CN111592739A - Preparation method of electromagnetic shielding plastic - Google Patents
Preparation method of electromagnetic shielding plastic Download PDFInfo
- Publication number
- CN111592739A CN111592739A CN202010483401.2A CN202010483401A CN111592739A CN 111592739 A CN111592739 A CN 111592739A CN 202010483401 A CN202010483401 A CN 202010483401A CN 111592739 A CN111592739 A CN 111592739A
- Authority
- CN
- China
- Prior art keywords
- electromagnetic shielding
- parts
- shielding plastic
- preparing
- hours
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L65/00—Compositions of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Compositions of derivatives of such polymers
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a preparation method of electromagnetic shielding plastic, which is characterized by comprising the following steps of: uniformly mixing 100 parts of polythiophene fluorenone polymer, 10-15 parts of steel fiber surface modification polypyrrole tube, 10-15 parts of Sn-Al-O-P, 1-3 parts of coupling agent and 1-3 parts of antioxidant, and then adding the mixture into a double-screw extruder for mixing and extruding to obtain the electromagnetic shielding plastic. The electromagnetic shielding plastic prepared by the method has more excellent mechanical property and better electromagnetic shielding effect.
Description
The invention relates to a divisional application of Chinese patent 'an electromagnetic shielding plastic and a preparation method thereof', wherein the application date is 8 months and 1 days in 2018, and the application number is 201810861294.5.
Technical Field
The invention relates to the technical field of high polymer materials, in particular to electromagnetic shielding plastic and a preparation method thereof.
Background
With the development of modern science and technology and electronic industry, electronic products such as various household appliances, office appliances, instruments and equipment are widely popularized and applied, convenience is brought to people, and meanwhile, a large amount of electromagnetic radiation is released, so that the health of people is harmed. For information security and human health, preventing information leakage and interference, the number of objects requiring electromagnetic shielding is increasing, the degree of shielding is increasing, and the time and space requirements for shielding are increasing. Therefore, it is imperative to find materials having better electromagnetic shielding function.
The material with the functions of electric conduction and electromagnetic shielding, which takes plastic as a base body, becomes a star in the current electromagnetic shielding material at lower cost due to lower density. Plastics do not have conductivity and magnetic permeability, and in order to realize electromagnetic shielding, plastics are often required to be modified, for example, conductive metal powder, conductive mica powder and the like are added into a plastic matrix to obtain electromagnetic shielding performance, however, due to the problems of compatibility of conductive particles and the plastic matrix, dispersibility of the conductive particles, processing conditions and the like, the shielding performance, mechanical performance and the like of the finally obtained material are often unsatisfactory.
Chinese patent 201210098259.5 discloses a method for preparing stainless steel fiber resin-based composite conductive plastic, wherein single stainless steel fiber is used as the basic component of conductive filler, the cost of raw materials is high, the function of no absorption loss of electromagnetic waves is realized, and the high shielding function is difficult to obtain.
Therefore, the composite electromagnetic shielding plastic has the advantages of light weight, low production cost, good shielding effect and excellent mechanical property, has wide market value and application prospect, and has a positive effect on promoting the safe and healthy development of the electronic communication industry.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention discloses an electromagnetic shielding plastic and a preparation method thereof, wherein the preparation method is simple and easy to implement, has low requirements on equipment, has non-harsh reaction conditions and is suitable for large-scale production; the prepared electromagnetic shielding plastic has excellent mechanical property, good weather resistance and stability and good electromagnetic shielding effect.
In order to achieve the purpose, the invention adopts the technical scheme that the electromagnetic shielding plastic is prepared from the following raw materials in parts by weight: 100 parts of polythiophene fluorenone polymer, 10-15 parts of steel fiber surface modification polypyrrole tube, 10-15 parts of Sn-Al-O-P, 1-3 parts of coupling agent and 1-3 parts of antioxidant.
Preferably, the antioxidant is selected from at least one of antioxidant 1010, antioxidant 1076; the coupling agent is selected from one or more of tetraisopropyl titanate coupling agent, silane coupling agent KH550, silane coupling agent KH560 and silane coupling agent KH 570.
