Preparation method of waste spinning regenerated deadening felt
By using ammonium cerium nitrate, modified antibacterial agents and hydrophobic additives in waste spinning recycled sound insulation felt, the antibacterial and hydrophobic properties of the fiber are improved, the problem of bacterial debris accumulation is solved, and the tear resistance and antibacterial properties are improved.
Patent Information
- Application Number
- CN202411218287.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-02
- Publication Date
- 2025-01-17
AI Technical Summary
In the prior art, the antibacterial properties of waste spinning recycled sound insulation felt are insufficient, resulting in the accumulation of bacterial debris and affecting the use performance.
Using ammonium cerium nitrate to initiate active fibers, combined with modified antibacterial agents and modified hydrophobic additives, the polymer quaternary ammonium salt and ester-based hydrophobic long chains are introduced through electron transfer and free radical mechanisms to enhance the antibacterial and hydrophobic properties of the fibers and degrade them. Bacterial remains to improve tear resistance.
It significantly improves the antibacterial properties and tear resistance of regenerated sound insulation felt, avoids the accumulation of bacterial debris, and enhances its self-cleaning ability.
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Figure BDA0005022207210000081
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of sound insulation material preparation, and particularly relates to a method for preparing waste spinning regenerated sound insulation felt. Background Art
[0002] With the rapid development of the textile industry, a large amount of waste textiles is generated while meeting market demand. Most of the waste textiles are made of non-degradable polymer materials such as polyvinyl chloride fibers. If they are not recycled, it will not only cause waste of resources but also pollute the environment. Sound insulation felt is a flexible high-density roll that can be prepared from high-density fibers and used for sound insulation and shock absorption of pipes and mechanical equipment. Therefore, waste textiles can be recycled to prepare sound insulation felt. However, there will be a large number of bacteria in the recycled waste textiles. The reproduction of microorganisms will decompose the cellulose material, weaken the tear strength of the sound insulation felt, and even produce adverse gases, which will reduce the performance of the fiber products.
[0003] In the prior art, when recycling waste textiles to make sound insulation felt, quaternary ammonium salt antibacterial agents are usually added to enhance their antibacterial properties. Quaternary ammonium salts can adsorb bacteria through electrostatics, then pass through the cell wall and bind to the cell membrane, destroying the cell membrane structure, causing the bacterial cytoplasm components to leak out, causing bacterial death, but cannot degrade bacterial remains, resulting in the accumulation of bacterial remains, affecting the long-term antibacterial effect of the quaternary ammonium salt surface. Therefore, how to improve the antibacterial properties of waste textile recycled sound insulation felt is a technical problem that needs to be solved at present. Summary of the invention
[0004] The purpose of the present invention is to provide a method for preparing waste spinning regenerated sound insulation felt to solve the problems in the background technology.
[0005] The purpose of the present invention can be achieved through the following technical solutions:
[0006] A method for preparing waste spinning regeneration sound insulation felt, comprising the following steps:
[0007] S1, soaking the pretreated fiber in acetone for 2-3 hours, ultrasonicating for 30 minutes, washing and drying, placing it in deionized water, adding cerium ammonium nitrate and nitric acid, stirring and reacting for 0.5-1 hour, and drying to obtain active fiber;
[0008] S2, add active fiber to carbon tetrachloride, stir and mix, add modified antibacterial agent and modified hydrophobic additive, stir and react at 25-30°C for 2-3h, and then filter, wash and dry to obtain modified fiber;
[0009] S3, combing the modified fibers, laying them into a net, and then subjecting them to a needle punching process and hot pressing to obtain a recycled sound insulation felt.
[0010] Furthermore, the weight ratio of the pretreated fiber, acetone, deionized water, cerium ammonium nitrate and nitric acid is 100-110:400-500:600-700:0.5-5:6-14.
[0011] Furthermore, the weight ratio of the carbon tetrachloride, the active fiber, the modified antibacterial agent, and the modified hydrophobic additive is 500-600:90-100:8-12:9-13.
[0012] Furthermore, the pretreated fibers are obtained by recycling and sterilizing waste fibers and then opening and combing them.
[0013] Furthermore, the modified antibacterial agent is prepared by the following steps:
[0014] A1. Add 4-aminobenzophenone and N,N-diethylethylamine to N,N-dimethylformamide, stir and mix, add methacryloyl chloride mixed solution dropwise under ice water bath condition, control the dropping time to be 20-30min, continue stirring and reacting at room temperature for 10-12h, and then filter, wash with 5wt% sodium carbonate aqueous solution and deionized water, and dry to obtain benzophenone derivatives; use N,N-dimethylformamide as solvent and N,N-diethylethylamine as catalyst to react the amino group in 4-aminobenzophenone with the acyl chloride in methacryloyl chloride to obtain benzophenone derivatives containing amide groups.
