CN109437211B - A kind of high-specific surface area and high absorption VOC type silica and preparation method thereof - Google Patents
A kind of high-specific surface area and high absorption VOC type silica and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to silica technical fields, and in particular to a kind of high-specific surface area and high absorption VOC type silica and preparation method thereof.Preparation method of the present invention includes S1, injects sulfuric acid solution into reactor tank, is stirred under room temperature, adds ZSM-5 type zeolite molecular sieve, continues to stir；Continue under S2, stirring be added dropwise sodium silicate solution, be added dropwise to system pH be 4.8~5.0 when, reduce rate of addition, control endpoint pH be 5.4~5.7, stop be added dropwise sodium silicate solution, continue stirring form thick gel to solution after, it is static；S3, after taking out thick gel, moisture is discharged with suction filtration machine, is dried, taken out broken, washing, drying, silica is made.The method of the present invention step is simple, and condition is controllable, and process stabilizing, production cost is low, is suitble to industrialized production, and product is significant to VOC clean-up effect, is with a wide range of applications.
Description
Technical field
The invention belongs to silica technical fields, and in particular to a kind of high-specific surface area and high absorption VOC type titanium dioxide
Silicon and preparation method thereof.
Background technique
In recent years, with the continuous improvement of living standards, the continuous improvement of living conditions, people increasingly focus on volatilizable
Property organic compound (Volatile Organic Compouds, VOC) pollution problem.Conventional VOC purification method is mainly wrapped
It includes: absorption process, absorption method, catalysis method, combustion method, condensation method, bioanalysis etc..Compared with other methods, absorption method has low dirt
The features such as contaminating, be efficient, economical and practical.Currently used porous adsorbent includes diatomite, active carbon, bentonite and silica
Deng, and silica adsorbent has the characteristics that nontoxic, tasteless, pollution-free, hydrodynamic performance is good, high mechanical strength, thus
It is widely used.
Currently, the most apparent density of traditional silica product is low, reference area and internal holes are small in size, are unfavorable for using
In absorption VOC gas.And the silica used as adsorbent mostly uses greatly the organosilicons such as silester as silicon source, although making
Reference area is obtained to be promoted, but pore volume is smaller, it is unobvious to the adsorption effect of VOC gas, and preparation method is cumbersome, at
This is high, is unfavorable for actual production and popularization and use.And the precipitation method using sodium metasilicate as silicon source are relatively easy, and energy consumption
It is small, at low cost, it is easy to industrialize, but in the method, the character of silica is easy to be influenced by preparation condition.
Such as patent document CN107324346A discloses a kind of preparation side of high-specific surface area high oil absorption value silica
Method, this method includes S1, into reaction kettle, implantation concentration is 6~10m of metabisulfite solution of 0.8~1.5mol/L3, it is heated to 70
~90 DEG C；S2, the sulfuric acid solution that concentration is 3.0~5.0mol/L is added, the flow velocity of the sulfuric acid solution is 1.5~2.5m3/ h,
Then with 10~15m3Water glass solution is added in the speed of/h, and the flow velocity for adjusting sulfuric acid solution is 1.5~2.5m3/ h, with control
The pH value of reaction process is 5.5~6.5, and after cocurrent reacts 10~20min, the flow velocity for adjusting sulfuric acid solution is 1.0~2.0m3/
H, the pH value for controlling reaction process is 8.5~9.5, and cocurrent reacts 10~20min；The pH of the reaction end of S3, regulating step S2
Value is 7.0, is 70~90 DEG C in temperature, after 10~30min of the lower ageing reaction of stirring, filters pressing, and washing, removing sulfate, dry,
Crush to get.The specific surface area of silica made from this method is greater than 475.45m2/ g, oil factor are greater than 322ml/100g,
Surfactant load capacity with higher.But this method needs the high temperature at 70~90 DEG C to carry out, and energy consumption is high, is unfavorable for
Industrialization.
