CN113150440B - Preparation method of flame-retardant polypropylene - Google Patents
Preparation method of flame-retardant polypropylene Download PDFInfo
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Abstract
The invention discloses a preparation method of flame-retardant polypropylene. The method is characterized in that phytic acid and beta-cyclodextrin are reacted, then beta-cyclodextrin intercalation LDH is prepared by modification through a coprecipitation method, and finally an LDH flame-retardant polypropylene composite material is prepared in a melt blending mode. The method is environment-friendly and efficient, and is particularly suitable for the flame retardant requirement of polypropylene. The invention uses simple ion exchange reaction to mix plant-acidified beta-cyclodextrin with NO 3 ‑ The nickel-aluminum LDH is reacted, and the thermal stability of the composite is obviously better than that of NO 3 ‑ The type nickel aluminum LDH has obviously enlarged LDH layer spacing and obviously improved dispersity in the PP base material. Can obviously improve the flame retardant property of PP and has important significance.
Description
Technical Field
The invention relates to a preparation method of flame-retardant polypropylene, in particular to a method for preparing flame-retardant polypropylene from LDH modified by phytic acid and beta-cyclodextrin, belonging to the field of flame-retardant engineering.
Background
Polypropylene is a polymer obtained by addition polymerization of propylene, and has a large market share as one of five general-purpose plastics. In 2018 only, the yield of polypropylene in five general-purpose plastics reaches 34%. Polypropylene has many advantages as a thermoplastic material. It is easy to process, low in cost, good in mechanical property, and can resist corrosion of acid, alkali, salt solution and organic solvent at 80 deg.C. Therefore, polypropylene has a very wide application in daily life, from daily necessities to medical instruments to automobile accessories and the like, and polypropylene is ubiquitous. In a certain sense, researchers think that polypropylene is an ideal choice for replacing other general-purpose plastics, and a feasible method is provided for solving the recycling problem of different high polymer materials.
Polypropylene, however, has a fatal weakness and is flammable. The melting point of the polypropylene is 165 ℃, the polypropylene begins to soften at 155 ℃, and the effective working temperature is-30-140 ℃. Polypropylene has a high flammability and burns quickly after ignition. During combustion, polypropylene can generate toxic gases such as dense smoke, carbon monoxide and the like, and can cause potential safety hazards to the life safety of human beings along with molten droplets, so that certain applications with higher safety requirements cannot be met. How to improve the flame retardant property of polypropylene and inhibit smoke and molten drops is of great significance. Because the halogen flame retardant has great harm to the environment, the halogen-free flame retardant is mainly used for the flame retardance of the polypropylene at the present stage, wherein the phosphorus flame retardant can act in the same gas phase and solidification, but the flame retardant has certain toxicological effect and is easily volatilized to cause harm to human bodies in the environment; the metal hydroxide flame retardant can delay the thermal degradation speed of the high polymer, slow or inhibit the combustion of the high polymer, promote carbonization and suppress smoke, but the addition amount is large, so that the mechanical property of the polymer can be greatly reduced; LDH is regarded as an efficient flame retardant as an environment-friendly inorganic flame retardant, has a unique two-dimensional layered structure and adjustable chemical components, and particularly has high flame retardant performance and smoke suppression performance. However, LDHs are hydrophilic and hardly compatible with polypropylene substrates, and can be intercalated with surfactants or by modifying the LDH interlayer anions in order to improve the dispersibility of the LDH in polypropylene. Up to now, the appearance of cyclodextrins modified with phytic acid as a relevant process for LDH intercalation has not been seen.
Disclosure of Invention
In order to overcome the problems, the invention aims to provide a preparation method of flame-retardant polypropylene, in particular to a preparation method of plant acid modified beta-cyclodextrin as an LDH intercalation, which has simple process and low cost and can show excellent flame-retardant performance and smoke suppression and molten drop prevention performance when used for flame retardance of polypropylene.
