CN106512925A - Hydrophobic zeolite as well as preparation method and application thereof - Google Patents
Hydrophobic zeolite as well as preparation method and application thereof Download PDFInfo
- Publication number
- CN106512925A CN106512925A CN201610964644.1A CN201610964644A CN106512925A CN 106512925 A CN106512925 A CN 106512925A CN 201610964644 A CN201610964644 A CN 201610964644A CN 106512925 A CN106512925 A CN 106512925A
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- zeolite
- hydrophobic
- preparation
- acidleach
- hydrophobic zeolite
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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
- B01J20/165—Natural alumino-silicates, e.g. zeolites
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
Abstract
The invention relates to synthesis of a hydrophobic zeolite, and in particular to the hydrophobic zeolite as well as a preparation method and application thereof. The preparation method of the hydrophobic zeolite comprises the following steps: firstly performing acid leaching treatment on natural clinoptilolite to obtain acid leached zeolite, and then performing heat treatment on the acid leached zeolite to obtain the hydrophobic zeolite. The preparation method of hydrophobic zeolite provided by the invention has the advantages of improves the silica-alumina ratio of the zeolite and enhancing surface hydrophobicity of the zeolite through performing the acid leaching treatment on the cheap natural clinoptilolite, and reducing silanol group content on the surface of the zeolite and further improving the surface hydrophobicity of the zeolite through performing the heat treatment on the acid leached zeolite. The zeolite prepared by the method provided by the invention is higher in hydrophobicity, is low in price, and is expected to be practical application in the fields of hydrophobic pollutant treatment and the like.
Description
【Technical field】
The present invention relates to the synthesis of hydrophobic zeolite, and in particular to a kind of hydrophobic zeolite and its preparation method and application.
【Background technology】
In recent years, hydrophobicity silica-rich zeolite is received as a kind of new adsorbent and is increasingly paid close attention to, in its structure
Aluminium content is very low, cation exchange capacity very little, and skeleton is presented neutral, lack in structure in strong Electrostatic Absorption heart-yang from
Son, primary attachment are worked by the lattice micropore surface that Si-O-Si is constituted, and show stronger hydrophobicity.Numerous studies are
Confirm, silica-rich zeolite is in high humidity environment or water to organic pollution such as trichloro ethylene, methyl tertiary butyl ether(MTBE), Polyethylene Glycol, double
Phenol A etc. is respectively provided with preferable adsorption effect, and wherein Y-zeolite hydrophobic zeolites are even above activity to the adsorption capacity of bisphenol-A
Charcoal.Silica-rich zeolite can be directly synthesized by hydro-thermal, and steam, acid, chelating agen, tetrachloro silicane and hexa-fluoride etc. are taken off to zeolite
The modes such as aluminum process are obtained, and wherein acidleach is processed because efficiently and becoming the current method for generally adopting the advantages of process is simple.
Although using the acidleach such as hydrochloric acid, oxalic acid, nitric acid process effectively can remove it is zeolite structured in aluminium element, improve zeolite
Silica alumina ratio, strengthen its surface hydrophobic, however, 1) Jing acidleach dealuminzation can leave room in the structure of zeolite, cause zeolite
Degree of crystallinity reduce, structural stability reduce；When dealuminzation is more than 50%, the structure of zeolite can occur destruction.2) acidleach dealuminzation
Raising of the zeolite afterwards with Si/Al ratio, its surface Bronsted and Lewis acid position and exchangeable cations etc. hydrophilic radical are big
It is big to reduce, but the silanol base that its surface is present causes zeolite surface still to keep higher hydrophilic.
【The content of the invention】
To solve problems of the prior art, it is an object of the invention to provide a kind of hydrophobic zeolite and its preparation side
Method and application, have higher structural stability and hydrophobicity, low cost by zeolite prepared by the method.
The technical scheme is that what is be achieved in that：
A kind of preparation method of hydrophobic zeolite, comprises the steps：
Acidleach process is carried out to natural clinoptilolite first, is improved the silica alumina ratio of zeolite, is obtained acidleach zeolite, then to acidleach
Zeolite carries out heat treatment reduces the silanol base content of acidleach zeolite surface, obtains hydrophobic zeolite.
The heat treatment is roasting heat treatment.
In the roasting process, sintering temperature is 400-1000 DEG C, and the time is 1-6h.
During the acidleach, natural clinoptilolite is immersed in inorganic acid solution of the concentration for 0.1-4mol/L carries out acid
Leaching.
Described leaching time is 6-24h.
After the natural clinoptilolite carries out acidleach process, then to zeolite by washing, being dried to obtain acidleach zeolite.
During the acidleach, material is constantly stirred.
The silica alumina ratio of the acidleach zeolite is 5.0-7.5.