For another example patent document CN105129806A discloses a kind of preparation side of washing powder high specific surface area silica
Method, this method include S1, water are added into reactor tank, are heated to 65~75 DEG C, glycerol is then added, stir evenly；S2,
Waterglass and sulfuric acid is added simultaneously, stops adding sulfuric acid when system pH is 2.0~3.0, is aged 1.5~2.5h；S3, it will be aged
Rear silica batch carry out pressure filtration washing, it is dry it is broken to get.The specific surface area that silica is made in this method is 600
~700m22.8~3.0cm of/g, Kong Rongwei3/ g, aperture are 16~20nm.Specific surface area, pore volume and the aperture of the silica
It is larger, but it is bad to the adsorption effect of VOC in practical application, this is because capillary occurs in intermediary hole (12~50nm)
Condense phenomenon, adsorption capacity is caused to weaken；This method also needs to heat simultaneously, and energy consumption is high, it is also necessary to use glycerol as helping
Agent.
Therefore, existing high specific surface area silica is limited to the adsorption effect of VOC, and preparation method energy consumption is high,
At high cost, therefore be badly in need of researching and developing a kind of simple process, low in cost, large specific surface area, pore volume and aperture are moderate and adsorb to VOC
Effective silica product is to meet the market demand.
Summary of the invention
In order to solve the problems in the existing technology (such as process energy consumption is big, at high cost, adsorption effect of the product to VOC
Difference etc.), the present invention provides the preparation method of a kind of high-specific surface area and high absorption VOC type silica, which exists
It is carried out under room temperature, the reactive mode of acid, compound ZSM-5 type zeolite molecular sieve, and strict control reaction mass is added dropwise using alkali
The conditions such as concentration, charging rate and pH value, high-specific surface area and high absorption VOC type silica is made.
The preparation method of high-specific surface area provided by the invention and high absorption VOC type silica, specifically includes following step
It is rapid:
S1,1.5~2.5m of sulfuric acid solution is injected into reactor tank3, stir under room temperature, add ZSM-5 type zeolite molecules
Sieve, continues 10~20min of stirring；
Continue that sodium silicate solution is added dropwise under S2, stirring, control rate of addition is 0.4~0.6m3/ h, is added dropwise to system pH
When being 4.8~5.0, reduce rate of addition to 0.02~0.03m3/ h, control endpoint pH are 5.4~5.7, stop that silicic acid is added dropwise
Sodium solution, continue stirring form thick gel to solution after, static 80~120min；
S3, after taking out thick gel, moisture is discharged with suction filtration machine, is placed in 8~12h of drying at 90~120 DEG C, then
Taking-up is crushed, is washed, is dried, and high-specific surface area and high absorption VOC type silica is made.
Further, the concentration of the sulfuric acid solution is 0.3~0.4mol/L.
Further, the speed of the stirring is 30~40Hz.
Further, the additional amount of the ZSM-5 type zeolite molecular sieve is 12~27kg.
Further, the silica alumina ratio of the ZSM-5 type zeolite molecular sieve is greater than 300, and specific surface area is greater than 300m2/
G, partial size are 5~20 μm.
Further, the concentration of the sodium silicate solution is 0.6~0.8mol/L, the modulus of the sodium metasilicate is 3.0~
3.5。
Correspondingly, the present invention also provides the preparation methods by above-mentioned high-specific surface area and high absorption VOC type silica
Silica obtained, 360~420m of specific surface area of the silica2/ g, 0.6~2.0cm of pore volume3/ g, aperture 7~
10nm, purified concentrations are 2mg/m at 35 DEG C3Purifying rate >=90% of toluene, clean-up effect is significant, has wide range of applications.
Of the invention the reaction mechanism is as follows: the present invention is reaction bottom liquid with dilute sulfuric acid, and a certain amount of sial ZSM-5 type is added
Zeolite molecular sieve is stirred until homogeneous, then certain density waterglass is added dropwise at normal temperature and is stirred to react, by controlling terminal pH
Value makes product form gel, finally by gel by filters pressing, drying, broken, sieving, wash and etc. after Gao Bibiao can be obtained
Area and high absorption VOC silica.
