CN108745271A - A kind of volatile benzenes sorbing material and preparation method thereof - Google Patents
A kind of volatile benzenes sorbing material and preparation method thereof Download PDFInfo
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- CN108745271A CN108745271A CN201810416019.2A CN201810416019A CN108745271A CN 108745271 A CN108745271 A CN 108745271A CN 201810416019 A CN201810416019 A CN 201810416019A CN 108745271 A CN108745271 A CN 108745271A
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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
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/42—Materials comprising a mixture of inorganic materials
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- Oil, Petroleum & Natural Gas (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of volatile benzenes sorbing materials and preparation method thereof, belong to material adsorption technology field.The sorbing material is activation glass fibre cotton, and preparation method is：Under agitation, it is that be slowly dropped to percent by volume be to be made into piranha solution in 30% aqueous hydrogen peroxide solution to 98% concentrated sulfuric acid by percent by volume, the volume ratio of the concentrated sulfuric acid and aqueous hydrogen peroxide solution is 7：3, it is then placed in glass fibre cotton, after reaction for 24 hours is stirred at room temperature, is washed, is placed in oven and dried with ethyl alcohol after taking-up, obtains activation glass fibre cotton.The sorbing material has good adsorption effect to benzene homologues, different for different benzene homologues, and 63% is up to the adsorption efficiency of aniline.
Description
Technical field
The invention belongs to material adsorption technology fields, and in particular to a kind of volatile benzenes sorbing material and its preparation side
Method.
Background technology
Widely distributed in air by the volatile organic matter of representative of benzene homologues, there are two types of distribution forms：Some with
In air, some are then adsorbed on particulate matter and float in the form of an aerosol in air for gaseous form loss.Volatility benzene
The characteristics of being object, is largely volatilized in construction, slow release in use.Due under this kind of compound room temperature in the form of steam
It is present in air, volatility is larger, and easily diffusion is in an atmosphere, serious to pollute environment and influence health.In recent years, for
Volatile benzenes content in air, source, genetic analysis and the research of variation tendency, has received widespread attention.
But particulate matter forms the relationship between volatile benzenes concentration, and volatile benzenes are in particulate matter in air
Content, particle diameter distribution and variation tendency are relative complex, and lack effective material or method comprehensively and accurately to monitor volatility
Benzene homologues are restricted the absorption research of the substance.Therefore, the cheap material of development cost and method easy to operate
It is carried out effectively to adsorb monitoring, to have a very important significance with harm to evaluate its influence to health.
Glass fibre has the work(such as preferable fire prevention, sound insulation, absorption, polymer precursor as widely used industrial goods
Can, it is widely used in industry.In existing technology, the glass fibre not being modified is as absorption volatile benzenes
Record and report.
Invention content
The improving eyesight of this hair is to provide a kind of volatile benzenes sorbing material and preparation method thereof.
The technical solution adopted in the present invention is：
A kind of volatile benzenes sorbing material, the sorbing material are activation glass fibre cotton.
A kind of preparation method of volatile benzenes sorbing material, includes the following steps：Under agitation, by volume hundred
It is to be made into piranha solution in 30% aqueous hydrogen peroxide solution to divide than being slowly dropped to percent by volume for 98% concentrated sulfuric acid, dense
The volume ratio of sulfuric acid and aqueous hydrogen peroxide solution is 7：3, it is then placed in glass fibre cotton, after reaction for 24 hours is stirred at room temperature, after taking-up
It is washed, is placed in oven and dried with ethyl alcohol, obtain activation glass fibre cotton.
Further, it is stirred using magneton.
Further, the activation glass fibre cotton is best to the adsorption effect of aniline.
After prepared by activation glass fibre cotton, volatile benzenes are adsorbed.Adsorption experimental apparatus is by 10mL
Round-bottomed flask (being put into magneton), anti-splash ball, condenser pipe, the rubber stopper with syringe, balloon composition.
Its specific adsorption method is：Benzene homologues in round-bottomed flask are heated reach boiling point after, be converted into gaseous state from liquid, on
Rise enter anti-splash ball, with activation glass fibre cotton (hydroxylating glass fibre cotton) contact, partly adsorb, it is not to be adsorbed then
Continue to ascend into condenser pipe, flow back afterwards leaves as drop to the cold, also has small part to remain in condenser pipe.