Further, the preparation method of the polythiophene fluorenone polymer comprises the following steps: adding 2, 5-di (5-bromothiophene-2-yl) thiophene, 2, 5-dihydroxy-9-fluorenone and an alkaline catalyst into a three-neck flask connected with a water separator, adding a high-boiling point solvent and toluene, heating a reaction system to 120-130 ℃, stirring and reacting for 5-7 hours under the protection of nitrogen or inert gas, removing water and toluene generated in the reaction process through the water separator, slowly raising the reaction temperature to 145 ℃ after removing water, continuing to stir and react for 8-10 hours, adding bis (4-hydroxyphenyl) phenylphosphine oxide, continuing to react for 1-2 hours, cooling the reaction system to room temperature, precipitating in water, performing suction filtration, washing for 4-6 times by using ethanol, then placing in a vacuum drying box at 75-85 ℃ for drying for 15-20 hours, thus obtaining a polythiophene fluorenone polymer.
Preferably, the mass ratio of the 2, 5-di (5-bromothiophene-2-yl) thiophene, the 2, 5-dihydroxy-9-fluorenone, the basic catalyst, the high boiling point solvent, the toluene and the bis (4-hydroxyphenyl) phenylphosphine oxide is 2:1 (0.3-0.5): 10-15: 3-6: 0.5.
Further, the high boiling point solvent is selected from one or more of dimethyl sulfoxide, N-methyl pyrrolidone and N, N-dimethylformamide; the alkaline catalyst is selected from one or more of potassium carbonate, cesium carbonate, sodium carbonate and sodium hydroxide; the inert gas is selected from one or more of helium, neon and argon.
Further, the preparation method of the steel fiber surface modified polypyrrole tube comprises the following steps: dispersing steel fiber in ethanol, adding chloropropyl triethoxysilane, stirring at 30-40 deg.C for reaction for 3-5 hr, adding polypyrrole tube and catalyst, stirring at 70-80 deg.C for 6-8 hr, vacuum filtering, washing with ethanol for 3-5 times, and drying at 70-80 deg.C for 8-10 hr in vacuum drying oven to obtain steel fiber surface modified polypyrrole tube.
Preferably, the mass ratio of the steel fiber, the ethanol, the chloropropyl triethoxysilane, the polypyrrole tube and the catalyst is (3-5): (10-15):1:2: (0.3-0.5).
Preferably, the catalyst is selected from at least one of sodium carbonate and potassium carbonate.
Preferably, the preparation method of Sn-Al-O-P comprises the following steps: adding stannic chloride, an aluminum source and phosphorus trichloride into a beaker containing ethanol, stirring for 0.5-1 h, then slowly adding sodium citrate, stirring vigorously for 4-5 h, transferring the solution into a hydrothermal reaction kettle with a polyvinyl fluoride lining, and reacting for 15-20 h at 200-220 ℃; cooling, washing, vacuum drying, grinding, sieving with a 400-mesh sieve of 200 meshes, then burning for 6-10 hours at 500-550 ℃ in a nitrogen atmosphere, and cooling to room temperature to obtain Sn-Al-O-P.
Furthermore, the mass ratio of the stannic chloride, the aluminum source, the phosphorus trichloride, the ethanol and the sodium citrate is 1:0.5:0.05 (10-15) to (3-4).
Preferably, the aluminum source is selected from one or more of aluminum nitrate, aluminum chloride and aluminum carbonate.
Preferably, the preparation method of the electromagnetic shielding plastic comprises the following steps: and uniformly mixing the raw materials, adding the mixture into a double-screw extruder, and mixing and extruding to obtain the electromagnetic shielding plastic.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
1) the electromagnetic shielding plastic provided by the invention has the advantages of simple and feasible preparation method, easily available raw materials, low price and small dependence on equipment, and is suitable for large-scale production.
2) The electromagnetic shielding plastic provided by the invention overcomes the technical problems that the shielding performance, the mechanical property and the like of the finally obtained material are often unsatisfactory due to the compatibility of the conductive particles and a plastic matrix, the dispersibility of the conductive particles, the processing conditions and the like of the traditional electromagnetic shielding plastic, and has the advantages of excellent mechanical property, good weather resistance and stability and good electromagnetic shielding effect.
