CN112194823A - Magnesium oxide with surface modification treatment - Google Patents
Magnesium oxide with surface modification treatment Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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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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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
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- C01F5/02—Magnesia
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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Abstract
The invention discloses magnesium oxide subjected to surface modification treatment, which is prepared from the following raw materials: the magnesium chloride-sodium trioxide-sodium silicate water dispersible agent comprises magnesium chloride, disodium trioxide, a dispersing agent, a modifier and distilled water, wherein the raw materials comprise the following components in percentage by mass: 30-50% of magnesium chloride, 20-40% of disodium trioxide, 8-15% of dispersant, 2-6% of modifier and 40-70% of distilled water; the method has the advantages of simplified process, mild condition, short time, high efficiency and greatly reduced energy consumption, adopts titanate coupling agent to carry out dry surface modification on the magnesium oxide, can change the magnesium oxide particles from hydrophilicity to hydrophobicity, has good dispersibility in organic solvent, has high uniformity and strong controllability, is easy to realize industrial preparation, and has important application prospect.
Description
Technical Field
The invention relates to the technical field of magnesium oxide, in particular to magnesium oxide with surface modification treatment.
Background
Magnesium oxide is an inorganic substance, has the chemical formula of MgO, is an oxide of magnesium, and is an ionic compound. The magnesia is a white solid at normal temperature, exists in nature in the form of periclase, is a raw material for smelting the magnesia, has high fireproof and insulating properties, can be converted into crystals after being burnt at a high temperature of more than 1000 ℃, and can be converted into dead-burned magnesia (namely magnesia) or sintered magnesia when the temperature is raised to 1500-2000 ℃.
The magnesium oxide material is odorless, tasteless and nontoxic, has extremely strong buffering performance and high-efficiency chemical adsorption performance, and has attracted extensive attention in the aspects of metallurgy, environment, building and the like.
However, the magnesium oxide powder is difficult to disperse in the polymer material due to the great difference between the magnesium oxide powder and the polymer material: the surface of the hydrophilic magnesium oxide powder is incompatible with the surface of the polymer to hinder combination; the expansion coefficients of the magnesium oxide powder and the high polymer material are different, so that the stress is not uniform when the material is heated, and the defects of material damage and the like are overcome.
Disclosure of Invention
The present invention has been made to solve the above problems occurring in the prior art, and an object of the present invention is to provide a surface-modified magnesium oxide.
In order to achieve the purpose, the invention provides the following technical scheme: the magnesium oxide with the surface modified treatment is prepared from the following raw materials: the magnesium chloride-sodium trioxide-sodium silicate water dispersible agent comprises magnesium chloride, disodium trioxide, a dispersing agent, a modifier and distilled water, wherein the raw materials comprise the following components in percentage by mass: 30-50% of magnesium chloride, 20-40% of disodium trioxide, 8-15% of dispersant, 2-6% of modifier and 40-70% of distilled water.
Preferably, the modifier is one or more of silicone oil, stearic acid and a titanate coupling agent, and the titanate coupling agent is preferred.
A preparation method of magnesium oxide with surface modification treatment comprises the following steps:
s1, taking magnesium chloride and disodium trioxide as raw materials, respectively adding the magnesium chloride and the disodium trioxide into a reaction kettle, then adding distilled water, and uniformly stirring to prepare a magnesium chloride and disodium trioxide solution for later use;
s2, adding a dispersing agent into the solution of the magnesium chloride and the disodium trioxide in the step S1, continuously stirring until the reaction is complete, standing, filtering to obtain a precipitate, and standing for 2-3 hours for later use;
s3, washing the precipitate obtained in the step S2 with deionized water for 3-5 times, soaking with a proper amount of absolute ethyl alcohol, filtering, and drying with microwaves for later use;
s4, calcining the precipitate dried in the step S3 at 450-550 ℃ for 3-4 hours to obtain nano magnesium oxide powder for later use;
s5, weighing a proper amount of the nano magnesium oxide powder obtained in the step S4, then ultrasonically oscillating the nano magnesium oxide powder in distilled water for 10 minutes, adding a proper amount of modifier solution, and then placing in a constant-temperature water bath environment at 35 ℃ for 20 minutes to obtain a mixed solution for later use;
s6, placing the mixed solution in the step S5 into a ball milling tank, carrying out ball milling processing at a certain rotating speed, and taking out a ball-milled product for later use;
s7, cleaning the ball-milled product in the step S6 with distilled water, and then placing the ball-milled product in microwave drying to obtain the surface modified magnesium oxide.
