CN112831115A - Air-permeable anti-static foam material and preparation method thereof - Google Patents

Air-permeable anti-static foam material and preparation method thereof Download PDF

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CN112831115A
CN112831115A CN202110111797.2A CN202110111797A CN112831115A CN 112831115 A CN112831115 A CN 112831115A CN 202110111797 A CN202110111797 A CN 202110111797A CN 112831115 A CN112831115 A CN 112831115A
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罗伟才
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    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
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Abstract

The invention discloses a breathable anti-static foam material and a preparation method thereof, wherein the foam material comprises the following raw materials in parts by weight: 100-120 parts of low-density polyethylene, 10-15 parts of glyceryl monostearate, 3-8 parts of talcum powder, 3-5 parts of antistatic agent, 1-3 parts of flame-retardant particles, 3-5 parts of foaming agent and 1-3 parts of nucleating agent; the antistatic agent and the flame-retardant particles are prepared in the preparation process, the antistatic agent is prepared by performing esterification reaction on the intermediate 5 and the intermediate 6 to prepare an intermediate 7, and the intermediate 7 is polymerized to prepare the antistatic agent, the antistatic agent can increase the volume conductivity of the foamed plastic, so that static electricity accumulated in the foamed plastic is timely conducted out, and the antistatic effect is further achieved.

Description

Air-permeable anti-static foam material and preparation method thereof
Technical Field
The invention relates to the technical field of foam material preparation, in particular to a breathable anti-static foam material and a preparation method thereof.
Background
During transportation, articles are usually protected by using foamed plastics such as polystyrene, polyethylene, polyurethane and other foamed plastics. For electronic products such as integrated circuits and communication devices which are susceptible to static electricity, the packaging material needs to have an antistatic function. Compared with polystyrene, polyethylene, polyurethane and other materials, the polyvinyl chloride has low price and excellent flame retardant property, so that the antistatic foam material produced by using the polyvinyl chloride is very suitable for packaging, transporting and storing electronic products.
Most of the existing foam materials are prepared from polymers with high volume resistivity, so that charges are easy to gather on the surface to generate a large amount of static electricity, the materials are easy to generate dust absorption phenomenon and even cause explosion, and the foam plastics are easy to burn due to the influence of the self form.
Disclosure of Invention
The invention aims to provide a breathable and antistatic foam material and a preparation method thereof.
The technical problems to be solved by the invention are as follows:
most of the existing foam materials are prepared from polymers with high volume resistivity, so that charges are easy to gather on the surface to generate a large amount of static electricity, the materials are easy to generate dust absorption phenomenon and even cause explosion, and the foam plastics are easy to burn due to the influence of the self form.
The purpose of the invention can be realized by the following technical scheme:
the breathable anti-static foam material comprises the following raw materials in parts by weight: 100-120 parts of low-density polyethylene, 10-15 parts of glyceryl monostearate, 3-8 parts of talcum powder, 3-5 parts of antistatic agent, 1-3 parts of flame-retardant particles, 3-5 parts of foaming agent and 1-3 parts of nucleating agent;
step S1: adding low-density polyethylene, glyceryl monostearate, talcum powder, an antistatic agent, flame-retardant particles and a nucleating agent into an internal mixer, and carrying out internal mixing for 15-20min at the temperature of 130-150 ℃ to prepare a mixture;
step S2: continuously banburying the mixture and the foaming agent prepared in the step S1 for 10-15min at the temperature of 100-110 ℃, adding the mixture and the foaming agent into a mold, and preserving heat for 10-15min at the temperature of 180-190 ℃ and the pressure of 1.5-2MPa to prepare a prefabricated product;
step S3: and adding the prefabricated product into a foaming mold, and foaming for 10-15min at the temperature of 80-100 ℃ to obtain the foam material.
Furthermore, the foaming agent is one or more of calcium carbonate, magnesium carbonate and sodium bicarbonate which are mixed in any proportion, and the nucleating agent is one or more of magnesium oxide, carbon black and mica which are mixed in any proportion.
