Synthesis, characterization and thermodynamics of the reaction of calcium methylphosphonate with n-alkylmonoamines

Lima, Cícero Bosco Alves de; Airoldi, Cláudio

doi:10.1016/s1466-6049(01)00089-7

Cited by 23 publications

(8 citation statements)

References 28 publications

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“…2 ppm are believed to be weak spinning side bands (ssb) as seen for PVPA-hydroxyapatite composites 20 and calcium methylphosphonate. 29 Spinning side bands such as these arise due to rotation of the NMR sample through field gradients in the XZ plane. 30 They are identifiable by their symmetrical spacing on each side of the parent centre band (in this case the PO 4 32 band at 2 .…”

Section: Resultsmentioning

confidence: 99%

Surface modification of bioceramics by grafting of tailored allyl phosphonic acid

Phillips¹,

Duncanson²,

Wilson³

et al. 2005

Advances in Applied Ceramics

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A new route to interfacial bonding between ceramic and matrix in biocomposites is identified. A tailored allyl phosphonic acid is used as a coupling agent bound to the surface of a bioceramic to form a 'grafted' calcium phosphate (CAP). The allyl phosphonic acid coupling agent is synthesised by reaction of allyl halide and trialkyl phosphite. Successful synthesis was confirmed by nuclear magnetic resonance and Fourier transform infrared spectroscopy (FTIR). The allyl phosphonic acid was incorporated onto calcium phosphate using a wet chemical coprecipitation synthesis route. The resulting 'grafted' CAP was characterised using FTIR coupled with photoacoustic sampling, and Fourier transform Raman spectroscopy (FTR). The spectroscopic data suggest an interaction between the allyl phosphonic acid and calcium phosphate resulting from observed reductions in intensity of the hydroxyl (3570 cm 21 ) and phosphate n 3 (1030 cm 21 ) peaks. The continued presence of C5C functionality on the surface of the grafted CAP was indicated by FTIR and FTR spectra (peaks at 1650 and 1635 cm 21 respectively) and confirmed by X-ray photoelectron spectroscopy (XPS). On the basis of these results, it is concluded that grafted CAP may be used to produce a chemically bonded composite with superior mechanical properties.

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Section: Resultsmentioning

confidence: 99%

Surface modification of bioceramics by grafting of tailored allyl phosphonic acid

Phillips¹,

Duncanson²,

Wilson³

et al. 2005

Advances in Applied Ceramics

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“…As observed, the values of variation in enthalpy for all the amines are exothermic in nature, however, they do not follow a well-defined order, when considering the sequence of the aliphatic amine chains. 45 In the same direction, the specific enthalpic values for the interactive processes (Δ int h) do not follow a linear order with the increase of the carbon atom chains, as was also observed for other systems. 34,35,37,45 It seems that the explanation for this behavior can be related to amine interferences in the free interlayer space of the lamella, which is already occupied by the voluminous phenyl group.…”

Section: Calorimetrymentioning

confidence: 52%

“…45 In the same direction, the specific enthalpic values for the interactive processes (Δ int h) do not follow a linear order with the increase of the carbon atom chains, as was also observed for other systems. 34,35,37,45 It seems that the explanation for this behavior can be related to amine interferences in the free interlayer space of the lamella, which is already occupied by the voluminous phenyl group. The increase of the amine chains assumes a more complex arrangement that contributes to the lack of an order sequence of values.…”