Preferably, the stirring time is 15 to 30min in step S1, and 30 to 50min in step S2.
Preferably, in the step S3, the dosage of the absolute ethyl alcohol is 75-125 mol/mL; the microwave drying time is 10-15 min.
Preferably, in step S5, the modification time is 1-6 h.
Preferably, in step S6, the ball milling speed is 240-300 r/min; the ball milling time is 1-3 h.
Compared with the prior art, the invention has the beneficial effects that:
1. the method has the advantages of simplified process, mild condition, short time, high efficiency and greatly reduced energy consumption, adopts titanate coupling agent to carry out dry surface modification on the magnesium oxide, can change the magnesium oxide particles from hydrophilicity to hydrophobicity, has good dispersibility in organic solvent, has high uniformity and strong controllability, is easy to realize industrial preparation, and has important application prospect.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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
The magnesium oxide with the surface modified treatment is prepared from the following raw materials: the magnesium chloride-sodium trioxide-sodium silicate water dispersible agent comprises magnesium chloride, disodium trioxide, a dispersing agent, a modifier and distilled water, wherein the raw materials comprise the following components in percentage by mass: 40% of magnesium chloride, 30% of disodium trioxide, 13% of a dispersant, 2% of a modifier and 60% of distilled water.
Wherein, the modifier is one or more of silicone oil, stearic acid and titanate coupling agent, and is preferably titanate coupling agent.
A preparation method of magnesium oxide with surface modification treatment comprises the following steps:
s1, taking magnesium chloride and disodium trioxide as raw materials, respectively adding the magnesium chloride and the disodium trioxide into a reaction kettle, then adding distilled water, and uniformly stirring to prepare a magnesium chloride and disodium trioxide solution for later use;
s2, adding a dispersing agent into the solution of the magnesium chloride and the disodium trioxide in the step S1, continuously stirring until the reaction is complete, standing, filtering to obtain a precipitate, and standing for 2-3 hours for later use;
s3, washing the precipitate obtained in the step S2 with deionized water for 3-5 times, soaking with a proper amount of absolute ethyl alcohol, filtering, and drying with microwaves for later use;
s4, calcining the precipitate dried in the step S3 at 450-550 ℃ for 3-4 hours to obtain nano magnesium oxide powder for later use;
s5, weighing an appropriate amount of the nano magnesium oxide powder obtained in the step S4, then ultrasonically oscillating the nano magnesium oxide powder in distilled water for 10 minutes, adding an appropriate amount of modifier solution, and then placing the mixture in a constant-temperature water bath environment at 35 ℃ for 20 minutes to obtain a mixed solution, wherein the modification time is 1 hour for later use;
s6, placing the mixed solution in the step S5 into a ball milling tank, carrying out ball milling processing at a certain rotating speed, and taking out a ball-milled product, wherein the ball milling rotating speed is 240r/min for later use;
s7, cleaning the ball-milled product in the step S6 with distilled water, and then placing the ball-milled product in microwave drying to obtain the surface modified magnesium oxide.