Further, the antistatic agent is prepared by the following steps:
step A1: adding sodium sulfide and methanol into a reaction kettle, stirring and dropwise adding methyl chloroacetate under the conditions that the rotation speed is 150-200r/min and the temperature is 40-50 ℃, dropwise adding for 2-3h, continuously reacting for 15-20min after dropwise adding, adding tetrabutylammonium bromide, reacting for 5-8h under the condition that the temperature is 25-30 ℃ to obtain an intermediate 1, adding a sodium methoxide solution into the reaction kettle, adding the intermediate 1 and diethyl oxalate under the conditions that the rotation speed is 200-300r/min and the temperature is 5-10 ℃, stirring for 5-10min, performing reflux reaction for 2-4h under the condition that the temperature is 70-80 ℃, removing the solvent, and adding a hydrochloric acid solution until the pH value of the reaction solution is 6 to obtain an intermediate 2;
the reaction process is as follows:
Figure BDA0002919322320000031
step A2: adding the intermediate 2, chloromethyl oxirane and N, N-dimethylformamide into a reaction kettle, stirring for 5-10min under the condition of the rotation speed of 200-150℃, adding potassium carbonate and triethylamine, reacting for 8-12h under the condition of the temperature of 130-150℃ to obtain an intermediate 3, adding the intermediate 3 and a sodium hydroxide solution into the reaction kettle, reacting for 2-3h under the conditions of the rotation speed of 150-200℃ and the temperature of 80-90℃, cooling to the temperature of 25-30 ℃, adjusting the pH of a reaction solution to 1-2 to obtain an intermediate 4, adding the intermediate 4 and dimethyl sulfoxide into the reaction kettle, stirring under the condition of the rotation speed of 200-300℃ until the intermediate 4 is completely dissolved, adding copper powder, stirring at the temperature of 150-180℃, reacting for 8-10h to obtain an intermediate 5;
the reaction process is as follows:
Figure BDA0002919322320000032
Figure BDA0002919322320000041
step A3: dissolving octadecylamine in ethanol, adding chloroacetic acid and triethylamine, reacting for 3-5h at the rotation speed of 150-200r/min and the temperature of 30-40 ℃ to obtain an intermediate 6, adding the intermediate 6, the intermediate 5 and concentrated sulfuric acid into a reaction kettle, reacting for 3-5h at the rotation speed of 150-80 ℃ and the temperature of 60-80 ℃ to obtain an intermediate 7, adding the intermediate 7 into a sodium polystyrene sulfonate aqueous solution, adding potassium persulfate, and reacting at the temperature of 25-30 ℃ to obtain the antistatic agent.
The reaction process is as follows:
Figure BDA0002919322320000042
further, the amount ratio of the sodium sulfide, the methanol, the methyl chloroacetate and the tetrabutylammonium bromide in the step A1 is 50g:100mL:20g:1.5g, the amount ratio of the sodium methoxide solution, the intermediate 1 and the diethyl oxalate is 50mL:1.5g:1.2g, the mass fraction of the sodium methoxide solution is 15%, the amount ratio of the intermediate 2, the chloromethyl oxirane, the potassium carbonate and the triethylamine in the step A2 is 5:30:2:3, the amount ratio of the intermediate 3 to the sodium hydroxide solution is 1g:10mL, the mass fraction of the sodium hydroxide solution is 10%, the amount ratio of the intermediate 4, the dimethyl sulfoxide and the copper powder is 1g:5mL:0.1g, the amount molar ratio of the octadecylamine and the chloroacetic acid in the step A3 is 1:2, the amount molar ratio of the intermediate 6 to the intermediate 5 is 1:2, and the amount of the concentrated sulfuric acid is 30-35% of the intermediate 6 by mass, the mass fraction of the concentrated sulfuric acid is 95%, the dosage ratio of the intermediate 7, the sodium polystyrene sulfonate aqueous solution and the potassium sulfate is 4g to 20mL to 0.2g, and the mass fraction of the sodium polystyrene sulfonate aqueous solution is 5-10%.
Further, the flame retardant particles are prepared by the following steps:
step B1: adding a nitric acid solution and a sulfuric acid solution into a reaction kettle, stirring for 5-10min at the rotation speed of 150-200r/min, adding toluene, continuing to react for 3-5h at the temperature of 80-85 ℃ to obtain an intermediate 8, adding iron powder and ethanol into the reaction kettle, performing reflux reaction for 3-5h at the temperature of 80-85 ℃, adding a hydrochloric acid solution for 20min, continuing to react for 5-8h, and adjusting the pH value of a reaction solution to 7-8 to obtain an intermediate 9;
the reaction process is as follows:
Figure BDA0002919322320000051
step B2: adding the intermediate 9, diphenylphosphine chloride and chloroform into a reaction kettle, stirring uniformly, adding triethylamine, carrying out reflux reaction for 5-8h at the temperature of 70-75 ℃ to obtain an intermediate 10, dispersing the intermediate 10 into deionized water, adding potassium dichromate, stirring at the rotation speed of 150-5 ℃ for 3-5 ℃ and adding concentrated sulfuric acid, stirring at the temperature of 20-30 ℃ for 3-5min, heating to 50-55 ℃, reacting for 1-1.5h to obtain an intermediate 11, dissolving graphene oxide into deionized water, adding the intermediate 11 and 1-hydroxybenzotriazole, reacting at the temperature of 40-50 ℃ for 3-5h, distilling to remove the deionized water, and preparing the flame-retardant particles.
The reaction process is as follows:
Figure BDA0002919322320000061
further, the mass ratio of the nitric acid solution, the sulfuric acid solution and the toluene in the step B1 is 3:8:2, the mass fraction of the nitric acid solution is 97%, the mass fraction of the sulfuric acid solution is 95%, the mass ratio of the intermediate 8, the iron powder, the ethanol and the hydrochloric acid solution is 2g:4.5g:60mL:10mL, the volume fraction of the ethanol is 90%, the hydrochloric acid solution is formed by mixing concentrated hydrochloric acid with the mass fraction of 36% and ethanol with the volume fraction of 95% in a volume ratio of 1:9, the molar ratio of the intermediate 9, the diphenylphosphinic chloride and the triethylamine in the step B2 is 1:2:1, the mass ratio of the intermediate 10, the potassium dichromate and the concentrated sulfuric acid is 1g:2.5g:8mL, the mass fraction of the concentrated sulfuric acid is 98%, and the mass ratio of the graphene oxide, the intermediate 11, the ethylenediamine and the 1-hydroxybenzotriazole is 5:3:1.2: 1.8.
