CN107159106A - A kind of preparation method of formaldehyde adsorbent and obtained formaldehyde adsorbent - Google Patents
A kind of preparation method of formaldehyde adsorbent and obtained formaldehyde adsorbent Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
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Abstract
The present invention provides a kind of preparation method of formaldehyde adsorbent, including：(1) pre-process：Molecular screen primary powder is dried 6 hours at 100 150 DEG C, is calcined 3 hours in 400 550 DEG C, room temperature is cooled in drier, is pulverized and sieved；(2) surface is alkalization modified：Gained sample is in Na2CO3Na is impregnated in solution2CO3Filter, obtained filter residue is dried 6 hours at 100 150 DEG C, be calcined 3 hours in 400 550 DEG C after 12.5 15 hours in solution, drying pulverizes and sieves；(3) transition metal ion-modified：Gained sample is placed in 0.015mol ˙ L‑1In soluble transition metal solution, stirred 3 hours at 70 90 DEG C, filtering is washed 3 times with deionized water, is dried 6 hours at 100 150 DEG C, is calcined 3 hours in 400 550 DEG C；(4) repeat step (3) twice, produces formaldehyde adsorbent.The formaldehyde adsorbent that the present invention is obtained is selectively strong, and PARA FORMALDEHYDE PRILLS(91,95) class polar molecule affinity is high, and receiving space is big, and absorption affinity is strong, in the absence of desorption phenomenon, and reliability is high, other pollutants such as also adsorbable indoor benzene homologues, ammonia.
Description
Technical field
The present invention relates to purification air technique field, and in particular to a kind of formaldehyde adsorbent preparation method.
Background technology
Formaldehyde is a kind of very important indoor air pollutants, and the harm to human body is especially prominent, studies room air
The removing of middle formaldehyde has very important significance.At present, absorption method has become harmful rotten gas in adsorbing and removing air
A kind of very effective control device, it mainly uses the absorption property of porous material to realize harmful and foul gas
Adsorbing and removing.Absorption method is suitable for almost all harmful rotten gases, have become removing pernicious gas it is the more commonly used one
Plant simple and direct and effective method.Activated carbon is a kind of conventional adsorbent, and some air cleaning units all use activated carbon conduct
Adsorbent.Because normal activated carbon is that surface is nonpolar, hydrophobic, the absorption affinity of this kind of polar molecule of PARA FORMALDEHYDE PRILLS(91,95) is limited,
And there is desorption phenomenon, it is impossible to effectively reduce indoor formaldehyde concentration.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides the preparation method and obtained formaldehyde absorbing of a kind of formaldehyde adsorbent
Agent, is made formaldehyde adsorbent by surface alkalization and transition metal ion-modified using molecular screen primary powder, indoor first is greatly reduced
Aldehyde concentration.
To solve the above problems, the technical solution adopted by the present invention is as follows：
A kind of preparation method of formaldehyde adsorbent, comprises the following steps：
(1) pre-process：Molecular screen primary powder is dried 6 hours at 100-150 DEG C, is calcined 3 hours in 400-550 DEG C, is dried
Room temperature is cooled in device, is pulverized and sieved, the sample that granularity is 20-40 mesh is taken；
(2) surface is alkalization modified：By sample obtained by step (1) in Na2CO3Na is impregnated in solution2CO312.5- in solution
Filter, obtained filter residue is dried 6 hours at 100-150 DEG C, be calcined 3 hours in 400-550 DEG C after 15 hours, dried, crushed
Sieving, takes Na in the sample that granularity is 20-40 mesh, this step2CO3The concentration of solution is 0.010-0.014molL-1, Na2CO3
The addition of solution is 50ml/ grams of sample；
(3) transition metal ion-modified：Sample obtained by step (2) is placed in 0.015molL-1Soluble transition metal is molten
In liquid, the addition of soluble transition metal solution is 80ml/ grams of sample, is stirred 3 hours at 70-90 DEG C, and deionization is used in filtering
Water is washed 3 times, is dried 6 hours at 100-150 DEG C, is calcined 3 hours in 400-550 DEG C；
(4) repeat step (3) twice, produces formaldehyde adsorbent.
Preferably, in step (3), the soluble transition metal solution is cobalt nitrate solution or copper nitrate solution.
Preferably, the molecular screen primary powder is the former powder of X-type zeolite molecular sieve or ZSM-5 zeolite molecular screen primary powder.
A kind of formaldehyde adsorbent, the formaldehyde adsorbent is made using any one above-mentioned method.