Example 2
The magnesium oxide with the surface modified treatment is prepared from the following raw materials: the magnesium chloride-sodium trioxide-sodium silicate water dispersible agent comprises magnesium chloride, disodium trioxide, a dispersing agent, a modifier and distilled water, wherein the raw materials comprise the following components in percentage by mass: 40% of magnesium chloride, 30% of disodium trioxide, 13% of a dispersing agent, 4% of a modifying agent and 60% of distilled water.
Wherein, the modifier is one or more of silicone oil, stearic acid and titanate coupling agent, and is preferably titanate coupling agent.
A preparation method of magnesium oxide with surface modification treatment comprises the following steps:
s1, taking magnesium chloride and disodium trioxide as raw materials, respectively adding the magnesium chloride and the disodium trioxide into a reaction kettle, then adding distilled water, and uniformly stirring to prepare a magnesium chloride and disodium trioxide solution for later use;
s2, adding a dispersing agent into the solution of the magnesium chloride and the disodium trioxide in the step S1, continuously stirring until the reaction is complete, standing, filtering to obtain a precipitate, and standing for 2-3 hours for later use;
s3, washing the precipitate obtained in the step S2 with deionized water for 3-5 times, soaking with a proper amount of absolute ethyl alcohol, filtering, and drying with microwaves for later use;
s4, calcining the precipitate dried in the step S3 at 450-550 ℃ for 3-4 hours to obtain nano magnesium oxide powder for later use;
s5, weighing an appropriate amount of the nano magnesium oxide powder obtained in the step S4, then ultrasonically oscillating the nano magnesium oxide powder in distilled water for 10 minutes, adding an appropriate amount of modifier solution, and then placing the mixture in a constant-temperature water bath environment at 35 ℃ for 20 minutes to obtain a mixed solution, wherein the modification time is 2 hours for later use;
s6, placing the mixed solution in the step S5 into a ball milling tank, carrying out ball milling processing at a certain rotating speed, and taking out a ball-milled product, wherein the ball milling rotating speed is 260r/min for later use;
s7, cleaning the ball-milled product in the step S6 with distilled water, and then placing the ball-milled product in microwave drying to obtain the surface modified magnesium oxide.
Example 3
The magnesium oxide with the surface modified treatment is prepared from the following raw materials: the magnesium chloride-sodium trioxide-sodium silicate water dispersible agent comprises magnesium chloride, disodium trioxide, a dispersing agent, a modifier and distilled water, wherein the raw materials comprise the following components in percentage by mass: 40% of magnesium chloride, 30% of disodium trioxide, 13% of a dispersing agent, 5% of a modifying agent and 60% of distilled water.
Wherein, the modifier is one or more of silicone oil, stearic acid and titanate coupling agent, and is preferably titanate coupling agent.
A preparation method of magnesium oxide with surface modification treatment comprises the following steps:
s1, taking magnesium chloride and disodium trioxide as raw materials, respectively adding the magnesium chloride and the disodium trioxide into a reaction kettle, then adding distilled water, and uniformly stirring to prepare a magnesium chloride and disodium trioxide solution for later use;
s2, adding a dispersing agent into the solution of the magnesium chloride and the disodium trioxide in the step S1, continuously stirring until the reaction is complete, standing, filtering to obtain a precipitate, and standing for 2-3 hours for later use;
s3, washing the precipitate obtained in the step S2 with deionized water for 3-5 times, soaking with a proper amount of absolute ethyl alcohol, filtering, and drying with microwaves for later use;
s4, calcining the precipitate dried in the step S3 at 450-550 ℃ for 3-4 hours to obtain nano magnesium oxide powder for later use;
s5, weighing an appropriate amount of the nano magnesium oxide powder obtained in the step S4, then ultrasonically oscillating the nano magnesium oxide powder in distilled water for 10 minutes, adding an appropriate amount of modifier solution, and then placing the mixture in a constant-temperature water bath environment at 35 ℃ for 20 minutes to obtain a mixed solution, wherein the modification time is 4 hours for later use;
s6, placing the mixed solution in the step S5 into a ball milling tank, carrying out ball milling processing at a certain rotating speed, and taking out a ball-milled product, wherein the ball milling rotating speed is 280r/min for later use;
s7, cleaning the ball-milled product in the step S6 with distilled water, and then placing the ball-milled product in microwave drying to obtain the surface modified magnesium oxide.