A preparation method of flame-retardant polypropylene is characterized by comprising the following steps:
1) dissolving beta-cyclodextrin and sodium hydroxide in deionized water, placing the mixture in a three-neck flask, magnetically stirring the mixture uniformly, heating the mixture to 60-80 ℃, and connecting a reflux pipe and a thermometer to the three-neck flask to obtain a solution;
2) dropwise adding a certain amount of phytic acid into the solution obtained in the step 1) within 3 hours, and stirring and reacting the mixed solution for 4 hours at the temperature of 60-80 ℃ after complete dropwise addition to obtain a reaction solution;
3) completely cooling the reaction liquid obtained in the step 2) to room temperature, adjusting the pH value to be neutral by using hydrochloric acid, purifying the product by using a dialysis tube, obtaining a product by using a rotary evaporator, and drying the product in an oven at 80 ℃ for 12 hours to obtain a white solid, namely the phytic acid modified beta-cyclodextrin (PCD);
4) PCD and Ni (NO) obtained in the step 3) 3 ) 2 ·6H 2 0、Al(NO 3 ) 3 ·9H 2 Dissolving O in deionized water according to a certain proportion, placing the mixture in a three-necked flask, magnetically stirring the mixture uniformly, and heating the mixture to 60-80 ℃ to obtain a mixed solution;
5) dropwise adding an alkaline solution into the mixed solution obtained in the step 4) to adjust the pH value to be 9-11, stirring for 30 minutes, transferring the mixed solution into an oven at 80 ℃, and crystallizing for 18 hours to obtain a crystallized product;
6) removing supernatant of the crystallized product obtained in the step 5), washing the precipitate with deionized water to be neutral, centrifuging, and freeze-drying the green solid to obtain the PCD-LDH flame retardant;
7) and (3) melting and blending the PCD-LDH flame retardant obtained in the step 6) and polypropylene according to the mass ratio of 1:5, wherein the mixing temperature is 180 ℃, the mixing time is 2 minutes, and the rotating speed is 20 r/m, and the obtained mixed product is the flame-retardant polypropylene.
The beta-cyclodextrin,The molar mass ratio of the phytic acid to the sodium hydroxide is 1:4: 5; the concentration of the hydrochloric acid is 1 mol/L; MVCO of the dialysis tubing was 1000; the alkaline solution is sodium hydroxide solution with the concentration of 1 mol/L; ni (NO) 3 ) 2 ·6H 2 0、Al(NO 3 ) 3 ·9H 2 O, PCD in a ratio of 20:10: 3.
The rotating speed in the centrifugal process is 8000rpm, and the centrifugal time is 10 min.
Compared with the background art, the invention has the beneficial effects that:
the phytic acid and beta-cyclodextrin are used as raw materials, and the phytic acid modified beta-cyclodextrin is prepared by a coprecipitation method to be used as nickel-aluminum LDH serving as an intercalation and used as a flame retardant of polypropylene. The obtained LDH has larger interlayer spacing and higher thermal stability, and can have good dispersibility in a polypropylene substrate. In addition, due to the existence of phytic acid and beta-cyclodextrin, carbon chains of polypropylene can participate in carbonization reaction to promote char formation, and a compact carbon layer is formed on the surface of the polypropylene to play roles of smoke suppression and molten drop prevention; meanwhile, the phytic acid and the beta-cyclodextrin are both environment-friendly materials, and have no harm to the environment and human bodies.
Drawings
Figure 1 is a field emission Scanning Electron Microscope (SEM) image of the phytic acid modified β -cyclodextrin intercalated LDH (PCD-LDH) prepared in example 3.
Figure 2 is an X-ray diffraction (XRD) pattern of the phytic acid modified β -cyclodextrin intercalated LDH (PCD-LDH) prepared in example 3.
Detailed Description
The present invention is further illustrated by the following examples.
Example 1:
1) dissolving 0.02mol of beta-cyclodextrin and 0.1mol of sodium hydroxide in 45ml of deionized water, placing the mixture in a three-neck flask, magnetically stirring the mixture uniformly, and heating the mixture to 60 ℃; a reflux pipe and a thermometer are linked on the three-neck flask to obtain a solution;
2) dripping 0.08mol of phytic acid into the solution obtained in the step 1) within 3 hours, and stirring and reacting the mixed solution at 60 ℃ for 4 hours after complete dripping to obtain reaction liquid;
3) cooling the reaction liquid obtained in the step 2) to room temperature after complete reaction, adjusting the pH to be neutral by using hydrochloric acid with the concentration of 1mol/L, purifying the product by using a dialysis tube with MVCO of 1000, finally obtaining a product by using a rotary evaporator, and drying the product in an oven at 80 ℃ for 12 hours to obtain white solid, namely PCD;
4) 0.03mol PCD and 0.2mol Ni (NO) obtained in the step 3) 3 ) 2 ·6H 2 0、0.1molAl(NO 3 ) 3 ·9H 2 Dissolving O in 300ml of deionized water, placing the mixture in a three-necked flask, magnetically stirring the mixture uniformly, and heating the mixture to 60 ℃ to obtain a mixed solution;
5) dropwise adding a sodium hydroxide solution with the concentration of 1mol/L into the mixed solution obtained in the step 4) to adjust the pH value to 9, stirring for 30 minutes, transferring the mixed solution into an oven at 80 ℃, and crystallizing for 18 hours to obtain a crystallized product;
6) removing supernatant of the crystallized product obtained in the step 5), taking precipitate, washing the precipitate to be neutral by using deionized water, centrifuging at the rotating speed of 8000rpm for 10min, and freeze-drying the green solid to obtain PCD-LDH;
7) and (3) melting and blending the PCD-LDH flame retardant obtained in the step 6) and polypropylene according to the mass ratio of 1:5, wherein the mixing temperature is 180 ℃, the mixing time is 2 minutes, the rotating speed is 20 r/m, and the final mixed product is the flame-retardant polypropylene composite material.