More specifically, the present invention uses the lower 0.3~0.4mol/L sulfuric acid solution of concentration and 0.6~0.8mol/L silicic acid
Sodium solution is reacted, and is reacted by the way of alkali is added dropwise toward acid.Because of in an acidic solution, the coordination of silicic acid molecule
Number is 6, and silicic acid molecule and positive monovalence silicate ion carry out hydroxyl connection reaction at this time, forms double silicic acid, by double silicic acid, three silicic acid, more
Silicic acid polymerize always just forms silica solution, until forming Silica hydrogel.Silica solution in gel process, further grow by particle
Greatly, as SiO in colloidal sol2Content when being more than a certain amount of, these primary particles mutually condenses that formation is open and continuous gel net
Network structure, particle discontinuously can be condensed to form Si-O-Si key in this gel, and system is made to have certain rigidity.And low concentration
Acid reacted with alkali and can effectively extend the reaction time, carry out fully reacting, and enable be nucleated particle sufficiently grow up, have
Biggish pore volume further increases its specific surface area.
Secondly, the present invention mixes the ZSM-5 type zeolite molecular sieve that silica alumina ratio is greater than 300, incorporation 10% before the reaction
~20%, because the basic unit in skeleton structure of zeolite is the four sides made of piling up with 1 silicon or aluminium atom as 4 oxygen originals
Body, therefore there is very big cavity structure, water or gas molecule can be adsorbed, and Si is former in the zeolite molecular sieve skeleton of ZSM-5 type
When son is replaced by Al atom, zeolite skeleton will have a negative electrical charge, this negative electrical charge by the unit price that is in outside skeleton or multivalence sun from
Son compensates, and showing on absorption property has higher affinity to polar molecule, for molecule similar in size, polarity is got over
It is big then easier adsorbed by molecular sieve.Gas in VOC contains polar bond mostly, such as: OH- ,=CO2、-NH4It can be given with some
Polarized molecule is (such as=C=C <, C6H5), therefore addition zeolite can effectively adsorb VOC.And the present invention selects silica alumina ratio big
It is in the reason of 300 zeolite, in the structure of zeolite, as skeleton structure of zeolite is desorbed in aluminium atom, so that zeolite surface
Micro pore volume and specific surface area increase, the diameter of the VOC in air is in 0.2~0.6nm, and zeolite pore is in 2nm, absorption
VOC is mainly by micro-porous adsorption, and the increase of micro pore volume can effectively increase the adsorbance of VOC.Meanwhile the mixed ratio of zeolite
When greater than 20%, product hardness is relatively low, easily formation powder, is unfavorable for production application.Therefore, when zeolite mixed ratio is
When 10%~20%, product had not only had preferable adsorption capacity but also had had certain hardness.
Finally, the flow velocity of control reaction mass is lower than 0.6m3/ h and endpoint pH are 5.4~5.7, when can extend reaction
Between, so that material is sufficiently reacted and is grown up, and specific surface area with higher and biggish micro pore volume, to improve product pair
The absorption property of VOC.
Therefore, compared with prior art, present invention has an advantage that
(1) preparation method of high-specific surface area of the present invention and high absorption VOC type silica carries out at normal temperature, without making
Used additives can be prepared by the silica that specific surface area is high, VOC absorption property is strong, and step is simple, and condition is controllable, and technique is steady
Fixed, production cost is low, is suitble to industrialized production.
(2) 360~420m of specific surface area of high-specific surface area of the present invention and high absorption VOC type silica2/ g, pore volume
0.6~2.0cm3/ g, 7~10nm of aperture, purified concentrations are 2mg/m at 35 DEG C3Purifying rate >=90% of toluene purifies VOC
Significant effect, and have certain hardness, it is with a wide range of applications.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
The raw materials used present invention is conventional commercial commodity, such as ZSM-5 type zeolite molecular sieve to create chemical industry together purchased from Zibo
Science and Technology Development Co., Ltd., trade name micron order ZSM-5 molecular sieve.
