CN114292438B - Preparation method of yellowing-resistant long-acting anti-aging material - Google Patents
Preparation method of yellowing-resistant long-acting anti-aging material Download PDFInfo
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- CN114292438B CN114292438B CN202210181737.2A CN202210181737A CN114292438B CN 114292438 B CN114292438 B CN 114292438B CN 202210181737 A CN202210181737 A CN 202210181737A CN 114292438 B CN114292438 B CN 114292438B
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- 239000000463 material Substances 0.000 title claims abstract description 47
- 230000003712 anti-aging effect Effects 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000004383 yellowing Methods 0.000 title claims abstract description 17
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 39
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052751 metal Inorganic materials 0.000 claims abstract description 24
- 239000002184 metal Substances 0.000 claims abstract description 24
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000013384 organic framework Substances 0.000 claims abstract description 23
- -1 salt compound Chemical class 0.000 claims abstract description 23
- IPJGAEWUPXWFPL-UHFFFAOYSA-N 1-[3-(2,5-dioxopyrrol-1-yl)phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1=CC=CC(N2C(C=CC2=O)=O)=C1 IPJGAEWUPXWFPL-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002351 wastewater Substances 0.000 claims abstract description 18
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003513 alkali Substances 0.000 claims abstract description 17
- 239000013522 chelant Substances 0.000 claims abstract description 17
- 229940018564 m-phenylenediamine Drugs 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 12
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 12
- 230000032683 aging Effects 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- VIQSRHWJEKERKR-UHFFFAOYSA-L disodium;terephthalate Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=C(C([O-])=O)C=C1 VIQSRHWJEKERKR-UHFFFAOYSA-L 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000011592 zinc chloride Substances 0.000 claims description 6
- 235000005074 zinc chloride Nutrition 0.000 claims description 6
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- 229910001510 metal chloride Inorganic materials 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 229940078552 o-xylene Drugs 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 150000003841 chloride salts Chemical class 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 229920000642 polymer Polymers 0.000 abstract description 5
- 239000004636 vulcanized rubber Substances 0.000 abstract description 5
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 238000006068 polycondensation reaction Methods 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- KEQFTVQCIQJIQW-UHFFFAOYSA-N N-Phenyl-2-naphthylamine Chemical compound C=1C=C2C=CC=CC2=CC=1NC1=CC=CC=C1 KEQFTVQCIQJIQW-UHFFFAOYSA-N 0.000 description 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 4
- VWOZHZWEKUOWRA-PLNGDYQASA-N C1=CC2=CC(=C1)N2C(=O)/C=C\C(=O)N Chemical compound C1=CC2=CC(=C1)N2C(=O)/C=C\C(=O)N VWOZHZWEKUOWRA-PLNGDYQASA-N 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- AAEHPKIXIIACPQ-UHFFFAOYSA-L calcium;terephthalate Chemical compound [Ca+2].[O-]C(=O)C1=CC=C(C([O-])=O)C=C1 AAEHPKIXIIACPQ-UHFFFAOYSA-L 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011976 maleic acid Substances 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- UYISKGVFPMWFJV-UHFFFAOYSA-N terephthalic acid;zinc Chemical compound [Zn].OC(=O)C1=CC=C(C(O)=O)C=C1 UYISKGVFPMWFJV-UHFFFAOYSA-N 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 206010027439 Metal poisoning Diseases 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000003878 thermal aging Methods 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a preparation method of a yellowing-resistant long-acting anti-aging material, which comprises the following specific preparation processes: s1, preparing a terephthalic acid metal salt compound organic framework material by using alkali deweighting wastewater; s2, adding m-phenylenediamine into the prepared maleic anhydride organic solution to obtain m-phenylene bismaleimide; s3, under continuous stirring, compounding an organic framework material with terephthalic acid metal salt and m-phenylene bismaleimide according to a certain mass ratio to dissolve in dimethylformamide to obtain a coordination chelate; s4, crushing the chelate prepared in the step S3 at normal temperature to obtain a target product. In the invention, the m-phenylene maleic amide polymer prepared by polycondensation of maleic anhydride and m-phenylenediamine has reactive NH groups and maleic double bonds on the polymer, and can play a role in protecting and stabilizing the degradation of vulcanized rubber.
