CN110127707A - A method of high hydrophobicity aerosil is prepared with product silica gel in phosphate fertilizer industry - Google Patents
A method of high hydrophobicity aerosil is prepared with product silica gel in phosphate fertilizer industry Download PDFInfo
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- CN110127707A CN110127707A CN201910507237.1A CN201910507237A CN110127707A CN 110127707 A CN110127707 A CN 110127707A CN 201910507237 A CN201910507237 A CN 201910507237A CN 110127707 A CN110127707 A CN 110127707A
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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
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
Abstract
The invention discloses a kind of methods for preparing high hydrophobicity aerosil with product silica gel in phosphate fertilizer industry, the solvent for reducing surface tension is added by washing, filtering by silica gel using product silica gel in phosphate fertilizer industry as silicon source in this method, ultrasonic wave dispersion, obtains silicon dioxide gel；By the way that basic catalyst catalysis is added, make colloidal sol polycondensation gel；Gel is by aging, solvent displacement, silicic acid anhydride, the powdered silica aeroge that must finally have excellent performance through constant pressure and dry.It is an advantage of the current invention that realizing, the resource utilization of product silica gel in phosphate fertilizer industry, promotion is environmentally friendly, economize the land resource, preparation cost greatly reduces, preparation process is simplified, the quality of product is very excellent.
Description
Technical field
The present invention relates to a kind of preparation processes of inexpensive hydrophobic silicon dioxide aerogel, belong to nano material technology neck
Domain.
Background technique
Aerosil is a kind of more empty materials of nanometer, with high porosity, bigger serface, low-density and low
The features such as thermal coefficient, the aerosil for being is in high temperature resistant heat insulation material, extremely-low density material, gas absorption and filtering
There is very extensive application prospect in the fields such as material, catalyst carrier material, drug carrier material.Although aerosil
It has excellent performance, but since preparation cost is high, this largely limits its popularization and application.
Currently, relatively common aerosil preparation process is sol-gel method.The ideal silicon source of this method is more
For organic silicon source, such as Shen Jun with ethyl orthosilicate (TEOS) for raw material, using sol-gel method and supercritical drying process system
For light nanoporous material aerosil, (Shen Jun, Wang Jue, Gan Lihua wait sol-gel processing to prepare SiO2Gas
Gel and its characteristic research [J] Journal of Inorganic Materials, 1995 (1): 69-75.), Deng Zhongsheng etc. using multi-polysiloxane as silicon source,
By sol-gel, surface modification and supercritical drying be prepared for hydrophobic type aerosil (Deng Zhongsheng, Wei Jiandong, cruelly
Yu Ping waits hydrophobic type SiO2Aeroge [J] Journal of Inorganic Materials, 2000,15 (2): 26-28.).In addition there are positive silicic acid first
Ester (TMOS), trimethylethoxysilane (TMES) etc., but organic silicon source price is more expensive, and portion of reagent has poison
Property.
Therefore the emphasis studied at present is transferred in cheap inorganic silicon source, such as waterglass, silica solution, rice hull ash, fine coal
Ash etc..CN106745000A discloses a kind of preparation method of waterglass base aerosil.This method is made with waterglass
For silicon source, the sodium ion in silicon source is removed by cation exchange resin.Later by the way that basic catalyst catalyzed polycondensation, molten is added
Agent replacement, surface modification, dry acquisition aerosil.
CN101844771A is disclosed using sodium silicate aqueous solution as silicon source, adjusts pH value to 1, in 50 DEG C of environment with concentrated hydrochloric acid
Middle standing gel, the n-hexane and trim,ethylchlorosilane for being successively then 20% with deionized water, ethyl alcohol, n-hexane and volume ratio
Mixed solution respectively handle for 24 hours, it is finally dry at 150 DEG C, obtain SiO2Aeroge.Relatively complicated, need are operated in such method
A large amount of inorganic byproducts present in more solvent displacement removal wet gel are wanted, aeroge are damaged larger.Flyash and rice husk
Ash belongs to that added value is low, utility value is low, even the substance of solid waste, prepares aerosil with substance of this kind
Its added value is substantially increased, and reduces cost.But using flyash, rice hull ash as the work of waste aerosil
Skill generally requires to leach element silicon therein with alkaline solution, and the impurity on the one hand removed in raw material is extremely difficult, on the other hand
Operating procedure is considerably increased, is produced cumbersome.
