CN109696497B - Automobile interior decoration material VOC qualitative and quantitative method - Google Patents
Automobile interior decoration material VOC qualitative and quantitative method Download PDFInfo
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Abstract
The invention belongs to the technical field of VOC detection, and provides a qualitative and quantitative method for VOC of an automotive interior material, which comprises the following steps: s01, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 3-6 hours, and collecting gas; s02, conveying the gas collected in S01 to a sample box, wherein the sample box contains the core-shell compound, and standing for 4-7 hours; s03, placing the core-shell compound in the sample box into a 2, 4-dinitrophenylhydrazine solution for reaction to generate a precipitate; s04 the precipitate in S03 was collected and subjected to a reverse reaction while collecting the gas and subjected to GC-O-MS test.
Description
Technical Field
The invention belongs to the technical field of VOC detection, and particularly relates to a qualitative and quantitative method for VOC of an automotive interior material.
Background
Volatile organic compounds emitted by automobiles are harmful to people, and when the VOC in the automobiles reaches a certain concentration, people feel headache, nausea and the like in a short time, and can twitch in severe cases and hurt the liver, kidney, brain and nervous system of people. VOCs are acronyms for volatile organic compounds (volatile organic compounds). VOCs in the general sense are commanding organic matters; but the definition in the environmental protection sense refers to an active class of volatile organic compounds, namely, volatile organic compounds which can cause harm. The VOC of the automotive interior material mainly includes benzene, toluene, xylene, ethylbenzene, styrene, formaldehyde, acetaldehyde, acrolein. Among them, the presence of formaldehyde increases the toxicity of benzene substances from the perspective of combined toxicity, and thus the content of formaldehyde in VOC plays an important role in combined toxicity. Meanwhile, formaldehyde is a raw material for preparing other chemicals, so that accurate recovery of formaldehyde is difficult. Therefore, a qualitative and quantitative method for formaldehyde and benzene substances in VOC is needed, which can not only perform accurate adsorption and desorption on formaldehyde substances, but also perform accurate quantitative detection on formaldehyde.
Disclosure of Invention
In order to solve the above technical problems, a first aspect of the present invention provides a method for qualitative and quantitative determination of VOC for automotive interior materials, the method comprising:
s01, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 3-6 hours, and collecting gas;
s02, conveying the gas collected in S01 to a sample box, wherein the sample box contains the core-shell compound, and standing for 4-7 hours;
s03, placing the core-shell compound in the sample box into a 2, 4-dinitrophenylhydrazine solution for reaction to generate a precipitate;
s04 the precipitate in S03 was collected and subjected to a reverse reaction while collecting the gas and subjected to GC-O-MS test.
As a preferred technical scheme, the preparation raw material of the core-shell compound contains disulfide.
As a preferred technical solution, the preparation method of the core-shell compound includes:
(1) preparing solution A of polyvinylpyrrolidone; (2) preparing a solution B of methacrylic acid and azobisisobutyronitrile; (3) under the protection of inert gas, dropwise adding the solution B into the solution A to prepare a core of the core-shell compound; (4) and (2) putting the core, formaldehyde and cobalt acetate in an acetonitrile solution, adding 4-VpY, N-methylene bisacrylamide and disulfide, adding ethylenediamine and ammonium persulfate, carrying out polymerization reaction for 5-20h, and carrying out suction filtration to obtain the core-shell microsphere, namely the core-shell compound.
As a preferred technical scheme, the reaction temperature of the S03 is 40-50 ℃.
As a preferable technical scheme, the 2, 4-dinitrophenylhydrazine solution is 0.01-0.05 g/mL of aqueous solution.
As a preferable technical scheme, the reverse reaction condition in S04 is that the pH value is in the range of 3-6.
As a preferable technical scheme, the method for collecting the precipitate in S03 in S04 is filtration collection.
As a preferred solution, the method further comprises the steps of:
s05, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 3-6 hours, and collecting gas;
s06, conveying the gas part collected in the S05 to a sample box, wherein the sample box contains the core-shell compound in the S04, and after standing for 4-7 hours, carrying out GC-O-MS test on the gas in the sample box;
s07 the other part of the gas collected in S05 was subjected to GC-O-MS test.
In a second aspect, the invention provides a core-shell compound, which is prepared by a preparation method of the core-shell compound.
In some preferred embodiments, the core-shell compound of the present invention is used for adsorbing VOCs in automotive interior parts.
The foregoing and other features, aspects, and advantages of the present application will become more readily apparent with reference to the following detailed description.
Detailed Description
Unless otherwise indicated, implied from the context, or customary in the art, all parts and percentages herein are by weight and the testing and characterization methods used are synchronized with the filing date of the present application. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definitions provided herein, the definition of the term provided herein controls.
The technical features of the technical solutions provided by the present invention are further clearly and completely described below with reference to the specific embodiments, and the scope of protection is not limited thereto.
The words "preferred", "preferably", "more preferred", and the like, in the present invention, refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention. The sources of components not mentioned in the present invention are all commercially available.
The invention provides a first aspect of a qualitative and quantitative method for VOC (volatile organic compounds) of an automotive interior material, which comprises the following steps:
s01, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 3-6 hours, and collecting gas;
s02, conveying the gas collected in S01 to a sample box, wherein the sample box contains the core-shell compound, and standing for 4-7 hours;
s03, placing the core-shell compound in the sample box into a 2, 4-dinitrophenylhydrazine solution for reaction to generate a precipitate;
s04 the precipitate in S03 was collected and subjected to a reverse reaction while collecting the gas and subjected to GC-O-MS test.
