Method for normal-pressure hydrogenation of unsaturated polymer using magnetic nano ferroferric oxide catalyst
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A ferric oxide, magnetic nanotechnology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., can solve problems affecting performance and other issues
Active Publication Date: 2013-02-06
BEIJING UNIV OF CHEM TECH
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The hydrogenation methods of unsaturated polymers studied by previous studies all use water-soluble homogeneous inorganic catalysts, such as copper sulfate, boric acid, and ferrous sulfate. However, water-soluble catalysts will continue to remain in the polymerization after the hydrogenation reaction is completed. In the later use of the polymer, it will inevitably affect its performance
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Embodiment 1
[0022] Add 100mL nitrile latex to the three-neck round bottom flask (system pH is 9.2, solid content is 40%), the reaction temperature is raised to 70°C, keep the temperature constant, add 23.6mL hydrazine hydrate (the molar ratio of hydrazine hydrate to carbon-carbon double bond 15:1), the addition amount of nano ferric oxide is 0.0g, 0.5g, 1.0g, 1.5g, 2.0g, 3.0g respectively, under the stirring speed of 400r / min, under air condition, react for 12h, After the hydrogenation reaction was completed, demulsify with isopropanol, dry, measure the infrared spectrum, and calculate the degree of hydrogenation. The results of the degree of hydrogenation are shown in Table 1.
[0023] Table 1 Effect of the addition amount of nano-Fe3O4 on the degree of hydrogenation
[0024]
Embodiment 2
[0026] Other conditions are the same as in Example 1, the addition of nanometer iron ferric oxide is 2.0g, change the mol ratio of hydrazine hydrate and carbon-carbon double bond, be respectively 3:1, 4:1, 5:1, 8:1,12 :1, 15:1, its hydrogenation degree results are shown in Table 2.
[0027] Table 2 Effect of the molar ratio of hydrazine hydrate to carbon-carbon double bond on the degree of hydrogenation
[0028]
Embodiment 3
[0030] Other conditions are the same as in Example 1, the addition amount of nanometer iron ferric oxide is 2.0g, the addition amount of hydrazine hydrate is 7.9mL (the molar ratio of hydrazine hydrate and carbon-carbon double bond is 5:1), change the stirring speed of the system, They are 200r / min, 300r / min, 400r / min, 500r / min respectively, and the hydrogenation degree results are shown in Table 3.
[0031] Table 3 Effect of stirring speed on degree of hydrogenation
[0032]
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Abstract
The invention discloses a method for normal-pressure hydrogenation of an unsaturated polymer using a magnetic nano ferroferric oxide catalyst. The method is characterized by comprising the following steps of: adding latex or glue solution of an unsaturated polymer into a reaction container, heating up to 30-90 DEG C, adding reducing agent hydrazine hydrate and the magnetic nano ferroferric oxide catalyst into a hydrogenation system, stirring for hydrogenation reaction under the condition of air, and preparing the hydrogenated polymer after reaction for 1-24h, wherein the unsaturated polymer system is nitrile latex or butyl benzene latex, or solution of nitrile rubber or solution of isoprene rubber. The method uses the nano ferroferric oxide catalyst in a solution hydrogenation system and an emulsion hydrogenation system of a macromolecular unsaturated polymer for the first time, and after the hydrogenation reaction is completed, nano ferroferric oxide is recycled through simple filtering and washed with deionized water for reuse, and redundant hydrazine hydrate is removed by generating nitrogen and water by-products so as to prepare a very pure hydrogenated product.
Description
Technical field: [0001] The invention relates to a catalyst for in-situ normal pressure hydrogenation of unsaturated polymers, which selectively hydrogenates the carbon-carbon double bonds on the molecular chains of unsaturated polymers, including the emulsion hydrogenation system of unsaturated polymers and solution hydrogenation system. Background technique: [0002] Unsaturated polymers, such as nitrile rubber, styrene-butadiene rubber, and isoprene rubber, contain unsaturated carbon-carbon double bonds, and their chemical properties are relatively active. Cross-linking or chain breaking occurs under the action of oxygen, ozone, and light. It affects the performance of rubber and limits the scope of use of unsaturated polymers. In order to solve this problem, unsaturated polymers are hydrogenated and modified. During the hydrogenation process, the carbon-carbon double bonds on the unsaturated molecular chains are partially hydrogenated or completely hydrogenated, thereby...
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