3) According to the electromagnetic shielding plastic provided by the invention, the polythiophene fluorenone polymer is added, and the conductivity of the electromagnetic shielding plastic is enabled to be realized due to a conjugated structure, and the conductivity of the electromagnetic shielding plastic is improved under the synergistic effect of the polythiophene fluorenone polymer, the polypyrrole and Sn-Al-O-P modified on the surface of the steel fiber, so that the electromagnetic shielding effect is better; the steel fiber is not corroded and oxidized by the surface modification of the polypyrrole tube, and the polypyrrole tube has conductivity, so that the conductivity is improved, and in addition, the compatibility and the dispersibility of the inorganic additive can be improved; by adding the P element, the plastic has excellent flame retardance.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention.
The raw materials used in the following examples of the present invention were purchased from Shanghai spring Xin import and export trade Co., Ltd.
Example 1
The electromagnetic shielding plastic is prepared from the following raw materials in parts by weight: 100 parts of polythiophene fluorenone polymer, 10 parts of steel fiber surface modification polypyrrole tube, 10 parts of Sn-Al-O-P, 1 part of tetraisopropyl titanate coupling agent and 10101 parts of antioxidant.
The preparation method of the polythiophene fluorenone polymer comprises the following steps: adding 20g of 2, 5-di (5-bromothiophene-2-yl) thiophene, 10g of 2, 5-dihydroxy-9-fluorenone and 3g of potassium carbonate into a three-neck flask connected with a water separator, adding 100g of dimethyl sulfoxide and 30g of toluene, heating the reaction system to 120 ℃, stirring and reacting for 5 hours under the protection of nitrogen, removing water and toluene generated in the reaction process through the water separator, slowly raising the reaction temperature to 135 ℃ after removing water, continuing to stir and react for 8 hours, adding 5g of bis (4-hydroxyphenyl) phenylphosphine oxide, continuing to react for 1 hour, cooling the reaction system to room temperature, precipitating in water, carrying out suction filtration, washing for 4 times with ethanol, and then placing in a vacuum drying oven at 75 ℃ for drying for 15 hours to obtain the polythiophene fluorenone polymer.
The preparation method of the steel fiber surface modified polypyrrole tube comprises the following steps: dispersing 30g of steel fiber in 100g of ethanol, adding 10g of chloropropyltriethoxysilane, stirring at 30 ℃ for reaction for 3 hours, adding 20g of polypyrrole tube and 3g of sodium carbonate, stirring at 70 ℃ for 6 hours, performing suction filtration, washing with ethanol for 3 times, and placing in a vacuum drying oven for drying at 70 ℃ for 8 hours to obtain the steel fiber surface modified polypyrrole tube.
The preparation method of the Sn-Al-O-P comprises the following steps: adding 10g of stannic chloride, 5g of aluminum nitrate and 0.5g of phosphorus trichloride into a beaker containing 100g of ethanol, stirring for 0.5h, then slowly adding 30g of sodium citrate, stirring vigorously for 4h, transferring the solution into a hydrothermal reaction kettle with a polyvinyl fluoride lining, and reacting for 15h at 200 ℃; cooling, washing, vacuum drying, grinding, sieving with 200 mesh sieve, igniting at 500 deg.C under nitrogen atmosphere for 6 hr, and cooling to room temperature to obtain Sn-Al-O-P.
The preparation method of the electromagnetic shielding plastic comprises the following steps: and uniformly mixing the raw materials, adding the mixture into a double-screw extruder, and mixing and extruding to obtain the electromagnetic shielding plastic.
Example 2
The electromagnetic shielding plastic is prepared from the following raw materials in parts by weight: 100 parts of polythiophene fluorenone polymer, 11 parts of steel fiber surface modification polypyrrole tube, 11 parts of Sn-Al-O-P, 5502 parts of silane coupling agent and 10762 parts of antioxidant.
