CN107337937A - A kind of preparation method for the surface-modified nano magnesium oxide material for being exclusively used in SMC thickenings - Google Patents
A kind of preparation method for the surface-modified nano magnesium oxide material for being exclusively used in SMC thickenings Download PDFInfo
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- CN107337937A CN107337937A CN201710431546.6A CN201710431546A CN107337937A CN 107337937 A CN107337937 A CN 107337937A CN 201710431546 A CN201710431546 A CN 201710431546A CN 107337937 A CN107337937 A CN 107337937A
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- C—CHEMISTRY; METALLURGY
- 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
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- 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
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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Abstract
The invention provides a kind of preparation method for the surface-modified nano magnesium oxide material for being exclusively used in SMC thickenings, belong to function nano Material Field, appropriate magnesium chloride or magnesium sulfate are dissolved in deionized water with polyvinyl alcohol and form solution A, is placed in 35 DEG C of water bath with thermostatic control；It will be dissolved in mole identical sodium carbonate in quantitative deionized water, and obtain the sodium carbonate liquor B of same concentrations；It is placed in 35 DEG C of water bath with thermostatic control；The half of sodium carbonate liquor is quickly first started into mechanical agitation；With 3~5 precipitations of deionized water rinsing, calcined 120~180 minutes under conditions of 450~550 DEG C；Continue to disperse powder ultrasonic in deionized water, to add appropriate sodium stearate solution；Cleaned up after standing with deionized water, surface-modified nano magnesium oxide material can be obtained by inserting drying in microwave.The modified magnesium oxide material uniform particle sizes that the present invention obtains, the surface-modified nano magnesium oxide material of thickening controllable-rate is obtained, there is important application prospect.
Description
Technical field
The invention belongs to function nano Material Field, and in particular to a kind of surface treatment scheme of SMC special magnesium oxides
Optimization.
Background technology
SMC material is by SMC special yarns, unsaturated-resin, low shrinkage additive, thickener and other fillers composition.Cause
With superior electric property, decay resistance, the advantages that high flexibility, in industries such as haulage vehicle, building, electronic/electrical gas
In have a wide range of applications.
In SMC preparation process, thickener is huge to the performance impact of SMC material.Increase for the chemistry of unsaturated polyester
Thick, most commonly used is alkali metal oxide or hydroxide, such as magnesia, calcium oxide or barium monoxide and corresponding hydroxide
Thing.But relevant industries experience and result of study show：Calcium associated materials are excessively sensitive to moisture, and the relevant thickening material cost of barium is too
Height, their applications as high quality thickener in SMC are all strongly limit, this causes magnesium based material particularly magnesia material
Material turns into the SMC thickening materials of most superiority of effectiveness.
Magnesium oxide material odorless, tasteless itself is nontoxic, and has extremely strong resiliency and efficient chemical adsorptivity, in smelting
The application study of gold, environment, building etc. receives extensive concern, and purposefully material surface is entered according to use environment
The related modified research of row achieves very big progress, including hydrophilicity regulation and control, optics, electricity and thermal property improve.But mesh
The preceding study on the modification for SMC thickeners is relatively fewer, and Hu etc., as covering, is given one kind and be directed to insatiable hunger using organic acid
With the preparation method of polyester resin fiberglass special magnesium oxide, pass through spray based on the nano oxidized magnesium material after preparing
Spill, stirring is carried out.A kind of (unsaturated polyester resin production fiberglass special magnesium oxide and preparation method thereof CN 103923491
A).But the surface modification that magnesia so far, is directly realized by production process makes it not have obvious breakthrough yet suitable for SMC.
The content of the invention
It is an object of the invention to provide a kind of preparation side for the surface-modified nano magnesium oxide material for being exclusively used in SMC thickenings
Method, preparation process and Process of Surface Modification are organically combined, obtain the oxidation for being capable of Effective Regulation SMC thickening rates
Magnesium material.The magnesium oxide material prepared using the program, thickening properties are controllable, and uniformity is good, and it is simply controllable to cut preparation parameter, easily
Amplify in technique, there is obvious application value.
