- Synthesis of well-dispersed ZnO nanomaterials by directly calcining zinc stearate
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Well-dispersed ZnO nanomaterials were synthesized by direct calcination of zinc stearate. Results from Fourier transform infrared (FT-IR) spectra and X-ray diffraction (XRD) indicated both the decomposition degree of organic ligand and the purity of calci
- Guo, Guangsheng,Shi, Chen,Tao, Dongliang,Qian, Weizhong,Han, Dongmei
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- Molecular rearrangement in a zinc stearate langmuir film dependent on a film preparation method studied using polarization-modulation infrared reflection absorption spectroscopy and X-ray absorption fine structure
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Molecular dynamic rearrangement in a Langmuir (L) film of zinc stearate in a cross section image has been analyzed by employing polarization modulation infrared reflection spectrometry (PM-IRRAS) and X-ray absorption fine structure (XAFS). The number of coordination on a zinc cation is evaluated by XAFS, and the coordination structure of the carboxylic group is revealed by the IR analysis. An L film prepared at a fixed area without using film-compression bar exhibits time-dependent change of the coordination structure about a zinc cation, and it attains a highly ordered coordination structure in the carboxylic group region. However, an L film prepared by the Langmuir technique using a compression bar exhibited ignorable spectral changes in both IR and X-ray analyses. The hydrocarbon chains in the compressed L film are better uniformed than the uncompressed film, but the uniformed molecular arrangement of the carboxylic group is restricted to be rearranged, and it does not attain a stable structure in terms of coordination on the zinc cation. ? 2012 American Chemical Society.
- Muro, Maiko,Harada, Makoto,Okada, Tetsuo,Hasegawa, Takeshi
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- Vibrational spectra and structures of zinc carboxylates II. Anhydrous zinc acetate and zinc stearate
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A normal mode analysis was carried out for a monoclinic anhydrous zinc acetate crystal in which the acetate groups had bridging bidentate coordination forms, and spectral assignments were made. Based on the assignments, a relation between the coordination structure of the carboxylate groups around the zinc atom and the vibrational frequencies of the carboxylate rocking mode was found. This relation was applied to zinc stearate to determine its coordination form, and we found that zinc stearate had a bridging bidentate form.
- Ishioka, Tsutomu,Shibata, Youko,Takahashi, Mizuki,Kanesaka, Isao
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- Infrared study on annealing effect on conformation of zinc stearate
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The molecular conformation and thermal transition behavior of two zinc stearate specimens, unannealed one and annealed one, were compared. The unannealed specimen has one thermal transition at 134 °C. Annealing was made by increasing temperature to 150 °C and cooling to room temperature slowly. This annealed specimen has an exothermic peak at 103 °C, and endothermic shoulders and a peak at 118, 124 and 131 °C, respectively. The observed frequencies of all bands of the unannealed specimen at room temperature are assigned to the all-trans conformation. We found new bands at 858, 823, 793, 766, 688, and 604 cm-1 for the annealed specimen. Based on the normal mode analyses, these bands are assigned to the TGT conformation at the COO end, where T means trans and G means gauche. The annealed specimen consists of almost all-trans molecule but partial molecules have the TGT conformation.
- Ishioka, Tsutomu,Kiritani, Atsushi,Kojima, Takuya
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- Infrared and XAFS study on structure and transition behavior of zinc stearate.
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Structure and transition behavior of zinc(II) stearate crystal were investigated by infrared and XAFS spectroscopies. Structure of zinc stearate at room temperature was estimated as follows. From XAFS analysis, the coordination number of the carboxylate groups around the zinc atom was evaluated as 4 and the Zn-O distance as 1.95 A. Based on the infrared spectrum and a normal mode analysis, the conformation of the alkyl chain was confirmed as all-trans and the sub-cell packing was considered as parallel type, and also the coordination form of the carboxylate groups was determined as bridging bidentate type. As increasing temperature, zinc stearate has a solid liquid phase transition at 130 degrees C. At the transition, the alkyl chains goes into liquid like state as reported by Mesubi but the coordination structure was confirmed to be maintained.
