CN106706611A - Method for immobilizing indicator by utilizing porous silica gel material and gas sensor and application - Google Patents
Method for immobilizing indicator by utilizing porous silica gel material and gas sensor and application Download PDFInfo
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- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/783—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour for analysing gases
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Abstract
The invention relates to a method for immobilizing an indicator by utilizing a porous silica gel material and a gas sensor and application. The method comprises the following three aspects: synthesis of silica sol and gel, immobilization of the indicator and application of the immobilized indicator in gas detection. The preparation method of the sensor comprises the following steps: taking two or more than two siloxane reagents as a mixed silicon source, hydrolyzing under acidic conditions to synthesize the silica sol and gel; respectively mixing the silica sol and gel with a specific alcohol-soluble or non-alcohol-soluble indicator, dispensing onto a substrate, drying under nitrogen protection, thereby obtaining the sensor which can be used for detecting specific gases. Because the silica sol and gel has a porous structure after aging, the specific surface area of the indicator immobilized on the substrate by utilizing the silica sol and gel is greatly enlarged, so the indicator is easily contacted with to-be-detected gases, and the sensitivity of the sensor on the gas detection is improved. Meanwhile, due to high stability of the silica gel, the storage time of the sensor prepared by utilizing the sol and gel immobilizing method is increased, and the practicality of the sensor is improved.
Description
Technical field
Tested or analysis of material the present invention relates to the synthesis of material and using optical instrument.Specifically
Say it is the synthesis of Bio-sil sol gel film, the fixation of indicator and immobilized rear indicator
The aspect of application three.Because Bio-sil collosol and gel has big specific surface area and stability,
So that using the sensor prepared by the immobilized indicator of silica gel collosol and gel in gas detection process
In there is sensitivity higher, and extend the holding time of sensor.
Background technology
Developing rapidly for Modern Live, result in urban atmospheres and becomes increasingly complex, to the mankind's
Influence is also increasing.Family life has been benefited in the exploitation of liquefied petroleum gas significantly, while
Also more blasts or disaster hidden-trouble are brought.In order to ensure " quality " of atmospheric environment and family
The safety of front yard gas, just be unable to do without accurately and effectively odor detection and alarm means：Many operations
Process (such as steel-making, fermentation, metallurgical, mine and automobile) is required for carrying out associated gas
Strict monitoring or quick regulation, will otherwise cause major accident with loss.Just because of gas and people
The existence and activity of class are so closely related, and the mankind have begun to the detection and control to gas very early
The research of method processed.
Conventional gas detection method is mainly instrumental method, including gas chromatograph
(GC) and mass spectrograph (MS) etc., these instrument system complex structures are cumbersome, involve great expense,
Test period is long, it is necessary to people carries out substantial amounts of intervention to be analyzed, it is impossible to continuously detected,
And typically sample at the scene, being then delivered to laboratory carries out off-line analysis, so that in the presence of sampling frequency
Rate is low, and sample it is not easy to maintain the shortcomings of.In addition, in many cases, it is necessary to know in time
Specific gas content, to formulate corresponding treatment Countermeasures rapidly.In face of these problems, most manage
The solution thought is exactly real-time detection in situ.Therefore site environment detection, mobile laboratory and
The concepts such as portable detector are proposed by many researchers.
Scientists have carried out substantial amounts of research and probe work to the field monitoring of gas, are based on
The different types of gas sensors such as optical principle, electrochemical principle, function nano material meet the tendency of
And give birth to.Among these, photochemistry colorimetric method is simple to operate because of its, with low cost and be subject to scientist
Extensive concern.But the chromogenic reaction of solution operates very cumbersome, and be not suitable for
In field assay.Indicator is immobilized in being on porous matrix (such as filter paper, cellulose ester membrane etc.)
A kind of effective method, conventional solid support method is to dissolve indicator by organic solvent,
To on porous matrix, after solvent volatilization, indicator is penetrated into the fiber of porous matrix drop coating.
However, this method indicator typically can be to crystallize precipitation, its specific surface area is in fact relatively still
It is smaller, it is unfavorable for its application in gas detection.
