CN108889283A - A kind of aerogel type calcium ions and magnesium ions adsorbent material preparation method - Google Patents

A kind of aerogel type calcium ions and magnesium ions adsorbent material preparation method Download PDF

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Publication number
CN108889283A
CN108889283A CN201810775121.1A CN201810775121A CN108889283A CN 108889283 A CN108889283 A CN 108889283A CN 201810775121 A CN201810775121 A CN 201810775121A CN 108889283 A CN108889283 A CN 108889283A
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zsof
porous
preparation
aerogel
adsorbent
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张毅
刘伟
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Yang Chengfeiyang
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Yang Chengfeiyang
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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
    • 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
    • B01J20/28002—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 physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00—Controlling or monitoring parameters in water treatment
    • C02F2209/05—Conductivity or salinity
    • C02F2209/055—Hardness

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Hydrology & Water Resources (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a kind of aerogel type calcium ions and magnesium ions adsorbent material preparation methods,Tetraethyl orthosilicate,Silica solution,NaOH,Polyacrylamide,Isopropanol,Tetrabutyl ammonium fluoride,N-hexane,Phenyl triethoxysilane,ZSOF porous nanometer material 1,5- cyclo-octadiene,Double 1,5- cyclo-octadiene nickel and 2,2'- bipyridyl is primary raw material,Using microemulsion as precursor,Low cost,The method for quickly preparing aeroge adsorbent and its composite material,Microemulsion is the transparent and homogeneous that two kinds of non soluble liquids spontaneously form under surfactant and cosurfactant effect,Thermodynamically stable dispersion,The water softening ZSOF porous aerogel ion adsorbent of preparation,Raw material is easy to get,Simple process is easy to operate,It is without secondary pollution,Significantly improve the bating effect to hardness of porous nanometer material.

Description

A kind of aerogel type calcium ions and magnesium ions adsorbent material preparation method
Technical field
The present invention relates to a kind of preparation methods of aerogel type calcium ions and magnesium ions adsorbent material, belong to water treatment field.
Background technique
The domestic water of our daily uses can be classified as soft water and hard water.Soft water such as distilled water is also referred to as drunk With water, main component is hydrogen and oxygen, relatively pure, feels soft since its hardness is low, and hard water such as underground water, containing calcium from Son and magnesium ion feel hard due to its high rigidity as its main component.Nowadays, it is supplied to most of families, office etc. Tap water be the hard water with high rigidity, not only contain the chlorine used in tap water purifying process, but also containing certain Heavy metal ion of amount, such as iron ion, copper ion, tin ion, zinc ion, mercury ion etc., they may be due to environmental pollution Aging with water pipe and generate.Although it is fatefulue that these heavy metal ion are not to human body, it is known that in heavy metal When ion is in conjunction with fatty acid, the exogenous material for causing to accelerate skin aging and skin disease such as allergic disease will be generated. In this case, hard water such as tap water is converted to soft water, and it is used extensively by the material for inventing a kind of demineralized water The method for making to obtain the most convenient of high-quality life water in family, office etc..
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of aerogel type calcium ions and magnesium ions adsorbent material, pass through this method The material of preparation has excellent adsorption of metal ions effect.
A kind of aerogel type calcium ions and magnesium ions adsorbent material preparation method, this approach includes the following steps：
Step 1 measures 60ml tetraethyl orthosilicate, and 20ml silica solution, it is poly- that high-speed stirred while sequentially adds 1.5gNaOH, 3g Acrylamide, 10ml isopropanol and 15ml deionized water, temperature are maintained at 50 DEG C, and ultrasonic disperse obtains transparent micro emulsion；
2g tetrabutyl ammonium fluoride, 30g n-hexane and 20g phenyl triethoxysilane are added into above-mentioned mixed liquor for step 2, high After speed stirring, ultrasonic treatment is until solution becomes semigel；
Step 3 takes 50gZSOF porous nanometer material to be placed in ready mold, then that above-mentioned gained semigel is uniform Mold is poured into, until ZSOF porous nanometer material is saturated with liquid, die cover plate is covered, prevents from volatilizing, stands after forty minutes, is formed The gel rubber material of one fiber composite of inorganic additive；
Gel rubber material is placed in aging 5h in 60 DEG C of ethyl alcohol by step 4, and ethyl alcohol volume is 5 times of gel rubber material volume；Aging is completed Afterwards, gel rubber material is put into carbon dioxide supercritical extraction kettle, setting pressure 12Mpa, temperature 50 C, after dry 6h, heat preservation Decompression, finally obtains enhanced fiber composite ZSOF porous aerogel ion adsorbent.