- Ishioka,Maeda,Watanabe,Kawauchi,Harada
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Read Online
- Catalytic deoxygenation of C18 fatty acid over supported metal Ni catalysts promoted by the basic sites of ZnAl2O4 spinel phase
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Highly active Zn-Al composite oxides were synthesized via a hydrothermal process followed by thermal treatment and were used as supports to prepare Ni-based hydrogenation catalysts for catalytic deoxygenation of oleic acid, stearic acid, and 1-octadecanol. The results showed that increasing the temperature of hydrothermal synthesis changed the morphology of the Zn-Al composite oxides from sheet-like structures to spheroidal structures. High hydrothermal synthesis temperatures enhanced the interaction between Zn and Al atoms, resulting in more ZnAl2O4 spinel phase. This phase not only improved the chemical stability of the support but also supplied strong basic sites which efficiently inhibited the formation of by-products and increased the yield of heptadecane in the catalytic deoxygenation of oleic acid. Stearic acid and 1-octadecanol could be readily transformed to alkanes in the presence of metallic Ni and ZnAl2O4 phase. Decarbonylation of the octadecanal intermediate and dehydrogenation of 1-octadecanol were key reaction pathways to produce heptadecane, in which decarbonylation was catalyzed by metallic Ni, while the dehydrogenation was attributed to synergistic catalysis between metallic Ni and the strong basic sites of the support. Individual metallic Ni only catalyzed the cleavage of C-H bonds but did not affect the O-H bond of 1-octadecanol.
- Li, Guangci,Chen, Lei,Fan, Ruikun,Liu, Di,Chen, Song,Li, Xuebing,Chung, Keng H.
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p. 213 - 222
(2019/01/14)
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- Preparation method of zinc stearate
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The invention provides a preparation method of zinc stearate. The preparation method of zinc stearate solves the technical problems that in an existing production process, single-pass smashing is adopted, and product uniformity is poor. The preparation method of zinc stearate includes the following steps that firstly, liquid stearic acid is delivered into a reaction kettle through a delivery pump for stirring heating, wherein the stirring time is 20-28 min, and the heating temperature is 120-150 DEG C; secondly, zinc oxide is added into the reaction kettle in three times, and a reaction is carried out at the temperature of 160-180 DEG C and the pressure of 0.18-0.24 Mpa, wherein the reaction time is 40-50 min; thirdly, zinc stearate generated after the reaction is delivered into a tabletting machine for tabletting; fourthly, tabletted zinc stearate is coarsely crushed through a common crushing machine; fifthly, coarsely-crushed zinc stearate is finely crushed through an airflow crushing system, and zinc stearate is obtained. The preparation method of zinc stearate has the advantage that product uniformity is good.
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Paragraph 0059; 0060; 0061; 0062; 0063
(2017/08/27)
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- Effect of Zn/Al ratio of Ni/ZnO-Al2O3 catalysts on the catalytic deoxygenation of oleic acid into alkane
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Ni-based catalysts supported on Zn-Al composite oxides have been prepared for the catalytic deoxygenation of oleic acid into diesel-ranged alkanes, and the effects of the Zn/Al ratio on the physico-chemical properties of the supports and the deoxygenation activity of the final catalyst were investigated in detail. The results showed that higher Zn/Al ratios led to lower specific surface area of the supports and weakening of the interaction between Ni species and supports thereby improving the reducibility of Ni species. However, higher Zn/Al ratios may limit the dispersion of Ni species, leading to a decrease in the exposure of metallic Ni. Because the conversion and deoxygenation of the reactants mainly depended on the hydrogenation capability of the catalysts which was controlled by the amount of exposed metallic Ni, the catalyst with a Zn/Al ratio of 2/1 showed the highest hydrogenation rate and alkane yield. Further decreasing the Zn/Al ratio led to strong metal-support interaction, making the Ni species difficult to reduce, which may also inhibit the formation of alkane products. In addition, the change in Zn/Al ratio affected intermediate type, which could affect the yield of alkane products.
