CN106000290A - Silica gel hydrophobic modification method achieved under action of microwaves - Google Patents
Silica gel hydrophobic modification method achieved under action of microwaves Download PDFInfo
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- CN106000290A CN106000290A CN201610546200.6A CN201610546200A CN106000290A CN 106000290 A CN106000290 A CN 106000290A CN 201610546200 A CN201610546200 A CN 201610546200A CN 106000290 A CN106000290 A CN 106000290A
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- silica gel
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- silane modifier
- dewatering
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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
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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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
- B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
- B01J20/3206—Organic carriers, supports or substrates
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- Chemical & Material Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a silica gel hydrophobic modification method achieved under the action of microwaves. Common kiselgel a particles with the pore size of 5 nm to 8 nm are adopted as raw materials; silica gel impurity removal pretreatment is carried out firstly, and then n-heptane, ethyl alcohol and trimethylchlorosilane are prepared into a silane modifier according to a certain proportion; pretreated silica gel is immersed in the silane modifier, the microwave effect is used for assisting in silica gel modification, and emifinished lyophobic silica gel is obtained; finally, the semifinished lyophobic silica gel is washed with n-heptane to remove the residual silane modifier, then filtering, drying and the like are carried out till the weight of the semifinished lyophobic silica gel does not change any more, and finished lyophobic silica gel with good lyophobic effect and adsorption performance is obtained.
Description
Technical field
The invention belongs to field of new material preparation, be specifically related to the preparation method of a kind of dewatering silica gel.
Background technology
Silica gel is the polymer of silicon oxide compound composition, and the hydroxyl of about 5% is contained on its surface, easily with water molecules, and its absorption
Moisture up to the 50% of sole mass, use usually used as desiccant, and be difficult to adsorb apolar substance, thus be commonly used for
Process the gas that water capacity is higher, drying and dehydrating.Hydrophilic is a significant properties of silica gel, but the hydrophilic of silica gel is often
Its absorption property is produced impact, easily produces absorption competition impact so that it is the organic steam of absorption is replaced by hydrone, and
And after the hydrone of absorption excess, owing to expansive force will destroy the rigid structure of silica gel, produce broken.But the low flammability of silica gel
It is made to have obtained the attention of people as the adsorbent of VOCs.Develop for this and there is high adsorption capacity and the good oil gas of hydrophobicity
Reclaiming silica gel special, dewatering silica gel becomes domestic and international research emphasis.Dewatering silica gel is actually and carries out hydrophobic to common silica gel
Change processes so that the silicone hydroxyl of Silica Surface is replaced by hydrophobic group, is nonpolar from intrinsic polarity transformation, or in system
Add modifying agent during standby silica gel thus obtain dewatering silica gel.In Japan, dewatering silica gel is widely used in petroleum vapor recovery neck
Territory, as a kind of Novel adsorption agent material, reduces the heat of adsorption produced in adsorption process, eliminates the danger that spontaneous combustion occurs
Property.To the main heat treatment of method of the hydrophobic modification of silica gel, add modifying agent after again heat treatment, be impregnated with organic silicon compound etc.
Method is by hydroxyl therein removing or by hydrophobic group substituting modification, thus obtains adsorbing the more preferable adsorbent of Organic substance effect,
The material structure that wherein high-temperature heat treatment is modified is easily destroyed, and hydrophobic effect is inconspicuous.The present invention is thin with commercially available conventional absorbent paper
Hole aerosil particles is raw material, uses normal heptane to mix homogeneously by a certain percentage with ethanol, adds a certain amount of trim,ethylchlorosilane and join
Become silane modifier, silica gel particle dipping is wherein modified, then carries out microwave treatment, prepare a kind of cheap and hydrophobic
Effect and the more superior dewatering silica gel of absorption property.
Retrieved domestic and foreign databases according to the technology of the present invention feature, find about the report preparing dewatering silica gel with silica gel for raw material
The most with patent.Such as, Wang Yingxia et al. utilizes tartaric acid that silica gel is carried out hydrophobic modification, is thermally treated resulting in subsequently
A kind of dewatering silica gel；Chinese patent CN101108731 propose a kind of with surface modification auxiliary agent as containing alkyl, saturated or unsaturated
One or more methods carrying out modified silica-gel of the compounds such as carboxylic acid group；Chinese patent CN104558543A proposes one by directly
Trigger monomer polymerization preparation has the method for the high molecular polymer modified silica-gel of biocompatibility；Chinese patent
CN105170098A proposition is a kind of, and with acetic anhydride as esterifying agent, p-methyl benzenesulfonic acid is catalyst, and anhydrous acetic acid is solvent, profit
By microwave heating, the method carrying out microwave-ester modified silica-gel.But there is not yet with conventional absorbent paper Kiselgel A microgranule as raw material,
Utilize trim,ethylchlorosilane to combine microwave treatment while being modified, prepare hydrophobicity more preferably, more superior hydrophobic of absorption property
The report of silica gel.