In summary, by adopting the above-described technical solution, the beneficial effects of the invention are as follows：
1st, molecular sieve is selectively strong, and PARA FORMALDEHYDE PRILLS(91,95) class polar molecule affinity is high；Internal cellular shape structure exists a large amount of uniform
Hole, specific surface area is big, and receiving space is big；Absorption affinity is strong, and in the absence of desorption phenomenon, reliability is high.
2nd, using surface alkalization and the chemiluminescence of two kinds of method of modifying of transition metal ions, effectively enhancing formaldehyde is inhaled
The suction-operated of attached dose of PARA FORMALDEHYDE PRILLS(91,95).
3rd, while other pollutants such as also adsorbable indoor benzene homologues, ammonia.
Embodiment
All features disclosed in this specification, can be with any in addition to mutually exclusive feature and/or step
Mode is combined.
Embodiment 1
Pretreatment：X-type zeolite molecular sieve original powder is dried 6 hours at 120 DEG C, removes absorption a large amount of on molecular screen primary powder
Free water, is calcined 3 hours in 500 DEG C, room temperature is cooled in drier, is pulverized and sieved, and takes the sample that granularity is 20-40 mesh；
Surface is alkalization modified：By sample obtained by pre-treatment step in Na2CO3Na is impregnated in solution2CO3Filtered in solution after 13 hours,
Obtained filter residue is dried 6 hours at 120 DEG C, is calcined 3 hours in 500 DEG C, and drying pulverizes and sieves, and it is 20-40 purposes to take granularity
Na in sample, this step2CO3The concentration of solution is 0.010molL-1, Na2CO3The addition of solution is 50ml/ grams of sample；Cross
Cross metal ion-modified：Sample obtained by the alkalization modified step in surface is placed in 0.015molL-1In cobalt nitrate solution, cobalt nitrate
The addition of solution is 80ml/ grams of sample, is stirred 3 hours at 75 DEG C, and filtering is washed 3 times with deionized water, and 6 are dried at 120 DEG C
Hour, it is calcined 3 hours in 500 DEG C；Repeat transition metal ion-modified step twice, produce formaldehyde adsorbent.
In the present embodiment, molecular sieve has a large amount of positively charged aluminium ions in the skeleton structure of spaciousness, molecular sieve to make boiling
Stone has strong electrostatic field, easily adsorbs polar molecule.X-type molecular sieve has the sial oxygen skeleton structure of faujasite, faujasite
Communicated between cage by twelve-ring, the formaldehyde molecule of absorption is easy to move into supercage.Na2CO3Solution is stronger as a kind of alkalescence
Alkaline solution, it is acid effectively to lower sample surfaces, and it is too strong and cause sample interior hole to change to be unlikely to alkalescence.
Transition metals cobalt has after changeable d layer electronics, ion exchange, changes simple hydrogen ion and sodium ion electron outside nucleus originally
Layer, causes the electric charge around cobalt ions to redistribute so that the electrostatic field inside molecular sieve is further enhanced, polarity increase, from
And improve the absorption property to polar molecule formaldehyde.
Embodiment 2
Pretreatment：X-type zeolite molecular sieve original powder is dried 6 hours at 120 DEG C, is calcined 3 hours in 500 DEG C, in drier
Room temperature is cooled to, is pulverized and sieved, the sample that granularity is 20-40 mesh is taken；Surface is alkalization modified：Sample obtained by pre-treatment step is existed
Na2CO3Na is impregnated in solution2CO3Filtered in solution after 13 hours, obtained filter residue is dried 6 hours at 120 DEG C, at 500 DEG C
Middle roasting 3 hours, drying pulverizes and sieves, and takes Na in the sample that granularity is 20-40 mesh, this step2CO3The concentration of solution is
0.010mol·L-1, Na2CO3The addition of solution is 50ml/ grams of sample；Transition metal ion-modified：Surface is alkalization modified
Sample obtained by step is placed in 0.015molL-1In copper nitrate solution, the addition of copper nitrate solution is 80ml/ grams of sample, 75
DEG C stirring 3 hours, filtering, with deionized water wash 3 times, 120 DEG C dry 6 hours, in 500 DEG C be calcined 3 hours；Repeated
Cross metal ion-modified step twice, produce formaldehyde adsorbent.
In the present embodiment, transition metal copper has after changeable d layer electronics, ion exchange, change originally simple hydrogen from
Son and sodium ion electron outside nucleus layer, cause the electric charge around copper ion to redistribute so that the electrostatic field inside molecular sieve enters one
Step enhancing, polarity is increased to improve the absorption property to polar molecule formaldehyde.