The content of the invention
It is used for gas it is an object of the invention to provide a kind of immobilized indicator of silica gel sol-gal process
The preparation and application of detection sensor.Bio-sil colloidal sol coacervation material in the present invention can be right
Indicator carry out effectively it is immobilized, formed silica gel after, with very big specific surface area, meanwhile, silicon
The acidproof alkali ability of glue is relatively strong, and translucency is good, and stability is high, therefore selects the material
Indicator is fixed in matrix can not only increase the specific surface area that indicator is contacted with gas,
So as to improve the sensitivity to gas detection, the stabilization of immobilized rear indicator is additionally improves
Property, the holding time of sensor is extended, for the commercialization of sensor provides possibility.
To achieve the above object, the technical solution adopted by the present invention is：
For gas detection indicator carried out using silica gel sol-gal process it is immobilized, it is specific by such as
It is prepared by lower process：
1) synthesis of silica gel collosol and gel：
1. silicone agent：EGME：Propylene glycol methyl ether acetate：Organic solvent：Urge
Agent：Surfactant：Water is with 1：2-4：1-2：0.2-0.8：0.1-0.8：0.005
- 0.04：0.5-1 volume ratios mix, and 55-85 DEG C hydrolyzes 1-8 hours, obtains the first silica gel molten
Gelling sol solution；
Or 2. silicone agent：EGME：Propylene glycol methyl ether acetate：Catalyst：Table
Face activating agent：Water is with 1：2-4：1-2：0.1-0.8：0.005-0.04：0.5-1 volumes
Than mixing, water at normal temperature solution 12-24 hours obtains the second silica gel sol gel solution；
2) fixation of indicator:
1. the fixation of non-prolamine indicator：0.5-15mg non-prolamine indicator is added to
In 1mL the first silica gel sol gel solutions, ultrasonic dissolution takes solution, drop coating in matrix,
The lower drying at room temperature of nitrogen protection obtains corresponding gas sensor；
Or the 2. fixation of alcohol-soluble indicator：0.5-15mg non-prolamine indicator is added to
In 1mL the second silica gel sol gel solutions, ultrasonic dissolution takes solution, drop coating in matrix,
The lower drying at room temperature of nitrogen protection obtains corresponding gas sensor.
Described silicone agent includes：Tetramethoxy-silicane, tetraethoxysilane, methyl three
Methoxy silane, MTES, normal octane triethoxysilane, (3- mercaptopropyis)
Trimethoxy silane, (3- aminopropyls) triethoxysilane, phenyl triethoxysilane, (3- chlorine
Propyl group) trimethoxy silane, one or two or more kinds in trim,ethylchlorosilane.
The indicator for gas detection is divided into alcohol-soluble indicator and non-prolamine is indicated
The class of agent two, wherein alcohol-soluble indicator include pH indicator class (Congo red, methyl red, phenol
Phthalein, thymolphthalein, alizarin yellow, methyl yellow, phenol red, basic fuchsin, chlorophenol red, cresols
Red, nitro-nitrogen yellow, soap Huang, bromophenol blue, bromthymol blue, thymol blue, bromocresol green,
Bromocresol purple, m-cresol purple, methyl orange, fluorescein, alizarin) and molten mutagens color class indicator
(rosolic acid, bromopyrogallol red, the red Nile, disperse orange #25, acridine orange base, dispersion
Orange #1 and disperse orange #3)；Non-prolamine indicator is metalloporphyrin class (zinc protoporphyrin, iron porphin
Quinoline, cadmium porphyrin, copper porphyrin, nickel-porphyrin, chromium porphyrin and Cob altporphyrin) in one kind or two kinds
More than.
In the collosol and gel building-up process catalyst used be 0.1-1M hydrochloric acid or nitric acid,
Organic solvent used is toluene, dimethylbenzene, hexamethylene, chloroform, the chloroethenes of 1,2- bis-
Alkane, tetrahydrofuran, dimethyl sulfoxide, ethanol, acetone, methyl alcohol, dimethylformamide, acetic acid,
One or two or more kinds in 1- propyl alcohol, n-hexane or acetonitrile.