Summary of the invention
For problem and shortage present in background technology, it is an object of the invention to the conventional absorbent paper so that aperture is 5～8nm thin
Hole silica gel (the most all representing with SG-0) microgranule is raw material, by it being processed and modified, and a kind of dewatering silica gel of preparation.
The technical scheme is that with SG-0 as raw material, first carry out silica gel pretreatment, then with normal heptane, ethanol and trimethyl
Chlorosilane is made into silane modifier according to a certain percentage, then pretreated silica gel is immersed in silane modifier and is aided with micro-
It is modified that ripple effect carries out silica gel, it is thus achieved that semi-finished product dewatering silica gel, finally by semi-finished product dewatering silica gel commercialization, obtains having good
Hydrophobic effect and the dewatering silica gel of absorption property.
The technical solution used in the present invention specifically includes following steps:
1. the pretreatment of silica gel: the SG-0 microgranule that aperture is 5～8nm is put into culture dish and is placed in vacuum drying oven, in temperature
Degree is 80～100 DEG C, vacuum is under 0.096～0.098MPa, is vacuum dried 2～4h.
2. silane modifier preparation: take normal heptane, ethanol and trim,ethylchlorosilane and mix in there-necked flask, wherein mixed proportion
1.0～2.0mL ethanol, 12～15mL normal heptane is added for every 1.0mL trim,ethylchlorosilane.
3. silica gel is modified: takes pretreated silica gel and adds in silane-modified agent solution and impregnate, and is aided with microwave and is modified,
Wherein dip time 8～12h, microwave power is 500～700W, and temperature is 50～80 DEG C, and the microwave action time is 10～30min,
Obtain semi-finished product dewatering silica gel.
4. prepared by dewatering silica gel commercialization: semi-finished product dewatering silica gel normal heptane cleans the silane modifier in remaining modified silica-gel,
Refilter, 3～5 times repeatedly, to remove the silane modifier in silica gel, then the silica gel after this filtration is put into there is evacuation merit
Can microwave oven be dried, be dried 2～3h under design temperature 60～80 DEG C, vacuum 0.085～0.09MPa, be adsorbed in remove
The normal heptane of Silica Surface, steam and microwave functionalization process again, make silica gel weight no longer change, and i.e. prepares and has well
Hydrophobic effect and the dewatering silica gel of absorption property.
It is an advantage of the current invention that:
(1) present invention utilizes cheap conventional absorbent paper Kiselgel A to be raw material, and raw material sources are extensive.
(2) present invention utilizes the method comparative maturity that trim,ethylchlorosilane is modified, simple to operate, it is not necessary to expensive instrument
Device, reagent.
(3) present invention utilizes microwave to be jointly modified silica gel with trim,ethylchlorosilane, and this effect is possible not only to heat modification
Temperature, it is also possible to be changed the situation of pore-size distribution, specific surface area and the surface functional group of silica gel, utilizes micro-especially twice
Wave heating and functionalization effect thereof, obtain the finished product dewatering silica gel with good hydrophobic effect and absorption property.
Accompanying drawing explanation
The common silica gel SG-0 of accompanying drawing 1, modified silica-gel SG-1 and modified silica-gel SG-2 pore-size distribution；
At 2 20 DEG C of accompanying drawing, common silica gel SG-0 and modified silica-gel SG-1, modified silica-gel SG-2 are to normal hexane, the suction of steam
Attached curve；
The circulation absorption normal hexane of accompanying drawing 3 modified silica-gel SG-1 and modified silica-gel SG-2, the adsorption curve performance map of steam.
Specific embodiment
Illustrate this patent below by some embodiments, but the present invention be not limited by the example:
Embodiment 1:
(1) silica gel pretreatment: 10g aperture about 7nm SG-0 microgranule is put in culture dish, is placed in vacuum drying oven,
Under temperature 100 DEG C, vacuum 0.096MPa, it is dried 4h, obtains the miscellaneous pretreated silica gel of evanescence of heat.