Embodiment 1, high-specific surface area of the present invention and high absorption VOC type silica and preparation method thereof
S1, into reactor tank, implantation concentration is the sulfuric acid solution 1.5m of 0.3mol/L3, it stirs under room temperature (20~30 DEG C),
ZSM-5 type zeolite molecular sieve 12kg is added, continues to stir 10min；
Continue under S2, stirring be added dropwise modulus be 3.0, the sodium silicate solution that concentration is 0.6mol/L, control rate of addition be
0.4m3/ h reduces rate of addition to 0.02m when to be added dropwise to system pH be 4.83/ h, control endpoint pH are 5.4, stop drop
Add sodium silicate solution, continue stirring form thick gel to solution after, static 80min；
S3, after taking out thick gel, moisture is discharged with suction filtration machine, is placed at 90 DEG C and dries 12h, further takes out progress
It is broken, take the oversize sample of partial size greater than 710 microns into product to be less than with 25 mesh sieving extracting screen underflow and with the sieving of 140 mesh
5%, sample of the partial size less than 45 microns is less than less than 2%, then by the product after sieving with originally water washing to sodium sulphate content
4%, taking-up is placed in 100 DEG C of baking ovens after drying, and high-specific surface area and high absorption VOC type silica is made.
The speed of the stirring is 30Hz；The silica alumina ratio of the ZSM-5 type zeolite molecular sieve is greater than 300, specific surface
Product is greater than 300m2/ g, partial size are 5~20 μm.
Embodiment 2, high-specific surface area of the present invention and high absorption VOC type silica and preparation method thereof
S1, into reactor tank, implantation concentration is the sulfuric acid solution 2.5m of 0.4mol/L3, it stirs under room temperature (20~30 DEG C),
ZSM-5 type zeolite molecular sieve 27kg is added, continues to stir 20min；
Continue under S2, stirring be added dropwise modulus be 3.5, the sodium silicate solution that concentration is 0.8mol/L, control rate of addition be
0.6m3/ h reduces rate of addition to 0.03m when to be added dropwise to system pH be 5.03/ h, control endpoint pH are 5.7, stop drop
Add sodium silicate solution, continue stirring form thick gel to solution after, static 120min；
S3, after taking out thick gel, moisture is discharged with suction filtration machine, is placed at 120 DEG C and dries 8h, further takes out progress
It is broken, take the oversize sample of partial size greater than 710 microns into product to be less than with 25 mesh sieving extracting screen underflow and with the sieving of 140 mesh
5%, sample of the partial size less than 45 microns is less than less than 2%, then by the product after sieving with originally water washing to sodium sulphate content
4%, taking-up is placed in 100 DEG C of baking ovens after drying, and high-specific surface area and high absorption VOC type silica is made.
The speed of the stirring is 40Hz；The silica alumina ratio of the ZSM-5 type zeolite molecular sieve is greater than 300, specific surface
Product is greater than 300m2/ g, partial size are 5~20 μm.
Embodiment 3, high-specific surface area of the present invention and high absorption VOC type silica and preparation method thereof
S1, into reactor tank, implantation concentration is the sulfuric acid solution 2.0m of 0.32mol/L3, it stirs under room temperature (20~30 DEG C),
ZSM-5 type zeolite molecular sieve 23kg is added, continues to stir 15min；
Continue under S2, stirring be added dropwise modulus be 3.2, the sodium silicate solution that concentration is 0.7mol/L, control rate of addition be
0.5m3/ h reduces rate of addition to 0.02m when to be added dropwise to system pH be 5.03/ h, control endpoint pH are 5.5, stop drop
Add sodium silicate solution, continue stirring form thick gel to solution after, static 90min；
S3, by thick gel take out after, moisture is discharged with suction filtration machine, is placed at 100 DEG C and dries 10h, further take out into
Row is broken, takes oversize partial size into product small greater than 710 microns of sample with 25 mesh sieving extracting screen underflow and with the sieving of 140 mesh
In 5%, sample of the partial size less than 45 microns is small to sodium sulphate content with originally water washing less than 2%, then by the product after sieving
In 4%, taking-up is placed in 100 DEG C of baking ovens after drying, and high-specific surface area and high absorption VOC type silica is made.
The speed of the stirring is 35Hz；The silica alumina ratio of the ZSM-5 type zeolite molecular sieve is greater than 300, specific surface
Product is greater than 300m2/ g, partial size are 5~20 μm.
