CN111303592B - Preparation method of phosphorus-aluminum type halogen-free low-smoke intrinsic flame-retardant IFR-PET - Google Patents
Preparation method of phosphorus-aluminum type halogen-free low-smoke intrinsic flame-retardant IFR-PET Download PDFInfo
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- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
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Abstract
The invention discloses a preparation method of phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET, which comprises the steps of heating and dissolving organic phosphonic acid in distilled water, adding aluminum hydroxide, stirring and reacting at 80-100 ℃ for 6-10h, carrying out reduced pressure distillation and drying to obtain a white solid, namely functionalized aluminum hydroxide; terephthalic acid, ethylene glycol and functional aluminum hydroxide are taken as raw materials, sd is taken as 2 O 3 Taking nitrogen as a protective gas as a catalyst, firstly carrying out esterification reaction for 4 to 7 hours at 0.2 to 0.35Mpa and 235 to 250 ℃, reacting for 0.5 to 1h at 95 to 105 ℃ under normal pressure after the esterification reaction is finished, then carrying out semi-polycondensation reaction for 0.5 to 1h at 250 to 270 ℃ under a semi-vacuum state, carrying out full-polycondensation reaction for 3 to 5h at 275 to 280 ℃ under a full-vacuum state, introducing nitrogen for discharging, granulating and drying to obtain the phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET. The composite material has excellent flame retardant and smoke suppression properties due to good compatibility of HAFR with PET matrix and formation of a dense continuous carbon layer during combustion.
Description
Technical Field
The invention relates to a preparation method of halogen-free low-smoke intrinsic flame retardant IFR-PET, in particular to a preparation method of phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET, belonging to the technical field of flame retardant materials and the technical field of high polymer materials.
Background
Polyethylene terephthalate (PET) is a thermoplastic polymer material. Due to good thermochemical stability, excellent mechanical properties, corrosion resistance and good textile property, the fiber is widely applied to the fields of packaging, electronic and electric appliances, buildings, automobiles and the like. Despite the above advantages, PET is extremely flammable, mainly consisting of three elements, hydrocarbon and oxygen, and is accompanied by severe melting and dropping during burning, and rapidly spreads after ignition, releasing a large amount of heat and toxic gases. Seriously threatens the life and property safety of people and limits the wide application of PET. Flame retardant modification of polyesters has therefore raised a high level of interest to the research, manufacturer, consumer and government sectors.
Flame retardants can be classified into reactive type and additive type according to their addition method. Addition type: the flame retardant does not participate in the polymerization process of the polymer, is simply blended with the polymer to achieve the flame retardant property, has low cost and easy industrial production, but seriously damages the mechanical property of the polymer and has low flame retardancy. Reaction type: the flame retardant participates in the polymerization of the polymer, the polymer is connected to the flame retardant before and after the esterification of the flame retardant, the flame retardant is high in flame retardance, small in addition amount and small in influence on mechanical properties.
Flame retardants are often classified as organic flame retardants according to their type. The organic flame retardant mainly comprises halogen flame retardant, phosphorus flame retardant and halogen-containing flame retardant, although the halogen-containing flame retardant has high-efficiency flame retardant effect, a large amount of smoke, toxic gas and biological deposition can be released during combustion of halogen-containing materials, the health of human beings is seriously harmed, and environmental pollution is caused, so that the research on the halogen-free, low-smoke, low-toxicity and environment-friendly flame retardant is a hotspot in recent years. The inorganic flame retardant mainly comprises metal oxides (magnesium hydroxide, aluminum hydroxide, magnesium oxide and the like), and the material containing the inorganic flame retardant releases bound water in the combustion process to reduce the surface temperature of the material. However, inorganic particles are difficult to disperse uniformly in organic polymers, and are easy to aggregate, so that the mechanical properties are seriously influenced, and a large amount of filling is required for achieving the flame retardant effect. Therefore, it is necessary to study the surface modification, select a surface modifier having excellent properties, improve the surface activity of particles, improve the dispersibility, and further improve the flame retardancy.
Disclosure of Invention
The invention aims to solve the technical problems and provides a preparation method of phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET.