A preparation method of a breathable anti-static foam material specifically comprises the following steps:
step S1: adding low-density polyethylene, glyceryl monostearate, talcum powder, an antistatic agent, flame-retardant particles and a nucleating agent into an internal mixer, and carrying out internal mixing for 15-20min at the temperature of 130-150 ℃ to prepare a mixture;
step S2: continuously banburying the mixture and the foaming agent prepared in the step S1 for 10-15min at the temperature of 100-110 ℃, adding the mixture and the foaming agent into a mold, and preserving heat for 10-15min at the temperature of 180-190 ℃ and the pressure of 1.5-2MPa to prepare a prefabricated product;
step S3: and adding the prefabricated product into a foaming mold, and foaming for 10-15min at the temperature of 80-100 ℃ to obtain the foam material.
The invention has the beneficial effects that: the invention discloses a process for preparing a ventilating antistatic foam material, which comprises the steps of preparing an antistatic agent, using methyl chloroacetate as a raw material to react with sodium sulfide to prepare an intermediate 1, reacting the intermediate 1 with diethyl oxalate to prepare an intermediate 2, reacting the intermediate 2 with chloromethyl oxirane to prepare an intermediate 3, treating the intermediate 3 with a sodium hydroxide solution to prepare an intermediate 4, reacting the intermediate 4 with copper powder to prepare an intermediate 5, reacting octadecylamine with chloroacetic acid to prepare an intermediate 6, carrying out esterification reaction on the intermediate 5 and the intermediate 6 to prepare an intermediate 7, polymerizing the intermediate 7 to prepare the antistatic agent, wherein the antistatic agent can increase the volume conductivity of the foam plastic and further lead static accumulated in the foam plastic to be conducted out in time, the flame-retardant particles are prepared by using toluene as a raw material, treating the toluene with a nitric acid solution and a sulfuric acid solution to prepare an intermediate 8, reducing the intermediate 8 to convert nitro groups on benzene rings into amino groups to prepare an intermediate 9, reacting the intermediate 9 with diphenylphosphinic chloride to prepare an intermediate 10, oxidizing the intermediate 10 to convert methyl groups into carboxyl groups, condensing the methyl groups with one amino group in ethylenediamine under the action of 1-hydroxybenzotriazole, condensing the other amino group in the ethylenediamine with the carboxyl group on graphene oxide to prepare the flame-retardant particles, and generating a coke layer on the surface of the material when the foamed plastic is combusted, wherein the coke layer can isolate oxygen and heat to extinguish flame.
Detailed Description
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.
Example 1
The breathable anti-static foam material comprises the following raw materials in parts by weight: 100 parts of low-density polyethylene, 10 parts of glyceryl monostearate, 3 parts of talcum powder, 3 parts of antistatic agent, 1 part of flame-retardant particles, 3 parts of magnesium carbonate and 1 part of carbon black;
step S1: adding low-density polyethylene, glyceryl monostearate, talcum powder, an antistatic agent, flame-retardant particles and carbon black into an internal mixer, and carrying out internal mixing for 15min at the temperature of 130 ℃ to prepare a mixture;
step S2: continuously banburying the mixture prepared in the step S1 and magnesium carbonate for 10min at the temperature of 100 ℃, adding the mixture into a mold, and preserving heat for 10min at the temperature of 180 ℃ and under the pressure of 1.5MPa to prepare a prefabricated product;
step S3: and adding the prefabricated product into a foaming mold, and foaming for 10min at the temperature of 80 ℃ to obtain the foam material.
The antistatic agent is prepared by the following steps:
step A1: adding sodium sulfide and methanol into a reaction kettle, stirring and dropwise adding methyl chloroacetate under the conditions of the rotating speed of 150r/min and the temperature of 40 ℃, dropwise adding for 2 hours, continuously reacting for 15 minutes after dropwise adding, adding tetrabutylammonium bromide, reacting for 5 hours under the condition of the temperature of 25 ℃ to prepare an intermediate 1, adding a sodium methoxide solution into the reaction kettle, adding the intermediate 1 and diethyl oxalate under the conditions of the rotating speed of 200r/min and the temperature of 5 ℃, stirring for 5 minutes, performing reflux reaction for 2 hours under the condition of the temperature of 70 ℃, removing a solvent, adding a hydrochloric acid solution until the pH value of a reaction solution is 6, and preparing an intermediate 2;
step A2: adding the intermediate 2, chloromethyl oxirane and N, N-dimethylformamide into a reaction kettle, stirring for 5min at the rotation speed of 200r/min, adding potassium carbonate and triethylamine, reacting for 8h at the temperature of 130 ℃ to obtain an intermediate 3, adding the intermediate 3 and a sodium hydroxide solution into the reaction kettle, reacting for 2h at the rotation speed of 150r/min and the temperature of 80 ℃, cooling to the temperature of 25 ℃, adjusting the pH of a reaction solution to 1 to obtain an intermediate 4, adding the intermediate 4 and dimethyl sulfoxide into the reaction kettle, stirring at the rotation speed of 200r/min until the intermediate 4 is completely dissolved, adding copper powder, and reacting for 8h at the temperature of 150 ℃ to obtain an intermediate 5;
step A3: dissolving octadecylamine in ethanol, adding chloroacetic acid and triethylamine, reacting for 3 hours at the rotation speed of 150r/min and the temperature of 30 ℃ to obtain an intermediate 6, adding the intermediate 6, the intermediate 5 and concentrated sulfuric acid into a reaction kettle, reacting for 3 hours at the rotation speed of 120r/min and the temperature of 60 ℃ to obtain an intermediate 7, adding the intermediate 7 into a sodium polystyrene sulfonate aqueous solution, adding potassium persulfate, and reacting at the temperature of 25 ℃ to obtain the antistatic agent.