The data process&analysis method of volatile benzenes sorbing material：It is 4h that adsorption experiment, which keeps adsorption time,
Time zero is since drop occurs in chamber wall.It is anti-to weigh out the activation glass fibre cotton that above-mentioned preparation method obtains after 4h in the balance
Front and back Δ B of poor quality is answered, this is practical adsorbed gas quality.And m0To be put into the activation glass fibers in anti-splash ball before heating
Vinylon and cotton blend quality.Adsorbance calculation formula：Q=Δ B/ (m0).Q：Adsorbance (unit：Mg/g), Δ B：Practical adsorbed gas quality
(unit：Mg), m0：Activate glass fibre cotton quality (unit：g).Meanwhile in order to control error, weighing out round-bottomed flask in the balance
It is of poor quality before and after reaction, calculate the gaseous mass m of volatilization1；Front and back of poor quality of anti-splash ball reaction is weighed up, calculating remains in anti-
Splash the gaseous mass m in ball2；Use ethyl alcohol rinse condenser pipe, after rotary evaporation, weigh up and remain in condenser pipe after experiment
Gaseous mass m3, it is possible thereby to calculate theoretical adsorbance Q0=(m1-m2-m3)/m0And compared with practical adsorbance Q,
Removal rate calculation formula：α=Q/m1Wherein, Q is practical adsorbance, m1For the gaseous mass of volatilization.By the activation after adsorption experiment
Glass fibre cotton takes out, and is first put into oven drying, removes moisture removal, then uses ethyl alcohol rinse, after placing back in oven drying 3h, title
Weight.Δ mc of poor quality before and after ethyl alcohol rinse is to represent the part that physical absorption occurs, and total adsorbance Q is compared with Δ mc,
And relationship comprehensive verification between thermodynamics and adsorption efficiency, adsorption time and adsorption efficiency is expressed as chemisorption or object
Reason absorption.
The present invention has the following advantages：
A kind of volatile benzenes sorbing material provided by the invention and its method processed, can be effectively prepared into using this method
To the activated material containing more silicone hydroxyl, which has good adsorption effect to benzene homologues.Prepared by this activation method
It is different for different benzene homologues to activate mineral wool adsorption effect, to the adsorption efficiency highest of aniline, reaches 63%.Simultaneously
Influence to evaluation volatile benzenes to health has a very important significance with harm
Description of the drawings
Fig. 1 is super-resolution awkward silence at a meeting scanning electron microscope (SEM) figure before glass fibre cotton activation；
Fig. 2 is super-resolution awkward silence at a meeting scanning electron microscope (SEM) figure activated after glass fibre cotton adsorption of aniline；
Fig. 3 is the structural schematic diagram of adsorption experimental apparatus；
Fig. 4 is the curve graph of the adsorption time and adsorbance that activate glass fibre cotton adsorption of aniline；
Fig. 5 is the infrared spectrogram for activating glass fibre cotton adsorption of aniline.
Specific implementation mode
The invention will be further described below in conjunction with the accompanying drawings.
Embodiment 1
Prepare activation glass fibre cotton：Referring to Fig.1, Fig. 1 is the super-resolution awkward silence at a meeting scanning electricity before glass fibre cotton activation
Sub- microscope figure.It is that be slowly dropped to percent by volume be 30% mistake to 98% concentrated sulfuric acid by percent by volume under magneton stirring
It aoxidizes in aqueous solution of hydrogen, is configured to Piranha solution, places into 5g glass fibre cottons, impregnate at room temperature more than for 24 hours.It takes again
Ethyl alcohol rinse is out used, is put into baking oven, is more than 100 DEG C of dryings for 24 hours.
