CN113884484A - Color-changing material for detecting and removing formaldehyde and preparation method and application thereof - Google Patents
Color-changing material for detecting and removing formaldehyde and preparation method and application thereof Download PDFInfo
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- CN113884484A CN113884484A CN202111144843.5A CN202111144843A CN113884484A CN 113884484 A CN113884484 A CN 113884484A CN 202111144843 A CN202111144843 A CN 202111144843A CN 113884484 A CN113884484 A CN 113884484A
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 518
- 239000000463 material Substances 0.000 title claims abstract description 119
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000001514 detection method Methods 0.000 claims abstract description 39
- -1 hydroxylamine salt compound Chemical class 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 28
- 238000001179 sorption measurement Methods 0.000 claims description 27
- 230000008859 change Effects 0.000 claims description 22
- 239000001913 cellulose Substances 0.000 claims description 21
- 229920002678 cellulose Polymers 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 239000003906 humectant Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- 239000011521 glass Substances 0.000 claims description 14
- 239000000919 ceramic Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 11
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 10
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 230000004075 alteration Effects 0.000 claims description 8
- ZNBNBTIDJSKEAM-UHFFFAOYSA-N 4-[7-hydroxy-2-[5-[5-[6-hydroxy-6-(hydroxymethyl)-3,5-dimethyloxan-2-yl]-3-methyloxolan-2-yl]-5-methyloxolan-2-yl]-2,8-dimethyl-1,10-dioxaspiro[4.5]decan-9-yl]-2-methyl-3-propanoyloxypentanoic acid Chemical compound C1C(O)C(C)C(C(C)C(OC(=O)CC)C(C)C(O)=O)OC11OC(C)(C2OC(C)(CC2)C2C(CC(O2)C2C(CC(C)C(O)(CO)O2)C)C)CC1 ZNBNBTIDJSKEAM-UHFFFAOYSA-N 0.000 claims description 7
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- PRZSXZWFJHEZBJ-UHFFFAOYSA-N thymol blue Chemical group C1=C(O)C(C(C)C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C(=CC(O)=C(C(C)C)C=2)C)=C1C PRZSXZWFJHEZBJ-UHFFFAOYSA-N 0.000 claims description 7
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- UDSAIICHUKSCKT-UHFFFAOYSA-N bromophenol blue Chemical compound C1=C(Br)C(O)=C(Br)C=C1C1(C=2C=C(Br)C(O)=C(Br)C=2)C2=CC=CC=C2S(=O)(=O)O1 UDSAIICHUKSCKT-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000008098 formaldehyde solution Substances 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- OLQIKGSZDTXODA-UHFFFAOYSA-N 4-[3-(4-hydroxy-2-methylphenyl)-1,1-dioxo-2,1$l^{6}-benzoxathiol-3-yl]-3-methylphenol Chemical compound CC1=CC(O)=CC=C1C1(C=2C(=CC(O)=CC=2)C)C2=CC=CC=C2S(=O)(=O)O1 OLQIKGSZDTXODA-UHFFFAOYSA-N 0.000 claims description 4
- 239000004952 Polyamide Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- YVJPMMYYRNHJAU-UHFFFAOYSA-N chembl1206021 Chemical compound C1=C(O)C(C(=O)O)=CC(N=NC=2C=CC(=CC=2)[N+]([O-])=O)=C1 YVJPMMYYRNHJAU-UHFFFAOYSA-N 0.000 claims description 4
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- PTHCMJGKKRQCBF-UHFFFAOYSA-N Cellulose, microcrystalline Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC)C(CO)O1 PTHCMJGKKRQCBF-UHFFFAOYSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 3
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 3
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- DHEZQYZJFCIQQA-UHFFFAOYSA-N hydron;o-[(4-methoxyphenyl)methyl]hydroxylamine;chloride Chemical compound Cl.COC1=CC=C(CON)C=C1 DHEZQYZJFCIQQA-UHFFFAOYSA-N 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 3
- HYDZPXNVHXJHBG-UHFFFAOYSA-N o-benzylhydroxylamine;hydron;chloride Chemical compound Cl.NOCC1=CC=CC=C1 HYDZPXNVHXJHBG-UHFFFAOYSA-N 0.000 claims description 3
- ZBDXGNXNXXPKJI-UHFFFAOYSA-N o-tert-butylhydroxylamine;hydrochloride Chemical compound Cl.CC(C)(C)ON ZBDXGNXNXXPKJI-UHFFFAOYSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- 239000000600 sorbitol Substances 0.000 claims description 3
- 239000000811 xylitol Substances 0.000 claims description 3
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 3
- 229960002675 xylitol Drugs 0.000 claims description 3
- 235000010447 xylitol Nutrition 0.000 claims description 3
- 239000010457 zeolite Substances 0.000 claims description 3
- KBXIJIPYZKPDRU-UHFFFAOYSA-N (aminooxy)acetic acid hemihydrochloride Chemical compound Cl.NOCC(O)=O.NOCC(O)=O KBXIJIPYZKPDRU-UHFFFAOYSA-N 0.000 claims description 2
- FRPHFZCDPYBUAU-UHFFFAOYSA-N Bromocresolgreen Chemical compound CC1=C(Br)C(O)=C(Br)C=C1C1(C=2C(=C(Br)C(O)=C(Br)C=2)C)C2=CC=CC=C2S(=O)(=O)O1 FRPHFZCDPYBUAU-UHFFFAOYSA-N 0.000 claims description 2
- HFVAFDPGUJEFBQ-UHFFFAOYSA-M alizarin red S Chemical compound [Na+].O=C1C2=CC=CC=C2C(=O)C2=C1C=C(S([O-])(=O)=O)C(O)=C2O HFVAFDPGUJEFBQ-UHFFFAOYSA-M 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 2
