CN110615919A - Low-smoke modified halogen-free flame retardant and preparation method thereof - Google Patents
Low-smoke modified halogen-free flame retardant and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/14—Peroxides
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- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Abstract
The invention discloses a low-smoke modified halogen-free flame retardant and a preparation method thereof, and particularly relates to the technical field of halogen-free flame retardants, wherein the low-smoke modified halogen-free flame retardant comprises the following components in parts by weight: 50-80 parts of magnesium hydroxide particles, 10-20 parts of dolomite powder, 5-10 parts of clay, 80-120 parts of deionized water, 5-10 parts of sepiolite powder, 1-5 parts of coupling agent, 1-5 parts of dicumyl peroxide and 1-5 parts of benzoyl peroxide. The magnesium hydroxide particles with small particle diameters are adopted, the surfaces of the magnesium hydroxide particles are modified to improve the compatibility of the magnesium hydroxide particles with polymers, and then the magnesium hydroxide particles are mixed with other polymers in the raw materials, so that the magnesium hydroxide particles can be fully compatible with effective components in the raw materials, the flame retardant efficiency of the flame retardant is improved, and the magnesium hydroxide is adopted as the main raw material, so that the magnesium hydroxide is low in smoke, non-toxic, more environment-friendly and green in the combustion process, and is favorable for popularization.
Description
Technical Field
The invention relates to the technical field of halogen-free flame retardants, in particular to a low-smoke modified halogen-free flame retardant and a preparation method thereof.
Background
When a fire disaster happens, a large amount of smoke and toxic corrosive hydrogen halide gas are generated in the flame retardant process of the halogen-containing flame retardant material, so that secondary harm is caused. The new flame-retardant system has small smoke amount during combustion and does not generate toxic and corrosive gases.
The halogen-free flame retardant additive mainly comprises phosphorus compounds and metal hydroxides. These two types of compounds are called pollution-free flame retardants because they do not volatilize and do not generate corrosive gases when burned, and there are several types of novel halogen-free flame retardants such as silicon-based flame retardants and nitrogen-based flame retardants. The novel halogen-free flame retardant becomes a new product meeting the development trend of international standards. However, in the use process of the existing halogen-free flame retardant, due to improper treatment of the raw materials, the compatibility of the raw materials is poor, the flame retardant components cannot be well compatible, and the flame retardant efficiency of the flame retardant is affected.
Disclosure of Invention
In order to overcome the defects in the prior art, the embodiment of the invention provides a low-smoke modified halogen-free flame retardant and a preparation method thereof, magnesium hydroxide particles with small particle diameters are adopted, the surface of the magnesium hydroxide particles is modified to improve the compatibility of the magnesium hydroxide particles and polymers, and then the magnesium hydroxide particles are mixed with other polymer sections in raw materials to ensure that the magnesium hydroxide particles are fully compatible with effective components in the raw materials, so that the flame retardant efficiency of the flame retardant is improved.
In order to achieve the purpose, the invention provides the following technical scheme: a low-smoke modified halogen-free flame retardant specifically comprises the following components in parts by weight: 50-80 parts of magnesium hydroxide particles, 10-20 parts of dolomite powder, 5-10 parts of clay, 80-120 parts of deionized water, 5-10 parts of sepiolite powder, 1-5 parts of coupling agent, 1-5 parts of dicumyl peroxide and 1-5 parts of benzoyl peroxide.
In a preferred embodiment, the composition specifically comprises the following components in parts by weight: 60-70 parts of magnesium hydroxide particles, 12-18 parts of dolomite powder, 6-8 parts of clay, 90-110 parts of deionized water, 6-8 parts of sepiolite powder, 2-4 parts of coupling agent, 2-4 parts of dicumyl peroxide and 2-4 parts of benzoyl peroxide.
In a preferred embodiment, the composition specifically comprises the following components in parts by weight: 65 parts of magnesium hydroxide particles, 15 parts of dolomite powder, 7 parts of clay, 100 parts of deionized water, 7 parts of sepiolite powder, 3 parts of coupling agent, 3 parts of dicumyl peroxide and 3 parts of benzoyl peroxide.
In a preferred embodiment, the coupling agent is one or a mixture of a titanate-based coupling agent and a silane coupling agent.
