CN109001193B - Preparation method of formaldehyde detection membrane - Google Patents
Preparation method of formaldehyde detection membrane Download PDFInfo
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- CN109001193B CN109001193B CN201810591227.6A CN201810591227A CN109001193B CN 109001193 B CN109001193 B CN 109001193B CN 201810591227 A CN201810591227 A CN 201810591227A CN 109001193 B CN109001193 B CN 109001193B
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Abstract
The invention discloses a preparation method of a formaldehyde detection membrane patch, which comprises the steps of loading and wrapping formaldehyde probe molecules by using a ternary photo-crosslinkable random copolymer P (St-co-VM-co-AMPS), preparing photo-crosslinkable polymer nanoparticles carrying the formaldehyde probe molecules, crosslinking the nanoparticles by ultraviolet irradiation, fixing the probe molecules, enhancing the stability of the probe molecules, and printing a nanoparticle solution on filter paper by an ink-jet printing technology at a certain pH and temperature to form a coating to obtain formaldehyde detection test paper; then, the pressure-sensitive adhesive is pasted on one surface of the formaldehyde detection film, and then the formaldehyde detection film is obtained by compounding the release paper, so that the formaldehyde detection film is very convenient and fast to use.
Description
Technical Field
The invention belongs to the field of high polymer materials and environmental detection, and particularly relates to a preparation method of a formaldehyde detection membrane.
Background
Formaldehyde is irritant and suffocating at normal temperature, is colorless gas, has great harm to human bodies, is one of environmental pollutants which is increasingly emphasized, and is one of the genuine pollutions of decoration in China.
In recent years, with the progress of chemical detection and analysis technology, rapid detection of formaldehyde has been rapidly developed, and formaldehyde test paper is a commonly used detection method, but the test paper has a short storage period due to easy migration of probe molecules.
Patent CN103819693A reports a preparation method of formaldehyde-sensitive nanoparticles, specifically, polymer P (St-alt-Man) is adopted as a carrier, and a formaldehyde detection probe is wrapped and loaded in the polymer carrier, so that the problem of instability of a small molecular probe is solved.
However, how to implement such nanoparticle solution into a device and a series of problems are encountered in the process of implementing the device, for example, the encapsulation performance of the polymer carrier to the probe molecules is not good, the probe molecules are easy to migrate out of the polymer carrier, and thus the stability of the nanoparticles cannot be guaranteed.
The photosensitive polymer is a macromolecular compound containing photosensitive elements in a polymer structure, and can be used for crosslinking polymer materials to different degrees through ultraviolet irradiation. Supposing that the photosensitive polymer nanoparticles wrapping the formaldehyde probe are prepared by adopting the polymer as a carrier, and ultraviolet irradiation crosslinking is carried out on the photosensitive polymer nanoparticles, so that probe molecules are fixed in the nanoparticles, the migration of the probe molecules can be avoided, the stability of the nanoparticles is improved, and the device formation is facilitated.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a formaldehyde detection film, which is characterized in that a pressure-sensitive adhesive layer is arranged on one surface of formaldehyde detection test paper, and then the formaldehyde detection test paper is prepared by compounding the pressure-sensitive adhesive layer and release paper, wherein the formaldehyde detection test paper is prepared by the following steps:
(1) synthesis of the Probe molecule KD-XA01
Dissolving 1 g of phenyl-1, 3-butanedione in 60ml of benzene, adding 3.08g of ammonium acetate and 1ml of acetic acid, refluxing at 80 ℃ for 12 hours in a nitrogen atmosphere to obtain a product, washing and drying the reaction product, and removing the solvent;
(2) synthesis of ternary photo-crosslinkable random copolymer P (St-co-VM-co-AMPS)
Dissolving 7.8g of AMPS (2-acrylamido-2-methylpropanesulfonic acid) monomer, 2.4g of styrene St and 1.2g of VM monomer in 15ml of DMF, stirring and introducing N2, adding AET0.34g and AIBN0.16g after 15min, introducing N215min again, sealing the bottle mouth, transferring into an oil bath at 70 ℃, reacting for 8 hours, taking a cup substrate, precipitating in acetone, dissolving with water, dialyzing, and freeze-drying to obtain a copolymer P (St-co-VM-co-AMPS);
(3) preparation of nanoparticle solutions
Weighing KD-XA010.03g, dissolving the KD-XA010.03g in 10ml of DMF, simultaneously weighing 5mg of polymer P (St-co-VM-co-AMPS) and dissolving in 100ml of water, slowly dropwise adding the polymer water solution into a DMF solution containing KD-XA01, and stirring to obtain a nano particle solution;
(4) nanoparticle photocrosslinking
Exposing the nanoparticle solution obtained in the step (3) under an ultraviolet lamp, and carrying out photo-crosslinking to fix probe molecules in the nanoparticles to obtain a crosslinked nanoparticle solution;
(5) preparation of test paper
And (3) adjusting the pH value of the crosslinked nano particle solution obtained in the step (4) to be about 2.5-3, filtering the solution by a filter membrane, keeping the temperature at 5-25 ℃, adding the solution into an ink box of an ink-jet printer, printing the surface of the filter paper of the A4 printing paper with the filter paper stuck on the surface, repeatedly printing for three times to ensure that enough probes form a uniform coating on the surface of the filter paper, and cutting the uniform coating into small pieces to obtain the test paper for detecting formaldehyde.
