CN115780035A - Horizontal wet ball mill with heating system and pressure control system and method for producing hexagonal flaky magnesium hydroxide by using same - Google Patents
Horizontal wet ball mill with heating system and pressure control system and method for producing hexagonal flaky magnesium hydroxide by using same Download PDFInfo
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- CN115780035A CN115780035A CN202211487927.3A CN202211487927A CN115780035A CN 115780035 A CN115780035 A CN 115780035A CN 202211487927 A CN202211487927 A CN 202211487927A CN 115780035 A CN115780035 A CN 115780035A
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Abstract
The invention belongs to the technical field of magnesium hydroxide fire retardants, and discloses a horizontal wet ball mill with a heating system and a pressure control system and a method for producing hexagonal flaky magnesium hydroxide by the same, wherein the heating system and the pressure control system are added to the traditional horizontal wet ball mill, so that a ball mill host can simultaneously complete the processing processes of fine grinding, grinding aid, surface modification and production of the hexagonal flaky magnesium hydroxide fire retardant, and the method comprises the following steps: brucite powder with the grain size of 2500 meshes, a grinding aid and a surface modifier are selected and continuously added into a ball milling host machine, fine milling, grinding aid, surface modification and crystal form control treatment are carried out at the temperature of 80-200 ℃, and then, the hexagonal flaky magnesium hydroxide flame retardant product with the grain size of 8000-10000 meshes is produced through filtering, drying and packaging.
Description
Technical Field
The invention relates to the technical field of magnesium hydroxide flame retardants, in particular to a horizontal wet ball mill with a heating system and a pressure control system and a method for producing hexagonal flaky magnesium hydroxide by using the same.
Background
In the 21 st century, the flame retardant is developing towards the trend of environmental protection, low toxicity, low smoke, high efficiency and low cost, the flame retardant property of magnesium hydroxide completely meets the requirement of the flame retardant for environmental protection, the magnesium hydroxide has the environment-friendly flame retardant with various properties of flame retardance, inorganic property, non-halogen property, smoke abatement, drip resistance, filling and the like, and is widely applied in the aspects of flame retardance, environmental protection, medicine, ceramics and the like, meanwhile, the requirement of people on flame retardant materials is continuously improved, and higher requirements are provided for the product granularity, the granularity distribution, the dispersibility and the surface modification, especially for the low-cost and high-efficiency production of hexagonal flaky high-flame retardant magnesium hydroxide flame retardants.
The magnesium hydroxide product ground and crushed by the wet ball mill has the advantages of fine granularity, narrow distribution, large specific surface area, high surface activity and high chemical reaction speed, magnesium hydroxide particles are easy to agglomerate into crystals in a random form under the action of the small-size effect, the interface effect and the surface effect of ultrafine powder, and the surface of a magnesium hydroxide flame retardant is hydrophilic and oleophobic. At present, the hexagonal flaky magnesium hydroxide flame retardant is mainly produced and prepared by synthesizing at normal temperature by a chemical alkali method and performing thermal recrystallization treatment at high temperature and high pressure water, and the process method has the defects of long flow, complex process, large product particles, easiness in agglomeration, high alkali consumption, high energy consumption, large waste liquid discharge amount, high production cost and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention controls the crystal form of magnesium hydroxide in the wet ball milling production process to directly produce the hexagonal flaky special crystal form and simultaneously complete the surface modification treatment process.
The invention aims to provide a horizontal wet ball mill with a heating system and a pressure control system and a method for producing hexagonal flaky magnesium hydroxide by using the same, which have the advantages of simple process flow, convenient production operation, no alkali consumption, low energy consumption, no waste liquid discharge, low production cost, fine product granularity, narrow distribution and the like, particularly can simultaneously realize the production process of crystal form control and surface modification in the production process of wet ball milling superfine grinding, and are easy to popularize and use in the industry.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the horizontal wet ball mill is provided with a heating system and a pressure control system, wherein the outer wall of the ball mill is provided with a heat conduction jacket, a hot oil pipe and a cooling water pipe are alternately arranged in the heat conduction jacket, the outer wall of the ball mill is provided with a safety valve, a feeding hole is provided with a temperature sensor A and a pressure sensor A, and a discharging hole is provided with a temperature sensor B and a pressure sensor B.
A method for producing hexagonal flaky magnesium hydroxide by a horizontal wet ball mill with a heating system and a pressure control system comprises the steps of respectively feeding raw materials, grinding aid and surface modifier into a premixing reaction tank, mixing and stirring by using a stirring paddle, heating a ball mill host machine by using heat conduction oil in a hot oil pipe, simultaneously carrying out fine grinding, grinding aid, surface modification and crystal form control production and processing in the ball mill host machine, increasing the introduction amount of cooling water in a cooling water pipe when the temperatures monitored by a temperature sensor A and a temperature sensor B are overhigh, reducing the introduction amount of the cooling water when the temperatures are overlow, and monitoring the pressure by a safety valve to ensure safety.
