
2O and water are configured to the gel slurry, then with this gel slurry dip-coating on honeycomb ceramic carrier, at last again in organic amine solution at a certain temperature crystallization make finished product through washing, drying and roasting again after several days with molecular sieve coating.Above-mentioned dip coating and original position hydro-thermal synthetic technology mainly contain combine with carrier surface not firm, molecular sieve dip-coating layer thin, complex process and the more high shortcoming of cost.
Summary of the invention
One of purpose of the present invention is to provide a kind of molecular sieve cellular material.
Two of purpose of the present invention is to provide a kind of preparation method's method of this cellular material.
For achieving the above object, the present invention adopts following technical scheme:
A kind of molecular sieve cellular material is characterized in that the composition of this cellular material and mass percent are:
Diluted acid 5～10%,
Described molecular sieve and binding agent are 300～600 purpose powders.
Above-mentioned molecular sieve is: 5A molecular sieve, 4A molecular sieve, 3A molecular sieve, 13X molecular sieve, ZSM series molecular sieve, beta-molecular sieve or Y zeolite.
Above-mentioned binding agent is: at least a in boehmite, cellulose, starch, polyvinyl alcohol, the phenolic resins.
The above-mentioned diluted acid concentration that is weight percentage is that 15～68% nitric acid, weight percent concentration are that 15～68% hydrochloric acid or weight percent concentration are 15～68% acetate.
A kind of preparation method who prepares above-mentioned molecular sieve cellular material is characterized in that the concrete steps of this method are: extrusion modling after the rubbing after above-mentioned each composition is fully mixed; Microwave drying is 3～30 minutes again, and drying is 2～15 hours under 100～150 ℃; Carry out roasting at last, the technology of roasting is: 500～700 ℃ of following roastings 2～10 hours, and reduce to room temperature then naturally and take out, promptly make the molecular sieve cellular material finished product.
Molecular sieve cellular material of the present invention is mainly by 5A molecular sieve, 4A molecular sieve, 3A molecular sieve, 13X molecular sieve, ZSM series molecular sieve, beta-molecular sieve and Y zeolite, binding agent and diluted acid compositions such as boehmite.Make finished product through operations such as mixing, rubbing, moulding, drying and roastings.The present invention utilizes molecular sieve to be prepared into cellular material, can be to NO, NO
2, VOCs, NH
3, H
2S and SO
2Carry out efficient adsorption cleaning Deng pernicious gas, also can be used as sewage purification material and catalyst carrier simultaneously.This material has advantages such as processing technology is simple, resistance is little, specific area is big, adsorption capacity is big, good stability, the low renewable repeated use of cost.This molecular sieve cellular material can be used as the scavenging material of waste gas and waste liquid, also can be used as catalyst carrier simultaneously, can be widely used in fields such as environmental protection, petrochemical industry and catalysis.
The performance evaluation of molecular sieve cellular material is carried out in Φ 16mm, the straight type glass tube of long 300mm reactor, and reaction gas volume air speed (GHSV) is 15000h
-1, get molecular sieve cellular material 8ml, be reflected under the normal temperature and pressure environment and carry out.Unstripped gas NOx concentration 15ppm, NO and NO
2Ratio is about 9: 1.
Description of drawings
Fig. 1 is the absorption purifying effect figure of 3X molecular sieve cellular material to NOx.
Fig. 2 is the absorption purifying effect figure of 5A molecular sieve cellular material to NOx.
Fig. 3 is the absorption purifying effect figure of Y zeolite cellular material to NOx.
Fig. 4 is the absorption purifying effect of type ZSM 5 molecular sieve cellular material to NOx.
The specific embodiment:
The present invention is further described below in conjunction with specific embodiment
Embodiment one: with the weight percent content of the 13X molecular sieve of 400 orders 75%, 20% the thin water al binder of plan and 5% is that rare nitric acid of 30% fully mixes the back rubbing in mixer; Molecular sieve blank after the rubbing is moved to extrusion modling in the single lead screw ex truding briquetting machine; The molecular sieve honeycomb briquet of extrusion molding was placed in the industrial microwave oven dry 10 minutes, again in the dislocation baking oven 120 ℃ dry 6 hours down; The molecular sieve honeycomb briquet of oven dry is moved to and carries out calcining process in the Muffle furnace, and condition is: heating rate is 5 ℃/minute, rises to 600 ℃ of insulations and reduces to the room temperature taking-up after 3 hours naturally and promptly make the molecular sieve cellular material finished product.