In a preferred embodiment, the mesh size of the dolomite powder, sepiolite powder and magnesium hydroxide particles is 200-300 mesh.
A preparation method of a low-smoke modified halogen-free flame retardant specifically comprises the following steps:
step one, diluting a surface treatment agent with a proper amount of inert solvent, pouring the diluted surface treatment agent into a stirring kettle, adding magnesium hydroxide particles into the stirring kettle, stirring and mixing at a low speed for 20-30 minutes at room temperature, heating to 90 ℃, and stirring at a high speed for 50-60 minutes to obtain modified magnesium hydroxide particles;
adding clay into a ball mill, mixing and crushing the clay by using the ball mill to obtain 0.5-1mm of clay crushed aggregates, filtering the clay crushed aggregates by using a screen to remove impurities in the clay crushed aggregates, adding the filtered clay crushed aggregates, dolomite powder and sepiolite powder into a stirring kettle, starting the stirring kettle, stirring for 20-30 minutes at a speed of 120/rpm, sealing, and standing for 2-3 hours to obtain a raw material mixture;
pouring deionized water, a coupling agent, dicumyl peroxide and benzoyl peroxide into a heating container with a heating function in sequence, stirring the mixture by using a stirrer for 5 to 10 minutes, heating the temperature in the heating container to 40 to 50 ℃, standing the mixture for 30 minutes, pouring the solution into the container, placing the container into a refrigerating chamber for refrigerating for 8 to 10 hours, taking the container out, and removing scum and impurities on the surface of the solution;
step four, adding the modified magnesium hydroxide particles prepared in the step one into a stirring kettle, then adding the raw material mixture obtained in the step two into the stirring kettle, starting the stirring kettle to stir for 5-10 minutes, pouring the solution obtained in the step three into the stirring kettle, starting the stirring kettle to stir for 20-30 minutes, pouring into a sealable container, sealing, placing in a room temperature environment, standing for 5-8 hours, and taking out to obtain the low-smoke modified halogen-free flame retardant.
In a preferred embodiment, in the first step, the rotation speed of the low-speed stirring is 30-40 rpm, and the high-speed stirring is 120-.
In a preferred embodiment, the screen used in the second step is made of a stainless material, the screen has a screen hole diameter of 0.5 to 1mm, and the temperature of the refrigerating chamber in the third step is set to 0 ℃.
The invention has the technical effects and advantages that:
1. the magnesium hydroxide particles with small particle diameters are adopted, the surfaces of the magnesium hydroxide particles are modified to improve the compatibility of the magnesium hydroxide particles with polymers, and then the magnesium hydroxide particles are mixed with other polymers in the raw materials, so that the magnesium hydroxide particles can be fully compatible with effective components in the raw materials, the flame retardant efficiency of the flame retardant is improved, and the magnesium hydroxide is adopted as the main raw material, so that the magnesium hydroxide is low in smoke, non-toxic, more environment-friendly and green in combustion process, and favorable for popularization;
2. by adding dolomite powder and sepiolite powder, ball-milling clay, mixing, fully stirring and mixing the clay and the raw materials, adding the coupling agent, dicumyl peroxide and benzoyl peroxide, the performance of the flame retardant can be improved, the combustion of combustible substances can be effectively retarded in the combustion process, and the polymer carbonization can be promoted.
