CN115710377B - Ni@Mg enhanced sepiolite composite carbon agent, preparation method thereof and application thereof in EVA - Google Patents

Ni@Mg enhanced sepiolite composite carbon agent, preparation method thereof and application thereof in EVA Download PDF

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CN115710377B
CN115710377B CN202211408289.1A CN202211408289A CN115710377B CN 115710377 B CN115710377 B CN 115710377B CN 202211408289 A CN202211408289 A CN 202211408289A CN 115710377 B CN115710377 B CN 115710377B
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sepiolite
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flame retardant
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庞洪昌
赵广义
沈茜雅
田朋
宁桂玲
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Dalian University of Technology
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Abstract

The invention discloses a Ni@Mg enhanced sepiolite composite charcoal agent, a preparation method and application thereof in EVA, and relates to the field of charcoal agents. A Ni@Mg enhanced sepiolite composite carbon agent comprises Ni@Mg and modified sepiolite; the proportion of Ni@Mg and modified sepiolite is 1:10-10:1 by weight. The Ni@Mg is nano hydroxide hybrid particles; the modified sepiolite is modified by adopting a surface treating agent. The composite char forming agent prepared by the invention can quickly form a compact protective char layer when flame retardant EVA is acted with a mineral flame retardant, thereby isolating heat and combustible gas from being transmitted, protecting a matrix and achieving good flame retardant effect. The invention solves the problem of low flame retardant efficiency of the mineral flame retardant when the EVA is independently flame-retarded.

Description

Ni@Mg enhanced sepiolite composite carbon agent, preparation method thereof and application thereof in EVA
Technical Field
The invention relates to the field of carbonizing agents, in particular to a Ni@Mg enhanced sepiolite compound carbonizing agent, a preparation method thereof and application thereof in EVA.
Background
Ethylene-vinyl acetate copolymer (EVA) is thermoplastic resin with very wide application fields, and is widely applied to the fields of foamed plastic products, wires and cables, shoe industry, toys, photovoltaic materials, solar cell adhesives and the like. The EVA has reduced high crystallinity, improved toughness, impact resistance, filler compatibility and heat sealability due to the introduction of vinyl acetate, as compared to Polyethylene (PE). However, EVA has a limiting oxygen index of only 17% -19%, is extremely easy to burn, and often has a molten drop phenomenon during burning. The relatively large fire hazard of EVA greatly limits its application, and flame retardant EVA composites have been a hotspot of research.
The principle of flame retardation of polyolefin materials can be divided into terminating free radical chain reactions, forming protective layers and cooling combustion systems. Terminating the radical chain reaction: the polyolefin is subjected to dehydrogenation reaction during thermal decomposition to generate a large amount of high-activity free radicals, and flame retardant effects such as brominated flame retardants, phosphorus flame retardants and the like are achieved by introducing flame retardants capable of quenching the free radicals. Forming a protective layer: the flame retardant can form an isolation layer during combustion, and the formed isolation layer can isolate heat and oxygen from transmitting and prevent combustible gas from escaping, so that the decomposition of a matrix, such as an intumescent flame retardant, expandable graphite and the like, is prevented. Cooling the combustion system: the fire retardant can generate dehydration, phase change and other endothermic reactions at a certain temperature, can greatly reduce the temperature of a combustion area, offset the heat required by further combustion, and achieve the purpose of fire retardation, such as magnesium hydroxide, aluminum hydroxide, water magnesite and the like. Among them, the mineral flame retardant used for cooling the combustion system is popular among researchers because of its low price and wide sources. However, when such flame retardants are used alone, the flame retarding efficiency is not high. Therefore, the Ni@Mg enhanced sepiolite composite carbon agent is prepared, and the carbon agent can form a compact protective carbon layer when being used together with a mineral flame retardant, so that a good flame retardant effect is achieved.