In some preferred embodiments, the method for the qualitative and quantitative determination of the VOC in the automotive interior material comprises the following steps:
s01, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 4-5 hours, and collecting gas;
s02, conveying the gas collected in S01 to a sample box, wherein the sample box contains the core-shell compound, and standing for 5-6 hours;
s03, placing the core-shell compound in the sample box into a 2, 4-dinitrophenylhydrazine solution for reaction to generate a precipitate;
s04 the precipitate in S03 was collected and subjected to a reverse reaction while collecting the gas and subjected to GC-O-MS test.
In some more preferred embodiments, the method for the qualitative and quantitative determination of the VOC in the automotive interior material comprises the following steps:
s01, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 4.5 hours, and collecting gas;
s02, conveying the gas collected in S01 to a sample box, wherein the sample box contains the core-shell compound, and standing for 5.5 hours;
s03, placing the core-shell compound in the sample box into a 2, 4-dinitrophenylhydrazine solution for reaction to generate a precipitate;
s04 the precipitate in S03 was collected and subjected to a reverse reaction while collecting the gas and subjected to GC-O-MS test.
In some embodiments, the starting materials for the preparation of the core shell compounds of the present invention comprise a disulfide.
In some preferred embodiments, the disulfide compounds of the present invention contain at least one double bond.
In some more preferred embodiments, the disulfide of the invention contains double bonds on both sides.
In some embodiments, the disulfide of the present invention is selected from the group consisting of divinyl disulfide, diallyl disulfide, propyl disulfide propylene, 1- (allyl disulfide) -1-propene, N ' - (dithiodivinyl) diethylamide, N ' - (dithiodivinyl) bis [ 3-aminopropionamide ], N ' -disulfanediylbis (N-butyl-1-butylamine), thiamine disulfide, dicyclohexyldisulfide, diphenyl disulfide, in combination with one or more of; preferably, the disulfide is selected from the group consisting of divinyl disulfide, diallyl disulfide, propyl propylene disulfide, 1- (allyl disulfide) -1-propylene in one or more combinations; more preferably, the disulfide is selected from the group consisting of divinyl disulfide, diallyl disulfide, and combinations of one or more thereof; most preferably, the disulfide is selected from diallyl disulfide.
The CAS number of the diallyl disulfide described in the present invention is 2179-57-9; the CAS number of the divinyl disulfide is 15805-34-2; the CAS number of the 1- (allyldithio) -1-propene is 33368-82-0.
In some embodiments, the method of preparing the core-shell compound of the present invention comprises:
(1) preparing solution A of polyvinylpyrrolidone; (2) preparing a solution B of methacrylic acid and azobisisobutyronitrile; (3) under the protection of inert gas, dropwise adding the solution B into the solution A to prepare a core of the core-shell compound; (4) and (2) putting the core, formaldehyde and cobalt acetate in an acetonitrile solution, adding 4-VpY, N-methylene bisacrylamide and disulfide, adding ethylenediamine and ammonium persulfate, carrying out polymerization reaction for 5-20h, and carrying out suction filtration to obtain the core-shell microsphere, namely the core-shell compound.
In some preferred embodiments, the method of preparing the core-shell compound of the present invention comprises:
(1) preparing solution A of polyvinylpyrrolidone; (2) a solution B of methacrylic acid and azobisisobutyronitrile; (3) under the protection of nitrogen atmosphere, dropwise adding the solution B into the solution A to prepare a core of the core-shell compound; (4) the core, 1-3mmol of formaldehyde and 1-3mmol of cobalt acetate are added into 5-15mL of acetonitrile solution, 5-10mmol of 4-VpY, 1-6mmol of N, N-methylene bisacrylamide and 1-6mmol of disulfide are added, 10-50 mu L of ethylenediamine and 30-60mg of ammonium persulfate are added, polymerization reaction is carried out for 5-20h at 35-50 ℃, and suction filtration is carried out to obtain the core-shell microsphere, namely the core-shell compound.
In some preferred embodiments, the method of preparing the core-shell compound of the present invention comprises:
(1) preparation of solution A: mixing polyvinylpyrrolidone (PVP for short) with distilled water, and stirring at 500-800 rpm until the PVP is completely dissolved to obtain a solution A; the concentration of PVP in the solution A is 20-40 mg/mL;
(2) preparation of solution B: adding 0.5-2mmol of toluene, 1-5mmol of 4-vinylpyridine and 0.2-1mmol of cobalt acetate into 5-15mL of methanol-tetrahydrofuran-dodecanol mixed solution, adding 0.5-1.5mmol of DMSO, carrying out ultrasonic treatment for 10-30 minutes, standing for 10-30 minutes, and adding 1-5mmol of methacrylic acid and 0.1-1mmol of azobisisobutyronitrile to obtain a solution B;
(3) preparation of the core-shell compound: under the protection of inert gas, dropwise adding the solution B into the solution A by using a constant-pressure dropping funnel, stirring at 500-700 rpm, and carrying out condensation reflux at 40-60 ℃ for 1-3 h; then, the temperature is increased to 70-80 ℃, and the reaction is carried out for 15-30 h; grinding the obtained product, sieving with 100-300 mesh sieve, and precipitating with acetone for 2-5 times; using 20-50mL of 0.05-0.2mol L-1Precipitating the EDTA solution for 2-5 times, performing Soxhlet extraction with methanol-acetic acid mixed solution at volume ratio of (8-10):1 for 35-45h, eluting with methanol for 10-15h, filtering, and vacuum drying the solid at 50-60 deg.C for 15-36h to obtain nucleus;
(4) preparation of the core-shell compound: the preparation method comprises the steps of putting a core, 1-3mmol of formaldehyde and 1-3mmol of cobalt acetate in 5-15mL of acetonitrile solution, adding 1-3mmol of DMSO, uniformly mixing, adding 5-10mmol of 4-VpY, 1-6mmol of N, N-methylene bisacrylamide and 1-6mmol of disulfide, performing ultrasonic dispersion for 25-30 min, introducing inert gas for 10-25 min to remove oxygen, adding 10-50 mu L of ethylenediamine and 30-60mg of ammonium persulfate, performing polymerization reaction for 5-20h at 35-50 ℃, and performing suction filtration to obtain the core-shell microsphere, namely the core-shell compound.
