CN114872353A - Preparation method and application of flame-retardant electromagnetic shielding film based on nylon waste silk - Google Patents
Preparation method and application of flame-retardant electromagnetic shielding film based on nylon waste silk Download PDFInfo
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- CN114872353A CN114872353A CN202210504915.0A CN202210504915A CN114872353A CN 114872353 A CN114872353 A CN 114872353A CN 202210504915 A CN202210504915 A CN 202210504915A CN 114872353 A CN114872353 A CN 114872353A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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Abstract
The invention discloses a preparation method and application of a flame-retardant electromagnetic shielding film based on waste nylon yarns. The prepared coating slurry and the conductive filler are respectively treated on the surface of the polyamide nylon fabric to prepare the high-temperature resistant electromagnetic shielding material with the sandwich structure. The method for preparing the multifunctional coating by taking the waste silk material as the raw material has simple technical means and easy obtainment of the raw material, and the produced material can be converted into the pulping raw material again for recycling after reaching the service life, thereby relieving the serious pollution of a large amount of waste to the environment, recycling the waste again, saving a large amount of energy loss, and having important advantages in environmental protection due to unique production and utilization advantages.
Description
Technical Field
The invention relates to the application field of waste nylon yarn textile materials, and particularly relates to a preparation method and application of a flame-retardant electromagnetic shielding film based on nylon waste yarn.
Background
The flexible multifunctional polymer-based electromagnetic interference shielding composite film has great application potential in the aspects of 5G communication technology, wearable electronic devices, sustainable energy, artificial skin, heat storage and the like. And with the popularization of small-sized precise electronic equipment such as a 5G smart phone, a computer and the like, the influence of electromagnetic waves on human health is increasingly urgent. At the same time, the integrated high-speed operation of electronic equipment results in elevated temperatures due to thermal concentrations, which threatens life and safe use of people and equipment. For microelectronic device products, the functional requirements of electromagnetic shielding and fire prevention are necessary, and therefore, people are paying attention to how to effectively adjust a multifunctional flexible film having high fire safety and electromagnetic wave pollution prevention between a device and the environment.
Zhengjinhuan et al (CN 106752883A, 2017.05.31) at Zhejiang theory of technology]The invention discloses a method for preparing polyamide wet coating slurry for preventing inorganic filler from settling, which utilizes sodium poly-p-styrene sulfonate as an anti-settling agent to prepare the polyamide wet coating slurry containing the inorganic filler, wherein when the addition amount of the sodium poly-p-styrene sulfonate is 1.5 percent of a polyamide coating slurry system, the settling height of the polyamide coating slurry after 1 day is 0mm (the settling height of the polyamide coating slurry after 1 day is 12mm when no additive is added), the static stability of the coating slurry is obviously improved, and the stability of the quality of a coating processing product can be better ensured. In the work, the introduction of the sodium poly-p-styrene sulfonate improves the surface potential of inorganic filler particles, so that the particles are uniformly dispersed in a system, and the mutual agglomeration among the particles is avoided, thereby improving the compatibility of the inorganic filler in coating slurry and providing a good solution for uniform dispersion of the inorganic flame-retardant filler. Military et al at northwest university of industry [ Nano Research ISSN 1998 once again 0124 CN 11-5974/O4]Fe is prepared by adopting in-situ polymerization and electrostatic spinning technology 3 O 4 Polyamic Acid (PA)A) Nanofiber membranes in Fe by vacuum assisted filtration 3 O 4 Surface deposition of Ti on PAA nanofiber film 3 C 2 T x nanosheets. Then the Polyimide (PI) is mixed with Ti 3 C 2 T x-(Fe 3 O 4 Polyamic acid (PAA)) composite film was obtained by hot pressing. So that the two sides of the film exhibit completely different characteristics. Fe 3 O 4 the/PI side has excellent hydrophobicity and insulation, Ti 3 C 2 The Tx side has hydrophilicity and excellent conductivity. The electromagnetic shielding effectiveness of the film reaches 66 dB. In addition, the composite film also has excellent electrothermal performance. When the applied voltage is 4V, the stable surface temperature reaches 108 ℃, and the work provides constructive inspiration for the preparation of the multifunctional film material designed by us. Compared with the traditional multifunctional film production technology at present, the processing mode of the suction filtration film is simple and convenient, but the processing mode cannot meet the requirements of current large-scale production and application, and is difficult to meet the application scenes of the multifunctional film in various industries at present.
