CN114410128A - Magnesium hydroxide ultra-fining and surface modification method and application thereof - Google Patents
Magnesium hydroxide ultra-fining and surface modification method and application thereof Download PDFInfo
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/028—Compounds containing only magnesium as metal
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon 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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Abstract
The invention discloses a method for magnesium hydroxide ultra-fining and surface modification and application thereof, relating to the technical field of magnesium hydroxide fire retardants. The method comprises the following steps: selecting brucite powder, a surface modifier and a solvent, continuously adding the brucite powder, the surface modifier and the solvent into a ball mill, carrying out an integrated treatment process of superfine grinding and mechanochemical modification, continuously conveying modified fine powder subjected to the integrated treatment of superfine grinding and mechanochemical modification into a primary airflow classifier and a secondary airflow classifier, and preparing magnesium hydroxide modified fine powder by continuously classifying for two times; collecting, drying and packaging the treated magnesium hydroxide powder. The invention has simple process, convenient operation, improved compatibility and dispersibility with high molecular materials, optimized flame retardant property, processability and mechanical property of high molecular polymers, high efficiency, high yield, low energy consumption, environmental protection, no pollution and wide application prospect.
Description
Technical Field
The invention relates to the technical field of magnesium hydroxide flame retardants, in particular to a method for superfine and surface modification of magnesium hydroxide and application thereof.
Background
In the 21 st century, the trend of flame retardants is toward environmental protection, low toxicity, low smoke, high efficiency, and multi-functionalization, europe has started to limit the sale of halogen-containing flame retardants, japan has prohibited the use of flame retardants that generate acidic gases during cable combustion, and the united states has established regulations for the use of low-halogen cable coatings. With the rapid development of Chinese economic construction, modern equipment such as many high-rise buildings, subways, tunnels, nuclear power stations, ships and the like are required to adopt low-smoke halogen-free flame-retardant wires and cables, and the requirements on the safety performance and the environmental protection performance of the flame retardant are higher and higher.
The flame retardant property of the magnesium hydroxide completely meets the requirement of the flame retardant on the development of environmental protection, and belongs to an inorganic non-halogen flame retardant which is harmless to human health and environmental protection.
At present, the magnesium hydroxide product ground by a ball mill in a dry method has the characteristics of large specific surface area, high surface activity, high chemical reaction speed and the like due to fine particle size, narrow distribution and uniform quality. However, due to the small size effect, the interface effect and the surface effect of the ultrafine powder, the ultrafine powder is easy to agglomerate, the surface of the magnesium hydroxide flame retardant is hydrophilic and oleophobic, the magnesium hydroxide powder without surface treatment is filled in a polymer material and is difficult to uniformly disperse in an organic polymer, and the mechanical property, the processing property and the like of the polymer material are seriously deteriorated, so that the surface modification treatment must be carried out on the magnesium hydroxide to improve the compatibility with the polymer and reduce the influence of the magnesium hydroxide on the processing property and the mechanical property of a polymer product.
The dry mechanochemical modification is that the surface activity of particles is enhanced by crushing, grinding, rubbing and other methods, so that the surface of powder with strong activity reacts and is attached to a surface modifier, thereby achieving the purpose of surface modification. The mechanochemical surface modification combines the superfine grinding and the surface modification, and compared with the ball-milling wet modification, the ball-milling dry modification has wide development prospect. In order to solve the technical problems of particle size and particle size distribution control, secondary agglomeration in the process of superfine modification and the like of the magnesium hydroxide flame retardant, it is particularly necessary to develop a method for superfine modification and surface modification of magnesium hydroxide and an application thereof.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a magnesium hydroxide superfine and surface modification method and application thereof, the process is simple, the operation is convenient, the compatibility and the dispersibility with high polymer materials are improved, the flame retardant property, the processing property and the mechanical property of high polymer are optimized, the efficiency is high, the yield is high, the energy consumption is low, the environment is protected, no pollution is caused, and the popularization and the use are easy.