Embodiment 3
Pretreatment：ZSM-5 zeolite molecular screen primary powder is dried 6 hours at 120 DEG C, is calcined 3 hours in 500 DEG C, drier
In be cooled to room temperature, pulverize and sieve, take granularity be 20-40 mesh sample；Surface is alkalization modified：By sample obtained by pre-treatment step
In Na2CO3Na is impregnated in solution2CO3Filtered in solution after 13 hours, obtained filter residue is dried 6 hours at 120 DEG C, 500
It is calcined 3 hours in DEG C, drying pulverizes and sieves, and takes Na in the sample that granularity is 20-40 mesh, this step2CO3The concentration of solution is
0.010mol·L-1, Na2CO3The addition of solution is 50ml/ grams of sample；Transition metal ion-modified：Surface is alkalization modified
Sample obtained by step is placed in 0.015molL-1In cobalt nitrate solution, the addition of cobalt nitrate solution is 80ml/ grams of sample, 75
DEG C stirring 3 hours, filtering, with deionized water wash 3 times, 120 DEG C dry 6 hours, in 500 DEG C be calcined 3 hours；Repeated
Cross metal ion-modified step twice, produce formaldehyde adsorbent.
In the present embodiment, ZSM-5 category rhombic systems, with three-dimensional channel structure, include two kinds of ducts that intersect, aperture
It is made up of ten-ring, the formaldehyde molecule of absorption is easy to move into supercage.
Embodiment 4
Pretreatment：ZSM-5 zeolite molecular screen primary powder is dried 6 hours at 120 DEG C, is calcined 3 hours in 500 DEG C, drier
In be cooled to room temperature, pulverize and sieve, take granularity be 20-40 mesh sample；Surface is alkalization modified：By sample obtained by pre-treatment step
In Na2CO3Na is impregnated in solution2CO3Filtered in solution after 13 hours, obtained filter residue is dried 6 hours at 120 DEG C, 500
It is calcined 3 hours in DEG C, drying pulverizes and sieves, and takes Na in the sample that granularity is 20-40 mesh, this step2CO3The concentration of solution is
0.010mol·L-1, Na2CO3The addition of solution is 50ml/ grams of sample；Transition metal ion-modified：Surface is alkalization modified
Sample obtained by step is placed in 0.015molL-1In copper nitrate solution, the addition of copper nitrate solution is 80ml/ grams of sample, 75
DEG C stirring 3 hours, filtering, with deionized water wash 3 times, 120 DEG C dry 6 hours, in 500 DEG C be calcined 3 hours；Repeated
Cross metal ion-modified step twice, produce formaldehyde adsorbent.
Comparative example 1
On the basis of embodiment 1, the step for saving transition metal ion-modified, remaining is identical with embodiment 1.
Comparative example 2
On the basis of embodiment 1, the step for surface is alkalization modified is saved, remaining is identical with embodiment 1.
Comparative example 3
On the basis of embodiment 4, the step for saving transition metal ion-modified, remaining is identical with embodiment 4.
Comparative example 4
On the basis of embodiment 4, the step for surface is alkalization modified is saved, remaining is identical with embodiment 4.
To formaldehyde adsorbent, activated carbon, X-type zeolite made from formaldehyde adsorbent made from embodiment 1-4, comparative example 1-2
Molecular screen primary powder and ZSM-5 zeolite molecular screen primary powder carry out performance test：Evaluated in continuous flowable state preventing fixed bed adsorber
The absorption property of adsorbent.The sample of sorbent accurately measured, is uniformly filled in ADSORPTION IN A FIXED BED post；Activated in nitrogen
Afterwards, after starting absorption after formaldehyde raw material gas constant concentration, adsorption column keeps 35 DEG C of constant temperature；It is online by chromatogram in experimentation
The change of concentration of formaldehyde, draws adsorption breakthrough curve, passes through breakthrough curve integral and calculating adsorbance in the front and rear gas of monitoring absorption；
When the concentration of formaldehyde in absorption tail gas reach entrance concentration when, define adsorption column and penetrate, the time now undergone is penetrates
Time.Specific test result is as shown in table 1.
