CN108325497A - A kind of aeroge-diatomite multiple stage filtration system and its application - Google Patents
A kind of aeroge-diatomite multiple stage filtration system and its application Download PDFInfo
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- CN108325497A CN108325497A CN201810128705.XA CN201810128705A CN108325497A CN 108325497 A CN108325497 A CN 108325497A CN 201810128705 A CN201810128705 A CN 201810128705A CN 108325497 A CN108325497 A CN 108325497A
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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
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/14—Diatomaceous earth
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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
- B01J20/28014—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 form
- B01J20/28047—Gels
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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
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Dispersion Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention relates to environmental technology fields, specifically disclose a kind of aeroge diatomite multiple stage filtration system and its application.The multiple stage filtration system includes shell and filter core, if alternately filling dried layer SiO in filter core2Aeroge and super-cell, wherein SiO2The porosity of aeroge is 80 95%, and specific surface area is 400 800m2/g.The present invention removes the harmful small molecule and macromolecular in waste liquid for handling waste liquid of drilling, using filters, and adsorption efficiency is higher.
Description
Technical field
The present invention relates to environmental technology field more particularly to a kind of aeroge-diatomite multiple stage filtration system and its applications.
Background technology
The drilling fluid used in petroleum drilling engineering returns to ground and forms drilling wastes.There are many containing in drilling fluid
Chemical composition, while containing harmful substances such as heavy metals in the landwaste carried, therefore there is great environmental hazard.To drilling well
The processing of waste is to destroy its colloidal suspension system stablized first, realizes and be separated by solid-liquid separation, then discarded to solid-state respectively again
Object and waste liquid carry out in-depth processing.Wherein, it is still one at present to the processing of waste liquid of drilling because its harmful substance complexity is various
Technical barrier.It is a kind of feasible means to remove harmful small molecule in waste liquid and macromolecular using filters, but current mistake
There is filter means certain limitation, main problem to be that different size of molecule cannot be adsorbed in wide range, inhale simultaneously
It is attached less efficient.
Invention content
For limitation existing for existing filtering, the problems such as can not adsorbing different size of molecule on a large scale, the present invention carries
For a kind of aeroge-diatomite multiple stage filtration system.
And a kind of application of aeroge-diatomite multiple stage filtration system.
To achieve the above object of the invention, the embodiment of the present invention uses the following technical solution：
A kind of aeroge-diatomite multiple stage filtration system, the multiple stage filtration system include shell and filter core, the filter core
If interior alternately filling dried layer SiO2Aeroge and super-cell, wherein SiO2The porosity of aeroge is 80-95%, compares table
Area is 400-800m2/g。
Compared with the existing technology, aeroge provided by the invention-diatomite multiple stage filtration system, by being by porosity
80-95%, specific surface area 400-800m2The SiO of/g2Aeroge and diatomite are alternately filled, and multiple stage filtration system is formed,
SiO2Aeroge hole size distribution is uniform, and the porosity is high, has the porous characterization of adsorption to different size molecule, can be to organic
Macromolecular and inorganic molecules fully adsorb.
And the application the present invention also provides aeroge-diatomite multiple stage filtration system in processing waste liquid of drilling field.
Description of the drawings
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to needed in the embodiment
Attached drawing is briefly described.It should be evident that drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is aeroge provided in an embodiment of the present invention-diatomite multiple stage filtration system schematic diagram.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The embodiment of the present invention provides a kind of aeroge-diatomite multiple stage filtration system, and the multiple stage filtration system includes outer
Shell and filter core, if alternately filling dried layer SiO in the filter core2Aeroge and super-cell, wherein SiO2The hole of aeroge
Rate is 80-95%, specific surface area 400-800m2/g。
Compared with the existing technology, aeroge provided by the invention-diatomite multiple stage filtration system, by being by porosity
80-95%, specific surface area 400-800m2The SiO of/g2Aeroge and diatomite are alternately filled, and multiple stage filtration system is formed,
SiO2Aeroge hole size distribution is uniform, and the porosity is high, has the porous characterization of adsorption to different size molecule, can be to organic
Macromolecular and inorganic molecules fully adsorb.
Specifically, the preferably described SiO2For aeroge using inorganic silicon source as raw material, preparation process is as follows：
Acid is added into silicate solutions, adjusting pH value is 3-4, and stirring, then hydrolysis obtains colloidal sol in a water bath；
Lye is added into colloidal sol, adjusting pH value is 8-10, stands aging in water-bath, obtains the wet gel of aging；
The wet gel of aging is replaced with non-polar organic solvent, it is dry, obtain SiO2Aeroge.