- 229940012189 methyl orange Drugs 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract description 15
- 230000004044 response Effects 0.000 abstract description 4
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- 239000003153 chemical reaction reagent Substances 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
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- 238000011002 quantification Methods 0.000 description 3
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- MGSRCZKZVOBKFT-UHFFFAOYSA-N thymol Natural products CC(C)C1=CC=C(C)C=C1O MGSRCZKZVOBKFT-UHFFFAOYSA-N 0.000 description 3
- 230000000007 visual effect Effects 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- ATJXMQHAMYVHRX-CPCISQLKSA-N Ellagic acid Natural products OC1=C(O)[C@H]2OC(=O)c3cc(O)c(O)c4OC(=O)C(=C1)[C@H]2c34 ATJXMQHAMYVHRX-CPCISQLKSA-N 0.000 description 2
- 239000005844 Thymol Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 238000013475 authorization Methods 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
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- ZHFPEICFUVWJIS-UHFFFAOYSA-M sodium 2-hydroxy-5-[(3-nitrophenyl)diazenyl]benzoate Chemical compound [Na+].Oc1ccc(cc1C([O-])=O)N=Nc1cccc(c1)[N+]([O-])=O ZHFPEICFUVWJIS-UHFFFAOYSA-M 0.000 description 2
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- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical class ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 1
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- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- 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
Abstract
The invention provides a color-changing material for detecting and removing formaldehyde, a preparation method and application thereof, and relates to the technical field of formaldehyde detection and removal. The color-changing material is placed in an automobile or an indoor room, when the formaldehyde concentration is 80ppb, the color of the color-changing material can be completely changed into yellow from purple after ten minutes of response time, so that whether the indoor formaldehyde concentration exceeds the standard or not can be preliminarily distinguished by naked eyes, the color can be changed into red after more than 10 hours, the color-changing material is suitable for various places, the specific surface area is large, the formaldehyde concentration can be rapidly and efficiently detected, and the formaldehyde pollutant in the room can be removed, so that the cost is lower.
Description
Technical Field
The invention relates to the technical field of formaldehyde detection and removal, in particular to a color-changing material for formaldehyde detection and removal and a preparation method and application thereof.
Background
Formaldehyde is colorless, has chemical activity and strong volatility, and can be leaked into air to cause pollution and health hazard. The indoor formaldehyde is mainly from buildingBuilding materials, artificial boards, adhesives, coatings, paints and the like, the world health organization stipulates that the maximum concentration of indoor formaldehyde is 0.08 mg/cubic meter, and people feel uncomfortable when the content of formaldehyde in indoor air is 0.30 mg/cubic meter. When the concentration reaches 0.50 mg/cubic meter, the irritation to skin and eyes can be caused, and when the concentration reaches 0.60 mg/cubic meter3Then (c) is performed. Central nervous system impairment, immune system impairment, blindness and respiratory dysfunction. When 30 mg/cubic meter is reached, the person will die immediately. Formaldehyde is also classified as a human carcinogen, for example, there is clear epidemiological evidence that long term exposure to formaldehyde can lead to nasopharyngeal carcinoma, as reported by the international cancer research institute. Therefore, the material for detecting and removing the high-performance formaldehyde has important significance for treating the indoor air environment.
In the aspect of formaldehyde detection: there are many methods of formaldehyde detection currently available, including spectrophotometry, gas chromatography, liquid chromatography, etc., but these benchtop instruments are off-line, based on expensive, complex equipment requiring long-term operation and specially trained users. In addition, there are some sensors such as semiconductor thin film sensors, surface acoustic wave sensors, chemical resistance sensors, etc., which are much easier to use and can perform online detection, but these sensors tend to have poor selectivity (resistance to interference) and low sensitivity. Colorimetric methods, by virtue of the extensive selection of molecular design and structural optimization, achieve high detection sensitivity and selectivity, and in some cases can be detected by naked eyes, but still reach detection limit levels as low as ppm-ppb.