In order to achieve the purpose, the invention is realized by the following technical scheme: a method for superfine grinding and surface modification of magnesium hydroxide, which prepares a magnesium hydroxide flame retardant by a ball-milling grinding superfine and mechanochemical reaction dry modification integrated process, comprises the following steps:
(1) selecting brucite powder with the particle size of 0-5mm, a surface modifier and a solvent, continuously adding the brucite powder, the surface modifier and the solvent into a ball mill, and carrying out integrated processing processes of superfine grinding and mechanochemical modification under the conditions that the ball milling rotation speed is 20rpm and the temperature is 60-120 ℃, wherein a grinding medium in the ball mill is grinding balls;
(2) continuously conveying the modified fine powder subjected to the integrated treatment of ultrafine grinding and mechanochemical modification in the step (1) to a primary airflow classifier and a secondary airflow classifier, and preparing 2500-8000-mesh magnesium hydroxide modified fine powder by continuous twice classification;
(3) collecting, drying and packaging the treated magnesium hydroxide powder.
Preferably, in the step (1), the surface modifier is one or more of stearic acid, organic carboxylate, silane coupling agent RSiX3, titanate coupling agent and phosphate coupling agent, and the dosage of the surface modifier is 0.5-5% of the brucite powder by mass.
Preferably, the silane coupling agent is RSiX3, wherein R is amino, mercapto, vinyl, epoxy, cyano or methacryloxy, and X is halogen, alkoxy or acyloxy.
Preferably, the solvent in the step (1) is one or a plurality of anhydrous ethanol, acetone and toluene organic auxiliary agents, and the dosage of the solvent is 0.5-2 times of the mass of the surface modifier.
Preferably, the magnesium hydroxide modified fine powder subjected to the integrated treatment of superfine grinding and mechanochemical modification in the step (2) is subjected to primary grading in a primary airflow classifier, wherein the primary grading particle size is 2500-8000 meshes; in the secondary airflow classifier, the secondary classification particle size is 100-400 meshes.
The application of the method for superfine modification and surface modification of magnesium hydroxide is characterized in that prepared magnesium hydroxide modified fine powder is used as a halogen-free flame retardant and applied to a low-smoke halogen-free cable material, and the low-smoke halogen-free cable material comprises the following raw materials in parts by weight: 165 parts of halogen-free flame retardant, 88 parts of base resin, 12 parts of compatilizer, 2 parts of coupling agent, 3 parts of lubricant and 1 part of antioxidant.
Preferably, the compatilizer is maleic anhydride grafted polyethylene, the lubricant is one or more of polyethylene wax, silicone powder and methyl silicone oil, and the antioxidant is pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] and distearyl thiodipropionate according to the mass ratio of 3: 4 in the presence of a catalyst.
The invention has the beneficial effects that: the method has the advantages of simple process and convenient operation, modifies the magnesium hydroxide flame retardant powder from a hydrophilic surface to a lipophilic surface, improves the intermiscibility and the dispersibility of the powder in a high-molecular polymer material, optimizes the comprehensive performances of the high-molecular polymer, such as flame retardant property, processability, mechanical property and the like, has high efficiency, high yield, low energy consumption, environmental protection, no pollution, wide application in industrial production process and wide application prospect.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
The specific implementation mode adopts the following technical scheme: a method for superfine grinding and surface modification of magnesium hydroxide, which prepares a magnesium hydroxide flame retardant by a ball-milling grinding superfine and mechanochemical reaction dry modification integrated process, comprises the following steps:
(1) selecting brucite powder with the particle size of 0-5mm, a surface modifier and a solvent, continuously adding the brucite powder, the surface modifier and the solvent into a ball mill, and carrying out integrated processing processes of superfine grinding and mechanochemical modification under the conditions that the ball milling rotation speed is 20rpm and the temperature is 60-120 ℃, wherein a grinding medium in the ball mill is grinding balls;
(2) continuously conveying the modified fine powder subjected to the integrated treatment of ultrafine grinding and mechanochemical modification in the step (1) to a primary airflow classifier and a secondary airflow classifier, and preparing 2500-8000-mesh magnesium hydroxide modified fine powder by continuous twice classification;
(3) collecting, drying and packaging the treated magnesium hydroxide powder.
It is worth noting that in the step (1), the surface modifier is compounded by one or more of stearic acid, organic carboxylate, silane coupling agent RSiX3, titanate coupling agent and phosphate coupling agent, and the dosage of the surface modifier is 0.5% -5% of the brucite powder by mass. The solvent is one or a plurality of anhydrous alcohol, acetone and toluene organic auxiliary agents, and the dosage of the solvent is 0.5 to 2 times of the mass of the surface modifier.
Wherein, the silane coupling agent is RSiX3, R is amino, sulfydryl, vinyl, epoxy group, cyano or methacryloxy, and X is halogen, alkoxy or acyloxy.