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:
a low-smoke modified halogen-free flame retardant comprises the following components: magnesium hydroxide particles, dolomite powder, clay, deionized water, sepiolite powder, a coupling agent, dicumyl peroxide and benzoyl peroxide;
specifically, the composition comprises the following components in parts by weight: 65 parts of magnesium hydroxide particles, 15 parts of dolomite powder, 7 parts of clay, 100 parts of deionized water, 7 parts of sepiolite powder, 3 parts of coupling agent, 3 parts of dicumyl peroxide and 3 parts of benzoyl peroxide;
furthermore, in the above components, the coupling agent is a mixture of titanate coupling agent and silane coupling agent, and the mesh number of the dolomite powder, the sepiolite powder and the magnesium hydroxide particles is 250 meshes;
on the basis, the preparation method of the low-smoke modified halogen-free flame retardant specifically comprises the following steps:
step one, diluting a surface treating agent with a proper amount of inert solvent, pouring the diluted surface treating agent into a stirring kettle, adding 65 parts of magnesium hydroxide particles into the stirring kettle, stirring and mixing at low speed of 35 revolutions per minute for 25 minutes at room temperature, heating to 90 ℃, and stirring at high speed of 130 revolutions per minute for 55 minutes to obtain modified magnesium hydroxide particles;
adding 7 parts of clay into a ball mill, mixing and crushing the clay by using the ball mill to obtain 0.8mm crushed clay, filtering the crushed clay by using a stainless steel screen with the diameter of a screen hole of 0.8mm to remove impurities in the crushed clay, adding the filtered crushed clay, 15 parts of dolomite powder and 7 parts of sepiolite powder into a stirring kettle, starting the stirring kettle, stirring at the speed of 120/rpm for 25 minutes, sealing, and standing for 2.5 hours to obtain a raw material mixture;
pouring 100 parts of deionized water, 3 parts of coupling agent, 3 parts of dicumyl peroxide and 3 parts of benzoyl peroxide into a heating container with a heating function in sequence, stirring the mixture for 8 minutes by using a stirrer, raising the temperature in the heating container to 45 ℃, standing the mixture for 30 minutes, pouring the solution into the container, placing the container into a refrigerating chamber with the temperature of 0 ℃ for refrigerating for 9 hours, taking the container out, and removing scum and impurities on the surface of the solution;
step four, adding the modified magnesium hydroxide particles prepared in the step one into a stirring kettle, then adding the raw material mixture obtained in the step two into the stirring kettle, opening the stirring kettle to stir for 8 minutes, pouring the solution obtained in the step three into the stirring kettle, opening the stirring kettle to stir for 25 minutes, pouring into a sealable container, sealing, standing for 7 hours at room temperature, and taking out to obtain the low-smoke modified halogen-free flame retardant.
Example 2:
a low-smoke modified halogen-free flame retardant comprises the following components: magnesium hydroxide particles, dolomite powder, clay, deionized water, sepiolite powder, a coupling agent, dicumyl peroxide and benzoyl peroxide;
specifically, the composition comprises the following components in parts by weight: 60 parts of magnesium hydroxide particles, 12 parts of dolomite powder, 6 parts of clay, 90 parts of deionized water, 6 parts of sepiolite powder, 2 parts of coupling agent, 2 parts of dicumyl peroxide and 2 parts of benzoyl peroxide;
furthermore, in the above components, the coupling agent is a mixture of titanate coupling agent and silane coupling agent, and the mesh number of the dolomite powder, the sepiolite powder and the magnesium hydroxide particles is 200 meshes;
on the basis, the preparation method of the low-smoke modified halogen-free flame retardant specifically comprises the following steps:
step one, diluting a surface treating agent by using a proper amount of inert solvent, pouring the diluted surface treating agent into a stirring kettle, adding 60 parts of magnesium hydroxide particles into the stirring kettle, stirring and mixing the magnesium hydroxide particles at a low speed of 30 revolutions per minute for 20 minutes at room temperature, heating the mixture to 90 ℃, and stirring the mixture at a high speed of 120 revolutions per minute for 50 minutes to obtain modified magnesium hydroxide particles;
adding 6 parts of clay into a ball mill, mixing and crushing the clay by using the ball mill to obtain 0.5mm crushed clay, filtering the crushed clay by using a stainless steel screen with the diameter of a screen hole of 0.5mm to remove impurities, adding the filtered crushed clay, 12 parts of dolomite powder and 6 parts of sepiolite powder into a stirring kettle, starting the stirring kettle, stirring at the speed of 120/rpm for 20 minutes, sealing, and standing for 2 hours to obtain a raw material mixture;
pouring 90 parts of deionized water, 2 parts of coupling agent, 2 parts of dicumyl peroxide and 2 parts of benzoyl peroxide into a heating container with a heating function in sequence, stirring the mixture for 5 minutes by using a stirrer, raising the temperature in the heating container to 40 ℃, standing the mixture for 30 minutes, pouring the solution into the container, placing the container into a refrigerating chamber with the temperature of 0 ℃ for refrigerating for 8 hours, taking the container out, and removing scum and impurities on the surface of the solution;
step four, adding the modified magnesium hydroxide particles prepared in the step one into a stirring kettle, then adding the raw material mixture obtained in the step two into the stirring kettle, opening the stirring kettle to stir for 5 minutes, pouring the solution obtained in the step three into the stirring kettle, opening the stirring kettle to stir for 20 minutes, pouring into a sealable container, sealing, standing for 5 hours at room temperature, and taking out to obtain the low-smoke modified halogen-free flame retardant.