The ZSOF porous nanometer material preparation method is as follows：
9.6mmol 1,5- cyclo-octadiene is added to the bis- 1,5- cyclo-octadiene nickel of 9.6mmol and 4.8mmol2,2'- by step 1 In the flask of the anhydrous toluene solution 100ml of bipyridyl；
Step 2 ,/80 DEG C of heating and 1 hour of constant temperature, obtain the toluene solution of purple；
1mmol eight is added into the toluene solution of purple obtained above for step 3（Align iodine substituted phenyl）Odaaps（{p- IC6H4SiO1.5}8）, it is stirred to react in 80 DEG C overnight, reaction obtains navy blue suspension；
After the navy blue suspension that step 3 obtains is cooled to room temperature, 50ml acetic acid is added in step 4, stirs 12 hours and mistake Filter, product use water respectively（5 times × 30ml）, ethyl alcohol（5 times × 30ml）And chloroform（5 times × 30ml）Processing, 100 DEG C of vacuum drying After obtain ZSOF porous nanometer material.
Beneficial effect：Water softening ZSOF porous aerogel ion adsorbent prepared by the present invention, using microemulsion as precursor, Low cost, the method for quickly preparing aeroge adsorbent and its composite material, microemulsion is two kinds of non soluble liquids on surface Transparent and homogeneous, the thermodynamically stable dispersion spontaneously formed under activating agent and cosurfactant effect, so that ZSOF is more Hole nano material is enclosed with layer of surface activating agent, and has certain condensed state structure, creates chemistry for adsorbing metal ions Activity and space, to significantly improve the bating effect to hardness of porous nanometer material.
Specific embodiment
Embodiment 1
A kind of aerogel type water softening preparation method of nano material, it is characterised in that this approach includes the following steps：
Step 1 measures 60ml tetraethyl orthosilicate, and 20ml silica solution, it is poly- that high-speed stirred while sequentially adds 1.5gNaOH, 3g Acrylamide, 10ml isopropanol and 15ml deionized water, temperature are maintained at 50 DEG C, and ultrasonic disperse obtains transparent micro emulsion；
2g tetrabutyl ammonium fluoride, 30g n-hexane and 20g phenyl triethoxysilane are added into above-mentioned mixed liquor for step 2, high After speed stirring, ultrasonic treatment is until solution becomes semigel；
Step 3 takes 50gZSOF porous nanometer material to be placed in ready mold, then that above-mentioned gained semigel is uniform Mold is poured into, until ZSOF porous nanometer material is saturated with liquid, die cover plate is covered, prevents from volatilizing, stands after forty minutes, is formed The gel rubber material of one fiber composite of inorganic additive；
Gel rubber material is placed in aging 5h in 60 DEG C of ethyl alcohol by step 4, and ethyl alcohol volume is 5 times of gel rubber material volume；Aging is completed Afterwards, gel rubber material is put into carbon dioxide supercritical extraction kettle, setting pressure 12Mpa, temperature 50 C, after dry 6h, heat preservation Decompression, finally obtains enhanced fiber composite ZSOF porous aerogel ion adsorbent.
