CN101070147A - Zirconium sulfuride intercalation assembling functional material producing method - Google Patents

Zirconium sulfuride intercalation assembling functional material producing method Download PDF

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CN101070147A
CN101070147A CN 200610078704 CN200610078704A CN101070147A CN 101070147 A CN101070147 A CN 101070147A CN 200610078704 CN200610078704 CN 200610078704 CN 200610078704 A CN200610078704 A CN 200610078704A CN 101070147 A CN101070147 A CN 101070147A
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intercalation
zirconium phosphate
zirconium
functional material
phosphate crystal
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吴良恒
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JIANGSU LVLING CHEMICAL GROUP CO Ltd
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JIANGSU LVLING CHEMICAL GROUP CO Ltd
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Abstract

It is a kind of intercalation assembly functional material made of zirconium phosphate, this material is combined with products of craft such as existing building materials, man-made plate, paper, dope and so on. It regards layers of zirconium phosphate as carriers, make a kind of zirconium phosphate intercalation assembly functional material which can absorb complex and harmonizing functional material such as formaldehyde and ammonia through layer-intercalating molecular, interlayer structure and assembly mode to design and adjust and control. The molecular formula is {Zr[(C2H5)4(NH2)5PO4]4.nH2O}.

Description

A kind of Zirconium sulfuride intercalation assembling functional material producing method
Technical field
The present invention relates to the bedded zirconium phosphate is carrier, prepares a kind of compound coordination function material of absorption (formaldehyde, ammonia) that has.
Background technology
" room air pollution " become the third-largest source of pollution after " pollution of bituminous coal type " and " pollution of photo-chemical smog type ".Room, back formaldehyde is newly fitted up by China, ammonia content generally exceeds standard, and ratio is generally more than 80%.Special survey that one in the U.S. lasts 5 years finds, indoor atmospheric pollution be outdoor 2-5 doubly, have in addition surpass 100 times, about 68% human body diseases is relevant with indoor pollution.Therefore, along with both at home and abroad indoor environment being required to improve day by day, how to avoid having become current important subject with the treatment chamber internal contamination.The domestic and international at present processing means that indoor gas is polluted, can reduce following a few class: 1, in the chemistry and technology (formaldehyde-trapping agent) 2, physical adsorption techniques (air purifier) 3, material seal technology 4, photocatalysis technology 5, the domestic and international prior art of negative aeroion technical Analysis, can find: the starting point of (1) most of technology is to eliminate the free formaldehyde that has discharged, cure the symptoms, not the disease, and this release will continue 5-15.Along with progressively implementing and the strict regulation of checking and accepting of fitting up of novel industry standards such as national building materials, the product that formaldehyde content is high can't come into the market, and this The Application of Technology market is with atrophy greatly; (2) attention degree of PARA FORMALDEHYDE PRILLS(91,95) generally is higher than other unwanted components such as ammonia at present, and considerable formaldehyde treated technology is not obvious to the ammonia effect.The improvement of indoor environment should consider that therefore the material of development should possess complex function from comprehensive aspect; (3) although photochemical catalysis, anion material can partly reach above-mentioned requirements, they are stronger to the dependency of outside, as light, air flowing etc., but add behind the artificial plate because isolated with the outside, its effect will only be surface composition, effect reduces; (4) though present formaldehyde-trapping agent is obvious to handling the formaldehyde effect, but because reasons such as thermodynamic stability is low, chemical compatibility difference, can not directly combine as filler with existing artificial board, coating, clear and the printing ink industry silicon oxide surface that once the amino-benzene yellow acid was attached to of Japan, and unresolved addressing the above problem.
Summary of the invention
In order to solve product formaldehyde, ammonias such as existing building materials, wood-based plate, paper, the coating problem that exceeds standard, the present invention is carrier with the bedded zirconium phosphate, the rare five amine alcohol of interlayer assembling tetrem organo-functional group, by intercalation molecule, interlayer structure, assembling mode design and regulation and control, prepare a kind of Zirconium sulfuride intercalation assembling functional material with the compound coordination function of absorption (formaldehyde, ammonia).
Technical scheme of the present invention
Technological line:
At first, synthesize phosphoric acid salt stratiform compound (M IV(HPO 4) 2NH 2O (M:Zr, Ce)) layered vector is regulated crystal water content, phosphoric acid functional group (PO in metallic element or the product by reaction conditions 4 3-, H 2PO 4 -) stoichiometry, make the adjustable in the 0.76-1.8nm scope of its interlamellar spacing;
Secondly, by surface functional group and interlayer design, make layered vector and functional group form layered composite structure;
The 3rd, in aqueous environment, with organic constituent between component displacement layer such as fat polyamine, polyvalent alcohol, by the preparation process condition, the control replacement amount, retained part not substitute activity component is the assimilating activity point of ammonia, obtains the coordination function material;
At last, after filtration, washing and thermal treatment obtains the finished product, detect and carry out application test.
Embodiment:
Main raw material: chlorine oxygen zirconium, phosphoric acid, polyamine, organic amine, alcohol, organic acid etc.
Major equipment: reactor (tetrafluoro liner), pressure filter, Equipment for Heating Processing, dispersion treatment and surface design device (control oneself and design and produce) etc.
Detection means: utilize XRD, IR, MRS, IP, TEM.SEM, means such as BET characterize product component, microtexture, physical and chemical performance and process mechanism; Formaldehyde and ammonia absorb and adopt twenty-feet equivalent unit-spectral absorption to measure and entrust detection;
Product application: adopt and in coating, Furniture panel, to dose mode and carry out, entrust relevant quality inspection organization assessed for performance and effect.
Specific embodiments
The carbonyl of formaldehyde is a unsaturated group, and many addition reactions take place easily.It is different with ethylene linkage, acetylene bond, and Sauerstoffatom nuclear is outer 8 electronics, and carbon nuclei has 6 electronics outward, and the electronegativity of Sauerstoffatom is stronger than carbon atom, so the two keys of carbon oxygen are a kind of band polar unsaturated link(age)s.Exist just because of this polar, the easier attack that is subjected to nucleophile of carbon atom in the carbonyl, many aminocompounds all are nucleophiles, can with the carbonyl addition, and addition reaction not merely rests on one step of addition, but lose water by intramolecularly in succession, and forming the two keys of carbon-oxygen, can represent with following equation:
Figure A20061007870400051
Y is amino (H in the formula 2N-) other group in addition.
Nitrogen-atoms in the amino combines with carbon atom in the carbonyl with its not shared electron pair, and a pair of transfer transport of π key forms a unstable intermediate between carbon-oxygen to oxygen, and this intermediate is once form, and hydrogen ion is moved on the oxygen by nitrogen at once, forms hydramine.By losing a part water in the hydramine, form the two keys of carbon-oxygen at last.By the addition of nucleophile and formaldehyde, make unbound state formaldehyde change into new compound and be fixed.The assembling tetraethylene pentamine is made formaldehyde absorption reaction component, thereby obtains Zirconium sulfuride intercalation assembling functional material, and its molecular formula is Zr[(C 2H 5) 4(NH 2) 5PO 4] 4NH 2O}.