In summary, the invention provides a method for preparing a flame-retardant electromagnetic shielding material based on waste nylon wires, which comprises the steps of dissolving calcium chloride in methanol, adding the waste nylon wires into a calcium chloride-methanol solution for dissolving, adding flame-retardant filler for continuous stirring until the filler is uniformly dispersed in slurry after the waste nylon wires are completely dissolved. Uniformly blade-coating the polyamide nylon wire surface by adopting a single-side blade-coating mode, carrying out solvent exchange solidification in a water bath, spraying the conductive filler on the other side, and then scraping and coating a layer of slurry on the surface of the conductive layer. The invention recycles the waste textile raw materials, fully recycles, develops and recycles the waste such as waste silk, waste yarn and the like generated in the production process, saves resources, protects the environment and can create considerable economic benefits. And the coating finishing technology endows the polyamide nylon fabric with the styles of paper and cloth, and the formed coating product has the characteristics of high strength, good air permeability and moisture permeability, excellent hand feeling and elasticity and the like. Has wide application prospect in the aspects of electromagnetic protective clothing, ink-jet printing, military camouflage and the like. On the more prominent aspect, the multifunctional film material produced and processed by the method can be dissolved and used repeatedly, so that the outstanding problem of high production raw material cost of enterprises is solved.
Disclosure of Invention
The preparation method of the flame-retardant electromagnetic shielding material is based on green recovery of waste nylon yarns, and combines the calcium ions and the polyamide nylon long chain to carry out a complex reaction, so that the crystallinity of the polymer long chain is reduced, the polymer long chain is converted into an amorphous state from a crystalline state, and the solubility of the polyamide nylon is increased.
The core idea of the invention is as follows: firstly, polyamide nylon waste silk is dissolved in calcium chloride-methanol solution, then flame-retardant filler is added into the slurry, so that the viscosity of the slurry is increased and the flame-retardant property of a coating is improved, finally the mixed slurry is processed on the surface of polyamide nylon fabric in a single-side blade coating mode, then conductive filler is sprayed between the fabric and the slurry to form a sandwich structure, the durability of the conductive filler is improved, and finally the high-temperature resistant electromagnetic shielding material is obtained. The method has the advantages of easily obtained raw materials, simplicity and capability of innovatively utilizing waste scraps generated in the production process of the polyamide fabric as the raw materials for coating pulping, is expected to become a self-circulation production process, and is a good environment-friendly, green and low-toxicity circulation process.
A preparation method of a flame-retardant electromagnetic shielding film based on nylon waste silk comprises the following steps:
s1, adding 15-25 parts by weight of metal salt into 50-70 parts by weight of methanol, stirring and dissolving under the condition of constant-temperature water bath, weighing 5-15 parts by weight of polyamide 6 waste wire, shearing and adding into the mixed solution, standing for 30min, stirring at high speed, adding 5-20 parts by weight of flame retardant into the solution after complete dissolution, continuously stirring for 1h until the flame retardant is uniformly dispersed, and pouring out; preparing polyamide 6 flame-retardant coating slurry for later use;
s2, taking the coating slurry prepared in the S1 to carry out single-side blade coating on the polyamide fabric, putting the polyamide coated fabric into a water bath to be solidified for a certain time, taking out the polyamide coated fabric, putting the polyamide coated fabric into a heat setting machine when no obvious water drops exist on the surface of the polyamide coated fabric, and carrying out heat setting;
s3, uniformly spraying a certain amount of conductive nano filler on the polyamide fabric by adopting a spraying mode on the other surface of the single-sided polyamide coated fabric manufactured in the S2, and repeating the operation in the S2 on the surface to manufacture the flame-retardant electromagnetic shielding material with the sandwich structure based on the waste nylon wires.
Preferably, in step S1, the metal salt is CaCl 2 、MgCl 2 、FeCl 3 、AlCl 3 、TiCl 4 One or more of them.
Preferably, in the step S1, the constant temperature water bath condition is 50 ℃ to 70 ℃.
Preferably, in the step S1, the waste polyamide nylon yarn is one or more of PA-6, PA-66, PA-11, PA-12 and PA-610.