In the collosol and gel building-up process surfactant used be lauryl sodium sulfate,
Neopelex, polysorbas20, L-7001, Span 60, cetyl trimethyl bromination
One kind in ammonium, triton x-100, polysorbate, Span 80 and sodium carboxymethylcellulose
Or more than two kinds, it is primarily to improve dispersed homogeneous degree of the indicator in matrix.
The matrix for immobilizing indicator is porous filter paper, nitric acid-acetic acid composite fibre
Cellulose ester film, polyvinylidene fluoride film, poly tetrafluoroethylene and non-porous poly terephthalic acid second two
One kind in alcohol ester film, polycarbonate membrane, polyethylene film, polychloroethylene film and polypropylene screen or
More than two kinds.
The detection that gas sensor prepared by the above method is used for gas is by colorimetric method：By gas
Body sensor is placed under test gas environment or guides under test gas by passing by gas piping
Sensor so that indicator is fully contacted with gas, by the change of indicator color to gas
Concentration carries out qualitative or half-quantitative detection.
The invention has the advantages that:
1. the method adjusts its pH value by the optimization to silica gel sol-gel system, hydrolysis
Ageing time etc., obtains the sol gel solution being best suitable for for immobilized indicator.Collosol and gel
After forming silica gel, loose structure makes it have very big specific surface area, so as to largely increase
Added the specific surface area that is contacted with gas of immobilized indicator, and then increased sensor to gas
The sensitivity of detection；
2. the acidproof alkali ability of silica gel is relatively strong, and translucency is good, is preferable indicator
Support material；
3. after collosol and gel forms silica gel, stability is high, extends the guarantor of the sensor for preparing
Deposit the time；
4. the immobilized indicator of silica gel collosol and gel is utilized, indicator is increased uniform in matrix
Property, improve the colorimetric effect of indicator；
5. the use of silica gel collosol and gel so that the immobilized matrix to indicator can not only be used
Porous film material, it is also possible to less expensive pore-free material, reduce being fabricated to for sensor
This.
Brief description of the drawings：
Fig. 1 coagulate indicator cadmium porphyrin with ethanol, chloroform, tetrahydrofuran, silica gel colloidal sol respectively
Drop coating is on acetyl cellulose film after the dissolving of glue, polyvinyl chloride and polyvinyl alcohol；
Fig. 2 cadmium porphyrins are used to determine the ammonia that concentration is 50ppm after utilizing distinct methods immobilized
When color change situation；
Fig. 3 are immobilized on poly terephthalic acid second two by by bromthymol blue using collosol and gel
The sensor prepared on alcohol ester film is the SO of 100ppm with concentration in different standing times2Gas
Response condition during precursor reactant.
Embodiment 1.
6 parts of cadmium porphyrin indicator of weight respectively 4mg are weighed, 1mL second is then used respectively
Alcohol, chloroform, tetrahydrofuran, silica gel collosol and gel (normal octane triethoxysilane：Ethylene glycol
Methyl ether：Propylene glycol methyl ether acetate：Tetrahydrofuran：0.2M hydrochloric acid：Polysorbas20：Water is with 1：
4.2：3.5：0.8：0.6：0.01：0.6 volume ratio mixes, and 65 DEG C hydrolyze 6 hours, obtain first
Silica gel sol gel solution；), polyvinyl chloride (polyvinyl chloride：Tetrahydrofuran is with 1:25 mass ratioes)
With polyvinyl alcohol (polyvinyl alcohol：Water is with 1：30 mass ratioes) ultrasonic dissolution, then use liquid relief
Rifle draws 1 microlitre of above-mentioned solution, drop coating on the acetyl cellulose film in 0.22 micron of aperture,
After drying with observation by light microscope using distinct methods dissolve cadmium porphyrin in matrix
Situation is simultaneously taken pictures, and it sees Fig. 1 using the picture details that microscope is obtained, as can be seen from the figure
In addition to the cadmium porphyrin indicator dissolved with silica gel collosol and gel, other method indicator are in acetic acid
Uniformity on cellulose ester membrane is all very poor, and with obvious indicator precipitation phenomenon.From admittedly
The uniformity and imaging effect of the indicator of load can be seen that using the immobilized instruction of sol-gal process
Agent will be significantly stronger than other methods.