The flame retardant particles are prepared by the following steps:
step B1: adding a nitric acid solution and a sulfuric acid solution into a reaction kettle, stirring for 5min at the rotation speed of 150r/min, adding toluene, continuing to react for 3h at the temperature of 80 ℃ to obtain an intermediate 8, adding iron powder and ethanol into the reaction kettle, performing reflux reaction for 3h at the temperature of 80 ℃, adding a hydrochloric acid solution, adding for 20min, continuing to react for 5h, and adjusting the pH value of a reaction solution to 7 to obtain an intermediate 9;
step B2: adding the intermediate 9, diphenylphosphine chloride and chloroform into a reaction kettle, stirring uniformly, adding triethylamine, carrying out reflux reaction for 5 hours at the temperature of 70 ℃ to obtain an intermediate 10, dispersing the intermediate 10 into deionized water, adding potassium dichromate, stirring at the rotation speed of 120r/min and the temperature of 3 ℃ and adding concentrated sulfuric acid, stirring at the temperature of 20 ℃ for 3 minutes, heating to the temperature of 50 ℃, reacting for 1 hour to obtain an intermediate 11, dissolving graphene oxide into deionized water, adding the intermediate 11, ethylenediamine and 1-hydroxybenzotriazole, reacting at the temperature of 40 ℃ for 3 hours, and distilling to remove the deionized water to obtain the flame-retardant particles.
Example 2
The breathable anti-static foam material comprises the following raw materials in parts by weight: 105 parts of low-density polyethylene, 12 parts of glyceryl monostearate, 4 parts of talcum powder, 4 parts of antistatic agent, 2 parts of flame-retardant particles, 4 parts of magnesium carbonate and 2 parts of carbon black;
step S1: adding low-density polyethylene, glyceryl monostearate, talcum powder, an antistatic agent, flame-retardant particles and carbon black into an internal mixer, and internally mixing for 20min at the temperature of 130 ℃ to prepare a mixture;
step S2: continuously banburying the mixture prepared in the step S1 and magnesium carbonate for 15min at the temperature of 100 ℃, adding the mixture into a mold, and preserving heat for 10min at the temperature of 180 ℃ and under the pressure of 2MPa to prepare a prefabricated product;
step S3: and adding the prefabricated product into a foaming mold, and foaming for 10min at the temperature of 100 ℃ to obtain the foam material.
The antistatic agent is prepared by the following steps:
step A1: adding sodium sulfide and methanol into a reaction kettle, stirring and dropwise adding methyl chloroacetate at the rotation speed of 200r/min and the temperature of 40 ℃, dropwise adding for 3 hours, continuously reacting for 15 minutes after dropwise adding, adding tetrabutylammonium bromide, reacting for 5 hours at the temperature of 30 ℃ to obtain an intermediate 1, adding a sodium methoxide solution into the reaction kettle, adding the intermediate 1 and diethyl oxalate at the rotation speed of 300r/min and the temperature of 5 ℃, stirring for 10 minutes, performing reflux reaction for 4 hours at the temperature of 70 ℃, removing a solvent, adding a hydrochloric acid solution until the pH value of the reaction solution is 6, and preparing an intermediate 2;
step A2: adding the intermediate 2, chloromethyl oxirane and N, N-dimethylformamide into a reaction kettle, stirring for 10min at the rotation speed of 200r/min, adding potassium carbonate and triethylamine, reacting for 12h at the temperature of 130 ℃ to obtain an intermediate 3, adding the intermediate 3 and a sodium hydroxide solution into the reaction kettle, reacting for 2h at the rotation speed of 150r/min and the temperature of 90 ℃, cooling to the temperature of 30 ℃, adjusting the pH value of a reaction solution to 1 to obtain an intermediate 4, adding the intermediate 4 and dimethyl sulfoxide into the reaction kettle, stirring at the rotation speed of 300r/min until the intermediate 4 is completely dissolved, adding copper powder, and reacting for 10h at the temperature of 150 ℃ to obtain an intermediate 5;
step A3: dissolving octadecylamine in ethanol, adding chloroacetic acid and triethylamine, reacting for 3h at the rotation speed of 150r/min and the temperature of 40 ℃ to obtain an intermediate 6, adding the intermediate 6, the intermediate 5 and concentrated sulfuric acid into a reaction kettle, reacting for 5h at the rotation speed of 150r/min and the temperature of 60 ℃ to obtain an intermediate 7, adding the intermediate 7 into a sodium polystyrene sulfonate aqueous solution, adding potassium persulfate, and reacting at the temperature of 25 ℃ to obtain the antistatic agent.