The method comprises the following steps:
s1, taking brucite powder, grinding aid, surface modifier and water, mixing the components in a proportion of 100: (0.1-0.5): (0.5-5.0): (100-1000) by mass, continuously adding into a premixing reaction tank;
s2, dispersing uniformly by a stirring paddle, continuously adding into a main machine of a ball mill, reacting for 0.5-6 hours at the temperature of 80-200 ℃ and the ball milling rotation speed of 100-1500rpm, and simultaneously finishing the processes of fine grinding, grinding aid, surface modification and crystal form control treatment;
s3, filtering, drying and packaging to produce a 8000-10000-mesh hexagonal flaky magnesium hydroxide flame retardant product.
Further, in the step S1, a solvent may also be added into the premixing reaction tank, and the amount of the solvent is 0.5 to 3.0 times of the mass of the surface modifier.
Preferably, the mass ratio of the brucite powder, the grinding aid, the surface modifier and the water in the step S1 is 100: (0.3-0.5): (0.5-2.5): (500-1000).
Preferably, in the step S1, the main machine of the ball mill reacts for 3 to 6 hours at the temperature of between 80 and 160 ℃ and at the ball milling rotating speed of between 1000 and 1500rpm, and meanwhile, the processes of fine grinding, grinding aid, surface modification and crystal form control treatment are completed.
Further, the grinding aid in step S1 may be silicone, triethanolamine, triisopropanolamine, ethylene glycol, diethanolisopropanolamine, vinyl glycol ether, polyacrylate, polycarboxylate, stearate, colloidal silica, or the like.
Further, the surface modifier in step S3 may be one or more of coupling agents, surfactants, silicones, unsaturated organic acids, water-soluble polymers, and the like.
Further, the coupling agent includes silanes, titanates, aluminates, and the like.
Further, the surfactant includes anionic, cationic and nonionic.
The solvent can be one or more of organic additives such as ethanol, isopropanol, acetone, toluene, xylene and the like.
Compared with the prior art, the invention has the following beneficial effects:
the invention has the advantages of simple process flow, convenient production operation, no alkali consumption, low energy consumption, no waste liquid discharge, low production cost, fine product granularity, narrow distribution and the like, and particularly can simultaneously realize the production process of crystal form control and surface modification in the production process of wet ball milling and ultrafine grinding.
Drawings
FIG. 1 is a schematic diagram of a horizontal wet ball mill with a heating system and a pressure control system according to the present invention;
FIG. 2 is an electron microscope image of a comparative reference example magnesium hydroxide product of the prior art;
FIG. 3 is an electron microscope image of a hexagonal magnesium hydroxide product according to example 1 of the present invention;
FIG. 4 is an electron microscope image of a hexagonal magnesium hydroxide product in example 2 of the present invention;
FIG. 5 is an electron microscope image of a hexagonal magnesium hydroxide product of example 3.
Wherein: 1. the method comprises the following steps of grinding, mixing and stirring, wherein the grinding aid comprises a ball mill outer wall, 2 a premixing reaction tank, 3 raw material feeding, 4 stirring paddles, 5 grinding aid feeding, 6 surface modifier feeding, 7 a discharging port, 8 a heat conduction jacket, 9 a hot oil pipe, 10 a cooling water pipe, 11 a safety valve, 12 a ball mill main machine, 13 a cooling water inlet, 14 a cooling water outlet, 15 a feeding port, 16 temperature sensors A and 17 pressure sensors A and 18, temperature sensors B and 19 and a pressure sensor B.
Detailed Description
In view of the disadvantages of the prior art, the present invention is directed to a horizontal wet ball mill with a heating system and a pressure control system and a method for producing hexagonal magnesium hydroxide flakes, which will be described in detail below with reference to the accompanying drawings and examples, wherein the examples of the present invention or the prior art are illustrated in the drawings. All other embodiments obtained without inventive step for a person skilled in the art are within the scope of protection of the present invention.
The technical solution of the present invention will be further explained with reference to the embodiments shown in the drawings.