- Chen, Lei,Zhang, Feng,Li, Guangci,Li, Xuebing
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p. 175 - 184
(2016/11/23)
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- A process for the preparation of bulk zinc stearate
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The invention provides a preparation method of bulk zinc stearate. The preparation method comprises the following steps: a. feeding stearic acid at normal pressure to a reaction kettle, heating up to 130-160 DEG C, then adding a catalyst and zinc oxide to the reaction kettle, and taking reaction for 80-120 minutes till reaching the molten state; b. adding an antioxidant, and stirring for 5-20 minutes; c. adding the molten zinc stearate prepared in the step b to a mold with a framework; d. cooling to obtain the required bulk zinc stearate with a certain shape. The preparation method disclosed by the invention is to add the molten zinc stearate prepared by the dry method to the framework to prepare the bulk zinc stearate, and cannot generate particles or microparticle dust in a processing workshop, so as to effectively improve the environment quality of the workshop, greatly reduce influence on health of workers in the workshop, and achieve a great promotional value and social significance.
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Paragraph 0023
(2017/04/03)
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- Modified zinc stearate production technology
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The invention provides a modified zinc stearate production technology comprising the following steps: (a) carrying out heating melting on stearic acid in a reaction kettle, adding zinc oxide at the temperature of 120 DEG C-150 DEG C while high-speed stirring, carrying out a reaction for 10-15 minutes, and then adding pure water; and (b) vacuumizing: sealing the reaction kettle, vacuumizing to the vacuum degree of 50-500 Pa, carrying out a reaction for 20-30 minutes, after cooling and temperature dropping, allowing the product to enter a pulverizer, and pulverizing. Compared with a traditional zinc stearate dry-process production technology, the prepared zinc stearate has the advantages of loose particles, easy pulverizing, fine product granularity, high reactivity and less energy consumption, and has quite obvious economic benefits and social benefits.
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Paragraph 0015
(2016/10/17)
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- Preparation method of improved zinc stearate
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The invention relates to a producing process for zinc stearate, and more particularly, relates to a preparation method of improved zinc stearate. The method comprises the following steps: adding deionized water to a reaction kettle, and heating up to 30-40 DEG C; under stirring, adding stearic acid to the reaction kettle, and dissolving the stearic acid; continuing to heat up to 60-80 DEG C, adding zinc oxide and hydrogen peroxide into the reaction kettle, sealing the reaction kettle, vacuumizing to the vacuum degree of 50-100 Pa, carrying out a reaction for 30-60 min, cooling to drop the temperature, allowing the obtained material to enter a pulverizer, and pulverizing to obtain the zinc stearate. The zinc stearate prepared by the method has the advantages of high activity, easy pulverization, fine grain size of the product and the like; the preparation method has the advantages of low energy consumption and environmental protection, and has obvious economic benefits and social benefits.
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Paragraph 0074; 0075
(2017/01/12)
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- METHODS OF METAL OXIDE NANOCRYSTALS PREPARATION
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Embodiments relate to methods of metal oxide nanocrystals preparation. In embodiments, a metal-organic precursor may be economically synthesized by reacting a metal with an organic acid. The organic acid may include an aliphatic chain longer than three carbon atoms. The metal may be In, Sn, Al, Ga, Zn, Cd, Sb, Bi, Ge, Mn, Ti, Nb, V, Cr, Mo, Fe, Y, Mg, Co, as well as mixtures thereof. Further processing of the metal-organic precursor (e.g. by pyrolysis, hydrolysis, or alcoholysis) produces metal oxide nanocrystals of desired characteristics. An metal-organic precursor of indium tin oxide (ITO) may be synthesized by reacting indium metal and tin metal with an organic acid having an aliphatic chain longer than three carbon atoms (e.g. stearic acid) at a temperature above 200° C. Further processing of the resulting metal-organic precursor yields ITO nanocrystals of regular shape, uniform size, and average diameter ranging of between about 1-500 nm.