The flame retardant particles are prepared by the following steps:
step B1: adding a nitric acid solution and a sulfuric acid solution into a reaction kettle, stirring for 5min at the rotation speed of 200r/min, adding toluene, continuing to react for 3h at the temperature of 85 ℃ to obtain an intermediate 8, adding iron powder and ethanol into the reaction kettle, performing reflux reaction for 3h at the temperature of 85 ℃, adding a hydrochloric acid solution, adding for 20min, continuing to react for 8h, and adjusting the pH value of a reaction solution to 7 to obtain an intermediate 9;
step B2: adding the intermediate 9, diphenylphosphine chloride and chloroform into a reaction kettle, stirring uniformly, adding triethylamine, carrying out reflux reaction for 5 hours at the temperature of 75 ℃ to obtain an intermediate 10, dispersing the intermediate 10 into deionized water, adding potassium dichromate, stirring at the rotation speed of 150r/min and the temperature of 3 ℃ and adding concentrated sulfuric acid, stirring at the temperature of 30 ℃ for 3 minutes, heating to 55 ℃, reacting for 1 hour to obtain an intermediate 11, dissolving graphene oxide into deionized water, adding the intermediate 11, ethylenediamine and 1-hydroxybenzotriazole, reacting at the temperature of 50 ℃ for 3 hours, and distilling to remove the deionized water to obtain the flame-retardant particles.
Example 3
The breathable anti-static foam material comprises the following raw materials in parts by weight: 115 parts of low-density polyethylene, 14 parts of glyceryl monostearate, 6 parts of talcum powder, 4 parts of antistatic agent, 2 parts of flame-retardant particles, 4 parts of magnesium carbonate and 2 parts of carbon black;
step S1: adding low-density polyethylene, glyceryl monostearate, talcum powder, an antistatic agent, flame-retardant particles and carbon black into an internal mixer, and carrying out internal mixing for 15min at the temperature of 150 ℃ to prepare a mixture;
step S2: continuously banburying the mixture prepared in the step S1 and magnesium carbonate for 10min at the temperature of 110 ℃, adding the mixture into a mold, and keeping the temperature for 15min at the temperature of 190 ℃ and the pressure of 1.5MPa to prepare a prefabricated product;
step S3: and adding the prefabricated product into a foaming mold, and foaming for 15min at the temperature of 80 ℃ to obtain the foam material.
The antistatic agent is prepared by the following steps:
step A1: adding sodium sulfide and methanol into a reaction kettle, stirring and dropwise adding methyl chloroacetate under the conditions of the rotation speed of 150r/min and the temperature of 50 ℃, dropwise adding for 2 hours, continuously reacting for 20 minutes after dropwise adding, adding tetrabutylammonium bromide, reacting for 8 hours under the condition of the temperature of 25 ℃ to obtain an intermediate 1, adding a sodium methoxide solution into the reaction kettle, adding the intermediate 1 and diethyl oxalate under the conditions of the rotation speed of 200r/min and the temperature of 10 ℃, stirring for 5 minutes, performing reflux reaction for 2 hours under the condition of the temperature of 80 ℃, removing a solvent, adding a hydrochloric acid solution until the pH value of the reaction solution is 6, and preparing an intermediate 2;
step A2: adding the intermediate 2, chloromethyl oxirane and N, N-dimethylformamide into a reaction kettle, stirring for 5min at the rotation speed of 300r/min, adding potassium carbonate and triethylamine, reacting for 8h at the temperature of 150 ℃ to obtain an intermediate 3, adding the intermediate 3 and a sodium hydroxide solution into the reaction kettle, reacting for 3h at the rotation speed of 200r/min and the temperature of 80 ℃, cooling to the temperature of 25 ℃, adjusting the pH of a reaction solution to be 2 to obtain an intermediate 4, adding the intermediate 4 and dimethyl sulfoxide into the reaction kettle, stirring at the rotation speed of 200r/min until the intermediate 4 is completely dissolved, adding copper powder, and reacting for 8h at the temperature of 180 ℃ to obtain an intermediate 5;
step A3: dissolving octadecylamine in ethanol, adding chloroacetic acid and triethylamine, reacting for 5 hours at the rotation speed of 200r/min and the temperature of 30 ℃ to obtain an intermediate 6, adding the intermediate 6, the intermediate 5 and concentrated sulfuric acid into a reaction kettle, reacting for 3 hours at the rotation speed of 120r/min and the temperature of 80 ℃ to obtain an intermediate 7, adding the intermediate 7 into a sodium polystyrene sulfonate aqueous solution, adding potassium persulfate, and reacting at the temperature of 30 ℃ to obtain the antistatic agent.