Example 1
The invention provides a method for producing hexagonal flaky magnesium hydroxide by using a horizontal wet ball mill additionally provided with a heating system and a pressure control system, which simultaneously completes the production and processing processes of fine grinding, grinding aid, surface modification and crystal form control in a traditional horizontal ball mill host, and comprises the following steps:
(1) Brucite powder (magnesium hydroxide powder) with the grain diameter of 2500 meshes, triethanolamine, sodium stearate and water are selected, and the weight ratio of 100:0.3:2.5:1000, continuously adding the mixture into a premixing reaction tank 2;
(2) After being dispersed uniformly by the stirring paddle 4, the mixture is continuously added into the main body 12 of the ball mill, and reacts for 6 hours at the temperature of 140 ℃ and the ball milling rotating speed of 500rpm, and meanwhile, the processes of fine grinding, grinding aid, surface modification and crystal form control treatment are completed;
(3) Then filtering, drying and packaging to produce the 10000-mesh hexagonal flaky magnesium hydroxide flame retardant product.
Example 2
The invention provides a method for producing hexagonal flaky magnesium hydroxide by using a horizontal wet ball mill additionally provided with a heating system and a pressure control system, which simultaneously completes the production and processing processes of fine grinding, grinding aid, surface modification and crystal form control in a traditional horizontal ball mill host, and comprises the following steps:
(1) Selecting 2500-mesh brucite powder (magnesium hydroxide powder), diethanol amine, titanate (acetone solvent) and water, and mixing the components in a proportion of 100:0.3:3.0:900, continuously adding the mixture into the premixing reaction tank 2;
(2) After being dispersed uniformly by the stirring paddle 4, the mixture is continuously added into the main body 12 of the ball mill, and reacts for 5 hours at the temperature of 150 ℃ and the ball milling rotation speed of 700rpm, and meanwhile, the processes of fine grinding, grinding aid, surface modification and crystal form control treatment are completed;
(3) Then filtering, drying and packaging to produce a 9000-mesh hexagonal flaky magnesium hydroxide flame retardant product.
Example 3
The invention provides a method for producing hexagonal flaky magnesium hydroxide by using a horizontal wet ball mill additionally provided with a heating system and a pressure control system, which simultaneously completes the production and processing processes of fine grinding, grinding aid, surface modification and crystal form control in a traditional horizontal ball mill host, and comprises the following steps:
(1) Selecting 2500-mesh brucite powder (magnesium hydroxide powder), diethanol monoisopropanolamine, vinyl tri (beta-methoxyethoxy) silane coupling agent (ethanol solvent) and water, and mixing the components in a proportion of 100:0.3:3.0:800, continuously adding the mixture into a premixing reaction tank 2;
(2) After being dispersed uniformly by the stirring paddle 4, the mixture is continuously added into the main body 12 of the ball mill, reacts for 4 hours at the temperature of 160 ℃ and the ball milling rotating speed of 1000rpm, and simultaneously finishes the processes of fine grinding, grinding aid, surface modification and crystal form control treatment;
(3) Then filtering, drying and packaging to produce a 8000-mesh hexagonal flaky magnesium hydroxide flame retardant product.
Comparative example
A comparison group is arranged, and brucite powder of the comparison group is prepared by adopting the following method:
(1) Brucite powder (magnesium hydroxide powder) with the particle size of 2500 meshes and water are selected, and the weight ratio of 100:900 proportion, continuously adding into the premixing reaction tank 2;
(2) After being uniformly dispersed by the stirring paddle 4, the mixture is continuously added into the main body 12 of the ball mill, and because a heating system and a pressure control system are not arranged, the temperature which can be usually maintained by the heat generated in the brucite powder grinding process is 10-60 ℃, and the reaction lasts for 6 hours under the condition that the ball milling rotating speed is 700 rpm;
(3) Then filtering, drying and packaging to produce the magnesium hydroxide flame retardant product with 5000 meshes.
The magnesium hydroxide flame retardant products of examples 1-3 were tested against the data associated with the comparative meal and the results are shown in the following table:
in conclusion, the method for producing hexagonal sheet magnesium hydroxide by using the horizontal wet ball mill with the heating system and the pressure control system, disclosed by the invention, has the advantages of simple process flow, convenience in production operation, no alkali consumption, low energy consumption, no waste liquid discharge, low production cost, fine product granularity, narrow distribution and the like, can be used for simultaneously realizing the production process of fine grinding, grinding aid, surface modification and crystal form control in the ball mill host by adding the automatic temperature control heating system and the automatic pressure control system of heat conduction oil in the traditional horizontal wet ball mill, especially in the production process of wet ball milling and ultrafine grinding, has a wide application range, and can be widely applied to the production of various industrial related fields.
The foregoing is merely a preferred embodiment of the invention and is not intended to exhaustive or to limit the invention to the precise embodiment disclosed. It will be appreciated by those skilled in the art that changes, modifications and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is to be accorded the broadest interpretation so as to encompass all such modifications and alterations as fall within the scope of the appended claims.
