阅读说明：本技术 一种低烟改性无卤阻燃剂及其制备方法 (Low-smoke modified halogen-free flame retardant and preparation method thereof ) 是由 邓娇容 甘祖荣 常红丽 于 2019-10-28 设计创作，主要内容包括：本发明公开了一种低烟改性无卤阻燃剂及其制备方法,具体涉及无卤阻燃剂技术领域,包括以下重量份成分：氢氧化镁颗粒50-80份、白云石粉末10-20份、粘土5-10份、去离子水80-120份、海泡石粉末5-10份、偶联剂1-5份、过氧化二异丙苯1-5份和过氧化苯甲酰1-5份。本发明通过采用颗粒直径小的氢氧化镁颗粒,并对其表面进行改性,以提高其与聚合物的相容性,然后与原料中的其他聚合物进行混合,使其能够与原料中的有效成分充分相容,有利于提高阻燃剂的阻燃效率,且由于采用氢氧化镁作为主要原料,在燃烧的过程中,低烟、无毒,更加环保绿色,有利于进行推广。(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.)

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 ℃.

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.