Preferably, the pH is adjusted to 2.85 in step (4).
Preferably, the temperature is maintained at 5 ℃ in step (4).
Preferably, the pressure-sensitive adhesive layer is an acrylic pressure-sensitive adhesive.
The application method of the formaldehyde detection membrane sticker is characterized by comprising the following steps: the release paper is torn off, and then the film is attached to an object to be attached in the environment to be detected, for example, the film is attached to the surface of a refrigerator at home to indicate whether formaldehyde exists in the home environment.
The invention has the beneficial effects that: (1) ternary photo-crosslinkable random copolymer P (St-co-VM-co-AMPS) is used as a polymer carrier, formaldehyde probe molecules are loaded and wrapped to prepare photo-crosslinkable polymer nanoparticles carrying the formaldehyde probe molecules, and the nanoparticles are crosslinked through ultraviolet irradiation, so that the probe molecules are fixed, and the stability of the probe molecules is enhanced. (2) And (3) printing the crosslinked nano particle solution on filter paper by an ink-jet printing technology at a certain pH and temperature to form a coating, so as to obtain the formaldehyde detection test paper and realize the device formation of the nano particles. The technological parameters of pH and temperature before sample injection of the ink-jet printer are optimized, and the optimal detection effect is ensured. (3) Make the convenient to use's pad pasting with the test paper, it can to tear off during the use from type paper, for example can paste in the refrigerator of living at home to remind at every moment whether there is formaldehyde to exist at home.
Drawings
FIG. 1 TEM image of P (St-co-VM-co-AMPS) nanoparticles encapsulating a probe molecule.
FIG. 2 shows the formaldehyde detection effect of nanoparticle solutions at different pH values.
FIG. 3 shows the formaldehyde detection effect of the nanoparticle solution at different temperatures.
FIG. 4 is a schematic view of an ink jet printer.
FIG. 5 shows the test effect of formaldehyde test paper.
FIG. 6 is a schematic view of a formaldehyde detecting patch.
In fig. 6, the layers are specifically as follows: 1 formaldehyde detection test paper layer, 2 pressure sensitive adhesive layer and 3 release layer.
Detailed Description
The present invention will be described in further detail with reference to examples, but the scope of the present invention is not to be construed as being limited thereto.
Example 1
(1) Synthesis of the Probe molecule KD-XA01
3.24g of 1-phenyl-1, 3-butanedione was dissolved in 60ml of benzene, 3.08g of ammonium acetate and 1ml of acetic acid were added, and the mixture was refluxed at 80 ℃ for 12 hours under a nitrogen atmosphere to obtain a product, and the reaction was washed, dried, and the solvent was removed.
(2) Synthesis of ternary photo-crosslinkable random copolymer P (St-co-VM-co-AMPS)
Dissolving 7.8g of AMPS monomer, 2.4g of styrene St2.4g and 1.2g of VM monomer in 15ml of DMF, stirring and introducing N2, adding 0.34g of AET0.16g and 0.16g of AIBNN after 15min, sealing the bottle mouth, transferring into an oil bath at 70 ℃, taking a cup substrate after reacting for 8 hours, precipitating in acetone, dissolving with water, dialyzing, and freeze-drying to obtain the copolymer P (St-co-VM-co-AMPS).