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(2015/11/17)
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- Characterisation of metal carboxylates by Raman and infrared spectroscopy in works of art
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This work introduces the complementary use of μ-Raman and μ-Fourier transform infrared (IR) spectroscopy for the detection of specific carbon chains and cations for the identification of metal carboxylates within oil paint microsamples. Metal carboxylates (metal soaps) form naturally when free fatty acids react with metal cations and may also be found as additives or degradation products. Twenty-two metal carboxylates were synthesised, and their spectra assembled in a reference database. Metal salts of cations commonly present in oil paintings were used, including lead, zinc, calcium, cadmium, copper and manganese. The fatty acids selected were the saturated acids palmitic (C1 6:0) and stearic (C18:0) and the polyunsaturated oleic acid (C1 8:1). Azelaic acid (C9 diacid), a product resulting from autoxidation of polyunsaturated acids, was also included. Metal carboxylates were characterised by Raman and IR spectroscopy, and their structures were confirmed by X-ray diffraction. Raman and IR spectroscopy proved to be complementary techniques for a full identification of the metal carboxylates in complex aged paint. Raman enables the differentiation of the carbon chain length in the C-C stretching region (1120-1040 cm-1), and IR distinguishes the metal cation in the COO- stretching absorption region (1650-1380cm-1). Principal component analysis was applied to the spectra in order to facilitate a fast and accurate method to discriminate between the different metal carboxylates and to aide in their identification. Finally, spectra from case studies were successfully projected in the principal component analysis models built, enabling a higher confidence level for the identification of copper palmitate and copper azelate in two 19th-century Portuguese oil paintings.
- Otero, Vanessa,Sanches, Diogo,Montagner, Cristina,Vilarigues, Mrcia,Carlyle, Leslie,Lopes, Joo A.,Melo, Maria J.
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p. 1197 - 1206
(2015/02/19)
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- POLYSULFIDE POLYOLS, THEIR PRODUCTION AND USE
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The present invention relates to polysulfide polyols, their production and use.
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(2014/08/07)
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- Zinc carboxylic salts used as catalyst in the biodiesel synthesis by esterification and transesterification: Study of the stability in the reaction medium
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Biodiesel is produced by the catalytic transesterification of renewable sources such as vegetable oils and animal fats. It is an attractive alternative to diesel fuel because of its environmental benefits. In this work, the transesterification of soybean
- Reinoso, Deborath M.,Damiani, Daniel E.,Tonetto, Gabriela M.
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- Methods for Making Organozinc Salts and Compositions Containing the Same
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Organic zinc salts and mixtures thereof, organic zinc salt coated particles, methods of preparing organic zinc salts and organic zinc salt coated particles, and various applications of such coated particles, including applications in rubber, other polymeric materials, and pesticides and/or fungicides are disclosed.
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Page/Page column 5
(2010/07/08)
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- Mixed saturated-unsaturated alkyl-chain assemblies: Solid solutions of zinc stearate and zinc oleate
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The linear saturated stearic acid and the bent mono-unsaturated oleic acid do not mix and form solid solutions. However, the zinc salts of these acids can. From X-ray diffraction and DSC measurements we show that the layered zinc stearate and zinc oleate salts form a homogeneous solid solution at all composition ratios. The solid solutions exhibit a single melting endotherm, with the melting temperature varying linearly with composition but with the enthalpy change showing a minimum. By monitoring features in the infrared spectra that are characteristic of the global conformation of the hydrocarbon chain, and hence can distinguish between stearate and oleate chains, it is shown that solid solution formation is realized by the introduction of gauche defects in a fraction of the stearate chains that are then no longer linear. This fraction increases with oleate concentration. It has also been possible from the spectroscopic measurements to establish a quantitative relation between molecular conformational order and the thermodynamic enthalpy of melting of the solid solutions.
- Barman,Vasudevan
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p. 5212 - 5217
(2008/10/09)
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- Catalytic oxidative cleavage of terminal olefins by chromium(III) stearate
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A new synthetic methodology for the preparation of carbonyl compounds from the oxidative cleavage of terminal olefins has been developed. With the use of TBHP in combination with chromium(III) stearate, selective oxidation of double bonds conjugated with aromatic ring or carbonyl group could be achieved at ambient temperature in moderate to excellent yield. The oxidative cleavage of electron rich α-methylstyrene derivatives proceeded in good to excellent yield whereas lower yields were observed in α-methylstyrene derivatives containing an electron withdrawing group. This developed oxidation reaction was believed to undergo via free radical process and high valent chromium oxo species.