[0015] A2, adding benzophenone derivatives and methacryloyloxyethyl dimethylbenzyl ammonium chloride to anhydrous ethanol, stirring and mixing, to obtain a modified antibacterial auxiliary agent;
[0016] Furthermore, the dosage ratio of the N,N-dimethylformamide, 4-aminobenzophenone, N,N-diethylethylamine and methacryloyl chloride mixed solution is 60mL: 5-7g: 5-8mL: 8-10mL; the methacryloyl chloride mixed solution is prepared by dissolving 4-6mL of methacryloyl chloride in 12mL of N,N-dimethylformamide.
[0017] Furthermore, the usage ratio of the anhydrous ethanol, the benzophenone derivative and the methacryloyloxyethyl dimethylbenzyl ammonium chloride is 50 mL: 0.5-5 g: 5-8 mL.
[0018] Furthermore, the modified hydrophobic additive is prepared by the following steps:
[0019] Add lauryl methacrylate to anhydrous ethanol, stir and mix, add acetyl dimethylamine and azobisisobutyronitrile, stir and react at 70-80°C for 1-3h, and then obtain a modified hydrophobic additive after rotary evaporation, anhydrous ethanol washing and drying; use acetyl dimethylamine as a catalyst, azobisisobutyronitrile as an initiator, and lauryl methacrylate as a copolymer monomer to obtain a modified hydrophobic additive containing an ester group and a long-chain alkane hydrophobic group through a free radical polymerization reaction.
[0020] Furthermore, the usage ratio of anhydrous ethanol, lauryl methacrylate, acetyl dimethylamine and azobisisobutyronitrile is 50 mL: 20-40 mL: 2-3 mL: 1-3 g.
[0021] Beneficial effects of the present invention:
[0022] The present invention uses ammonium cerium nitrate as an initiator, and tetravalent cerium salt promotes the generation of free radicals on the carbon chain of the pretreated fiber through electron transfer in an acidic environment, thereby inducing the generation of active sites on the surface of the pretreated fiber;
[0023] The modified antibacterial agent of the present invention contains a polymer quaternary ammonium salt methacryloyloxyethyl dimethyl benzyl ammonium chloride. When the activated fiber is treated, the polymer quaternary ammonium salt can be combined with the hydroxyl group on the molecular chain of the activated fiber through the carbon-carbon double bond, so as to introduce the polymer quaternary ammonium salt with antibacterial property on the surface of the activated fiber. Compared with the small molecule quaternary ammonium salt, the polymer quaternary ammonium salt has a stronger charge density and electrostatic effect, and can adsorb and kill bacteria and other microorganisms on the surface of the regenerated sound insulation felt more quickly, thereby improving the antibacterial property of the regenerated sound insulation felt. In addition, the modified antibacterial agent contains a benzophenone derivative. When the activated fiber is treated, the benzophenone derivative is grafted onto the active fiber through the addition reaction of the carbonyl group and the activated fiber. At the same time, the ketone carbonyl group on the molecular chain of the benzophenone derivative can generate active oxides such as peroxides through a free radical mechanism, degrade bacterial debris on the surface of the regenerated sound insulation felt, effectively avoid the accumulation of bacterial debris, further improve the antibacterial property of the regenerated sound insulation felt, and at the same time, the tear strength of the regenerated sound insulation felt is improved.
[0024] The modified hydrophobic additive of the present invention contains an ester group and a hydrophobic long-chain alkane. When treating active fibers, the modified hydrophobic additive can combine with the hydroxyl group on the surface of the active fibers through the ester group, and form a complex molecular entanglement on the surface of the active fibers through the hydrophobic long-chain alkane, thereby improving the hydrophobic property of the prepared regenerated sound insulation felt, effectively preventing the adhesion of microbial membranes such as bacteria on the surface of the regenerated sound insulation felt, and thus improving the antibacterial property of the regenerated sound insulation felt.