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confidence: 52%

Intercalation and thermochemistry of amines in lamellar titanium phenylarsonate

Ruiz¹,

Airoldi²

2005

J. Braz. Chem. Soc.

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O composto lamelar fenilarsonato de titânio foi sintetizado e intercalado com alquilmonoaminas (metil a heptil), diaminoetano e diaminobutano, lutidina e α-picolina. A matriz original foi caracterizada por análise elementar, difração de raios X, análise de superfície, porosidade, espectroscopia de absorção na região do infravermelho, termogravimetria e microscopia eletrônica de varredura. Os difratogramas de raios X não mostraram aumento significativo de distâncias interlamelares, e a intercalação foi comprovada por técnicas como a termogravimetria que indicou a perda de massa correspondendo às aminas. A condição ideal de intercalação foi efetuada com injeções de 30,0x10 -6 dm 3 da amina 0,50 mol dm -3 em suspensão de aproximadamente 10x10 -3 g das matrizes. Os números de moles intercalados com as alquilmonoaminas seguiram uma ordem aleatória em relação ao aumento da cadeia alifática, com valores entálpicos de -9,18 ± 0,07; -12,10 ± 0,20; -7,61 ± 0,02; -6,88 ± 0,01; -9,47 ± 0,03; -12,84 ± 0,10 e -14,78 ± 0,10 kJ mol -1 para a seqüência das alquilmonoaminas e variaram de -3,66 ± 0,30 a -10,92 ± 1,50 kJ mol -1 para alquildiaminas. Com as aminas aromáticas não ocorreu um efeito térmico significativo nas intercalações, fato que foi atribuído ao grande volume do grupo fenila presente no interior das lamelas, que impede a inserção da base na cavidade lamelar.The lamellar compound titanium phenylarsonate was synthesized and intercalated with alkylmonoamines (methyl to heptyl), diaminoethane, diaminobutane, lutidine and α-picoline. The host was characterized through elemental analysis, X-ray diffraction, surface analysis, porosity, infrared spectroscopy, thermogravimetry and electronic scanning microscopy. The intercalated compounds did not show significant increases in the interlamellar distances through X-ray diffractometry. The intercalation was confirmed by the thermogravimetric technique, indicating mass losses that correspond to the amines. The ideal intercalation was established by adding increments of 30.0x10 -6 dm 3 of 0.50 mol dm -3 of each amine into a suspension of about 10x10 -3 g of matrix. The number of moles intercalated with alkylmonoamines followed an aleatory order in relation to the increase of the aliphatic chain and the enthalpic values gave -9. 18 ± 0.07; -12.10 ± 0.20; -7.61 ± 0.02; -6.88 ± 0.01; -9.47 ± 0.03; -12.84 ± 0.10 and -14.78 ± 0.10 kJ mol -1 for the sequence of alkylmonoamines and varied from -3.66 ± 0.30 to -10.92 ± 1.50 kJ mol -1 for the alkyldiamines. The aromatic amines presented small thermal effects and the unfavorable intercalation is attributed to the large volume of the phenyl group inside the lamella, which hinders insertion of these bases inside the lamellar cavity.Keywords: lamellar compound, intercalation, calorimetry, alkylmonoamines, alkyldiamines, aromatic amines IntroductionA huge number of natural or synthesized materials, normally classified as typical inorganic substances, embodying clays, double hydroxides, phosphates, phosphonates, graphite, silicates, niobates, ...

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“…Direct acquisition involving host-guest quantitative intercalation effects can be attained through the calorimetric technique, which provides, in one operation, the variation in enthalpy and the equilibrium constant determination at the solid/liquid interface, as reported for a limited number of systems [13][14][15][16][17][18].…”

Section: Introductionmentioning

confidence: 99%

Calorimetric data on intercalation of some aromatic amines into barium phenylphosphonate at the solid/liquid interface

Lazarin

Airoldi

2005

The Journal of Chemical Thermodynamics

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Synthesis, characterization and thermodynamics of the reaction of calcium methylphosphonate with n-alkylmonoamines

Cited by 23 publications

References 28 publications

Surface modification of bioceramics by grafting of tailored allyl phosphonic acid

Surface modification of bioceramics by grafting of tailored allyl phosphonic acid

Intercalation and thermochemistry of amines in lamellar titanium phenylarsonate

Calorimetric data on intercalation of some aromatic amines into barium phenylphosphonate at the solid/liquid interface

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