The flame retardant particles are prepared by the following steps:
step B1: adding a nitric acid solution and a sulfuric acid solution into a reaction kettle, stirring for 10min at the rotation speed of 150r/min, adding toluene, continuing to react for 5h at the temperature of 80 ℃ to obtain an intermediate 8, adding iron powder and ethanol into the reaction kettle, performing reflux reaction for 5h at the temperature of 80 ℃, adding a hydrochloric acid solution, adding for 20min, continuing to react for 5h, and adjusting the pH value of a reaction solution to 8 to obtain an intermediate 9;
step B2: adding the intermediate 9, diphenylphosphine chloride and chloroform into a reaction kettle, stirring uniformly, adding triethylamine, carrying out reflux reaction for 8 hours at the temperature of 70 ℃ to obtain an intermediate 10, dispersing the intermediate 10 into deionized water, adding potassium dichromate, stirring at the rotation speed of 120r/min and the temperature of 5 ℃ and adding concentrated sulfuric acid, stirring at the temperature of 20 ℃ for 5 minutes, heating to the temperature of 50 ℃, reacting for 1.5 hours to obtain an intermediate 11, dissolving graphene oxide into deionized water, adding the intermediate 11, ethylenediamine and 1-hydroxybenzotriazole, reacting at the temperature of 40 ℃ for 5 hours, and distilling to remove the deionized water to obtain the flame-retardant particles.
Example 4
The breathable anti-static foam material comprises the following raw materials in parts by weight: 120 parts of low-density polyethylene, 15 parts of glyceryl monostearate, 8 parts of talcum powder, 5 parts of antistatic agent, 3 parts of flame-retardant particles, 5 parts of magnesium carbonate and 3 parts of carbon black;
step S1: adding low-density polyethylene, glyceryl monostearate, talcum powder, an antistatic agent, flame-retardant particles and carbon black into an internal mixer, and internally mixing for 20min at the temperature of 150 ℃ to prepare a mixture;
step S2: continuously banburying the mixture prepared in the step S1 and magnesium carbonate for 15min at the temperature of 110 ℃, adding the mixture into a mold, and keeping the temperature for 15min at the temperature of 190 ℃ and under the pressure of 2MPa to prepare a prefabricated product;
step S3: and adding the prefabricated product into a foaming mold, and foaming for 15min at the temperature of 100 ℃ to obtain the foam material.
The antistatic agent is prepared by the following steps:
step A1: adding sodium sulfide and methanol into a reaction kettle, stirring and dropwise adding methyl chloroacetate at the rotation speed of 200r/min and the temperature of 50 ℃, dropwise adding for 3 hours, continuously reacting for 20 minutes after dropwise adding, adding tetrabutylammonium bromide, reacting for 8 hours at the temperature of 30 ℃ to obtain an intermediate 1, adding a sodium methoxide solution into the reaction kettle, adding the intermediate 1 and diethyl oxalate at the rotation speed of 300r/min and the temperature of 10 ℃, stirring for 10 minutes, performing reflux reaction for 4 hours at the temperature of 80 ℃, removing a solvent, adding a hydrochloric acid solution until the pH value of the reaction solution is 6, and preparing an intermediate 2;
step A2: adding the intermediate 2, chloromethyl oxirane and N, N-dimethylformamide into a reaction kettle, stirring for 10min at the rotation speed of 300r/min, adding potassium carbonate and triethylamine, reacting for 12h at the temperature of 150 ℃ to obtain an intermediate 3, adding the intermediate 3 and a sodium hydroxide solution into the reaction kettle, reacting for 3h at the rotation speed of 200r/min and the temperature of 90 ℃, cooling to the temperature of 30 ℃, adjusting the pH of a reaction solution to be 2 to obtain an intermediate 4, adding the intermediate 4 and dimethyl sulfoxide into the reaction kettle, stirring at the rotation speed of 300r/min until the intermediate 4 is completely dissolved, adding copper powder, and reacting for 10h at the temperature of 180 ℃ to obtain an intermediate 5;
step A3: dissolving octadecylamine in ethanol, adding chloroacetic acid and triethylamine, reacting for 5 hours at the rotation speed of 200r/min and the temperature of 40 ℃ to obtain an intermediate 6, adding the intermediate 6, the intermediate 5 and concentrated sulfuric acid into a reaction kettle, reacting for 5 hours at the rotation speed of 150r/min and the temperature of 80 ℃ to obtain an intermediate 7, adding the intermediate 7 into a sodium polystyrene sulfonate aqueous solution, adding potassium persulfate, and reacting at the temperature of 30 ℃ to obtain the antistatic agent.
