Mechanism studies of thermolysis process in copolyamide 66 containing triaryl phosphine oxide

Yang, Xiaofeng; Li, Qiao Ling; Chen, Zhi Ping; Zhang, Lei; Zhou, You

doi:10.1007/s10973-012-2579-9

Cited by 14 publications

(12 citation statements)

References 12 publications

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“…Recently, investigations have appeared on the thermolysis behavior of triarylphosphine oxide, especially when used as building blocks in co-polymers. It is generally thought that the triarylphosphine oxide is converted to phosphoric acid upon combustion and after cooling and hydration [9,10], where it is likely that amounts of polyphosphoric acids remain, where in our case phosphoric acids can also be esterified with silanol groups. In those cases where sea-sand was used as a protective covering layer in the column chromatography, both the sodium and sulfur contents in the recycled silica gel rose (to 1.4 w% Na and to 775 ppm S for 10 X recycled silica gel).…”

Section: Resultsmentioning

confidence: 99%

Our Experience of Using Thermally Recycled Silica Gel in a Teaching and Small Research Laboratory Setting

Wahshi

Alqahtani

Abdulla

et al. 2018

22nd International Electronic Conference on Synthetic Organic Chemistry

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Organic synthetic research laboratories generate a large amount of waste. Some of the waste is the silica gel used as the stationary phase in column chromatographic separations. Here, the authors discuss the possibility of recycling silica gel wastes thermally at 600 °C, at which temperature the remnant adsorbed organic material combusts. It could be shown that the recycled silica gel maintains its adsorption characteristics. The process could be repeated 10 times with any discernable deterioration of the separation properties of the silica gel for the product mixture of the reactions used in this research. In those cases where triphenyl oxide remained on the silica gel after the separation of the reaction mixture, such as after Wittig olefination and Appel-type reactions, an increase of phosphorus content was noted in the silica gel after thermal treatment. The original and recycled silica gel was partly analyzed by Brunauer-Emmett-Teller (BET) surface measurements, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS) and in inductively coupled plasma optical emission spectroscopy (ICP-OES). The process significantly reduced waste production in our laboratory and also led to a reduction in costs associated with acquiring new silica gel and with the management and the disposal of spent silica gel. A simple environmental impact assessment has been carried out.

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Section: Resultsmentioning

confidence: 99%

Our Experience of Using Thermally Recycled Silica Gel in a Teaching and Small Research Laboratory Setting

Wahshi

Alqahtani

Abdulla

et al. 2018

22nd International Electronic Conference on Synthetic Organic Chemistry

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“…As the incorporation of DDP, C―P covalent bond appeared in the chain of FRPA66 and the bond energy of C―P bond was 260 kJ·mol −1 . However, the bond energy of C―C bond was 349 kJ·mol −1 , so the bond energy of C―P covalent bond was lower than that of C―C bond . It meant that the C―P covalent bond was easier to split in intrinsically flame‐retarded materials when heated.…”

Section: Resultsmentioning

confidence: 99%

Preparation and characterizations of inherent flame retarded polyamide 66 containing the phosphorus linking pendent group

Liu

Zhang

et al. 2017

Polymers for Advanced Techs

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Polyamide 66 (PA66) containing the phosphorus linking pendent group with inherent flame retardancy property was prepared by condensation polymerization of hexamethylene diammonium adipate (AH salt) and 9,10-dihydro-10-[2,3-di(hydroxycarbonyl)propyl]-10phosphaphenanthrene-10-oxide (DDP) as a co-monomer. Prior to condensation polymerization, DDP was reacted with hexamethylene diamine (HMDA), which made DDP easier to react with AH salt. Then, the DDP-HMDA was introduced into AH salt solution to prepare inherent flame retarded PA66 (FRPA66). Fourier transform infrared spectra, nuclear magnetic resonance spectra, gel permeation chromatography, differential scanning calorimetry, thermogravimetric analysis, tensile test, vertical burning test, limiting oxygen index test, cone calorimetry, and scanning electron microscopy were utilized to investigate the properties of FRPA66.Experimental results indicated that the bulky pendent phosphorus group tended to destroy the structure regularity of FRPA66 and the molecular weight, crystallinity, and thermal stability reduced. The tensile strength of FRPA66 containing 5 wt% of DDP was 58.44 MPa, and it can achieve a V-0 rating according to the vertical burning test with the limiting oxygen index value of 33.2%. This indicated that the inherent flame retarded PA66 expanded the application of PA66 materials.

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“…The phosphorus-containing polymers, therefore, have been extensively synthesized and characterized to investigate the improvement of thermal properties. [24][25][26][27][28] Phosphoruscontaining polyamides were for the first time provided by Joseph Pellon. [29] These phosphorus-containing polyamides generally were found to be amorphousrelatively low softening materials having an extended solubility range.…”

Section: Introductionmentioning

confidence: 99%

Phosphorus-containing polymers from THPS. II: synthesis and property of phosphorus-containing hyperbranched aromatic-aliphatic polyamides

Tan

Sun

Zhang

et al. 2015

Designed Monomers and Polymers

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Phosphorus-containing hyperbranched aromatic-aliphatic polyamides are prepared via direct polymerization of triacid (B 3 ) with different diamines (A 2 ), which for improving the processability of aromatic polyamides while keeping exellent thermal and mechanical property. The triacid (B 3 ), tris(2-carboxyethyl)phosphine oxide (TCEPO), is synthesized from tetrakis(hydroxymethyl)phosphonium sulfate and its structure is verified by Fourier transform infrared, 1 H, 13 C and 31 P NMR spectroscopy. Then, the polycondensation reaction of TCEPO with p-phenylene diamine, 4,4′-oxyphenylene diamine and 4,4′-methylenedianiline result in three phosphorus-containing hyperbranched aromatic-aliphatic polyamides, and the degree of branching is found between 0.66 and 0.71. Gel permeation chromatography measurement reveal that all hyperbranched aromatic-aliphatic polyamides have moderate number-averaged molecular weights and narrow molecular weight distribution. The Dynamic mechanical thermal analysis results show all polymers have two glass transition temperatures (T g ) in the temperature range 85.3-128.0°C and have high storage modulus about 1.52-3.19 GPa at 50°C. The TGA results reveal the initial degradation temperatures (T 5 ) and the temperatures for 10% gravimetric loss (T 10 ) for the hyperbranched aromatic-aliphatic polyamides are in the range of 214-250 and 256-333°C, and the maximum decomposition temperatures (T m ) are about 500°C, and also the char yields of polymers at 850°C are about 39.4-48.4%, which indicate good thermal stability.

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Mechanism studies of thermolysis process in copolyamide 66 containing triaryl phosphine oxide

Cited by 14 publications

References 12 publications

Our Experience of Using Thermally Recycled Silica Gel in a Teaching and Small Research Laboratory Setting

Our Experience of Using Thermally Recycled Silica Gel in a Teaching and Small Research Laboratory Setting

Preparation and characterizations of inherent flame retarded polyamide 66 containing the phosphorus linking pendent group

Phosphorus-containing polymers from THPS. II: synthesis and property of phosphorus-containing hyperbranched aromatic-aliphatic polyamides

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