- Jarupinthusophon, Suekanya,Thong-In, Uthumporn,Chavasiri, Warinthorn
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p. 289 - 294
(2008/10/09)
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- Room temperature molecular and lattice structures of a homologous series of anhydrous zinc(II) n-alkanoate
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The room temperature structures and lattice arrangements of a homologous series of zinc(II) n-alkanoates from chain length, nC = 4-20, inclusive, have been studied using infrared spectroscopy, X-ray diffraction and polarizing light microscopy. Lattice parameters from single crystal and powder diffraction data, for zinc(II) hexanoate, are compared to validate the use of the powder method. Since they are in excellent agreement, the powder data are analyzed by a software programme to determine lattice parameters for all the homologues. These are used, in conjunction with infrared, X-ray, density and molecular model calculations to determine molecular and lattice structures. The compounds are isostructural, in that, each zinc atom is tetrahedrally coordinated to oxygen atoms from four different carboxylate groups and each ligand forms a Z,E-type bidentate bridge with two tetrahedral zinc atoms resulting in a syn-anti arrangement. The hydrocarbon chains are in the fully extended all-trans configuration and are tilted at an average angle of 60° to the zinc basal plane. For the short chain length compounds with nC ≤ 8, a double bilayer in-plane-perpendicular-perpendicular-in-plane arrangement of hydrocarbon chains, with two molecules per unit cell, is indicated. For the others, an interdigitating in-plane-in-plane bilayer with head-to-tail interactions, with one molecule per unit cell, is proposed. A geometric model is presented to account for odd-even chain effects and to explain the differences in melting points and densities between these adducts. All the compounds crystallize in the monoclinic space group with P symmetry and are arranged in a two-dimensional network along the ac plane within the unit cell.
- Taylor, Richard A.,Ellis, Henry A.
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- Melting of saturated fatty acid zinc soaps
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The melting of alkyl chains in the saturated fatty acid zinc soaps of different chain lengths, Zn(CnH2n-1COO)2; n = 11, 13, 15, and 17, have been investigated by powder X-ray diffraction, differential scanning calorimetry, and vibrational spectroscopy. These compounds have a layer structure with the alkyl chains arranged as tilted bilayers and with all methylene chains adopting a planar, all-trans conformation at room temperature. The saturated fatty acid zinc soaps exhibit a single reversible melting transition with the associated enthalpy change varying linearly with alkyl chain length, but surprisingly, the melting temperature remaining constant. Melting is associated with changes in the conformation of the alkyl chains and in the nature of coordination of the fatty acid to zinc. By monitoring features in the infrared spectra that are characteristic of the global conformation of the alkyl chains, a quantitative relation between conformational disorder and melting is established. It is found that, irrespective of the alkyl chain length, melting occurs when 30% of the chains in the soap are disordered. These results highlight the universal nature of the melting of saturated fatty acid zinc soaps and provide a simple explanation for the observed phenomena.
- Barman,Vasudevan
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p. 22407 - 22414
(2008/10/09)
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- Contrasting melting behavior of zinc stearate and zinc oleate
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The influence of a double bond in the middle of an otherwise flexible hydrocarbon chain on the melting of such assemblies has been investigated by comparing the melting behavior of zinc stearate and zinc oleate. By monitoring features in the infrared spectra that are characteristic of the global conformation of the hydrocarbon chain, it is shown that the double bond effectively decouples the thermal evolution of conformational disorder in the chain segments on either side of the double bond and the melting of each of these segments in the assembly occurs as independent events.
- Barman,Vasudevan
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p. 651 - 654
(2008/10/09)
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- METHOD FOR PRODUCING METAL CARBOXYLATES
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The invention relates to a method and to a device for producing metal carboxylates from a reaction mixture. According to said method, the reaction mixture is treated with the aid of a microwave in at least one step of said method.