Disclosure of Invention
According to the invention, ni@Mg is prepared by a one-step hydrothermal method and is compounded with modified sepiolite to prepare the Ni@Mg enhanced sepiolite compound carbon agent, and the compound carbon agent can rapidly form a compact protective carbon layer when being used for flame-retardant EVA (ethylene vinyl acetate) under the combined action of the compound carbon agent and a mineral flame retardant, so that heat and combustible gas are isolated from being transmitted, a substrate is protected, and a good flame-retardant effect is achieved.
The invention provides a Ni@Mg enhanced sepiolite composite carbon agent, which comprises Ni@Mg and modified sepiolite; the mass ratio of Ni@Mg to modified sepiolite is 1-10:1-10; the Ni@Mg is nano hydroxide hybrid particles; the modified sepiolite is modified by adopting a surface treating agent.
Further, in the technical scheme, the mass ratio of Ni to Mg in the Ni@Mg is 1-3:1.
The invention provides a preparation method of Ni@Mg enhanced sepiolite composite charcoal agent, which comprises the following steps:
step 1, preparation of Ni@Mg:
(1) Grinding a magnesium oxide raw material, a nickel source and a solvent in proportion to obtain slurry;
(2) Transferring the reactant slurry into a static hydrothermal kettle, and reacting for 8-12 h at 150-220 ℃;
(3) After the reaction is finished, the dried Ni@Mg is obtained through post-treatment and is crushed;
step 2, preparing modified sepiolite:
s1, uniformly stirring sepiolite particles and a solvent according to a proportion;
s2, adding the surface treating agent into the mixed slurry according to a certain proportion, and stirring at 25-30 ℃ for 2-5 h;
s3, under the condition of continuously stirring, drying in a circulating water bath at 70-90 ℃, and finally crushing to prepare the modified sepiolite;
wherein the surface treating agent in S2 is one or two or more of cetyltrimethylammonium chloride, octadecyl trimethylammonium chloride, cetyltrimethylammonium bromide and octadecyl trimethylammonium bromide.
Further, in the above technical scheme, in the step 1, ball milling is adopted in the step (1), the magnesia raw material, the nickel source and the solvent are proportionally put into a ball milling tank, corundum balls are added, and the ball milling is carried out for 2-4 hours to prepare slurry. The ratio of the amounts of the magnesium oxide raw material and the nickel source material is 100:30-50; the nickel source is one or two or more of nickel nitrate, nickel acetate, nickel chloride and nickel sulfate; the solvent in the step (1) is deionized water; the mass ratio of the magnesium oxide raw material to the nickel source to the solvent is 1-3:2-10.
Further, in the above technical scheme, in step 1, the post-treatment in step (3) is suction filtration, washing and drying; the filter cake is washed by ethanol for 2-4 times, the drying temperature is 70-120 ℃, and the drying time is 8-12 hours; and (3) crushing the mixture by a crusher to obtain Ni@Mg with the particle size smaller than 1 mu m.
Further, in the above technical scheme, in step 2, the stirring of S1 is performed by using a high-speed disperser, the rotation speed of the high-speed disperser is 800-1500 r/min, and the dispersing time is 10-30 min; the solvent in the S1 is water, and the mass ratio of the sepiolite particles to the water is 1-3:4-10.
Further, in the above technical scheme, in the step 2, the addition amount of the S2 surface treatment agent accounts for 10% -15% by mass; and (3) crushing in the step (S3) by using a crusher to obtain the modified sepiolite with the particle size smaller than 20 mu m.
The invention also provides application of the Ni@Mg enhanced sepiolite composite carbon forming agent, wherein the composite carbon forming agent and the mineral flame retardant are compounded and applied to EVA.
Further, in the technical scheme, the mass ratio of the composite char forming agent to the mineral flame retardant is 1:3-10.
Further, in the above technical scheme, the mineral flame retardant comprises one of hydromagnesite flame retardant and brucite mineral flame retardant.
Drawings
FIG. 1 is a scanning electron microscope image of Ni@Mg of example 1.
FIG. 2 is a scanning electron microscope image of the modified sepiolite of example 1.