The preparation method of the polythiophene fluorenone polymer comprises the following steps: adding 20g of 2, 5-di (5-bromothiophene-2-yl) thiophene, 10g of 2, 5-dihydroxy-9-fluorenone and 3.5g of cesium carbonate into a three-necked bottle connected with a water separator, adding 115g of N-methylpyrrolidone and 40g of toluene, heating the reaction system to 122 ℃, stirring and reacting for 5.5 hours under the protection of helium, removing water and toluene generated in the reaction process through the water separator, slowly raising the reaction temperature to 138 ℃ after water is removed, continuously stirring and reacting for 8.5 hours, adding 5g of bis (4-hydroxyphenyl) phenyl phosphine oxide, continuously reacting for 1.2 hours, cooling the reaction system to room temperature, precipitating in water, carrying out suction filtration, washing for 5 times by using ethanol, and then drying in a vacuum drying box at 77 ℃ for 16 hours to obtain the polythiophene fluorenone polymer.
The preparation method of the steel fiber surface modified polypyrrole tube comprises the following steps: dispersing 35g of steel fiber in 120g of ethanol, adding 10g of chloropropyltriethoxysilane, stirring and reacting at 33 ℃ for 3.5 hours, adding 20g of polypyrrole tube and 3.5g of potassium carbonate, stirring at 73 ℃ for 6.5 hours, performing suction filtration, washing with ethanol for 4 times, and placing in a vacuum drying oven at 74 ℃ for 9 hours to obtain the steel fiber surface modified polypyrrole tube.
The preparation method of the Sn-Al-O-P comprises the following steps: adding 10g of stannic chloride, 5g of aluminum chloride and 0.5g of phosphorus trichloride into a beaker containing 125g of ethanol, stirring for 0.7h, then slowly adding 33g of sodium citrate, stirring vigorously for 4.5h, transferring the solution into a hydrothermal reaction kettle with a polyvinyl fluoride lining, and reacting for 17h at 205 ℃; cooling, washing, vacuum drying, grinding, sieving with 250 mesh sieve, burning at 510 deg.C under nitrogen atmosphere for 7 hr, and cooling to room temperature to obtain Sn-Al-O-P.
The preparation method of the electromagnetic shielding plastic comprises the following steps: and uniformly mixing the raw materials, adding the mixture into a double-screw extruder, and mixing and extruding to obtain the electromagnetic shielding plastic.
Example 3
The electromagnetic shielding plastic is prepared from the following raw materials in parts by weight: 100 parts of polythiophene fluorenone polymer, 13 parts of steel fiber surface modification polypyrrole tube, 13 parts of Sn-Al-O-P, 5602 parts of silane coupling agent KH and 10103 parts of antioxidant.
The preparation method of the polythiophene fluorenone polymer comprises the following steps: adding 20g of 2, 5-di (5-bromothiophene-2-yl) thiophene, 10g of 2, 5-dihydroxy-9-fluorenone and 4g of sodium carbonate into a three-neck flask connected with a water separator, adding 130g of N, N-dimethylformamide and 45g of toluene, heating the reaction system to 124 ℃, stirring and reacting for 6 hours under the protection of neon gas, removing water and toluene generated in the reaction process through the water separator, slowly raising the reaction temperature to 141 ℃ after water is removed, continuing stirring and reacting for 9 hours, adding 5g of bis (4-hydroxyphenyl) phenylphosphine oxide, continuing reacting for 1.5 hours, cooling the reaction system to room temperature, precipitating in water, carrying out suction filtration, washing for 5 times with ethanol, and then placing in a vacuum drying box at 80 ℃ for drying for 17 hours to obtain the polyfluorenone polymer.
The preparation method of the steel fiber surface modified polypyrrole tube comprises the following steps: dispersing 40g of steel fiber in 135g of ethanol, adding 10g of chloropropyltriethoxysilane, stirring and reacting for 4.2 hours at 35 ℃, then adding 20g of polypyrrole tube and 4.2g of sodium carbonate, stirring for 7.2 hours at 75 ℃, then performing suction filtration, washing for 5 times by using ethanol, and then placing in a vacuum drying oven for drying for 9.2 hours at 76 ℃ to obtain the steel fiber surface modified polypyrrole tube.
The preparation method of the Sn-Al-O-P comprises the following steps: adding 10g of stannic chloride, 5g of aluminum carbonate and 0.5g of phosphorus trichloride into a beaker containing 142g of ethanol, stirring for 0.8h, slowly adding 36g of sodium citrate, stirring vigorously for 4.7h, transferring the solution into a hydrothermal reaction kettle with a polyvinyl fluoride lining, and reacting for 17.5h at 210 ℃; cooling, washing, vacuum drying, grinding, sieving with 300 mesh sieve, igniting at 530 deg.C under nitrogen atmosphere for 8.5 hr, and cooling to room temperature to obtain Sn-Al-O-P.