The ZSOF porous nanometer material preparation method is as follows：
9.6mmol 1,5- cyclo-octadiene is added to the bis- 1,5- cyclo-octadiene nickel of 9.6mmol and 4.8mmol2,2'- by step 1 In the flask of the anhydrous toluene solution 100ml of bipyridyl；
Step 2 ,/80 DEG C of heating and 1 hour of constant temperature, obtain the toluene solution of purple；
1mmol eight is added into the toluene solution of purple obtained above for step 3（Align iodine substituted phenyl）Odaaps（{p- IC6H4SiO1.5}8）, it is stirred to react in 80 DEG C overnight, reaction obtains navy blue suspension；
After the navy blue suspension that step 3 obtains is cooled to room temperature, 50ml acetic acid is added in step 4, stirs 12 hours and mistake Filter, product use water respectively（5 times × 30ml）, ethyl alcohol（5 times × 30ml）And chloroform（5 times × 30ml）Processing, 100 DEG C of vacuum drying After obtain ZSOF porous nanometer material.
Embodiment 2
Step 1 measures 50ml tetraethyl orthosilicate, and 20ml silica solution, it is poly- that high-speed stirred while sequentially adds 1.5gNaOH, 3g Acrylamide, 10ml isopropanol and 15ml deionized water, temperature are maintained at 50 DEG C, and ultrasonic disperse obtains transparent micro emulsion；Remaining Preparation and embodiment 1 are identical.
Embodiment 3
Step 1 measures 40ml tetraethyl orthosilicate, and 20ml silica solution, it is poly- that high-speed stirred while sequentially adds 1.5gNaOH, 3g Acrylamide, 10ml isopropanol and 15ml deionized water, temperature are maintained at 50 DEG C, and ultrasonic disperse obtains transparent micro emulsion；Remaining Preparation and embodiment 1 are identical.
Embodiment 4
Step 1 measures 30ml tetraethyl orthosilicate, and 20ml silica solution, it is poly- that high-speed stirred while sequentially adds 1.5gNaOH, 3g Acrylamide, 10ml isopropanol and 15ml deionized water, temperature are maintained at 50 DEG C, and ultrasonic disperse obtains transparent micro emulsion；Remaining Preparation and embodiment 1 are identical.
Embodiment 5
Step 1 measures 20ml tetraethyl orthosilicate, and 20ml silica solution, it is poly- that high-speed stirred while sequentially adds 1.5gNaOH, 3g Acrylamide, 10ml isopropanol and 15ml deionized water, temperature are maintained at 50 DEG C, and ultrasonic disperse obtains transparent micro emulsion；Remaining Preparation and embodiment 1 are identical.
Embodiment 6
Step 1 measures 10ml tetraethyl orthosilicate, and 20ml silica solution, it is poly- that high-speed stirred while sequentially adds 1.5gNaOH, 3g Acrylamide, 10ml isopropanol and 15ml deionized water, temperature are maintained at 50 DEG C, and ultrasonic disperse obtains transparent micro emulsion；Remaining Preparation and embodiment 1 are identical.
Embodiment 7
Step 1 measures 60ml tetraethyl orthosilicate, and 15ml silica solution, it is poly- that high-speed stirred while sequentially adds 1.5gNaOH, 3g Acrylamide, 10ml isopropanol and 15ml deionized water, temperature are maintained at 50 DEG C, and ultrasonic disperse obtains transparent micro emulsion；Remaining Preparation and embodiment 1 are identical.
Embodiment 8
Step 1 measures 60ml tetraethyl orthosilicate, and 10ml silica solution, it is poly- that high-speed stirred while sequentially adds 1.5gNaOH, 3g Acrylamide, 10ml isopropanol and 15ml deionized water, temperature are maintained at 50 DEG C, and ultrasonic disperse obtains transparent micro emulsion；Remaining Preparation and embodiment 1 are identical.
Embodiment 9
Step 1 measures 60ml tetraethyl orthosilicate, 20 ml silica solution, and high-speed stirred while sequentially adds 5g modified Nano leech Mountain flour, 1.5gNaOH, 3g polyacrylamide, 10ml isopropanol and 15ml deionized water, temperature are maintained at 50 DEG C, and ultrasonic disperse obtains To transparent micro emulsion；Remaining preparation and embodiment 1 are identical.
