CN110551357B - Flame-retardant magnesium-aluminum hydrotalcite/carboxyl POSS composite material and preparation method thereof - Google Patents
Flame-retardant magnesium-aluminum hydrotalcite/carboxyl POSS composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses flame-retardant magnesium-aluminum hydrotalcite/carboxylThe POSS-based composite material and the preparation method thereof solve the problems of poor dispersibility and insufficient thermal stability of hydrotalcite in the composite material. The technical scheme of the invention is as follows: first, Mg containing hydrotalcite layer sheet composition is prepared2+、Al3+A nitrate mixed solution; then, preparing a carboxyl POSS composite material; finally, Mg consisting of hydrotalcite-containing laminates2+、Al3+And (3) dripping the nitrate mixed solution into the carboxyl POSS composite material solution, aging and drying to obtain the flame-retardant magnesium aluminum hydrotalcite/POSS composite material. The preparation method has simple process, low cost of used materials, no need of calcination, high temperature and other treatments, and reduced energy consumption and reaction cost; the prepared composite material has good thermal stability and smoke suppression performance, and the mechanical property of the composite material can be improved.
Description
Technical Field
The invention belongs to the field of preparation of flame-retardant nano composite materials, and particularly relates to a preparation method of a flame-retardant hydrotalcite/POSS nano composite material.
Technical Field
In recent years, hydrotalcite is widely used in polymer nanocomposites, because it has a very high tunability, and can significantly improve the flame retardant properties of polymers. Hydrotalcite is difficult to disperse uniformly and stably in a polymer matrix due to the size effect, strong hydrophilicity, strong affinity between hydroxide layers, and the like. Therefore, it is very necessary to organically modify the hydrotalcite before it is used as nanoparticles. To date, a number of organic modifiers have been successfully used to modify hydrotalcites.
Polyhedral oligomeric siloxane POSS is a well-defined class of nanostructured molecules containing a siliceous cage core and externally attached organic substituents. These three-dimensional nanoclusters follow Rn(SiO1.5)nWhen the apex (R) is included, the diameter of the compound is 1 to 3 nm.The siloxane cages in POSS provide a thermally and chemically robust framework, while the organic functions can be chemically modified in a controlled manner, making POSS a promising class of nanoscale building blocks for advanced functional nanomaterials. Unlike traditional organic compounds, POSS are odorless and environmentally friendly because they do not release volatile organic components. It has been reported that acid groups such as-COOH have been successfully introduced into POSS structures, making it possible to use POSS as an ionic intercalator. Therefore, the carboxyl POSS is expected to improve the thermal stability and the fire resistance when used for modifying hydrotalcite.
Disclosure of Invention
The invention aims to provide a preparation method of a flame-retardant magnesium aluminum hydrotalcite/carboxyl POSS composite material, and solves the problems of poor dispersibility and insufficient thermal stability of hydrotalcite in the composite material.
In order to solve the problems, the invention adopts the technical scheme that:
the preparation method of the magnesium-aluminum flame-retardant hydrotalcite/carboxyl POSS composite material comprises the following specific steps:
the following quantities are in parts by mass:
the method comprises the following steps: firstly, weighing 4-10 parts of Mg (NO)3)2·6H2O, 2-5 parts of Al (NO)3)3·9H2Dissolving O in 20-50 parts of deionized water to obtain Mg containing hydrotalcite laminate2+、Al3+The nitrate mixed solution is marked as A;
step two: adding 0.32 part of Sodium Dodecyl Sulfate (SDS) and 40 parts of distilled water, heating the mixture in a water bath to 60 ℃, adding 0.13 part of vinyl POSS (POSS-Vi), stirring and reacting for 1.5 hours, adding 3 batches of 13.15 parts of methacrylic acid (MAA) and an initiator aqueous solution (1.92 g of ammonium persulfate APS and 0.48g of sodium bisulfite RH are respectively dissolved in distilled water with the mass being 10 times of that of the mixture), reacting for 3.5 hours at constant temperature, and naturally cooling to room temperature to obtain the carboxyl POSS composite material. Weighing 3-7 parts of synthesized carboxyl POSS, and dissolving in 20-50 parts of deionized water to obtain a solution B;
step three: dropping the solution A prepared in the step one into the solution B prepared in the step two under the protection of inert gas at 80 ℃, continuously and violently stirring, adjusting the pH of the solution to 10 by using a NaOH solution, continuing stirring for 1 hour after the dropping is finished, putting the obtained solution into an 80 ℃ oven, aging for 10 hours, washing and centrifuging by using deionized water until the pH of a supernatant is neutral, and drying a filter cake in vacuum at 80 ℃ for 4 hours to obtain the flame-retardant magnesium-aluminum hydrotalcite/POSS composite material.