In some more preferred embodiments, the method of preparing the core-shell compound of the present invention comprises:
(1) preparation of solution A: mixing polyvinylpyrrolidone with distilled water, and stirring at 550rpm until the polyvinylpyrrolidone is completely dissolved to obtain a solution A; the concentration of PVP in the solution A is 28 mg/mL;
(2) preparation of solution B: adding 1mmol of toluene, 3mmol of 4-vinylpyridine and 0.6mmol of cobalt acetate into 10mL of methanol-tetrahydrofuran-dodecanol mixed solution, adding 1mmol of DMSO, carrying out ultrasonic treatment for 15 minutes, standing for 20 minutes, and adding 3mmol of methacrylic acid and 0.5mmol of azobisisobutyronitrile to obtain a solution B;
(3) preparation of the core-shell compound: under the protection of inert gas, dropwise adding the solution B into the solution A by using a constant-pressure dropping funnel, stirring at 600rpm, and carrying out condensation reflux at 50 ℃ for 2 hours; then the temperature is increased to 75 ℃ and the reaction is carried out for 24 hours; grinding the obtained product, sieving with 200 mesh sieve, and precipitating with acetone for 3 times; with 40mL0.1mol L-1The EDTA solution was settled 3 times, thenSoxhlet extracting with methanol-acetic acid mixed solution at volume ratio of 9:1 for 40h, eluting with methanol for 12h, filtering, and vacuum drying the solid at 55 deg.C for 24h to obtain nucleus;
(4) preparation of the core-shell compound: putting a core, 2mmol of formaldehyde and 2mmol of cobalt acetate in 10mL of acetonitrile solution, adding 2mmol of DMSO, uniformly mixing, adding 8mmol of 4-VpY, 4mmol of N, N-methylene bisacrylamide and 4mmol of disulfide, performing ultrasonic dispersion for 28min, introducing inert gas for 20min to remove oxygen, adding 30 mu L of ethylenediamine and 46.9mg of ammonium persulfate, performing polymerization reaction for 10h at 45 ℃, and performing suction filtration to obtain the core-shell microsphere, namely the core-shell compound.
The 4-VpY is 4-vinylpyridine; the DMSO is dimethyl sulfoxide; the EDTA is ethylene diamine tetraacetic acid; the volume ratio of the methanol-tetrahydrofuran-dodecanol is 1:1: 1.
The inert gas in the invention is not specially required, and includes but is not limited to any one or combination of a plurality of helium, argon and nitrogen; preferably, the inert gas is nitrogen.
In some embodiments, the reaction temperature of S03 in the present invention is 40 to 50 ℃; preferably, the reaction temperature of S03 is 45 ℃.
In some embodiments, the 2, 4-dinitrophenylhydrazine solution is 0.01-0.05 g/mL of aqueous solution; preferably, the 2, 4-dinitrophenylhydrazine solution is 0.02-0.04 g/mL of aqueous solution; more preferably, the 2, 4-dinitrophenylhydrazine solution is 0.03g/mL of aqueous solution.
In some embodiments, the reverse reaction conditions in S04 in the present invention are a pH in the range of 3 to 6; preferably, the reverse reaction condition in S04 is a pH value ranging from 4 to 5; more preferably, the reverse reaction condition in S04 is a pH of 4.
In some embodiments, the method of collecting the precipitate in S03 in S04 of the present invention is collection by filtration.
In the invention, a core-shell compound is adopted to adsorb formaldehyde, the core-shell compound is a core-shell molecular imprinting, the molecular imprinting takes formaldehyde as a template, so that the formaldehyde can be adsorbed, the formaldehyde and other VOCs in the VOCs can be separated, and the adsorbed formaldehyde and hydrazine react to generate a precipitate, so that the formaldehyde and other substances are thoroughly separated, and presumably, the core-shell molecular imprinting can adsorb the formaldehyde, and the disulfide bond on the surface of the molecular imprinting can be recombined under the alkalescent condition, so that the formaldehyde adsorbed by the molecular imprinting can be released under the alkalescent condition, and the formaldehyde and the hydrazine react to generate the precipitate; meanwhile, the precipitate can react reversely under the acidic condition to generate formaldehyde and hydrazine, and the disulfide bond is stable under the acidic condition, so that the originally adsorbed formaldehyde can be completely released, and the formaldehyde and other VOC substances can be perfectly separated, so that the content of the formaldehyde can be accurately measured, and the subsequent reutilization can be carried out.
In some embodiments, the steps of the methods of the present invention further comprise:
s05, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 3-6 hours, and collecting gas;
s06, conveying the gas part collected in the S05 to a sample box, wherein the sample box contains the core-shell compound in the S04, and after standing for 4-7 hours, carrying out GC-O-MS test on the gas in the sample box;
s07 the other part of the gas collected in S05 was subjected to GC-O-MS test.
In some preferred embodiments, the steps of the method further comprise:
s05, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 4-5 hours, and collecting gas;
s06, conveying the gas part collected in the S05 to a sample box, wherein the sample box contains the core-shell compound in the S04, and after standing for 5-6 hours, carrying out GC-O-MS test on the gas in the sample box;
s07 the other part of the gas collected in S05 was subjected to GC-O-MS test.
In some more preferred embodiments, the steps of the method further comprise:
s05, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 4.5 hours, and collecting gas;
s06, conveying the gas part collected in the S05 to a sample box, wherein the sample box contains the core-shell compound in the S04, and after standing for 5.5 hours, carrying out GC-O-MS test on the gas in the sample box;
s07 the other part of the gas collected in S05 was subjected to GC-O-MS test.