(3) Preparation of nanoparticle solutions
KD-XA010.03g is weighed and dissolved in 10ml of DMF, while 5mg of polymer P (St-co-VM-co-AMPS) is weighed and dissolved in 100ml of water, the aqueous polymer solution is slowly dropped into the DMF solution containing KD-XA01, and stirring is carried out, thus obtaining the nanoparticle solution.
(4) Nanoparticle photocrosslinking
And (4) exposing the nanoparticle solution obtained in the step (3) under an ultraviolet lamp, and carrying out photo-crosslinking to fix the probe molecules in the nanoparticles to obtain a crosslinked nanoparticle solution.
(5) Preparation of test paper
And (3) adjusting the pH value of the crosslinked nano particle solution obtained in the step (4) to be about 2.85, filtering the solution by using a filter membrane, keeping the temperature at 5 ℃, adding the solution into an ink box of an ink-jet printer, printing the solution on the filter paper surface of the A4 printing paper with the filter paper adhered on the surface, repeatedly printing for three times to ensure that enough probes form a uniform coating on the surface of the filter paper, and cutting the solution into small pieces to obtain the test paper for formaldehyde detection.
Example 2
The pH was set to 3.65 in step (5) in example 1, and the rest was not changed.
Example 3
The pH was set to 4.68 in step (5) in example 1, and the rest was not changed.
Example 4
The pH was set to 5.54 in step (5) in example 1, and the rest was not changed.
Example 5
The pH was set to 6.32 in step (5) in example 1, and the rest was not changed.
Example 6
The temperature in step (5) in example 1 was set to 15 ℃ and was not changed in any other way.
Example 7
The temperature in step (5) in example 1 was set to 25 ℃ and was not changed in any other way.
Example 8
The temperature in step (5) in example 1 was set to 35 ℃ and was not changed otherwise.
Example 9
The temperature in step (5) in example 1 was set to 45 ℃ and was not changed in any other way.
Example 10
One side of the test paper in the example 1 is pasted with acrylic acid series pressure-sensitive adhesive, and then is compounded with release paper to prepare the formaldehyde detection film (as shown in figure 6), and the release paper is torn off when in use.
As shown in FIGS. 1 to 3, P (St-co-VM-co-AMPS) nanoparticles are spheroidal particles, and the detection effect is the best when the pH is 2.85, but is not obvious when the pH is 4.68 or more. The detection effect is better when the temperature is within the range of 5-25 ℃, and the detection effect is not good when the temperature is above 35 ℃. Fig. 2 and fig. 3 show that the solutions have the most obvious yellowing at pH 2.85 and temperature 5 ℃, i.e. the best detection effect, so that the optimal process condition is to adjust the pH of the nanoparticle solution to 2.85 and control the temperature to 5 ℃ before the injection of the ink-jet printer. The photo-crosslinked nanoparticle solution with the adjusted pH and temperature was printed on the surface of the filter paper by the inkjet printer of fig. 4 to form a uniform coating layer, and a formaldehyde test paper was obtained, which turned yellow in color when encountering formaldehyde (fig. 5).
