CN111378299B - Method for modifying surface of magnesium hydroxide by using dopamine-induced transition metal ions - Google Patents
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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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- 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
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic 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 relates to the field of compounds for modifying high molecular materials, in particular to a method for modifying the surface of magnesium hydroxide by utilizing dopamine-induced transition metal ions. Meanwhile, by utilizing good charring property and strong free radical trapping property of dopamine, combining the advantages of transition metal ions for catalyzing charring, promoting matrix crosslinking and the like, compared with the single addition of magnesium hydroxide, the high-molecular base material has higher flame retardant efficiency, thermal stability and hydrophobicity.
Description
Technical Field
The invention relates to the field of compounds for modifying high polymer materials, in particular to a method for modifying the surface of magnesium hydroxide by using dopamine-induced transition metal ions.
Background
The magnesium hydroxide has a typical lamellar structure, and has the advantages of high purity, small particle size, capability of carrying out in-situ coating modification and the like. However, magnesium hydroxide has high surface energy, and unmodified magnesium hydroxide is easy to agglomerate and has poor dispersing performance. Secondly, magnesium hydroxide has good hydrophilic property, most polymer matrix materials are hydrophobic, the compatibility of the two is poor, and the processing property and the mechanical property of the high molecular base material are influenced by excessive use of the magnesium hydroxide. In addition, the high filling of magnesium hydroxide causes an intergrowth phenomenon in which cracks are generated at the interface of the inorganic flame retardant and the base material. An effective way to improve the compatibility of magnesium hydroxide with polymeric substrates and to ensure the processability and mechanical properties of the substrates is to modify the surface of magnesium hydroxide.
Dopamine is a biological neurotransmitter, has multifunctional surface deposition capabilities, and can be easily coated on almost all types of surfaces simply by the self-polymerizing nature of dopamine hydrochloride (DOPA) in alkaline aqueous solutions. Meanwhile, polydopamine also has good char forming capability, and is expected to improve the char forming and flame retardant properties of the material. In addition, polydopamine and its derivatives are widely used in the fields of biomedical science, sensing, water treatment, polymer nanocomposites, energy storage/conversion and catalysis due to their surface having abundant amino groups, catechol groups and excellent precursors of graphite-like N-doped carbon.
Transition metal ions will affect certain polymer material properties, they can catalyze the cross-linking of the polymer matrix and promote the formation of char-forming species, further inhibiting the combustion of the polymer. There is increasing interest in using transition metal ions for the control of synthesis and flame retardants.
Disclosure of Invention
The invention aims to provide a method for modifying the surface of magnesium hydroxide by utilizing dopamine-induced transition metal ions, which overcomes the defects in the prior art, successfully coats the transition metal ions and dopamine on the surface of the magnesium hydroxide through a mild reaction, and enables a high-molecular base material to have higher flame retardant efficiency, thermal stability and hydrophobicity compared with the method of singly adding magnesium hydroxide.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for modifying the surface of magnesium hydroxide by dopamine-induced transition metal ions is characterized in that different transition metal ions are complexed with dopamine, and the surface of the magnesium hydroxide is modified in a liquid phase deposition mode, and the method comprises the following specific synthetic steps:
1) dispersing: ultrasonically dispersing 0.5-1g of magnesium hydroxide in 1000-1500ml of distilled water, and ultrasonically treating for 30 min; 2) reacting, weighing 0.5-1g of dopamine and 0.213-0.426g of transition metal compound, adding into the dispersed magnesium hydroxide solution, stirring for 10min, adding 1.21-1.815g of buffer solution with pH of 8.5, and stirring at normal temperature for at least 12 hours; 3) separating, centrifugally washing and drying to obtain the modified magnesium hydroxide.
The buffer in step 2) is any one of Tris (hydroxymethyl) aminomethane (Tris), Tris Buffered Saline (TBS), Phosphate Buffered Saline (PBS), and Tris boric acid (TBE) buffer.
The dopamine in the step 2) is any one of dopamine hydrochloride (DOPA), N-3, 4-dihydroxyphenethyl methyl vinyl propionate (DMA), 6-nitro dopamine, 6-cyano dopamine and 6-carboxyl dopamine.
The transition metal compound in the step 2) is FeCl2、FeCl3、FeO、Fe2O3、Fe(OH)2、Fe(OH)3、FeSO4·7H2O、Fe2(SO4) 3、CoO、Co(OH) 2、CoCl2、CoSO4、NiO、Ni2O3、Ni(OH) 2、NiSO4、NiCl2、Ni(NO3) 2、CuO、Cu2O、Cu(OH) 2、CuCl、CuS、Cu2S、CuSO4、CuSO4·5H2O、CuCN。
Compared with the prior art, the invention has the following beneficial effects: 1) transition metal ions and dopamine are successfully coated on the surface of the magnesium hydroxide through a mild reaction, so that the surface hydrophobicity is improved. 2) The invention combines the excellent flame-retardant and smoke-inhibiting properties of the material by utilizing the good char-forming property of dopamine, the characteristic of capturing free radical ions in the combustion process and the unique thermal decomposition characteristic of magnesium hydroxide, and can obviously improve the flame-retardant, smoke-inhibiting, anti-dripping and other properties of the material. 3) The invention fully exerts the characteristic that the transition metal ions promote the crosslinking of the matrix, forms the carbon protective layer with mechanical strength and plays a role in inhibiting the flame development and propagation.