The modified Nano vermiculite powder, preparation method thereof is as follows：
By 10 parts of methylcellulose, 15 parts of neopelexes are dissolved in 60 parts of deionized waters, are sufficiently stirred with glass bar It mixes and uniformly obtains dispersant solution, then pour into 80 parts of vermiculites in ball grinder, and the solution previously prepared is added, use glass bar It stirs evenly, is put into planetary mills and carries out ball milling, planetary mills revolving speed is 200r/min, and product is poured into glass dish after ball milling In, and place it in vacuum oven and be dried, temperature is 70 DEG C, until drying, finally by the product of drying It is crushed with pulverizer to obtain modified Nano vermiculite power.
Embodiment 10
Step 1 measures 60ml tetraethyl orthosilicate, and 5ml silica solution, it is poly- that high-speed stirred while sequentially adds 1.5gNaOH, 3g Acrylamide, 10ml isopropanol and 15ml deionized water, temperature are maintained at 50 DEG C, and ultrasonic disperse obtains transparent micro emulsion；Remaining Preparation and embodiment 1 are identical.
Reference examples 1
It is with 1 difference of embodiment：In the step 1 of porous aerogel ion adsorbent preparation, NaOH is not added, remaining step Suddenly identical with embodiment 1.
Reference examples 2
It is with 1 difference of embodiment：In the step 1 of porous aerogel ion adsorbent preparation, polyacrylamide is not added, Remaining step is identical with embodiment 1.
Reference examples 3
It is with 1 difference of embodiment：In the step 2 of porous aerogel ion adsorbent preparation, 25gZSOF porous nano material is taken Material is placed in ready mold, remaining step is identical with embodiment 1.
Reference examples 4
It is with 1 difference of embodiment：In the step 2 of porous aerogel ion adsorbent preparation, 5gZSOF porous nano material is taken It is identical with embodiment 1 that material is placed in remaining step in ready mold.
Reference examples 5
It is with 1 difference of embodiment：In the step 3 of porous aerogel ion adsorbent preparation, gel rubber material is put into dioxy Change in carbon supercritical extraction reactor, setting pressure 6Mpa, temperature 50 C, remaining step is identical with embodiment 1.
Reference examples 6
It is with 1 difference of embodiment：In the step 3 of porous aerogel ion adsorbent preparation, gel rubber material is put into dioxy Change carbon supercritical extraction reactor in, be arranged pressure 12Mpa, 90 DEG C of temperature, remaining step is identical with embodiment 1.
Reference examples 7
It is with 1 difference of embodiment：In the step 1 of ZSOF porous nanometer material preparation, by 4.8mmol 1,5- cyclo-octadiene It is added to the flask of the anhydrous toluene solution 100ml of the bis- 1,5- cyclo-octadiene nickel of 9.6mmol and 4.8mmol2,2'- bipyridyl In, remaining step is identical with embodiment 1.
Reference examples 8
It is with 1 difference of embodiment：In the step 1 of ZSOF porous nanometer material preparation, by 9.6mmol 1,5- cyclo-octadiene It is added to the flask of the anhydrous toluene solution 100ml of the bis- 1,5- cyclo-octadiene nickel of 4.8mmol and 4.8mmol2,2'- bipyridyl In, remaining step is identical with embodiment 1.Reference examples 9
It is with 1 difference of embodiment：In the step 1 of ZSOF porous nanometer material preparation, 1,5- cyclo-octadiene is not added, Remaining step is identical with embodiment 1.
Reference examples 10
It is with 1 difference of embodiment：In the step of prepared by ZSOF porous nanometer material, double 1,5- cyclo-octadiene are not added Nickel, remaining step are identical with embodiment 1.
It chooses the nanocomposite being prepared and carries out hardness determination, foundation respectively《Drinking water standard method of inspection》 GB5750-85, testing result reflect that the hardness of water refers to the concentration of calcium ion in water, magnesium ion, hardness list by the hardness of water Position is ppm, and 1ppm represents calcium carbonate content 1mg/L in water.Test sample water hardness is 320ppm.