The core in the core-shell type molecular imprinting takes the benzene-containing substance as a molecular template, so that the benzene-containing substance can be adsorbed, and then the content of the benzene-containing substance is accurately measured in the subsequent GC-O-MS, so that the content ratio of formaldehyde and the benzene-containing substance can be compared, and the joint toxicity of the automobile VOC can be judged. The applicant finds that the core-shell type molecular imprinting has the advantages that the inner core can adsorb toluene, and the shell can adsorb formaldehyde; the shell raw material can enhance the adsorptivity of benzene and toluene; probably, formaldehyde has additive and synergistic effects on benzene-containing substances, the molecular imprinting prepared by the method can separate the two substances, even the two substances and the rest of VOC (volatile organic compounds), and pure formaldehyde is obtained, so that the formaldehyde is recycled.
In a second aspect, the invention provides a core-shell compound, which is prepared by a preparation method of the core-shell compound.
In some embodiments, the core shell compound is used to adsorb VOCs in automotive upholstery.
The invention provides a qualitative and quantitative method for VOC of automotive interior materials and a core-shell compound,
the present invention is described in detail below by way of examples, which are only used for further illustration of the present invention and are not to be construed as limiting the present invention, and the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are within the scope of the present invention.
Example 1
A method for qualitatively and quantitatively determining VOC of automotive interior materials comprises the following steps:
s01, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 4.5 hours, and collecting gas;
s02, conveying the gas collected in S01 to a sample box, wherein the sample box contains the core-shell compound, and standing for 5.5 hours;
s03, placing the core-shell compound in the sample box into a 2, 4-dinitrophenylhydrazine solution for reaction to generate a precipitate;
s04 collecting the precipitate in S03, carrying out reverse reaction on the precipitate, simultaneously collecting gas, and carrying out GC-O-MS test;
the preparation raw material of the core-shell compound comprises disulfide, wherein the disulfide is diallyl disulfide; the reaction temperature of the S03 is 45 ℃; the 2, 4-dinitrophenylhydrazine solution is 0.03g/mL of aqueous solution; the reverse reaction condition in S04 is pH 4; the method for collecting the precipitate in S03 in S04 is to collect the precipitate by filtration; the inert gas is nitrogen;
the preparation method of the core-shell compound comprises the following steps:
(1) preparation of solution A: mixing polyvinylpyrrolidone with distilled water, and stirring at 550rpm until the polyvinylpyrrolidone is completely dissolved to obtain a solution A; the concentration of polyvinylpyrrolidone in the solution A is 28 mg/mL;
(2) preparation of solution B: adding 1mmol of toluene, 3mmol of 4-vinylpyridine and 0.6mmol of cobalt acetate into 10mL of methanol-tetrahydrofuran-dodecanol mixed solution, adding 1mmol of DMSO, carrying out ultrasonic treatment for 15 minutes, standing for 20 minutes, and adding 3mmol of methacrylic acid and 0.5mmol of azobisisobutyronitrile to obtain a solution B;
(3) preparation of the core-shell compound: under the protection of inert gas, dropping with constant pressureDropwise adding the solution B into the solution A by using a liquid funnel, stirring at 600rpm, and carrying out condensation reflux at 50 ℃ for 2 hours; then the temperature is increased to 75 ℃ and the reaction is carried out for 24 hours; grinding the obtained product, sieving with 200 mesh sieve, and precipitating with acetone for 3 times; with 40mL0.1mol L-1Precipitating the EDTA solution for 3 times, performing Soxhlet extraction with a methanol-acetic acid mixed solution with a volume ratio of 9:1 for 40h, finally eluting with methanol for 12h, filtering, and vacuum drying the solid at 55 ℃ for 24h to obtain nuclei;
(4) preparation of the core-shell compound: putting a core, 2mmol of formaldehyde and 2mmol of cobalt acetate in 10mL of acetonitrile solution, adding 2mmol of DMSO, uniformly mixing, adding 8mmol of 4-VpY, 4mmol of N, N-methylene bisacrylamide and 4mmol of disulfide, performing ultrasonic dispersion for 28min, introducing inert gas for 20min to remove oxygen, adding 30 mu L of ethylenediamine and 46.9mg of ammonium persulfate, performing polymerization reaction for 10h at 45 ℃, and performing suction filtration to obtain a core-shell microsphere, namely the core-shell compound;
the steps of the method further comprise:
s05, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 4.5 hours, and collecting gas;
s06, conveying the gas part collected in the S05 to a sample box, wherein the sample box contains the core-shell compound in the S04, and after standing for 5.5 hours, carrying out GC-O-MS test on the gas in the sample box;
s07 the other part of the gas collected in S05 was subjected to GC-O-MS test.
