CN110054499A - A kind of silicon nitride microballoon of area load molecular sieve, preparation method and applications - Google Patents

A kind of silicon nitride microballoon of area load molecular sieve, preparation method and applications Download PDF

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CN110054499A
CN110054499A CN201910455568.5A CN201910455568A CN110054499A CN 110054499 A CN110054499 A CN 110054499A CN 201910455568 A CN201910455568 A CN 201910455568A CN 110054499 A CN110054499 A CN 110054499A
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molecular sieve
silicon nitride
microballoon
area load
preparation
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蒋仁会
叶枫
郭露村
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YANGZHOU FINE ELECTRON TECHNOLOGY Co Ltd
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YANGZHOU FINE ELECTRON TECHNOLOGY Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/02Loose filtering material, e.g. loose fibres
    • B01D39/06Inorganic material, e.g. asbestos fibres, glass beads or fibres
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    • C01B39/02Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
    • C01B39/36Pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11
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    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
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Abstract

A kind of silicon nitride microballoon of area load molecular sieve, preparation method and applications are related to molecular sieve, ceramic chemical industry and filtration and separation techniques field.ZSM-5 molecular sieve with methyl is sprayed on silicon nitride ceramics microsphere surface, through dry to get the ZSM-5 molecular sieve in the load of silicon nitride ceramics microsphere surface with methyl.Present invention process is simple, and by spraying, the ZSM-5 molecular sieve with methyl is distributed in substrate --- silicon nitride ceramics microsphere surface, then, the solid fraction micro-sphere material of formation convenient further packaging, transport i.e. curable through 80 DEG C of drying.The modification of methylic molecular sieve is so that silicon nitride ceramics microballoon can effectively adsorb organic substance, while generating repulsion to water and water-soluble substances with compared with strong-hydrophobicity.Reach bulky grain and organic filtration, centrifugation in excellent water.