Fig. 3 is a graph comparing heat release rates of comparative example 1, comparative example 2, comparative example 3 and examples 1, 2, and 3.
Fig. 4 is a photograph of the burnt carbon residue of comparative example 1 (a), comparative example 2 (b), comparative example 3 (c), example 1 (d), example 2 (e), example 3 (f) and example 4 (g), respectively.
The invention has the beneficial effects that
According to the invention, ni@Mg is prepared by a one-step hydrothermal method and is compounded with modified sepiolite to prepare the Ni@Mg enhanced sepiolite compound carbon agent, and the compound carbon agent can rapidly form a compact protective carbon layer when being used for flame-retardant EVA (ethylene vinyl acetate) under the combined action of the compound carbon agent and a mineral flame retardant, so that heat and combustible gas are isolated from being transmitted, a substrate is protected, and a good flame-retardant effect is achieved. The invention solves the problem of low flame retardant efficiency of the mineral flame retardant when the EVA is independently flame-retarded.
Detailed Description
The following non-limiting examples will provide those skilled in the art with a more complete understanding of the invention, but are not intended to limit the invention in any way, and are intended to provide numerous non-essential modifications and adaptations to the invention as described above, and yet fall within the scope of the invention.
Comparative example 1
Only hydromagnesite flame retardant is added, and the total flame retardant filling amount is 51.5 percent, so that the flame retardant is applied to 48.5 percent EVA. Peak heat release rate of composite 450.9KW/m 2 The surface of the burnt carbon residue has more holes and cracks and poorer flame retardant property.
Comparative example 2
10g of magnesium oxide raw material, 22g of nickel acetate and 90ml of deionized water are put into a ball milling tank, 150g of corundum balls are added, and ball milling is carried out for 2 hours to prepare slurry; transferring the reactant slurry into a static hydrothermal kettle, and reacting for 12 hours at 170 ℃; after the reaction is finished, carrying out suction filtration, washing a filter cake with ethanol for 2-4 times, putting the filter cake into an oven at 80 ℃ for drying for 12 hours, and finally crushing the filter cake by a crusher to obtain Ni@Mg;
the addition amount of Ni@Mg is 8%, the addition amount of hydromagnesite flame retardant is 43.5%, and the total addition amount of Ni@Mg and the flame retardant filling amount is 51.5%, so that the additive is applied to 48.5% EVA. Compared with 51.5 percent of filling hydromagnesite fire retardant which is used alone, the peak value of the heat release rate of the composite material is 356.4KW/m 2 The reduction is 20.9%, the holes and cracks on the surface of the burnt carbon residue are less, and the flame retardant property is improved.
Comparative example 3
50g of sepiolite and 200ml of water are taken in a stirring tank, and a high-speed dispersing machine is used for dispersing for 30min after rotating speed is adjusted to 800 r/min. Thereafter, 2.25g of octadecyl trimethyl ammonium bromide and 5.25g of octadecyl trimethyl ammonium chloride were dissolved in 80ml of technical ethanol. Then adding the ethanol solution of the surface treating agent into a high-speed dispersing machine, adjusting the rotating speed to 1500r/min, and stirring the mixed slurry for 3 hours at the temperature of 25-30 ℃. Drying was performed by a circulating water bath at 85 ℃ with constant stirring. Crushing the dried sepiolite by using a crusher to obtain modified sepiolite;
the addition amount of sepiolite is 8%, the addition amount of hydromagnesite flame retardant is 43.5%, and the total addition amount of Ni@Mg and the addition amount of flame retardant is 51.5%, so that the additive is applied to 48.5% EVA. Compared with 51.5 percent of filling hydromagnesite fire retardant which is used alone, the peak value of the heat release rate of the composite material is 330.9KW/m 2 The reduction is 26.6%, the surface of the burnt carbon residue is provided with small holes, and the flame retardant property is improved.
