[Study on the Preparation of N-Tert-Butylbenzothiazole-2-Sulphenamide and Its Spectral Analysis].

In the study, N-tert-butylbenzothiazole-2-sulphenamide (TBBS) was synthesized with one-step method with hydrogen peroxide as the oxidant. TBBS was detected and characterized with FTIR，UV-Vis，XRD and TG-DSC. Its micro-structure and intrinsic regularity were revealed. Chemical bond types into TBBS molecule were revealed with FTIR. The final product was determined TBBS. Three absorption peaks were detected by UV-Vis at 228.3，281.5，298.3 nm respectively, due to n→σ*，π→π*，n→π* electronic transitions. It could provide experimental basis with enterprise to test TBBS product quality and speculate its structure. The phase composition and structure of TBBS were revealed by crystallographic data from XRD detecting such as cell parameters, crystal face index. The phase composition and qualitative identification of TBBS structure were completed. Two kinds of information were detected by TG-DSC as quality change and thermal effect. The DSC curve of TBBS was very complex. There were a small absorption peak of 53.3 ℃ as a small amount of tert-butylamine containing in TBBS was oxidized. Three exothermic peaks of 117.4，269.2，373.7 ℃, due to transition peak and decomposition phase of TBBS respectively. The decomposition temperature of TBBS was very high. It could provide reference for research on rubber vulcanizing properties by TBBS on rubber vulcanizing machine. This study could provide the basis experimental data on the enterprises to designate the working standard tracing detection of TBBS industrialized production. The performance index of TBBS was judged. The project of TBBS industry standard could be declared by the enterprises, written a draft standard.

[Preparation of Rubber Accelerator Tetraisobutylthiuram Monosulfide and Its Spectral Analysis].

In the study, rubber accelerator tetraisobutylthiuram monosulfide (TiBTM) was synthesized by two-step method with hydrogen peroxide as oxidant firstly. TiBTM was detected and characterized by FTIR, XRD, TG-DSC. Its micro-structure and intrinsic regularity were revealed. Chemical bond types into TiBTM molecule were revealed by FTIR. TiBTM phase composition and structure were given by crystallographic data from XRD detecting such as cell parameters, crystal face index. The phase composition and qualitative identification of TiBTM structure were completed. Two kinds of information were detected by TG-DSC as quality change and thermal effect. TiBTM phase transition and decomposition temperature were 75.1 and 287.0 ℃ respectively. Uhe decomposition temperature of TiBTM was very high, samples possessing with high purity, without other impurities. It could provided reference with research on rubber vulcanizing and multiple functional properties by TiBTM on rubber vulcanizing machine. This study can provide the basis experimental data on the enterprises to designate the working standard tracing detection of TiBTM industrialized production. The best technological conditions and parameters could be provided for the enterprises to adopt cleaner production process of TiBTM. Performance index of TiBTM was judged. The project of TiBTM industry standard can be declared by the enterprises, written a draft standard.

[Preparation of Zinc O,O,O',O'-Tetrabutyl Bis(Phosphorodithioate) and Its Spectral Analysis].

In the study, zinc O,O,O',O'-tetrabutyl bis(phosphorodithioate) (ZBPD) was synthesized with two-step method firstly. ZBPD was detected and characterized with UV-vis, FT-IR andTG-DSC. Its micro-structure and intrinsic regularity were revealed. Two absorption peaks were detected with UV-Vis at 212.0 and 227.0 nm respectively caused by n→σ*, π→π* electron transition. The intensity of peaks was changed with the regularity with different ZBPD concentration. It could provide the basic data with the enterprise of ZBPD product quality inspection. Chemical bond types into ZBPD molecule were revealed by FT-IR. Two kinds of information were detected by TG-DSC as quality change and thermal effect. The DSC curve of ZBPD was very complex. There were a wide absorption peak of 84.3 ℃, four exothermic peaks of 245.0, 344.3, 476.1, 344.3 ℃, due to the molecular structure of ZBPD and small amounts of impurities. The decomposition temperature of ZBPD was very high. It could provided reference with research on rubber vulcanizing properties by ZBPD on rubber vulcanizing machine. This study could provide the basis experimental data on the enterprises to designate the working standard tracing detection of ZBPD industrialized production. Performance index of ZBPD was judged. The project of ZBPD industry standard could be declared by the enterprises, written a draft standard.