(2) silane modifier preparation: measure 75mL normal heptane in there-necked flask, adds 5mL's subsequently in there-necked flask
Ethanol, mix homogeneously, the trim,ethylchlorosilane adding 5mL adds in there-necked flask, carries out preparing required silane modifier.
(3) silica gel hydrophobically modified: silica gel pretreated in above-mentioned steps 1 is added the silane mixture of preparation in above-mentioned steps 2
Carry out under solution room temperature impregnating 10h, it is thus achieved that semi-finished product dewatering silica gel.
(4) prepared by dewatering silica gel commercialization: above-mentioned semi-finished product dewatering silica gel normal heptane cleans the silicon in remaining modified silica-gel
Alkane modifying agent, refilters, and 3 times to remove the silane modifier in silica gel repeatedly, then the silica gel after this filtration is put into vacuum does
In dry case, under design temperature 70 DEG C, vacuum 0.09MPa, it is dried 2h, is adsorbed in the normal heptane of Silica Surface, water to remove
Steam, makes silica gel weight no longer change, and i.e. prepares only by the modified silica-gel SG-1 after silane modifier hydrophobically modified.
Embodiment 2:
(1) silica gel pretreatment: 10g aperture about 7nm SG-0 microgranule is put in culture dish, is placed in vacuum drying oven,
Under temperature 100 DEG C, vacuum 0.096MPa, it is dried 4h, obtains the miscellaneous pretreated silica gel of evanescence of heat.
(2) silane modifier preparation: measure 75mL normal heptane in there-necked flask, adds 5mL's subsequently in there-necked flask
Ethanol, mix homogeneously, the trim,ethylchlorosilane adding 5mL adds in there-necked flask, carries out preparing required silane modifier.
(3) silica gel is modified: silica gel pretreated in above-mentioned steps 1 adds the silane mixture solution of preparation in above-mentioned steps 2
In, after impregnating 1h under room temperature, put in microwave oven, under microwave power is 500W, temperature 70 C, act on 20min,
Under without microwave action, continue dipping subsequently, make dipping total time reach 10h, it is thus achieved that semi-finished product dewatering silica gel.
(4) prepared by dewatering silica gel commercialization: that is cleaned by semi-finished product dewatering silica gel normal heptane in remaining modified silica-gel is silane-modified
Agent, refilters, and 3 times to remove the silane modifier in silica gel repeatedly, then is put into by the silica gel after this filtration and have evacuation merit
The microwave oven of energy is dried, and is dried 2h under design temperature 70 DEG C, vacuum 0.09MPa, is just being adsorbed in Silica Surface to remove
Heptane, steam and microwave functionalization process again, make silica gel weight no longer change, i.e. prepare silane modifier at microwave action
The modified silica-gel SG-2 of lower hydrophobically modified.
Accompanying drawing 1, accompanying drawing 2, accompanying drawing 3 are the actual modified result sign of embodiment 1, embodiment 2.From accompanying drawing 1, accompanying drawing 2,
Accompanying drawing 3 is it can be seen that the average pore size of (1) common silica gel SG-0, modified silica-gel SG-1 and modified silica-gel SG-2 is respectively
7.13nm, 6.61nm, 5.57nm, and broadly fall into mesoporous material, total pore volume is respectively 0.823cm3/g、0.845cm3/g、
0.600cm3/g；Specific surface area is respectively 461.68m2/g、511.51m2/g、430.99m2/g.(2) when 20 DEG C, SG-0,
After SG-1 and SG-2 is to water vapor adsorption 8h, its adsorbance is respectively 0.154g/g, 0.089g/g, 0.022g/g；SG-0、
After SG-1 and SG-2 is to normal hexane absorption 8h, its adsorbance is respectively 0.369g/g, 0.309g/g, 0.322g/g；Silica gel leads to
Crossing modified, the hydrophobic performance of SG-1, SG-2 is obtained for raising, and wherein SG-2 modified hydrophobic effect becomes apparent from, and relatively changes
Water absorption rate before property reduces 600%.(3) SG-1, SG-2 to the adsorbance after water vapor adsorption 8h respectively from initial 0.089
G/g, 0.022g/g rise to repeat to adsorb 0.111g/g, 0.037g/g when the 7th time；Normal hexane is adsorbed 8h by SG-1, SG-2
After adsorbance drop to 0.297g/g, 0.302g/g when repeating to adsorb the 7th time respectively from initial 0.309g/g, 0.322g/g；
Can be obtained by data analysis: along with the increase of SG-1, SG-2 absorption number of times, obvious normal hexane adsorbance does not occur
Decline or water vapor adsorption amount rise phenomenon, the circulation absorption better performances of the silica gel that this explanation is modified, can use for a long time.