Embodiment 4, high-specific surface area of the present invention and high absorption VOC type silica and preparation method thereof
S1, into reactor tank, implantation concentration is the sulfuric acid solution 1.5m of 0.4mol/L3, it stirs under room temperature (20~30 DEG C),
ZSM-5 type zeolite molecular sieve 23kg is added, continues to stir 15min；
Continue under S2, stirring be added dropwise modulus be 3.2, the sodium silicate solution that concentration is 0.8mol/L, control rate of addition be
0.4m3/ h reduces rate of addition to 0.02m when to be added dropwise to system pH be 5.03/ h, control endpoint pH are 5.4, stop drop
Add sodium silicate solution, continue stirring form thick gel to solution after, static 120min；
S3, by thick gel take out after, moisture is discharged with suction filtration machine, is placed at 100 DEG C and dries 10h, further take out into
Row is broken, takes oversize partial size into product small greater than 710 microns of sample with 25 mesh sieving extracting screen underflow and with the sieving of 140 mesh
In 5%, sample of the partial size less than 45 microns is small to sodium sulphate content with originally water washing less than 2%, then by the product after sieving
In 4%, taking-up is placed in 100 DEG C of baking ovens after drying, and high-specific surface area and high absorption VOC type silica is made.
The speed of the stirring is 30Hz；The silica alumina ratio of the ZSM-5 type zeolite molecular sieve is greater than 300, specific surface
Product is greater than 300m2/ g, partial size are 5~20 μm.
Comparative example 1
Compared with Example 3, difference of the invention is only that: the concentration of the sulfuric acid solution is 0.7mol/L.
Comparative example 2
Compared with Example 3, difference of the invention is only that: the concentration of the sodium silicate solution is 1.2mol/L.
Comparative example 3
Compared with Example 3, difference of the invention is only that: continue under S2, stirring be added dropwise modulus be 3.2, concentration is
The sodium silicate solution of 0.7mol/L, control rate of addition are 0.8m3/ h, be added dropwise to system pH be 5.0 when, reduce rate of addition
To 0.07m3/ h, control endpoint pH are 5.5, stop that sodium silicate solution is added dropwise, and continue stirring to solution and form thick gel
Afterwards, static 90min.
Comparative example 4
Compared with Example 3, difference of the invention is: change the addition manner of material, specifically:
S1, concentration is taken to be the sulfuric acid solution 2.0m of 0.32mol/L3, ZSM-5 type zeolite molecular sieve 23kg is added, under room temperature
15min is stirred, mixed liquor is made；
S2, under room temperature, stirring, into reactor tank, that the sodium metasilicate that modulus is 3.2, concentration is 0.7mol/L is added dropwise is molten simultaneously
Liquid and mixed liquor, the rate of addition for controlling sodium silicate solution is 0.5m3/ h, and adjust mixing flow velocity make system pH 5.0,
After mixed liquor is added dropwise, static 90min；
S3, after taking out product, moisture is discharged with suction filtration machine, is placed at 100 DEG C and dries 10h, further take out and be crushed,
With 25 mesh sieving extracting screen underflow and the sample for taking oversize partial size into product to be greater than 710 microns with the sieving of 140 mesh less than 5%,
Sample of the partial size less than 45 microns less than 2%, then by the product after sieving with originally water washing to sodium sulphate content less than 4%,
Taking-up is placed in 100 DEG C of baking ovens after drying, and silica is made.
Comparative example 5
Compared with Example 3, difference of the invention is only that: the additional amount of the ZSM-5 type zeolite molecular sieve improve to
35kg。
The performance detection of test example, high-specific surface area of the present invention and high absorption VOC type silica
(1) using high-performance surface analysis instrument (brand is precise and tiny Gao Bo, model JW-BK200) to Examples 1 to 4
And specific surface area, pore volume and the aperture of 1~5 silica of comparative example are detected.
(2) using gas chromatograph (being purchased from Shandong Jin Pu Analytical Instrument Co., Ltd, model GC2010) test implementation
Silica prepared by example 1~4 and comparative example 1~5 is 2mg/m to concentration at 35 DEG C3Toluene (VOC is most representative
Be toluene) efficiency that is purified, to investigate its purifying rate.
Test result is as shown in table 1 below.