Example 2:
1) dissolving 0.02mol of beta-cyclodextrin and 0.1mol of sodium hydroxide in 45ml of deionized water, placing the mixture in a three-neck flask, magnetically stirring the mixture uniformly, and heating the mixture to 80 ℃; a reflux pipe and a thermometer are linked on the three-neck flask to obtain a solution;
2) dripping 0.08mol of phytic acid into the solution obtained in the step 1) within 3 hours, and stirring and reacting the mixed solution at 80 ℃ for 4 hours after complete dripping to obtain reaction liquid;
3) cooling the reaction liquid obtained in the step 2) to room temperature after complete reaction, adjusting the pH to be neutral by using hydrochloric acid with the concentration of 1mol/L, purifying the product by using a dialysis tube with MVCO of 1000, finally obtaining a product by using a rotary evaporator, and drying the product in an oven at 80 ℃ for 12 hours to obtain white solid, namely PCD;
4) will be provided with0.03mol PCD and 0.2mol Ni (NO) obtained in step 3) 3 ) 2 ·6H 2 0、0.1molAl(NO 3 ) 3 ·9H 2 Dissolving O in 300ml of deionized water, placing the mixture in a three-necked flask, magnetically stirring the mixture uniformly, and heating the mixture to 80 ℃ to obtain a mixed solution;
5) dropwise adding a sodium hydroxide solution with the concentration of 1mol/L into the mixed solution obtained in the step 4), adjusting the pH value to 11, stirring for 30 minutes, transferring the mixed solution into an oven at 80 ℃, and crystallizing for 18 hours to obtain a crystallized product;
6) removing the supernatant of the crystallized product obtained in the step 5), washing the precipitate with deionized water to be neutral, centrifuging at the rotating speed of 8000rpm for 10min, and freeze-drying the green solid to obtain PCD-LDH;
7) and (3) melting and blending the PCD-LDH flame retardant obtained in the step 6) and polypropylene according to the mass ratio of 1:5, wherein the mixing temperature is 180 ℃, the mixing time is 2 minutes, the rotating speed is 20 r/m, and the final mixed product is the flame-retardant polypropylene composite material.
Example 3:
1) dissolving 0.02mol of beta-cyclodextrin and 0.1mol of sodium hydroxide in 45ml of deionized water, placing the mixture in a three-neck flask, magnetically stirring the mixture uniformly, and heating the mixture to 70 ℃; a reflux pipe and a thermometer are linked on the three-neck flask to obtain a solution;
2) dripping 0.08mol of phytic acid into the solution obtained in the step 1) within 3 hours, and stirring and reacting the mixed solution at 70 ℃ for 4 hours after complete dripping to obtain reaction liquid;
3) cooling the reaction liquid obtained in the step 2) to room temperature after complete reaction, adjusting the pH to be neutral by using hydrochloric acid with the concentration of 1mol/L, purifying the product by using a dialysis tube with MVCO of 1000, finally obtaining a product by using a rotary evaporator, and drying the product in an oven at 80 ℃ for 12 hours to obtain white solid, namely PCD;
4) mixing the 0.03mol PCD obtained in the step 3) and 0.2mol Ni (NO) 3 ) 2 ·6H 2 0、0.1molAl(NO 3 ) 3 ·9H 2 Dissolving O in 300ml of deionized water, placing the mixture in a three-necked flask, magnetically stirring the mixture uniformly, and heating the mixture to 70 ℃ to obtain a mixed solution;
5) dropwise adding a sodium hydroxide solution with the concentration of 1mol/L into the mixed solution obtained in the step 4), adjusting the pH value to 10, stirring for 30 minutes, transferring the mixed solution into an oven with the temperature of 80 ℃, and crystallizing for 18 hours to obtain a crystallized product;
6) removing supernatant of the crystallized product obtained in the step 5), taking precipitate, washing the precipitate to be neutral by using deionized water, centrifuging at the rotating speed of 8000rpm for 10min, and freeze-drying the green solid to obtain PCD-LDH;
7) and (3) melting and blending the PCD-LDH flame retardant obtained in the step 6) and polypropylene according to the mass ratio of 1:5, wherein the mixing temperature is 180 ℃, the mixing time is 2 minutes, the rotating speed is 20 r/m, and the final mixed product is the flame-retardant polypropylene composite material.