Description
Technical Field
The invention belongs to the field of rubber additives, and relates to a preparation method of a yellowing-resistant long-acting anti-aging material.
Background
In the use process of the rubber, the rubber can be aged under the influence of external factors (such as ozone aging, thermal oxidation aging and the like), so that the physical and mechanical properties of the rubber are changed, the rubber loses elasticity, the mechanical properties are reduced, and the service life is shortened. In order to solve the problem of rubber aging, it is necessary to add an anti-aging material to the rubber in order to inhibit or delay the aging process and to extend the service life.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides the preparation method of the yellowing-resistant long-acting anti-aging material, which takes the metal terephthalate compound organic framework material as a carrier, and the m-phenylene bismaleimide is loaded in the coordination chelate in the framework, thereby being beneficial to the compatibility of the metal terephthalate and the rubber, improving the mechanical strength and the ultraviolet light resistance stability of the rubber and improving the oxidation resistance of the rubber.
A preparation method of a yellowing-resistant long-acting anti-aging material comprises the following specific preparation processes:
s1, preparing a terephthalic acid metal salt compound organic framework material by using alkali deweighting wastewater;
s2, preparing a maleic anhydride organic solution in a reaction kettle, then adding a certain amount of m-phenylenediamine into the prepared maleic anhydride organic solution, heating to 120-150 ℃ under normal pressure, mixing and refluxing for 4-8 hours, filtering, washing, and vacuum drying at 50 ℃ to obtain m-phenylene bismaleimide;
s3, under the condition of continuous stirring, dissolving a terephthalic acid metal salt compound organic framework material and m-phenylene bismaleimide in dimethylformamide according to a certain mass ratio, heating to 45-50 ℃, preserving heat for 30-60min, and then evaporating a mixture of the dimethylformamide and water in vacuum to obtain a coordination chelate;
s4, crushing the chelate prepared in the step S3 at normal temperature to obtain a target product.
Preferably, the specific preparation steps of the step S1 are as follows:
s1-1: decolorizing and removing impurities from the alkali-reduced wastewater, and adjusting the pH value of the alkali-reduced wastewater to 7.5-9;
s1-2: and (2) adding the pre-prepared metal chloride solution into the alkali reduction wastewater treated in the step (S1-1), uniformly mixing and stirring to react for 20-120min, and filtering, washing and drying to obtain the terephthalic acid metal salt compound organic framework material.
Preferably, the main component of the alkali deweighting wastewater after the decoloring and impurity removing treatment in the step S1-1 is sodium terephthalate, and the content is 98.6% or more.
Preferably, the metal chloride salt solution in the step S1-2 is a mixed solution of a calcium chloride solution and a zinc chloride solution, wherein the mass fraction of the calcium chloride solution is 25% -50%, and the mass fraction of the zinc chloride solution is 15% -30%.
Preferably, in the step S1-2, n (ca2+) +n (zn2+): n (sodium terephthalate) =1-1.1:1.
Preferably, in the step S2, the solvent of the maleic acid organic solution is o-xylene, and the concentration of the maleic anhydride organic solution is 2mol/L.
Preferably, the molar ratio of the maleic anhydride to the m-phenylenediamine is 1:1.
Preferably, the mass ratio of the terephthalic acid metal salt compounded organic framework material to the m-phenylene bismaleimide is 1-5:1.
The beneficial effects are that: the invention provides a preparation method of a yellowing-resistant long-acting anti-aging material, which has the following advantages:
(1) In the reaction process, the m-phenylene maleic amide polymer is prepared by polycondensation of maleic acid and m-phenylenediamine, has reactive NH groups and maleic double bonds on the polymer, and can protect and stabilize the degradation of vulcanized rubber.
(2) The target product of the invention is a coordination chelate which takes terephthalic acid metal salt compound organic framework material as a carrier and takes m-phenylene bismaleimide as a carrier to be loaded in the framework, thereby improving the stability of amino.
