CN109603896A - A kind of purifying formaldehyde material - Google Patents
A kind of purifying formaldehyde material Download PDFInfo
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- CN109603896A CN109603896A CN201811643222.XA CN201811643222A CN109603896A CN 109603896 A CN109603896 A CN 109603896A CN 201811643222 A CN201811643222 A CN 201811643222A CN 109603896 A CN109603896 A CN 109603896A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
- B01J29/0316—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41 containing iron group metals, noble metals or copper
- B01J29/0325—Noble metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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Abstract
The present invention provides a kind of purifying formaldehyde materials, are made of DD3R molecular sieve and noble metal active component, are calculated with the type 100% of catalyst, and the mass fraction of molecular sieve is 90-95%, and the mass fraction of noble metal active component is 5-10%.The present invention is selected by the absorption carrier to noble metal active ingredient, ensure that it carries out Preferential adsorption decomposition for the formaldehyde in gas, to ensure that the decomposing and purifying rate of formaldehyde.
Description
Technical field
This application involves a kind of material for air purification more particularly to a kind of materials purified at room temperature to formaldehyde in air
Material.
Background technique
The harmful substances such as formaldehyde, benzene,toluene,xylene can be released in newly-decorated house, these harmful substances are to people
Body harm is especially big, and Long Term Contact can cause to seriously affect to human health even can threat to life.Relative to other types dirt
Gas is contaminated down to 6 months deenergized periods, and the deenergized period of formaldehyde is longer, or is up to 3-15.So being passed through after house decoration
After the ventilation for spending some months dissipates taste, need preferentially preferentially to purify the formaldehyde in interior.Common formaldehyde pollutants are gone
Except method has physisorphtion (such as active carbon, molecular sieve), bioanalysis, Ozonation, plant degradation method and catalysis oxygen
Change method etc..Physical method is easy to be influenced by absorption aperture using porous material removal formaldehyde and absorbability is limited；Bioanalysis
Once although removal effect of formaldehyde is good but harm caused by microorganism leakage is bigger；Ozonation be easy to cause secondary
Pollution；Plant degradation method can be limited to a certain extent with degradation of formaldehyde but the absorbability of its PARA FORMALDEHYDE PRILLS(91,95), this method can
To remove formaldehyde as auxiliary；Catalytic oxidation is currently used removal formaldehyde the best way.
Catalyst used by common catalytic oxidation is frequently with molecular sieve (such as ZSM-5, HY, MCM-41, MCM-
48, NaY, SBA-15 etc.), the porous materials such as titanium oxide are as catalyst carrier.But discovery formaldehyde is urged in practical applications
Change is decomposed into water and carbon dioxide, and wherein water will lead to catalyst inactivation, carbon dioxide and can be adsorbed by porous material, cause to urge
The performance that formaldehyde is catalytically decomposed in agent is lower and lower.Moreover, preparation catalyst material experimental determination effect with actually answer
It is larger with middle difference on effect, this is because effect measuring is carried out frequently with single formaldehyde gas in laboratory, and practical application
Gas in other than formaldehyde also containing a plurality of types of gas types such as benzene,toluene,xylene, acetone, water, exist with formaldehyde
Competitive Adsorption is generated in catalytic process, causes last purifying formaldehyde effect and efficacy in laboratory difference huge.
In view of the above-mentioned problems, the present invention provides a kind of purification materials purified for formaldehyde in indoor air gas
Material, overcomes a variety of polluted gas technical problem that competitive Adsorption causes purifying formaldehyde rate low on the adsorbent material.
Summary of the invention
The present invention provides a kind of purifying formaldehyde materials, are made of DD3R molecular sieve and noble metal active component, to urge
The type 100% of agent calculates, and the mass fraction of molecular sieve is 90-95%, and the mass fraction of noble metal active component is 5-10%；
The preparation method of the purifying formaldehyde material the following steps are included:
(1) water, amantadine and cosolvent are mixed, handling through high frequency ultrasound is completely dissolved amantadine, and stirs in ice bath
The salting liquid of silicon source and noble metal is added dropwise under the conditions of mixing, then is aged to form amantadine through high-temperature stirring: silicon source: noble metal source:
Cosolvent: water molar ratio is the Synthesis liquid of 30-50:100:5-20:100-500:5000-50000；
(2) crystal seed well prepared in advance is added in Synthesis liquid according to the mass ratio that mass ratio is 0.2-2%, and by Synthesis liquid
It is placed in microwave reaction kettle, and stirs hydrothermal synthesis 48-72h under microwave condition, synthesis temperature is 150-180 DEG C；
(3) after hydrothermal synthesis, the Synthesis liquid in microwave reaction kettle is poured into container for evaporation and is evaporated moisture in Synthesis liquid
And solid material is dried；
(4) solid material of drying roasts 3-4h under ozone environment to prepare required purifying formaldehyde material.