The limiting oxygen index of the flame-retardant polypropylene composite material taking the three phytic acid modified beta-cyclodextrin intercalated LDH prepared in the examples 1, 2 and 3 as the flame retardant is measured. Table 1 shows the characterization results of the flame retardant polypropylene composite material using three phytic acid modified β -cyclodextrin intercalated LDHs prepared in example 1, example 2, and example 3 as flame retardants. As can be seen from the data in Table 1, the limit oxygen indexes of the flame-retardant polypropylene composite material (a), (b) and (c) which takes the phytic acid modified beta-cyclodextrin intercalated LDH obtained by the preparation method as the flame retardant can reach 23.3, 23.8 and 24.5.
TABLE 1
As shown in fig. 1, as can be seen from the field emission scanning electron micrograph of the phytic acid modified β -cyclodextrin intercalated LDH prepared in example 3, the dimensions thereof are micron-sized, the dispersion is uniform, and due to the abundant hydroxyl groups on the surface, a slight mutual attraction phenomenon occurs locally.
As shown in fig. 2, from the X-ray diffraction (XRD) pattern of the phytic acid modified β -cyclodextrin intercalated LDH prepared in example 3, it can be seen that the prepared LDH has higher crystallinity and larger interlayer spacing.
The foregoing lists merely illustrate specific embodiments of the invention. The present invention is not limited to the above embodiments, and many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (1)
1. A preparation method of flame-retardant polypropylene is characterized by comprising the following steps:
1) dissolving beta-cyclodextrin and sodium hydroxide in deionized water, placing the mixture in a three-neck flask, magnetically stirring the mixture uniformly, heating the mixture to 60-80 ℃, and connecting a reflux pipe and a thermometer to the three-neck flask to obtain a solution;
2) dropwise adding a certain amount of phytic acid into the solution obtained in the step 1) within 3 hours, wherein the molar ratio of beta-cyclodextrin, phytic acid and sodium hydroxide is 1:4:5, and stirring and reacting the mixed solution at 60-80 ℃ for 4 hours after complete dropwise addition to obtain a reaction solution;
3) completely cooling the reaction liquid obtained in the step 2) to room temperature, adjusting the pH to be neutral by hydrochloric acid, wherein the concentration of the hydrochloric acid is 1mol/L, purifying the product by a dialysis tube, wherein the MVCO (model view controller) of the dialysis tube is 1000, obtaining a product by a rotary evaporator, and drying the product in an oven at 80 ℃ for 12 hours to obtain white solid, namely PCD;
4) PCD and Ni (NO) obtained in the step 3) 3 ) 2 ·6H 2 O、Al(NO 3 ) 3 ·9H 2 Dissolving O in deionized water according to the molar ratio of 3:20:10, placing the mixture in a three-neck flask, magnetically stirring the mixture uniformly, and heating the mixture to 60-80 ℃ to obtain a mixed solution;
5) dropwise adding an alkaline solution into the mixed solution obtained in the step 4) to adjust the pH value to be 9-11, wherein the alkaline solution is a sodium hydroxide solution with the concentration of 1mol/L, stirring for 30 minutes, transferring the mixed solution into an oven at 80 ℃, and crystallizing for 18 hours to obtain a crystallized product;
6) removing supernatant of the crystallized product obtained in the step 5), washing the precipitate with deionized water to be neutral, and freeze-drying the green solid after centrifugation, wherein the rotation speed of the centrifugation process is 8000rpm and the time is 10min, so as to obtain the PCD-LDH flame retardant;
7) and (3) melting and blending the PCD-LDH flame retardant obtained in the step 6) and polypropylene according to the mass ratio of 1:5, wherein the mixing temperature is 180 ℃, the mixing time is 2 minutes, the rotating speed is 20 r/m, and the obtained mixing product is the flame-retardant polypropylene.
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