CN102642842A discloses a kind of method for preparing aerosil with acidic silicasol, molten with acid silicon
Glue is raw material, directly forms gel under the action of acidand basecatalysts, prepares and is not related to organic solvent in gel process and improves it
SiO is made by overcritical or constant pressure and dry after solvent displacement, surface are silylated in the safety of production2Aeroge.
The method eliminates the step for needing to remove the cation such as sodium, potassium when waterglass is silicon source, shortens preparation flow.But silicon is molten
Glue cost is still higher, and silica solution production can also use waterglass mostly, unavoidable to make to contain in silica solution
Inorganic byproduct.If do not handled these by-products, these by-products are eventually entered in aerosil, shadow
Ring its performance.
Phosphate fertilizer industry by-product silica gel (majority is acidity) is mainly derived from waste gas containing fluoride (ocratation) absorption process.Its
Reaction equation are as follows: H2O+2SiF4→2H2SiF6+SiO2.This silica gel can become the reason of aerosil after treatment
Think silicon source.As a kind of byproduct of phosphatic fertilizer, which is usually taken as solid waste stacking.If preparing titanium dioxide using it
Silica aerogel will be able to achieve the resource utilization of product silica gel in phosphate fertilizer industry, can preserve the ecological environment and obtain biggish warp
Ji benefit.
Summary of the invention
The problem to be solved in the present invention is the high added value resource utilization problem for phosphate fertilizer industry by-product silica gel, is provided
A kind of preparation process is simple, cost is relatively low, reaction condition is controllable and the method for aerosil function admirable obtained.
The present invention adopts the following technical scheme that realization.
A method of high hydrophobicity aerosil being prepared with product silica gel in phosphate fertilizer industry, the method for the present invention includes such as
Lower step:
(1) preparation of silica dioxide gel:
Product silica gel in phosphate fertilizer industry is washed with deionized water, filters, obtains filter cake；
Deionized water is added into filter cake and reduces the solvent of surface tension, obtains silica gel solution；
Silica gel solution is heated, and silica gel solution is dispersed with ultrasonic wave, obtains silicon dioxide gel；
Become silica dioxide gel with basic catalyst catalysis silicon dioxide gel polycondensation；
(2) solvent is replaced
With the water in dehydrated alcohol or n-hexane exchange removal silica dioxide gel, wet gel is obtained；
(3) surface hydrophobicity is handled
Silicic acid anhydride is carried out to wet gel using three kinds of dehydrated alcohol, n-hexane, hexamethyldisilazane substances, must be changed
Property gel；
(4) constant pressure and dry
The modified gel obtained is washed through dehydrated alcohol, is then dried, it is final to obtain hydrophobic silicon dioxide aerogel.
Above-mentioned steps content is preparing final products of the present invention: when hydrophobic silicon dioxide aerogel, according to general technology
Technological means caused by personnel's normal logic thinking may be implemented.But to performance very excellent aeroge when, need
Incorporate following technical essential.
It is further in step of the present invention (1), to increase aging process step after silica dioxide gel is made,
The silica dioxide gel that will be obtained carries out aging process: silica dioxide gel carries out at aging under 50 DEG C~60 DEG C temperature environments
Reason；Ageing time is controlled in 6~12h.
It is further that in step of the present invention (1), the mass ratio of the deionized water and product silica gel in phosphate fertilizer industry is
1:0.2~0.4.
It is further that in step of the present invention (1), the silica gel after washing, which is configured to solid content, with deionized water is
25%~30% solution；The pH of silica gel solution is 3~5.
It is further that in step of the present invention (1), the temperature for heating silica gel solution is 60 DEG C~80 DEG C；For dividing
The ultrasonic frequency for dissipating silica gel solution is 40kHz~60kHz, jitter time 30min.