Example 3:
a low-smoke modified halogen-free flame retardant comprises the following components: magnesium hydroxide particles, dolomite powder, clay, deionized water, sepiolite powder, a coupling agent, dicumyl peroxide and benzoyl peroxide;
specifically, the composition comprises the following components in parts by weight: 70 parts of magnesium hydroxide particles, 18 parts of dolomite powder, 8 parts of clay, 110 parts of deionized water, 8 parts of sepiolite powder, 4 parts of coupling agent, 4 parts of dicumyl peroxide and 4 parts of benzoyl peroxide;
furthermore, in the above components, the coupling agent is a mixture of titanate coupling agent and silane coupling agent, and the mesh number of the dolomite powder, the sepiolite powder and the magnesium hydroxide particles is 300 meshes;
on the basis, the preparation method of the low-smoke modified halogen-free flame retardant specifically comprises the following steps:
step one, diluting a surface treating agent by using a proper amount of inert solvent, pouring the diluted surface treating agent into a stirring kettle, adding 70 parts of magnesium hydroxide particles into the stirring kettle, stirring and mixing the magnesium hydroxide particles at a low speed of 40 revolutions per minute for 30 minutes at room temperature, heating the mixture to 90 ℃, and stirring the mixture at a high speed of 150 revolutions per minute for 60 minutes to obtain modified magnesium hydroxide particles;
adding 8 parts of clay into a ball mill, mixing and crushing the clay by using the ball mill to obtain 1mm crushed clay, filtering the crushed clay by using a stainless steel screen with the diameter of a screen hole of 1mm to remove impurities in the crushed clay, adding 18 parts of filtered crushed clay, 18 parts of dolomite powder and 8 parts of sepiolite powder into a stirring kettle, starting the stirring kettle, stirring for 30 minutes at the speed of 120/rpm, sealing, and standing for 3 hours to obtain a raw material mixture;
step three, sequentially pouring 110 parts of deionized water, 4 parts of coupling agent, 4 parts of dicumyl peroxide and 4 parts of benzoyl peroxide into a heating container with a heating function, stirring the mixture for 10 minutes by using a stirrer, heating the temperature in the heating container to 50 ℃, standing the mixture for 30 minutes, pouring the solution into the container, placing the container into a refrigerating chamber with the temperature of 0 ℃ for refrigerating for 10 hours, taking the container out, and removing scum and impurities on the surface of the solution;
step four, adding the modified magnesium hydroxide particles prepared in the step one into a stirring kettle, then adding the raw material mixture obtained in the step two into the stirring kettle, opening the stirring kettle to stir for 10 minutes, pouring the solution obtained in the step three into the stirring kettle, opening the stirring kettle to stir for 30 minutes, pouring into a sealable container, sealing, standing for 8 hours at room temperature, and taking out to obtain the low-smoke modified halogen-free flame retardant.
Example 4
Unlike the examples 1 to 3, in this example, the coupling agent is specifically a titanate-based coupling agent;
on the basis, the preparation method of the low-smoke modified halogen-free flame retardant specifically comprises the following steps:
step one, diluting a surface treating agent by using a proper amount of inert solvent, pouring the diluted surface treating agent into a stirring kettle, adding 70 parts of magnesium hydroxide particles into the stirring kettle, stirring and mixing the magnesium hydroxide particles at a low speed of 40 revolutions per minute for 30 minutes at room temperature, heating the mixture to 90 ℃, and stirring the mixture at a high speed of 150 revolutions per minute for 60 minutes to obtain modified magnesium hydroxide particles;
adding 8 parts of clay into a ball mill, mixing and crushing the clay by using the ball mill to obtain 1mm crushed clay, filtering the crushed clay by using a stainless steel screen with the diameter of a screen hole of 1mm to remove impurities in the crushed clay, adding 18 parts of filtered crushed clay, 18 parts of dolomite powder and 8 parts of sepiolite powder into a stirring kettle, starting the stirring kettle, stirring for 30 minutes at the speed of 120/rpm, sealing, and standing for 3 hours to obtain a raw material mixture;
step three, sequentially pouring 110 parts of deionized water, 4 parts of coupling agent, 4 parts of dicumyl peroxide and 4 parts of benzoyl peroxide into a heating container with a heating function, stirring the mixture for 10 minutes by using a stirrer, heating the temperature in the heating container to 50 ℃, standing the mixture for 30 minutes, pouring the solution into the container, placing the container into a refrigerating chamber with the temperature of 0 ℃ for refrigerating for 10 hours, taking the container out, and removing scum and impurities on the surface of the solution;
step four, adding the modified magnesium hydroxide particles prepared in the step one into a stirring kettle, then adding the raw material mixture obtained in the step two into the stirring kettle, opening the stirring kettle to stir for 10 minutes, pouring the solution obtained in the step three into the stirring kettle, opening the stirring kettle to stir for 30 minutes, pouring into a sealable container, sealing, standing for 8 hours at room temperature, and taking out to obtain the low-smoke modified halogen-free flame retardant.