Detailed Description
The following examples are presented to further illustrate embodiments of the present invention:
the present invention is described in detail below by way of examples, it should be noted that the following examples are only used for further illustration of the present invention, and should not be construed as limiting the scope of the present invention, and that the non-essential modifications and adaptations of the present invention by those skilled in the art according to the present disclosure described above will still fall within the scope of the present invention.
Example 1
1) Dispersing: ultrasonically dispersing 0.5g of magnesium hydroxide in 1000ml of distilled water, and ultrasonically treating for 30 min; 2) reaction: 0.5g dopamine hydrochloride (dopamine), 0.213g FeCl are weighed out3(transition metal compound) was added to the dispersed magnesium hydroxide solution, stirred for 10min, added with 1.21g of Tris (hydroxymethyl) aminomethane (Tris) buffer (pH8.5), and stirred at room temperature for 12 hours; 2) separation: centrifugally washing and drying to obtain the surface functionalized magnesium hydroxide.
Example 2
1) Dispersing: ultrasonically dispersing 0.5g of magnesium hydroxide in 1000ml of distilled water, and ultrasonically treating for 30 min; 2) reaction: 0.8g dopamine hydrochloride (dopamine), 0.213g FeCl are weighed out3(transition metal compound) was added to the dispersed magnesium hydroxide solution, stirred for 10min, added with 1.21g of Tris (hydroxymethy) aminomethane (Tris) (pH8.5) buffer (pH8.5), and stirred at room temperature for 12 hours; 2) separation: centrifugally washing and drying to obtain the surface functionalized magnesium hydroxide.
Example 3
1) Dispersing: ultrasonically dispersing 0.5g of magnesium hydroxide in 1000ml of distilled water, and ultrasonically treating for 30 min; 2) reaction: 0.2g dopamine hydrochloride (dopamine), 0.213g FeCl are weighed out3(transition metal compound) was added to the dispersed magnesium hydroxide solution, stirred for 10min, added with 1.21g of Tris (hydroxymethy) aminomethane (Tris) (pH8.5) buffer (pH8.5), and stirred at room temperature for 12 hours; 2) separation: centrifugally washing and drying to obtain the surface functionalized magnesium hydroxide.
Example 4
1) Dispersing: ultrasonically dispersing 0.5g of magnesium hydroxide in 1000ml of distilled water, and ultrasonically treating for 30 min; 2) reaction: 0.5g dopamine hydrochloride (dopamine), 0.426g FeCl were weighed out3(transition metal compound) was added to the dispersed magnesium hydroxide solution, stirred for 10min and then 1.21g of Tri was addeds (hydroxyymethyl) aminomethane (Tris) (pH8.5) buffer (pH8.5), and stirring at room temperature for 12 hours; 2) separation: centrifugally washing and drying to obtain the surface functionalized magnesium hydroxide.
Example 5
1) Dispersing: ultrasonically dispersing 0.5g of magnesium hydroxide in 1000ml of distilled water, and ultrasonically treating for 30 min; 2) reaction: 0.5g dopamine hydrochloride (dopamine), 0.213g NiCl were weighed out2(transition metal compound) was added to the dispersed magnesium hydroxide solution, stirred for 10min, added with 1.21g of Tris (hydroxymethy) aminomethane (Tris) (pH8.5) buffer (pH8.5), and stirred at room temperature for 12 hours; 2) separation: centrifugally washing and drying to obtain the surface functionalized magnesium hydroxide.
Example 6
1) Dispersing: ultrasonically dispersing 0.5g of magnesium hydroxide in 1000ml of distilled water, and ultrasonically treating for 30 min; 2) reaction: 0.5g of 6-nitrodopamine (dopamine), 0.213g of FeCl were weighed out3(transition metal compound) was added to the dispersed magnesium hydroxide solution, stirred for 10min, added with 1.21g of Tris (hydroxymethy) aminomethane (Tris) (pH8.5) buffer (pH8.5), and stirred at room temperature for 12 hours; 2) separation: centrifugally washing and drying to obtain the surface functionalized magnesium hydroxide.
Example 7
1) Dispersing: ultrasonically dispersing 0.5g of magnesium hydroxide in 1000ml of distilled water, and ultrasonically treating for 30 min; 2) reaction: 0.5g of 6-cyanodopamine (dopamine), 0.213g of FeCl were weighed out3(transition metal compound) was added to the dispersed magnesium hydroxide solution, stirred for 10min, added with 1.21g of Tris (hydroxymethy) aminomethane (Tris) (pH8.5) buffer (pH8.5), and stirred at room temperature for 12 hours; 2) separation: centrifugally washing and drying to obtain the surface functionalized magnesium hydroxide.