[0025] The present invention uses waste spinning as a base material, induces the generation of active sites on the surface of pretreated fibers through ammonium cerium nitrate, and introduces a modified antibacterial agent with antibacterial and bacterial residue decomposition functions, thereby improving the antibacterial properties of the regenerated sound insulation felt while also improving the tear strength of the regenerated sound insulation felt; in addition, the long chain of the polymer quaternary ammonium salt in the modified antibacterial agent also has hydrophobic properties, and can be entangled with the long chain of the modified hydrophobic auxiliary agent through a complex molecular chain, further improving the hydrophobicity of the regenerated sound insulation felt, thereby giving the regenerated sound insulation felt a potential self-cleaning ability, and improving the antibacterial properties and tear strength of the regenerated sound insulation felt. DETAILED DESCRIPTION
[0026] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0027] Example 1
[0028] This embodiment provides a modified antibacterial agent, which is prepared by the following steps:
[0029] A1. Add 4 mL of methacryloyl chloride to 12 mL of N,N-dimethylformamide to obtain a methacryloyl chloride mixed solution;
[0030] A2. Add 5 g of 4-aminobenzophenone and 5 mL of N,N-diethylethylamine to 60 mL of N,N-dimethylformamide, stir and mix, add 8 mL of methacryloyl chloride mixture dropwise under ice-water bath conditions, control the dropping time to 20 min, continue stirring and reacting at room temperature for 10 h, then filter, wash with 5 wt% sodium carbonate aqueous solution and deionized water, and dry to obtain a benzophenone derivative;
[0031] A3. Add 0.5 g of benzophenone derivative and 5 mL of methacryloyloxyethyl dimethylbenzyl ammonium chloride to 50 mL of anhydrous ethanol, stir and mix to obtain a modified antibacterial adjuvant.
[0032] Example 2
[0033] This embodiment provides a modified antibacterial agent, which is prepared by the following steps:
[0034] A1. Add 5 mL of methacryloyl chloride to 12 mL of N,N-dimethylformamide to obtain a methacryloyl chloride mixed solution;
[0035] A2. Add 6 g of 4-aminobenzophenone and 7 mL of N,N-diethylethylamine to 60 mL of N,N-dimethylformamide, stir and mix, add 9 mL of methacryloyl chloride mixture dropwise under ice-water bath conditions, control the dropping time to 25 min, continue stirring and reacting at room temperature for 11 h, then filter, wash with 5 wt% sodium carbonate aqueous solution and deionized water, and dry to obtain a benzophenone derivative;
[0036] A3. Add 3.5 g of benzophenone derivative and 6 mL of methacryloyloxyethyl dimethylbenzyl ammonium chloride to 50 mL of anhydrous ethanol, stir and mix to obtain a modified antibacterial adjuvant.
[0037] Example 3
[0038] This embodiment provides a modified antibacterial agent, which is prepared by the following steps:
[0039] A1. Add 6 mL of methacryloyl chloride to 12 mL of N,N-dimethylformamide to obtain a methacryloyl chloride mixed solution;
[0040] A2. Add 7 g of 4-aminobenzophenone and 8 mL of N,N-diethylethylamine to 60 mL of N,N-dimethylformamide, stir and mix, add 10 mL of methacryloyl chloride mixture dropwise under ice-water bath conditions, control the dropping time to 30 min, continue stirring and reacting at room temperature for 12 h, then filter, wash with 5 wt% sodium carbonate aqueous solution and deionized water, and dry to obtain a benzophenone derivative;
[0041] A3. Add 5 g of benzophenone derivative and 8 mL of methacryloyloxyethyl dimethylbenzyl ammonium chloride to 50 mL of anhydrous ethanol, stir and mix to obtain a modified antibacterial adjuvant.
[0042] Example 4
[0043] This embodiment provides a modified hydrophobic additive, which is prepared by the following steps:
[0044] Add 20 mL of lauryl methacrylate to 50 mL of anhydrous ethanol, stir and mix, add 2 mL of acetyldimethylamine and 1 g of azobisisobutyronitrile, stir and react at 70° C. for 1 h, then rotary evaporate, wash with anhydrous ethanol, and dry to obtain a modified hydrophobic additive.
[0045] Example 5
[0046] This embodiment provides a modified hydrophobic additive, which is prepared by the following steps:
[0047] Add 30 mL of lauryl methacrylate to 50 mL of anhydrous ethanol, stir and mix, add 2.5 mL of acetyldimethylamine and 1.5 g of azobisisobutyronitrile, stir and react at 75° C. for 1.5 h, then rotary evaporate, wash with anhydrous ethanol, and dry to obtain a modified hydrophobic additive.