Preferably, in step S1, the flame retardant is one or more of ammonium polyphosphate, montmorillonite, aluminum hydroxide, magnesium hydroxide, kaolin, and hydrotalcite.
Preferably, in the step S2, the thickness of the single-sided knife coating is 0.02mm to 0.08 mm.
Preferably, in the step S2, the water bath coagulation time is 1-30S, the heat setting temperature is 100-185 ℃, and the heat setting time is 20-180S.
Preferably, in step S3, the conductive nano-filler is one or more of silver nanowires, titanium carbide, graphene, and carbon nanotubes.
Preferably, in the step S3, the concentration of the conductive nano solution is 1g/L-10g/L, and the spraying loading amount of the nano conductive filler is 0.1g/m 2 -10g/m 2 。
A flame-retardant electromagnetic shielding film based on nylon waste silk is prepared by any one of the methods.
Compared with the prior art, the invention has the following advantages:
firstly, with the enhancement of social environmental awareness, researchers pay more attention to the treatment mode of non-toxic and environment-friendly waste polymers, the method disclosed by the invention uses two most common chemical reagents, namely calcium chloride and methanol solution, to dissolve and pulp polyamide nylon, compared with the traditional chemical treatment technology, the method avoids the release of toxic gases and carcinogens in the use and preparation processes, and the calcium chloride and methanol solvent used by the method can solve the problems of the release of harmful gases such as formaldehyde and the like in the use process, has wide sources, and is an environment-friendly preparation way.
The invention takes the nylon 6 waste silk as the raw material to be fully recycled, developed and reused, which is beneficial to environmental protection and reasonable resource utilization, and can promote the economic growth of enterprises, further promote the recycling and reuse of waste chemical fibers, and the prepared composite membrane material can be changed into the raw material for producing the original slurry again after reaching the service life, and can be repeatedly purified and used, thereby achieving the self-circulation-self-supply system for material use, having good social value for the polyamide nylon base material coating material technology, and conforming to the strategic targets of peak-to-peak carbon-based coating, carbon neutralization and extraction.
And thirdly, the production mode of the composite membrane material can meet the selective composite processing of multiple functions, various processing requirements of the multifunctional membrane at present are met, and the multifunctional membrane material is easier to realize industrialization compared with the traditional suction filtration processing mode and has wider application market.
Fourthly, the coating slurry prepared by the invention is coated on the surface of the fabric by blade coating, then the fabric enters a water bath, and the methanol solvent in the coating slurry is removed by displacement, so that the coating agent forms a coating film on the surface of the fabric, and micropores with different apertures are formed on the surface of the coating film, the formation of the micropores makes up the problem of poor air permeability of the traditional coating electromagnetic shielding material, reduces the overall weight of the material, and meets the current production requirements of multifunction and light weight.
Description of the figures
Fig. 1 is an electromagnetic shielding material sprayed with silver nanowires of different contents;
FIG. 2 is a TG and DTG diagram of pure PA-6 and flame retardant electromagnetic shielding material PA-6;
FIG. 3 is a scanning image of conductive silver nanowires in the middle of a sandwich layer;
FIG. 4 is a camouflage formed by ink jet printing on the surface of a film material;
fig. 5 is a diagram of the re-dissolution process of the prepared composite film material.
Detailed Description
It should be noted that the embodiments and features of the embodiments of the present invention may be combined with each other without conflict.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention selects the waste nylon yarn to prepare the coating slurry, the polyamide nylon as the treated fabric and the ammonium polyphosphate as the inorganic flame-retardant additive as the embodiment for representative description, which only represents a part of the implementation content of the invention and is not used for limiting the invention, and the technical scheme recorded in each embodiment can be modified or part of the technical characteristics can be equivalently replaced.