Example 5
Unlike examples 1 to 4, in this example, the coupling agent is specifically a silane coupling agent;
on the basis, the preparation method of the low-smoke modified halogen-free flame retardant specifically comprises the following steps:
step one, diluting a surface treating agent by using a proper amount of inert solvent, pouring the diluted surface treating agent into a stirring kettle, adding 70 parts of magnesium hydroxide particles into the stirring kettle, stirring and mixing the magnesium hydroxide particles at a low speed of 40 revolutions per minute for 30 minutes at room temperature, heating the mixture to 90 ℃, and stirring the mixture at a high speed of 150 revolutions per minute for 60 minutes to obtain modified magnesium hydroxide particles;
adding 8 parts of clay into a ball mill, mixing and crushing the clay by using the ball mill to obtain 1mm crushed clay, filtering the crushed clay by using a stainless steel screen with the diameter of a screen hole of 1mm to remove impurities in the crushed clay, adding 18 parts of filtered crushed clay, 18 parts of dolomite powder and 8 parts of sepiolite powder into a stirring kettle, starting the stirring kettle, stirring for 30 minutes at the speed of 120/rpm, sealing, and standing for 3 hours to obtain a raw material mixture;
step three, sequentially pouring 110 parts of deionized water, 4 parts of coupling agent, 4 parts of dicumyl peroxide and 4 parts of benzoyl peroxide into a heating container with a heating function, stirring the mixture for 10 minutes by using a stirrer, heating the temperature in the heating container to 50 ℃, standing the mixture for 30 minutes, pouring the solution into the container, placing the container into a refrigerating chamber with the temperature of 0 ℃ for refrigerating for 10 hours, taking the container out, and removing scum and impurities on the surface of the solution;
step four, adding the modified magnesium hydroxide particles prepared in the step one into a stirring kettle, then adding the raw material mixture obtained in the step two into the stirring kettle, opening the stirring kettle to stir for 10 minutes, pouring the solution obtained in the step three into the stirring kettle, opening the stirring kettle to stir for 30 minutes, pouring into a sealable container, sealing, standing for 8 hours at room temperature, and taking out to obtain the low-smoke modified halogen-free flame retardant.
Example 6
Unlike examples 1 to 3, in this example, the mesh number of the dolomite powder, the sepiolite powder and the magnesium hydroxide particles was 100 mesh;
on the basis, the preparation method of the low-smoke modified halogen-free flame retardant specifically comprises the following steps:
step one, diluting a surface treating agent by using a proper amount of inert solvent, pouring the diluted surface treating agent into a stirring kettle, adding 70 parts of magnesium hydroxide particles into the stirring kettle, stirring and mixing the magnesium hydroxide particles at a low speed of 40 revolutions per minute for 30 minutes at room temperature, heating the mixture to 90 ℃, and stirring the mixture at a high speed of 150 revolutions per minute for 60 minutes to obtain modified magnesium hydroxide particles;
adding 8 parts of clay into a ball mill, mixing and crushing the clay by using the ball mill to obtain 1mm crushed clay, filtering the crushed clay by using a stainless steel screen with the diameter of a screen hole of 1mm to remove impurities in the crushed clay, adding 18 parts of filtered crushed clay, 18 parts of dolomite powder and 8 parts of sepiolite powder into a stirring kettle, starting the stirring kettle, stirring for 30 minutes at the speed of 120/rpm, sealing, and standing for 3 hours to obtain a raw material mixture;
step three, sequentially pouring 110 parts of deionized water, 4 parts of coupling agent, 4 parts of dicumyl peroxide and 4 parts of benzoyl peroxide into a heating container with a heating function, stirring the mixture for 10 minutes by using a stirrer, heating the temperature in the heating container to 50 ℃, standing the mixture for 30 minutes, pouring the solution into the container, placing the container into a refrigerating chamber with the temperature of 0 ℃ for refrigerating for 10 hours, taking the container out, and removing scum and impurities on the surface of the solution;
step four, adding the modified magnesium hydroxide particles prepared in the step one into a stirring kettle, then adding the raw material mixture obtained in the step two into the stirring kettle, opening the stirring kettle to stir for 10 minutes, pouring the solution obtained in the step three into the stirring kettle, opening the stirring kettle to stir for 30 minutes, pouring into a sealable container, sealing, standing for 8 hours at room temperature, and taking out to obtain the low-smoke modified halogen-free flame retardant.