Example 8
1) Dispersing: ultrasonically dispersing 0.5g of magnesium hydroxide in 1000ml of distilled water, and ultrasonically treating for 30 min; 2) reaction: 0.5g of 6-nitrodopamine (dopamine), 0.213g of CoCl were weighed out2(transition metal compound) is added to the dispersed magnesium hydroxide solution and stirred 10After min, 1.21g of Tris (hydroxymethyl) aminomethane (Tris) (pH8.5) buffer (pH8.5) was added, and the mixture was stirred at room temperature for 12 hours; 2) separation: centrifugally washing and drying to obtain the surface functionalized magnesium hydroxide.
Example 9
1) Dispersing: ultrasonically dispersing 0.5g of magnesium hydroxide in 1000ml of distilled water, and ultrasonically treating for 30 min; 2) reaction: 0.5g of 6-nitrodopamine (dopamine) and 0.213g of CuCN (transition metal compound) are weighed and added into the dispersed magnesium hydroxide solution, stirred for 10min, added with 1.21g of Tris (hydroxymethyl) aminomethane (Tris) (pH8.5) buffer solution (pH8.5), and stirred for 12 hours at normal temperature; 2) separation: centrifugally washing and drying to obtain the surface functionalized magnesium hydroxide.
The hydrophobicity test and thermogravimetric analysis are carried out on unmodified magnesium hydroxide and the examples 1-9, the hydrophobicity and thermal stability of the surface modification of the magnesium hydroxide by dopamine-induced transition metal ions are shown in the table I, and as can be seen, the example 1 has higher thermal stability and better hydrophobicity compared with other examples, so that the application field of the inorganic flame retardant is greatly expanded.
Watch 1
In the above embodiment, the buffer in step 2) may be any one of Tris (hydroxymethyl) aminomethane (Tris), Tris Buffered Saline (TBS), Phosphate Buffer Saline (PBS), and Tris boric acid (TBE) buffer, in addition to Tris (hydroxymethyl) aminomethane (Tris). The dopamine can be selected from 6-carboxydopamine and N-3, 4-dihydroxyphenethyl methyl vinyl propionate (DMA) besides dopamine hydrochloride (DOPA), 6-nitro-dopamine and 6-cyano-dopamine.
Removing FeCl from the transition metal compound in the step 2)3、NiCl2、CoCl2Besides CuCN, FeCl can also be selected2、FeO、Fe2O3、Fe(OH)2、Fe(OH)3、FeSO4·7H2O、Fe2(SO4) 3、CoO、Co(OH) 2、CoSO4、NiO、Ni2O3、Ni(OH) 2、NiSO4、Ni(NO3) 2、CuO、Cu2O、Cu(OH) 2、CuCl、CuS、Cu2S、CuSO4、CuSO4·5H2Any one of O.
Claims (3)
1. A method for modifying the surface of magnesium hydroxide by dopamine-induced transition metal ions is characterized in that different transition metal ions are complexed with dopamine, and the surface of the magnesium hydroxide is modified in a liquid phase deposition mode, and the method comprises the following specific synthesis steps:
1) dispersing: ultrasonically dispersing 0.5-1g of magnesium hydroxide in 1000-1500ml of distilled water, and ultrasonically treating for 30 min;
2) reacting, weighing 0.5-1g of dopamine and 0.213-0.426g of transition metal compound, adding into the dispersed magnesium hydroxide solution, stirring for 10min, adding 1.21-1.815g of buffer solution with pH of 8.5, and stirring at normal temperature for at least 12 hours; wherein the transition metal compound is FeCl2、FeCl3、FeO、Fe2O3、Fe(OH)2、Fe(OH)3、FeSO4·7H2O、Fe2(SO4)3、CoO、Co(OH)2、CoCl2、CoSO4、NiO、Ni2O3、Ni(OH)2、NiSO4、NiCl2、Ni(NO3)2、CuO、Cu2O、Cu(OH)2、CuCl、CuS、Cu2S、CuSO4、CuSO4·5H2O、CuCN；
3) Separating, centrifugally washing and drying to obtain the modified magnesium hydroxide.
2. The method of claim 1, wherein the buffer in step 2) is any one of Tris (hydroxymethyl) aminomethane (Tris), Tris Buffered Saline (TBS), phenatebuffersaline (pbs), Tris boric acid (TBE) buffer.
3. The method for surface modification of magnesium hydroxide by dopamine-induced transition metal ions according to claim 1, wherein the dopamine in step 2) is any one of dopamine hydrochloride (DOPA), N-3, 4-dihydroxyphenethylmethyl-alanine (DMA), 6-nitro-dopamine, 6-cyano-dopamine, 6-carboxy-dopamine.
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| CN113354873A (en) * | 2021-06-16 | 2021-09-07 | 桂林理工大学 | Preparation method of hybrid mesoporous material, product and application thereof |
| CN113499483B (en) * | 2021-06-28 | 2022-05-24 | 福州大学 | Nano copper sulfide coating modified memory alloy esophageal stent and preparation method thereof |
| CN113462024A (en) * | 2021-06-30 | 2021-10-01 | 福建师范大学 | Polydopamine and metal ion modified montmorillonite flame retardant and preparation method thereof |
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