Examples
With reference to fig. 1-5, 21g of calcium chloride and 60g of methanol are added into a 250mL three-necked bottle, the three-necked bottle is placed in a 60 ℃ constant temperature water bath kettle to be heated and stirred, 10g of waste nylon yarn is taken out to be added into the solution to be dissolved after the calcium chloride is completely dissolved, high-speed stirring is started after the waste nylon yarn is completely dissolved, after the waste nylon yarn is continuously dissolved for 1 hour, 8g of ammonium polyphosphate is added into the solution, high-speed stirring is carried out until the ammonium polyphosphate is uniformly dispersed in the solution, and slurry is poured out for later use. Spreading polyamide fabric on a polytetrafluoroethylene plate with the thickness of 20cm multiplied by 20cm, taking the coating slurry prepared in the previous step to carry out single-side blade coating on the polyamide fabric, ensuring that the thickness of the coating layer of the blade coating is 0.02mm, putting the polyamide coated fabric into a water bath to be solidified for 6s, and taking out the polyamide coated fabric until no polyamide coated fabric exists on the surfaceWhen the water drops obviously, putting the mixture into a heat setting machine at 165 ℃, and taking out the mixture after heat setting for 120 s. Uniformly spraying silver nanowires on the other side of the prepared single-side wet-process-coated polyamide nylon in a spraying manner to enable the loading capacity of the polyamide nylon to reach 0.2mg/cm 2 . And then, on the basis of the conductive coating, scraping a layer of the prepared slurry, solidifying in a water bath for 6s, taking out, putting into a heat setting machine at 165 ℃ when no obvious water drops exist on the surface, and taking out after heat setting for 120s to obtain the flame-retardant electromagnetic shielding material based on the waste nylon yarn.
Thermogravimetric tests are carried out, and the results are shown in the following table I, wherein the results are that pure PA-6 and flame-retardant electromagnetic shielding material PA-6 have 5 percent of thermal weight loss, maximum constant temperature and 800 ℃ loss rate statistics
Under the condition that other conditions are not changed, the using amount of ammonium polyphosphate is adjusted to be 1g, 5g, 10g, 15 g, 20 g, 25 g and 30g respectively, the flame-retardant electromagnetic shielding material is prepared, a flame-retardant test is carried out, and the flame-retardant effects of the two fabrics are measured by a limit oxygen index instrument.
Table two: flame retardancy test for ammonium polyphosphate flame retardant fillers of different masses
| Sample numbering | Ammonium polyphosphate/g | Limiting oxygen index | Whether molten drop or not |
| 1 | 1 | 24.1 | Is that |
| 2 | 5 | 24.6 | Slight dripping |
| 3 | 10 | 28.2 | Whether or not |
| 4 | 15 | 31.6 | Whether or not |
| 5 | 20 | 34.8 | Whether or not |
| 6 | 25 | 36.3 | Whether or not |
| 7 | 30 | 37.6 | Whether or not |
The implementation result shows that: under otherwise unchanged conditions, the metal salt is replaced by MgCl 2 、FeCl 3 、AlCl 3 、TiCl 4 The flame-retardant electromagnetic shielding material with the same effect can also be prepared.
The waste polyamide nylon wires are PA-6, PA-66, PA-11, PA-12 and PA-610, and the flame-retardant electromagnetic shielding material with the same effect can be prepared.
Under the condition that other conditions are not changed, the flame retardant is replaced by ammonium polyphosphate, montmorillonite, aluminum hydroxide, magnesium hydroxide, kaolin and hydrotalcite to achieve similar effects.
Under the condition that other conditions are not changed, the conductive nano filler can be silver nanowires, titanium carbide, graphene and carbon nano tubes.
The technical means for preparing the multifunctional coating by taking the waste silk material generated in the production process as the raw material is simple, and the raw material is easy to obtain. The required coating slurry is obtained quickly, efficiently and safely, and the produced material can be converted into the pulping raw material again for recycling after the service life of the produced material is reached. The invention relieves the serious pollution of a large amount of wastes to the environment; the waste is recycled, a large amount of energy consumption is saved, and the unique production and utilization advantages enable the waste to occupy important advantages in environmental protection. And the coating endows the fabric with the ink jet printing function as printing paper, and the application range of the material is widened.
The characterization methods referred to in the examples and comparative examples illustrate that:
the dissolution and addition of the polyamide fabric surface size and flame retardant was observed by means of a field emission scanning electron microscope SEM (ULTRA 55, Zeiss, Germany).
And measuring the flame-retardant effect of the flame-retardant filler by using a limit oxygen index meter so as to judge different optimal addition ratios.
The water resistance, durability of the flame retardant finish on the polyamide fabric coating surface was measured by the water resistance test. Thus, the adhesion effect of the flame-retardant finishing on the surface of the polyester-cotton fabric is judged.