Claims (10)
1. The horizontal wet ball mill with the heating system and the pressure control system is characterized in that a heat conduction jacket (8) is arranged on the outer wall (1) of the ball mill, a hot oil pipe (9) and a cooling water pipe (10) are alternately arranged in the heat conduction jacket (8), a safety valve (11) is arranged on the outer wall (1) of the ball mill, a temperature sensor A (16) and a pressure sensor A (17) are arranged at a feeding port (15), and a temperature sensor B (18) and a pressure sensor B (19) are arranged at a discharging port (7).
2. The method for producing the hexagonal flaky magnesium hydroxide by the horizontal wet ball mill with the heating system and the pressure control system is characterized in that raw material feeding (3), grinding aid feeding (5) and surface modifier feeding (6) are respectively fed into a premixing reaction tank (2), mixing and stirring are carried out by using a stirring paddle (4), a ball mill host (12) is heated by heat conduction oil in a hot oil pipe (9), fine grinding, grinding aid, surface modification and crystal form control production and processing are simultaneously carried out in the ball mill host (12), when the temperatures monitored by a temperature sensor A (16) and a temperature sensor B (18) are overhigh, the introduction amount of cooling water in a cooling water pipe (10) is increased, when the temperatures are overlow, the introduction amount of the cooling water is reduced, and a safety valve (11) is used for monitoring the pressure to ensure safety.
3. The method for producing hexagonal flaky magnesium hydroxide by using the horizontal wet ball mill with the heating system and the pressure control system as claimed in claim 2, wherein the method comprises the following steps:
s1, taking magnesium hydroxide powder, a grinding aid, a surface modifier and water, mixing the components in a ratio of 100: (0.1-0.5): (0.5-5.0): (100-1000) by mass, continuously adding into the premixing reaction tank (2);
s2, after being uniformly dispersed by the stirring paddle (4), the mixture is continuously added into a main machine (12) of the ball mill, and reacts for 0.5 to 12 hours at the temperature of between 80 and 200 ℃ and at the ball milling rotating speed of between 100 and 1500rpm, and meanwhile, the processes of fine grinding, grinding aid, surface modification and crystal form control treatment are completed;
s3, filtering, drying and packaging to produce a 8000-10000-mesh hexagonal flaky magnesium hydroxide flame retardant product.
4. The method for producing hexagonal flaky magnesium hydroxide by using the horizontal wet ball mill with the heating system and the pressure control system as claimed in claim 3, wherein the solvent is added into the premixing reaction tank (2) in the step S1, and the amount of the solvent is 0.5-3.0 times of the mass of the surface modifier.
5. The method for producing hexagonal flaky magnesium hydroxide by using the horizontal wet ball mill with the heating system and the pressure control system as claimed in claim 3, wherein the mass ratio of the brucite powder, the grinding aid, the surface modifier and the water in the step S1 is 100: (0.3-0.5): (0.5-2.5): (500-1000).
6. The method for producing hexagonal flaky magnesium hydroxide by using the horizontal wet ball mill with the heating system and the pressure control system according to claim 3, wherein in the step S1, the ball mill main body (12) reacts for 3 to 6 hours at 80 to 160 ℃ and at a ball milling rotation speed of 1000 to 1500rpm, and the processes of fine grinding, grinding aid, surface modification and crystal form control are completed simultaneously.
7. The method for producing hexagonal flaky magnesium hydroxide by using the horizontal wet ball mill with the heating system and the pressure control system as claimed in claim 3, wherein the grinding aid in the step S1 is any one of organosilicon, triethanolamine, triisopropanolamine, ethylene glycol, diethanol monoisopropanolamine, vinyl glycol ether, polyacrylate, polycarboxylate, stearate and colloidal silica.
8. The method for producing hexagonal flaky magnesium hydroxide by using the horizontal wet ball mill with the heating system and the pressure control system as claimed in claim 3, wherein the surface modifier in the step S3 is one or more of coupling agents, surfactants, silicones, unsaturated organic acids and water-soluble polymers.
9. The method for producing hexagonal flaky magnesium hydroxide by using the horizontal wet ball mill with the heating system and the pressure control system as claimed in claim 3, wherein the coupling agent comprises silanes, titanates and aluminates; the surfactant includes anionic, cationic and nonionic.
10. The method for producing hexagonal flaky magnesium hydroxide by using the horizontal wet ball mill with the heating system and the pressure control system as claimed in claim 4, wherein the solvent is one or more of ethanol, isopropanol, acetone, toluene and xylene.
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