Example 4
The magnesium oxide with the surface modified treatment is prepared from the following raw materials: the magnesium chloride-sodium trioxide-sodium silicate water dispersible agent comprises magnesium chloride, disodium trioxide, a dispersing agent, a modifier and distilled water, wherein the raw materials comprise the following components in percentage by mass: 40% of magnesium chloride, 30% of disodium trioxide, 13% of a dispersing agent, 6% of a modifying agent and 60% of distilled water.
Wherein, the modifier is one or more of silicone oil, stearic acid and titanate coupling agent, and is preferably titanate coupling agent.
A preparation method of magnesium oxide with surface modification treatment comprises the following steps:
s1, taking magnesium chloride and disodium trioxide as raw materials, respectively adding the magnesium chloride and the disodium trioxide into a reaction kettle, then adding distilled water, and uniformly stirring to prepare a magnesium chloride and disodium trioxide solution for later use;
s2, adding a dispersing agent into the solution of the magnesium chloride and the disodium trioxide in the step S1, continuously stirring until the reaction is complete, standing, filtering to obtain a precipitate, and standing for 2-3 hours for later use;
s3, washing the precipitate obtained in the step S2 with deionized water for 3-5 times, soaking with a proper amount of absolute ethyl alcohol, filtering, and drying with microwaves for later use;
s4, calcining the precipitate dried in the step S3 at 450-550 ℃ for 3-4 hours to obtain nano magnesium oxide powder for later use;
s5, weighing an appropriate amount of the nano magnesium oxide powder obtained in the step S4, then ultrasonically oscillating the nano magnesium oxide powder in distilled water for 10 minutes, adding an appropriate amount of modifier solution, and then placing the mixture in a constant-temperature water bath environment at 35 ℃ for 20 minutes to obtain a mixed solution, wherein the modification time is 6 hours for later use;
s6, placing the mixed solution in the step S5 into a ball milling tank, carrying out ball milling processing at a certain rotating speed, and taking out a ball-milled product, wherein the ball milling rotating speed is 300r/min for later use;
s7, cleaning the ball-milled product in the step S6 with distilled water, and then placing the ball-milled product in microwave drying to obtain the surface modified magnesium oxide.
Examples of the experiments
Subject: the surface-modified magnesium oxide of the present invention and the ordinary magnesium oxide were selected and divided into example 1 group, example 2 group, example 3 group, example 4 group and control group, respectively.
The experimental basis is as follows: the degree of oleophilicity can be used as one of the parameters for evaluating the modification effect.
The experimental method comprises the following steps: the group of example 1, the group of example 2, the group of example 3, the group of example 4 and the control group were placed in 50ml of distilled water, methanol was added dropwise, and when the powder floating on the water surface was completely wetted, the amount of methanol added a was recorded, then: the degree of oleophilic transformation is [ a/(a +50) ] × 100%.
The results of the experiments are shown in the following table:
from the various embodiments above, it is known that: the invention has simplified process, mild condition, short time, high efficiency and greatly reduced energy consumption, adopts titanate coupling agent to carry out dry surface modification on the magnesium oxide, can change the hydrophilicity of the magnesium oxide particles into hydrophobicity, and has good dispersibility in organic solvent, and the better process conditions of the dry surface modification are as follows: the dosage of the modifier is 4 percent, the modification time is 2 hours, and the ball milling rotating speed is 260 r/min.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A surface-modified magnesium oxide characterized by: the feed is prepared from the following raw materials: the magnesium chloride-sodium trioxide-sodium silicate water dispersible agent comprises magnesium chloride, disodium trioxide, a dispersing agent, a modifier and distilled water, wherein the raw materials comprise the following components in percentage by mass: 30-50% of magnesium chloride, 20-40% of disodium trioxide, 8-15% of dispersant, 2-6% of modifier and 40-70% of distilled water.