Embodiment 2.
In Example 1. cadmium porphyrin indicator is dissolved using different solvents and immobilized to acetic acid fibre
The sensor obtained on dimension cellulose ester film, is taken pictures using mobile phone or camera and obtains its priming color figure
Piece, in being connected on it while being put into ammonia concentration for the closed container of 50ppm, takes after 2 minutes
Go out, taken pictures so as to obtain the color diagram of sensor after ammonia reacts with mobile phone or camera again
Piece；With Photoshop softwares to reacting front and rear using the immobilized indicator of distinct methods and ammonia
Color be digitized, extract digitlization after RGB (RGB) value, and to obtain
Rgb value carries out subtractive respectively, so as to the color change value △ R before and after being reacted, △ G,
△ B, then use formulaIt is calculated and is reacted with ammonia
Front and rear color change value.Be can be seen that from the picture of Fig. 2 a color changes and use silica gel colloidal sol
The color change of the sensor of the immobilized preparation of gel is the most obvious, to 6 sensor colors changes
Rgb value carry out the result that the difference histogram of the color change that subtractive is tried to achieve is indicated
Fig. 2 b are seen, as can be seen that being determined with sensor prepared by silica gel sol-gal process from Fig. 2 b
When concentration is the ammonia of 50ppm, its color difference is more than 200, is far longer than and is consolidated using other
Sensor prepared by support method, thus carries out immobilized side using collosol and gel to indicator
Method is substantially better than other methods, significantly improves the detection sensitivity of sensor.
Embodiment 3.
6mg indicator bromthymol blues are weighed, 1mL sol gel solutions is added thereto to (molten
The preparation method of glue gel is：Tetraethoxysilane：Normal octane triethoxysilane：Ethylene glycol
Methyl ether：Propylene glycol methyl ether acetate：0.1M nitric acid：Span 80：Water is with 1：1.5：4：3：
0.5：0.04：1 volume ratio mixes, and water at normal temperature solution 16 hours obtains the second silica gel collosol and gel
Solution) and 40 microlitres of concentration be the TBAH aqueous solution of 1M, ultrasonic dissolution, Ran Houyong
Liquid-transfering gun draws 1 microlitre of drop coating in polyethylene terephthalate film, and drop coating is had into instruction
The lower room temperature of film nitrogen protection of agent keeps in dark place, stand-by.Take the immobilized film for having indicator a piece of,
(two holes are left on capsule, one is used for air inlet, one in being placed on transparent plastic caddy
It is individual for outlet, other places are fully sealed) prepare for determining SO2The sensing of gas
Device, the sensor that will be prepared is scanned with EPSON V200 scanners to its priming color
Imaging, then by air inlet to be passed through in sensor concentration be 100ppm SO2Gas is (empty
Gas is used as carrier gas, relative humidity 33%), gas flow rate 500mL/min, 5min to be ventilated
Afterwards with scanner pair and SO2Reacted sensor is imaged.With Photoshop softwares pair
With SO2The color of indicator is digitized before and after gas reaction, extracts the RGB after digitlization
Value, and to obtain rgb value carry out subtractive respectively, so as to before and after react color change
Change value △ R, △ G, △ B, then use formulaCalculate
Obtain and SO2Color change value before and after gas reaction.Using above-mentioned same method, to system
Get ready, be stored in two days, one month, two months, three months and four months in nitrogen environment
Same a collection of preparation bromothymol blue sensor to SO2The response condition of gas is investigated,
As shown in Figure 3 a, the histogram of the difference of its color change is shown in Fig. 3 b tables to its color change situation
1 is the SO of the sensor to 100ppm of different holding times2Color change difference, calculate
It is 2.419034 to obtain its standard deviation.Result above display utilizes the immobilized instruction of sol-gal process
Agent is conducive to preparing the long-term preservation of sensor, can at least preserve more than four months, illustrates profit
The sensor prepared with this kind of method has stability well.