In addition, the magnesium hydroxide modified fine powder subjected to the integrated treatment of superfine grinding and mechanochemical modification in the step (2) is subjected to primary grading with a particle size of 2500-8000 meshes in a primary airflow classifier; in the secondary airflow classifier, the secondary classification particle size is 100-400 meshes.
The application of the method for superfine modification and surface modification of magnesium hydroxide is characterized in that prepared magnesium hydroxide modified fine powder is used as a halogen-free flame retardant and applied to a low-smoke halogen-free cable material, and the low-smoke halogen-free cable material comprises the following raw materials in parts by weight: 165 parts of halogen-free flame retardant, 88 parts of base resin, 12 parts of compatilizer, 2 parts of coupling agent, 3 parts of lubricant and 1 part of antioxidant.
It is noted that the compatilizer is maleic anhydride grafted polyethylene, the lubricant is one or more of polyethylene wax, silicone powder and methyl silicone oil, and the antioxidant is pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] and distearyl thiodipropionate according to the mass ratio of 3: 4 in the presence of a catalyst.
The magnesium hydroxide flame retardant powder is modified from a hydrophilic surface to a lipophilic surface in the specific embodiment, and the process for preparing the magnesium hydroxide flame retardant by integrating the superfine powder and the surface modification is simple, convenient to operate, high in efficiency, large in yield, low in energy consumption, environment-friendly and pollution-free, and has the technical advantages that:
the magnesium hydroxide is subjected to ball-milling superfine grinding and mechanochemical modification integrated treatment, and compared with magnesium hydroxide obtained after dry grinding treatment by common grinding equipment, the magnesium hydroxide is finer in granularity, narrower in distribution, more uniform in quality, larger in specific surface area and higher in surface activity.
Secondly, the prepared modified superfine magnesium hydroxide improves the compatibility and the dispersibility with high polymer materials, and obviously improves the mechanical property, the processing fluidity, the flame retardant property and the like of the high polymer composite material.
Example 1: a method for magnesium hydroxide ultra-fining and surface modification comprises the following steps: selecting brucite powder with the particle size of 0-5mm, 1.0% of stearic acid surface modifier and absolute ethyl alcohol, continuously adding the brucite powder, the stearic acid surface modifier and the absolute ethyl alcohol into a ball mill, and carrying out integrated treatment of superfine grinding and mechanochemical modification at the temperature of 60-120 ℃ to prepare 2500-8000-mesh magnesium hydroxide modified fine powder; collecting, drying and packaging the treated magnesium hydroxide powder.
Example 2: a method for magnesium hydroxide ultra-fining and surface modification comprises the following steps: selecting brucite powder with the particle size of 0-5mm, 0.5 percent of stearic acid, 0.5 percent of titanate surface modifier and acetone, continuously adding the brucite powder, the stearic acid, the titanate surface modifier and the acetone into a ball mill, and carrying out integrated treatment of superfine grinding and mechanochemical modification at the temperature of 60-120 ℃ to prepare 2500-8000-mesh magnesium hydroxide modified fine powder; collecting, drying and packaging the treated magnesium hydroxide powder.
Example 3: a method for magnesium hydroxide ultra-fining and surface modification comprises the following steps: brucite powder with the particle size of 0-5mm, 1.5 percent of vinyl tri (beta-methoxyethoxy) silane surface modifier and toluene are selected to be continuously added into a ball mill, and the superfine grinding and the mechanochemical modification are carried out to be integrated under the condition of 60-120 ℃ to prepare 2500-sand 8000-mesh magnesium hydroxide modified fine powder; collecting, drying and packaging the treated magnesium hydroxide powder.
Example 4: the application of the magnesium hydroxide superfine and surface modification method is characterized in that the magnesium hydroxide modified fine powder prepared in the embodiment 1, the embodiment 2 or the embodiment 3 is used as a halogen-free flame retardant to be applied to the preparation of a low-smoke halogen-free cable material, and the low-smoke halogen-free cable material comprises the following raw materials in parts by weight: 165 parts of halogen-free flame retardant, 88 parts of base resin, 12 parts of compatilizer, 2 parts of coupling agent, 3 parts of lubricant and 1 part of antioxidant, and the cable material corresponding to the embodiment 1, the embodiment 2 or the embodiment 3 is prepared respectively.