The preparation method of the electromagnetic shielding plastic comprises the following steps: and uniformly mixing the raw materials, adding the mixture into a double-screw extruder, and mixing and extruding to obtain the electromagnetic shielding plastic.
Example 4
The electromagnetic shielding plastic is prepared from the following raw materials in parts by weight: 100 parts of polythiophene fluorenone polymer, 14 parts of steel fiber surface modification polypyrrole tube, 14 parts of Sn-Al-O-P, 3 parts of coupling agent and 3 parts of antioxidant; the antioxidant is a mixture formed by mixing an antioxidant 1010 and an antioxidant 1076 according to the mass ratio of 2: 3; the coupling agent is a mixture formed by mixing tetraisopropyl titanate coupling agent, silane coupling agent KH550, silane coupling agent KH560 and silane coupling agent KH570 according to the mass ratio of 1:2:1: 3.
The preparation method of the polythiophene fluorenone polymer comprises the following steps: adding 20g of 2, 5-di (5-bromothiophene-2-yl) thiophene, 10g of 2, 5-dihydroxy-9-fluorenone and 4.5g of an alkaline catalyst into a three-neck flask connected with a water separator, adding 145g of a high-boiling point solvent and 55g of toluene, heating a reaction system to 128 ℃, stirring and reacting for 6.5 hours under the protection of argon, removing water and toluene generated in the reaction process through the water separator, slowly raising the reaction temperature to 143 ℃ after water is removed, continuing stirring and reacting for 9.5 hours, adding 5g of bis (4-hydroxyphenyl) phenyl phosphine oxide, continuing reacting for 1.9 hours, cooling the reaction system to room temperature, precipitating in water, carrying out suction filtration, washing for 6 times by using ethanol, and then placing in a vacuum drying oven at 83 ℃ for drying for 19 hours to obtain the polythiophene fluorenone polymer; the high-boiling-point solvent is a mixture formed by mixing dimethyl sulfoxide, N-methyl pyrrolidone and N, N-dimethylformamide according to the mass ratio of 1:2: 3; the alkaline catalyst is a mixture formed by mixing potassium carbonate, cesium carbonate, sodium carbonate and sodium hydroxide according to the mass ratio of 1:2:3: 1.
The preparation method of the steel fiber surface modified polypyrrole tube comprises the following steps: dispersing 48g of steel fiber in 147g of ethanol, adding 10g of chloropropyltriethoxysilane, stirring at 38 ℃ for reaction for 4.8 hours, adding 20g of polypyrrole tube and 4.8g of catalyst, stirring at 79 ℃ for 7.9 hours, performing suction filtration, washing with ethanol for 4 times, and placing in a vacuum drying oven at 79 ℃ for drying for 9.8 hours to obtain the steel fiber surface modified polypyrrole tube; the catalyst is a mixture formed by mixing sodium carbonate and potassium carbonate according to a mass ratio of 3: 5.
The preparation method of the Sn-Al-O-P comprises the following steps: adding 10g of stannic chloride, 5g of aluminum source and 0.5g of phosphorus trichloride into a beaker containing 145g of ethanol, stirring for 0.9h, slowly adding 39g of sodium citrate, stirring vigorously for 4.9h, transferring the solution into a hydrothermal reaction kettle with a polyvinyl fluoride lining, and reacting for 19.5h at 218 ℃; cooling, washing, vacuum drying, grinding, sieving with 350 mesh sieve, igniting at 540 deg.C under nitrogen atmosphere for 9.5 hr, and cooling to room temperature to obtain Sn-Al-O-P; the aluminum source is a mixture formed by mixing aluminum nitrate, aluminum chloride and aluminum carbonate according to the mass ratio of 1:2: 3.
The preparation method of the electromagnetic shielding plastic comprises the following steps: and uniformly mixing the raw materials, adding the mixture into a double-screw extruder, and mixing and extruding to obtain the electromagnetic shielding plastic.