Claims (4)

1, a kind of Zirconium sulfuride intercalation assembling functional material is characterized in that having adopted more optimized process conditions production Zirconium phosphate crystal, in advance to the Zirconium phosphate crystal intercalation processing, then it is replaced into fat polyamine by alkanamine.
2, according to claim 1, phosphoric acid salt stratiform compound (M IV(HPO 4) 2NH 2Preparation process and the technological design of O (M:Zr, Ce)).
3, according to claim 1, synthesis condition is after the zirconium phosphate optimization: F/Zr<2.0; [H 3PO 4]>0.5M, reaction times 2-4 hour; Temperature of reaction 70-90 ℃, product yield>95%, advantages of good crystallization, it is few to reunite, median size 3.9 μ m.
4, according to claim 1, in that directly Zirconium phosphate crystal to be carried out the intercalation time long, weak effect, be difficult under the suitability for industrialized production situation, the n-Butyl Amine 99 that we select can not occur peeling off under specific molar ratio carries out pre-intercalation, increase the interlamellar spacing of Zirconium phosphate crystal, at room temperature carry out intercalation processing with tetramine ethene five amine again, making originally, the interlamellar spacing of 7.6  is increased to more than 20 .
CN 200610078704 2006-05-10 2006-05-10 Zirconium sulfuride intercalation assembling functional material producing method Pending CN101070147A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101829544A (en) * 2010-05-11 2010-09-15 常州大学 High-capacity zirconium phosphate material for absorbing phenolic compound and preparation method thereof
CN103011118A (en) * 2012-12-10 2013-04-03 常州大学 Method for preparing zirconium phosphate layer column material by guide assembly technology

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101829544A (en) * 2010-05-11 2010-09-15 常州大学 High-capacity zirconium phosphate material for absorbing phenolic compound and preparation method thereof
CN103011118A (en) * 2012-12-10 2013-04-03 常州大学 Method for preparing zirconium phosphate layer column material by guide assembly technology
CN103011118B (en) * 2012-12-10 2014-08-13 常州大学 Method for preparing zirconium phosphate layer column material by guide assembly technology

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