It is further that in step of the present invention (1), the solvent for reducing surface tension is diethanol amine or triethanolamine
One of；Silica gel solution and the mass ratio for reducing the solvent of surface tension are 1:0.005~1:0.008.
It is further that in step of the present invention (1), basic catalyst is in sodium hydroxide, potassium hydroxide or ammonium hydroxide
One kind；The pH value of solution is 6~7 after basic catalyst catalysis.
It is further that in step (2) of the present invention, the swap time using dehydrated alcohol is 8h~12h, every 2h~4h mono-
It is secondary；The mass ratio of dehydrated alcohol and wet gel is 1:1~2:1；Or, the use of the swap time of n-hexane is 12h, every 6h exchange one
It is secondary；The mass ratio of n-hexane and wet gel is 1:1.
It is further in step (3) of the present invention, to use three kinds of dehydrated alcohol, n-hexane, hexamethyldisilazane substances pair
The sequencing that wet gel carries out silicic acid anhydride is dehydrated alcohol, hexamethyldisilazane, n-hexane；Wherein, anhydrous second
Alcohol, hexamethyldisilazane, n-hexane, wet gel mass ratio be 1:1:4:4 or 1:1:1:2；Dehydrated alcohol, two silicon of hexamethyl
Amine alkane, every kind of substance of n-hexane time for adding be 30min, after being added dropwise to complete, the time of the silicic acid anhydride of silica gel is
12h-24h, temperature are controlled at 30 DEG C -50 DEG C.
It is further that constant pressure and dry described in step (4) of the present invention uses two step seasonings, two step seasonings are, first
Dry 1h~2h in the environment of temperature is 60 DEG C, then continue dry 1h~2h in the environment of temperature is 200 DEG C.
Beneficial effects of the present invention: 1) resource utilization of product silica gel in phosphate fertilizer industry is realized: due to choosing phosphate fertilizer by-product silicon
Glue becomes the higher silica gas of added value as silicon source, by the byproduct of phosphatic fertilizer of the lower even waste of this added value
Gel.2) environmental protection, economize the land resource: due to waste material generally as waste landfill processing, needed for enterprise especially
Prepare, obtain the right to use of tract area, and on the soil after landfill byproduct of phosphatic fertilizer, it is still desirable to raise to it
Dirt, rainwater dissolution, soil pollution etc. are controlled, and need sizable capital investment, and will cause to a certain degree to environment
Destruction.And method of the invention exactly solves the above problem, turns waste into wealth, and really brings material benefit for enterprise.3) it prepares
Cost greatly reduces: compared with using organic silicon source or silica solution, using product silica gel in phosphate fertilizer industry as silicon source, greatly reduces silicon
Source cost.4) preparation process simplifies；Compared with organic silicon source, eliminates and prepare the hydrolytic process that wet gel is subjected to；With water
The inorganic silicon source such as glass is compared, avoid spent ion exchange resin processing byproduct ion or waterglass Hydrolyze method preparation after repeatedly
Water-washing desalting process, reduces process flow.5) aerosil produced by the present invention, tested analysis showed that it is average
20~50nm of aperture, 400~600m of specific surface area2/ g, 0.015~0.030w/ of thermal coefficient (mk), to the contact angle of water
140 °~160 °, quality is very excellent.
The present invention is further explained With reference to embodiment.
Specific embodiment
In order to introduce technical solution of the present invention in more detail, specific embodiment has been carried out below, but of the invention
Content is not limited to following embodiment.
A method of high hydrophobicity aerosil being prepared with product silica gel in phosphate fertilizer industry, the method for the present invention includes such as
Lower step:
(1) preparation of silica dioxide gel:
Product silica gel in phosphate fertilizer industry is washed with deionized water, filters, obtains filter cake；
Deionized water is added into filter cake and reduces the solvent of surface tension, obtains silica gel solution；
Silica gel solution is heated, and silica gel solution is dispersed with ultrasonic wave, obtains silicon dioxide gel；
Become silica dioxide gel with basic catalyst catalysis silicon dioxide gel polycondensation；
(2) solvent is replaced
With the water in dehydrated alcohol or n-hexane exchange removal silica dioxide gel, wet gel is obtained；
(3) surface hydrophobicity is handled
Silicic acid anhydride is carried out to wet gel using three kinds of dehydrated alcohol, n-hexane, hexamethyldisilazane substances, must be changed
Property gel；
(4) constant pressure and dry
The modified gel obtained is washed through dehydrated alcohol, is then dried, it is final to obtain hydrophobic silicon dioxide aerogel.