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Page/Page column 31-32
(2008/06/13)
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- Synthesis of biodiesel via homogeneous Lewis acid catalyst
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Nowadays, most biodiesel (fatty acids methyl esters, FAME) is produced by the transesterification of triglycerides (TG) of refined/edible type oils using methanol and an homogeneous alkaline catalyst. However, production costs are still rather high compared with the ones of petroleum-based diesel fuel. To lower costs and make biodiesel competitive less-expensive feedstocks such as waste fats or non-edible type oils could be used. The use of homogeneous alkaline catalysts in the transesterification of such types of fats and oils poses great difficulties due to the presence of large amounts of free fatty acids (FFA). This paper studies the use of carboxylic salts as a possible alternative, because these catalysts are active also in the presence of high FFA concentrations. The most active catalyst (Cd, Mn, Pb, Zn carboxylic salts) have been individuated and a correlation of the activities with the cation acidity has been found.
- Di Serio,Tesser,Dimiccoli,Cammarota,Nastasi,Santacesaria
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p. 111 - 115
(2008/10/09)
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- Zinc acrylate particle composition, method for production thereof, and golf ball using the composition
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A zinc acrylate particle composition which is substantially fine and, even when kneaded with a rubber composition, is capable of being uniformly dispersed and kneaded in a state very rarely inducing fast adhesion or agglomeration, a method for the production thereof, and a golf ball using the composition are provided. The zinc acrylate particle composition contemplated by this invention comprises zinc acrylate satisfying the conditions that the proportion accounted for by the zinc acrylate particles measuring not less than 300 μm in particle size as determined by the dry type method be not more than 20% by mass of all the particles, that the median of particle sizes as determined by the dry type method be in the range of 10-300 μm, and that the ratio of the median (A) of particle sizes as determined by the dry type method to the median (B) of particle sizes as determined by the wet type method exceed 2, and an anionic surfactant.
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- High skin friction cosmetic creams containing dispersed zinc oxide particles as inorganic sunscreen
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A high skin friction cosmetic composition that can provide the consumer-desired sensory properties of traditional vanishing creams, containing solid asymmetric particles and ZnO incorporated by an inventive process. According to the inventive process the temperature during the mixing of ZnO and asymmetric particles is controlled at less than 80° C. and the time of mixing is limited to about 10 minutes. After about 10 minutes, the reaction is quenched by cooling to about 50° C.
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- High shear process for making metallic esters
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A process to make a metallic ester which comprises:(a) mixing at least one metallic salt with at least one partially heated acidic organic moiety form a heated slurry at a first temperature;(b) reacting said slurry under shear conditions to form a micro-emulsion for no longer than about two minutes at a second higher temperature to form a pumpable metallic ester; and(c) collecting said metallic ester.
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Page/Page column 4-5
(2008/06/13)
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- Preparation of metal carboxylates and their stabilizing performance under intense high-pressure shear treatment
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Solid-phase synthesis of certain metal carboxylates and their effect on stabilization of polyvinyl chloride under intense high-pressure shear treatment were studied.
- Akhmetkhanov,Kolesov,Kadyrov,Karmilov,Zaikov
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p. 842 - 845
(2007/10/03)
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- Process for preparing fatty acid zinc salts
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A process for preparing fatty acid zinc salts comprising the steps of:stirring a slurry mixture comprising zinc oxide, at least one catalyst, and water at a temperature in the range of from about 55° C. to about 65° C.; adding at least one fatty acid in its liquid state to said stirred slurry mixture; and reacting the fatty acid with the zinc oxide in the presence of the catalyst in the water at a temperature of from about 60° C. to about 75° C. until substantially all of the fatty acid has reacted. The final product mixture can then be filtered and dried to give a fatty acid zinc salt in high yield.