2. A surface-modified magnesium oxide according to claim 1, wherein: the modifier is one or more of silicone oil, stearic acid and titanate coupling agent, and is preferably titanate coupling agent.
3. A method for preparing magnesium oxide with surface modification treatment is characterized in that: the method comprises the following steps:
s1, taking magnesium chloride and disodium trioxide as raw materials, respectively adding the magnesium chloride and the disodium trioxide into a reaction kettle, then adding distilled water, and uniformly stirring to prepare a magnesium chloride and disodium trioxide solution for later use;
s2, adding a dispersing agent into the solution of the magnesium chloride and the disodium trioxide in the step S1, continuously stirring until the reaction is complete, standing, filtering to obtain a precipitate, and standing for 2-3 hours for later use;
s3, washing the precipitate obtained in the step S2 with deionized water for 3-5 times, soaking with a proper amount of absolute ethyl alcohol, filtering, and drying with microwaves for later use;
s4, calcining the precipitate dried in the step S3 at 450-550 ℃ for 3-4 hours to obtain nano magnesium oxide powder for later use;
s5, weighing a proper amount of the nano magnesium oxide powder obtained in the step S4, then ultrasonically oscillating the nano magnesium oxide powder in distilled water for 10 minutes, adding a proper amount of modifier solution, and then placing in a constant-temperature water bath environment at 35 ℃ for 20 minutes to obtain a mixed solution for later use;
s6, placing the mixed solution in the step S5 into a ball milling tank, carrying out ball milling processing at a certain rotating speed, and taking out a ball-milled product for later use;
s7, cleaning the ball-milled product in the step S6 with distilled water, and then placing the ball-milled product in microwave drying to obtain the surface modified magnesium oxide.
4. A surface-modified magnesium oxide according to claim 3, wherein: in step S1, the stirring time is 15-30 min, and in step S2, the stirring time is 30-50 min.
5. A surface-modified magnesium oxide according to claim 3, wherein: in step S3, the amount of absolute ethyl alcohol is 75-125 mol/mL; the microwave drying time is 10-15 min.
6. A surface-modified magnesium oxide according to claim 3, wherein: in step S5, the modification time is 1-6 h.
7. A surface-modified magnesium oxide according to claim 3, wherein: in step S6, the ball milling speed is 240-300 r/min; the ball milling time is 1-3 h.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106430261A (en) * | 2016-09-13 | 2017-02-22 | 苏州市泽镁新材料科技有限公司 | Method for preparing particle-evenly-dispersed nanometer magnesium oxide |
| CN107337937A (en) * | 2017-06-09 | 2017-11-10 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method for the surface-modified nano magnesium oxide material for being exclusively used in SMC thickenings |
-
2020
- 2020-10-29 CN CN202011180155.XA patent/CN112194823A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106430261A (en) * | 2016-09-13 | 2017-02-22 | 苏州市泽镁新材料科技有限公司 | Method for preparing particle-evenly-dispersed nanometer magnesium oxide |
| CN107337937A (en) * | 2017-06-09 | 2017-11-10 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method for the surface-modified nano magnesium oxide material for being exclusively used in SMC thickenings |
Non-Patent Citations (3)
| Title |
|---|
| 徐景文等: "钛酸酯偶联剂改性纳米MgO的研究", 《塑料助剂》 * |
| 蒋红梅: "沉淀转化法制备纳米氧化镁及表面改性工艺研究", 《中国优秀博硕士学位论文全文数据库（硕士） 工程科技I辑》 * |
| 蒋红梅等: "一种纳米氧化镁表面改性工艺的研究", 《无机盐工业》 * |
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