Above-mentioned steps content is preparing final products of the present invention: when hydrophobic silicon dioxide aerogel, according to general technology
Technological means caused by personnel's normal logic thinking may be implemented.But to performance very excellent aeroge when, need
Incorporate following technical essential.
It is further in step of the present invention (1), to increase aging process step after silica dioxide gel is made,
The silica dioxide gel that will be obtained carries out aging process: silica dioxide gel carries out at aging under 50 DEG C~60 DEG C temperature environments
Reason；Ageing time is controlled in 6~12h.
It is further that in step of the present invention (1), the mass ratio of the deionized water and product silica gel in phosphate fertilizer industry is
1:0.2~0.4.
It is further that in step of the present invention (1), the silica gel after washing, which is configured to solid content, with deionized water is
25%~30% solution；The pH of silica gel solution is 3~5.
It is further that in step of the present invention (1), the temperature for heating silica gel solution is 60 DEG C~80 DEG C；For dividing
The ultrasonic frequency for dissipating silica gel solution is 40kHz~60kHz, jitter time 30min.
It is further that in step of the present invention (1), the solvent for reducing surface tension is diethanol amine or triethanolamine
One of；Silica gel solution and the mass ratio for reducing the solvent of surface tension are 1:0.005~1:0.008.
It is further that in step of the present invention (1), basic catalyst is in sodium hydroxide, potassium hydroxide or ammonium hydroxide
One kind；The pH value of solution is 6~7 after basic catalyst catalysis.
It is further that in step (2) of the present invention, the swap time using dehydrated alcohol is 8h~12h, every 2h~4h mono-
It is secondary；The mass ratio of dehydrated alcohol and wet gel is 1:1~2:1；Or, the use of the swap time of n-hexane is 12h, every 6h exchange one
It is secondary；The mass ratio of n-hexane and wet gel is 1:1.
It is further in step (3) of the present invention, to use three kinds of dehydrated alcohol, n-hexane, hexamethyldisilazane substances pair
The sequencing that wet gel carries out silicic acid anhydride is dehydrated alcohol, hexamethyldisilazane, n-hexane；Wherein, anhydrous second
Alcohol, hexamethyldisilazane, n-hexane, wet gel mass ratio be 1:1:4:4 or 1:1:1:2；Dehydrated alcohol, two silicon of hexamethyl
Amine alkane, every kind of substance of n-hexane time for adding be 30min, after being added dropwise to complete, the time of the silicic acid anhydride of silica gel is
12h-24h, temperature are controlled at 30 DEG C -50 DEG C.
It is further that constant pressure and dry described in step (4) of the present invention uses two step seasonings, two step seasonings are, first
Dry 1h~2h in the environment of temperature is 60 DEG C, then continue dry 1h~2h in the environment of temperature is 200 DEG C.
Operate embodiment:
Embodiment 1
100g product silica gel in phosphate fertilizer industry is washed using 250ml deionized water, filters, obtains filter cake；Into filter cake be added go from
Sub- water and the solvent for reducing surface tension, obtain silica gel solution；The solvent for reducing surface tension is one of diethanol amine；Silica gel
Solution and the mass ratio for reducing the solvent of surface tension are 1:0.005.Solid content is 30% in silica gel solution.In 60 DEG C of temperature
Under silica gel solution is heated, and silica gel solution is dispersed with ultrasonic wave, ultrasonic frequency 40kHz, jitter time
For 30min.With basic catalyst: sodium hydroxide, catalysis silicon dioxide gel polycondensation become silica dioxide gel；Solution after catalysis
PH value be 6.Silica dioxide gel is subjected to aging process, aging process temperature is 50 DEG C, and the processing time is 6h.