1. Preparation of phosphorus-aluminum type halogen-free low-smoke intrinsic flame-retardant IFR-PET
The invention discloses a preparation method of phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET, which comprises the following steps:
(1) Heating and dissolving organic phosphonic acid in distilled water, adding aluminum hydroxide, stirring and reacting at 80-100 ℃ for 6-10 h, carrying out reduced pressure distillation, and drying to obtain a white solid, namely functionalized aluminum Hydroxide (HAFR). Wherein the organic phosphonic acid is at least one of phosphorus element-containing organic phosphonic acids such as bis (4-carboxyphenyl) phenylphosphine oxide, phenylphosphonic acid, 2-carboxyethyl (phenyl) phosphinic acid, hydroxyethylidene diphosphonic acid, methylphosphonic acid and the like; the mass ratio of the aluminum hydroxide to the organic phosphonic acid is 1 to 1; the drying temperature is 60 to 80 ℃, and the drying time is 6 to 10 hours.
(2) Terephthalic acid, ethylene glycol and functional aluminum hydroxide are taken as raw materials, sd is taken as 2 O 3 Taking nitrogen as a catalyst, firstly carrying out esterification reaction for 4 to 7 hours at 0.2 to 0.35Mpa and 235 to 250 ℃, reacting for 0.5 to 1h at 95 to 105 ℃ and normal pressure after the esterification reaction is finished, then carrying out semi-polycondensation reaction for 0.5 to 1h at 250 to 270 ℃ in a semi-vacuum state, then carrying out full polycondensation reaction for 3 to 5h at 275 to 280 ℃ in a full-vacuum state, introducing nitrogen for discharging, granulating and drying to obtain the phosphorus-aluminum type low-smoke halogen-free productAnd (3) characterizing flame retardant IFR-PET. Wherein the mass ratio of the ethylene glycol to the terephthalic acid to the functionalized aluminum hydroxide is 1.033 to 1.091; sd 2 O 3 The mass ratio of the terephthalic acid to the terephthalic acid is 1.0001 to 1; the drying temperature is 60 to 80 ℃, and the drying time is 6 to 10 hours.
2. Structural performance of phosphorus-aluminum type halogen-free low-smoke intrinsic flame-retardant IFR-PET
The structure and performance of the phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET are analyzed and explained by taking the case that the organic phosphoric acid selects the hydroxyethylidene diphosphonic acid as an example.
FIG. 1 is a plot of the infrared absorption spectra of functionalized aluminum Hydroxide (HAFR), aluminum hydroxide (ATH), and hydroxyethylidene diphosphonic acid (HEDP). As can be seen from FIG. 1, 3620cm -1 OH as aluminium hydroxide - Peak of stretching vibration of 1142cm -1 Characteristic absorption peak of P = O, 1456cm -1 Is a characteristic absorption peak of P-C, 1060cm -1 、920cm -1 Is a characteristic absorption peak of P-O-C, and 3616cm -1 The vibration peak of the hydroxyl group shrinkage of the aluminum hydroxide is obviously weakened but not completely disappeared, which indicates that the product contains hydroxyl groups. The successful synthesis of the functionalized aluminum hydroxide can be judged according to the infrared spectrogram.
FIG. 2 is an XRD pattern of functionalized aluminum Hydroxide (HAFR) and aluminum hydroxide (ATH). It can be observed from the XRD curve that the position of the diffraction peak of the functionalized aluminum hydroxide is identical to that of the diffraction peak of the aluminum hydroxide, but the intensity and width of the peak are significantly weakened due to the smaller particle size of the functionalized aluminum hydroxide.
FIG. 3 is a graph of the heat release rate of phosphorus-aluminum type halogen-free low smoke intrinsic flame retardant IFR-PET. In the figure, a, b, c and d are respectively phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET with the dosage of HAFR accounting for 0 percent, 3 percent, 5 percent and 7 percent of the mass of the terephthalic acid. It can be seen from the figure that pure PET has a high peak heat release rate (p-HRR) of 953.7KW/m 2 When the dosage of the HAFR is 3 percent, 5 percent and 7 percent of the mass of the terephthalic acid, the peak value of the heat release rate of the phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET is respectively reduced to 655.8 kW/m 2 、585.1k3%W/m 2 And 556.2KW/m 2 When the amount of HAFR is 7 mass% based on the amount of terephthalic acid used% of the total weight of the phosphorus-aluminum type halogen-free low-smoke intrinsic flame-retardant IFR-PET is reduced by 41.6 percent compared with pure PET. Has better flame retardant effect under low addition amount, and plays a role in heat insulation and oxygen insulation due to the fact that dehydration of aluminum hydroxide and formation of metaphosphoric acid promote the formation of a compact carbon layer.