The elemental composition of the polyamide fabric surface was observed by EDS.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of a flame-retardant electromagnetic shielding film based on nylon waste silk is characterized by comprising the following steps:
s1, adding 15-25 parts by mass of metal salt into 50-70 parts by mass of methanol, stirring and dissolving under the condition of constant-temperature water bath, weighing 5-15 parts by mass of polyamide 6 waste wire, shearing and adding into the mixed solution, standing for 30min, stirring at high speed, adding 5-20 parts by mass of flame retardant into the solution after complete dissolution, continuously stirring for 1h, and pouring out after the flame retardant is uniformly dispersed to prepare polyamide 6 flame-retardant coating slurry for later use;
s2, taking the coating slurry prepared in S1 to carry out single-side blade coating on the polyamide fabric, putting the polyamide coated fabric into a water bath for coagulation for a certain time, taking out the polyamide coated fabric, putting the polyamide coated fabric into a heat setting machine when no obvious water drops exist on the surface of the polyamide coated fabric, and carrying out heat setting;
s3, uniformly spraying a certain amount of conductive nano filler on the polyamide fabric by adopting a spraying mode on the other surface of the single-sided polyamide coated fabric manufactured in the S2, and repeating the operation in the S2 on the surface to manufacture the flame-retardant electromagnetic shielding material with the sandwich structure based on the waste nylon wires.
2. The method for preparing the flame-retardant electromagnetic shielding material based on the waste nylon yarn as claimed in claim 1, wherein the metal salt is CaCl 1 2 、MgCl 2 、FeCl 3 、AlCl 3 、TiCl 4 One or more of them.
3. The method for preparing a flame retardant electromagnetic shielding film based on nylon waste silk according to claim 2, wherein the constant temperature water bath condition is 50 ℃ to 70 ℃ in the step S1.
4. The method for preparing the flame retardant electromagnetic shielding material based on the waste nylon yarn as claimed in any one of claims 1 to 3, wherein in the step S1, the waste polyamide nylon yarn is one or more of PA-6, PA-66, PA-11, PA-12 and PA-610.
5. The method for preparing a flame-retardant electromagnetic shielding film based on nylon waste filaments according to claim 4, wherein in the step S1, the flame retardant is one or more of ammonium polyphosphate, montmorillonite, aluminum hydroxide, magnesium hydroxide, kaolin and hydrotalcite.
6. The method for preparing a flame retardant electromagnetic shielding film based on nylon waste silk according to claim 1, wherein the thickness of the single-sided blade coating is 0.02mm to 0.08mm in step S2.
7. The method for preparing a flame retardant electromagnetic shielding film based on nylon waste silk according to claim 6, wherein in the step S2, the water bath coagulation time is 1-30S, the heat setting temperature is 100-185 ℃, and the heat setting time is 20-180S.
8. The method for preparing a flame-retardant electromagnetic shielding film based on nylon waste silk according to claim 1, wherein in the step S3, the conductive nano filler is one or more of silver nanowires, titanium carbide, graphene and carbon nanotubes.
9. The method for preparing a flame retardant electromagnetic shielding film based on nylon waste silk as claimed in any one of claims 5 to 9, wherein in the step S3, the concentration of the conductive nano solution is 1g/L to 10g/L, and the spraying loading amount of the nano conductive filler is 0.1g/m 2 -10g/m 2 。
10. A flame-retardant electromagnetic shielding film based on nylon waste, which is prepared by the method of any one of claims 1 to 9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115233455A (en) * | 2022-09-23 | 2022-10-25 | 江苏恒力化纤股份有限公司 | Method for preparing full-nylon composite coating fabric from nylon 6 waste silk |
| CN115652650A (en) * | 2022-10-22 | 2023-01-31 | 贵州省材料产业技术研究院 | Flexible electromagnetic shielding PVC composite film and preparation method thereof |
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2022
- 2022-05-10 CN CN202210504915.0A patent/CN114872353A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115233455A (en) * | 2022-09-23 | 2022-10-25 | 江苏恒力化纤股份有限公司 | Method for preparing full-nylon composite coating fabric from nylon 6 waste silk |
| CN115233455B (en) * | 2022-09-23 | 2023-01-31 | 江苏恒力化纤股份有限公司 | Method for preparing full-nylon composite coating fabric from nylon 6 waste silk |
| CN115652650A (en) * | 2022-10-22 | 2023-01-31 | 贵州省材料产业技术研究院 | Flexible electromagnetic shielding PVC composite film and preparation method thereof |
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