To reach above-mentioned expected purpose, the present invention adopts the following technical scheme that：
A kind of preparation method of surface-modified nano magnesium oxide material for being exclusively used in SMC thickenings provided by the invention, specifically
Processing step is：
1) appropriate magnesium chloride or magnesium sulfate are dissolved in deionized water with polyvinyl alcohol and form solution A, be placed in 35 DEG C of perseverance
In tepidarium；
2) mole identical sodium carbonate in step 1) is dissolved in quantitative deionized water, obtains the sodium carbonate of same concentrations
Solution B；It is placed in 35 DEG C of water bath with thermostatic control；
3) by the half amount of the sodium carbonate liquor B in step 2), directly pour into and start mechanical agitation in solution A；One timing
Between after remaining solution B is slowly added to, continue stirring to react completely formed precipitation；
4) by the sediment in step 3) using after deionized water rinsing 3~5 times, mistake after being infiltrated with appropriate absolute ethyl alcohol
Filter, is placed into microwave and is dried；
5) by sediment dried in step 4), calcined 120~180 minutes under conditions of 450~550 DEG C；
6) by the powder obtained in step 5) using ultrasonic disperse in deionized water, add sodium stearate solution and by pH
Value adjust to 9.5~10.5 alkaline range after as in water bath with thermostatic control environment；
7) suspension in step 6) is filtered, cleaned up with deionized water, inserting drying in microwave can obtain
Surface-modified nano magnesium oxide material.
Compared with prior art, the beneficial effects of the invention are as follows：Pattern control is modified with surface in the present invention and combined
Come, by controlling relevant parameter and filling method in course of reaction, the surface-modified nano of thickening controllable-rate can be obtained
Magnesium oxide material, the uniformity is high, and controllability is strong, it is easy to accomplish and it is industrially prepared, there is important application prospect.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1：
19g magnesium chlorides (0.2mol) powder and mass fraction is weighed to be put into beaker for 5% poly-vinyl alcohol solution 40mL,
Add deionized water to be placed in 200mL in 35 DEG C of water bath with thermostatic control, turn into solution A；Sodium carbonate 21.2g (0.2mol) is weighed to be dissolved in
200mL deionized waters form solution B, in juxtaposition and water bath with thermostatic control；100mL solution Bs are quickly poured into solution A, and start into
Row mechanical agitation；Remaining 100mL solution Bs are at the uniform velocity added with 10mL/min speed after 5 minutes, after persistently stirring 20 minutes
Stop；By sediment deionized water rinsing 3 times after standing 30 minutes, add 20mL absolute ethyl alcohols and infiltrated, be placed on microwave
Dried 15 minutes in drying chamber；Taken out after being calcined 180 minutes under the conditions of dried sediment is placed on into 450 DEG C；Weigh drying
Powder 5g afterwards is put into 100mL deionized waters, and ultrasonic disperse is after 10 minutes；The hard fatty acids that mass fraction is 5% are added to receive
Solution 18mL；Add after pH value is modulated 9.5 by appropriate sodium hydroxide solution to be put into 35 DEG C of waters bath with thermostatic control and react 20 minutes, by institute
Suspension filtering is obtained, deionized water rinsing 2~3 times, surface modification can be obtained for dry 15 minutes by, which being put into microwave drying chamber, receives
Rice magnesium oxide material.
Embodiment 2：
24g magnesium sulfate (0.2mol) powder and mass fraction is weighed to be put into beaker for 5% poly-vinyl alcohol solution 40mL,
Add deionized water to be placed in 200mL in 35 DEG C of water bath with thermostatic control, turn into solution A；Sodium carbonate 21.2g (0.2mol) is weighed to be dissolved in
200mL deionized waters form solution B, in juxtaposition and water bath with thermostatic control；100mL solution Bs are quickly poured into solution A, and start into
Row mechanical agitation；Remaining 100mL solution Bs are at the uniform velocity added with 10mL/min speed after 5 minutes, after persistently stirring 20 minutes
Stop；By sediment deionized water rinsing 3 times after standing 30 minutes, add 15mL absolute ethyl alcohols and infiltrated, be placed on microwave
Dried 15 minutes in drying chamber；Taken out after being calcined 150 minutes under the conditions of dried sediment is placed on into 500 DEG C；Weigh drying
Powder 5g afterwards is put into 100mL deionized waters, and ultrasonic disperse is after 10 minutes；The hard fatty acids that mass fraction is 5% are added to receive
Solution 15mL；Add after pH value is adjusted to 10 by appropriate sodium hydroxide solution to be put into 35 DEG C of waters bath with thermostatic control and react 20 minutes, by institute
Suspension filtering is obtained, deionized water rinsing 2~3 times, surface modification can be obtained for dry 15 minutes by, which being put into microwave drying chamber, receives
Rice magnesium oxide material.