By the silica dioxide gel dehydrated alcohol or n-hexane exchange removal water therein after aging process, obtain wet solidifying
Glue；It the use of the swap time of dehydrated alcohol is 8h, every 2h is primary；The mass ratio of dehydrated alcohol and wet gel is 1:1；
Silicic acid anhydride successively is carried out to wet gel using three kinds of dehydrated alcohol, n-hexane, hexamethyldisilazane substances,
Wherein, dehydrated alcohol, hexamethyldisilazane, n-hexane, wet gel mass ratio be 1:1:4:4；Dehydrated alcohol, hexamethyl two
Silicon amine alkane, every kind of substance of n-hexane time for adding be 30min, after being added dropwise to complete, the time of the silicic acid anhydride of silica gel is
12h, temperature are controlled at 30 DEG C.Obtain modified gel.
It is dry that obtained modified gel is carried out to two steps after dehydrated alcohol washs: first dry in the environment of temperature is 60 DEG C
Dry 1h, then continue dry 1h in the environment of temperature is 200 DEG C.Finally obtain hydrophobic silicon dioxide aerogel.It is prepared
Hydrophobic silicon dioxide aerogel parameter are as follows: specific surface area is 412.4m2/ g, average pore size 48nm, the contact angle to water are
157 °, thermal coefficient is 0.029W/ (mK).
Embodiment 2
75g product silica gel in phosphate fertilizer industry is washed using 250ml deionized water, filters, obtains filter cake；Deionization is added into filter cake
Water and the solvent for reducing surface tension, obtain silica gel solution；The solvent for reducing surface tension is one of triethanolamine；Silica gel is molten
Liquid and the mass ratio for reducing the solvent of surface tension are 1:0.007.Solid content is 28% in silica gel solution.70 DEG C at a temperature of
Silica gel solution is heated, and silica gel solution is dispersed with ultrasonic wave, ultrasonic frequency 50kHz, jitter time is
30min.With basic catalyst: ammonium hydroxide, catalysis silicon dioxide gel polycondensation become silica dioxide gel；The pH value of solution after catalysis
It is 6.5.Silica dioxide gel is subjected to aging process, aging process temperature is 55 DEG C, and the processing time is 8h.
By the silica dioxide gel dehydrated alcohol or n-hexane exchange removal water therein after aging process, obtain wet solidifying
Glue；Swap time using n-hexane is 12h, and every 6h exchange is primary；The mass ratio of n-hexane and wet gel is 1:1.
Silicic acid anhydride successively is carried out to wet gel using three kinds of dehydrated alcohol, n-hexane, hexamethyldisilazane substances,
Wherein, dehydrated alcohol, hexamethyldisilazane, n-hexane, wet gel mass ratio be 1:1:1:2；Dehydrated alcohol, hexamethyl two
Silicon amine alkane, every kind of substance of n-hexane time for adding be 30min, after being added dropwise to complete, the time of the silicic acid anhydride of silica gel is
18h, temperature are controlled at 40 DEG C.Obtain modified gel.
It is dry that obtained modified gel is carried out to two steps after dehydrated alcohol washs: first dry in the environment of temperature is 60 DEG C
Dry 1.5h, then continue dry 1.5h in the environment of temperature is 200 DEG C.Finally obtain hydrophobic silicon dioxide aerogel.
The silica airsetting specific surface area being prepared is 512.2m2/ g, average pore size 29nm, the contact angle to water are
152 °, thermal coefficient is 0.024W/ (mK).
Embodiment 3
100g product silica gel in phosphate fertilizer industry is washed using 250ml deionized water, filters, obtains filter cake；Into filter cake be added go from
Sub- water and the solvent for reducing surface tension, obtain silica gel solution；The solvent for reducing surface tension is one of triethanolamine；Silica gel
Solution and the mass ratio for reducing the solvent of surface tension are 1:0.008.Solid content is 30% in silica gel solution.In 80 DEG C of temperature
Under silica gel solution is heated, and silica gel solution is dispersed with ultrasonic wave, ultrasonic frequency 60kHz, jitter time
For 30min.With basic catalyst: potassium hydroxide, catalysis silicon dioxide gel polycondensation become silica dioxide gel；Solution after catalysis
PH value be 7.Silica dioxide gel is subjected to aging process, aging process temperature is 60 DEG C, and the processing time is 10h.