The flame retardant particles are prepared by the following steps:
step B1: adding a nitric acid solution and a sulfuric acid solution into a reaction kettle, stirring for 10min at the rotation speed of 200r/min, adding toluene, continuing to react for 5h at the temperature of 85 ℃ to obtain an intermediate 8, adding iron powder and ethanol into the reaction kettle, performing reflux reaction for 5h at the temperature of 85 ℃, adding a hydrochloric acid solution, adding for 20min, continuing to react for 8h, and adjusting the pH value of a reaction solution to 8 to obtain an intermediate 9;
step B2: adding the intermediate 9, diphenylphosphine chloride and chloroform into a reaction kettle, stirring uniformly, adding triethylamine, carrying out reflux reaction for 8 hours at the temperature of 75 ℃ to obtain an intermediate 10, dispersing the intermediate 10 into deionized water, adding potassium dichromate, stirring at the rotation speed of 150r/min and the temperature of 5 ℃ and adding concentrated sulfuric acid, stirring at the temperature of 30 ℃ for 5 minutes, heating to the temperature of 55 ℃, reacting for 1.5 hours to obtain an intermediate 11, dissolving graphene oxide into deionized water, adding the intermediate 11, ethylenediamine and 1-hydroxybenzotriazole, reacting at the temperature of 50 ℃ for 5 hours, and distilling to remove the deionized water to obtain the flame-retardant particles.
Comparative example
This comparative example is a common foam on the market.
The foams obtained in examples 1 to 4 and comparative example were subjected to the performance test, the test results of which are shown in Table 1 below;
TABLE 1
Figure BDA0002919322320000161
As can be seen from Table 1 above, the foams obtained in examples 1 to 4 had a volume resistivity of 106Omega cm, a burning time of 7-8s and no generation of drips, and the foam obtained in the comparative example has a volume resistivity of 013Omega cm, the burning time is 15s, and a small amount of dripping occurs, which shows that the antistatic flame retardant coating has good antistatic property and flame retardance.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.

Claims (7)

1. A breathable, antistatic foam material, characterized by: the feed comprises the following raw materials in parts by weight: 100-120 parts of low-density polyethylene, 10-15 parts of glyceryl monostearate, 3-8 parts of talcum powder, 3-5 parts of antistatic agent, 1-3 parts of flame-retardant particles, 3-5 parts of foaming agent and 1-3 parts of nucleating agent;
step S1: adding low-density polyethylene, glyceryl monostearate, talcum powder, an antistatic agent, flame-retardant particles and a nucleating agent into an internal mixer, and carrying out internal mixing for 15-20min at the temperature of 130-150 ℃ to prepare a mixture;
step S2: continuously banburying the mixture and the foaming agent prepared in the step S1 for 10-15min at the temperature of 100-110 ℃, adding the mixture and the foaming agent into a mold, and preserving heat for 10-15min at the temperature of 180-190 ℃ and the pressure of 1.5-2MPa to prepare a prefabricated product;
step S3: and adding the prefabricated product into a foaming mold, and foaming for 10-15min at the temperature of 80-100 ℃ to obtain the foam material.
2. The breathable, antistatic foam material of claim 1, wherein: the foaming agent is one or more of calcium carbonate, magnesium carbonate and sodium bicarbonate which are mixed in any proportion, and the nucleating agent is one or more of magnesium oxide, carbon black and mica which are mixed in any proportion.
3. The breathable, antistatic foam material of claim 1, wherein: the antistatic agent is prepared by the following steps:
step A1: adding sodium sulfide and methanol into a reaction kettle, stirring and dropwise adding methyl chloroacetate under the conditions that the rotation speed is 150-200r/min and the temperature is 40-50 ℃, dropwise adding for 2-3h, continuously reacting for 15-20min after dropwise adding, adding tetrabutylammonium bromide, reacting for 5-8h under the condition that the temperature is 25-30 ℃ to obtain an intermediate 1, adding a sodium methoxide solution into the reaction kettle, adding the intermediate 1 and diethyl oxalate under the conditions that the rotation speed is 200-300r/min and the temperature is 5-10 ℃, stirring for 5-10min, performing reflux reaction for 2-4h under the condition that the temperature is 70-80 ℃, removing the solvent, and adding a hydrochloric acid solution until the pH value of the reaction solution is 6 to obtain an intermediate 2;
step A2: adding the intermediate 2, chloromethyl oxirane and N, N-dimethylformamide into a reaction kettle, stirring for 5-10min under the condition of the rotation speed of 200-150℃, adding potassium carbonate and triethylamine, reacting for 8-12h under the condition of the temperature of 130-150℃ to obtain an intermediate 3, adding the intermediate 3 and a sodium hydroxide solution into the reaction kettle, reacting for 2-3h under the conditions of the rotation speed of 150-200℃ and the temperature of 80-90℃, cooling to the temperature of 25-30 ℃, adjusting the pH of a reaction solution to 1-2 to obtain an intermediate 4, adding the intermediate 4 and dimethyl sulfoxide into the reaction kettle, stirring under the condition of the rotation speed of 200-300℃ until the intermediate 4 is completely dissolved, adding copper powder, stirring at the temperature of 150-180℃, reacting for 8-10h to obtain an intermediate 5;
step A3: dissolving octadecylamine in ethanol, adding chloroacetic acid and triethylamine, reacting for 3-5h at the rotation speed of 150-200r/min and the temperature of 30-40 ℃ to obtain an intermediate 6, adding the intermediate 6, the intermediate 5 and concentrated sulfuric acid into a reaction kettle, reacting for 3-5h at the rotation speed of 150-80 ℃ and the temperature of 60-80 ℃ to obtain an intermediate 7, adding the intermediate 7 into a sodium polystyrene sulfonate aqueous solution, adding potassium persulfate, and reacting at the temperature of 25-30 ℃ to obtain the antistatic agent.