(3) The calcium terephthalate can be used as an auxiliary agent to improve the mechanical strength of the rubber;
(4) The calcium terephthalate and the zinc terephthalate have good complexing effect on heavy metal ions, can stabilize the heavy metal ions, and play a role in preventing metal poisoning.
Detailed Description
In order to better understand the technical solutions in the present application, the following description will clearly and completely describe the technical solutions in the embodiments of the present application, and it is obvious that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without making any inventive effort, shall fall within the scope of the present application.
A preparation method of a yellowing-resistant long-acting anti-aging material comprises the following specific preparation processes:
s1, preparing a terephthalic acid metal salt compound organic framework material by using alkali deweighting wastewater;
s2, preparing a maleic anhydride organic solution in a reaction kettle, then adding a certain amount of m-phenylenediamine into the prepared maleic anhydride organic solution, heating to 120-150 ℃ under normal pressure, mixing and refluxing for 4-8 hours, filtering, washing, and vacuum drying at 50 ℃ to obtain m-phenylene bismaleimide;
s3, under the condition of continuous stirring, dissolving a terephthalic acid metal salt compound organic framework material and m-phenylene bismaleimide in dimethylformamide according to a certain mass ratio, heating to 45-50 ℃, preserving heat for 30-60min, and then evaporating a mixture of the dimethylformamide and water in vacuum to obtain a coordination chelate;
s4, crushing the chelate prepared in the step S3 at normal temperature to obtain a target product.
The specific steps for preparing the terephthalic acid metal salt compound organic framework material by using the alkali deweighting wastewater are as follows:
s1-1: the alkali deweighting wastewater is decolored and decontaminated, the pH value of the alkali deweighting wastewater is regulated to 7.5, and the main component of the alkali deweighting wastewater after the decoloration and decontaminating treatment is sodium terephthalate with the content of 98.6 percent;
s1-2: and (2) adding the pre-prepared metal chloride solution into the alkali-reduction wastewater treated in the step (S1-1), uniformly mixing and stirring for reacting for 20-120min, and then filtering, washing and drying to obtain the terephthalic acid metal salt compound organic framework material, wherein the mixed solution of the calcium chloride solution and the zinc chloride solution is 25% by mass, the zinc chloride solution is 30% by mass, and the ratio of the total added molar quantity of calcium ions and zinc ions to the molar quantity of sodium terephthalate is 1.
The metal terephthalate compound organic framework material prepared according to the above steps is the metal terephthalate compound organic framework material used in examples 1-3.
Example 1
The preparation method of the yellowing-resistant long-acting anti-aging material comprises the following steps: adding a certain amount of m-phenylenediamine (the molar ratio of maleic anhydride to m-phenylenediamine is 1:1) into 2mol/L maleic anhydride organic solution, heating to 145 ℃ under normal pressure, mixing, refluxing for 5 hours, filtering, washing, and vacuum drying at 50 ℃ to obtain m-phenylene bismaleimide (the molar ratio of maleic anhydride to m-phenylenediamine is 1:1); under continuous stirring, dissolving a metal terephthalate compound organic framework material and m-phenylene bismaleimide in dimethylformamide according to a certain mass ratio (the mass ratio of the metal terephthalate compound organic framework material to the m-phenylene bismaleimide is 5:1), heating to 50 ℃, preserving heat for 30min, and then evaporating a mixture of the dimethylformamide and water in vacuum to obtain a coordination chelate; and (3) crushing the chelate prepared in the step (S3) at normal temperature to obtain a target product.
Example 2
The preparation method of the yellowing-resistant long-acting anti-aging material comprises the following steps: adding a certain amount of m-phenylenediamine (the molar ratio of maleic anhydride to m-phenylenediamine is 1:1) into 2mol/L maleic anhydride organic solution, heating to 145 ℃ under normal pressure, mixing, refluxing for reaction for 6 hours, filtering, washing, and vacuum drying at 50 ℃ to obtain m-phenylene bismaleimide (the molar ratio of maleic anhydride to m-phenylenediamine is 1:1); under continuous stirring, dissolving a metal terephthalate compound organic framework material and m-phenylene bismaleimide in dimethylformamide according to a certain mass ratio (the mass ratio of the metal terephthalate compound organic framework material to the m-phenylene bismaleimide is 3:1), heating to 45 ℃, preserving heat for 45min, and then evaporating a mixture of the dimethylformamide and water in vacuum to obtain a coordination chelate; and (3) crushing the chelate prepared in the step (S3) at normal temperature to obtain a target product.