Through the six groups of embodiments, six low-smoke modified halogen-free flame retardants can be obtained, the performance tests are respectively carried out on the low-smoke modified halogen-free flame retardants, and then the performance tests are carried out on the commercially available common halogen-free flame retardants, so that the performances of the low-smoke modified halogen-free flame retardants in the six groups of embodiments are improved differently, wherein the low-smoke modified halogen-free flame retardant in embodiment 1 has the best performance and the highest value, and in the testing process, the obtained parameters are as follows:
from the above data, it can be seen that the performance of each example of the present invention is significantly improved due to the commercially available products, the flue gas yield and the acid gas generation amount;
magnesium hydroxide particles with small particle diameters are adopted, the surfaces of the magnesium hydroxide particles are modified to improve the compatibility of the magnesium hydroxide particles with polymers, and then the magnesium hydroxide particles are mixed with other polymer sections in the raw materials, so that the magnesium hydroxide particles can be fully compatible with effective components in the raw materials, the flame retardant efficiency of the flame retardant is improved, and the magnesium hydroxide is adopted as the main raw material, so that the magnesium hydroxide is low in smoke, non-toxic, more environment-friendly and green in combustion process, and favorable for popularization;
by adding dolomite powder and sepiolite powder, ball-milling clay, mixing, fully stirring and mixing the clay and the raw materials, adding the coupling agent, dicumyl peroxide and benzoyl peroxide, the performance of the flame retardant can be improved, the combustion of combustible substances can be effectively retarded in the combustion process, and the polymer carbonization can be promoted.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (8)
1. A low-smoke modified halogen-free flame retardant is characterized by comprising the following components in parts by weight: 50-80 parts of magnesium hydroxide particles, 10-20 parts of dolomite powder, 5-10 parts of clay, 80-120 parts of deionized water, 5-10 parts of sepiolite powder, 1-5 parts of coupling agent, 1-5 parts of dicumyl peroxide and 1-5 parts of benzoyl peroxide.
2. The low-smoke modified halogen-free flame retardant according to claim 1, which is characterized by comprising the following components in parts by weight: 60-70 parts of magnesium hydroxide particles, 12-18 parts of dolomite powder, 6-8 parts of clay, 90-110 parts of deionized water, 6-8 parts of sepiolite powder, 2-4 parts of coupling agent, 2-4 parts of dicumyl peroxide and 2-4 parts of benzoyl peroxide.
3. The low-smoke modified halogen-free flame retardant according to claim 1, which is characterized by comprising the following components in parts by weight: 65 parts of magnesium hydroxide particles, 15 parts of dolomite powder, 7 parts of clay, 100 parts of deionized water, 7 parts of sepiolite powder, 3 parts of coupling agent, 3 parts of dicumyl peroxide and 3 parts of benzoyl peroxide.
4. The low-smoke modified halogen-free flame retardant according to claim 1, characterized in that: the coupling agent is one or a mixture of titanate coupling agent and silane coupling agent.
5. The low-smoke modified halogen-free flame retardant according to claim 1, characterized in that: the mesh number of the dolomite powder, the sepiolite powder and the magnesium hydroxide particles is 200-300 meshes.