Embodiment 3：
23.6g magnesium chloride hexahydrates (0.2mol) powder and mass fraction is weighed to be put into for 3% poly-vinyl alcohol solution 40mL
In beaker, add deionized water and be placed in 200mL in 35 DEG C of water bath with thermostatic control, turn into solution A；Weigh sodium carbonate 21.2g
(0.1mo2) is dissolved in 200mL deionized waters and forms solution B, in juxtaposition and water bath with thermostatic control；100mL solution Bs are quickly poured into solution A
In, and proceed by mechanical agitation；Remaining 100mL solution Bs are at the uniform velocity added with 10mL/min speed after 5 minutes, continued
Stirring stops after 20 minutes；By sediment deionized water rinsing 3 times after standing 20 minutes, add 15mL absolute ethyl alcohols and soaked
Profit, it is placed in microwave drying chamber and dries 15 minutes；Taken after being calcined 120 minutes under the conditions of dried sediment is placed on into 550 DEG C
Go out；Weigh dried powder 5g to be put into 100mL deionized waters, ultrasonic disperse is after 10 minutes；It is 5% to add mass fraction
Hard fatty acids receive solution 12mL；Add after pH value is adjusted to 10.5 by appropriate sodium hydroxide solution to be put into 35 DEG C of waters bath with thermostatic control and react
20 minutes, gained suspension is filtered, deionized water rinsing 2~3 times, be put into and dry 15 minutes and can obtain in microwave drying chamber
Surface-modified nano magnesium oxide material.
Embodiment 4：
Weigh 49.2g epsom salts (MgSO4.7H2O) (0.2mol) powder and the polyvinyl alcohol that mass fraction is 4% are molten
Liquid 40mL is put into beaker, is added deionized water and is placed in 200mL in 35 DEG C of water bath with thermostatic control, turns into solution A；Weigh carbonic acid
21.2g (0.2mol) is dissolved in 200mL deionized waters and forms solution B, in juxtaposition and water bath with thermostatic control；100mL solution Bs are quickly poured into
In solution A, and proceed by mechanical agitation；Remaining 100mL solution Bs are at the uniform velocity added with 10mL/min speed after 5 minutes,
Stop after persistently stirring 20 minutes；By sediment deionized water rinsing 3 times after standing 30 minutes, add 25mL absolute ethyl alcohols and enter
Row infiltration, is placed in microwave drying chamber and dries 15 minutes；Calcined 120 minutes under the conditions of dried sediment is placed on into 550 DEG C
After take out；Weigh dried powder 5g to be put into 100mL deionized waters, ultrasonic disperse is after 10 minutes；Adding mass fraction is
5% hard fatty acids receive solution 15mL；Add after pH value is adjusted to 10.5 by appropriate sodium hydroxide solution and be put into 35 DEG C of waters bath with thermostatic control
Middle reaction 20 minutes, gained suspension is filtered, deionized water rinsing 2~3 times, is put into microwave drying chamber and is dried 15 minutes i.e.
Surface-modified nano magnesium oxide material can be obtained.
The preferred embodiments of the present invention have shown and described in described above, as previously described, it should be understood that the present invention is not office
Be limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and available for various other combinations, modification and
Environment, and can be changed in the scope of the invention is set forth herein by the technology or knowledge of above-mentioned teaching or association area
It is dynamic, and the change and change that those skilled in the art are carried out do not depart from the spirit and scope of the present invention, then all should be appended by the present invention
In scope of the claims.