By carrying out ultrafine grinding and mechanochemical modification integrated treatment on the magnesium hydroxide, the cable material prepared by the cable materials of the embodiments 1, 2 and 3 has more excellent performance, finer surface particle size distribution, more smoothness and fineness, more excellent elongation and melt index performance and higher popularization and use value compared with the cable material prepared by obtaining the magnesium hydroxide flame retardant after common grinding treatment.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A method for superfine grinding and surface modification of magnesium hydroxide is characterized in that a magnesium hydroxide flame retardant is prepared by a ball-milling grinding superfine and mechanochemical reaction dry modification integrated process, and comprises the following steps:
(1) selecting brucite powder with the particle size of 0-5mm, a surface modifier and a solvent, continuously adding the brucite powder, the surface modifier and the solvent into a ball mill, and carrying out integrated processing processes of superfine grinding and mechanochemical modification under the conditions that the ball milling rotation speed is 20rpm and the temperature is 60-120 ℃, wherein a grinding medium in the ball mill is grinding balls;
(2) continuously conveying the modified fine powder subjected to the integrated treatment of ultrafine grinding and mechanochemical modification in the step (1) to a primary airflow classifier and a secondary airflow classifier, and preparing 2500-8000-mesh magnesium hydroxide modified fine powder by continuous twice classification;
(3) collecting, drying and packaging the treated magnesium hydroxide powder.
2. The method for ultrafining and surface-modifying magnesium hydroxide according to claim 1, wherein the surface modifier in step (1) is one or more selected from stearic acid, organic carboxylate, silane coupling agent RSiX3, titanate coupling agent and phosphate coupling agent.
3. The method of claim 2, wherein said silane coupling agent is RSiX3, wherein R is amino, mercapto, vinyl, epoxy, cyano or methacryloxy, and X is halogen, alkoxy or acyloxy.
4. The method for magnesium hydroxide superfining and surface modification according to claim 1, wherein the solvent in step (1) is one or more of absolute ethyl alcohol, acetone and toluene organic auxiliary agents.
5. The method for ultrafining and surface-modifying magnesium hydroxide according to claim 1, wherein the amount of the surface modifier used in the step (1) is 0.5-5% by mass of brucite powder.
6. The method for ultrafining and surface-modifying magnesium hydroxide as claimed in claim 1, wherein the solvent used in step (1) is used in an amount of 0.5-2 times the mass of the surface modifier.
7. The method for magnesium hydroxide ultrafining and surface modification as claimed in claim 1, wherein the magnesium hydroxide modified fine powder subjected to the integrated treatment of ultrafine grinding and mechanochemical modification in step (2) is subjected to primary classification with a particle size of 2500-8000 meshes in a primary air classifier; in the secondary airflow classifier, the secondary classification particle size is 100-400 meshes.
8. The application of the magnesium hydroxide superfine and surface modification method is characterized in that the prepared magnesium hydroxide modified fine powder is used as a halogen-free flame retardant and applied to a low-smoke halogen-free cable material, and the low-smoke halogen-free cable material comprises the following raw materials in parts by weight: 165 parts of halogen-free flame retardant, 88 parts of base resin, 12 parts of compatilizer, 2 parts of coupling agent, 3 parts of lubricant and 1 part of antioxidant.
9. The method for magnesium hydroxide superfining and surface modification according to claim 8, wherein the compatibilizer is maleic anhydride grafted polyethylene, the lubricant is one or more of polyethylene wax, silicone powder and methyl silicone oil, and the antioxidant is pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] and distearyl thiodipropionate in a mass ratio of 3: 4 in the presence of a catalyst.
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| CN116216751A (en) * | 2023-04-11 | 2023-06-06 | 湖南恒光化工有限公司 | Preparation process of magnesium hydroxide |
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| CN115780035A (en) * | 2022-11-25 | 2023-03-14 | 大连亚泰科技新材料股份有限公司 | Horizontal wet ball mill with heating system and pressure control system and method for producing hexagonal flaky magnesium hydroxide by using same |
| CN115780035B (en) * | 2022-11-25 | 2023-09-29 | 大连亚泰科技新材料股份有限公司 | Horizontal wet ball mill with heating system and pressure control system and method for producing hexagonal flaky magnesium hydroxide by using horizontal wet ball mill |
| CN116216751A (en) * | 2023-04-11 | 2023-06-06 | 湖南恒光化工有限公司 | Preparation process of magnesium hydroxide |
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