CN108862311A - A kind of preparation method of the high silica ZSM-5 molecular sieve for VOCs degradation - Google Patents
A kind of preparation method of the high silica ZSM-5 molecular sieve for VOCs degradation Download PDFInfo
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- CN108862311A CN108862311A CN201811006951.4A CN201811006951A CN108862311A CN 108862311 A CN108862311 A CN 108862311A CN 201811006951 A CN201811006951 A CN 201811006951A CN 108862311 A CN108862311 A CN 108862311A
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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
- B01D53/02—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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- 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
- 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
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline 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
- C01B39/36—Pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11
- C01B39/38—Type ZSM-5
- C01B39/40—Type ZSM-5 using at least one organic template directing agent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The present invention relates to a kind of preparation methods of high silica ZSM-5 molecular sieve for VOCs degradation, including：（1）Silicon source, alkali source, template, ZSM-5 molecular sieve crystal seed are mixed with water, form gel；（2）By step（1）Described in gel be placed in reaction kettle in carrying out hydro-thermal process, after reaction, be separated by solid-liquid separation, washed, being dried, roasted and obtain molecular screen primary powder；（3）By step（2）Ion exchange is carried out in gained molecular screen primary powder merging ammonium salt solution, to obtain ammonium type ZSM-5 molecular sieve, then roasting obtains HZSM-5 molecular sieve.High silica ZSM-5 molecular sieve produced by the present invention is applied to have the characteristics that large amount of adsorption, hydrophobic performance are strong, easily regenerate in VOCs degradation.
Description
Technical field
The present invention relates to Zeolite synthesis method and technology fields, and in particular to a kind of high silica ZSM-5 for VOCs degradation
The preparation method of molecular sieve.
Background technique
Volatility machine object (VOCs) refers to organic compound of the saturated vapour pressure greater than 0.13 kPa at standard conditions, packet
It includes hydrocarbon, aldehyde, ketone, alcohol, ether, ester, hetero atom and replaces 300 gas chromatographies such as hydrocarbon.VOCs is with many kinds of, source is wide in atmosphere
General, the features such as toxicity is big, concentration is relatively low but the total amount of pollutant is big.Absorption method is one of main VOCs purification method, with
Other methods are compared, and absorption method has many advantages, such as that technical maturity, easy to operate, low energy consumption, purification efficiency is high, are suitable for low dense
The VOCs purification of degree, high air quantity, but there is also adsorption efficiencies under high-temperature low, VOCs under high humility absorption is suppressed etc. and to lack
Point.Therefore, more efficient adsorbent is developed, overcomes the influence of high temperature, high humidity to absorption, and find more inexpensive adsorbent
Regeneration method, this by be adsorption method for purifying VOCs research direction.
Zeolite molecular sieve is excellent one of adsorbent, be widely used in basic organic chemical industry, petrochemical industry production on,
In the improvement of pernicious gas, it is also commonly used for SO2、NOx、CO、CO2, NH3, CCl4, vapor and gaseous state hydrocarbon exhaust it is net
Change.Mainly since it has the characteristics that：1, molecular sieve adsorptive selectivity is strong.This is because the pore size of molecular sieve is neat
It is uniform, and be a kind of ionic adsorbent, therefore, it can be according to bulk of molecule and polar different progress selective absorptions；
2, molecular sieve adsorption ability is strong.Even if the composition concentration of gas is very low, still there is biggish adsorption capacity.3, in higher temperature
Still there is biggish adsorption capacity under degree, and other adsorbents are influenced by temperature very greatly, thus under the conditions of identical temperature, point
The adsorption capacity of son sieve is big.