Embodiment 2
The process for activating glass fibre cotton adsorption experiment is as follows：
With reference to Fig. 3, adsorption experimental apparatus is injected by 10mL round-bottomed flasks 1 (being put into magneton), anti-splash ball 3, condenser pipe 2, band
Rubber stopper 5, the balloon 4 of device form.Under nitrogen protection, benzene homologues (0.4~0.6g) are weighed in round-bottomed flask 1, are heated to
Boiling is converted into gaseous state from liquid, and the activated glass fibre cotton of gas (0.1~0.2g) absorption, not to be adsorbed then enters
Condenser pipe 2, forms liquid afterwards to the cold.
Remarks：The other measures for reducing experimental error are as follows
1. before carrying out adsorption experiment every time, glass fibre cotton will be placed in vacuum drying chamber more than for 24 hours in advance, it is ensured that its
It is fully dried, ensures that the moisture shown is removed.
2. a whole set of experimental provision will be evacuated, while bottom puts on and is full of after installing with vacuum pump in device
The balloon 4 of nitrogen, it is ensured that entire adsorption experiment keeps higher air-tightness without gas leak phenomenon.
3. switching to gaseous state from liquid after being heated for benzene homologues when drop occurs in chamber wall and being returned afterwards to the cold in condenser pipe 2
The critical point of stream, from here on timing remove device after 4h.This experiment is 4h to the adsorption time of all benzene homologues.
The data process&analysis method of volatile benzenes sorbing material：It is 4h that adsorption experiment, which keeps adsorption time,
Time zero is since drop occurs in chamber wall.It is anti-to weigh out the activation glass fibre cotton that above-mentioned preparation method obtains after 4h in the balance
Front and back Δ B of poor quality is answered, this is practical adsorbed gas quality.And m0To be put into the activation glass in anti-splash ball 3 before heating
Cellucotton quality.Adsorbance calculation formula：Q=Δ B/ (m0).Q：Adsorbance (unit：Mg/g), Δ B：Practical adsorbed gas constitution
Measure (unit：Mg), m0：Activate glass fibre cotton quality (unit：g).Meanwhile in order to control error, weighing out round bottom burning in the balance
It is of poor quality before and after 1 reaction of bottle, calculate the gaseous mass m of volatilization1；Weigh up of poor quality, the calculating residual that anti-splash ball 3 reacts front and back
Gaseous mass m in anti-splash ball 32；Use ethyl alcohol rinse condenser pipe, after rotary evaporation, weigh up and remain in condensation after experiment
Gaseous mass m in pipe 23, it is possible thereby to calculate theoretical adsorbance Q0=(m1-m2-m3)/m0And with practical adsorbance Q into
Row comparison, removal rate calculation formula：α=Q/m1Wherein, Q is practical adsorbance, m1For the gaseous mass of volatilization.By adsorption experiment
Rear activation glass fibre cotton takes out, and is first put into oven drying, removes moisture removal, then with ethyl alcohol rinse, places back in oven drying
After 3h, weigh.Δ mc of poor quality before and after ethyl alcohol rinse is to represent the part that physical absorption occurs, total adsorbance Q and Δ mc into
Row compares and relationship comprehensive verification between thermodynamics and adsorption efficiency, adsorption time and adsorption efficiency is expressed as chemistry
Absorption or physical absorption.