Claims (3)
1. A preparation method of a formaldehyde detection membrane paste is characterized by comprising the following steps: the formaldehyde detection test paper is prepared by arranging a pressure-sensitive adhesive layer on one surface of the formaldehyde detection test paper and compounding the pressure-sensitive adhesive layer with release paper, and the formaldehyde detection test paper is prepared by the following steps:
(1) synthesis of the Probe molecule KD-XA01
Dissolving 1 g of phenyl-1, 3-butanedione in 60ml of benzene, adding 3.08g of ammonium acetate and 1ml of acetic acid, refluxing at 80 ℃ for 12 hours in a nitrogen atmosphere to obtain a product, washing and drying the reaction product, and removing the solvent;
(2) synthesis of ternary photo-crosslinkable random copolymer P (St-co-VM-co-AMPS)
Dissolving 7.8g of AMPS monomer, 2.4g of styrene St2.4g and 1.2g of VM monomer in 15ml of DMF, and stirring to introduce N2Adding AET0.34g and AIBN0.16g after 15min, and introducing N2Sealing the bottle opening for 15min, transferring into 70 ℃ oil bath, reacting for 8 hours, taking a cup substrate, precipitating in acetone, dissolving with water, dialyzing, and freeze-drying to obtain a copolymer P (St-co-VM-co-AMPS);
(3) preparation of nanoparticle solutions
Weighing KD-XA010.03g, dissolving the KD-XA010.03g in 10ml of DMF, simultaneously weighing 5mg of polymer P (St-co-VM-co-AMPS) and dissolving in 100ml of water, slowly dropwise adding the polymer water solution into a DMF solution containing KD-XA01, and stirring to obtain a nano particle solution;
(4) nanoparticle photocrosslinking
Exposing the nanoparticle solution obtained in the step (3) under an ultraviolet lamp, and carrying out photo-crosslinking to fix probe molecules in the nanoparticles to obtain a crosslinked nanoparticle solution;
(5) preparation of test paper
And (3) adjusting the pH value of the crosslinked nano particle solution obtained in the step (4) to 2.85, filtering the solution by a filter membrane, keeping the temperature at 5-25 ℃, adding the solution into an ink box of an ink-jet printer, printing on the surface of the filter paper of the A4 printing paper with the filter paper adhered on the surface, repeatedly printing for three times to ensure that enough probes form a uniform coating on the surface of the filter paper, and cutting the coating into small pieces to obtain the test paper for formaldehyde detection.
2. The preparation method of the formaldehyde detection membrane sticker as claimed in claim 1, wherein the preparation method comprises the following steps: in the preparation process of the formaldehyde test paper, the temperature is kept at 5 ℃ in the step (5).
3. The preparation method of the formaldehyde detection membrane sticker as claimed in claim 1, wherein the preparation method comprises the following steps: the pressure-sensitive adhesive layer is acrylic acid series pressure-sensitive adhesive.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63221235A (en) * | 1987-03-09 | 1988-09-14 | Endou Fumio | Detection of formaldehyde in clothing |
| CN101812182A (en) * | 2010-02-02 | 2010-08-25 | 江南大学 | Preparation method of photoelectric sensitive charged nanometer particles |
| CN103819693A (en) * | 2014-03-14 | 2014-05-28 | 江南大学 | Preparation method of formaldehyde sensitive type nanoparticle solution |
| CN103819703A (en) * | 2014-03-14 | 2014-05-28 | 江南大学 | Preparation method of formaldehyde sensitive type hyaluronic acid film sensor |
| CN103865217A (en) * | 2014-03-14 | 2014-06-18 | 江南大学 | Polyvinyl alcohol membrane material with formaldehyde detection effect and preparation method thereof |
| CN205719999U (en) * | 2016-06-21 | 2016-11-23 | 上海瑞鑫科技仪器有限公司 | Formaldehyde in food Test paper |
-
2018
- 2018-06-10 CN CN201810591227.6A patent/CN109001193B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63221235A (en) * | 1987-03-09 | 1988-09-14 | Endou Fumio | Detection of formaldehyde in clothing |
| CN101812182A (en) * | 2010-02-02 | 2010-08-25 | 江南大学 | Preparation method of photoelectric sensitive charged nanometer particles |
| CN103819693A (en) * | 2014-03-14 | 2014-05-28 | 江南大学 | Preparation method of formaldehyde sensitive type nanoparticle solution |
| CN103819703A (en) * | 2014-03-14 | 2014-05-28 | 江南大学 | Preparation method of formaldehyde sensitive type hyaluronic acid film sensor |
| CN103865217A (en) * | 2014-03-14 | 2014-06-18 | 江南大学 | Polyvinyl alcohol membrane material with formaldehyde detection effect and preparation method thereof |
| CN205719999U (en) * | 2016-06-21 | 2016-11-23 | 上海瑞鑫科技仪器有限公司 | Formaldehyde in food Test paper |
Non-Patent Citations (2)
| Title |
|---|
| 双亲性无规共聚物P(VM-co-AMPS)的自组装及其性能;郑俊超 等;《功能高分子学报》;20110930;第24卷(第3期);全文 * |
| 双亲性无规共聚物自组装胶束结构及其乳化性能;刘娜 等;《物理化学学报》;20130228;第29卷(第2期);全文 * |
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