Study on Crosslinking in Diimide Reduction of Nitrile Butadiene Rubber

2006 ◽  
Vol 79 (4) ◽  
pp. 602-609
Author(s):  
Shuqin Zhou ◽  
Shaoyi Li ◽  
Huadong Bai

Abstract Acrylonitrile-butadiene rubber (NBR) in latex form was selectively hydrogenated by redox system consisting of hydrazine hydrate and hydrogen peroxide, with boric acid as catalyst. Soluble hydrogenated NBR latex was obtained; but the coagulated products were gelled on drying. This problem becomes the major obstacle for the hydrogenation technique to be commercialized. It is important to study the crosslinking reaction in the system and to solve the problem. The cause for the crosslink was investigated in three possibilities: (i) crosslinking caused by the hydrogenation of CN group; (ii) by the oxidation of C=C double bonds and (iii) by radicals in the system. The control of the crosslink was also studied. The oil resistant nitrile group —CN on the polymer chain had no change during drying process. There were no signs of carbonyl group C=O formed by oxidation and amine like groups -NH- formed by the hydrogenation of CN in HNBR gel fraction. The newly formed alkoxyl radicals were detected by ESR spectroscopy analysis in the hydrogenation system after specific reaction time. Crosslinking reaction was controlled to a large extent by using hydroquinone as gel inhibitor.

2006 ◽  
Vol 11-12 ◽  
pp. 391-394
Author(s):  
Zeng Yan Wei ◽  
Dong Mei Yue ◽  
Xiao Ting Mo ◽  
Li Qun Zhang

Hydrogenation of neoprene (CR) latex was carried out by utilization of diimide with boric acid as a catalyst. Various hydrogenation conditions were studied and the hydrogenation degree could reach 48.1%. The most effective ratio of hydrogen peroxide/hydrazine hydrate was 0.8. The hydrogenation degree increased with increasing the temperature, the amount of boric acid and hydrazine hydrate. However, it decreased as prolonging the reaction time. The gel content was also investigated. Microstructure of hydrogenated neoprene (HCR) was characterized by IR and 1HNMR.


1990 ◽  
Vol 55 (10) ◽  
pp. 2377-2380
Author(s):  
Hamza A. Hussain

Nitroxide free radicals prepared from diethylamine, piperidine and pyrrolidine by oxidation with hydrogen peroxide were studied by ESR spectroscopy. The changes in the 14N splitting constant (aN) caused by the addition of KBr or tetraethylammonium bromide were measured in dependence on the concentration of the ions. For diethylamine nitroxide and piperidine nitroxide, the results are discussed in terms of two equilibria: the one, involving the anion, is associated with a gain or loss of hydrogen bonds to the nitroxide oxygen atom, the other is associated with the formation of solvent shared units involving the cation, which results in changes in the hydrogen bonding strenght. The large increase in the aN value in the case of pyrrolidine nitroxide is explained in terms of an interaction from one side of the positively charged N atom; the increase in aN in the case of diethylamine and piperidine nitroxides is explained in terms of interactions with both sides of the positively charged N atom.


2021 ◽  
Vol 597 ◽  
pp. 94-103
Author(s):  
Manoj P. Rayaroth ◽  
Dasom Oh ◽  
Chung-Seop Lee ◽  
Nitee Kumari ◽  
In Su Lee ◽  
...  

2015 ◽  
Vol 17 (4) ◽  
pp. 23-31 ◽  
Author(s):  
Agnieszka Wróblewska ◽  
Edyta Makuch ◽  
Małgorzata Dzięcioł ◽  
Roman Jędrzejewski ◽  
Paweł Kochmański ◽  
...  

Abstract This work presents the studies on the optimization the process of allyl alcohol epoxidation over the Ti-SBA-15 catalyst. The optimization was carried out in an aqueous medium, wherein water was introduced into the reaction medium with an oxidizing agent (30 wt% aqueous solution of hydrogen peroxide) and it was formed in the reaction medium during the processes. The main investigated technological parameters were: the temperature, the molar ratio of allyl alcohol/hydrogen peroxide, the catalyst content and the reaction time. The main functions the process were: the selectivity of transformation to glycidol in relation to allyl alcohol consumed, the selectivity of transformation to diglycidyl ether in relation to allyl alcohol consumed, the conversion of allyl alcohol and the selectivity of transformation to organic compounds in relation to hydrogen peroxide consumed. The analysis of the layer drawings showed that in water solution it is best to conduct allyl alcohol epoxidation in direction of glycidol (selectivity of glycidol 54 mol%) at: the temperature of 10–17°C, the molar ratio of reactants 0.5–1.9, the catalyst content 2.9–4.0 wt%, the reaction time 2.7–3.0 h and in direction of diglycidyl ether (selectivity of diglycidyl ether 16 mol%) at: the temperature of 18–33°C, the molar ratio of reactants 0.9–1.65, the catalyst content 2.0–3.4 wt%, the reaction time 1.7–2.6 h. The presented method allows to obtain two very valuable intermediates for the organic industry.


2017 ◽  
Vol 19 (1) ◽  
pp. 11-16 ◽  
Author(s):  
Shuang Zhang ◽  
Long Zhang

Abstract In this paper, 2,5-furandicarboxylic acid (FDCA) was efficiently prepared by the direct oxidation of 5-hydroxymethylfurfural (5-HMF) using hydrogen peroxide (H2O2) in alkaline conditions without any catalysts. The effects of reaction parameters on the process were systematically investigated and the optimal parameters were obtained as follows: molar ratio of 5-HMF:KOH:H2O2 was 1:4:8, reaction temperature and reaction time were determined as 70°C and 15 minutes, respectively. Under these conditions, the yield of FDCA was 55.6% and the purity of FDCA could reach 99%. Moreover, we have speculated the detailed oxidation mechanism of 5-HMF assisted by hydrogen peroxide in alkaline condition to synthesize FDCA.


Catalysts ◽  
2020 ◽  
Vol 10 (9) ◽  
pp. 1078
Author(s):  
Hang Zhang ◽  
Zhipeng Ma ◽  
Yunpeng Min ◽  
Huiru Wang ◽  
Ru Zhang ◽  
...  

Several kinds of composite materials with phosphotungstic acid (PTA) as the catalyst were prepared with activated carbon as support, and their structures were characterized. According to the Box–Behnken central combination principle, the mathematical model of the heterogeneous system is established. Based on the single-factor experiments, the reaction temperature, the reaction time, the amount of hydrogen peroxide and the loading capacity of PTA were selected as the influencing factors to study the catalyzed oxidation of hydrogen peroxide and degradation of high molecular weight chitosan. The results of IR showed that the catalyst had a Keggin structure. The results of the mercury intrusion test showed that the pore structure of the supported PTA catalyst did not change significantly, and with the increase of PTA loading, the porosity and pore volume decreased regularly, which indicated that PTA molecules had been absorbed and filled into the pore of activated carbon. The results of Response Surface Design (RSD) showed that the optimum reaction conditions of supported PTA catalysts for oxidative degradation of high molecular weight chitosan by hydrogen peroxide were as follows: reaction temperature was 70 ℃, reaction time was 3.0 h, the ratio of hydrogen peroxide to chitosan was 2.4 and the catalyst loading was 30%. Under these conditions, the yield and molecular weight of water-soluble chitosan were 62.8% and 1290 Da, respectively. The supported PTA catalyst maintained high catalytic activity after three reuses, which indicated that the supported PTA catalyst had excellent catalytic activity and stable performance compared with the PTA catalyst.


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