Example 2
A method for qualitatively and quantitatively determining VOC of automotive interior materials comprises the following steps:
s01, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 3 hours, and collecting gas;
s02, conveying the gas collected in the S01 to a sample box, wherein the sample box contains the core-shell compound, and standing for 4 hours;
s03, placing the core-shell compound in the sample box into a 2, 4-dinitrophenylhydrazine solution for reaction to generate a precipitate;
s04 collecting the precipitate in S03, carrying out reverse reaction on the precipitate, simultaneously collecting gas, and carrying out GC-O-MS test;
the preparation raw material of the core-shell compound comprises disulfide, and the disulfide is divinyl disulfide; the reaction temperature of the S03 is 40 ℃; the 2, 4-dinitrophenylhydrazine solution is 0.01g/mL of aqueous solution; the reverse reaction condition in S04 is a pH of 3; the method for collecting the precipitate in S03 in S04 is to collect the precipitate by filtration; the inert gas is nitrogen;
the preparation method of the core-shell compound comprises the following steps:
(1) preparation of solution A: mixing polyvinylpyrrolidone with distilled water, and stirring at 500rpm until the polyvinylpyrrolidone is completely dissolved to obtain a solution A; the concentration of polyvinylpyrrolidone in the solution A is 20 mg/mL;
(2) preparation of solution B: adding 0.5mmol of toluene, 1mmol of 4-vinylpyridine and 0.2mmol of cobalt acetate into 5mL of methanol-tetrahydrofuran-dodecanol mixed solution, adding 0.5mmol of DMSO, carrying out ultrasonic treatment for 10 minutes, standing for 10 minutes, and adding 1mmol of methacrylic acid and 0.1mmol of azobisisobutyronitrile to obtain a solution B;
(3) preparation of the core-shell compound: under the protection of inert gas, dropwise adding the solution B into the solution A by using a constant-pressure dropping funnel, stirring at 500rpm, and carrying out condensation reflux for 1h at 40 ℃; then the temperature is increased to 70 ℃ and the reaction is carried out for 15 h; grinding the obtained product, sieving with 100 mesh sieve, and precipitating with acetone for 2 times; using 20mL of 0.05mol L-1The EDTA solution is settled for 2 times, then the Soxhlet extraction is carried out for 35h by using a methanol-acetic acid mixed solution with the volume ratio of 8:1, finally the elution is carried out for 10h by using methanol, the filtration is carried out, and the solid is dried for 15h under vacuum at 50 ℃ to obtain the nucleus;
(4) preparation of the core-shell compound: putting a core, 1mmol of formaldehyde and 1mmol of cobalt acetate in 5mL of acetonitrile solution, adding 1mmol of DMSO, uniformly mixing, then adding 5mmol of 4-VpY, 1mmol of N, N-methylene bisacrylamide and 1mmol of disulfide, performing ultrasonic dispersion for 25min, introducing inert gas for 10min to remove oxygen, then adding 10 mu L of ethylenediamine and 30mg of ammonium persulfate, performing polymerization reaction at 35 ℃ for 5h, and performing suction filtration to obtain a core-shell microsphere, namely the core-shell compound;
the steps of the method further comprise:
s05, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 3 hours, and collecting gas;
s06, conveying the gas part collected in the S05 to a sample box, wherein the sample box contains the core-shell compound in the S04, and after standing for 4 hours, carrying out GC-O-MS test on the gas in the sample box;
s07 the other part of the gas collected in S05 was subjected to GC-O-MS test.
Example 3
A method for qualitatively and quantitatively determining VOC of automotive interior materials comprises the following steps:
s01, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 6 hours, and collecting gas;
s02, conveying the gas collected in the S01 to a sample box, wherein the sample box contains the core-shell compound, and standing for 7 hours;
s03, placing the core-shell compound in the sample box into a 2, 4-dinitrophenylhydrazine solution for reaction to generate a precipitate;
s04 collecting the precipitate in S03, carrying out reverse reaction on the precipitate, simultaneously collecting gas, and carrying out GC-O-MS test;
the preparation raw material of the core-shell compound comprises disulfide, and the disulfide is divinyl disulfide; the reaction temperature of the S03 is 50 ℃; the 2, 4-dinitrophenylhydrazine solution is 0.05g/mL of aqueous solution; the reverse reaction condition in S04 is pH 6; the method for collecting the precipitate in S03 in S04 is to collect the precipitate by filtration; the inert gas is argon;
the preparation method of the core-shell compound comprises the following steps:
(1) preparation of solution A: mixing polyvinylpyrrolidone with distilled water, and stirring at 800rpm until the polyvinylpyrrolidone is completely dissolved to obtain a solution A; the concentration of the polyvinylpyrrolidone in the solution A is 40 mg/mL;
(2) preparation of solution B: adding 1.5mmol DMSO into a mixed solution of 2mmol toluene, 5mmol 4-vinylpyridine and 1mmol cobalt acetate in 15mL methanol-tetrahydrofuran-dodecanol, carrying out ultrasonic treatment for 30 minutes, standing for 30 minutes, and adding 1-5mmol methacrylic acid and 1mmol azobisisobutyronitrile to obtain a solution B;
(3) preparation of the core-shell compound: under the protection of inert gas, dropwise adding the solution B into the solution A by using a constant-pressure dropping funnel, stirring at 700rpm, and carrying out condensation reflux at 60 ℃ for 3 hours; then the temperature is increased to 80 ℃ and the reaction is carried out for 30 hours; grinding the obtained product, sieving with 300 mesh sieve, and precipitating with acetone for 5 times; 50mL of 0.2mol L-1Precipitating the EDTA solution for 5 times, performing Soxhlet extraction with a methanol-acetic acid mixed solution with a volume ratio of 10:1 for 45h, finally eluting with methanol for 15h, filtering, and vacuum drying the solid at 60 ℃ for 36h to obtain nuclei;
(4) preparation of the core-shell compound: putting a core, 3mmol of formaldehyde and 3mmol of cobalt acetate in 15mL of acetonitrile solution, adding 3mmol of DMSO, uniformly mixing, then adding 10mmol of 4-VpY, 6mmol of N, N-methylene bisacrylamide and 6mmol of disulfide, ultrasonically dispersing for 30min, introducing inert gas for 25min to remove oxygen, then adding 50 mu L of ethylenediamine and 60mg of ammonium persulfate, carrying out polymerization reaction at 50 ℃ for 20h, and carrying out suction filtration to obtain a core-shell microsphere, namely the core-shell compound;
the steps of the method further comprise:
s05, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 6 hours, and collecting gas;
s06, conveying the gas part collected in the S05 to a sample box, wherein the sample box contains the core-shell compound in the S04, and after standing for 7 hours, carrying out GC-O-MS test on the gas in the sample box;
s07 the other part of the gas collected in S05 was subjected to GC-O-MS test.