FIG. 4 is a graph of the total heat release rate of a phosphorus-aluminum type halogen-free low smoke intrinsic flame retardant IFR-PET. In the figure, a, b, c and d are respectively phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET with the dosage of HAFR accounting for 0 percent, 3 percent, 5 percent and 7 percent of the mass of terephthalic acid. The results show that the total heat release rate of pure PET is as high as 77.9MJ/m 2 When different amounts of HAFR are added, the total heat release rate is obviously reduced, and when the amount of the HAFR is 7 percent of the mass of the terephthalic acid, the total heat release rate is reduced to 62.2MJ/m 2 The overall heat release rate was reduced by 20.0%.
Fig. 5, 6 and 7 are a smoke release rate graph, a carbon monoxide release rate graph and a carbon dioxide release rate graph of the phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET, respectively. In the figure, a, b, c and d are respectively phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET with the dosage of HAFR accounting for 0 percent, 3 percent, 5 percent and 7 percent of the mass of terephthalic acid. When the amount of HAFR is 7% of the mass of terephthalic acid, the smoke release rate, the carbon monoxide release rate and the carbon dioxide release rate of the phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET are respectively reduced by 38%, 39% and 36%. This is because the formation of a dense carbon layer is promoted by dehydration and the formation of metaphosphoric acid at high temperature, and the release of smoke is effectively suppressed.
The flame retardant performance of the phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET is tested by adopting the GB/T2460-93 standard. The test results show that: the oxygen index is not less than 30.
In conclusion, the invention utilizes the reaction of organic phosphonic acid and aluminum hydroxide to obtain HAFR with hydroxyl active groups, and the HAFR is grafted to a PET matrix to prepare the phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET.
Drawings
FIG. 1 is a plot of the infrared absorption spectra of functionalized aluminum Hydroxide (HAFR), aluminum hydroxide (ATH), and hydroxyethylidene diphosphonic acid (HEDP).
FIG. 2 is an XRD pattern of functionalized aluminum Hydroxide (HAFR) and aluminum hydroxide (ATH).
FIG. 3 is a graph of the heat release rate of phosphorus-aluminum type halogen-free low smoke intrinsic flame retardant IFR-PET.
FIG. 4 is a graph of the total heat release rate of phosphorus-aluminum type halogen-free low smoke intrinsic flame retardant IFR-PET.
FIG. 5 is a graph of the smoke release rate of a phosphorus-aluminum type halogen-free low smoke intrinsic flame retardant IFR-PET.
FIG. 6 is a graph of carbon monoxide release rate from a phosphorus-aluminum type halogen-free low smoke intrinsic flame retardant IFR-PET.
FIG. 7 is a graph of carbon dioxide release rate from a phosphorus-aluminum type halogen-free low smoke intrinsic flame retardant IFR-PET.
Detailed Description
The preparation method and properties of the phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET of the invention are further explained by the following specific examples.
Example 1
(1) Adding 200mL of distilled water into a 500mL round-bottom flask, adding 10.4g of weighted hydroxyethylidene diphosphonic acid into the flask, heating the flask to 100 ℃ to completely dissolve the hydroxyethylidene diphosphonic acid, adding 7.8g of weighted aluminum hydroxide into the flask, magnetically stirring the mixture for 8 hours at 100 ℃, then carrying out reduced pressure distillation, and drying the mixture at 70 ℃ for 12 h to obtain white functionalized aluminum hydroxide solid.
(2) Adding 17.4g of HAFR, 581g of terephthalic acid, 282g of ethylene glycol and 0.0581g of antimony trioxide into a 1.5L magnetic stirring reaction kettle, filling nitrogen to enable the pressure to reach 0.05MPa, raising the temperature to 235 ℃ to react for 5h, removing moisture after the esterification reaction is finished to enable the kettle to keep normal pressure, closing an esterification valve to react for 0.5h at 100 ℃ and normal pressure, opening a polycondensation valve after the normal pressure reaction is finished, opening a vacuum pump to carry out half-vacuum state and 260 ℃ half-polycondensation reaction for 0.5 zxft 3532, carrying out full-vacuum state and 280 ℃ full-polycondensation reaction after the reaction is finished, introducing nitrogen to discharge, granulating and drying to obtain the phosphorus-aluminum type low-smoke zero-halogen intrinsic flame retardant IFR-PET.
(3) The amount of HAFR used was 3% by mass of terephthalic acid in the form of phosphorus-aluminumThe halogen-free low-smoke intrinsic flame-retardant IFR-PET heat release performance is as follows: the peak heat release rate was 655.8 kW/m 2 The peak value of the total heat release rate is 65.5MJ/m 2 The smoke release rate is 0.12m 2 The peak values of the carbon monoxide release rate and the carbon dioxide release rate are 0.0159 g/s and 0.50 g/s respectively.