The different holding time sensors of table 1. are to 100ppm SO2The response condition of gas
| Holding time | Two days | One month | Two months | Three months | Four months | Standard deviation |
| Color change value | 62.87672 | 64.37975 | 65.24765 | 65.89373 | 69.38166 | 2.419034 |
Method and gas sensor and application the present invention relates to a kind of immobilized indicator of silica gel material, its
Include that the synthesis of silica gel collosol and gel, the immobilized of indicator and immobilized rear indicator are examined in gas
Three aspects of application in survey.Using two kinds or more than two kinds silicone agents as mixing silicon
Source, hydrolyzed under acidic conditions synthesized silicon rubber collosol and gel.Respectively by the collosol and gel with it is specific
The indicator mixing of alcohol-soluble or non-prolamine, in drop coating to matrix, the lower drying of nitrogen protection,
So as to obtain the sensor that can be used for detecting specific gas.Due to the aging rear tool of silica gel collosol and gel
There is loose structure, so as to largely improve be immobilized on matrix using silica gel collosol and gel
On indicator specific surface area, make it easier to be contacted with test gas, improve sensor
Sensitivity to gas detection.Simultaneously as the high stability of silica gel itself, increased utilization
The holding time of sensor prepared by the immobilized method of collosol and gel, improve the practicality of sensor.
Claims (8)
1. a kind of method of the material solid supported indicator of utilization Bio-sil, it is characterised in that：For gas
The indicator of detection is carried out immobilized using silica gel sol-gal process, is specifically prepared according to the following procedure：
1) synthesis of silica gel collosol and gel：
1. silicone agent：EGME：Propylene glycol methyl ether acetate：Organic solvent：Catalyst：
Surfactant：Water is with 1：2-4：1-2：0.2-0.8：0.1-0.8：0.005-0.04：
0.5-1 volume ratios mix, and 55-85 DEG C hydrolyzes 1-8 hours, obtains the first silica gel collosol and gel
Solution；
Or 2. silicone agent：EGME：Propylene glycol methyl ether acetate：Catalyst：Live on surface
Property agent：Water is with 1：2-4：1-2：0.1-0.8：0.005-0.04：0.5-1 volume ratios are mixed
Close, water at normal temperature solution 12-24 hours obtains the second silica gel sol gel solution；
2) fixation of indicator:
1. the fixation of non-prolamine indicator：0.5-15mg non-prolamine indicator is added to 1mL
In first silica gel sol gel solution, ultrasonic dissolution takes solution, drop coating in matrix, nitrogen
The lower drying at room temperature of protection obtains corresponding gas sensor；
Or the 2. fixation of alcohol-soluble indicator：0.5-15mg non-prolamine indicator is added to 1mL
In second silica gel sol gel solution, ultrasonic dissolution takes solution, drop coating in matrix, nitrogen
The lower drying at room temperature of protection obtains corresponding gas sensor.
2. method according to claim 1, it is characterised in that：Described silicone agent includes：
Tetramethoxy-silicane, tetraethoxysilane, MTMS, methyltriethoxy silane
Alkane, normal octane triethoxysilane, (3- mercaptopropyis) trimethoxy silane, (3- aminopropyls) three
Ethoxysilane, phenyl triethoxysilane, (3- chloropropyls) trimethoxy silane, trimethyl
One or two or more kinds in chlorosilane.