Preferably, the maturing temperature of Yu Suoshu is 300-400 DEG C.
Preferably, the noble metal is one of Pt, Pd, Au and Ag or a variety of.
Preferably, the cosolvent is ethylenediamine.
Preferably, the crystal seed is one of sigma-1, DD3R and ZSM-58.
Preferably, the solid material of drying is ground before roasting.
Preferably, the frequency of the high frequency ultrasound is 20-25kHz, power 500-1800w.
Preferably, the crystal seed is the sieve particle of non-removed template method.
Advantages of the present invention
1. firstly, the present invention uses silica zeolite as adsorbent material, in the water and air for avoiding Formaldehyde decomposition generation
Hydrone by molecular sieve absorb to reduce catalyst inactivation a possibility that.
2. secondly, the present invention uses DD3R molecular sieve as adsorbent material, since the molecular sieve pore passage diameter of DDR configuration is big
In the kinetic diameter of formaldehyde, and it is less than between the dynamics of pollution gas such as benzene,toluene,xylene, acetone, therefore can be with
It avoids other pollution gas from entering in the duct DD3R to be adsorbed, ensure that the opposite single adsorption of adsorbent material PARA FORMALDEHYDE PRILLS(91,95) gas
Property.
3. in addition, since Formaldehyde decomposition can also generate carbon dioxide gas, and can also have a certain amount of dioxy in air
Change carbon, the present invention also mixes the salting liquid of noble metal with the Synthesis liquid of DD3R molecular sieve, will be expensive using in-situ synthesis
Metal Supported is on sieve particle, and part noble metal enters in framework of molecular sieve instead of element silicon, and due to noble metal
Ionic radius be greater than silicon, so as to cause molecular sieve bore diameter relative reduction so that have the dynamics close with the aperture DDR between
The adsorptivity of carbon dioxide be minimized, similarly ensure that the opposite single adsorption of adsorbent material PARA FORMALDEHYDE PRILLS(91,95) gas.
4. its synthetic method is optimized in the present invention, such as using high-power for DD3R molecular sieve adsorbent material
High frequency ultrasound instrument guarantees the hands such as the dissolution of amantadine, the specific surface area for using the mode of microwave cooperation stirring to reduce material
Section guarantees that finally prepd material has excellent purifying formaldehyde ability.
Specific embodiment
Embodiment 1
(1) amantadine is broken into graininess to be put into beaker, and is broken after adding suitable ethylenediamine, water using ultrasonic cell
Broken instrument carries out ultrasonic treatment 15min, setpoint frequency 20kHz, power 900w to it.Ice water is placed the beaker after ultrasonic treatment
In mixture, rotor is added after its cooling, suitable silica solution and H2PtCl4 solution are successively added dropwise under stirring.Drop
After adding, jar agitation is heated to 90 DEG C and keeps 30min to form amantadine: silicon source: noble metal source: ethylenediamine:
Water molar ratio is the Synthesis liquid of 47:100:10:400:11240.
(2) by DD3R sieve particle well prepared in advance after ball milling (partial size 300nm) according to mass ratio be 0.5%
Mass ratio be added in Synthesis liquid, and Synthesis liquid is placed in microwave reaction kettle, and stir hydrothermal synthesis under microwave condition
For 72h to guarantee that the silicon source in Synthesis liquid is utilized entirely, synthesis temperature is 160 DEG C.
(3) after hydrothermal synthesis, the Synthesis liquid in microwave reaction kettle is poured into container for evaporation, makes to synthesize at high temperature
Moisture is evaporated and dries in liquid, and will reunite makes its dispersion with solid particle grinding together.
(4) solid material of drying roasts 3-4h under ozone environment to preparing required purifying formaldehyde materials A,
Set temperature is 300 DEG C.