A kind of hydrophobic zeolite, the hydrophobic zeolite are to be to the adsorbance of vapor under the conditions of 75% in relative humidity
6.5-29.7mg/g。
A kind of application of hydrophobic zeolite, hydrophobic zeolite are used to adsorb hydrophobic contaminant.
Compared with prior art, the present invention has the advantages that：The positive effect of the present invention is：The preparation of the present invention
The preparation method of hydrophobic zeolite by carrying out acidleach process to cheap natural clinoptilolite, improves the sial of zeolite first
Than and enhance its surface hydrophobic；Heat treatment is carried out to acidleach zeolite again, its structural stability is improve, zeolite table is reduced
The silanol base content in face simultaneously further increases its surface hydrophobic, and the hydrophobic zeolite prepared by the method for the present invention is had
Higher structural stability and hydrophobicity, and price is low, the field such as hydrophobic contaminant process has good practical application.
The hydrophobic zeolite of the present invention, is 6.5-29.7mg/g to the adsorbance of vapor, takes 1.0g hydrophobic zeolites, will
Sample is placed in the 500mL beakers containing 250mL sodium chloride saturated solutions, and 48h is placed under room temperature air-proof condition, takes out sample
Weighing, investigating the change of example weight, it is 6.5-29.7mg/g hydrophobic zeolite to be calculated to the adsorbance of vapor, significantly
Less than the 49.3mg/g of natural clinoptilolite, hydrophobicity increases.
【Description of the drawings】
Fig. 1 is the XRD spectrum of natural clinoptilolite (a), acidleach zeolite (b) and 600 DEG C of roastings zeolite (c).
【Specific embodiment】
Come that the present invention is described further with reference to the accompanying drawings and examples.
When hydrophobic zeolite is prepared using natural clinoptilolite, natural clinoptilolite is immersed concentration first is the present invention
Acidleach 6-24h in the inorganic acid solution of 0.1-4mol/L, mineral acid can adopt nitric acid, material constantly be entered during acidleach
Row stirring, acidleach improve the silica alumina ratio of zeolite, and before acidleach, the silica alumina ratio of zeolite is 3.6, and Jing after acidleach, the silica alumina ratio of zeolite is carried
It is high to arrive 5.0-7.5；
After the completion of acidleach is processed, then pass through washing to zeolite, be dried to obtain acidleach zeolite, then to acidleach zeolite in 400-
At 1000 DEG C, roasting 1-6h obtains hydrophobic zeolite, reduces the silanol base content of acidleach zeolite surface.
The hydrophobic zeolite prepared by the method for the present invention can be used in adsorbing hydrophobic contaminant, in relative humidity be
It is 6.5-29.7mg/g to the adsorbance of vapor under the conditions of 75%.
With reference to embodiment, the present invention is further illustrated.
Embodiment 1：
The preparation method of the hydrophobic zeolite of the present embodiment is carried out in accordance with the following steps：
Natural clinoptilolite is immersed into salpeter solution of the concentration for 0.1mol/L first, is processed under conditions of being stirred continuously
6h, then Jing washings, it is dried to obtain acidleach zeolite, the silica alumina ratio of acidleach zeolite is 5.0；Again by the roasting at 400 DEG C of acidleach zeolite
1h, obtains hydrophobic zeolite (XRD spectrum of sample is as shown in Figure 1).
1.0g hydrophobic zeolites are weighed, sample is placed in the 500mL beakers containing 250mL sodium chloride saturated solutions, in phase
It is 75% to humidity, under room temperature air-proof condition, places 48h, take out sample weighing, investigates the change of example weight, be computed
It is 29.7mg/g to the adsorbance of vapor to hydrophobic zeolite, less than the 49.3mg/g of natural clinoptilolite, hydrophobicity has been carried
It is high.
Embodiment 2～18, method are shown in Table 1 with embodiment 1, the condition and water vapor adsorption amount of each embodiment.
Table 1
Can draw with reference to above-described embodiment, Jing after inorganic acid solution process, silica alumina ratio is improved natural clinoptilolite, and with
The increase of acid concentration and the prolongation of leaching time, the silica alumina ratio of zeolite is continuously increased, its water vapor adsorption amount constantly drops therewith
It is low；And the zeolite after acidleach, again after fired process, its water vapor adsorption amount is further reduced, and with the rising of sintering temperature
With the prolongation of roasting time, its water vapor adsorption amount constantly reduces, can finally obtain with the zeolite adsorption material compared with high hydrophobicity
Material.
Claims (10)
1. a kind of preparation method of hydrophobic zeolite, it is characterised in that comprise the steps：
Acidleach process is carried out to natural clinoptilolite first, is improved the silica alumina ratio of zeolite, is obtained acidleach zeolite, then to acidleach zeolite
Carrying out heat treatment reduces the silanol base content of acidleach zeolite surface, obtains hydrophobic zeolite.
2. the preparation method of a kind of hydrophobic zeolite according to claim 1, it is characterised in that the heat treatment is roasting
Heat treatment.