In the first step, the Mg2+、Al3+Mg of nitrate mixed solution2+、Al3+The molar ratio is 3: 1.
and in the second step, the carboxyl POSS is prepared by taking vinyl trimethoxy silane as a raw material through a hydrolytic condensation reaction.
In the third step, the inert gas is nitrogen.
The flame-retardant magnesium-aluminum hydrotalcite/POSS composite material is prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation method of the flame-retardant magnesium aluminum hydrotalcite/carboxyl POSS composite material is simple in process, low in cost of the used materials and capable of meeting the environment-friendly requirement; and the treatment such as calcination, high temperature and the like is not needed, so that the energy consumption and the reaction cost are reduced.
2. The prepared carboxyl POSS has a large number of carboxyl functional groups, and can well improve the agglomeration phenomenon of hydrotalcite and enable the composite material to be better dispersed.
3. The flame-retardant magnesium-aluminum hydrotalcite/carboxyl POSS composite material is prepared by using the special structural composition of hydrotalcite and POSS, so that the thermal stability and smoke suppression of the composite material are improved, and the mechanical property of the composite material can be improved.
Drawings
FIG. 1 is an XRD test of the flame-retardant magnesium aluminum hydrotalcite/carboxyl POSS composite material prepared in example 5;
FIG. 2 is an infrared detection of the flame-retardant magnesium aluminum hydrotalcite/carboxyl POSS composite material prepared in example 5;
FIG. 3 shows TEM results of the flame-retardant magnesium aluminum hydrotalcite/carboxyl POSS composite material prepared in example 5.
Detailed Description
The present invention is described in detail below with reference to examples, which are provided for further illustration of the present invention and are not to be construed as limiting the scope of the present invention.
The preparation method of the flame-retardant magnesium aluminum hydrotalcite/carboxyl POSS composite material comprises the following specific steps: the following amounts are in parts by mass:
the method comprises the following steps: the method comprises the following steps: firstly, weighing 4-10 parts of Mg (NO)3)2·6H2O, 2-5 parts of Al (NO)3)3·9H2Dissolving O in 20-50 parts of deionized water to obtain Mg containing hydrotalcite laminate2+、Al3+The nitrate mixed solution was designated as A.
Step two: firstly, 0.32 part of Sodium Dodecyl Sulfate (SDS) and 40 parts of distilled water are added into a 150mL three-neck flask provided with a stirrer and a condensing device, the temperature is raised to 60 ℃ by water bath, 0.13 part of vinyl POSS (POSS-Vi) is added, stirring reaction is carried out for 1.5h, then 13.15 parts of methacrylic acid (MAA) and initiator aqueous solution (1.92 parts of ammonium persulfate and 0.48 part of sodium bisulfite RH are respectively dissolved by 10 times of distilled water) are added into 3 batches, and after constant temperature reaction is carried out for 3.5 h, natural cooling is carried out to room temperature, thus obtaining the carboxyl POSS composite material. 3-7 parts of the synthesized carboxyl POSS are weighed and dissolved in 20-50 parts of deionized water, and the obtained solution is marked as B.
Step three: dropping the solution A into the solution B under the protection of inert gas at 80 ℃, continuously and violently stirring, adjusting the pH of the solution to be about 10 by using a NaOH solution, continuing stirring for 1h after the dropping is finished, aging the obtained solution in an oven at 80 ℃ for 10 h, washing and centrifuging by using deionized water until the pH of a supernatant is neutral, and drying a filter cake in vacuum at 80 ℃ for 4h to obtain the magnesium-aluminum hydrotalcite/carboxyl POSS composite material.
In the step one, Mg in the prepared solution A2+、Al3+The molar ratio is 3: 1.
in the second step, the carboxyl POSS is prepared by taking vinyl trimethoxy silane as a raw material through a hydrolytic condensation reaction.
In the third step, the inert gas is used under the condition of nitrogen atmosphere.