Example 1
10g of magnesium oxide raw material, 22g of nickel acetate and 90ml of deionized water are put into a ball milling tank, 150g of corundum balls are added, and ball milling is carried out for 2 hours to prepare slurry; transferring the reactant slurry into a static hydrothermal kettle, and reacting for 12 hours at 170 ℃; filtering after the reaction is finished, washing a filter cake with ethanol for 2-4 times, putting the filter cake into an oven at 80 ℃ for drying for 12 hours, and finally crushing the filter cake by a crusher to obtain Ni@Mg, wherein the particle size of the Ni@Mg is less than 1 mu m; the Ni@Mg scanning electron microscope chart is shown in FIG. 1.
50g of sepiolite and 200ml of water are taken in a stirring tank, and a high-speed dispersing machine is used for dispersing for 30min after rotating speed is adjusted to 800 r/min. Thereafter, 2.25g of octadecyl trimethyl bromide and 5.25g of octadecyl trimethyl ammonium chloride were dissolved in 80ml of technical ethanol. Then adding the ethanol solution of the surface treating agent into a high-speed dispersing machine, adjusting the rotating speed to 1500r/min, and stirring the mixed slurry for 3 hours at the temperature of 25-30 ℃. Drying was performed by a circulating water bath at 85 ℃ with constant stirring. After drying, crushing the dried product by using a crusher to obtain modified sepiolite, wherein the particle size of the modified sepiolite is less than 20 mu m; the scanning electron microscope diagram of the modified sepiolite is shown in figure 2.
Ni@Mg and modified sepiolite are compounded according to the mass ratio of 2:3, the adding amount is 8%, the adding amount of hydromagnesite flame retardant is 43.5%, the total adding amount of char forming agent and flame retardant is 51.5%, and the modified sepiolite is applied to 48.5% EVA. Compared with 51.5 percent of filling hydromagnesite fire retardant which is used alone, the peak value of the heat release rate of the composite material is 267.1KW/m 2 The reduction is 40.8%, no holes or cracks exist on the surface of the burnt carbon residue, and the flame retardant property is better.
Example 2
10g of magnesium oxide raw material, 36.3 nickel nitrate hexahydrate and 90ml of deionized water are put into a ball milling tank, 150g of corundum balls are added, and ball milling is carried out for 2 hours to prepare slurry; transferring the reactant slurry into a static hydrothermal kettle, and reacting for 12 hours at 170 ℃; filtering after the reaction is finished, washing a filter cake with ethanol for 2-4 times, putting the filter cake into an oven at 80 ℃ for drying for 12 hours, and finally crushing the filter cake by a crusher to obtain Ni@Mg, wherein the particle size of the Ni@Mg is less than 1 mu m;
50g of sepiolite and 200ml of water are taken in a stirring tank, and a high-speed dispersing machine is used for dispersing for 30min after rotating speed is adjusted to 800 r/min. Thereafter, 3g of octadecyl trimethyl bromide and 4.5g of octadecyl trimethyl ammonium chloride were dissolved in 80ml of technical ethanol. Then adding the ethanol solution of the surface treating agent into a high-speed dispersing machine, adjusting the rotating speed to 1500r/min, and stirring the mixed slurry for 3 hours at the temperature of 25-30 ℃. Drying was performed by a circulating water bath at 85 ℃ with constant stirring. After drying, crushing the dried product by using a crusher to obtain modified sepiolite, wherein the particle size of the modified sepiolite is less than 20 mu m;
Ni@Mg and modified sepiolite are compounded according to the mass ratio of 1:1, the adding amount is 8%, the adding amount of hydromagnesite flame retardant is 43.5%, the total adding amount of char forming agent and flame retardant is 51.5%, and the modified sepiolite is applied to 48.5% EVA. Compared with 51.5 percent of filling hydromagnesite fire retardant which is used alone, the peak value of the heat release rate of the composite material is 302.1KW/m 2 The flame retardant is reduced by 33%, no holes or cracks are formed on the surface of the burnt carbon residue, and the flame retardant performance is improved.