3. the preparation method of a kind of hydrophobic zeolite according to claim 2, it is characterised in that in the roasting process,
Sintering temperature is 400-1000 DEG C, and the time is 1-6h.
4. the preparation method of a kind of hydrophobic zeolite according to claim 1, it is characterised in that during the acidleach,
Natural clinoptilolite is immersed in inorganic acid solution of the concentration for 0.1-4mol/L carries out acidleach.
5. the preparation method of a kind of hydrophobic zeolite according to claim 1, it is characterised in that described leaching time is
6-24h。
6. a kind of preparation method of hydrophobic zeolite according to claim 1, it is characterised in that the natural clinoptilolite
After carrying out acidleach process, then to zeolite by washing, being dried to obtain acidleach zeolite.
7. the preparation method of a kind of hydrophobic zeolite according to claim 1, it is characterised in that during the acidleach,
Material is constantly stirred.
8. a kind of preparation method of hydrophobic zeolite according to claim 1, it is characterised in that the silicon of the acidleach zeolite
Aluminum ratio is 5.0-7.5.
9. a kind of hydrophobic zeolite, it is characterised in that the hydrophobic zeolite is obtained by the preparation method of claim 1, institute
State hydrophobic zeolite in relative humidity to be under the conditions of 75% is 6.5-29.7mg/g to the adsorbance of vapor.
10. a kind of application of hydrophobic zeolite, it is characterised in that the hydrophobicity boiling prepared by the preparation method of claim 1
Stone is used to adsorb hydrophobic contaminant.
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| CN201610964644.1A CN106512925A (en) | 2016-10-28 | 2016-10-28 | Hydrophobic zeolite as well as preparation method and application thereof |
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| CN201610964644.1A CN106512925A (en) | 2016-10-28 | 2016-10-28 | Hydrophobic zeolite as well as preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108079939A (en) * | 2017-12-19 | 2018-05-29 | 陕西科技大学 | A kind of magnetism high-specific surface area silica-rich zeolite and its preparation method and application |
| CN109908627A (en) * | 2019-04-09 | 2019-06-21 | 陕西科技大学 | Micro-nano structure silica/zeolite prepares and based on the super hydrophilic underwater superoleophobic film of micro-nano structure silica/zeolite and preparation |
| CN114349020A (en) * | 2021-08-19 | 2022-04-15 | 复榆(张家港)新材料科技有限公司 | High-silicon mordenite and preparation method thereof |
| CN115724438A (en) * | 2022-10-20 | 2023-03-03 | 陕西科技大学 | High-hydrophobicity organic modified natural zeolite and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3551353A (en) * | 1968-10-04 | 1970-12-29 | Mobil Oil Corp | Dealuminzation of mordenite |
-
2016
- 2016-10-28 CN CN201610964644.1A patent/CN106512925A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3551353A (en) * | 1968-10-04 | 1970-12-29 | Mobil Oil Corp | Dealuminzation of mordenite |
Non-Patent Citations (2)
| Title |
|---|
| N. Y. CHEN等: "Hydrophobic Properties of Zeolites", 《THE JOURNAL OF PHYSICAL CHEMISTRY》 * |
| YASUTAKA KUWAHARA等: "TiO2 photocatalyst for degradation of organic compounds in water and air supported on highly hydrophobic FAU zeolite: Structural, sorptive, and photocatalytic studies", 《JOURNAL OF CATALYSIS》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108079939A (en) * | 2017-12-19 | 2018-05-29 | 陕西科技大学 | A kind of magnetism high-specific surface area silica-rich zeolite and its preparation method and application |
| CN108079939B (en) * | 2017-12-19 | 2021-01-08 | 陕西科技大学 | Magnetic high-specific surface area high-silicon zeolite and preparation method and application thereof |
| CN109908627A (en) * | 2019-04-09 | 2019-06-21 | 陕西科技大学 | Micro-nano structure silica/zeolite prepares and based on the super hydrophilic underwater superoleophobic film of micro-nano structure silica/zeolite and preparation |
| CN109908627B (en) * | 2019-04-09 | 2021-04-20 | 陕西科技大学 | Preparation of micro-nano structure silicon oxide/zeolite, super-hydrophilic underwater super-oleophobic film based on micro-nano structure silicon oxide/zeolite and preparation |
| CN114349020A (en) * | 2021-08-19 | 2022-04-15 | 复榆(张家港)新材料科技有限公司 | High-silicon mordenite and preparation method thereof |
| CN115724438A (en) * | 2022-10-20 | 2023-03-03 | 陕西科技大学 | High-hydrophobicity organic modified natural zeolite and preparation method thereof |
| CN115724438B (en) * | 2022-10-20 | 2024-03-22 | 陕西科技大学 | High-hydrophobicity organic modified natural zeolite and preparation method thereof |
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