Description

A kind of silicon nitride microballoon of area load molecular sieve, preparation method and applications
Technical field
The present invention relates to molecular sieve, ceramic chemical industry and filtration and separation techniques fields.
Technical background
Silicon-nitride-based ceramic is made of silicon nitride powder and ceramic post sintering sintering adjuvant, non-shrinking nothing when being a kind of sintering Machine material ceramics, have the advantageous properties such as high intensity, low-density, high temperature resistant, resistance to strong acid.It is made pottery by the silicon nitride of hot die-casting molding Porcelain micro-sphere material has the advantage that chemical stability is good, acid and alkali-resistance and organic solvent;Fabulous emergency heat and cooling property resistance chilling performance, work Temperature may be up to 1000 DEG C;Anti-microbial property is good, is not easy by bacterial degradation, and stronger structural stability is nontoxic, there is larger surface Product, is particularly suitable for the processing of food and drug.It, can only but when due to exposed silicon nitride ceramics microballoon as filtering material The solid bulky grain being provided purely in separation liquid, and the ingredient in liquid can be largely adsorbed, it will cause what liquid effectively formed It is lost.
For molecular sieve as a kind of porous material haveing excellent performance, it is excellent to have that surface area is big, hydrothermally stable, adsorption capacity are strong etc. Point can more have good hydrophobicity, to water after methyl in its surface modification while generating effectively absorption to organic matter Soluble substance is without absorption, by You Gaoxiao in the organic matter separation of its application in aqueous solution.But distributed molecular sieve at Type is poor, needs to remove by operations such as filterings in aqueous solution, not only troublesome in poeration, and filter paper can cause shadow to solution composition It rings.
Existing filter using funnel as filtration supports, filter paper is laid in funnel, when mixture to be filtered oneself It when funnel upper end is injected, by the filtration of filter paper, filters out filtered solution from the outlet of funnel lower end, and is retained down by filter paper Substance then stay on filter paper.The durability of filter paper is poor, and filter paper blocks and causes filter efficiency low in order to prevent, Ren Menxu Ceaselessly to replace filter paper.In addition, filter paper can not also be filtered the mixture containing large particulate matter, it is even more impossible to selective mistakes Filter organic matter.
Summary of the invention
For disadvantages described above, an object of the present disclosure be to propose it is a kind of shape, durability is strong, can to bulky grain and The silicon nitride microballoon for the area load molecular sieve that Organic substance in water is separated simultaneously.
The invention is characterized in that there is the ZSM-5 molecular sieve of methyl in the load of silicon nitride ceramics microsphere surface.
The beneficial effects of the present invention are: effectively filtering component is the silicon nitride microballoon that area load has molecular sieve, loaded Molecular sieve surface with a large amount of hydrophobic methyl, can effectively filter, separate organic components in aqueous solution;Meanwhile by In the hydrophobic molecule sieve structure of filtration fraction silicon nitride ceramics microsphere surface, can accomplish not influencing completely water-soluble in aqueous solution Property component;Meanwhile silicon nitride ceramic material is nontoxic with molecular screen material, surface area is very big, and high temperature resistant, durability is strong, the mistake Filter can be used in a variety of situations, be particularly suitable for the fields such as pharmacy, food.
Further, the diameter of silicon nitride ceramics microballoon of the present invention is 0.5 ± 0.002cm.The diameter is silicon nitride microballoon It is easier to molding one kind in synthesis technology, moreover, overall microsphere surface product reduces if diameter is excessive, cannot be filled with filtrate Tap touching;If diameter is too small, it will be greatly reduced liquid by speed, influence filter efficiency.
The second object of the present invention is to propose the preparation method of the silicon nitride microballoon of above-mentioned area load molecular sieve.
ZSM-5 molecular sieve with methyl is sprayed on silicon nitride ceramics microsphere surface, through drying,.
The temperature environment of the drying is 80 DEG C, and molecular sieve slurry can quickly, uniformly volatilize at this temperature, effectively be attached to Silicon nitride microsphere surface.
Present invention process is simple, and by spraying, the ZSM-5 molecular sieve with methyl is distributed in substrate --- silicon nitride Ceramic microsphere surface, then it is i.e. curable through 80 DEG C of drying, the solid fraction micro-sphere material of formation is convenient further to pack, transport and answers With.
Further, in the present invention, the specific preparation method of substrate --- silicon nitride ceramics microballoon is: by silicon nitride powder End, alumina powder, yttrium oxide powder, dispersing agent and deionized water mixing obtain mixing blank, then will mix blank through spherical shape Spherical green body is made in mold, then calcines 0.5h~3h under conditions of 1650 DEG C~1700 DEG C and pressure are 0.5MPa, obtains Silicon nitride ceramics microballoon.The silicon nitride microballoon shape of this method production is regular, and mechanical strength, there is good hydrothermally stable Property.
The partial size of above-mentioned alpha-silicon nitride powders is 0.5 μm~2.5 μm, and the partial size of alumina powder is 0.3 μm~5.0 μm, oxygen The partial size for changing yttrium powder end is 0.1 μm~5.0 μm;The alpha-silicon nitride powders account for the 65~90% of mixing blank gross mass, alumina powder End accounts for the 2~4% of mixing blank gross mass, and yttrium oxide powder accounts for the 6~8% of mixing blank gross mass.In this method selected by material Partial size, dosage, proportion be repeatedly the experiment gained best Application Range of synthesizing silicon nitride microballoon.