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Page column 5
(2008/06/13)
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- Zinc acrylate particle composition, method for production thereof, and golf ball using the composition
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A zinc acrylate particle composition which is substantially fine and, even when kneaded with a rubber composition, is capable of being uniformly dispersed and kneaded in a state very rarely inducing fast adhesion or agglomeration, a method for the production thereof, and a golf ball using the composition are provided. The zinc acrylate particle composition contemplated by this invention comprises zinc acrylate satisfying the conditions that the proportion accounted for by the zinc acrylate particles measuring not less than 300 μm in particle size as determined by the dry type method be not more than 20% by mass of all the particles, that the median of particle sizes as determined by the dry type method be in the range of 10-300 μm, and that the ratio of the median (A) of particle sizes as determined by the dry type method to the median (B) of particle sizes as determined by the wet type method exceed 2, and an anionic surfactant.
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- Method for production of zinc acrylate
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A method is provided for the production of zinc acrylate which possesses an essentially fine constitution, permits easy pulverization into a fine powder, and, when kneaded with a rubber composition, attains uniform diffusion in a state very rarely inducing fast adhesion or formation of cluster. The fine zinc acrylate powder is obtained by a method which comprises causing acrylic acid and a higher fatty acid of 12-30 carbon atoms to react with zinc oxide in an organic solvent while continuing dispersion of the zinc oxide in the organic solvent in the presence of an anionic surfactant.
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- Aspects of the Inorganic Chemistry of Rubber Vulcanisation. Part 4. Dialkyl- and Diaryl-dithiophosphate and -dithiophosphinate Complexes of Zinc: Phosphorus-31 Nuclear Magnetic Resonance Spectral Studies and Structures of 4>2P(OC6H4Me-p)2)3> and 4>2PPh2
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The complexes 4>2P(OC6H4Me-p)2)3> and 4>2PPh2)3> have been prepared by treatment of 2PR2)2> with (NR'4>2PR2> (R=OC6H4Me-p or Ph, R'=Me or Et).Preparation of 2(S2P(OPri)2)>- and 2PR2)2(S2CNMe2)>- (R=OC6H4Me-p or Ph) is also described.From reactions of 2P(OR)2)2> (R=Pri or C6H4Me-p) with H2O2 or ButO(OH), zinc phosphates and ZnSO4 have been obtained, and 2P(OPh)2)2> and 2P(OPh)2)3>- react with ROH (R=Et or Pri) in solution to give amongst other products 2P(OR)2)2> and 2P(OR)2>- with loss of phenol.The 31P n.m.r. spectra of a series of dialkyl- and diaryl-dithiophosphate and -phosphinate complexes have been recorded and used to establish rapid exchange within the equilibrium 2P(OR)2)3>- 2P(OR)2)2> + 2P(OR)2>-.The structures of the title compounds have been determined crystallographically: 4>2P(OC6H4Me-p)2)3> is monoclinic with a=29.311(9), b=11.032(3), c=17.515(5) Angstroem, β=106.83(2) deg, space group P21/a, Z=4, and 2490 reflections give R 0.0532; 4>2PPh2)3> is monoclinic with a=11.160(6), b=9.962(5), c=43.11(3) Angstroem, β=104.73(5) deg, space group P21/c, Z=4, and 3304 reflections give R 0.0411.Both have slightly distorted tetrahedral geometries in which one S2PR2 ligand is bidentate, and the other two are unidentate.
- McCleverty, Jon A.,Kowalski, Rick S. Z.,Bailey, Neil A.,Mulvaney, Robert,O'Cleirigh, Donal A.
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p. 627 - 634
(2007/10/02)
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- Aspects of the Inorganic Chemistry of Rubber Vulcanisation. Part 1. Reactions of Zinc Bis(dithiocarbamates) and Bis(benzothiazole-2-thiolates) with Carboxylates, and the Structure of 2(μ-OCOMe)>
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Reaction of with (R=Me or n-Bu; R'=Me, Et, n-Pr, or n-Bu) gives -, but when R'=n-C5H11, n-C6H13, n-C7H15, n-C8H17, or C17H35, only has been isolated.Treatment of n> (
- McCleverty, Jon A.,Spencer, Neil,Bailey, Neil A.,Shackleton, Stephen L.
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p. 1939 - 1944
(2007/10/02)
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