Comparative example 1
(1) using silica solution as silicon source, TPAOH is template, and being configured to molar ratio with deionized water is SiO2: H2PtCl4:
TPAOH: H2O=100:10: 5: 1000 Synthesis liquid.
(2) by silicalite-1 molecular sieve well prepared in advance, (partial size 300nm) according to mass ratio is after ball milling
0.5% mass ratio is added in Synthesis liquid, and Synthesis liquid is placed in microwave reaction kettle, and stirs hydro-thermal under microwave condition
72h is synthesized, synthesis temperature is 160 DEG C.
(3) after hydrothermal synthesis, the Synthesis liquid in microwave reaction kettle is poured into container for evaporation, makes to synthesize at high temperature
Moisture is evaporated and dries in liquid, and will reunite makes its dispersion with solid particle grinding together.
(4) solid material of drying roasts 3-4h under ozone environment to prepare required purifying formaldehyde material
D1, set temperature are 300 DEG C.
Documents 2
(1) amantadine is broken into graininess to be put into beaker, and is broken after adding suitable ethylenediamine, water using ultrasonic cell
Broken instrument carries out ultrasonic treatment 15min, setpoint frequency 20kHz, power 900w to it.Ice water is placed the beaker after ultrasonic treatment
In mixture, rotor is added after its cooling, suitable silica solution is added dropwise under stirring.After completion of dropwise addition, beaker is stirred
Mix and be heated to 90 DEG C and keep 30min to form amantadine: silicon source: ethylenediamine: water molar ratio is 47:100:400:11240
Synthesis liquid.
(2) by DD3R sieve particle well prepared in advance after ball milling (partial size 300nm) according to mass ratio be 0.5%
Mass ratio be added in Synthesis liquid, and Synthesis liquid is placed in microwave reaction kettle, and stir hydrothermal synthesis under microwave condition
For 72h to guarantee that the silicon source in Synthesis liquid is utilized entirely, synthesis temperature is 160 DEG C.
(3) after hydrothermal synthesis, Synthesis liquid centrifugation, cleaning, the drying in microwave reaction kettle are obtained into DD3R molecular sieve
Particle.Sieve particle is dispersed in H2PtCl4 solution, after stirring a period of time, moisture is removed in 80 DEG C of stirring evaporations and dries
It is dry.
(4) solid material of drying roasts 3-4h under ozone environment to prepare required purifying formaldehyde material
D2, set temperature are 300 DEG C.
Comparative example 3
(1) amantadine is broken into graininess to be put into beaker, and is broken after adding suitable ethylenediamine, water using ultrasonic cell
Broken instrument carries out ultrasonic treatment 15min, setpoint frequency 20kHz, power 900w to it.Ice water is placed the beaker after ultrasonic treatment
In mixture, rotor is added after its cooling, suitable silica solution and H2PtCl4 solution are successively added dropwise under stirring.Drop
After adding, jar agitation is heated to 90 DEG C and keeps 30min to form amantadine: silicon source: noble metal source: ethylenediamine:
Water molar ratio is the Synthesis liquid of 47:100:10:400:11240.
(2) by DD3R sieve particle well prepared in advance after ball milling (partial size 300nm) according to mass ratio be 0.5%
Mass ratio be added in Synthesis liquid, and Synthesis liquid is placed in microwave reaction kettle, and stir hydrothermal synthesis under microwave condition
For 72h to guarantee that the silicon source in Synthesis liquid is utilized entirely, synthesis temperature is 160 DEG C.
(3) after hydrothermal synthesis, the Synthesis liquid in microwave reaction kettle is subjected to eccentric cleaning, drying obtains solid material
Material, will reunite makes its dispersion with solid particle grinding together.
(4) solid material of drying roasts 3-4h under ozone environment to prepare required purifying formaldehyde material
D3, set temperature are 300 DEG C.
Documents 4
(1) amantadine is broken into graininess to be put into beaker, and is broken after adding suitable ethylenediamine, water using ultrasonic cell
Broken instrument carries out ultrasonic treatment 15min, setpoint frequency 20kHz, power 900w to it.Ice water is placed the beaker after ultrasonic treatment
In mixture, rotor is added after its cooling, suitable silica solution and H2PtCl4 solution are successively added dropwise under stirring.Drop
After adding, jar agitation is heated to 90 DEG C and keeps 30min to form amantadine: silicon source: noble metal source: ethylenediamine:
Water molar ratio is the Synthesis liquid of 47:100:10:400:11240.