The dispersing agent is the anionic surfactant of the adjustable alpha-silicon nitride powders surface potentials such as lignosulfonates.
In addition, the present invention further discloses the preparation method of the ZSM-5 molecular sieve with methyl: first by sodium chlorate, Tetrapropylammonium hydroxide and water after mixing, are blended into methyl silicone grease and tetramethoxy silicone grease, obtain molecular sieve precursor, so Molecular sieve precursor is aged 4 days at 180 DEG C afterwards, obtains the ZSM-5 molecular sieve with methyl.This method, which can be produced effectively, to be had The molecular sieve of excellent hydrophobic oleophilic oil type, and molecular sieve pore passage compound with regular structure, absorption, filter efficiency are high.
The sodium chlorate accounts for the 0.2% of molecular sieve precursor gross mass, and tetrapropylammonium hydroxide accounts for the total matter of molecular sieve precursor The 14% of amount, tetramethoxy silicone grease accounts for the 21% of molecular sieve precursor gross mass, and methyl silicone grease accounts for molecular sieve precursor gross mass 5%, remaining is water.Proportion selected by material is the ZSM-5 molecular sieve that synthesis has methyl obtained by many experiments in this method Best selection value.
The purpose of third of the present invention is the application for proposing the silicon nitride microballoon of the above area load molecular sieve.
That is, the silicon nitride microballoon of area load molecular sieve is seated in funnel as filtrate.
Using the silicon nitride microballoon of the above area load molecular sieve as filtrate, the filterings material such as filter paper of funnel is substituted Material can effectively absorb and filter the bulky grain in mixed system and have in the case where not influencing water-soluble component in aqueous solution Machine object ingredient.
Detailed description of the invention
Fig. 1 is a kind of schematic diagram of application structure of the invention.
Specific embodiment
One, silicon nitride ceramics microballoon is prepared:
Alpha-silicon nitride powders, alumina powder, yttrium oxide powder are mixed with dispersing agent, deionized water, prepare mixing base Material.
In the above raw material, 0.5 μm~2.5 μm of alpha-silicon nitride powders partial size, additive amount is the 65~90% of total powder weight;Oxygen Change 0.3 μm~5.0 μm of aluminium powder partial size, additive amount is the 2~4% of total powder weight;Yttrium oxide powder partial size be 0.1 μm~ 5.0 μm, additive amount is the 6~8% of total powder weight;Dispersing agent is the 12.8% of total powder weight;Remaining is deionized water, is closed Metering is 100%.
The above dispersing agent is the anion surface active of the adjustable alpha-silicon nitride powders surface potential such as lignosulfonates Agent.
The above mixing blank is squeezed into microballoon mold, is calcined between 1650 DEG C to 1700 DEG C, heat preservation 0.5h~ 3h, pressure 0.5MPa form the silicon nitride ceramics microballoon that diameter is 0.5 ± 0.002cm.
Two, preparation has the ZSM-5 molecular sieve of methyl:
After mixing by sodium chlorate, tetrapropylammonium hydroxide and water, methyl silicone grease and tetramethoxy silicone grease are added, obtains and divides Molecular sieve precursor, is then aged 4 days at 180 DEG C, obtains the ZSM-5 molecular sieve with methyl, silica alumina ratio by son sieve presoma It is 30~40: 1.
Wherein, the sodium chlorate accounts for the 0.2% of molecular sieve precursor gross mass, and tetrapropylammonium hydroxide accounts for molecular sieve forerunner The 14% of body gross mass, tetramethoxy silicone grease account for the 21% of molecular sieve precursor gross mass, and it is total that methyl silicone grease accounts for molecular sieve precursor The 5% of quality, remaining is deionized water, total amount 100%.
Three, the silicon nitride microballoon of area load molecular sieve is prepared:
ZSM-5 molecular sieve with methyl is sprayed on silicon nitride ceramics microsphere surface, under conditions of temperature environment is 80 DEG C Dry solidification to get area load molecular sieve silicon nitride microballoon.
Four, it applies:
1, the production of filter:
The silicon nitride microballoon of area load molecular sieve is fitted into globular glass chamber, the upper/lower terminal of the chamber is respectively provided with One is less than the through-hole of the microspherulite diameter.
Tubaeform glass funnel is welded on a through-hole, straight glass outlet tube is welded on another through-hole.
The product of formation is communicated between tubaeform glass funnel 1 and straight glass outlet tube 2 spherical as shown in Figure 1: Glass chamber 3 is filled with the silicon nitride microballoon 4 of area load molecular sieve in globular glass chamber 3.
2, filtering use and effect:
It is placed below straight glass outlet tube 2 and receives ware, to be filtered mix is added into the tubaeform glass funnel 1 of filter Zoarium system, can be realized effective filtering by the silicon nitride microballoon 4 of the area load molecular sieve in globular glass chamber 3.
Shaggy silicon nitride ceramics microballoon is formed by hot die-casting method, is used as filter base material, existing compared with Large ratio surface Product, and stablize corrosion-resistant, the effective component that may filter that organic matter in aqueous solution is provided --- methylic Supported on Zeolite is supported. Methylic molecular sieve is synthesized by hydro-thermal method, is combined closely by colloid and shaggy silicon nitride microballoon.Methylic point The modification of son sieve can effectively adsorb organic substance so that silicon nitride ceramics microballoon has compared with strong-hydrophobicity, at the same to water with it is water-soluble Property substance generate repulsion.Reach bulky grain and organic filtration, centrifugation in excellent water.
Embodiment described above is only that preferred embodiment of the invention is described, not limiting the scope of the invention, Without departing from the spirit of the design of the present invention, the various changes that those of ordinary skill in the art make technical solution of the present invention Shape and improvement should all fall into the protection scope that claims of the present invention determines.