Acidified by inorganic silicic acid, hydrolysis obtains colloidal sol, stands aging, and non-polar organic solvent displacement drying obtains gas
Gel, method is simple, obtained SiO2Aeroge porosity is 80-95%, specific surface area 400-800m2/g。
Preferably, the silicate is a concentration of：0.1-1mol/L；The silicate is waterglass.
Silicate concentration is excessively high, and water phase is reduced, and obtains the decline of wet gel time；Silicate concentration is too low, and water phase increases, water
The relative increase of amount has a notable detrimental effect to end properties (such as density), in wet gel the increase of moisture improve follow-up work
The difficulty of skill is easy to cause the notable aggravation of contraction.
Preferably, the SiO2For aeroge using organic silicon source as raw material, preparation process is as follows：
Absolute ethyl alcohol is added into organic silicon source and carries out alcoholization processing, acid is added, adjusting pH value is 3-4, then stirring exists
Hydrolysis obtains colloidal sol in water-bath；
The first solvent is added into colloidal sol, aging is stood in water-bath, obtains the wet gel of aging；
The wet gel of aging is replaced with non-polar organic solvent, it is dry, obtain SiO2Aeroge.
Water in organic silicon source is gone out using ethanol replacement, then carries out acidification concentration, obtains colloidal sol, aging is stood passing through,
Non-polar organic solvent displacement drying obtains aeroge, and method is simple, obtained SiO2Aeroge porosity is 80-95%, than
Surface area is 400-800m2/g。
Preferably, the organic silicon source is methyltrimethoxysilane, positive silicic acid second vinegar, diethyl dichlorosilane, pregnancy
Base disiloxane, dimethyldichlorosilane, dimethyldimethoxysil,ne, positive silicic acid second vinegar, chloropropyl triethoxysilane, two
Ethyl diethoxy silane, methyl trichlorosilane, methyltriethoxysilane, dimethyl diethoxysilane, three second of vinyl
At least one of oxysilane, ethyl trimethoxy silane；The organic silicon source it is a concentration of：0.1-1mol/L.
Silicon source excessive concentration, water phase are reduced, and obtain the decline of wet gel time；Silicon source concentration is too low, and water phase increases, water
Relative increase has a notable detrimental effect to end properties (such as density), in wet gel the increase of moisture improve subsequent technique
Difficulty is easy to cause the notable aggravation of contraction.
The volume ratio of the ethyl alcohol and organic silicon solution is 0.5-2：1；First solvent be methanol, ethyl alcohol, isopropanol,
At least one of butanol；The volume ratio of first solvent and colloidal sol is 0.5-1：1.
Gel time is related with quantity of solvent, and the first solvent is excessive, and aerosol time is long, but colloidal sol density is small, if first
Too little solvent, although aerosol time is short, colloidal sol density is big.
Preferably, the acid is one kind in the hydrochloric acid, sulfuric acid, organic acid of a concentration of 1-2mol/L；Acid is carried out to silicon source
Change concentration.
Hydrolysis obtains the condition of colloidal sol and is in the water-bath：Temperature：60-80 DEG C, the time：1-2h；It is stood in the water-bath
Ageing time is 45-48h.
Temperature increases the mutual collision for being conducive to colloidal sol particle and condense, and temperature raising and gel time are inversely proportional pass
System, but excessively high temperature be easy to cause structure unevenness with it is coarse, therefore selection 60-80 DEG C；If temperature is too low, energy under low temperature
Be hydrolyzed, polycondensation and dehydration, dissolved adhesiveness saltation zone time are obviously prolonged, obtain stable, can preserving the long period, just
In the colloidal sol of film forming, but temperature is too low, and colloidal sol and wet colloidal sol journey time are obviously prolonged, and are unfavorable for industrialization.
The non-polar organic solvent is one kind in n-hexane, hexamethylene, normal heptane；The non-polar organic solvent with
The volume ratio of wet gel is 3-10:1.
Non-polar organic solvent is excessive, and time swap is long, is unfavorable for industrialized development, and non-polar organic solvent is very few, wet
Gel density is big, is unfavorable for forming porosity height, the big aeroge of reference area.
The time swap is 23-24h；The drying condition is：30-60 DEG C, 24-48h.