With the continuous deepening of research, zeolite runner concentration technique is to administer and grow up for low concentration VOCs at present
A kind of new technology, be combined with chemical method, form zeolite runner concentration+incineration technology.Entire zeolite runner absorption is dense
In contracting technology, the hydrophobic shape zeolite molecular sieve for Adsorption Concentration is the core of its technology, and zeolite molecular sieve is inhaled as hydrophobicity
The advantage of enclosure material is more and more obvious, and is had multinomial patent both at home and abroad at present and is related to be used for using zeolite molecular sieve as adsorbent
Handle VOCs report, mainly have US6281406B1, US4705909, CN1781885A, CN11055906A,
CN1280977A, CN1749226A, CN201710375783 etc., when synthesized molecular sieve is as adsorbent in above-mentioned patent,
There is following major defects：One, molecular sieve as adsorbent when need to add some inorganic or organic material as bonding
Agent use, this resulted in product synthesis step it is cumbersome and in the process also need add poisonous and harmful substance, be unfavorable for industrial life
It produces；Two, template used in Zeolite synthesis is expensive, and subsequent processing work is many and diverse, and adsorbent cost is caused to occupy height not
Under；Three, molecular sieve is exactly regeneration issues as the maximum difficult point of adsorbent, does not refer to this problem in above-mentioned patent.To sum up come
It sees, urgent need develops that a kind of simple process, adsorption effect be good, low-cost zeolite molecular sieve meets day as adsorbent
The demand for the VOC treatment process opened up increasingly.
Summary of the invention
It is an object of the invention in view of the shortcomings of the prior art, develop a kind of technique letter for being suitable for VOCs degradation
Single, good, the low-cost high silica ZSM-5 zeolite molecular sieve of absorption property preparation method.
In order to realize that the purpose of foregoing invention, the present invention are realized using following scheme：
A kind of preparation method of the high silica ZSM-5 molecular sieve for VOCs degradation, it is characterised in that：Include the following steps：
（1）Silicon source, alkali source, template, ZSM-5 molecular sieve crystal seed are mixed with water, form gel；
（2）By step（1）Middle gained gel, which is placed in reaction kettle, carries out hydro-thermal process, after reaction, successively carries out solid-liquid point
Molecular screen primary powder is obtained from, washing, dry, roasting；
（3）By step（2）Ion exchange is carried out in middle gained molecular screen primary powder merging ammonium salt solution, to obtain ammonium type ZSM-5 points
Son sieve, then roasting obtains HZSM-5 molecular sieve.
Further, the step（1）Middle silicon source selects solid silicone, silica solution, waterglass, white carbon black, diatomite, silicon
One of hydrochlorate and ethyl orthosilicate are a variety of；
Further, the step（1）Middle alkali source selects one of sodium hydroxide and potassium hydroxide or a variety of；
Further, the step（1）Middle template select methylamine, diethylamine, tetraethylammonium bromide, tetraethyl ammonium hydroxide,
4-propyl bromide, tetrapropylammonium hydroxide, 1,6- hexamethylene diamine, n-butylamine, cetyl trimethylammonium bromide（CTAB）In
It is one or more.
Further, the step（1）In ZSM-5 molecular sieve crystal seed select it is commercially available or self-control ZSM-5 molecular sieve crystal seed.
Further, the step（1）In silicon source, alkali source, template, water in terms of its oxide, each component molar ratio
For SiO2：Na2O：Template：H2O=1：0.05-0.20：0.05-0.30：15-40；The step（1）Middle molecular sieve seed and silicon
SiO in source2The mass ratio of component is 1:0.02-0.08.
Further, the step（2）Middle hydro-thermal process temperature is 150-1800 DEG C, hydrothermal conditions 24-48h.
Further, in the step（2）With（3）Between it is further comprising the steps of：By step（2）Gained molecular screen primary powder
Carrying out step（3）Ion-exchange treatment before using acid solution carry out acidleach processing, then roasting obtain molecular sieve precursor；
In acidleach treatment process, the concentration of the acid solution is 0.5-2mol/L, and the acid solution is selected from hydrochloric acid, nitric acid, sulfuric acid and phosphorus
One of acid is a variety of；Acidleach processing consolidates mass ratio 2-18 in liquid:1, temperature carries out under the conditions of being 60-90 DEG C.
Further, the step（3）Intermediate ion give-and-take conditions are：By the step（2）Middle gained molecular screen primary powder is set
1-4h is stirred in the ammonium salt solution of 0.5 ~ 2 mol/L, products therefrom and ammonium salt solution mass ratio are 10-20 after dry crystallization：
1, under the conditions of 60 ~ 95 DEG C of exchange temperature, repeat ion exchange process 1 ~ 3 time；The ammonium salt solution selects ammonium sulfate, chlorine
Change one of ammonium or ammonium nitrate solution.
Further, the step（2）In, drying temperature is 120 DEG C, drying time 12h；The step（2）With（3）
In, maturing temperature is 500-550 DEG C, calcining time 6-12 hours.