Example 5
The electromagnetic shielding plastic is prepared from the following raw materials in parts by weight: 100 parts of polythiophene fluorenone polymer, 15 parts of steel fiber surface modification polypyrrole tube, 15 parts of Sn-Al-O-P, 15 parts of silane coupling agent KH 5703 parts and 10763 parts of antioxidant.
The preparation method of the polythiophene fluorenone polymer comprises the following steps: adding 20g of 2, 5-di (5-bromothiophene-2-yl) thiophene, 10g of 2, 5-dihydroxy-9-fluorenone and 5g of sodium hydroxide into a three-neck flask connected with a water separator, adding 150g of N-methylpyrrolidone and 60g of toluene, heating the reaction system to 130 ℃, stirring and reacting for 7 hours under the protection of nitrogen, removing water and toluene generated in the reaction process through the water separator, slowly raising the reaction temperature to 145 ℃ after water is removed, continuing stirring and reacting for 10 hours, adding 5g of bis (4-hydroxyphenyl) phenylphosphine oxide, continuing reacting for 2 hours, cooling the reaction system to room temperature, precipitating in water, carrying out suction filtration, washing for 6 times with ethanol, and then placing in a vacuum drying box at 85 ℃ for drying for 20 hours to obtain the polythiophene fluorenone polymer.
The preparation method of the steel fiber surface modified polypyrrole tube comprises the following steps: dispersing 50g of steel fiber in 150g of ethanol, adding 10g of chloropropyltriethoxysilane, stirring at 40 ℃ for reaction for 5 hours, adding 20g of polypyrrole tube and 5g of sodium carbonate, stirring at 80 ℃ for 8 hours, performing suction filtration, washing with ethanol for 5 times, and then placing in a vacuum drying oven for drying at 80 ℃ for 10 hours to obtain the steel fiber surface modified polypyrrole tube.
The preparation method of the Sn-Al-O-P comprises the following steps: adding 10g of stannic chloride, 5g of aluminum chloride and 0.5g of phosphorus trichloride into a beaker containing 150g of ethanol, stirring for 1h, then slowly adding 40g of sodium citrate, stirring vigorously for 5h, transferring the solution into a hydrothermal reaction kettle with a polyvinyl fluoride lining, and reacting for 20h at 220 ℃; cooling, washing, vacuum drying, grinding, sieving with 400 mesh sieve, burning at 550 deg.C under nitrogen atmosphere for 10 hr, and cooling to room temperature to obtain Sn-Al-O-P.
The preparation method of the electromagnetic shielding plastic comprises the following steps: and uniformly mixing the raw materials, adding the mixture into a double-screw extruder, and mixing and extruding to obtain the electromagnetic shielding plastic.
Comparative example
The present example provides a plastic-based composite material with conductive and electromagnetic shielding functions, its formulation and preparation method are the same as those of example 1 of publication No. CN 102250414B.
The performance test, the test method and the test result of the electromagnetic shielding plastics of examples 1 to 5 and comparative example are shown in Table 1.
TABLE 1
As can be seen from table 1, the electromagnetic shielding inhibiting plastic disclosed in the embodiment of the present invention has better mechanical properties, more excellent flame retardancy, and better electromagnetic shielding effect compared with the electromagnetic shielding plastic in the prior art.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. The preparation method of the electromagnetic shielding plastic is characterized by comprising the following steps of: uniformly mixing 100 parts of polythiophene fluorenone polymer, 10-15 parts of steel fiber surface modification polypyrrole tube, 10-15 parts of Sn-Al-O-P, 1-3 parts of coupling agent and 1-3 parts of antioxidant, and then adding the mixture into a double-screw extruder for mixing and extruding to obtain the electromagnetic shielding plastic.
2. The method for preparing electromagnetic shielding plastic according to claim 1, wherein the antioxidant is at least one selected from antioxidant 1010 and antioxidant 1076; the coupling agent is selected from one or more of tetraisopropyl titanate coupling agent, silane coupling agent KH550, silane coupling agent KH560 and silane coupling agent KH 570.