Example 1
The method comprises the following steps: first, 4.6 parts of Mg (NO) are weighed3)2·6H2O, 2.3 parts of Al (NO)3)3·9H2Dissolving O in 24 parts of deionized water, and obtaining Mg containing hydrotalcite laminate2+、Al3+The nitrate mixed solution was designated as A.
Step two: firstly, 0.32 part of Sodium Dodecyl Sulfate (SDS) and 40 parts of distilled water are added into a 150mL three-neck flask provided with a stirrer and a condensing device, the temperature is raised to 60 ℃ by water bath, 0.13 part of vinyl POSS (POSS-Vi) is added, stirring reaction is carried out for 1.5h, then 13.15 parts of methacrylic acid MAA and initiator aqueous solution (1.92 parts of ammonium persulfate APS and 0.48 part of sodium bisulfite RH are respectively dissolved by 10 times of distilled water) are added into 3 batches, and after constant temperature reaction is carried out for 3.5 h, natural cooling is carried out to room temperature, thus obtaining the carboxyl POSS composite material. 3.02 parts of the synthesized carboxy POSS were weighed out and dissolved in 24 parts of deionized water, and the resulting solution was designated B.
Step three: dropping the solution A into the solution B under the protection of inert gas at 80 ℃, continuously and violently stirring, adjusting the pH of the solution to be about 10 by using a NaOH solution, continuing stirring for 1h after the dropping is finished, aging the obtained solution in an oven at 80 ℃ for 10 h, washing and centrifuging by using deionized water until the pH of a supernatant is neutral, and drying a filter cake in vacuum at 80 ℃ for 4h to obtain the magnesium-aluminum hydrotalcite/carboxyl POSS composite material.
Example 2
The method comprises the following steps: first, 5.6 parts of Mg (NO) are weighed3)2·6H2O, 2.6 parts of Al (NO)3)3·9H2Dissolving O in 28 parts of deionized water, and obtaining Mg containing hydrotalcite laminate2+、Al3+The nitrate mixed solution was designated as A.
Step two: firstly, 0.32 part of Sodium Dodecyl Sulfate (SDS) and 40 parts of distilled water are added into a 150mL three-neck flask provided with a stirrer and a condensing device, the temperature is raised to 60 ℃ by water bath, 0.13 part of vinyl POSS (POSS-Vi) is added, stirring reaction is carried out for 1.5h, then 13.15 parts of methacrylic acid MAA and initiator aqueous solution (1.92 parts of ammonium persulfate APS and 0.48 part of sodium bisulfite RH are respectively dissolved by 10 times of distilled water) are added into 3 batches, and after constant temperature reaction is carried out for 3.5 h, natural cooling is carried out to room temperature, thus obtaining the carboxyl POSS composite material. 3.41 parts of the synthesized carboxy POSS were weighed into 28 parts of deionized water and the resulting solution was designated B.
Step three: dropping the solution A into the solution B under the protection of inert gas at 80 ℃, continuously and violently stirring, adjusting the pH of the solution to be about 10 by using a NaOH solution, continuing stirring for 1h after the dropping is finished, aging the obtained solution in an oven at 80 ℃ for 10 h, washing and centrifuging by using deionized water until the pH of a supernatant is neutral, and drying a filter cake in vacuum at 80 ℃ for 4h to obtain the magnesium-aluminum hydrotalcite/carboxyl POSS composite material.
Example 3
The method comprises the following steps: first, 6.5 parts of Mg (NO) are weighed3)2·6H2O, 3.2 parts of Al (NO)3)3·9H2Dissolving O in 33 parts of deionized water, and obtaining Mg containing hydrotalcite laminate2+、Al3+The nitrate mixed solution was designated as A.
Step two: firstly, 0.32 part of Sodium Dodecyl Sulfate (SDS) and 40 parts of distilled water are added into a 150mL three-neck flask provided with a stirrer and a condensing device, the temperature is raised to 60 ℃ by water bath, 0.13 part of vinyl POSS (POSS-Vi) is added, stirring reaction is carried out for 1.5h, then 13.15 parts of methacrylic acid MAA and initiator aqueous solution (1.92 parts of ammonium persulfate APS and 0.48 part of sodium bisulfite RH are respectively dissolved by 10 times of distilled water) are added into 3 batches, and after constant temperature reaction is carried out for 3.5 h, natural cooling is carried out to room temperature, thus obtaining the carboxyl POSS composite material. 4.16 parts of the synthesized carboxy POSS were weighed out and dissolved in 34 parts of deionized water, and the resulting solution was designated B.