By the silica dioxide gel dehydrated alcohol or n-hexane exchange removal water therein after aging process, obtain wet solidifying
Glue；Swap time using n-hexane is 12h, and every 6h exchange is primary；The mass ratio of n-hexane and wet gel is 1:1.
Silicic acid anhydride successively is carried out to wet gel using three kinds of dehydrated alcohol, n-hexane, hexamethyldisilazane substances,
Wherein, dehydrated alcohol, hexamethyldisilazane, n-hexane, wet gel mass ratio be 1:1:4:4；Dehydrated alcohol, hexamethyl two
Silicon amine alkane, every kind of substance of n-hexane time for adding be 30min, after being added dropwise to complete, the time of the silicic acid anhydride of silica gel is
16h, temperature are controlled at 45 DEG C.Obtain modified gel.
It is dry that obtained modified gel is carried out to two steps after dehydrated alcohol washs: first dry in the environment of temperature is 60 DEG C
Dry 2h, then continue dry 2h in the environment of temperature is 200 DEG C.Finally obtain hydrophobic silicon dioxide aerogel.
The silica airsetting specific surface area being prepared is 573.6m2/ g, average pore size 37nm, the contact angle to water are
147 °, thermal coefficient is 0.022W/ (mK).
Embodiment 4
50g product silica gel in phosphate fertilizer industry is washed using 250ml deionized water, filters, obtains filter cake；Deionization is added into filter cake
Water and the solvent for reducing surface tension, obtain silica gel solution；The solvent for reducing surface tension is diethanol amine；Silica gel solution and reduction
The mass ratio of the solvent of surface tension is 1:0.008.Solid content is 26% in silica gel solution.75 DEG C at a temperature of it is molten to silica gel
Liquid is heated, and is dispersed with ultrasonic wave to silica gel solution, ultrasonic frequency 55kHz, jitter time 30min.With
Basic catalyst: ammonium hydroxide, catalysis silicon dioxide gel polycondensation become silica dioxide gel；The pH value of solution is 6.7 after catalysis.It will
Silica dioxide gel carries out aging process, and aging process temperature is 52 DEG C, and the processing time is 12h.
By the silica dioxide gel dehydrated alcohol or n-hexane exchange removal water therein after aging process, obtain wet solidifying
Glue；It the use of the swap time of dehydrated alcohol is 12h, every 4h is primary；The mass ratio of dehydrated alcohol and wet gel is 2:1；
Silicic acid anhydride successively is carried out to wet gel using three kinds of dehydrated alcohol, n-hexane, hexamethyldisilazane substances,
Wherein, dehydrated alcohol, hexamethyldisilazane, n-hexane, wet gel mass ratio be 1:1:1:2；Dehydrated alcohol, hexamethyl two
Silicon amine alkane, every kind of substance of n-hexane time for adding be 30min, after being added dropwise to complete, the time of the silicic acid anhydride of silica gel is
For 24 hours, temperature control is at 50 DEG C.Obtain modified gel.
It is dry that obtained modified gel is carried out to two steps after dehydrated alcohol washs: first dry in the environment of temperature is 60 DEG C
Dry 1.5h, then continue dry 2h in the environment of temperature is 200 DEG C.Finally obtain hydrophobic silicon dioxide aerogel.
The silica airsetting specific surface area being prepared is 612.5m2/ g, average pore size 20nm, the contact angle to water are
160 °, thermal coefficient is 0.015W/ (mK).
Embodiment 5
62.5g product silica gel in phosphate fertilizer industry is washed using 250ml deionized water, filters, obtains filter cake；Into filter cake be added go from
Sub- water and the solvent for reducing surface tension, obtain silica gel solution；The solvent for reducing surface tension is one of triethanolamine；Silica gel
Solution and the mass ratio for reducing the solvent of surface tension are 1:0.006.Solid content is 25% in silica gel solution.In 65 DEG C of temperature
Under silica gel solution is heated, and silica gel solution is dispersed with ultrasonic wave, ultrasonic frequency 45kHz, jitter time
For 30min.With basic catalyst: sodium hydroxide, catalysis silicon dioxide gel polycondensation become silica dioxide gel；Solution after catalysis
PH value be 6.3.Silica dioxide gel is subjected to aging process, aging process temperature is 57 DEG C, and the processing time is 6h.