(2) by DD3R sieve particle well prepared in advance after ball milling (partial size 300nm) according to mass ratio be 0.5%
Mass ratio be added in Synthesis liquid, and Synthesis liquid is placed in common response kettle, and stir under baking oven hydrothermal synthesis 72h with
Guarantee that the silicon source in Synthesis liquid is utilized entirely, synthesis temperature is 160 DEG C.
(3) after hydrothermal synthesis, the Synthesis liquid in microwave reaction kettle is poured into container for evaporation, makes to synthesize at high temperature
Moisture is evaporated and dries in liquid, and will reunite makes its dispersion with solid particle grinding together.
(4) solid material of drying roasts 3-4h under ozone environment to prepare required purifying formaldehyde material
D4, set temperature are 300 DEG C.
Comparative example 5
(1) amantadine is broken into graininess to be put into beaker, and is broken after adding suitable ethylenediamine, water using ultrasonic cell
Broken instrument carries out ultrasonic treatment 15min, setpoint frequency 20kHz, power 900w to it.Ice water is placed the beaker after ultrasonic treatment
In mixture, rotor is added after its cooling, suitable silica solution and H2PtCl4 solution are successively added dropwise under stirring.Drop
After adding, jar agitation is heated to 90 DEG C and keeps 30min to form amantadine: silicon source: noble metal source: ethylenediamine:
Water molar ratio is the Synthesis liquid of 47:100:10:400:11240.
(2) by DD3R sieve particle well prepared in advance after ball milling (partial size 300nm) according to mass ratio be 0.5%
Mass ratio be added in Synthesis liquid, and Synthesis liquid is placed in microwave reaction kettle, and stir hydrothermal synthesis under microwave condition
For 72h to guarantee that the silicon source in Synthesis liquid is utilized entirely, synthesis temperature is 160 DEG C.
(3) after hydrothermal synthesis, the Synthesis liquid in microwave reaction kettle is poured into container for evaporation, makes to synthesize at high temperature
Moisture is evaporated and dries in liquid, and will reunite makes its dispersion with solid particle grinding together.
(4) solid material of drying roasts 3-4h under common hot environment to prepare required purifying formaldehyde material
Expect D5, set temperature is 700 DEG C.
Contrast test
Scavenging material prepared by 500mg above-described embodiment and comparative example 1-3 is taken respectively, is placed in tubular fixed-bed reactor
It is tested, will be protected at room temperature, composite pollution gas (40% formaldehyde, 20% toluene, 20% dimethylbenzene and 20% acetone) bubbling,
Reaction system is blown by nitrogen, control Reactor inlet concentration of formaldehyde is 50mg/m3, and reaction velocity (GHSV) is 30000mlg-
1h-1, Activity evaluation are as shown in table 1.
1 scavenging material evaluation result of table
As shown in Table 1, in the exhaust gas containing multiple pollutant, scavenging material PARA FORMALDEHYDE PRILLS(91,95) provided by the present invention it is net
Change ability is best.
It the foregoing is merely embodiments of the present invention are illustrated, is not intended to restrict the invention, for the technology of this field
For personnel, all within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on be should be included in
Within protection scope of the present invention.
Claims (7)
1. a kind of purifying formaldehyde material, it is characterised in that it is made of DD3R molecular sieve and noble metal active component, with catalyst
Type 100% calculate, the mass fraction of molecular sieve is 90-95%, and the mass fraction of noble metal active component is 5-10%；It is described
The preparation method of purifying formaldehyde material the following steps are included:
(1) water, amantadine and cosolvent are mixed, handling through high frequency ultrasound is completely dissolved amantadine, and stirs in ice bath
The salting liquid of silicon source and noble metal is added dropwise under the conditions of mixing, then is aged to form amantadine through high-temperature stirring: silicon source: noble metal source:
Cosolvent: water molar ratio is the Synthesis liquid of 30-50:100:5-20:100-500:5000-50000；
(2) crystal seed well prepared in advance is added in Synthesis liquid according to the mass ratio that mass ratio is 0.2-2%, and by Synthesis liquid
It is placed in microwave reaction kettle, and stirs hydrothermal synthesis 48-72h under microwave condition, synthesis temperature is 150-180 DEG C；
(3) after hydrothermal synthesis, the Synthesis liquid in microwave reaction kettle is poured into container for evaporation and is evaporated moisture in Synthesis liquid
And solid material is dried；
(4) solid material of drying roasts 3-4h under ozone environment to prepare required purifying formaldehyde material.