The ZSM-5 molecular sieve that preparation method of the present invention is prepared is applied in the degradation of VOCs, with the prior art
It compares, the present invention has the following technical effects：
1）Synthesis technology simple possible, raw materials used cheap, process is added without any noxious material, and product cost is low, ring
Packing pressure is small.
2）Zeolite synthesis is carried out using crystal seed revulsion new technology, it is low not only to have reduced template dosage, but also improve life
Efficiency is produced, synthesized product has small partial size, large specific surface area, good hydrophobic performance and powerful VOCs absorption property.
3）Zeolite product hydrothermal stability with higher prepared by the present invention and good regenerability.
4）The ZSM-5 molecular sieve of the method for the present invention preparation is mainly used in VOCs degradation aspect, there is good adsorptivity
Energy and regenerability.
Detailed description of the invention
The XRD spectrum for the high silica ZSM-5 sieve sample that Fig. 1 is embodiment 1-5 and prepared by comparative example；
Fig. 2 is the SEM spectrum of high silica ZSM-5 sieve sample prepared by embodiment 1.
Specific embodiment
Invention is further explained combined with specific embodiments below, but the present invention is not limited to following embodiments.
It is raw materials used in embodiment to be described below：
The preparation method for making ZSM-5 molecular sieve crystal seed by oneself is as follows：By 3.0 g sodium hydroxides, 70g silica solution, be dissolved in 120 g go from
In sub- water, gel is fitted into crystallizing kettle by 11gTPAOH after mixing evenly, 24 h of crystallization at 160 DEG C, and the product after crystallization is washed
It washs to pH=8,100 DEG C of 12 h of drying, obtains self-control ZSM-5 molecular sieve crystal seed.
Embodiment 1
By silicon source（Select 30% silica solution）, alkali source（Select NaOH）, template（Select 4-propyl bromide）, according to
SiO2：NaOH：TPABr：H2O =200：25：10：3000 molar ratio is prepared by mixing into gel, addition self-control ZSM-5 molecule
Sieve crystal seed is placed in crystallizing kettle, makes ZSM-5 molecular sieve crystal seed and SiO by oneself2Mass ratio is 1:100, the crystallization 48h at 160 DEG C, it is brilliant
The high silicon of the preparation of embodiment 1 is obtained after acid exchange and Ammonium Salt Ionic exchange after separating, washing, drying, roast after the completion of changing
ZSM-5 sieve sample A.
Embodiment 2
By silicon source（Select 30% silica solution）, alkali source（Select NaOH）, template（Select 4-propyl bromide）, according to SiO2：
NaOH：TPABr：H2O =200：25：10：3000 molar ratio is prepared by mixing into gel, and it is brilliant to add commercially available ZSM-5 molecular sieve
Kind is placed in crystallizing kettle, commercially available ZSM-5 molecular sieve crystal seed and SiO2Mass ratio is 1:100, crystallization 48h, crystallization are complete at 160 DEG C
The high silica ZSM-5 of the preparation of embodiment 2 is obtained after acid exchange and Ammonium Salt Ionic exchange after separating, washing, drying, roast after
Sieve sample B.
Embodiment 3
By silicon source（Select 30% silica solution）, alkali source（Select NaOH）, template（Select 4-propyl bromide）, according to SiO2：
NaOH：TPABr：H2O =200：25：10：3000 molar ratio is prepared by mixing into gel, and it is brilliant to add commercially available ZSM-5 molecular sieve
Kind is placed in crystallizing kettle, commercially available ZSM-5 molecular sieve crystal seed and SiO2Mass ratio is 3:100, crystallization 48h, crystallization are complete at 160 DEG C
The high silica ZSM-5 of the preparation of embodiment 3 is obtained after acid exchange and Ammonium Salt Ionic exchange after separating, washing, drying, roast after
Sieve sample C.
Embodiment 4
By silicon source（Select 30% silica solution）, alkali source（Select NaOH）, template（Select 4-propyl bromide）, according to SiO2：
NaOH：TPABr：H2O =200：25：10：3000 molar ratio is prepared by mixing into gel, and it is brilliant to add commercially available ZSM-5 molecular sieve
Kind is placed in crystallizing kettle, commercially available ZSM-5 molecular sieve crystal seed and SiO2Mass ratio is 5:100, crystallization 48h, crystallization are complete at 160 DEG C
The high silica ZSM-5 of the preparation of embodiment 4 is obtained after acid exchange and Ammonium Salt Ionic exchange after separating, washing, drying, roast after
Sieve sample D.