Claims (10)

1. a kind of silicon nitride microballoon of area load molecular sieve, it is characterised in that: have in the load of silicon nitride ceramics microsphere surface The ZSM-5 molecular sieve of methyl.
2. the silicon nitride microballoon of area load molecular sieve according to claim 1, it is characterised in that: the silicon nitride ceramics is micro- The diameter of ball is 0.5 ± 0.002cm.
3. the preparation method of the silicon nitride microballoon of area load molecular sieve as described in claim 1, it is characterised in that: will have first The ZSM-5 molecular sieve of base is sprayed on silicon nitride ceramics microsphere surface, through drying,.
4. the preparation method of the silicon nitride microballoon of area load molecular sieve according to claim 3, it is characterised in that: described dry Dry temperature environment is 80 DEG C.
5. the preparation method of the silicon nitride microballoon of area load molecular sieve according to claim 3, it is characterised in that: will nitrogenize Si powder, alumina powder, yttrium oxide powder, dispersing agent and deionized water mixing obtain mixing blank, then will mixing blank warp Spherical green body is made in spherical die, then calcines 0.5h~3h under conditions of 1650 DEG C~1700 DEG C and pressure are 0.5MPa, Obtain silicon nitride ceramics microballoon.
6. the preparation method of the silicon nitride microballoon of area load molecular sieve according to claim 5, it is characterised in that: the nitrogen The partial size of SiClx powder is 0.5 μm~2.5 μm, and the partial size of alumina powder is 0.3 μm~5.0 μm, the partial size of yttrium oxide powder It is 0.1 μm~5.0 μm;The alpha-silicon nitride powders account for the 65~90% of mixing blank gross mass, and it is total that alumina powder accounts for mixing blank The 2~4% of quality, yttrium oxide powder account for the 6~8% of mixing blank gross mass.
7. the preparation method of the silicon nitride microballoon of area load molecular sieve according to claim 5, it is characterised in that: described point Powder is lignosulfonates.
8. the preparation method of the silicon nitride microballoon of area load molecular sieve according to claim 3, it is characterised in that: first by chlorine Sour sodium, tetrapropylammonium hydroxide and water after mixing, are blended into methyl silicone grease and tetramethoxy silicone grease, obtain molecular sieve forerunner Then molecular sieve precursor is aged 4 days at 180 DEG C, obtains the ZSM-5 molecular sieve with methyl by body.
9. the preparation method of the silicon nitride microballoon of area load molecular sieve according to claim 8, it is characterised in that: the chlorine Sour sodium accounts for 0.2 % of molecular sieve precursor gross mass, and tetrapropylammonium hydroxide accounts for 14 % of molecular sieve precursor gross mass, tetramethyl Oxygroup silicone grease accounts for the 21% of molecular sieve precursor gross mass, and methyl silicone grease accounts for the 5% of molecular sieve precursor gross mass, remaining for go from Sub- water, total amount 100%.
10. the application of the silicon nitride microballoon of area load molecular sieve as described in claim 1, it is characterised in that: by area load The silicon nitride microballoon of molecular sieve is seated in funnel as filtrate.
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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10309009A1 (en) * 2003-03-01 2004-09-09 Scheffler, Michael, Dr.rer.nat. Zeolite coating of polymer-derived ceramics where e.g. aluminum is added to the coating solution and/or ceramic which acts as a carrier and also provides network-formers
CN102583434A (en) * 2012-03-20 2012-07-18 辽宁工业大学 Method for preparing ZSM-5 zeolite molecular sieve microspheres
CN103372379A (en) * 2013-07-14 2013-10-30 浙江大学 Preparation method of molecular sieve composite membrane by taking metallic oxide as carrier
CN105622109A (en) * 2016-03-17 2016-06-01 长沙理工大学 Preparation method of silicon nitride ceramic ball and silicon nitride ceramic ball
CN106278368A (en) * 2016-08-15 2017-01-04 北京大学深圳研究生院 A kind of composite molecular sieve film and its preparation method and application
CN106999866A (en) * 2014-11-25 2017-08-01 三菱化学株式会社 The manufacture method of porous support zeolite film composite and porous support zeolite film composite
CN107684835A (en) * 2017-08-14 2018-02-13 苏州博清高新材料有限公司 A kind of filter for sewage disposal
CN107902723A (en) * 2017-11-29 2018-04-13 成都创客之家科技有限公司 A kind of silicon nitride base porous ceramics drinking water filter cartridge
CN108264057A (en) * 2016-12-30 2018-07-10 中国石油天然气股份有限公司 A kind of method of the controllable ZSM-5 zeolite of synthesis in solid state wellability
CN109529523A (en) * 2018-11-26 2019-03-29 吉林大学 Molecular sieve core-mesoporous organosilicon hollow shell multi-stage porous composite material and preparation method