Example 4
A method for qualitatively and quantitatively determining VOC of automotive interior materials comprises the following steps:
s01, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 4 hours, and collecting gas;
s02, conveying the gas collected in the S01 to a sample box, wherein the sample box contains the core-shell compound, and standing for 5 hours;
s03, placing the core-shell compound in the sample box into a 2, 4-dinitrophenylhydrazine solution for reaction to generate a precipitate;
s04 collecting the precipitate in S03, carrying out reverse reaction on the precipitate, simultaneously collecting gas, and carrying out GC-O-MS test;
the preparation raw material of the core-shell compound comprises disulfide, and the disulfide is divinyl disulfide; the reaction temperature of the S03 is 45 ℃; the 2, 4-dinitrophenylhydrazine solution is 0.02g/mL of aqueous solution; the reverse reaction condition in S04 is pH 4; the method for collecting the precipitate in S03 in S04 is to collect the precipitate by filtration; the inert gas is argon;
the preparation method of the core-shell compound comprises the following steps:
(1) preparation of solution A: mixing polyvinylpyrrolidone with distilled water, and stirring at 550rpm until the polyvinylpyrrolidone is completely dissolved to obtain a solution A; the concentration of polyvinylpyrrolidone in the solution A is 28 mg/mL;
(2) preparation of solution B: adding 1mmol of toluene, 3mmol of 4-vinylpyridine and 0.6mmol of cobalt acetate into 10mL of methanol-tetrahydrofuran-dodecanol mixed solution, adding 1mmol of DMSO, carrying out ultrasonic treatment for 15 minutes, standing for 20 minutes, and adding 3mmol of methacrylic acid and 0.5mmol of azobisisobutyronitrile to obtain a solution B;
(3) preparation of the core-shell compound: under the protection of inert gas, dropwise adding the solution B into the solution A by using a constant-pressure dropping funnel, stirring at 600rpm, and carrying out condensation reflux at 50 ℃ for 2 hours; then the temperature is increased to 75 ℃ and the reaction is carried out for 24 hours; grinding the obtained product, sieving with 200 mesh sieve, and precipitating with acetone for 3 times; with 40mL0.1mol L-1Precipitating the EDTA solution for 3 times, performing Soxhlet extraction with a methanol-acetic acid mixed solution with a volume ratio of 9:1 for 40h, finally eluting with methanol for 12h, filtering, and vacuum drying the solid at 55 ℃ for 24h to obtain nuclei;
(4) preparation of the core-shell compound: putting a core, 2mmol of formaldehyde and 2mmol of cobalt acetate in 10mL of acetonitrile solution, adding 2mmol of DMSO, uniformly mixing, adding 8mmol of 4-VpY, 4mmol of N, N-methylene bisacrylamide and 4mmol of disulfide, performing ultrasonic dispersion for 28min, introducing inert gas for 20min to remove oxygen, adding 30 mu L of ethylenediamine and 46.9mg of ammonium persulfate, performing polymerization reaction for 10h at 45 ℃, and performing suction filtration to obtain a core-shell microsphere, namely the core-shell compound;
the steps of the method further comprise:
s05, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 4 hours, and collecting gas;
s06, conveying the gas part collected in the S05 to a sample box, wherein the sample box contains the core-shell compound in the S04, and after standing for 5 hours, carrying out GC-O-MS test on the gas in the sample box;
s07 the other part of the gas collected in S05 was subjected to GC-O-MS test.
Example 5
A method for qualitatively and quantitatively determining VOC of automotive interior materials comprises the following steps:
s01, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 4 hours, and collecting gas;
s02, conveying the gas collected in the S01 to a sample box, wherein the sample box contains the core-shell compound, and standing for 5 hours;
s03, placing the core-shell compound in the sample box into a 2, 4-dinitrophenylhydrazine solution for reaction to generate a precipitate;
s04 collecting the precipitate in S03, carrying out reverse reaction on the precipitate, simultaneously collecting gas, and carrying out GC-O-MS test;
the preparation raw material of the core-shell compound comprises disulfide, and the disulfide is divinyl disulfide; the reaction temperature of the S03 is 45 ℃; the 2, 4-dinitrophenylhydrazine solution is 0.02g/mL of aqueous solution; the reverse reaction condition in S04 is pH 4; the method for collecting the precipitate in S03 in S04 is to collect the precipitate by filtration; the inert gas is argon;
the preparation method of the core-shell compound comprises the following steps:
(1) preparation of solution A: mixing polyvinylpyrrolidone with distilled water, and stirring at 550rpm until the polyvinylpyrrolidone is completely dissolved to obtain a solution A; the concentration of polyvinylpyrrolidone in the solution A is 28 mg/mL;
(2) preparation of solution B: adding 1mmol of toluene, 3mmol of 4-vinylpyridine and 0.6mmol of cobalt acetate into 10mL of methanol-tetrahydrofuran-dodecanol mixed solution, adding 1mmol of DMSO, carrying out ultrasonic treatment for 15 minutes, standing for 20 minutes, and adding 3mmol of methacrylic acid and 0.5mmol of azobisisobutyronitrile to obtain a solution B;
(3) preparation of the core-shell compound: under the protection of inert gas, dropwise adding the solution B into the solution A by using a constant-pressure dropping funnel, stirring at 600rpm, and carrying out condensation reflux at 50 ℃ for 2 hours; then the temperature is increased to 75 ℃ and the reaction is carried out for 24 hours; grinding the obtained product, sieving with 200 mesh sieve, and precipitating with acetone for 3 times; with 40mL0.1mol L-1Precipitating the EDTA solution for 3 times, performing Soxhlet extraction with a methanol-acetic acid mixed solution with a volume ratio of 9:1 for 40h, finally eluting with methanol for 12h, filtering, and vacuum drying the solid at 55 ℃ for 24h to obtain nuclei;
(4) preparation of the core-shell compound: putting a core, 2mmol of formaldehyde and 2mmol of cobalt acetate in 10mL of acetonitrile solution, adding 2mmol of DMSO, uniformly mixing, adding 8mmol of 4-VpY, 4mmol of N, N-methylene bisacrylamide and 4mmol of disulfide, performing ultrasonic dispersion for 28min, introducing inert gas for 20min to remove oxygen, adding 30 mu L of ethylenediamine and 46.9mg of ammonium persulfate, performing polymerization reaction for 10h at 45 ℃, and performing suction filtration to obtain a core-shell microsphere, namely the core-shell compound;
the steps of the method further comprise:
s05, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 4 hours, and collecting gas;
s06, conveying the gas part collected in the S05 to a sample box, wherein the sample box contains the core-shell compound in the S04, and after standing for 5 hours, carrying out GC-O-MS test on the gas in the sample box;
s07 the other part of the gas collected in S05 was subjected to GC-O-MS test.