Step three: dropping the solution A into the solution B under the protection of inert gas at 80 ℃, continuously and violently stirring, adjusting the pH of the solution to be about 10 by using a NaOH solution, continuing stirring for 1h after the dropping is finished, aging the obtained solution in an oven at 80 ℃ for 10 h, washing and centrifuging by using deionized water until the pH of a supernatant is neutral, and drying a filter cake in vacuum at 80 ℃ for 4h to obtain the magnesium-aluminum hydrotalcite/carboxyl POSS composite material.
Example 4
The method comprises the following steps: first, 7.7 parts of Mg (NO) are weighed3)2·6H2O, 3.8 parts of Al (NO)3)3·9H2Dissolving O in 42 parts of deionized water, and obtaining Mg containing hydrotalcite laminate2+、Al3+The nitrate mixed solution was designated as A.
Step two: firstly, 0.32 part of Sodium Dodecyl Sulfate (SDS) and 40 parts of distilled water are added into a 150mL three-neck flask provided with a stirrer and a condensing device, the temperature is raised to 60 ℃ by water bath, 0.13 part of vinyl POSS (POSS-Vi) is added, stirring reaction is carried out for 1.5h, then 13.15 parts of methacrylic acid MAA and initiator aqueous solution (1.92 parts of ammonium persulfate APS and 0.48 part of sodium bisulfite RH are respectively dissolved by 10 times of distilled water) are added into 3 batches, and after constant temperature reaction is carried out for 3.5 h, natural cooling is carried out to room temperature, thus obtaining the carboxyl POSS composite material. 5.19 parts of the synthesized carboxy POSS were weighed out and dissolved in 42 parts of deionized water, and the resulting solution was designated B.
Step three: dropping the solution A into the solution B under the protection of inert gas at 80 ℃, continuously and violently stirring, adjusting the pH of the solution to be about 10 by using a NaOH solution, continuing stirring for 1h after the dropping is finished, aging the obtained solution in an oven at 80 ℃ for 10 h, washing and centrifuging by using deionized water until the pH of a supernatant is neutral, and drying a filter cake in vacuum at 80 ℃ for 4h to obtain the magnesium-aluminum hydrotalcite/carboxyl POSS composite material.
Example 5
The method comprises the following steps: first, 9.6 parts of Mg (NO) are weighed3)2·6H2O, 4.7 parts of Al (NO)3)3·9H2Dissolving O in 50mL of deionized water, and dissolving the obtained Mg containing hydrotalcite laminate2+、Al3+The nitrate mixed solution was designated as A.
Step two: firstly, 0.32 part of Sodium Dodecyl Sulfate (SDS) and 40 parts of distilled water are added into a 150mL three-neck flask provided with a stirrer and a condensing device, the temperature is raised to 60 ℃ by water bath, 0.13 part of vinyl POSS (POSS-Vi) is added, stirring reaction is carried out for 1.5h, then 13.15 parts of methacrylic acid MAA and initiator aqueous solution (1.92 parts of ammonium persulfate APS and 0.48 part of sodium bisulfite RH are respectively dissolved by 10 times of distilled water) are added into 3 batches, and after constant temperature reaction is carried out for 3.5 h, natural cooling is carried out to room temperature, thus obtaining the carboxyl POSS composite material. 6.17 parts of the synthesized carboxy POSS were weighed into 50 parts of deionized water and the resulting solution was designated B.
Step three: dropping the solution A into the solution B under the protection of inert gas at 80 ℃, continuously and violently stirring, adjusting the pH of the solution to be about 10 by using a NaOH solution, continuing stirring for 1h after the dropping is finished, aging the obtained solution in an oven at 80 ℃ for 10 h, washing and centrifuging by using deionized water until the pH of a supernatant is neutral, and drying a filter cake in vacuum at 80 ℃ for 4h to obtain the magnesium-aluminum hydrotalcite/carboxyl POSS composite material.