Embodiment two: with the weight percent content of the 5A molecular sieve of 400 orders 75%, 20% the thin water al binder of plan and 5% is that rare nitric acid of 30% fully mixes the back rubbing in mixer; Molecular sieve blank after the rubbing is moved to extrusion modling in the single lead screw ex truding briquetting machine; The molecular sieve honeycomb briquet of extrusion molding was placed in the industrial microwave oven dry 10 minutes, again in the dislocation baking oven 120 ℃ dry 6 hours down; The molecular sieve honeycomb briquet of oven dry is moved to and carries out calcining process in the Muffle furnace, and condition is: heating rate is 5 ℃/minute, rises to 600 ℃ of insulations and reduces to the room temperature taking-up after 3 hours naturally and promptly make the molecular sieve cellular material finished product.
Embodiment three: with the weight percent content of the Y zeolite of 400 orders 75%, 20% the thin water al binder of plan and 5% is that rare nitric acid of 30% fully mixes the back rubbing in mixer; Molecular sieve blank after the rubbing is moved to extrusion modling in the single lead screw ex truding briquetting machine; The molecular sieve honeycomb briquet of extrusion molding was placed in the industrial microwave oven dry 10 minutes, again in the dislocation baking oven 120 ℃ dry 6 hours down; The molecular sieve honeycomb briquet of oven dry is moved to and carries out calcining process in the Muffle furnace, and condition is: heating rate is 5 ℃/minute, rises to 600 ℃ of insulations and reduces to the room temperature taking-up after 3 hours naturally and promptly make the molecular sieve cellular material finished product.
Embodiment four: with the weight percent content of the type ZSM 5 molecular sieve of 400 orders 75%, 20% the thin water al binder of plan and 5% is that rare nitric acid of 30% fully mixes the back rubbing in mixer; Molecular sieve blank after the rubbing is moved to extrusion modling in the single lead screw ex truding briquetting machine; The molecular sieve honeycomb briquet of extrusion molding was placed in the industrial microwave oven dry 10 minutes, again in the dislocation baking oven 120 ℃ dry 6 hours down; The molecular sieve honeycomb briquet of oven dry is moved to and carries out calcining process in the Muffle furnace, and condition is: heating rate is 5 ℃/minute, rises to 600 ℃ of insulations and reduces to the room temperature taking-up after 3 hours naturally and promptly make the molecular sieve cellular material finished product.
Claims (5)
1. molecular sieve cellular material is characterized in that the composition of this cellular material and mass percent are:
Molecular sieve 80～70%, binding agent 15～20%
Diluted acid 5～10%,
Described molecular sieve and binding agent are 300～600 purpose powders.
2. the molecular sieve cellular material of method according to claim 1 is characterized in that described molecular sieve is: 5A molecular sieve, 4A molecular sieve, 3A molecular sieve, 13X molecular sieve, ZSM series molecular sieve, beta-molecular sieve or Y zeolite.
3. the molecular sieve cellular material of method according to claim 1 is characterized in that described binding agent is: at least a in boehmite, cellulose, starch, polyvinyl alcohol, the phenolic resins.
4. the molecular sieve cellular material of method according to claim 1 is characterized in that the described diluted acid concentration that is weight percentage is that 15～68% nitric acid, weight percent concentration are that 15～68% hydrochloric acid or weight percent concentration are 15～68% acetate.
5. a preparation method who prepares molecular sieve cellular material according to claim 1 is characterized in that the concrete steps of this method are: extrusion modling after the rubbing after above-mentioned each composition is fully mixed; Microwave drying is 3～30 minutes again, and drying is 2～15 hours under 100～150 ℃; Carry out roasting at last, the technology of roasting is: 500～700 ℃ of following roastings 2～10 hours, and reduce to room temperature then naturally and take out, promptly make the molecular sieve cellular material finished product.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102671691A (en) * | 2012-05-28 | 2012-09-19 | 四川君和环保工程有限公司 | Low-temperature SCR (Selective Catalytic Reduction) denitrification catalyst, as well as preparation method and application thereof |
| CN107583604A (en) * | 2017-11-02 | 2018-01-16 | 景德镇佳奕新材料有限公司 | A kind of hydrophobicity honeycomb-shaped zeolite material and its preparation method and application |