The time of break-through and adsorbance of the different adsorbent PARA FORMALDEHYDE PRILLS(91,95)s of table 1
| Adsorbent | Time of break-through (min) | Adsorbance (mg/ml) |
| Embodiment 1 | 760 | 233.6 |
| Embodiment 2 | 744 | 227.1 |
| Embodiment 3 | 753 | 230.7 |
| Embodiment 4 | 741 | 225.8 |
| Comparative example 1 | 576 | 175.0 |
| Comparative example 2 | 459 | 141.6 |
| Comparative example 3 | 572 | 173.8 |
| Comparative example 4 | 448 | 138.2 |
| Activated carbon | 3 | 0.9 |
| X-type zeolite molecular sieve original powder | 370 | 113.0 |
| ZSM-5 zeolite molecular screen primary powder | 368 | 112.5 |
As can be seen from Table 1：Under identical testing conditions, the effect of X-type and the former powder formaldehyde adsorption of ZSM-5 molecular sieve is big
Cause is identical, far above activated carbon；Comparative example 1-4 understands, through surface is alkalization modified or transition metal ion-modified after, formaldehyde
Adsorbent formaldehyde adsorption effect increases, and surface is alkalization modified more preferable than transition metal ion-modified effect；Embodiment
1-4 is understood, modified twice through surface alkalization and transition metal ions, and formaldehyde adsorbent formaldehyde adsorption effect changes compared with surface alkalization
Property and transition metal ion-modified adsorption effect superposition increases twice, show that surface is alkalization modified and transition metal ions changes
Property has chemiluminescence to molecular sieve adsorption effect of formaldehyde.
Claims (4)
1. a kind of preparation method of formaldehyde adsorbent, it is characterised in that comprise the following steps：
(1) pre-process：Molecular screen primary powder is dried 6 hours at 100-150 DEG C, is calcined 3 hours in 400-550 DEG C, in drier
Room temperature is cooled to, is pulverized and sieved, the sample that granularity is 20-40 mesh is taken；
(2) surface is alkalization modified：By sample obtained by step (1) in Na2CO3Na is impregnated in solution2CO312.5-15 is small in solution
When after filter, obtained filter residue 100-150 DEG C dry 6 hours, in 400-550 DEG C be calcined 3 hours, drying, pulverize and sieve,
Take Na in the sample that granularity is 20-40 mesh, this step2CO3The concentration of solution is 0.010-0.014mol ˙ L-1, Na2CO3Solution
Addition is 50ml/ grams of sample；
(3) transition metal ion-modified：Sample obtained by step (2) is placed in 0.015mol ˙ L-1In soluble transition metal solution,
The addition of soluble transition metal solution is 80ml/ grams of sample, is stirred 3 hours at 70-90 DEG C, and deionized water water is used in filtering
Wash 3 times, dried 6 hours at 100-150 DEG C, is calcined 3 hours in 400-550 DEG C；
(4) repeat step (3) twice, produces formaldehyde adsorbent.
2. the preparation method of formaldehyde adsorbent according to claim 1, it is characterised in that：In step (3), the solubility
Transition metal solution is cobalt nitrate solution or copper nitrate solution.
3. formaldehyde adsorbent according to claim 1, it is characterised in that the molecular screen primary powder is X-type zeolite molecular sieve
Former powder or ZSM-5 zeolite molecular screen primary powder.
4. a kind of formaldehyde adsorbent, it is characterised in that：Using claim 1-3, any one method is made the formaldehyde adsorbent.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111437874A (en) * | 2020-03-02 | 2020-07-24 | 珠海格力电器股份有限公司 | Formaldehyde removal catalyst and preparation method and application thereof |
| CN115709094A (en) * | 2022-11-14 | 2023-02-24 | 化学与精细化工广东省实验室 | Non-noble metal catalyst for formaldehyde purification and preparation method thereof |
| CN115715970A (en) * | 2022-11-18 | 2023-02-28 | 浙江工业大学 | Black talc-based nano mineral crystal and preparation method thereof |
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| CN102247746A (en) * | 2011-07-18 | 2011-11-23 | 哈尔滨工程大学 | Formaldehyde elimination agent and preparation method thereof |
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| CN104741130A (en) * | 2013-12-27 | 2015-07-01 | 江苏瑞丰科技实业有限公司 | Normal temperature formaldehyde removal catalysis material |
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| CN101932383A (en) * | 2008-01-25 | 2010-12-29 | 道达尔石油化学产品研究弗吕公司 | Process for obtaining modified molecular sieves |
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| CN111437874A (en) * | 2020-03-02 | 2020-07-24 | 珠海格力电器股份有限公司 | Formaldehyde removal catalyst and preparation method and application thereof |
| CN115709094A (en) * | 2022-11-14 | 2023-02-24 | 化学与精细化工广东省实验室 | Non-noble metal catalyst for formaldehyde purification and preparation method thereof |
| CN115715970A (en) * | 2022-11-18 | 2023-02-28 | 浙江工业大学 | Black talc-based nano mineral crystal and preparation method thereof |
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Application publication date: 20170915 |