Toluene, benzene, aniline, chlorobenzoyl chloride, benzylalcohol, two are carried out using the activation glass fibre cotton that embodiment 1 is prepared
The parameter of toluene, benzaldehyde, styrene, phenol, aniline adsorption experiment, adsorption experiment is shown in Table 1 to table 10, and absorption result is shown in Table
11。
Table 1 activates glass fibre cotton adsorption of aniline parameter
Table 2 activates glass fibre cotton and adsorbs chlorobenzoyl chloride parameter
Table 3 activates glass fibre cotton adsorbing phenol parameter
Table 4 activates glass fibre cotton and adsorbs benzene parameter
Table 5 activates glass fibre cotton and adsorbs dimethylbenzene parameter
Table 6 activates glass fibre cotton and adsorbs benzylalcohol parameter
Table 7 activates glass fibre cotton and adsorbs salicylide parameter
Table 8 activates glass fibre cotton and adsorbs benzaldehyde parameter
Table 9 activates glass fibre cotton and adsorbs styrene parameter
Table 10 activates glass fibre cotton and adsorbs toluene parameter
Table 11 activates glass fibre cotton absorption result
| The mineral wool of Piranha solution treatments | Practical adsorbance (g) | Adsorption rate |
| Toluene | 0.052 | 30% |
| Benzene | 0.134 | 25% |
| Aniline | 0.142 | 63% |
| Chlorobenzoyl chloride | 0.063 | 26% |
| Benzylalcohol | 0.142 | 53% |
| Dimethylbenzene | 0.323 | 60% |
| Benzaldehyde | 0.058 | 14% |
| Styrene | 0.041 | 29% |
| Phenol | 0.228 | 53% |
| Salicylide | 0.061 | 15% |
As can be seen from Table 11, the activation glass fibre cotton that embodiment 1 is prepared is to common volatile containing aromatic radical
Property compound all there is certain absorption property, and to the adsorption effect highest of aniline, reached 63%.Activate glass fibre cotton
The super-resolution awkward silence at a meeting scanning electron microscope diagram of adsorption of aniline is shown in Fig. 2, under identical amplification factor, relative to cellucotton raw material
Fig. 1, the cellucotton surface after absorption adhere to fine particle shape substance, show have novel substance obviously to be adsorbed.From reaction unit
Fig. 3 shows that adsorption operations are simple, is easy for other systems and carries out explorative experiment research.Under nitrogen protection, the accuracy of data
It improves, avoids generating absorption deviation because of gas leakage.The adsorption time of adsorption of aniline and the curve graph of adsorbance are shown in Fig. 4, from figure
It can obtain and reach saturation after adsorbing 4 hours, absorption total amount is constant, and adsorption time is short.Activate glass fibre cotton adsorption of aniline
Infrared spectrogram is shown in Fig. 5.Mineral wool after the Piranha solution treatments can be used as effective suction to volatile aroma compounds
Enclosure material has many advantages, such as that quality is small, large specific surface area；Experimental implementation is simple, is easy to be amplified experimental study；And to aniline
Adsorption efficiency highest have certain in removal volatile aroma compounds, the especially use containing amino benzenes derivates
Application value.
It should be noted last that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although ginseng
It is described the invention in detail according to preferred embodiment, it will be understood by those of ordinary skill in the art that, it can be to the present invention
Technical solution be modified or replaced equivalently, without departing from the spirit of the technical scheme of the invention and range, should all cover
In the scope of the claims of the present invention.
Claims (4)
1. a kind of volatile benzenes sorbing material, which is characterized in that the sorbing material is activation glass fibre cotton.
2. a kind of preparation method of volatile benzenes sorbing material, which is characterized in that include the following steps：By percent by volume
It is slowly added into glass fibre cotton and is stirred to react for 30% aqueous hydrogen peroxide solution, 105 DEG C are heated at reflux 1~4h, filter
Afterwards, it is washed, is placed in oven and dried using ethyl alcohol, obtain activation glass fibre cotton.
3. the preparation method of volatile benzenes sorbing material according to claim 2, which is characterized in that using magneton into
Row is stirred to react.
4. the preparation method of volatile benzenes sorbing material according to claim 2 or 3, which is characterized in that the work
It is best to the adsorption effect of salicylide to change glass fibre cotton.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109701483A (en) * | 2018-05-03 | 2019-05-03 | 江汉大学 | A kind of volatile benzenes adsorbent material and preparation method thereof |
| CN109701481A (en) * | 2018-05-03 | 2019-05-03 | 江汉大学 | A kind of volatile benzenes adsorbent material and preparation method thereof |
| CN112442896A (en) * | 2019-08-30 | 2021-03-05 | 江汉大学 | Glass fiber cotton containing aryl and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109701483A (en) * | 2018-05-03 | 2019-05-03 | 江汉大学 | A kind of volatile benzenes adsorbent material and preparation method thereof |
| CN109701481A (en) * | 2018-05-03 | 2019-05-03 | 江汉大学 | A kind of volatile benzenes adsorbent material and preparation method thereof |
| CN112442896A (en) * | 2019-08-30 | 2021-03-05 | 江汉大学 | Glass fiber cotton containing aryl and application thereof |
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