3. The method for preparing the electromagnetic shielding plastic according to claim 1, wherein the method for preparing the polythiophene fluorenone polymer comprises the following steps: adding 2, 5-di (5-bromothiophene-2-yl) thiophene, 2, 5-dihydroxy-9-fluorenone and an alkaline catalyst into a three-neck flask connected with a water separator, adding a high-boiling point solvent and toluene, heating a reaction system to 120-130 ℃, stirring and reacting for 5-7 hours under the protection of nitrogen or inert gas, removing water and toluene generated in the reaction process through the water separator, slowly raising the reaction temperature to 145 ℃ after removing water, continuing to stir and react for 8-10 hours, adding bis (4-hydroxyphenyl) phenylphosphine oxide, continuing to react for 1-2 hours, cooling the reaction system to room temperature, precipitating in water, performing suction filtration, washing for 4-6 times by using ethanol, then placing in a vacuum drying box at 75-85 ℃ for drying for 15-20 hours, thus obtaining a polythiophene fluorenone polymer.
4. The method for preparing electromagnetic shielding plastic according to claim 3, wherein the mass ratio of 2, 5-bis (5-bromothien-2-yl) thiophene, 2, 5-dihydroxy-9-fluorenone, basic catalyst, high boiling point solvent, toluene and bis (4-hydroxyphenyl) phenylphosphine oxide is 2:1 (0.3-0.5): 10-15): 3-6: 0.5.
5. The method for preparing electromagnetic shielding plastic according to claim 3, wherein the high boiling point solvent is one or more selected from dimethyl sulfoxide, N-methyl pyrrolidone and N, N-dimethylformamide; the alkaline catalyst is selected from one or more of potassium carbonate, cesium carbonate, sodium carbonate and sodium hydroxide; the inert gas is selected from one or more of helium, neon and argon.
6. The method for preparing electromagnetic shielding plastic according to claim 1, wherein the method for preparing the steel fiber surface modified polypyrrole tube comprises the following steps: dispersing steel fiber in ethanol, adding chloropropyl triethoxysilane, stirring at 30-40 deg.C for reaction for 3-5 hr, adding polypyrrole tube and catalyst, stirring at 70-80 deg.C for 6-8 hr, vacuum filtering, washing with ethanol for 3-5 times, and drying at 70-80 deg.C for 8-10 hr in vacuum drying oven to obtain steel fiber surface modified polypyrrole tube.
7. The method for preparing electromagnetic shielding plastic according to claim 6, wherein the mass ratio of the steel fiber, the ethanol, the chloropropyltriethoxysilane, the polypyrrole tube and the catalyst is (3-5): 10-15):1:2 (0.3-0.5); the catalyst is selected from at least one of sodium carbonate and potassium carbonate.
8. The method for preparing an electromagnetic shielding plastic according to claim 1, wherein the method for preparing Sn-Al-O-P comprises the following steps: adding stannic chloride, an aluminum source and phosphorus trichloride into a beaker containing ethanol, stirring for 0.5-1 h, then slowly adding sodium citrate, stirring vigorously for 4-5 h, transferring the solution into a hydrothermal reaction kettle with a polyvinyl fluoride lining, and reacting for 15-20 h at 200-220 ℃; cooling, washing, vacuum drying, grinding, sieving with a 400-mesh sieve of 200 meshes, then burning for 6-10 hours at 500-550 ℃ in a nitrogen atmosphere, and cooling to room temperature to obtain Sn-Al-O-P.
