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Continuous hydrogenation production device and method for carbon-carbon double bonds in conjugated diene polymer

A conjugated diene, polymer technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, ruthenium organic compounds, etc., can solve the problem of high warehouse costs, building and operation management costs, large Working capital, etc.

Pending Publication Date: 2020-10-16
山东京博中聚新材料有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, warehouses are expensive not only because of their building and operating overhead, but also because of the large amount of working capital

Method used

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  • Continuous hydrogenation production device and method for carbon-carbon double bonds in conjugated diene polymer
  • Continuous hydrogenation production device and method for carbon-carbon double bonds in conjugated diene polymer
  • Continuous hydrogenation production device and method for carbon-carbon double bonds in conjugated diene polymer

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preparation example Construction

[0151] The preparation method of the catalyst for catalytic hydrogenation of conjugated diene latex is characterized in that it comprises the following steps:

[0152] In the Shrek system, an inert gas atmosphere is used to mix the Grubbs catalyst and the ligand. The molar mass ratio of the Grubbs catalyst to the ligand is 1:1-1:20, and the Grubbs catalyst is Grubbs Ⅱ catalyst or Grubbs Ⅲ catalyst, add organic solvent, react at 20-80°C for 0.1-24h or 4-10d, the reaction condition is reflux reaction or stirring reaction, under vacuum condition, remove the organic solvent , collected the solid, washed, and dried in vacuo to obtain the catalyst.

[0153] The mass percentage of the catalyst in the present invention in the polymer in the conjugated diene latex is 0.0001% to 5wt%; preferably 0.001wt% to 4wt%; more preferably 0.01wt% to 3wt%; most preferably 0.01wt% %~0.5wt%.

[0154] The auxiliary agent is selected from one or more of linear (alkene) acid salts, linear alkyl sulfa...

Embodiment 1-1

[0166] A preparation method of a catalyst for catalytic hydrogenation of conjugated diene latex of the present invention comprises the following steps: in the Shrek system, using a nitrogen gas atmosphere, 0.1 mmol of the Grubbs II catalyst and a ligand 2-(3 -Butene)pyridine 0.2mmol mixed, add organic solvent dichloromethane 15mL, at 20 ℃, heat reflux 4h, under vacuum condition, remove organic solvent dichloromethane, collect solid, adopt hexane to wash, wash three times, each time The amount of hexane was 5 mL, and it was dried under vacuum to obtain a light green solid, which was designated as catalyst IVa.

[0167] After measuring, this catalyst IVa is 0.063mmol, and yield is 63%, and its structural formula is as follows:

[0168]

Embodiment 1-2

[0170] A preparation method of a catalyst for catalytic hydrogenation of conjugated diene latex of the present invention comprises the following steps: in the Shrek system, using an argon gas atmosphere, 0.1 mmol of the Grubbs II catalyst and a ligand 2-( 3-butene) pyridine 1.4mmol mixed, add organic solvent dichloromethane 15mL, at 80 ℃, heat reflux 24h, under vacuum condition, remove organic solvent dichloromethane, collect solid, adopt hexane to wash, wash three times, every The amount of hexane was 5 mL, and it was vacuum-dried to obtain a light green solid, which was designated as catalyst IVa.

[0171] After measuring, this catalyst IVa is 0.080mmol, and yield is 80%, and its structural formula is as follows:

[0172]

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Abstract

The invention provides a continuous hydrogenation method of carbon-carbon double bonds in a conjugated diene polymer, which comprises the following steps: mixing conjugated diene latex, a catalyst andan assistant in a raw material pretreatment kettle to obtain a mixture; wherein the catalyst is a group VIII metal compound shown as a formula (I); filtering the mixture, mixing with hydrogen generated by a hydrogen generation device, preheating by a preheater, and reacting in a hydrogenation reactor to obtain a hydrogenated copolymer; subjecting the hydrogenated copolymer to heat exchange through the raw material preheater and gas-liquid separation through the gas-liquid separation tank, and conveying hydrogenated copolymer latex at the bottom of the tank to the product tank through the product conveying pump. A novel hydrogenation catalyst is adopted and combined with devices such as a tubular reactor, so that the selective hydrogenation reaction of conjugated diene can be efficiently realized, and a high-hydrogenation-degree product with the hydrogenation degree higher than 95% is obtained. According to the method, a continuous hydrogenation mode is adopted, so that the product stability between batches can be improved, and the production efficiency and the process safety are improved; according to the invention, the reaction conditions are mild.

Description

technical field [0001] The invention relates to the technical field of catalytic hydrogenation, in particular to a continuous hydrogenation production device and method for carbon-carbon double bonds in conjugated diene polymers. Background technique [0002] Currently, the hydrogenation of polymer-based dienes using one catalyst is usually achieved by a semi-batch process. Chemical reactions can be performed in batch mode, continuous mode or semi-batch mode. Until now, the hydrogenation of dienes based on polymers using one catalyst was usually achieved by a semi-batch process. [0003] US-B 5,561,197 and US-B 5,258,467 teach the production of hydrogenated polymers in a semi-batch mode using organo-metallic catalysts. [0004] Most often, however, a continuous approach is more favorable in terms of operation, maintenance, production and cost. In general, the most common types of reactors used in a continuous process are continuous stirred tank reactors and tubular reacto...

Claims

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Application Information

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IPC IPC(8): C07F15/00B01J31/22C08C19/02
CPCC07F15/0046B01J31/2278B01J31/2273C08C19/02B01J2531/821B01J2531/0233B01J2531/0238B01J2231/645
Inventor 周德芳王辉黎艳艳曹峰郭宗磊佟伟超王传齐杜庆之李泽珊郝福兰刘振学蔡颖辉栾波
Owner 山东京博中聚新材料有限公司
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