2. material according to claim 1, it is characterised in that the maturing temperature is 300-400 DEG C.
3. material according to claim 1, it is characterised in that the noble metal be one of Pt, Pd, Au and Ag or
It is a variety of.
4. material according to claim 1, it is characterised in that the cosolvent is ethylenediamine.
5. material according to claim 1, it is characterised in that the crystal seed is in sigma-1, DD3R and ZSM-58
It is a kind of.
6. material according to claim 1, it is characterised in that grind the solid material of drying before roasting.
7. material according to claim 1, it is characterised in that by the frequency of the high frequency ultrasound be 20-25kHz, power
For 500-1800w.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811643222.XA CN109603896B (en) | 2018-12-29 | 2018-12-29 | Formaldehyde purification material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811643222.XA CN109603896B (en) | 2018-12-29 | 2018-12-29 | Formaldehyde purification material |
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| Publication Number | Publication Date |
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| CN109603896A true CN109603896A (en) | 2019-04-12 |
| CN109603896B CN109603896B (en) | 2020-10-20 |
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| CN201811643222.XA Expired - Fee Related CN109603896B (en) | 2018-12-29 | 2018-12-29 | Formaldehyde purification material |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786065A (en) * | 2012-08-21 | 2012-11-21 | 浙江师范大学 | Method for preparing full-silicon DD3R zeolite molecular sieve with pure phase and uniform crystal morphology and size |
| CN103127952A (en) * | 2011-12-01 | 2013-06-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Supported nano-silver catalyst capable of eliminating formaldehyde at room temperature and preparation method thereof |
| CN104925826A (en) * | 2015-06-02 | 2015-09-23 | 中国科学院上海高等研究院 | Method for preparing DD3R molecular sieve |
| CN105668578A (en) * | 2016-04-13 | 2016-06-15 | 中国科学院上海高等研究院 | Method for quickly synthesizing DD3R molecular sieve |
| CN106540741A (en) * | 2016-10-19 | 2017-03-29 | 浙江大学 | It is used at room temperature eliminating catalyst of formaldehyde and preparation method thereof |
| CN107715831A (en) * | 2017-11-13 | 2018-02-23 | 刘庆玉 | One kind is used to remove CO in admixture of gas2Adsorbent and preparation method thereof |
| CN108246351A (en) * | 2018-02-11 | 2018-07-06 | 浙江大学 | For the total silicon ZSM-5 molecular sieve catalyst and preparation method of room temperature purifying formaldehyde |
| CN108421559A (en) * | 2018-02-11 | 2018-08-21 | 浙江大学 | Total silicon Beta molecular sieve catalysts and preparation method for room temperature purifying formaldehyde |
-
2018
- 2018-12-29 CN CN201811643222.XA patent/CN109603896B/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103127952A (en) * | 2011-12-01 | 2013-06-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Supported nano-silver catalyst capable of eliminating formaldehyde at room temperature and preparation method thereof |
| CN102786065A (en) * | 2012-08-21 | 2012-11-21 | 浙江师范大学 | Method for preparing full-silicon DD3R zeolite molecular sieve with pure phase and uniform crystal morphology and size |
| CN104925826A (en) * | 2015-06-02 | 2015-09-23 | 中国科学院上海高等研究院 | Method for preparing DD3R molecular sieve |
| CN105668578A (en) * | 2016-04-13 | 2016-06-15 | 中国科学院上海高等研究院 | Method for quickly synthesizing DD3R molecular sieve |
| CN106540741A (en) * | 2016-10-19 | 2017-03-29 | 浙江大学 | It is used at room temperature eliminating catalyst of formaldehyde and preparation method thereof |
| CN107715831A (en) * | 2017-11-13 | 2018-02-23 | 刘庆玉 | One kind is used to remove CO in admixture of gas2Adsorbent and preparation method thereof |
| CN108246351A (en) * | 2018-02-11 | 2018-07-06 | 浙江大学 | For the total silicon ZSM-5 molecular sieve catalyst and preparation method of room temperature purifying formaldehyde |
| CN108421559A (en) * | 2018-02-11 | 2018-08-21 | 浙江大学 | Total silicon Beta molecular sieve catalysts and preparation method for room temperature purifying formaldehyde |
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