Understand through data above analysis contrast: silane modifier at microwave action under SG-0 is modified the modified silica-gel that obtains
SG-2 is less than the modified silica-gel SG-1 average pore size that only obtained by silane modifier modification, and the hydrophobic performance of SG-2 and
Normal hexane absorption property is higher than SG-1, and SG-2 has good circulation absorption performance simultaneously, and this shows that silane modifier is micro-
Carry out under ripple effect that silica gel is modified has the effect become apparent from.
Claims (5)
1. silica gel hydrophobically modified method under a microwave action, it is characterized in that: with common aerosil particles as raw material, first silica gel pretreatment is carried out, silane modifier it is made into according to a certain percentage again with normal heptane, ethanol and trim,ethylchlorosilane, then pretreated silica gel is immersed in silane modifier and is aided with microwave action and carry out silica gel modification, obtain semi-finished product dewatering silica gel, finally by semi-finished product dewatering silica gel commercialization, obtain the dewatering silica gel with good hydrophobic effect and absorption property.
2. silica gel hydrophobically modified method under a kind of microwave action as claimed in claim 1, its silica gel preprocessed features is: be that 5～8nm common pore Bibulous Silica Gel microgranules are put into culture dish and are placed in vacuum drying oven by aperture, temperature be 80～100 DEG C, vacuum be under 0.096～0.098MPa, be vacuum dried 2～4h.
3. silica gel hydrophobically modified method under a kind of microwave action as claimed in claim 1, its silane modifier is characterised by: takes normal heptane, ethanol and trim,ethylchlorosilane and mixes in there-necked flask, and wherein mixed proportion is that every 1.0mL trim,ethylchlorosilane adds 1.0～2.0mL ethanol, 12～15mL normal heptane.
4. silica gel hydrophobically modified method under a kind of microwave action as claimed in claim 1, its silica gel modification is characterised by: takes in the pretreated silica gel silane-modified agent solution of addition and impregnates, and be aided with microwave and be modified, wherein dip time 8～12h, microwave power is 500～700W, temperature is 50～80 DEG C, and the microwave action time is 10～30min, it is thus achieved that semi-finished product dewatering silica gel.
5. silica gel hydrophobically modified method under a kind of microwave action as claimed in claim 1, its semi-finished product dewatering silica gel commercialization is characterised by: semi-finished product dewatering silica gel normal heptane cleans the silane modifier in remaining modified silica-gel, refilter, need 3～5 times repeatedly, to remove the silane modifier in silica gel, again the silica gel after this filtration is put into and there is the microwave oven of evacuation function be dried, design temperature 60～80 DEG C, 2～3h it are dried under vacuum 0.085～0.09MPa, to remove the normal heptane being adsorbed in Silica Surface, steam and again microwave functionalization process, silica gel weight is made no longer to change, i.e. prepare the dewatering silica gel with good hydrophobic effect and absorption property.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687246A (en) * | 2005-03-28 | 2005-10-26 | 广州吉必时科技实业有限公司 | Method for preparing hydrophobic type nano silicon dioxide thruogh continuous surface treatment |
| US20080241408A1 (en) * | 2007-04-02 | 2008-10-02 | Scott Cumberland | Colloidal Particles for Lotus Effect |
| CN104355313A (en) * | 2014-08-06 | 2015-02-18 | 泉州三欣新材料科技有限公司 | Simple and easy preparation method for silicon dioxide hydrophobic porous materials |
-
2016
- 2016-07-12 CN CN201610546200.6A patent/CN106000290A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687246A (en) * | 2005-03-28 | 2005-10-26 | 广州吉必时科技实业有限公司 | Method for preparing hydrophobic type nano silicon dioxide thruogh continuous surface treatment |
| US20080241408A1 (en) * | 2007-04-02 | 2008-10-02 | Scott Cumberland | Colloidal Particles for Lotus Effect |
| CN104355313A (en) * | 2014-08-06 | 2015-02-18 | 泉州三欣新材料科技有限公司 | Simple and easy preparation method for silicon dioxide hydrophobic porous materials |
Non-Patent Citations (2)
| Title |
|---|
| RYAN A. HAYN等: "Preparation of highly hydrophobic and oleophobic textile surfaces using microwave-promoted silane coupling", 《J MATER SCI》 * |
| 黄维秋等: "油气吸附剂及其改性方法", 《环境工程学报》 * |
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