Embodiment 5
By silicon source（Select 30% silica solution）, alkali source（Select NaOH）, template（Select 4-propyl bromide）, according to SiO2：
NaOH：TPABr：H2O =200：25：10：3000 molar ratio is prepared by mixing into gel, and it is brilliant to add commercially available ZSM-5 molecular sieve
Kind is placed in crystallizing kettle, commercially available ZSM-5 molecular sieve crystal seed and SiO2Mass ratio is 8:100, crystallization 48h, crystallization are complete at 160 DEG C
The high silica ZSM-5 of the preparation of embodiment 5 is obtained after acid exchange and Ammonium Salt Ionic exchange after separating, washing, drying, roast after
Sieve sample E.
Comparative example
Select the F reference as a comparison sample of the commercially available high silica ZSM-5 molecular sieve of Uop Inc..Sieve sample A, B of implementation 1-5,
C, the XRD diagram of D, E and the sieve sample F of comparative example are shown in attached drawing 1.
The test of molecular sieve absorption property
Referring to standard GB/T 6287-1986《Molecular sieve Static Water determining adsorption method》Testing example 1-5 and comparison respectively
The hydrophobic performance of high silica ZSM-5 sieve sample prepared by example, while several frequently seen organic matter is chosen as the source VOCs
Sample is tested, and is compared by embodiment and comparative example, and experimental result is as shown in table 1.
The absorption property of high silica ZSM-5 sieve sample prepared by one embodiment 1-5 of table and comparative example tests table
Data are that high silica ZSM-5 sieve sample adsorbs high silica ZSM-5 sieve sample quality shared by homologue kind quality in table
Percentage, as can be seen from the data in table 1,（1）Compared with comparative example gained sample F, the high silicon of preparation method acquisition of the invention
ZSM-5 molecular sieve sample is weaker than the sample of comparative example acquisition to the suction-operated of water, illustrates preparation method preparation of the invention
High silica ZSM-5 molecular sieve has stronger hydrophobicity；（2）The high silica ZSM-5 molecular sieve of preparation method preparation of the invention is to each
The adsorbance of kind VOCs molecule is above the sample of comparative example acquisition.
Finally it should be noted that：Above embodiments are only to illustrate the present invention and not limit technology described in the invention
Scheme, therefore, although this specification is referring to above-mentioned each embodiment, the present invention has been described in detail, this
Field it is to be appreciated by one skilled in the art that still can modify to the present invention or equivalent replacement, and all do not depart from this
The technical solution and its improvement of the spirit and scope of invention, should all cover within the scope of the claims of the present invention.
Claims (10)
1. a kind of preparation method of the high silica ZSM-5 molecular sieve for VOCs degradation, it is characterised in that：Include the following steps：
（1）Silicon source, alkali source, template, ZSM-5 molecular sieve crystal seed are mixed with water, form gel；
（2）By step（1）Middle gained gel, which is placed in reaction kettle, carries out hydro-thermal process, after reaction, successively carries out solid-liquid point
Molecular screen primary powder is obtained from, washing, dry, roasting；
（3）By step（2）Ion exchange is carried out in middle gained molecular screen primary powder merging ammonium salt solution, to obtain ammonium type ZSM-5 points
Son sieve, then roasting obtains HZSM-5 molecular sieve.
2. a kind of preparation method of high silica ZSM-5 molecular sieve for VOCs degradation according to claim 1, feature exist
In：The step（1）Middle silicon source selects solid silicone, silica solution, waterglass, white carbon black, diatomite, silicate and positive silicic acid second
One of ester is a variety of.
3. a kind of preparation method of high silica ZSM-5 molecular sieve for VOCs degradation according to claim 1, feature exist
In：The step（1）Middle alkali source selects one of sodium hydroxide and potassium hydroxide or a variety of.