Preferably, the super-cell calcines 2-5h using diatomite as raw material at 500 DEG C, then in lye
2-4h is impregnated, adjustment pH value is 6-7.
By diatomite by calcining removal impurity.
Preferably, the diatomite：Purity ＞ 99%, grain diameter≤200 μm；And/or
The concentration of lye is 0.08-0.12mol/L；And/or
PH value is adjusted using the HCl of 0.1~1mol/L.
Preferably, the filter core uses PE sintered filter cores；The SiO2The thickness of aeroge and super-cell ratio is
1:5-5:1；The shell further includes absorbing devices.
Suction strainer 100~1000kPa of negative pressure of absorbing devices, to improve filtering rate.
And the present invention also provides the aeroge-diatomite multiple stage filtration systems in processing waste liquid of drilling field
Application.
It is provided in an embodiment of the present invention in order to better illustrate, it is illustrated below by embodiment is further.
Embodiment 1
The present embodiment provides a kind of aeroge-diatomite multiple stage filtration system, including shell and filter core, alternately filled out in filter core
If filling dried layer SiO2Aeroge and super-cell, wherein SiO2The porosity of aeroge is 80-95%, and specific surface area is
400-800m2/g。
Select PE sintered filter cores as filter core, SiO2Aeroge and super-cell thickness ratio 1:1.Filter core is with stainless
Outer steel shell encapsulates.Absorbing devices, suction strainer negative pressure 1000kPa, to improve filtering rate are installed in stainless steel casing water outlet.
Above-mentioned SiO2For aeroge using inorganic silicon source as raw material, preparation process is as follows：
1mol/L hydrochloric acid is added into 0.5mol/L sodium silicate solution, adjusting pH value is 3-4, stirs 15-20min, then
Hydrolysis obtains colloidal sol, bath temperature in a water bath：60 DEG C, time 2h；
The sodium hydroxide of 1mol/L is added into colloidal sol, it is 9 to adjust pH value, and aging 48h is stood in water-bath, obtains aging
Wet gel；
The wet gel of aging n-hexane is replaced for 24 hours, the volume ratio of n-hexane and wet gel is 5:1, in 50- under normal pressure
Dry 24-27h, obtains SiO at 60 DEG C2Aeroge.
Above-mentioned super-cell is with purity ＞ 99%, and grain diameter≤200 μm diatomite is raw material, at 500 DEG C
2.5h is calcined, then impregnates 3h in 0.1mol/L lye, then the HCl of 0.1mol/L is used to adjust pH value as 7.
Embodiment 2
The present embodiment provides a kind of aeroge-diatomite multiple stage filtration system, including shell and filter core, alternately filled out in filter core
If filling dried layer SiO2Aeroge and super-cell, wherein SiO2The porosity of aeroge is 80-95%, and specific surface area is
400-800m2/g。
Select PE sintered filter cores as filter core, SiO2Aeroge and super-cell thickness ratio 5:1.Filter core is with stainless
Outer steel shell encapsulates.Absorbing devices, suction strainer negative pressure 100kPa, to improve filtering rate are installed in stainless steel casing water outlet.
Above-mentioned SiO2For aeroge using organic silicon source as raw material, preparation process is as follows：
The absolute ethyl alcohol that 2 times of volumes are added into 1mol/L organic silicon sources carries out alcoholization processing, and the sulfuric acid of 2mol/L is added,
Adjusting pH value is 3-4, stirs 15-20min, and then hydrolysis obtains colloidal sol, bath temperature in a water bath：80 DEG C, the time：1h；
The isopropanol with colloidal sol same volume is added into colloidal sol, aging 48h is stood in water-bath, obtains the wet gel of aging；
The wet gel of aging is replaced with normal heptane, the volume ratio of normal heptane and wet gel is 3:1, in 30-40 under normal pressure
Dry 45-48h, obtains SiO at DEG C2Aeroge is dried, and SiO is obtained2Aeroge.
Above-mentioned super-cell is with purity ＞ 99%, and grain diameter≤200 μm diatomite is raw material, at 500 DEG C
5h is calcined, then impregnates 2h in 0.1mol/L lye, pH value is adjusted as 7 in the HCl for using 1mol/L.