By the silica dioxide gel dehydrated alcohol or n-hexane exchange removal water therein after aging process, obtain wet solidifying
Glue；It the use of the swap time of dehydrated alcohol is 9h, every 3h is primary；The mass ratio of dehydrated alcohol and wet gel is 1.5:1；Successively make
Silicic acid anhydride is carried out to wet gel with three kinds of dehydrated alcohol, n-hexane, hexamethyldisilazane substances, wherein dehydrated alcohol,
Hexamethyldisilazane, n-hexane, wet gel mass ratio be 1:1:4:4；Dehydrated alcohol, hexamethyldisilazane, n-hexane
The time for adding of every kind of substance is 30min, and after being added dropwise to complete, the time of the silicic acid anhydride of silica gel is 14h, and temperature control exists
35℃.Obtain modified gel.
It is dry that obtained modified gel is carried out to two steps after dehydrated alcohol washs: first dry in the environment of temperature is 60 DEG C
Dry 1.2h, then continue dry 1.6h in the environment of temperature is 200 DEG C.Finally obtain hydrophobic silicon dioxide aerogel.
The silica airsetting specific surface area being prepared is 434.1m2/ g, average pore size 43nm, the contact angle to water are
146 °, thermal coefficient is 0.027W/ (mK).
Above-described is only some embodiments of the invention (since technical parameter of the invention has numerical value model
It encloses, therefore embodiment cannot be exhaustive, protection scope documented by the present invention will put model with numberical range and other technologies of the invention
Subject to enclosing), well known particular content or common sense do not describe excessively herein in scheme.It should be pointed out that above-described embodiment is not to appoint
Where formula limitation is of the invention, for those skilled in the art, all to be obtained by the way of equivalent substitution or equivalent transformation
The technical solution obtained is fallen within the scope of protection of the present invention.This application claims protection scope should be in its claim
Subject to appearance, the records such as specific embodiment in specification can be used for explaining the content of claim.
Claims (10)
1. a kind of method for preparing high hydrophobicity aerosil with product silica gel in phosphate fertilizer industry, which is characterized in that this method packet
Include following steps:
(1) preparation of silica dioxide gel:
Product silica gel in phosphate fertilizer industry is washed with deionized water, filters, obtains filter cake；
Deionized water is added into filter cake and reduces the solvent of surface tension, obtains silica gel solution；
Silica gel solution is heated, and silica gel solution is dispersed with ultrasonic wave, obtains silicon dioxide gel；
Become silica dioxide gel with basic catalyst catalysis silicon dioxide gel polycondensation；
(2) solvent is replaced
With the water in dehydrated alcohol or n-hexane exchange removal silica dioxide gel, wet gel is obtained；
(3) surface hydrophobicity is handled
Silicic acid anhydride is carried out to wet gel using three kinds of dehydrated alcohol, n-hexane, hexamethyldisilazane substances, must be modified solidifying
Glue；
(4) constant pressure and dry
The modified gel obtained is washed through dehydrated alcohol, is then dried, it is final to obtain hydrophobic silicon dioxide aerogel.
2. a kind of method for preparing high hydrophobicity aerosil with product silica gel in phosphate fertilizer industry according to claim 1,
It is characterized in that, increasing aging process step, i.e., the dioxy that will be obtained after silica dioxide gel is made in the step (1)
SiClx gel carries out aging process: silica dioxide gel carries out aging process under 50 DEG C~60 DEG C temperature environments；Ageing time
Control is in 6~12h.