Example 3
The preparation method of the yellowing-resistant long-acting anti-aging material comprises the following steps: adding a certain amount of m-phenylenediamine (the molar ratio of maleic anhydride to m-phenylenediamine is 1:1) into 2mol/L maleic anhydride organic solution, heating to 150 ℃ under normal pressure, mixing, refluxing for reaction for 8 hours, filtering, washing, and vacuum drying at 50 ℃ to obtain m-phenylene bismaleimide (the molar ratio of maleic anhydride to m-phenylenediamine is 1:1); under continuous stirring, dissolving a terephthalic acid metal salt compound organic framework material and m-phenylene bismaleimide in dimethylformamide according to a certain mass ratio (the mass ratio of the terephthalic acid metal salt compound organic framework material to the m-phenylene bismaleimide is 1:1)), heating to 45 ℃, preserving heat for 60min, and then evaporating a mixture of the dimethylformamide and water in vacuum to obtain a coordination chelate; and (3) crushing the chelate prepared in the step (S3) at normal temperature to obtain a target product.
The solvent of the maleic acid organic solution used in examples 1 to 3 was o-xylene, and the concentration of the maleic anhydride organic solution was 2mol/L. Examples 1, 2, 3 and phenyl-beta-naphthylamine (PBN, commercial grade) were kneaded according to the compounding formulation shown in table 1 to give samples 1, 2, 3 and 4, respectively.
Table 1: mixing formula
(1) The rubber materials obtained by mixing the samples 1, 2, 3 and 4 are respectively subjected to physical and mechanical property test and weather-proof aging test before aging and after aging (100 ℃ multiplied by 7 d) according to the national standard.
The weather-proof aging test method comprises the following steps: taking the same standard sample, cutting the sample into equal 3 pieces according to the length direction of the sample and the calendaring and extruding directions, folding the sample according to 360 degrees, fixing the same part of the sample, then placing the sample at the sun-facing position of the same position, and observing the aging condition of the surface of the sample.
The test results are shown in Table 2:
TABLE 2 results of mechanical Properties and thermal aging resistance test of samples
From the above experimental results, the following conclusions were drawn:
1) The addition of the anti-aging material of the invention can lead the heat aging resistance of NR vulcanized rubber to exceed that of the antioxidant PBN commonly used in the rubber industry, which is not only due to the benzene ring structure, but also due to the effect that the double bond of the maleic acid part can capture free radicals.
2) The physical and mechanical properties of NR vulcanized rubber are superior to those of an antioxidant PBN commonly used in the rubber industry by adding the anti-aging material, and the anti-aging material is characterized in that the anti-aging material introduces terephthalate with a rigid structure into the rubber through chelation between the terephthalate and m-phenylene maleamide polymer. Thereby improving the physical and mechanical properties of the rubber.
(2) The physical and mechanical properties of the compounds obtained by kneading the above-mentioned samples 1, 2, 3 and 4 were shown in Table 3, respectively, after irradiation with ultraviolet light for 200 hours.