In terms of formaldehyde removal: some existing formaldehyde adsorption materials mainly comprise three-dimensional porous materials such as activated carbon, silica gel, molecular sieves, bentonite and polyamide, and the products have certain adsorption capacity, but have the common defects that the formaldehyde concentration cannot be visually detected and the formaldehyde removal effect cannot be judged, and a user cannot timely judge the effectiveness of adsorption and replace the adsorbent in real time when using the formaldehyde adsorption materials. In addition, some visual formaldehyde scavengers have appeared, but they still have some disadvantages, including high price, lack of substantial removal effect, and side effects that harm the living environment. For example, in a patent with chinese authorization No. CN100563793C and named visible harmful gas remover, potassium permanganate is used to oxidize and remove formaldehyde, and the color changes before and after the reaction of potassium permanganate are visualized, but the formaldehyde concentration cannot be detected. In addition, the potassium permanganate has strong oxidizing property, damages the respiratory tract and the skin of a human body, can also damage clothes and furniture, and has the color change range from red to brown and has no acute color change; the patent with Chinese authorization number of CN102527228B and name of a visible color-changing formaldehyde scavenger utilizes an adsorption material to adsorb formaldehyde, and then the formaldehyde is catalyzed and oxidized into formic acid, the acidity of the formic acid can lead color-changing components to change color, and the formaldehyde scavenging condition is sensed through color change. However, the formaldehyde concentration cannot be evaluated, and in addition, the catalyst is expensive and has a limit in mass production.
Therefore, most of the current materials can only meet unilateral formaldehyde detection or unilateral formaldehyde removal. Therefore, at present, a material which has complete functions, low cost, easy operation, environmental protection and green, can conveniently and rapidly detect the concentration of formaldehyde and has the capability of efficiently removing the formaldehyde does not exist.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the color-changing material for detecting and removing formaldehyde and the preparation method and the application thereof, the preparation process is simple, the color-changing material is also a porous material, the formaldehyde concentration can be conveniently, rapidly and quantitatively detected, the formaldehyde-removing capability is high, and the color-changing material is suitable for high-efficiency and low-cost formaldehyde detection and removal in places such as automobiles, indoor rooms and the like.
The invention is realized by the following technical scheme:
a preparation method of a color-changing material for formaldehyde detection and removal comprises the following steps:
step 1, uniformly mixing a hydroxylamine salt compound solution, a mixed indicator and a humectant, wherein the mixed indicator is thymol blue and m-cresol purple, the thymol blue and bromophenol blue, methyl orange and bromocresol green, alizarin yellow R and alizarin red S, or alizarin yellow R and bromophenol blue, and the mass ratio of the hydroxylamine salt compound in the mixed indicator, the humectant and the hydroxylamine salt compound solution is (1-2): (30-35):10, so as to obtain a mixed solution;
and 3, taking the compound out of the mixed system and drying to obtain the color-changing material for detecting and removing formaldehyde.
Preferably, the hydroxylamine salt compound in the step 1 is one or two of hydroxylamine hydrochloride, hydroxylamine sulfate, p-methoxybenzyloxyamine hydrochloride, O- (carboxymethyl) hydroxylamine half-hydrochloride, O-benzylhydroxylamine hydrochloride, hydroxylamine-O-sulfonic acid and O-tert-butylhydroxylamine hydrochloride;
the humectant is glycerol, sorbitol, butanediol, polyethylene glycol, propylene glycol, hexanediol, xylitol or polypropylene glycol.
Preferably, the hydroxylamine salt compound solution described in step 1 is obtained by the following process:
according to the mass ratio of (20-25) to (20-25), adding the hydroxylamine salt compound into deionized water and methanol, and uniformly stirring to obtain the hydroxylamine salt compound solution.
Preferably, in the five pairs of mixed indicators described in step 1, the mass ratio of the first indicator to the second indicator in each pair of mixed indicators is 5: 7.
Preferably, in the step 2, one or two of sodium bicarbonate and sodium hydroxide are used for adjusting the pH value of the mixed solution;
the porous adsorption material is polyamide or cellulose sponge, porous cellulose paper, porous cellulose cloth, cellulose gel, porous silica gel, kaolin, molecular sieve, zeolite, argil or clay.
Preferably, the mass ratio of the porous adsorption material in the step 2 to the humectant in the step 1 is (5-15): (30-35);
and 2, soaking the porous adsorption material in a mixed system, firstly carrying out ultrasonic treatment for 10-25min, and then standing for 0.5-1.5h to form a compound.
Preferably, step 3 vacuum drying the complex at 30-50 deg.C for 30-60 min.
The color-changing material for formaldehyde detection and removal obtained by the preparation method of the color-changing material for formaldehyde detection and removal.