The inspection result tested before and after water demineralization
The experimental results showed that ZSOF porous aerogel ion adsorbent provided by the invention has good water demineralization effect, material For material under standard test condition, the removal rate of metal ion is higher, it is better to illustrate bating effect, conversely, effect is poorer；Implement Example 1 arrives embodiment 10, changes the proportion of each raw material composition in adsorbent material respectively, has different journeys to the softening performance of material The influence of degree is 3 in tetraethyl orthosilicate, silica solution volume proportion：1, when other ingredient dosages are fixed, softening performance and metal Ion remaval effect is best；It is worth noting that modified Nano vermiculite power is added in embodiment 9, removal effect is significantly improved, explanation Modified Nano vermiculite power has better optimization function to the ionic adsorption performance of filling-material structure；Reference examples 1 no longer add to reference examples 2 Enter NaOH and polyacrylamide, removal effect is decreased obviously, and illustrates that NaOH and polyacrylamide are critically important to materials synthesis；Control Example 3 reduces the dosage of ZSOF porous nanometer material, effect is obviously deteriorated to reference examples 4；Reference examples 5 change dioxy to reference examples 6 Change the pressure and temperature of carbon supercritical extract, effect is also bad, illustrates absorption of the state modulator to composite material of extraction process Modification plays an important role；Reference examples 7 to reference examples 10 change the proportion and composition of ZSOF porous nanometer material primary raw material, effect Fruit is substantially reduced, and it is very big to illustrate that the synthesis of ZSOF can be influenced by raw material composition；Therefore the porous gas of ZSOF prepared by the present invention is used Gelular ion adsorbent has excellent water demineralization effect.

Claims (2)

1. a kind of aerogel type calcium ions and magnesium ions adsorbent material preparation method, it is characterised in that this approach includes the following steps：
Step 1 measures 60ml tetraethyl orthosilicate, and 20ml silica solution, it is poly- that high-speed stirred while sequentially adds 1.5gNaOH, 3g Acrylamide, 10ml isopropanol and 15ml deionized water, temperature are maintained at 50 DEG C, and ultrasonic disperse obtains transparent micro emulsion；
2g tetrabutyl ammonium fluoride, 30g n-hexane and 20g phenyl triethoxysilane are added into above-mentioned mixed liquor for step 2, high After speed stirring, ultrasonic treatment is until solution becomes semigel；
Step 3 takes 50gZSOF porous nanometer material to be placed in ready mold, then that above-mentioned gained semigel is uniform Mold is poured into, until ZSOF porous nanometer material is saturated with liquid, die cover plate is covered, prevents from volatilizing, stands after forty minutes, is formed The gel rubber material of one fiber composite of inorganic additive；
Gel rubber material is placed in aging 5h in 60 DEG C of ethyl alcohol by step 4, and ethyl alcohol volume is 5 times of gel rubber material volume；Aging is completed Afterwards, gel rubber material is put into carbon dioxide supercritical extraction kettle, setting pressure 12Mpa, temperature 50 C, after dry 6h, heat preservation Decompression, finally obtains enhanced fiber composite ZSOF porous aerogel ion adsorbent.
2. a kind of preparation method of aerogel type calcium ions and magnesium ions adsorbent material according to claim 1, it is characterised in that it states,
The ZSOF porous nanometer material preparation method is as follows：
9.6mmol 1,5- cyclo-octadiene is added to the bis- 1,5- cyclo-octadiene nickel of 9.6mmol and 4.8mmol2,2'- by step 1 In the flask of the anhydrous toluene solution 100ml of bipyridyl；
Step 2 ,/80 DEG C of heating and 1 hour of constant temperature, obtain the toluene solution of purple；
{ p-IC is added into the toluene solution of purple obtained above for step 36H4SiO1.5}8, it is stirred to react in 80 DEG C overnight, Reaction obtains navy blue suspension；
After the navy blue suspension that step 3 obtains is cooled to room temperature, 50ml acetic acid is added in step 4, stirs 12 hours and mistake Filter, product use water, ethyl alcohol and the processing of chloroform cleaning treatment respectively, obtain ZSOF porous nanometer material after 100 DEG C of vacuum drying.
CN201810775121.1A 2018-07-16 2018-07-16 A kind of aerogel type calcium ions and magnesium ions adsorbent material preparation method Pending CN108889283A (en)

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Application Number Priority Date Filing Date Title
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