Example 6
The difference from example 1 is that the starting materials for the preparation of the core-shell compounds do not contain disulfides, and no disulfide is added in the preparation process (4) of the core-shell compounds.
Example 7
The difference from example 1 is that the disulfide is propylpropylene disulfide.
Example 8
The difference from example 1 is that the disulfide is diphenyl disulfide.
Example 9
A method for qualitatively and quantitatively determining VOC of automotive interior materials comprises the following steps:
s01, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 4.5 hours, and collecting gas;
s02 transferring the gas collected in S01 to a sample box containing the shell compound, and standing for 5.5 hours;
s03, placing the shell compound in the sample box into a 2, 4-dinitrophenylhydrazine solution for reaction to generate a precipitate;
s04 collecting the precipitate in S03, carrying out reverse reaction on the precipitate, simultaneously collecting gas, and carrying out GC-O-MS test;
the preparation raw material of the core-shell compound comprises disulfide, wherein the disulfide is diallyl disulfide; the reaction temperature of the S03 is 45 ℃; the 2, 4-dinitrophenylhydrazine solution is 0.03g/mL of aqueous solution; the reverse reaction condition in S04 is pH 4; the method for collecting the precipitate in S03 in S04 is to collect the precipitate by filtration; the inert gas is nitrogen;
adding 2mmol of formaldehyde and 2mmol of cobalt acetate into 10mL of acetonitrile solution, adding 2mmol of DMSO, uniformly mixing, adding 8mmol of 4-VpY, 4mmol of N, N-methylene bisacrylamide and 4mmol of disulfide, performing ultrasonic dispersion for 28min, introducing inert gas for 20min to remove oxygen, adding 30 mu L of ethylenediamine and 46.9mg of ammonium persulfate, performing polymerization reaction at 45 ℃ for 10h, and performing suction filtration to obtain the shell compound.
The steps of the method further comprise:
s05, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 4.5 hours, and collecting gas;
s06, conveying the gas part collected in the S05 to a sample box, wherein the sample box contains the shell compound in the S04, and after standing for 5.5 hours, carrying out GC-O-MS test on the gas in the sample box;
s07 the other part of the gas collected in S05 was subjected to GC-O-MS test.
Example 10
A method for qualitatively and quantitatively determining VOC of automotive interior materials comprises the following steps:
s01, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 4.5 hours, and collecting gas;
s02 transferring the gas collected in S01 to a sample box containing the nuclear compound, and standing for 5.5 hours;
s03, putting the nuclear compound in the sample box into a 2, 4-dinitrophenylhydrazine solution for reaction to generate a precipitate;
s04 collecting the precipitate in S03, carrying out reverse reaction on the precipitate, simultaneously collecting gas, and carrying out GC-O-MS test;
the reaction temperature of the S03 is 45 ℃; the 2, 4-dinitrophenylhydrazine solution is 0.03g/mL of aqueous solution; the reverse reaction condition in S04 is pH 4; the method for collecting the precipitate in S03 in S04 is to collect the precipitate by filtration; the inert gas is nitrogen;
the preparation method of the core-shell compound comprises the following steps:
(1) preparation of solution A: mixing polyvinylpyrrolidone with distilled water, and stirring at 550rpm until the polyvinylpyrrolidone is completely dissolved to obtain a solution A; the concentration of polyvinylpyrrolidone in the solution A is 28 mg/mL;
(2) preparation of solution B: adding 1mmol of toluene, 3mmol of 4-vinylpyridine and 0.6mmol of cobalt acetate into 10mL of methanol-tetrahydrofuran-dodecanol mixed solution, adding 1mmol of DMSO, carrying out ultrasonic treatment for 15 minutes, standing for 20 minutes, and adding 3mmol of methacrylic acid and 0.5mmol of azobisisobutyronitrile to obtain a solution B;
(3) preparation of the core compound: under the protection of inert gas, dropwise adding the solution B into the solution A by using a constant-pressure dropping funnel, stirring at 600rpm, and carrying out condensation reflux at 50 ℃ for 2 hours; then the temperature is increased to 75 ℃ and the reaction is carried out for 24 hours; grinding the obtained product, sieving with 200 mesh sieve, and precipitating with acetone for 3 times; with 40mL0.1mol L-1The EDTA solution is settled for 3 times, then the Soxhlet extraction is carried out for 40h by using a methanol-acetic acid mixed solution with the volume ratio of 9:1, finally the elution is carried out for 12h by using methanol, the filtration is carried out, and the solid is dried for 24h under vacuum at the temperature of 55 ℃ to obtain the nuclear compound;
the steps of the method further comprise:
s05, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 4.5 hours, and collecting gas;
s06, conveying the gas part collected in the S05 to a sample box, wherein the sample box contains the nuclear compound in the S04, and after standing for 5.5 hours, carrying out GC-O-MS test on the gas in the sample box;
s07 the other part of the gas collected in S05 was subjected to GC-O-MS test.