3. method according to claim 1, it is characterised in that：It is described for gas detection
Indicator is divided into alcohol-soluble indicator and the class of non-prolamine indicator two, wherein alcohol-soluble indicator
Including pH indicator class (Congo red, methyl red, phenolphthalein, thymolphthalein, alizarin yellow, first
Base Huang, phenol red, basic fuchsin, chlorophenol red, cresol red, nitro-nitrogen yellow, soap Huang, bromophenol blue,
Bromthymol blue, thymol blue, bromocresol green, bromocresol purple, m-cresol purple, methyl orange,
Fluorescein, alizarin) and molten mutagens color class indicator (rosolic acid, bromopyrogallol red, Buddhist nun sieve
River is red, disperse orange #25, acridine orange base, disperse orange #1 and disperse orange #3)；Non-prolamine
Indicator be metalloporphyrin class (zinc protoporphyrin, ferriporphyrin, cadmium porphyrin, copper porphyrin, nickel-porphyrin,
Chromium porphyrin and Cob altporphyrin) in one or two or more kinds.
4. method according to claim 1, it is characterised in that：The collosol and gel building-up process
In catalyst used be 0.1-1M hydrochloric acid or nitric acid, organic solvent used is toluene, two
Toluene, hexamethylene, chloroform, 1,2- dichloroethanes, tetrahydrofuran, dimethyl sulfoxide,
In ethanol, acetone, methyl alcohol, dimethylformamide, acetic acid, 1- propyl alcohol, n-hexane or acetonitrile
One or two or more kinds.
5. method according to claim 1, it is characterised in that：The collosol and gel building-up process
In surfactant used be lauryl sodium sulfate, neopelex, tween
20th, L-7001, Span 60, cetyl trimethylammonium bromide, triton x-100, poly- mountain
One or two or more kinds in pears alcohol, Span 80 and sodium carboxymethylcellulose, it is mainly
In order to improve dispersed homogeneous degree of the indicator in matrix.
6. method according to claim 1, it is characterised in that：It is described for immobilizing indicator
Matrix is porous filter paper, nitric acid-acetic acid mixed cellulose ester membrane, polyvinylidene fluoride film, poly-
Tetrafluoroethylene and non-porous polyethylene terephthalate film, polycarbonate membrane, poly- second
One or two or more kinds in alkene film, polychloroethylene film and polypropylene screen.
7. the gas sensor that prepared by a kind of any methods describeds of claim 1-6.
8. the application of gas sensor described in a kind of claim 7, it is characterised in that：The preparation
Gas sensor be used for gas detection be by colorimetric method：Gas sensor is placed in be measured
Guide under test gas by sensor so that indicator in gaseous environment or by gas piping
It is fully contacted with gas, qualitative or half is carried out to the concentration of gas by the change of indicator color
Quantitative determination.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112076729A (en) * | 2020-09-15 | 2020-12-15 | 西南石油大学 | Preparation method of long-chain saturated alkane silane-loaded silicon dioxide adsorbent |
| CN112354493A (en) * | 2020-09-28 | 2021-02-12 | 金华洁灵家居用品有限公司 | pH value sensitive microcapsule, preparation method and application |
| CN114480557A (en) * | 2021-12-27 | 2022-05-13 | 上海理工大学 | Method for rapidly screening high-yield exopolysaccharide streptococcus thermophilus |
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| CN102466638A (en) * | 2010-11-12 | 2012-05-23 | 中国科学院大连化学物理研究所 | Indicator fixation test paper for heavy metal ion detection, preparation thereof and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112076729A (en) * | 2020-09-15 | 2020-12-15 | 西南石油大学 | Preparation method of long-chain saturated alkane silane-loaded silicon dioxide adsorbent |
| CN112076729B (en) * | 2020-09-15 | 2022-04-22 | 西南石油大学 | Preparation method of long-chain saturated alkane silane-loaded silicon dioxide adsorbent |
| CN112354493A (en) * | 2020-09-28 | 2021-02-12 | 金华洁灵家居用品有限公司 | pH value sensitive microcapsule, preparation method and application |
| CN112354493B (en) * | 2020-09-28 | 2022-09-16 | 金华洁灵家居用品有限公司 | pH value sensitive microcapsule, preparation method and application |
| CN114480557A (en) * | 2021-12-27 | 2022-05-13 | 上海理工大学 | Method for rapidly screening high-yield exopolysaccharide streptococcus thermophilus |
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| CN106706611B (en) | 2020-09-01 |
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