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10309009A1 (en) * 2003-03-01 2004-09-09 Scheffler, Michael, Dr.rer.nat. Zeolite coating of polymer-derived ceramics where e.g. aluminum is added to the coating solution and/or ceramic which acts as a carrier and also provides network-formers
CN102583434A (en) * 2012-03-20 2012-07-18 辽宁工业大学 Method for preparing ZSM-5 zeolite molecular sieve microspheres
CN103372379A (en) * 2013-07-14 2013-10-30 浙江大学 Preparation method of molecular sieve composite membrane by taking metallic oxide as carrier
CN106999866A (en) * 2014-11-25 2017-08-01 三菱化学株式会社 The manufacture method of porous support zeolite film composite and porous support zeolite film composite
CN105622109A (en) * 2016-03-17 2016-06-01 长沙理工大学 Preparation method of silicon nitride ceramic ball and silicon nitride ceramic ball
CN106278368A (en) * 2016-08-15 2017-01-04 北京大学深圳研究生院 A kind of composite molecular sieve film and its preparation method and application
CN108264057A (en) * 2016-12-30 2018-07-10 中国石油天然气股份有限公司 A kind of method of the controllable ZSM-5 zeolite of synthesis in solid state wellability
CN107684835A (en) * 2017-08-14 2018-02-13 苏州博清高新材料有限公司 A kind of filter for sewage disposal
CN107902723A (en) * 2017-11-29 2018-04-13 成都创客之家科技有限公司 A kind of silicon nitride base porous ceramics drinking water filter cartridge
CN109529523A (en) * 2018-11-26 2019-03-29 吉林大学 Molecular sieve core-mesoporous organosilicon hollow shell multi-stage porous composite material and preparation method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
FENG HUI: "In-situ synthesis of ZSM-5 on silica gel and studies on its catalytic activity", 《JOURNAL OF FUEL CHEMISTRY AND TECHNOLOGY》 *

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Application publication date: 20190726