Table 1
From upper table 1:
(1) 360~420m of specific surface area of 1~4 silica of the embodiment of the present invention2/ g, 0.6~2.0cm of pore volume3/ g,
7~10nm of aperture, purified concentrations are 2mg/m at 35 DEG C3Purifying rate >=90% of toluene, it is significant to the clean-up effect of VOC, and
And there is certain hardness, have granular sensation, it is not easy to be crushed into powder, thus can used in multiple fields, had good
Application prospect.
(2) compared with Example 3, the concentration of sulfuric acid solution and sodium silicate solution has been respectively increased in comparative example 1 and 2, comparison
Example 3 then improves the rate of addition of sodium silicate solution, and the specific surface area of 1 silica of Comparative result example, pore volume and aperture are bright
It is aobvious to reduce, the purifying rate of toluene is reduced；And the pore volume of 3 silica of comparative example 2 and comparative example and aperture also obviously subtract
It is few, the clean-up effect of toluene is weakened, while the hardness decline of 3 silica of comparative example.
(3) compared with Example 3, comparative example 4 changes the addition manner of material, as a result the pore volume of its silica and
Aperture substantially reduces, and hardness is decreased obviously；And comparative example 5 then increases the additional amount of ZSM-5 type zeolite molecular sieve, as a result
The pore volume of its silica and aperture are reduced, and hardness is decreased obviously, easily formation powder, are unfavorable for actual production and application.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (4)
1. the preparation method of a kind of high-specific surface area and high absorption VOC type silica, which comprises the following steps:
S1,1.5~2.5m of sulfuric acid solution is injected into reactor tank3, it stirs under room temperature, adds ZSM-5 type zeolite molecular sieve, after
10~20min of continuous stirring；
Continue that sodium silicate solution is added dropwise under S2, stirring, control rate of addition is 0.4~0.6m3/ h, being added dropwise to system pH is 4.8
When~5.0, reduce rate of addition to 0.02~0.03m3/ h, control endpoint pH are 5.4~5.7, and it is molten to stop dropwise addition sodium metasilicate
Liquid, continue stirring form thick gel to solution after, static 80~120min；
S3, after taking out thick gel, moisture is discharged with suction filtration machine, is placed in 8~12h of drying at 90~120 DEG C, further takes out
It is crushed, washed, dried, high-specific surface area and high absorption VOC type silica is made；
The concentration of the sulfuric acid solution is 0.3~0.4mol/L；
The additional amount of the ZSM-5 type zeolite molecular sieve is 12~27kg；
The silica alumina ratio of the ZSM-5 type zeolite molecular sieve is greater than 300；
The concentration of the sodium silicate solution is 0.6~0.8mol/L, and the modulus of the sodium metasilicate is 3.0~3.5.
2. the preparation method of high-specific surface area as described in claim 1 and high absorption VOC type silica, which is characterized in that institute
The speed for stating stirring is 30~40Hz.
3. the preparation method of high-specific surface area as described in claim 1 and high absorption VOC type silica, which is characterized in that institute
The silica alumina ratio for stating ZSM-5 type zeolite molecular sieve is greater than 300, and specific surface area is greater than 300m2/ g, partial size are 5~20 μm.
4. made from the preparation method of high-specific surface area and high absorption VOC type silica as described in any one of claims 1 to 3
Silica, which is characterized in that 360~420m of specific surface area of the silica2/ g, 0.6~2.0cm of pore volume3/ g, hole
7~10nm of diameter, purified concentrations are 2mg/m at 35 DEG C3Purifying rate >=90% of toluene.
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| PCT/CN2019/092111 WO2020098273A1 (en) | 2018-11-14 | 2019-06-20 | High-specific-surface-area high-voc-adsorption silicon dioxide and preparation method therefor |
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| CN109437211B (en) * | 2018-11-14 | 2019-06-25 | 广州市飞雪材料科技有限公司 | A kind of high-specific surface area and high absorption VOC type silica and preparation method thereof |
| CN112897539B (en) * | 2021-02-03 | 2023-06-09 | 华东理工大学 | Spherical silicon dioxide powder and preparation method and application thereof |
| CN114702839B (en) * | 2022-03-31 | 2023-01-24 | 安徽江淮汽车集团股份有限公司 | Preparation method of polyolefin VOC (volatile organic compound) improved filler and composite material containing polyolefin VOC improved filler |
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