The application of the color-changing material for formaldehyde detection and removal comprises the following steps:
step 1, placing the color-changing material for detecting and removing formaldehyde in an automobile or an indoor room for ten minutes, wherein the color-changing material adsorbs and degrades the formaldehyde in the space, the color-changing material is changed from the initial purple to yellow, and a total color difference is obtained compared with the color of the color-changing material before use;
the formaldehyde generating device comprises a sealed transparent box body, wherein a temperature and humidity controller, a temperature and humidity sensor, a humidifier, a ptc ceramic heating plate and a fan are placed in the sealed transparent box body, the temperature and humidity controller is respectively connected with the temperature and humidity sensor, the ptc ceramic heating plate and the humidifier, the fan is fixed below the ptc ceramic heating plate, two pipelines are arranged outside the sealed transparent box body, a circulating pump is installed in a first pipeline, an air inlet end of the first pipeline and an air outlet end of a second pipeline are respectively installed in the sealed transparent box body, an air outlet end of the first pipeline and an air inlet end of the second pipeline are respectively connected in an air bottle filled with formaldehyde solution with volume concentration of more than 10%, when formaldehyde in the formaldehyde generating device reaches set concentration, the air outlet end of the first pipeline and the air inlet end of the second pipeline are closed, and the air outlet end of the first pipeline, The air inlet end of the second pipeline is respectively connected with the two ends of the glass tube in a sealing manner;
step 3, adjusting the concentration of formaldehyde in the formaldehyde generating device in the step 2, repeating the process in the step 2 to manufacture a new adsorption sheet, and repeating the step 2 to obtain a total color difference corresponding to the concentration of another formaldehyde in the formaldehyde generating device;
step 4, repeating the step 3 three to five times, combining the step 2 and the step 3 to obtain a plurality of groups of formaldehyde concentrations and corresponding total chromatic aberration, and obtaining a corresponding relation between the formaldehyde concentrations and the total chromatic aberration according to the plurality of groups of formaldehyde concentrations and the corresponding total chromatic aberration;
and 5, substituting the total color difference obtained in the step 1 into the corresponding relation in the step 4 to obtain the concentration of formaldehyde in the automobile or the indoor room.
The application of the color-changing material for formaldehyde detection and removal is that the color-changing material for formaldehyde detection and removal is firstly placed in an automobile or an indoor room for more than 10 hours, and then the previous process is repeated to replace the new color-changing material until the latest color-changing material keeps the initial color and does not change any more, the formaldehyde concentration in the space is less than 10ppb, and the removal of formaldehyde in the automobile or the indoor room is completed.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention relates to a preparation method of a color-changing material for detecting and removing formaldehyde, which comprises the steps of firstly exploring the mass ratio of a mixed indicator, a humectant and a hydroxylamine salt compound through experiments, then uniformly mixing the mixed indicator, the humectant and the hydroxylamine salt compound to obtain a mixed solution, and then adjusting the pH value of the mixed solution to 4.25-4.5. The humectant can retain water in the porous adsorbent material and can make the mixed indicator develop color permanently, and the color-changing material pairFormaldehyde gas is continuously adsorbed, and the molecular structure of hydroxylamine salt compound contains-NH2And HX, wherein-NH2The method is characterized in that a stable compound containing C ═ N double bonds is generated by the reaction with carbonyl of formaldehyde, HX is released at the same time, the pH value of a system is reduced to the color change point of a mixed indicator, the mixed indicator is protonated, the color of an adsorption material is changed, when the formaldehyde concentration is 80ppb, the color of a color-changing material can be completely changed from purple to yellow after ten minutes of response time, so that whether the indoor formaldehyde concentration exceeds the standard or not can be preliminarily distinguished by naked eyes, then the corresponding relation between the formaldehyde concentration and the total color difference can be obtained according to the total color difference of the color-changing material before and after color change and the linear relation between different formaldehyde concentrations, and finally the actual accurate formaldehyde concentration is obtained according to the total color difference of the color-changing material before and after color change in the actual space. The hydroxylamine salt compound loaded on the porous adsorption material and formaldehyde have irreversible chemical reaction, so that the aim of removing the formaldehyde can be fulfilled. Therefore, the invention obtains the functional material which has perfect functions, low cost, easy operation, environmental protection and green, can conveniently, quickly and qualitatively detect the concentration of the formaldehyde and has high-efficiency formaldehyde removal capability, can obtain the approximate concentration of the formaldehyde in real time through the depth of color change of the material, can visually sense the formaldehyde removal effect through the color change, reminds a user to replace the material in time at any time and ensures the formaldehyde removal effect. The invention adopts green environment-friendly porous material; and the reaction product is a nontoxic and harmless compound with a C ═ N double bond structure, so that secondary pollution is avoided.
The color-changing material has various forms, is suitable for various places, has large specific surface area, can quickly and efficiently detect the concentration of formaldehyde, removes indoor formaldehyde pollutants, and has lower cost.
When the color-changing material is used for detecting the concentration of formaldehyde, the color-changing material can be placed in an automobile or an indoor room for ten minutes, so that the color-changing material can adsorb and degrade the formaldehyde in the space, the formaldehyde is changed from the initial purple to yellow, a total color difference is obtained compared with the color before use, then a formaldehyde generating device formed by a temperature and humidity controller, a temperature and humidity sensor, a humidifier, a ptc ceramic heating plate and a fan in a sealed transparent box body, two pipelines, a circulating pump and a gas cylinder filled with formaldehyde solution outside is utilized to reach the set concentration, the color-changing material is cut into a shape with a regular figure cross section and is placed into a corresponding glass tube, the glass tube is hermetically connected with the gas inlet end and the gas outlet end of the formaldehyde generating device, and the formaldehyde in the formaldehyde generating device can be adsorbed by the color-changing material, when the color-changing material is changed from the initial purple to the yellow, the total color difference corresponding to the formaldehyde concentration in the formaldehyde generating device is obtained, the corresponding relation between the formaldehyde concentration and the total color difference can be obtained according to a plurality of groups of formaldehyde concentrations and the corresponding total color differences after a plurality of times of repetition, and finally the formaldehyde concentration in the automobile or the indoor room can be obtained by bringing the initially obtained total color difference into the corresponding relation. The method has high sensitivity, can detect the formaldehyde concentration of about 10ppb in the theoretical lowest detection line, has richer color change, has smaller detection error and stronger anti-interference capability from the initial color to the second color and then to the third color, and has lower influence of the external environment change on the detection result.