Example 3
10g of magnesium oxide raw material, 36.3 nickel nitrate hexahydrate and 90ml of deionized water are put into a ball milling tank, 150g of corundum balls are added, and ball milling is carried out for 2 hours to prepare slurry; transferring the reactant slurry into a static hydrothermal kettle, and reacting for 12 hours at 170 ℃; filtering after the reaction is finished, washing a filter cake with ethanol for 2-4 times, putting the filter cake into an oven at 80 ℃ for drying for 12 hours, and finally crushing the filter cake by a crusher to obtain Ni@Mg, wherein the particle size of the Ni@Mg is less than 1 mu m;
50g of sepiolite and 200ml of water are taken in a stirring tank, and a high-speed dispersing machine is used for dispersing for 30min after rotating speed is adjusted to 800 r/min. Thereafter, 3g of octadecyl trimethyl bromide and 4.5g of octadecyl trimethyl ammonium chloride were dissolved in 80ml of technical ethanol. Then adding the ethanol solution of the surface treating agent into a high-speed dispersing machine, adjusting the rotating speed to 1500r/min, and stirring the mixed slurry for 3 hours at the temperature of 25-30 ℃. Drying was performed by a circulating water bath at 85 ℃ with constant stirring. After drying, crushing the dried product by using a crusher to obtain modified sepiolite, wherein the particle size of the modified sepiolite is less than 20 mu m;
Ni@Mg and modified sepiolite are compounded according to a mass ratio of 5:3, the adding amount is 8%, the adding amount of hydromagnesite flame retardant is 43.5%, the total adding amount of char forming agent and flame retardant is 51.5%, and the modified sepiolite is applied to 48.5% EVA. Compared with 51.5 percent of filling hydromagnesite fire retardant which is used alone, the peak value of the heat release rate of the composite material is 293.1KW/m 2 The flame retardant is reduced by 35%, no holes or cracks are formed on the surface of the burnt carbon residue, and the flame retardant performance is improved.
Example 4
10g of magnesium oxide raw material, 36.3 nickel nitrate hexahydrate and 90ml of deionized water are put into a ball milling tank, 150g of corundum balls are added, and ball milling is carried out for 2 hours to prepare slurry; transferring the reactant slurry into a static hydrothermal kettle, and reacting for 12 hours at 170 ℃; filtering after the reaction is finished, washing a filter cake with ethanol for 2-4 times, putting the filter cake into an oven at 80 ℃ for drying for 12 hours, and finally crushing the filter cake by a crusher to obtain Ni@Mg, wherein the particle size of the Ni@Mg is less than 1 mu m;
50g of sepiolite and 200ml of water are taken in a stirring tank, and a high-speed dispersing machine is used for dispersing for 30min after rotating speed is adjusted to 800 r/min. Thereafter, 3g of octadecyl trimethyl bromide and 4.5g of octadecyl trimethyl ammonium chloride were dissolved in 80ml of technical ethanol. Then adding the ethanol solution of the surface treating agent into a high-speed dispersing machine, adjusting the rotating speed to 1500r/min, and stirring the mixed slurry for 3 hours at the temperature of 25-30 ℃. Drying was performed by a circulating water bath at 85 ℃ with constant stirring. After drying, crushing the dried product by using a crusher to obtain modified sepiolite, wherein the particle size of the modified sepiolite is less than 20 mu m;
Ni@Mg and modified sepiolite are compounded according to a mass ratio of 5:3, the adding amount is 8%, the adding amount of brucite mineral flame retardant is 43.5%, the total adding amount of char forming agent and flame retardant is 51.5%, and the modified sepiolite is applied to 48.5% EVA. Compared with 51.5 percent of brucite mineral flame retardant which is filled singly, the peak value of the heat release rate of the composite material is275.1KW/m 2 The flame retardant is reduced by 36%, no holes or cracks are formed on the surface of the burnt carbon residue, and the flame retardant performance is improved.