[Preparation of TBSI with NS-Acetic Anhydride Method and Its Spectral Analysis].

In the study, N-t-butyl-2-benzothiazole sulfenimide (TBSI) was prepared by NS-acetic anhydride method with acetic anhydride as solvent. It was detected with FTIR, XRD, UV-Vis, TG-DTA. Micro-structure and essence disciplinarian of them were disclosed. Chemical bond types into TBSI molecule were revealed with FTIR. TBSI phase composition and structure were revealed with crystallographic data from XRD detecting such as cell parameters and crystal face index. The phase composition and qualitative identification of TBSI structure were completed. The absorption peaks were detected by UV-vis at 228.3, 281.3 and 298.3 nm, respectively caused by n→σ*, π→π*, n→π* electron transition. It could provide basic data with the enterprise of ZBPD product quality inspection. Two kinds of information were detected with TG-DTA as quality change and thermal effect. There were three absorption peaks of 46.5, 188.9, 368. 5 ℃ due to a few residual solvent volatilization in the sample, phase transition peak and decomposition peak. The decomposition temperature of TBSI was very high. It could provided reference with research on rubber vulcanizing properties with TBSI on rubber vulcanizing machine. This study could provide basis experimental data on the enterprises to designate the working standard tracing detection of TBSI industrialized production. Performance index of TBSI was judged. The project of TBSI industry standard could be declared by the enterprises, written a draft standard.

Poly[(2,2'-bipyridine-κN,N')(µ(3)-2,4,6-trimethyl-isophthalato-κO,O:O:O,O)cadmium].

In the crystal structure of the polymeric title complex, [Cd(C(11)H(10)O(4))(C(10)H(8)N(2))](n), the Cd(II) cation is chelated by one 2,2-bipyridine ligand and two carboxyl groups from two trimethyl-isophthalate (TMIPA) anions, and is further coordinated by one carboxyl-ate O atom from a third TMIPA anion, forming a distorted penta-gonal-bipyramidal geometry. Each TMIPA anion bridges three Cd(II) cations, forming polymeric complex sheets parallel to (001). Weak C-H⋯O hydrogen bonding occurs between adjacent sheets.

Piperazine-1,4-diium diacetate.

In the title salt, C(4)H(12)N(2) (2+)·2C(2)H(3)O(2) (-), the piperazine-1,4-diium cation has 2/m symmetry with the NH(2) unit located on a mirror plane and the acetate anion has m symmetry with all non-H atoms and one H atom located on a mirror plane. The piperazine ring adopts a chair conformation. In the crystal, the cations are linked with the anions via N-H⋯O hydrogen bonding into chains parallel to the c axis.

N-(2-Hy-droxy-benz-yl)adamantan-1-aminium 4-methyl-benzene-sulfonate.

In the crystal structure of the title salt, C(17)H(24)NO(+)·C(7)H(7)O(3)S(-), the N-(2-hy-droxy-benz-yl)adamantan-1-aminium cations and 4-methyl-benzene-sulfonate anions are linked by O-H⋯O and N-H⋯O hydrogen bonds. C-H⋯π inter-actions are also observed between the cation and the anion.

4-[(2-Hy-droxy-naphthalen-1-yl)(morpholin-4-yl)meth-yl]benzonitrile.

The title compound, C(22)H(20)N(2)O(2), was synthesized via a multicomponent reaction using naphthalen-2-ol, morpholine and 4-formyl-benzonitrile. The dihedral angle between the naphthalene ring system and the benzene ring is 81.25 (10)°. The morpholine ring adopts a chair conformation. The mol-ecular conformation is stabilized by intra-molecular O-H⋯N and C-H⋯O hydrogen bonds. In the crystal, inter-molecular C-H⋯N hydrogen bonds link mol-ecules into helical chains running parallel to the c axis.

