Polar-reversible transformation solvent for isobutylene hydroformylation reaction

An isobutylene hydroformyl and reversible technology, applied in the chemical industry, can solve the problems of volatile solvent loss and high energy consumption, and achieve the effect of reducing energy consumption

Active Publication Date: 2015-04-29
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to address the above technical problems, to provide a method that can solve the problems of high energy consumption and solvent volatile loss in the traditional solvent and product separation process, which can be solved under normal temperature and pressure conditions. The nature of the reversible change of the polarity of the solvent realizes the separation of the solvent and the product and the recovery of the solvent, which reduces energy consumption and does not have a solvent loss. A polarity reversible change solvent is used in isobutylene hydroformylation reaction

Method used

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  • Polar-reversible transformation solvent for isobutylene hydroformylation reaction

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Experimental program
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Effect test

Embodiment 1

[0018] In a 250mL autoclave, add about 0.2g triphenylphosphinecarbonyl rhodium catalyst and 90mL CyNMe 2 As a solvent, the N 2 After replacement, fill in about 45g of isobutene, and then fill in a certain amount of mixed gas (CO / H 2 Volume ratio, 55:45), the temperature was raised to 100°C, and the reaction was carried out at 2.5MPa for 2h, and the rotation speed was 350rpm. After the reaction, the system was cooled to room temperature, about 100 mL of water was added to the system, and CO was passed at a flow rate of 200 mL / min. 2 After 30min, the solvent entered into the aqueous phase and separated from the organic phase of the product. The product phase is further separated and purified, and the yield of the obtained isovaleraldehyde is 70%, and the purity of the isovaleraldehyde product is 98%, wherein the nitrogen content is lower than 0.1%. The water phase was passed through N at a flow rate of 200mL / min 2 1 h, solvent CyNMe 2 It is dissociated from the water phase...

Embodiment 2

[0020] In a 250mL autoclave, add about 0.2g triphenylphosphinecarbonylrhodium catalyst and 100mL CyNMe 2 As a solvent, the N 2 After replacement, fill in about 45g of isobutene, and then fill in a certain amount of mixed gas (CO / H 2 Volume ratio, 55:45), the temperature was raised to 100°C, and the reaction was carried out at 2.5MPa for 2h, and the rotation speed was 350rpm. After the reaction, the system was cooled to room temperature, about 100 mL of water was added to the system, and CO was passed at a flow rate of 200 mL / min. 2 After 20min, the solvent enters the aqueous phase and separates the organic phase of the product. The product phase is further separated and purified, and the yield of isovaleraldehyde obtained is 65%, and the purity of the isovaleraldehyde product is 95%, wherein the nitrogen content is 2%. The water phase was passed through N at a flow rate of 200mL / min 2 1 h, solvent CyNMe 2 It is dissociated from the water phase and used for the next reac...

Embodiment 3

[0022] In the autoclave of 500mL, add about 0.35g triphenylphosphine carbonyl rhodium catalyst and 170mLCyNMe 2 As a solvent, the N 2 Fill in about 80g of isobutene after replacement, and then fill in a certain amount of mixed gas (CO / H 2 , 55:45), the temperature was raised to 100°C, and the reaction was carried out at 2.5MPa for 2h with a rotation speed of 350rpm. After the reaction, the system was cooled to room temperature, about 200 mL of water was added to the system, and CO was passed at a flow rate of 200 mL / min. 2 After 50min, the solvent entered into the aqueous phase and separated from the organic phase of the product. The product phase is further separated and purified, and the yield of the obtained isovaleraldehyde is 63%, and the purity of the isovaleraldehyde product is 98%, wherein the nitrogen content is lower than 0.1%. The water phase was passed through N at a flow rate of 200mL / min 2 2h, solvent CyNMe 2 It is dissociated from the water phase and used ...

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Abstract

The invention belongs to the field of chemical industry, relates to solvents with different polarities used in different steps of the chemical reaction process, and in particular relates to a polar reversible transformation solvent for an isobutylene hydroformylation reaction. According to the reaction, N,N-dimethyl cyclohexyl amine (CyNMe2) serves as a solvent for generating isovaleraldehyde in the isobutylene hydroformylation reaction, and the polarity of the CyNMe2 is increased in a production separation tower under the actions of water and CO2 so as to realize separation of the product from the solvent; in a solvent recycling tower, CyNMe2 is dissociated from the aqueous phase by virtue of the gas stripping action of inert gases such as N2, and the solvent is recovered so as to be recycled. The traditional solvent and product separation process needs to be finished by distillation, and therefore the problems such as high energy consumption, solvent volatilization and loss and the like are caused. By utilizing the polar reversible transformation properties of the solvent under the normal temperature and normal pressure conditions, the aims of separating the solvent from the product and recycling the solvent are achieved, the energy consumption is reduced, and the solvent loss is avoided.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to solvents with different polarities used in different steps of the chemical reaction process, in particular to a polarity reversible conversion solvent used for isobutene hydroformylation reaction. Background technique [0002] The hydroformylation reaction process of olefins often adopts an oil phase homogeneous catalytic system, the catalyst and the reaction raw materials are all dissolved in the same phase, the reaction is not limited by mass transfer, and the reaction rate is fast. However, there is also the problem of separation of the solvent and the product after the reaction, which often requires the use of distillation, which consumes a lot of heat energy and also affects the stability of the catalyst. In the distillation process, the unreacted raw material olefins are polymerized and the product aldehydes are condensed to produce tar. The tar will carry the catalyst, whic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/02C07C45/50
CPCC07C45/50C07C45/78C07C47/02
Inventor 陶川东谭平华王小莉毛震波赖崇伟李洁陈群文
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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