Claims (9)

1. The Ni@Mg enhanced sepiolite composite carbon agent is characterized by comprising Ni@Mg and modified sepiolite; the mass ratio of Ni@Mg to modified sepiolite is 1-10:1-10; the Ni@Mg is nano hydroxide hybrid particles; the modified sepiolite is modified by adopting a surface treating agent;
the preparation method of the Ni@Mg enhanced sepiolite composite carbon agent comprises the following steps:
step 1, preparation of Ni@Mg:
(1) Grinding a magnesium oxide raw material, a nickel source and a solvent in proportion to obtain slurry;
(2) Transferring the reactant slurry into a static hydrothermal kettle, and reacting for 8-12 h at 150-220 ℃;
(3) After the reaction is finished, the dried Ni@Mg is obtained through post-treatment and is crushed;
step 2, preparing modified sepiolite:
s1, uniformly stirring sepiolite particles and a solvent according to a proportion to obtain mixed slurry;
s2, adding the surface treating agent into the mixed slurry according to a proportion, and stirring at 25-30 ℃ for 2-5 h;
s3, under the condition of continuously stirring, drying in a circulating water bath at 70-90 ℃, and finally crushing to prepare the modified sepiolite;
wherein the surface treating agent in S2 is one or two or more of cetyltrimethylammonium chloride, octadecyl trimethylammonium chloride, cetyltrimethylammonium bromide and octadecyl trimethylammonium bromide.
2. The ni@mg enhanced sepiolite composite charcoal agent of claim 1, wherein the mass ratio of Ni to Mg in the ni@mg is 1-3:1.
3. The Ni@Mg enhanced sepiolite composite charcoal agent according to claim 1, wherein in the step 1, ball milling is adopted in the grinding in the step 1, a magnesium oxide raw material, a nickel source and a solvent are put into a ball milling tank according to a proportion, corundum balls are added, and the ball milling is carried out for 2-4 hours to prepare slurry; the ratio of the amounts of the magnesium oxide raw material and the nickel source material is 100:30-50; the nickel source is one or two or more of nickel nitrate, nickel acetate, nickel chloride and nickel sulfate; the solvent in the step (1) is deionized water; the mass ratio of the magnesium oxide raw material to the nickel source to the solvent is 1-3:2-10.
4. The Ni@Mg enhanced sepiolite composite charcoal agent according to claim 1, wherein in the step 1, the post-treatment in the step (3) is suction filtration, washing and drying, the washing adopts ethanol to wash a filter cake for 2-4 times, and the drying temperature is 70-120 ℃ and the drying time is 8-12 hours; and (3) crushing the mixture by a crusher to obtain Ni@Mg with the particle size smaller than 1 mu m.
5. The Ni@Mg enhanced sepiolite composite charcoal agent according to claim 1, wherein in the step 2, a high-speed dispersing machine is adopted for stirring in the step S1, the rotating speed of the high-speed dispersing machine is 800-1500 r/min, and the dispersing time is 10-30 min; the solvent in the S1 is water, and the mass ratio of the sepiolite particles to the water is 1-3:4-10.
6. The Ni@Mg enhanced sepiolite composite charcoal agent according to claim 1, wherein in the step 2, the addition amount of the surface treatment agent is 10% -15% by mass; and (3) crushing in the step (S3) by using a crusher to obtain the modified sepiolite with the particle size smaller than 20 mu m.
7. The use of the ni@mg enhanced sepiolite composite char agent of claim 1, wherein the composite char agent is applied to EVA in combination with a mineral flame retardant.
8. The use of the Ni@Mg enhanced sepiolite composite char agent according to claim 7, wherein the mass ratio of the composite char agent to the mineral flame retardant is 1:3-10.
9. The use of the ni@mg enhanced sepiolite composite char of claim 8, wherein said mineral flame retardant comprises one of hydromagnesite flame retardant, brucite mineral flame retardant.
CN202211408289.1A 2022-11-10 2022-11-10 Ni@Mg enhanced sepiolite composite carbon agent, preparation method thereof and application thereof in EVA Active CN115710377B (en)

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