When the color-changing material is used for removing formaldehyde, the color-changing material is required to be placed in an automobile or an indoor room for more than 10 hours, the color-changing material is changed into final red, and then the color-changing material cannot be used any more.
Drawings
FIG. 1 is a graph showing the color change of the porous cellulose paper obtained in example 1 of the present invention after detection of different formaldehyde concentrations (0ppb, 80ppb, 250ppb, 400ppb, 600ppb, 800 ppb).
FIG. 2 is a linear relationship between total color difference and formaldehyde concentration when formaldehyde concentration of the porous cellulose paper obtained in example 1 of the present invention is measured.
FIG. 3 is a graph showing the selectivity of the porous cellulose paper obtained in example 1 of the present invention to formaldehyde.
FIG. 4 is a diagram of a formaldehyde generating apparatus described in example 1 of the present invention.
FIG. 5 is a schematic representation of the porous cellulose paper obtained in example 1 of the present invention.
FIG. 6 is a real diagram of the upper surface of the sponge obtained in example 2 of the present invention.
In the figure: the device comprises a temperature and humidity controller 1, a temperature and humidity sensor 2, a humidifier 3, a ptc ceramic heating plate 4, a fan 5, a pressure gauge 6, a first pipeline 7, a circulating pump 8, a second pipeline 9, an air bottle 10, a wafer 11 and a glass tube 12.
Detailed Description
The present invention is further described in detail with reference to the following specific examples, which are not intended to limit the scope of the invention.
The invention relates to a preparation method of a color-changing material for detecting and removing formaldehyde with high efficiency, low cost and quantification, which comprises the following steps:
step 1, uniformly mixing a hydroxylamine salt compound solution, a mixed indicator and a humectant according to the mass ratio of (52-60) to (1-2) to (30-35), then adjusting the pH value of the mixed solution to 4.25-4.5 by using a pH adjusting reagent, wherein the mass ratio of the pH adjusting reagent to the mixed indicator is (1-2) to (1-2), so as to obtain a mixed solution, so that the mixed indicator can be purple in the pH range, and color change can be conveniently observed later;
the hydroxylamine salt compound solution is obtained by the following process according to the mass ratio of (20-25) to (20-25), firstly adding the hydroxylamine salt compound into deionized water and methanol, fully stirring until the hydroxylamine salt compound is dissolved uniformly, wherein the hydroxylamine salt compound is one or two of hydroxylamine hydrochloride, hydroxylamine sulfate, p-methoxybenzyloxyamine hydrochloride, O- (carboxymethyl) hydroxylamine hemihydrochloride, O-benzylhydroxylamine hydrochloride, hydroxylamine-O-sulfonic acid and O-tert-butylhydroxylamine hydrochloride; the mixed indicator is thymol blue-m-cresol purple, thymol blue-bromophenol blue, methyl orange-bromocresol green, alizarin yellow R-alizarin red S and alizarin yellow R-bromophenol blue, wherein the mass ratio of the thymol blue to the m-cresol purple is 5: 7; the humectant is glycerol, sorbitol, butanediol, polyethylene glycol, propylene glycol, hexanediol, xylitol or polypropylene glycol; the pH regulator is one or two of sodium bicarbonate and sodium hydroxide;
The adsorption material as carrier comprises polyamide and cellulose sponge, porous cellulose paper, porous cellulose cloth, cellulose gel, porous silica gel, kaolin, molecular sieve, zeolite, clay, and clay material. The molecular structure of the hydroxylamine salt compound contains-NH2And HX, wherein-NH2Reacting with carbonyl of formaldehyde to generate a stable compound containing C ═ N double bonds, and releasing HX at the same time, wherein the pH value of the system is reduced to the color changing point of the mixed indicator, so that the mixed indicator is protonated, and the color of the adsorbing material is changed; the aim of removing formaldehyde is achieved by means of irreversible chemical reaction between hydroxylamine salt compounds loaded on the porous material and formaldehyde. The reaction principle is as follows: the first step is as follows: the formaldehyde and the hydroxylamine salt compound generate irreversible chemical reaction to generate C ═ N double bonds and release acid. 2HCHO + (NH)2-OH)2·HX→2H2C＝NOH+HX+2H2And O, a second step: the released acid will protonate the mixed indicator resulting in a color change.