| CN107890850A (en) * | 2017-11-16 | 2018-04-10 | 四川大学 | A kind of monoblock type adsorbent of molecular sieve and its preparation method and application |
| CN108745314A (en) * | 2018-06-15 | 2018-11-06 | 广州市环境保护设备厂有限公司 | A kind of polystyrene crosslinked divinylbenzene resin honeycomb ceramics and preparation method thereof |
| CN109453738A (en) * | 2018-12-12 | 2019-03-12 | 江苏楚锐环保科技有限公司 | Hydrophobic zeolite molecular sieve honeycomb body manufacturing method and its dedicated manufacturing equipment |
| CN109589912A (en) * | 2019-01-29 | 2019-04-09 | 山东奥福环保科技股份有限公司 | A kind of concentration runner adsorbent material and preparation method thereof |
| CN112808229A (en) * | 2020-12-22 | 2021-05-18 | 昆明理工大学 | Preparation method and application of copper and manganese modified Beta molecular sieve adsorption-catalytic oxidant |
| CN113713849A (en) * | 2021-09-15 | 2021-11-30 | 美埃(中国)环境科技股份有限公司 | Adsorption catalysis material and preparation method thereof |
| CN117019107A (en) * | 2023-10-07 | 2023-11-10 | 星远智维邯郸环境科技有限公司 | Blast furnace gas purifying adsorbent and preparation method and application thereof |
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|---|---|---|---|---|
| US4800187A (en) * | 1987-10-28 | 1989-01-24 | Corning Glass Works | Method of crystallizing a zeolite on the surface of a monolithic ceramic substrate |
| CN1269262A (en) * | 1999-04-07 | 2000-10-11 | 中国科学院大连化学物理研究所 | In-site molecular sieve synthesizing process on lumpy honeycomb cordierite ceramic carrier |
| CN1288781A (en) * | 1999-09-22 | 2001-03-28 | 中国科学院大连化学物理研究所 | Method of in-situ synthesizing ferrierite on lumpy cordierite honeycomb ceramic carrier |
| CN101591025A (en) * | 2009-06-29 | 2009-12-02 | 中南大学 | A kind of method of utilizing kaolin to prepare binderless A type zeolite molecular sieve |
-
2010
- 2010-09-15 CN CN2010102156815A patent/CN101905145B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4800187A (en) * | 1987-10-28 | 1989-01-24 | Corning Glass Works | Method of crystallizing a zeolite on the surface of a monolithic ceramic substrate |
| CN1269262A (en) * | 1999-04-07 | 2000-10-11 | 中国科学院大连化学物理研究所 | In-site molecular sieve synthesizing process on lumpy honeycomb cordierite ceramic carrier |
| CN1288781A (en) * | 1999-09-22 | 2001-03-28 | 中国科学院大连化学物理研究所 | Method of in-situ synthesizing ferrierite on lumpy cordierite honeycomb ceramic carrier |
| CN101591025A (en) * | 2009-06-29 | 2009-12-02 | 中南大学 | A kind of method of utilizing kaolin to prepare binderless A type zeolite molecular sieve |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102671691A (en) * | 2012-05-28 | 2012-09-19 | 四川君和环保工程有限公司 | Low-temperature SCR (Selective Catalytic Reduction) denitrification catalyst, as well as preparation method and application thereof |
| CN107583604A (en) * | 2017-11-02 | 2018-01-16 | 景德镇佳奕新材料有限公司 | A kind of hydrophobicity honeycomb-shaped zeolite material and its preparation method and application |
| CN107890850A (en) * | 2017-11-16 | 2018-04-10 | 四川大学 | A kind of monoblock type adsorbent of molecular sieve and its preparation method and application |
| CN108745314A (en) * | 2018-06-15 | 2018-11-06 | 广州市环境保护设备厂有限公司 | A kind of polystyrene crosslinked divinylbenzene resin honeycomb ceramics and preparation method thereof |
| CN108745314B (en) * | 2018-06-15 | 2019-10-29 | 广州市环境保护设备厂有限公司 | A kind of polystyrene crosslinked divinylbenzene resin honeycomb ceramics and preparation method thereof |
| CN109453738A (en) * | 2018-12-12 | 2019-03-12 | 江苏楚锐环保科技有限公司 | Hydrophobic zeolite molecular sieve honeycomb body manufacturing method and its dedicated manufacturing equipment |
| CN109589912A (en) * | 2019-01-29 | 2019-04-09 | 山东奥福环保科技股份有限公司 | A kind of concentration runner adsorbent material and preparation method thereof |
| CN109589912B (en) * | 2019-01-29 | 2021-09-17 | 山东奥福环保科技股份有限公司 | Concentrated rotating wheel adsorption material and preparation method thereof |
| CN112808229A (en) * | 2020-12-22 | 2021-05-18 | 昆明理工大学 | Preparation method and application of copper and manganese modified Beta molecular sieve adsorption-catalytic oxidant |
| CN113713849A (en) * | 2021-09-15 | 2021-11-30 | 美埃(中国)环境科技股份有限公司 | Adsorption catalysis material and preparation method thereof |
| CN117019107A (en) * | 2023-10-07 | 2023-11-10 | 星远智维邯郸环境科技有限公司 | Blast furnace gas purifying adsorbent and preparation method and application thereof |
| CN117019107B (en) * | 2023-10-07 | 2023-12-15 | 星远智维邯郸环境科技有限公司 | Blast furnace gas purifying adsorbent and preparation method and application thereof |
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| CN101905145B (en) | 2012-11-07 |
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