9. The method for preparing electromagnetic shielding plastic according to claim 8, wherein the mass ratio of the tin tetrachloride to the aluminum source to the phosphorus trichloride to the ethanol to the sodium citrate is 1:0.5:0.05 (10-15) to (3-4); the aluminum source is selected from one or more of aluminum nitrate, aluminum chloride and aluminum carbonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010483401.2A CN111592739A (en) | 2018-08-01 | 2018-08-01 | Preparation method of electromagnetic shielding plastic |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810861294.5A CN108912614B (en) | 2018-08-01 | 2018-08-01 | Electromagnetic shielding plastic and preparation method thereof |
| CN202010483401.2A CN111592739A (en) | 2018-08-01 | 2018-08-01 | Preparation method of electromagnetic shielding plastic |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810861294.5A Division CN108912614B (en) | 2018-08-01 | 2018-08-01 | Electromagnetic shielding plastic and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111592739A true CN111592739A (en) | 2020-08-28 |
Family
ID=64393635
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810861294.5A Active CN108912614B (en) | 2018-08-01 | 2018-08-01 | Electromagnetic shielding plastic and preparation method thereof |
| CN202010483401.2A Withdrawn CN111592739A (en) | 2018-08-01 | 2018-08-01 | Preparation method of electromagnetic shielding plastic |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810861294.5A Active CN108912614B (en) | 2018-08-01 | 2018-08-01 | Electromagnetic shielding plastic and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN108912614B (en) |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FI82702C (en) * | 1987-07-29 | 1991-04-10 | Neste Oy | Non-conductive plastic composites containing poly (3-alkylthiophene) |
| CN102250414B (en) * | 2011-05-25 | 2013-03-13 | 广东高怡新工程塑料有限公司 | Plastic-based composite material with electricity conducting and electromagnetic shielding functions and preparation method thereof |
| JP2013143354A (en) * | 2012-01-12 | 2013-07-22 | Gunze Ltd | Proton conductive electrolyte membrane and fuel cell using the same |
| CN102617986B (en) * | 2012-04-05 | 2013-11-06 | 天津市飞荣达科技有限公司 | Method for preparing stainless steel fiber resin matrix composite conductive plastics |
| KR20150057555A (en) * | 2013-11-20 | 2015-05-28 | 광주과학기술원 | Manufacturing method for electromagnetic wave shielding material |
-
2018
- 2018-08-01 CN CN201810861294.5A patent/CN108912614B/en active Active
- 2018-08-01 CN CN202010483401.2A patent/CN111592739A/en not_active Withdrawn
Also Published As
| Publication number | Publication date |
|---|---|
| CN108912614A (en) | 2018-11-30 |
| CN108912614B (en) | 2020-08-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111100303B (en) | Preparation method and application of organic phosphine grafted hollow metal organic framework material | |
| CN109627829A (en) | A kind of liquid metal conductive coating and its preparation method and application | |
| CN101286375B (en) | Conductive compound material and method for making same | |
| CN104497809A (en) | Conductive powder coating | |
| CN109423636B (en) | Preparation method of secondary silver-plated high-conductivity filler | |
| CN105219346B (en) | Bio-based carried by nano carbon fiber Conjugate ferrite absorbing material and preparation method thereof | |
| CN112745610A (en) | Modified Mxene/PVA flame-retardant composite material and preparation method thereof | |
| CN109957144B (en) | Preparation method of conductive filler with silver-plated surface | |
| CN113205932B (en) | Low-temperature-resistant anti-pollution-flashover ceramic insulator and manufacturing process thereof | |
| CN111768889B (en) | Electric power composite grease and preparation method and application thereof | |
| CN112188660B (en) | Preparation method of water-based graphene-based electrothermal film | |
| CN107331437A (en) | Graphene low-temperature solidified silver paste compound and preparation method thereof | |
| CN112694661A (en) | Electromagnetic shielding polypropylene composite material with heat conduction and wave absorption functions and preparation method thereof | |
| CN101665235B (en) | Method for preparing n-type doped zinc oxide nanometer powder | |
| CN108912614B (en) | Electromagnetic shielding plastic and preparation method thereof | |
| CN110195351B (en) | Preparation method of carbon nanotube/copper sulfide composite electromagnetic shielding fabric | |
| CN108962496A (en) | A kind of preparation method of solar battery specific complex transparent conductive film | |
| CN112795054A (en) | Cyclic cross-linked polyphosphazene surface modified nickel-cobalt double hydroxide flame retardant and preparation method thereof | |
| CN105714404B (en) | A kind of preparation method of cuprous sulfide/PET composite conducting fibers | |
| CN109988411B (en) | Flame-retardant smoke-suppression thermoplastic polyurethane antistatic composite material and preparation method thereof | |
| CN110218409B (en) | Preparation method of polyacrylonitrile electromagnetic shielding film | |
| CN111269452B (en) | Preparation method of carboxyl nitrile rubber composite film for electromagnetic shielding | |
| CN113284672A (en) | Preparation method of silver nanowire conductive paste | |
| CN113604192A (en) | High-temperature addition type organic silicon electromagnetic shielding adhesive and preparation method thereof | |
| CN103117134B (en) | A kind of preparation method of the solar cell conductive mixed slurry containing butyl stearate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20200828 |