In order to show that the magnalium hydrotalcite/carboxyl POSS composite material is successfully prepared, the composite material prepared in the example 5 is subjected to detection such as infrared detection, XRD detection and the like. The XRD detection result is shown in figure 1, the magnalium hydrotalcite/carboxyl POSS composite material has characteristic crystal face diffraction peak of hydrotalcite, and weak diffraction peak appears at higher 2 theta, which shows that the crystal form regularity is reduced. The (003) or (006) diffraction peak position thereof is shifted toward a low 2 theta angle with respect to hydrotalcite, and the interlayer distance is also increased. There is a weaker diffraction peak at 2 θ =6.84 °, which is likely the peak of the carboxylate, indicating intercalation of POSS into the interlayer to form intercalation products. The infrared detection result is shown in FIG. 2, at 1213.1cm-1And 1564.2cm-1The vibration peak of the Si-O-Si framework and the stretching vibration peak of the carboxyl can be respectively seen, and the peak position of the carboxyl is shifted, which indicates that the carboxyl in the object and the hydroxyl of the laminate are interacted.
The TEM detection result is shown in FIG. 3, obvious lattice fringes of POSS and hydrotalcite can be observed, and the hydrotalcite is uniformly dispersed, which indicates that the POSS intercalation modified hydrotalcite composite material is successfully prepared.
The above description is only a preferred embodiment of the present invention, and is not limited to the embodiment, and the protection scope of the present invention is not limited thereto.
Claims (6)
1. The preparation method of the flame-retardant magnesium aluminum hydrotalcite/carboxyl POSS composite material is characterized by comprising the following steps of:
the method comprises the following specific steps of:
the method comprises the following steps: firstly, weighing 4-10 parts of Mg (NO)3)2·6H2O, 2-5 parts of Al (NO)3)3·9H2Dissolving O in 20-50 parts of deionized water to obtain Mg containing hydrotalcite laminate2+、Al3+The nitrate mixed solution is marked as A;
step two: firstly, adding 0.32 part of Sodium Dodecyl Sulfate (SDS) and 40 parts of distilled water into a 150mL three-neck flask provided with a stirrer and a condensing device, heating the mixture to 60 ℃ in a water bath, adding 0.13 part of vinyl POSS, stirring and reacting for 1.5h, adding 13.15 parts of methacrylic acid MAA and an initiator aqueous solution into 3 batches, reacting for 3.5 h at a constant temperature, and naturally cooling to room temperature to obtain a carboxyl POSS composite material;
weighing 3-7 parts of synthesized carboxyl POSS, and dissolving in 20-50 parts of deionized water to obtain a solution B;
step three: dropping the solution A into the solution B under the protection of inert gas at 80 ℃, continuously and violently stirring, adjusting the pH of the solution to 10 by using a NaOH solution, continuing stirring for 1h after the dropping is finished, aging the obtained solution in an oven at 80 ℃ for 10 h, washing and centrifuging by using deionized water until the pH of a supernatant is neutral, and drying a filter cake in vacuum at 80 ℃ for 4h to obtain the magnesium-aluminum hydrotalcite/carboxyl POSS composite material.
2. The preparation method of the flame-retardant magnesium aluminum hydrotalcite/carboxyl POSS composite material according to claim 1, which is characterized in that:
in the step one, Mg in the prepared solution A2+、Al3+The molar ratio is 3: 1.
3. the preparation method of the flame-retardant magnesium aluminum hydrotalcite/carboxyl POSS composite material according to claim 2, which is characterized in that:
in the second step, 1.92 parts of ammonium persulfate APS and 0.48 part of sodium bisulfite RH are dissolved in 10 times of distilled water by mass respectively.
4. The preparation method of the flame-retardant magnesium aluminum hydrotalcite/carboxyl POSS composite material according to claim 3, wherein the preparation method comprises the following steps:
in the second step, the vinyl POSS is prepared by taking vinyl trimethoxy silane as a raw material through a hydrolytic condensation reaction.
5. The preparation method of the flame-retardant magnesium aluminum hydrotalcite/carboxyl POSS composite material according to claim 4, wherein the preparation method comprises the following steps:
in the third step, the inert gas used is nitrogen.
6. The preparation method of any one of claims 1 to 5, wherein the flame retardant magnesium aluminum hydrotalcite/carboxyl POSS composite material is prepared.
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| CN107868249A (en) * | 2017-11-30 | 2018-04-03 | 陕西科技大学 | Carboxyl-functional cage-type silsesquioxane and its method based on substitution reaction synthesis |
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