4. A breathable, antistatic foam material according to claim 3, wherein: the using amount ratio of the sodium sulfide, the methanol, the methyl chloroacetate and the tetrabutylammonium bromide in the step A1 is 50g:100mL:20g:1.5g, the using amount ratio of the sodium methoxide solution, the intermediate 1 and the diethyl oxalate is 50mL:1.5g:1.2g, the mass fraction of the sodium methoxide solution is 15%, the using amount ratio of the intermediate 2, the chloromethyl oxirane, the potassium carbonate and the triethylamine in the step A2 is 5:30:2:3, the using amount ratio of the intermediate 3 to the sodium hydroxide solution is 1g:10mL, the mass fraction of the sodium hydroxide solution is 10%, the using amount ratio of the intermediate 4, the dimethyl sulfoxide and the copper powder is 1g:5mL:0.1g, the using amount molar ratio of the octadecylamine and the chloroacetic acid in the step A3 is 1:2, the using amount molar ratio of the intermediate 6 to the intermediate 5 is 1:2, and the using amount of the concentrated sulfuric acid is 30-35% of the mass of the intermediate 6, the mass fraction of the concentrated sulfuric acid is 95%, the dosage ratio of the intermediate 7, the sodium polystyrene sulfonate aqueous solution and the potassium sulfate is 4g to 20mL to 0.2g, and the mass fraction of the sodium polystyrene sulfonate aqueous solution is 5-10%.
5. The breathable, antistatic foam material of claim 1, wherein: the flame retardant particles are prepared by the following steps:
step B1: adding a nitric acid solution and a sulfuric acid solution into a reaction kettle, stirring for 5-10min at the rotation speed of 150-200r/min, adding toluene, continuing to react for 3-5h at the temperature of 80-85 ℃ to obtain an intermediate 8, adding iron powder and ethanol into the reaction kettle, performing reflux reaction for 3-5h at the temperature of 80-85 ℃, adding a hydrochloric acid solution for 20min, continuing to react for 5-8h, and adjusting the pH value of a reaction solution to 7-8 to obtain an intermediate 9;
step B2: adding the intermediate 9, diphenylphosphine chloride and chloroform into a reaction kettle, stirring uniformly, adding triethylamine, carrying out reflux reaction for 5-8h at the temperature of 70-75 ℃ to obtain an intermediate 10, dispersing the intermediate 10 into deionized water, adding potassium dichromate, stirring at the rotation speed of 150-5 ℃ for 3-5 ℃ and adding concentrated sulfuric acid, stirring at the temperature of 20-30 ℃ for 3-5min, heating to 50-55 ℃, reacting for 1-1.5h to obtain an intermediate 11, dissolving graphene oxide into deionized water, adding the intermediate 11 and 1-hydroxybenzotriazole, reacting at the temperature of 40-50 ℃ for 3-5h, distilling to remove the deionized water, and preparing the flame-retardant particles.
6. The breathable, antistatic foam material of claim 5, wherein: the mass ratio of the nitric acid solution, the sulfuric acid solution and the toluene in the step B1 is 3:8:2, the mass fraction of the nitric acid solution is 97%, the mass fraction of the sulfuric acid solution is 95%, the mass ratio of the intermediate 8, the iron powder, the ethanol and the hydrochloric acid solution is 2g:4.5g:60mL:10mL, the volume fraction of the ethanol is 90%, the hydrochloric acid solution is concentrated hydrochloric acid with the mass fraction of 36% and the ethanol with the volume fraction of 95% are mixed according to the volume ratio of 1:9, the molar ratio of the intermediate 9, the diphenyl hypophosphoryl chloride and the triethylamine in the step B2 is 1:2:1, the mass ratio of the intermediate 10, the potassium dichromate and the concentrated sulfuric acid is 1g:2.5g:8mL, the mass fraction of the concentrated sulfuric acid is 98%, and the mass ratio of the chromic acid, the intermediate 11, the ethylenediamine and the 1-hydroxybenzotriazole is 5:3:1.2: 1.8.
7. The method for preparing the air-permeable antistatic foam material according to claim 1, wherein the method comprises the following steps: the method specifically comprises the following steps:
step S1: adding low-density polyethylene, glyceryl monostearate, talcum powder, an antistatic agent, flame-retardant particles and a nucleating agent into an internal mixer, and carrying out internal mixing for 15-20min at the temperature of 130-150 ℃ to prepare a mixture;
step S2: continuously banburying the mixture and the foaming agent prepared in the step S1 for 10-15min at the temperature of 100-110 ℃, adding the mixture and the foaming agent into a mold, and preserving heat for 10-15min at the temperature of 180-190 ℃ and the pressure of 1.5-2MPa to prepare a prefabricated product;
step S3: and adding the prefabricated product into a foaming mold, and foaming for 10-15min at the temperature of 80-100 ℃ to obtain the foam material.
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