Example 1
The invention relates to a preparation method of a color-changing material for detecting and removing formaldehyde with high efficiency, low cost and quantification, which comprises the following steps:
dissolving 5g of hydroxylamine sulfate in 120mL of deionized water and 100mL of methanol, and uniformly stirring to prepare 55 parts of formaldehyde reaction reagent (solution a), wherein the methanol is dissolved to form a color developing agent; adding 1 part of mixed color developing agent (0.25g of thymol blue and 0.35g of bromophenol blue) into the solution a, and uniformly stirring to obtain a solution b; to solution b was added 35 parts of glycerol (100mL) to give solution c, followed by addition of 2 parts of sodium bicarbonate (1g) to solution c to maintain the pH of the solution at 4.25 to give solution d. And (3) soaking 7 parts of the standby porous cellulose paper in the solution d in advance, performing ultrasonic treatment in an ultrasonic machine for 10min, standing for 1h, and drying in a vacuum drying oven at 30 ℃ for 30min to prepare the purple color-changing material capable of detecting and removing formaldehyde.
The invention forms formaldehyde with certain concentration in a closed box body, and the specific process is as follows:
as shown in fig. 4, a temperature and humidity controller 1, a temperature and humidity sensor 2, a humidifier 3, a ptc ceramic heating plate 4 and a fan 5 are placed in a sealed transparent box, a protective door is arranged on the front surface of the sealed transparent box, the temperature and humidity sensor 2 is connected to the left side of the temperature and humidity controller 1, the ptc ceramic heating plate 4 and the fan 5 are respectively fixed on two supporting surfaces of a double-layer supporting frame, the fan 5 is located below the ptc ceramic heating plate 4, and the ptc ceramic heating plate 4 and the humidifier 3 are respectively connected to the left side of the temperature and humidity controller 1. A pressure gauge 6 is arranged above the sealed transparent box body, and the pressure gauge 6 is used for monitoring the pressure in the sealed box body. Two pipelines are arranged outside the sealed transparent box body, a circulating pump 8 is installed in the first pipeline 7, the air inlet end of the first pipeline 7 and the air outlet end of the second pipeline 9 are respectively installed above and below the left side of the sealed transparent box body, the air outlet end of the first pipeline 7 and the air inlet end of the second pipeline 9 are respectively marked as an interface B and an interface A, and the two pipelines are respectively connected into a gas cylinder 10 filled with 37% of formaldehyde solution.
The power supply of the temperature and humidity controller 1 and the fan 5 are distributed outside the sealed transparent box body, the two power lines are connected with the temperature and humidity controller 1 and the fan 5 through two through holes formed in the protective door, each power line is sealed with the corresponding through hole, the temperature and humidity controller 1 can set parameters through remote control, and the temperature (30 ℃) of the ptc ceramic heating plate 4 is set on the controller.
The installation of the fan 5 can make the formaldehyde gas in the closed box body be uniformly distributed. The formaldehyde solution which is continuously volatilized is placed in a closed flask which is connected with a closed box body through a pipeline to form a closed environment, then the formaldehyde gas is circulated through a circulating pump 8 which works all the time, the concentration of the formaldehyde in the box body reaches a certain value (80-800ppb) through a period of time, and a connector A and a connector B are closed.
When formaldehyde is detected and removed, the color-changing material is cut into an original sheet shape to obtain a wafer 11, then the wafer 11 is arranged in a cylindrical glass tube 12, the diameter of the wafer 11 is the same as the inner diameter of the glass tube 12, the wafer 11 is parallel to the cross section of the glass tube 12, finally, the interface A is connected to the inlet of the glass tube 12, and the interface B is connected to the outlet of the glass tube 12.
Therefore, the formaldehyde generating device can obtain a plurality of groups of formaldehyde concentrations and corresponding total chromatic aberration, and further obtain the corresponding relation or linear equation of the formaldehyde concentrations and the total chromatic aberration.
The material is placed in a closed space with the formaldehyde concentration of 300ppb, the color of the material is changed from purple to yellow after ten minutes of response to the formaldehyde, and at the moment, the judgment can be carried out according to the depth degree of the color changed from purple to yellow, and the formaldehyde concentration value in the room is roughly determined to be 250-290 ppb. The color difference value between the color-changing material and the initial material is measured by a color reader to be 13.00, and the linear equation is substituted for calculation, so that the indoor formaldehyde concentration value is 289.57 ppb. Then the material is continuously reacted with formaldehyde, the material is changed from yellow to red, after 10 hours, the color is not continuously deepened by visual observation, a new material can be replaced, and the material is continuously adsorbed and removed. The initial color was maintained when new material was placed and no further change occurred, indicating a formaldehyde concentration of < 10ppb in the space.
The color of the porous cellulose paper in FIG. 1 corresponds to 0ppb before detection of formaldehyde, and the colors thereafter correspond to the colors of the porous cellulose paper after detection of 80ppb, 250ppb, 400ppb, 600ppb, and 800ppb of formaldehyde, respectively. Wherein 0ppb, 80ppb, 250ppb, 400ppb, 600ppb and 800ppb are directly measured by a hand-held instrument before formaldehyde is detected. The blank color is purple, the first image is light yellow, the last image is dark yellow, the yellow of the middle three images is gradually deepened, and the specific color can be deduced according to the total color difference with the blank color in the image 2.