Performance testing
Test 1:
testing formaldehyde: the VOC was collected and the collected gas was divided equally into two fractions, the first fraction was measured directly by GCMS and the second fraction was measured using the method described in examples 1-10 of the present invention. And comparing the test results of the two modes, and judging the accuracy.
And (3) testing 2:
testing toluene: the VOC was collected and the collected gas was divided equally into two fractions, the first being measured directly by GCMS and the second being the core-shell compound that had been used to adsorb formaldehyde in test 1, which was used to adsorb toluene using the method described in examples 1-10 of the present invention. And comparing the test results of the two modes, and judging the accuracy.
The test results are shown in table 1:
TABLE 1
As can be seen from the test results of examples 1 to 10 in which formaldehyde and toluene were separately tested, the method described in example 1 adsorbs formaldehyde and reacts formaldehyde with hydrazine to generate a precipitate, which can completely separate formaldehyde from other substances and completely release the originally adsorbed formaldehyde, thereby accurately measuring the formaldehyde content and enabling subsequent reuse. Toluene is used as a template of molecular imprinting, so that the inner core can adsorb toluene, the shell can adsorb formaldehyde, and the shell raw material can enhance the adsorbability of benzene and toluene; toluene was adsorbed by the method of example 1, and then the gas after adsorption was tested to show that no toluene substance was detected, and the inner core had effective adsorption effect on toluene.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all equivalent variations and modifications made according to the present invention are included in the scope of the present invention.
Claims (8)
1. A qualitative and quantitative method for VOC of automotive interior materials is characterized by comprising the following steps:
s01, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 3-6 hours, and collecting gas;
s02, conveying the gas collected in S01 to a sample box, wherein the sample box contains the core-shell compound, and standing for 4-7 hours;
s03, placing the core-shell compound in the sample box into a 2, 4-dinitrophenylhydrazine solution for reaction to generate a precipitate;
s04 collecting the precipitate in S03, carrying out reverse reaction on the precipitate, simultaneously collecting gas, and carrying out GC-O-MS test;
the preparation raw material of the core-shell compound comprises disulfide, and the disulfide is selected from one or more of divinyl disulfide and diallyl disulfide;
the preparation method of the core-shell compound comprises the following steps:
(1) preparing solution A of polyvinylpyrrolidone;
(2) adding 0.5-2mmol of toluene, 1-5mmol of 4-vinylpyridine and 0.2-1mmol of cobalt acetate into 5-15mL of methanol-tetrahydrofuran-dodecanol mixed solution, adding 0.5-1.5mmol of DMSO, carrying out ultrasonic treatment for 10-30 minutes, standing for 10-30 minutes, and adding 1-5mmol of methacrylic acid and 0.1-1mmol of azobisisobutyronitrile to obtain a solution B;
(3) under the protection of inert gas, dropwise adding the solution B into the solution A to prepare a core of the core-shell compound;
(4) putting the core, formaldehyde and cobalt acetate in acetonitrile solution, adding 4-vinylpyridine, N-methylene bisacrylamide and disulfide, adding ethylenediamine and ammonium persulfate, carrying out polymerization reaction for 5-20h, and carrying out suction filtration to obtain the core-shell microsphere, namely the core-shell compound.
2. The method of claim 1, wherein the reaction temperature of S03 is 40-50 ℃.
3. The qualitative and quantitative method for VOC of automotive interior material of claim 1, characterized in that the 2, 4-dinitrophenylhydrazine solution is 0.01-0.05 g/mL of aqueous solution.
4. The method of claim 1, wherein the reverse reaction condition in S04 is pH range of 3-6.
5. The method of claim 1, wherein the step of collecting S03 precipitate in S04 is filtration collection.
6. The method of claim 1, wherein the method further comprises the steps of:
s05, taking the automobile interior trim, preparing the automobile interior trim into a sample of 100mm multiplied by 100mm, putting the sample into a 10L Tedlar air bag, placing the sample in an oven at 65 +/-2 ℃ for 3-6 hours, and collecting gas;
s06, conveying the gas part collected in the S05 to a sample box, wherein the sample box contains the core-shell compound in the S04, and after standing for 4-7 hours, carrying out GC-O-MS test on the gas in the sample box;
s07 the other part of the gas collected in S05 was subjected to GC-O-MS test.
7. A core-shell compound is characterized by being prepared by the following steps:
(1) preparing solution A of polyvinylpyrrolidone;
(2) adding 0.5-2mmol of toluene, 1-5mmol of 4-vinylpyridine and 0.2-1mmol of cobalt acetate into 5-15mL of methanol-tetrahydrofuran-dodecanol mixed solution, adding 0.5-1.5mmol of DMSO, carrying out ultrasonic treatment for 10-30 minutes, standing for 10-30 minutes, and adding 1-5mmol of methacrylic acid and 0.1-1mmol of azobisisobutyronitrile to obtain a solution B;
(3) under the protection of inert gas, dropwise adding the solution B into the solution A to prepare a core of the core-shell compound;
(4) putting the core, formaldehyde and cobalt acetate in acetonitrile solution, adding 4-vinylpyridine, N-methylene bisacrylamide and disulfide, adding ethylenediamine and ammonium persulfate, carrying out polymerization reaction for 5-20h, and carrying out suction filtration to obtain core-shell microspheres, namely the core-shell compound;
the disulfide is selected from one or more of divinyl disulfide and diallyl disulfide.
8. The core shell compound of claim 7, for use in adsorbing VOCs in automotive upholstery.
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