TABLE 3 physical and mechanical Properties of samples after UV irradiation
From the above experimental results, the following conclusions were drawn: the anti-aging material can lead the ultraviolet resistance of NR vulcanized rubber to exceed the antioxidant PBN commonly used in rubber industry, not only due to the resonance effect of benzene rings and the stabilization effect of double bonds of maleic groups on formed free radicals, but also due to the synergistic effect of calcium terephthalate and zinc terephthalate, stable chelate is formed with m-phenylene maleamide, thereby improving the stability of amino groups in m-phenylene maleamide.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (6)
1. The preparation method of the yellowing-resistant long-acting anti-aging material is characterized by comprising the following specific preparation processes:
s1: the preparation method of the terephthalic acid metal salt compound organic framework material by utilizing the alkali deweighting wastewater comprises the following specific preparation steps:
s1-1: decolorizing and removing impurities from the alkali-reduced wastewater, and adjusting the pH value of the alkali-reduced wastewater to 7.5-9;
s1-2: adding the pre-prepared metal chloride solution into the alkali deweighting wastewater treated in the step S1-1, uniformly mixing and stirring for reacting for 20-120min, and then filtering, washing and drying to obtain the alkali deweighting wastewater;
the metal chloride salt solution is a mixed solution of a calcium chloride solution and a zinc chloride solution, wherein the mass fraction of the calcium chloride solution is 25% -50%, and the mass fraction of the zinc chloride solution is 15% -30%;
s2: preparing maleic anhydride organic solution in a reaction kettle, adding a certain amount of m-phenylenediamine into the prepared maleic anhydride organic solution, heating to 120-150 ℃ under normal pressure, mixing and refluxing for 4-8 hours, filtering, washing, and vacuum drying at 50 ℃ to obtain m-phenylene bismaleimide;
s3: under the condition of continuous stirring, dissolving a terephthalic acid metal salt compound organic framework material and m-phenylene bismaleimide in dimethylformamide according to a certain mass ratio, heating to 45-50 ℃, preserving heat for 30-60min, and then evaporating a mixture of the dimethylformamide and water in vacuum to obtain a coordination chelate;
s4: and (3) crushing the chelate prepared in the step (S3) at normal temperature to obtain a target product.
2. The method for preparing a yellowing-resistant and long-acting anti-aging material according to claim 1, wherein the main component of the alkali-reduced wastewater subjected to the decoloring and impurity-removing treatment in the step S1-1 is sodium terephthalate, and the content is 98.6% or more.
3. The method for producing a yellowing resistant and aging resistant material according to claim 1, wherein n (Ca 2+ ）+ n（Zn 2+ ): n (sodium terephthalate) =1-1.1:1.
4. The method for preparing a yellowing resistant and long-acting anti-aging material according to claim 1, wherein in the step S2, the solvent of the maleic anhydride organic solution is o-xylene, and the concentration of the maleic anhydride organic solution is 2mol/L.
5. The method for preparing the yellowing resistant and long-acting anti-aging material according to claim 1, wherein the molar ratio of maleic anhydride to m-phenylenediamine is 1:1.
6. The method for preparing the yellowing-resistant long-acting anti-aging material according to claim 1, wherein the mass ratio of the metal terephthalate compound organic framework material to the m-phenylene bismaleimide is 1-5:1.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4154737A (en) * | 1976-05-05 | 1979-05-15 | E. I. Du Pont De Nemours And Company | Preparation of maleimides and dimaleimides |
| CN1686871A (en) * | 2005-04-23 | 2005-10-26 | 陈一鸣 | Method for preparing antiager from wastewater of alkali weight reduction |
| CN110922638A (en) * | 2019-12-23 | 2020-03-27 | 常州市五洲环保科技有限公司 | Method for preparing protective material for rubber by recycling textile white mud |
| CN112500536A (en) * | 2020-12-31 | 2021-03-16 | 常州市五洲化工有限公司 | Preparation method of long-acting anti-tarnishing anti-aging agent |
-
2022
- 2022-02-26 CN CN202210181737.2A patent/CN114292438B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4154737A (en) * | 1976-05-05 | 1979-05-15 | E. I. Du Pont De Nemours And Company | Preparation of maleimides and dimaleimides |
| CN1686871A (en) * | 2005-04-23 | 2005-10-26 | 陈一鸣 | Method for preparing antiager from wastewater of alkali weight reduction |
| CN110922638A (en) * | 2019-12-23 | 2020-03-27 | 常州市五洲环保科技有限公司 | Method for preparing protective material for rubber by recycling textile white mud |
| CN112500536A (en) * | 2020-12-31 | 2021-03-16 | 常州市五洲化工有限公司 | Preparation method of long-acting anti-tarnishing anti-aging agent |
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