Example 2
(1) The same as example 1;
(2) Adding 29 g of HAFR, 581g of terephthalic acid, 282g of ethylene glycol and 00.08715 g antimony trioxide into a 1.5L magnetic stirring reaction kettle, introducing nitrogen to enable the pressure to reach 0.05MPa, raising the temperature to 235 ℃ to react for 5h, removing water after the esterification reaction is finished to enable the kettle to keep normal pressure, closing an esterification valve to react for 0.5h at 100 ℃ and normal pressure, opening a polycondensation valve to start a vacuum pump to perform semi-vacuum state and semi-polycondensation reaction at 260 ℃ for 0.5h after the normal pressure reaction is finished, performing full polycondensation reaction at 280 ℃ and 7h after the reaction is finished, introducing nitrogen to discharge, granulating and drying to obtain the phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET.
(3) The HAFR dosage is 5 percent of the heat release performance of the phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET by the mass of the terephthalic acid: the peak value of the heat release rate is 585.1kW/m 2 The peak value of the total heat release rate is 66.5MJ/m2, and the smoke release rate is 0.117m 2 The peak values of the carbon monoxide release rate and the carbon dioxide release rate are 0.0127g/s and 0.454g/s respectively.
Example 3
(1) The same as example 1;
(2) Adding 40.6 g of HAFR, 581g terephthalic acid, 282g ethylene glycol and 0.1162 g antimony trioxide into a 1.5L magnetic stirring reaction kettle, introducing nitrogen to enable the pressure to reach 0.05MPa, raising the temperature to 235 ℃, reacting 5h, removing water to enable the kettle to keep normal pressure after the esterification reaction is finished, closing an esterification valve, reacting 0.5h at 100 ℃ and normal pressure, opening a polycondensation valve after the normal pressure reaction is finished, opening a vacuum pump to perform half-vacuum state and 260 ℃ half-polycondensation reaction for 0.5h, performing full-vacuum state and 280 ℃ full-polycondensation reaction after the reaction is finished, introducing nitrogen to discharge, granulating, and drying to obtain the phosphorus-aluminum type halogen-free intrinsic low-smoke flame retardant IFR-PET.
(3) The HAFR dosage is 7 percent of the thermal release performance of the phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET by the mass of the terephthalic acid: the peak value of the heat release rate is 556.2KW/m 2 The peak value of the total heat release rate is 62.2MJ/m 2 The smoke release rate was 0.116 m2/s, and the peak carbon monoxide release rate and carbon dioxide release rate were 0.0128 g/s and 0.436 g/s, respectively.
Claims (4)
1. A preparation method of phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET comprises the following steps:
(1) Heating and dissolving organic phosphonic acid in distilled water, adding aluminum hydroxide, reacting for 6 to 10h at the temperature of 80 to 100 ℃ under stirring, distilling under reduced pressure, and drying to obtain white solid, namely functionalized aluminum hydroxide; the organic phosphonic acid is hydroxyethylidene diphosphonic acid; the mass ratio of the aluminum hydroxide to the organic phosphonic acid is 3:4;
(2) Terephthalic acid, ethylene glycol and functional aluminum hydroxide are taken as raw materials, and Sb is taken as 2 O 3 Taking nitrogen as a protective gas, carrying out esterification reaction for 4 to 7 hours at 0.2 to 0.35MPa and 235 to 250 ℃, reacting for 0.5 to 1h at 95 to 105 ℃ and normal pressure after the esterification reaction is finished, carrying out semi-polycondensation reaction for 0.5 to 1h at 250 to 270 ℃ in a semi-vacuum state, carrying out full-polycondensation reaction for 3 to 5h at 275 to 280 ℃ in a full-vacuum state, introducing nitrogen for discharging, carrying out granulation and drying to obtain the phosphorus-aluminum type low-smoke halogen-free intrinsic flame retardant IFR-PET; the mass ratio of the ethylene glycol to the terephthalic acid to the functionalized aluminum hydroxide is 1.1:0.033 to 1.3.
2. The preparation method of the phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET as claimed in claim 1, characterized in that: in the step (1), the drying temperature is 60 to 80 ℃, and the drying time is 6 to 10 hours.
3. The preparation method of the phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET as claimed in claim 1, characterized in that: in step (2), sb 2 O 3 The mass ratio of the terephthalic acid to the terephthalic acid is 1.0001 to 1.
4. The preparation method of the phosphorus-aluminum type halogen-free low-smoke intrinsic flame retardant IFR-PET as claimed in claim 1, characterized in that: in the step (2), the drying temperature is 60 to 80 ℃, and the drying time is 6 to 10 hours.
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