Syntheses, crystal-solution structures and magnetic properties of a series of decanuclear heterometallic [LnCoCo] (Ln = Eu, Gd, Tb, Dy) clusters.

Four unprecedented decanuclear heterometallic [Ln2CoII4CoIII4] clusters based on a diethanolamine ligand (H2dea), namely [Eu2CoII4CoIII4(dea)8(HCOO)4(OH)2(Cl)2(CH3OH)2]Cl2·4CH3OH·2H2O (1), [Gd2CoII4CoIII4(dea)8(HCOO)4(OH)2(Cl)2(CH3OH)2]Cl2·4CH3OH·2H2O (2), [Tb2CoII4CoIII4(dea)8(HCOO)4(OH)2(Cl)2(CH3OH)2]Cl2·2CH3OH·4H2O (3) and [Dy2CoII4CoIII4(dea)8(HCOO)4(OH)2(Cl)2(CH3OH)2]Cl2·2CH3OH·4H2O (4) were synthesized through a facile solution method. Single-crystal X-ray diffraction analyses reveal that complexes 1-4 consist of a [Ln2CoII4CoIII4] core, which is constructed by bridging a quasi-double cuboidal [Ln2CoII2CoIII2] core with two [CoIICoIII] units. Electrospray ionization mass spectrometry (ESI-MS) using methanol solution reveals that complexes 1-4 are stable in the solution, and the clusters undergo three different substitution reactions (Cl- replaced by OH-, OH- replaced by CH3O- and HCOO- replaced by OH-/CH3O-) at the same time in the ionization state. Magnetic susceptibilities reveal ferromagnetic couplings within complexes 3 and 4, and the magnetocaloric effect (MCE) for 2 was also evaluated and the maximum entropy change (-ΔSm) value reaches 16.3 J kg-1 K-1 at about 3 K and 5 T.

Distribution and fate of nonylphenol in an aquatic microcosm.

An aquatic microcosm consisting of four compartments, namely surface microlayer (SM), water sediment and biota (zebra fish), was developed to investigate the distribution and fate of nonylphenol (NP) in an aquatic environment. Level III and level IV fugacity-based multimedia models were used to calculate the distribution and fate of NP. Data obtained from model calculations were in good agreement with those of the experiments. Results of the model calculations showed that 86.50% of all NP input was removed by advective outflow, while 61.99% of the remainder was distributed to the sediment phase, 34.89% to the water phase, 2.50x10(-2)% to SM and 3.13% to the biotic phase. This finding demonstrates that sediment plays a key role in the fate of NP and acts as a sink in the aquatic environment. Bioconcentration factor (BCF) of NP in the zebra fish was high and varied in different parts of the fish. The highest BCF was 1440 in the viscera. After the uptake experiment, depuration of NP in clean water indicated that, the concentration of residue NP in the zebra fish was still high. This implies that NP in fish can pose a potential threat to human health due to its bioaccumulation in the food chain.

Sorption of small metabolites of nonylphenol polyethoxylates in single and complex systems on aquatic suspended particulate matter.

Sorption of nonylphenol (NP), nonylphenol monoethoxylate (NP1EO) and nonylphenol diethoxylate (NP2EO) as well as their binary and ternary mixtures were studied and compared on three simulated suspended particulate matters (SPMs). Sorption dynamics of NP on the three SPMs could be divided into two phases, the rapid sorption phase and the slow sorption phase. A third phase, 'apparent desorption' occurred before the slow sorption phase for NP1EO and NP2EO as well as for all mixtures. Initial sorption rate increased with the OC% content of the SPMs. At low concentration, the sorption of NP, NP1EO and NP2EO (only at low concentration for 3# SPM) followed linear isotherm on the three SPMs. The linear Kd value of NP or NP1EO increased with the OC% content of SPM. In mixtures, sorption of NP, NP1EO and NP2EO increased significantly, and a 'critical point', after which sorption increased significantly, was observed in certain sorption isotherms.