Claims (5)
- A kind of 1. preparation method for the surface-modified nano magnesium oxide material for being exclusively used in SMC thickenings, it is characterised in that concrete technology Step is：1) appropriate magnesium chloride or magnesium sulfate are dissolved in deionized water with polyvinyl alcohol and form solution A, be placed in 35 DEG C of thermostatted water In bath；Wherein the concentration of magnesium chloride or magnesium sulfate is 1mol/L；Volume fraction of the polyvinyl alcohol in mixed solution is 40%；2) proper amount of sodium carbonate is dissolved in deionized water, is prepared into the solution B that concentration is 1mol/L；Take the solution B of same volume； It is placed in 35 DEG C of water bath with thermostatic control；3) semi-direct pour into of the sodium carbonate liquor B in step 2) is started into mechanical agitation in solution A；According to one after 5 minutes Constant speed rate at the uniform velocity poured second half into 10 minutes；It is complete to reaction to continue stirring；Filtering obtains sediment after standing, stands Time is 20~30 minutes；4) sediment in step 3) is filtered, juxtaposition using after deionized water rinsing 3~5 times after appropriate absolute ethyl alcohol infiltration Enter microwave to be dried；5) by sediment dried in step 4), calcined 120~180 minutes under conditions of 450~550 DEG C；6) it is 1 according to quality by the powder obtained in step 5):20 ratio sonic oscillation 10 minutes in deionized water；Add The sodium stearate solution that appropriate mass fraction is 5%；Soda acid is added to adjust pH value to rearmounted in 9.5~10.5 alkaline range 20 minutes in 35 DEG C of water bath with thermostatic control environment；7) suspension in step 6) is filtered, cleaned up with deionized water, surface can be obtained by inserting drying in microwave Modified Nano magnesium oxide material.
- 2. the preparation method of the surface-modified nano magnesium oxide material according to claim 1 for being exclusively used in SMC thickenings, it is special Sign is that the concentration of poly-vinyl alcohol solution is 3%~5% (mass fraction) in step 1).
- 3. the preparation method of the surface-modified nano magnesium oxide material according to claim 1 for being exclusively used in SMC thickenings, it is special Sign is that step 3) mid-early stage mechanical agitation rotating speed is 600~800r/min, and mixing speed is 200~400r/ when at the uniform velocity adding min。
- 4. the preparation method of the surface-modified nano magnesium oxide material according to claim 1 for being exclusively used in SMC thickenings, it is special Sign is that the dosage of step 4) absolute ethyl alcohol is 75~125mol/mL；The microwave drying time is 10~15 minutes.
- 5. the preparation method of the surface-modified nano magnesium oxide material according to claim 1 for being exclusively used in SMC thickenings, it is special Sign is that the addition volume of sodium stearate solution is 12~18% of the volume of solution after ultrasound in step 5).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112194823A (en) * | 2020-10-29 | 2021-01-08 | 刘士福 | Magnesium oxide with surface modification treatment |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271319A (en) * | 2015-10-28 | 2016-01-27 | 内江师范学院 | Method for preparing nanometer MgO |
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2017
- 2017-06-09 CN CN201710431546.6A patent/CN107337937A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271319A (en) * | 2015-10-28 | 2016-01-27 | 内江师范学院 | Method for preparing nanometer MgO |
Non-Patent Citations (2)
| Title |
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| 蒋红梅: ""沉淀转化法制备纳米氧化镁及表面改性工艺研究"", 《中国优秀硕士学位论文全文数据库（工程科技I辑）》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112194823A (en) * | 2020-10-29 | 2021-01-08 | 刘士福 | Magnesium oxide with surface modification treatment |
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Address after: Suzhou City, Jiangsu province 215500 Changshou City Shanghu town yuanyangqiao industrial district Applicant after: SUZHOU ZEMEI NEW MATERIAL TECHNOLOGY CO., LTD. Address before: 215500 Jiangsu city of Changzhou province Changshou City Shanghu town yuanyangqiao industrial district Applicant before: SUZHOU ZEMEI NEW MATERIAL TECHNOLOGY CO., LTD. |
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Application publication date: 20171110 |