[0048] Example 6
[0049] This embodiment provides a modified hydrophobic additive, which is prepared by the following steps:
[0050] Add 40 mL of lauryl methacrylate to 50 mL of anhydrous ethanol, stir and mix, add 3 mL of acetyldimethylamine and 3 g of azobisisobutyronitrile, stir and react at 80° C. for 3 h, then rotary evaporate, wash with anhydrous ethanol, and dry to obtain a modified hydrophobic additive.
[0051] Example 7
[0052] This embodiment provides a method for preparing a regenerated sound insulation felt, comprising the following steps:
[0053] S1, disinfecting the recovered waste textiles, and then opening and combing them to obtain pretreated fibers;
[0054] S2, soaking 100 parts by weight of the pretreated fiber in 400 parts by weight of acetone for 2 hours, ultrasonicating for 30 minutes, washing and drying, placing in 600 parts by weight of deionized water, adding 0.5 parts by weight of ammonium cerium nitrate and 6 parts by weight of nitric acid, stirring for 0.5 hours, and drying to obtain active fibers;
[0055] S3, adding 90 parts by weight of active fiber to 500 parts by weight of carbon tetrachloride, stirring and mixing, adding 8 parts by weight of modified antibacterial agent and 9 parts by weight of modified hydrophobic additive, stirring and reacting at 25° C. for 2 hours, and then filtering, washing and drying to obtain modified fiber;
[0056] S4, combing the modified fibers, laying them into a net, and then subjecting them to a needle punching process and hot pressing to obtain a recycled sound insulation felt.
[0057] Example 8
[0058] This embodiment provides a method for preparing a regenerated sound insulation felt, comprising the following steps:
[0059] S1, disinfecting the recovered waste textiles, and then opening and combing them to obtain pretreated fibers;
[0060] S2, soaking 105 parts by weight of the pretreated fiber in 450 parts by weight of acetone for 2.5 hours, ultrasonicating for 30 minutes, washing and drying, placing in 650 parts by weight of deionized water, adding 3 parts by weight of ammonium cerium nitrate and 10 parts by weight of nitric acid, stirring for 0.5 hours, and drying to obtain active fiber;
[0061] S3, add 95 parts by weight of active fiber to 550 parts by weight of carbon tetrachloride, stir and mix, add 10 parts by weight of modified antibacterial agent and 11 parts by weight of modified hydrophobic additive, stir and react at 28°C for 2.5h, and then filter, wash and dry to obtain modified fiber;
[0062] S4, combing the modified fibers, laying them into a net, and then subjecting them to a needle punching process and hot pressing to obtain a recycled sound insulation felt.
[0063] Example 9
[0064] This embodiment provides a method for preparing a regenerated sound insulation felt, comprising the following steps:
[0065] S1, disinfecting the recovered waste textiles, and then opening and combing them to obtain pretreated fibers;
[0066] S2, soaking 110 parts by weight of the pretreated fiber in 500 parts by weight of acetone for 3 hours, ultrasonicating for 30 minutes, washing and drying, placing in 700 parts by weight of deionized water, adding 5 parts by weight of ammonium cerium nitrate and 14 parts by weight of nitric acid, stirring for 1 hour, and drying to obtain active fiber;
[0067] S3, adding 100 parts by weight of active fiber to 600 parts by weight of carbon tetrachloride, stirring and mixing, adding 12 parts by weight of modified antibacterial agent and 13 parts by weight of modified hydrophobic additive, stirring and reacting at 30° C. for 3 hours, and then filtering, washing and drying to obtain modified fiber;
[0068] S4, combing the modified fibers, laying them into a net, and then subjecting them to a needle punching process and hot pressing to obtain a recycled sound insulation felt.
[0069] Comparative Example 1: Compared with Example 7, the modified antibacterial agent was replaced with a small molecule quaternary ammonium salt in equal amount, and the rest was the same.
[0070] Comparative Example 2: Compared with Example 7, no modified hydrophobic additive was added, and the rest was the same.
[0071] Comparative Example 3: Compared with Example 7, the modified hydrophobic additive was replaced with an equal amount of a commercially available hydrophobic additive, and the rest was the same.