4. a kind of preparation method of high silica ZSM-5 molecular sieve for VOCs degradation according to claim 1, feature exist
In：The step（1）Middle template selects methylamine, diethylamine, tetraethylammonium bromide, tetraethyl ammonium hydroxide, tetrapropyl bromination
Ammonium, tetrapropylammonium hydroxide, 1,6- hexamethylene diamine, n-butylamine, cetyl trimethylammonium bromide（CTAB）One of or it is a variety of.
5. a kind of preparation method of high silica ZSM-5 molecular sieve for VOCs degradation according to claim 1, feature exist
In：The step（1）In ZSM-5 molecular sieve crystal seed select it is commercially available or self-control ZSM-5 molecular sieve crystal seed.
6. a kind of preparation method of high silica ZSM-5 molecular sieve for VOCs degradation according to claim 1, feature exist
In：The step（1）In silicon source, alkali source, template, water in terms of its oxide, each component molar ratio be SiO2：Na2O：Template
Agent：H2O=1：0.05-0.20：0.05-0.30：15-40；The step（1）SiO in middle molecular sieve seed and silicon source2The matter of component
Amount is than being 1:0.02-0.08.
7. a kind of preparation method of high silica ZSM-5 molecular sieve for VOCs degradation according to claim 1, feature exist
In：The step（2）Middle hydro-thermal process temperature is 150-1800 DEG C, hydrothermal conditions 24-48h.
8. a kind of preparation method of high silica ZSM-5 molecular sieve for VOCs degradation according to claim 1, feature exist
In：In the step（2）With（3）Between it is further comprising the steps of：By step（2）Gained molecular screen primary powder is carrying out step（3）
Ion-exchange treatment before using acid solution carry out acidleach processing, then roasting obtain molecular sieve precursor；Acidleach treatment process
In, the concentration of the acid solution is 0.5-2mol/L, the acid solution be selected from one of hydrochloric acid, nitric acid, sulfuric acid and phosphoric acid or
It is a variety of；Acidleach processing consolidates mass ratio 2-18 in liquid:1, temperature carries out under the conditions of being 60-90 DEG C.
9. a kind of preparation method of high silica ZSM-5 molecular sieve for VOCs degradation according to claim 1, feature exist
In：The step（3）Intermediate ion give-and-take conditions are：By the step（2）Middle gained molecular screen primary powder is placed in 0.5 ~ 2 mol/L's
1-4h is stirred in ammonium salt solution, products therefrom and ammonium salt solution mass ratio are 10-20 after dry crystallization：1, in 60 ~ 95 DEG C of friendship
It changes under the conditions of temperature, repeats ion exchange process 1 ~ 3 time；The ammonium salt solution selects ammonium sulfate, ammonium chloride or ammonium nitrate solution
One of.
10. a kind of preparation method of high silica ZSM-5 molecular sieve for VOCs degradation according to claim 1, feature
It is：The step（2）In, drying temperature is 120 DEG C, drying time 12h；The step（2）With（3）In, maturing temperature is
500-550 DEG C, calcining time 6-12 hours.
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| CN110339809A (en) * | 2019-08-13 | 2019-10-18 | 淄博齐创化工科技开发有限公司 | A kind of adsorbent and preparation method for VOCs absorption |
| CN110496595A (en) * | 2019-09-11 | 2019-11-26 | 江苏国瓷天诺新材料科技股份有限公司 | A kind of preparation method of the class solid phase VOCs that crystallite dimension is controllable degradation high silica ZSM-5 molecular sieve |
| CN110787767A (en) * | 2019-08-15 | 2020-02-14 | 北京科技大学 | Hydrophobic adsorbent and preparation method thereof |
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| CN110787767A (en) * | 2019-08-15 | 2020-02-14 | 北京科技大学 | Hydrophobic adsorbent and preparation method thereof |
| CN110787767B (en) * | 2019-08-15 | 2021-03-23 | 北京科技大学 | Hydrophobic adsorbent and preparation method thereof |
| CN110496595A (en) * | 2019-09-11 | 2019-11-26 | 江苏国瓷天诺新材料科技股份有限公司 | A kind of preparation method of the class solid phase VOCs that crystallite dimension is controllable degradation high silica ZSM-5 molecular sieve |
| CN111203175A (en) * | 2020-02-26 | 2020-05-29 | 北京泷涛环境科技有限公司 | Honeycomb hydrophobic molecular sieve adsorbent and preparation method and application thereof |
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