Fig. 2 is a linear relationship curve of the total color difference of the porous cellulose paper obtained in example 1 when formaldehyde concentration in fig. 1 is detected and the total color difference after detection is 4.32, 11.84, 17.59, 23.13 and 34.64 respectively, and is shown as Δ E ab, wherein the total color difference of the porous cellulose paper before formaldehyde detection is 0, so that the formaldehyde concentration and the total color difference of the porous cellulose paper before and after adsorption are in a linear relationship, and the material can be used for formaldehyde detection.
As can be seen from the selectivity chart shown in FIG. 3, the total color difference of the porous cellulose paper after adsorbing formaldehyde is large, while the total color difference of other common VOCs gases is negligible, which indicates that the porous cellulose paper can selectively detect formaldehyde in the environment because of-NH in hydroxylamine salt2Can specifically recognize-CHO in formaldehyde, and has an aldehyde-amine condensation reaction with the-CHO.
It can be seen from fig. 5 that the color of the starting material is purple and, in addition, due to the continuous pore and volume uniformity of the tissue fiber structure, a uniform distribution of hydroxylamine sulfate and pH indicator is produced throughout the area and thus can exhibit a uniform color change when exposed to formaldehyde.
Example 2
The invention relates to a preparation method of a color-changing material for detecting and removing formaldehyde with high efficiency, low cost and quantification, which comprises the following steps:
dissolving 5g of hydroxylamine sulfate in 120mL of deionized water and 100mL of methanol, and uniformly stirring to prepare 55 parts of formaldehyde reaction reagent (solution a); adding 1 part of mixed color developing agent (0.25g of thymol blue and 0.35g of m-cresol purple) into the solution a, and uniformly stirring to obtain a solution b; to solution b was added 35 parts of glycerol (100mL) to give solution c, followed by addition of 2 parts of sodium bicarbonate (1g) to solution c to maintain the pH of the solution at 4.27 to give solution d. And (3) soaking 7 parts of white water-absorbing fibrous material sponge in the solution d in advance, performing ultrasonic treatment in an ultrasonic machine for 10min, standing for 1h, and drying in a vacuum drying oven at 30 ℃ for 30min to prepare the purple color-changing material for detecting and removing formaldehyde.
The material is placed in a closed space with the formaldehyde concentration of 800ppb, the color of the material is changed from purple to yellow after ten minutes of response to formaldehyde, the judgment can be carried out according to the shade degree of the color changed from purple to yellow, the indoor formaldehyde concentration value is roughly determined to be about 790ppb, the color difference value between the color-changing material and the initial material is measured by a color reader to be 33.90, a linear equation is substituted for calculation, and the indoor formaldehyde concentration value is 787.19 ppb. Then the material is continuously reacted with formaldehyde, the material is changed from yellow to red, after 10 hours, the color is not continuously deepened by visual observation, a new material can be replaced, and the material is continuously adsorbed and removed. The initial color was maintained when new material was placed and no further change occurred, indicating a formaldehyde concentration of < 10ppb in the space.
It can be seen from fig. 6 that the color of the starting material is purple and, in addition, due to the continuous pore and volume uniformity of the sponge, a uniform distribution of hydroxylamine sulfate and pH indicator is produced throughout the area and thus can exhibit a uniform color change when exposed to formaldehyde.
Examples 1 and 2 the data relating to the detection and removal of formaldehyde are given in the following table:
| test sample | Actual formaldehyde concentration | Detected concentration of formaldehyde | Color change |
| Example 1 | 300ppb | 289.57ppb | Purple → yellow → red |
| Example 2 | 800ppb | 787.19ppb | Purple → yellow → red |
The actual formaldehyde concentration is directly measured by a handheld instrument, and the detected formaldehyde concentration is obtained by acquiring the total color difference through a color reader and then is calculated in the corresponding relation between the formaldehyde concentration and the total color difference.
Claims (10)
1. A preparation method of a color-changing material for formaldehyde detection and removal is characterized by comprising the following steps:
step 1, uniformly mixing a hydroxylamine salt compound solution, a mixed indicator and a humectant, wherein the mixed indicator is thymol blue and m-cresol purple, the thymol blue and bromophenol blue, methyl orange and bromocresol green, alizarin yellow R and alizarin red S, or alizarin yellow R and bromophenol blue, and the mass ratio of the hydroxylamine salt compound in the mixed indicator, the humectant and the hydroxylamine salt compound solution is (1-2): (30-35):10, so as to obtain a mixed solution;
step 2, adjusting the pH value of the mixed solution to 4.25-4.5 to obtain a mixed system, soaking the porous adsorption material in the mixed system, and standing to adsorb hydroxylamine salt compounds, a mixed indicator and a humectant on the porous adsorption material to form a compound;
and 3, taking the compound out of the mixed system and drying to obtain the color-changing material for detecting and removing formaldehyde.
2. The method for preparing a color-changing material for formaldehyde detection and removal according to claim 1, wherein the hydroxylamine salt compound in step 1 is one or two of hydroxylamine hydrochloride, hydroxylamine sulfate, p-methoxybenzyloxyamine hydrochloride, O- (carboxymethyl) hydroxylamine hemihydrochloride, O-benzylhydroxylamine hydrochloride, hydroxylamine-O-sulfonic acid, O-tert-butylhydroxylamine hydrochloride;
the humectant is glycerol, sorbitol, butanediol, polyethylene glycol, propylene glycol, hexanediol, xylitol or polypropylene glycol.