[0072] Performance tests were performed on Examples 7 to 9 and Comparative Examples 1 to 3. Antibacterial performance: refer to GB / T20944.3-2008, use the quantitative test-oscillation method to test, and calculate the antibacterial rate. At the same time, the tear strength of the sample before and after being placed in the colony dish was tested. The tear strength reference: GB / T 3917.2-2009; contact angle test: refer to GB / T 42694-2023. The larger the contact angle, the better the hydrophobic performance. The results are shown in Table 1:
[0073] Table 1
[0074]
[0075] It can be seen from Table 1 that the regenerated sound insulation board prepared by modified antibacterial agent and modified hydrophobic additive in Examples 7-9 has a contact angle significantly higher than that of Comparative Examples 1-3, and has good hydrophobic properties. At the same time, the tear strength before and after being placed in the colony dish is higher than that of Comparative Examples 1-3, and has good antibacterial properties; in addition, compared with Comparative Examples 1-2, Example 7 has a higher antibacterial rate, indicating that under the synergistic effect of the modified antibacterial agent and the modified hydrophobic additive, the regenerated sound insulation felt has higher antibacterial properties.
[0076] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.
[0077] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A method for preparing waste spinning regeneration sound insulation felt, characterized in that: The following steps are involved: S1, soaking the pretreated fiber in acetone for 2-3 hours, ultrasonicating for 30 minutes, washing and drying, placing it in deionized water, adding cerium ammonium nitrate and nitric acid, stirring and reacting for 0.5-1 hour, and drying to obtain active fiber; S2, add active fiber to carbon tetrachloride, stir and mix, add modified antibacterial agent and modified hydrophobic additive, stir and react at 25-30°C for 2-3h, and then filter, wash and dry to obtain modified fiber; S3, combing the modified fibers, laying them into a net, and then subjecting them to a needle punching process and hot pressing to obtain a recycled sound insulation felt.
2. The method for preparing waste spinning regeneration sound insulation felt according to claim 1, characterized in that: The weight ratio of the pretreated fiber, acetone, deionized water, cerium ammonium nitrate and nitric acid is 100-110:400-500:600-700:0.5-5:6-14.
3. The method for preparing waste spinning regenerated sound insulation felt according to claim 1, characterized in that: The weight ratio of the carbon tetrachloride, the active fiber, the modified antibacterial agent and the modified hydrophobic auxiliary agent is 500-600:90-100:8-12:9-13.
4. The method for preparing waste spinning regenerated sound insulation felt according to claim 1, characterized in that: The pretreated fibers are obtained by recycling and sterilizing waste fibers and then opening and combing them.
5. The method for preparing waste spinning regenerated sound insulation felt according to claim 1, characterized in that: The modified antibacterial agent is prepared by the following steps: A1. Add 4-aminobenzophenone and N,N-diethylethylamine to N,N-dimethylformamide, stir and mix, add methacryloyl chloride mixture dropwise under ice-water bath condition, control the dropping time to be 20-30min, continue stirring and reacting at room temperature for 10-12h, filter, wash with 5wt% sodium carbonate aqueous solution and deionized water, and dry to obtain benzophenone derivative; A2. Add benzophenone derivatives and methacryloyloxyethyl dimethylbenzyl ammonium chloride to anhydrous ethanol, stir and mix, and obtain a modified antibacterial auxiliary agent.
6. The method for preparing waste spinning regenerated sound insulation felt according to claim 5, characterized in that: The dosage ratio of the N,N-dimethylformamide, 4-aminobenzophenone, N,N-diethylethylamine and methacryloyl chloride mixed solution is 60mL: 5-7g: 5-8mL: 8-10mL; the methacryloyl chloride mixed solution is prepared by dissolving 4-6mL of methacryloyl chloride in 12mL of N,N-dimethylformamide.
7. The method for preparing waste spinning regeneration sound insulation felt according to claim 5, characterized in that: The usage ratio of the anhydrous ethanol, the benzophenone derivative and the methacryloyloxyethyl dimethylbenzyl ammonium chloride is 50 mL: 0.5-5 g: 5-8 mL.
8. The method for preparing waste spinning regenerated sound insulation felt according to claim 1, characterized in that: The modified hydrophobic additive is prepared by the following steps: Add lauryl methacrylate to anhydrous ethanol, stir and mix, add acetyl dimethylamine and azobisisobutyronitrile, stir and react at 70-80° C. for 1-3 hours, and then perform rotary evaporation, wash with anhydrous ethanol, and dry to obtain a modified hydrophobic additive.
9. The method for preparing waste spinning regeneration sound insulation felt according to claim 8, characterized in that: The usage ratio of anhydrous ethanol, lauryl methacrylate, acetyl dimethylamine and azobisisobutyronitrile is 50 mL: 20-40 mL: 2-3 mL: 1-3 g.