6. A preparation method of the low-smoke modified halogen-free flame retardant according to any one of claims 1 to 5, which is characterized by comprising the following steps:
step one, diluting a surface treatment agent with a proper amount of inert solvent, pouring the diluted surface treatment agent into a stirring kettle, adding magnesium hydroxide particles into the stirring kettle, stirring and mixing at a low speed for 20-30 minutes at room temperature, heating to 90 ℃, and stirring at a high speed for 50-60 minutes to obtain modified magnesium hydroxide particles;
adding clay into a ball mill, mixing and crushing the clay by using the ball mill to obtain 0.5-1mm of clay crushed aggregates, filtering the clay crushed aggregates by using a screen to remove impurities in the clay crushed aggregates, adding the filtered clay crushed aggregates, dolomite powder and sepiolite powder into a stirring kettle, starting the stirring kettle, stirring for 20-30 minutes at a speed of 120/rpm, sealing, and standing for 2-3 hours to obtain a raw material mixture;
pouring deionized water, a coupling agent, dicumyl peroxide and benzoyl peroxide into a heating container with a heating function in sequence, stirring the mixture by using a stirrer for 5 to 10 minutes, heating the temperature in the heating container to 40 to 50 ℃, standing the mixture for 30 minutes, pouring the solution into the container, placing the container into a refrigerating chamber for refrigerating for 8 to 10 hours, taking the container out, and removing scum and impurities on the surface of the solution;
step four, adding the modified magnesium hydroxide particles prepared in the step one into a stirring kettle, then adding the raw material mixture obtained in the step two into the stirring kettle, starting the stirring kettle to stir for 5-10 minutes, pouring the solution obtained in the step three into the stirring kettle, starting the stirring kettle to stir for 20-30 minutes, pouring into a sealable container, sealing, placing in a room temperature environment, standing for 5-8 hours, and taking out to obtain the low-smoke modified halogen-free flame retardant.
7. The preparation method of the low-smoke modified halogen-free flame retardant according to claim 6, characterized in that: in the first step, the rotation speed of the low-speed stirring is 30-40 rpm, and the high-speed stirring is 120-150 rpm.
8. The preparation method of the low-smoke modified halogen-free flame retardant according to claim 6, characterized in that: the screen used in the second step is made of stainless steel materials, the diameter of the screen hole of the screen is 0.5-1mm, and the temperature of the refrigerating chamber in the third step is set to be 0 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11220608B2 (en) * | 2017-10-04 | 2022-01-11 | Nouryon Chemicals International B.V. | Powder mixture comprising organic peroxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20120077748A (en) * | 2010-12-31 | 2012-07-10 | 한국세라믹기술원 | Method for manufacturing organic and norganic complex blowing form using methyl methacrylate resin and an organic and norganic complex blowing form |
| CN104292532A (en) * | 2014-09-29 | 2015-01-21 | 无为县茂林电缆材料有限公司 | Shock-resistant high-elasticity flame-retardant rubber material |
| CN109503930A (en) * | 2017-09-14 | 2019-03-22 | 上海电缆厂（南京）有限公司 | A kind of flame-proof cable material |
| CN109912848A (en) * | 2019-03-18 | 2019-06-21 | 重庆华塑科技有限公司 | A kind of mixed type fire retardant and preparation method thereof for modified plastics |
-
2019
- 2019-10-28 CN CN201911028947.2A patent/CN110615919A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20120077748A (en) * | 2010-12-31 | 2012-07-10 | 한국세라믹기술원 | Method for manufacturing organic and norganic complex blowing form using methyl methacrylate resin and an organic and norganic complex blowing form |
| CN104292532A (en) * | 2014-09-29 | 2015-01-21 | 无为县茂林电缆材料有限公司 | Shock-resistant high-elasticity flame-retardant rubber material |
| CN109503930A (en) * | 2017-09-14 | 2019-03-22 | 上海电缆厂（南京）有限公司 | A kind of flame-proof cable material |
| CN109912848A (en) * | 2019-03-18 | 2019-06-21 | 重庆华塑科技有限公司 | A kind of mixed type fire retardant and preparation method thereof for modified plastics |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11220608B2 (en) * | 2017-10-04 | 2022-01-11 | Nouryon Chemicals International B.V. | Powder mixture comprising organic peroxide |
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Application publication date: 20191227 |