3. The method for preparing a color-changing material for formaldehyde detection and removal according to claim 1, wherein the hydroxylamine salt compound solution in step 1 is obtained by the following procedure:
according to the mass ratio of (20-25) to (20-25) of 1, adding the hydroxylamine salt compound into deionized water and methanol, and uniformly stirring to obtain the hydroxylamine salt compound solution.
4. The method of claim 1, wherein the mass ratio of the first indicator to the second indicator in each of the five pairs of mixed indicators in step 1 is 5: 7.
5. The method for preparing a color-changing material for formaldehyde detection and removal according to claim 1, wherein step 2 uses one or both of sodium bicarbonate and sodium hydroxide to adjust the pH of the mixed solution;
the porous adsorption material is polyamide or cellulose sponge, porous cellulose paper, porous cellulose cloth, cellulose gel, porous silica gel, kaolin, molecular sieve, zeolite, argil or clay.
6. The method for preparing the color-changing material for formaldehyde detection and removal according to claim 1, wherein the mass ratio of the porous adsorption material in step 2 to the humectant in step 1 is (5-15): (30-35);
and 2, soaking the porous adsorption material in a mixed system, firstly carrying out ultrasonic treatment for 10-25min, and then standing for 0.5-1.5h to form a compound.
7. The method for preparing a color-changing material for formaldehyde detection and removal according to claim 1, wherein the compound is vacuum-dried at 30 to 50 ℃ for 30 to 60min in step 3.
8. A color-changing material for formaldehyde detection and removal obtained by the method for producing a color-changing material for formaldehyde detection and removal according to any one of claims 1 to 7.
9. Use of a colour change material for formaldehyde detection and removal according to claim 8, comprising the steps of:
step 1, placing the color-changing material for formaldehyde detection and removal according to claim 8 in an automobile or an indoor room for ten minutes, wherein the color-changing material adsorbs and degrades formaldehyde in the space, the color-changing material changes from the initial purple to yellow, and a total color difference is obtained compared with the color of the color-changing material before use;
step 2, cutting the color-changing material for formaldehyde detection and removal according to claim 8 into a shape with a regular pattern cross section to obtain an adsorption sheet, installing the adsorption sheet in a glass tube, and then hermetically connecting two ends of the glass tube with an air inlet end and an air outlet end of a formaldehyde generation device, wherein the adsorption sheet adsorbs and degrades formaldehyde in the formaldehyde generation device, the color-changing material is changed from the initial purple to yellow, and compared with the color of the color-changing material before use, the total color difference corresponding to the concentration of the formaldehyde in the formaldehyde generation device is obtained;
the formaldehyde generating device comprises a sealed transparent box body, wherein a temperature and humidity controller, a temperature and humidity sensor, a humidifier, a ptc ceramic heating plate and a fan are placed in the sealed transparent box body, the temperature and humidity controller is respectively connected with the temperature and humidity sensor, the ptc ceramic heating plate and the humidifier, the fan is fixed below the ptc ceramic heating plate, two pipelines are arranged outside the sealed transparent box body, a circulating pump is installed in a first pipeline, an air inlet end of the first pipeline and an air outlet end of a second pipeline are respectively installed in the sealed transparent box body, an air outlet end of the first pipeline and an air inlet end of the second pipeline are respectively connected in an air bottle filled with formaldehyde solution with volume concentration of more than 10%, when formaldehyde in the formaldehyde generating device reaches set concentration, the air outlet end of the first pipeline and the air inlet end of the second pipeline are closed, and the air outlet end of the first pipeline, The air inlet end of the second pipeline is respectively connected with the two ends of the glass tube in a sealing manner;
step 3, adjusting the concentration of formaldehyde in the formaldehyde generating device in the step 2, repeating the process in the step 2 to manufacture a new adsorption sheet, and repeating the step 2 to obtain a total color difference corresponding to the concentration of another formaldehyde in the formaldehyde generating device;
step 4, repeating the step 3 three to five times, combining the step 2 and the step 3 to obtain a plurality of groups of formaldehyde concentrations and corresponding total chromatic aberration, and obtaining a corresponding relation between the formaldehyde concentrations and the total chromatic aberration according to the plurality of groups of formaldehyde concentrations and the corresponding total chromatic aberration;
and 5, substituting the total color difference obtained in the step 1 into the corresponding relation in the step 4 to obtain the concentration of formaldehyde in the automobile or the indoor room.
10. The use of the color-changing material for formaldehyde detection and removal according to claim 8, wherein the color-changing material for formaldehyde detection and removal according to claim 8 is placed in an automobile or an indoor room for 10 hours or more, and the previous process is repeated to replace the new color-changing material until the latest color-changing material maintains the original color and does not change, and the formaldehyde concentration in the space is less than 10ppb, and the removal of formaldehyde from the automobile or the indoor room is completed.
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