It is used for aeroge-diatomite multiple stage filtration system prepared by embodiment 1,2 to handle waste liquid of drilling, using filtering hand
Harmful small molecule and macromolecular in section removal waste liquid, and adsorption efficiency is higher.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modification, equivalent replacement or improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (10)
1. a kind of aeroge-diatomite multiple stage filtration system, it is characterised in that：The multiple stage filtration system includes shell and filter
Core, if alternately filling dried layer SiO in the filter core2Aeroge and super-cell, wherein SiO2The porosity of aeroge is
80-95%, specific surface area 400-800m2/g。
2. aeroge as described in claim 1-diatomite multiple stage filtration system, it is characterised in that：The SiO2Aeroge is with nothing
Machine silicon source is raw material, and preparation process is as follows：
Acid is added into silicate solutions, adjusting pH value is 3-4, and stirring, then hydrolysis obtains colloidal sol in a water bath；
Lye is added into colloidal sol, adjusting pH value is 8-10, stands aging in water-bath, obtains the wet gel of aging；
The wet gel of aging is replaced with non-polar organic solvent, it is dry, obtain SiO2Aeroge.
3. aeroge as claimed in claim 2-diatomite multiple stage filtration system, it is characterised in that：The concentration of the silicate
For：0.1-1mol/L；And/or
The silicate is waterglass.
4. aeroge as described in claim 1-diatomite multiple stage filtration system, it is characterised in that：The SiO2Aeroge is to have
Machine silicon source is raw material, and preparation process is as follows：
Absolute ethyl alcohol is added into organic silicon source and carries out alcoholization processing, acid is added, adjusting pH value is 3-4, stirring, then in water-bath
Middle hydrolysis obtains colloidal sol；
The first solvent is added into colloidal sol, aging is stood in water-bath, obtains the wet gel of aging；
The wet gel of aging is replaced with non-polar organic solvent, it is dry, obtain SiO2Aeroge.
5. aeroge as claimed in claim 4-diatomite multiple stage filtration system, it is characterised in that：The organic silicon source is first
Base trimethoxy silane, positive silicic acid second vinegar, diethyl dichlorosilane, hexamethyldisiloxane, dimethyldichlorosilane, dimethyl
Dimethoxysilane, positive silicic acid second vinegar, chloropropyl triethoxysilane, diethyldiethoxysilane, methyl trichlorosilane, first
In ethyl triethoxy silicane alkane, dimethyl diethoxysilane, vinyltriethoxysilane, ethyl trimethoxy silane at least
It is a kind of；And/or
The organic silicon source it is a concentration of：0.1-1mol/L；And/or
The volume ratio of the ethyl alcohol and organic silicon solution is 0.5-2：1；And/or
First solvent is at least one of methanol, ethyl alcohol, isopropanol, butanol；And/or
The volume ratio of first solvent and colloidal sol is 0.5-1：1.
6. such as claim 2-5 any one of them aeroge-diatomite multiple stage filtration system, it is characterised in that：The acid is
One kind in the hydrochloric acid of a concentration of 1-2mol/L, sulfuric acid, organic acid；And/or
Hydrolysis obtains the condition of colloidal sol and is in the water-bath：Temperature：60-80 DEG C, the time：1-2h；And/or
It is 45-48h that ageing time is stood in the water-bath；And/or
The non-polar organic solvent is one kind in n-hexane, hexamethylene, normal heptane；And/or
The volume ratio of the non-polar organic solvent and wet gel is 3-10:1；And/or
The time swap is 23-24h；And/or
The drying condition is：30-60 DEG C, 24-48h.
7. aeroge as described in any one in claim 1-5-diatomite multiple stage filtration system, it is characterised in that：The diatom
Native filter aid calcines 2-5h using diatomite as raw material at 500 DEG C, and 2-4h is then impregnated in lye, and adjustment pH value is 6-7.
8. aeroge as claimed in claim 7-diatomite multiple stage filtration system, it is characterised in that：The diatomite：Purity
＞ 99%, grain diameter≤200 μm；And/or
The concentration of lye is 0.08-0.12mol/L；And/or
PH value is adjusted using the HCl of 0.1~1mol/L.
9. aeroge as described in any one in claim 1-5-diatomite multiple stage filtration system, it is characterised in that：The filter core
Using PE sintered filter cores；And/or
The SiO2The thickness of aeroge and super-cell ratio is 1:5-5:1；And/or
The shell further includes absorbing devices.
10. if claim 1-9 any one of them aeroge-diatomite multiple stage filtration system is in processing waste liquid of drilling field
Application.
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Cited By (1)
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| CN114481148A (en) * | 2022-02-15 | 2022-05-13 | 南通宝正环保科技有限公司 | Recycling process of stainless steel waste acid |
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