3. a kind of side for preparing high hydrophobicity aerosil with product silica gel in phosphate fertilizer industry according to claim 1 or 2
Method, which is characterized in that in the step (1), the mass ratio of the deionized water and product silica gel in phosphate fertilizer industry be 1:0.2~
0.4。
4. a kind of side for preparing high hydrophobicity aerosil with product silica gel in phosphate fertilizer industry according to claim 1 or 2
Method, which is characterized in that in the step (1), with deionized water by the silica gel after washing be configured to solid content be 25%~
30% solution；The pH of silica gel solution is 3~5.
5. a kind of side for preparing high hydrophobicity aerosil with product silica gel in phosphate fertilizer industry according to claim 1 or 2
Method, which is characterized in that in the step (1), the temperature for heating silica gel solution is 60 DEG C~80 DEG C；For dispersing silica gel solution
Ultrasonic frequency be 40kHz~60kHz, jitter time 30min.
6. a kind of side for preparing high hydrophobicity aerosil with product silica gel in phosphate fertilizer industry according to claim 1 or 2
Method, which is characterized in that in the step (1), the solvent for reducing surface tension is one of diethanol amine or triethanolamine；
Silica gel solution and the mass ratio for reducing the solvent of surface tension are 1:0.005~1:0.008.
7. a kind of side for preparing high hydrophobicity aerosil with product silica gel in phosphate fertilizer industry according to claim 1 or 2
Method, which is characterized in that in the step (1), basic catalyst is one of sodium hydroxide, potassium hydroxide or ammonium hydroxide；Alkali
Property catalyst after solution pH value be 6~7.
8. a kind of side for preparing high hydrophobicity aerosil with product silica gel in phosphate fertilizer industry according to claim 1 or 2
Method, which is characterized in that the use of the swap time of dehydrated alcohol is 8h~12h, every 2h~4h is primary in step (2)；Dehydrated alcohol
Mass ratio with wet gel is 1:1~2:1；Or, the use of the swap time of n-hexane being 12h, every 6h exchange is primary；N-hexane with
The mass ratio of wet gel is 1:1.
9. a kind of side for preparing high hydrophobicity aerosil with product silica gel in phosphate fertilizer industry according to claim 1 or 2
Method, which is characterized in that in step (3), using dehydrated alcohol, n-hexane, three kinds of substances of hexamethyldisilazane to wet gel into
The sequencing of row silicic acid anhydride is dehydrated alcohol, hexamethyldisilazane, n-hexane；Wherein, dehydrated alcohol, hexamethyl
Disilazane, n-hexane, wet gel mass ratio be 1:1:4:4 or 1:1:1:2；Dehydrated alcohol, hexamethyldisilazane, just oneself
The time for adding of every kind of substance of alkane is 30min, and after being added dropwise to complete, the time of the silicic acid anhydride of silica gel is 12h-24h, temperature
Control is at 30 DEG C -50 DEG C.
10. a kind of side for preparing high hydrophobicity aerosil with product silica gel in phosphate fertilizer industry according to claim 1 or 2
Method, which is characterized in that constant pressure and dry described in step (4) uses two step seasonings, and it is first 60 in temperature that two step seasonings, which are,
Dry 1h~2h in the environment of DEG C, then continue dry 1h~2h in the environment of temperature is 200 DEG C.
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| CN105800623A (en) * | 2016-03-26 | 2016-07-27 | 北京工业大学 | Method for preparing silicon dioxide aerogel heat insulation material at low cost with industrial waste residues of pipeline residues in phosphate fertilizer plants as raw materials |
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| KR20070013664A (en) * | 2005-07-27 | 2007-01-31 | 김종길 | New proces for producing silica and fluorine compound from hexafluorosilicic acid |
| CN1772608A (en) * | 2005-10-01 | 2006-05-17 | 薛彦辉 | Process of producing sodium metasilicate pentahydrate with waste industrial silicone gel |
| CN101318662A (en) * | 2008-07-10 | 2008-12-10 | 云南省化工研究院 | Method for preparing liquid soluble glass with silica gel in atmosphere pressure |
| CN102161487A (en) * | 2011-03-09 | 2011-08-24 | 云南云天化国际化工股份有限公司 | Method for producing pure silicon by using by-product silica gel in phosphate fertilizer industry |
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