A liquid-liquid mixing device and method for processing polymer solution

Abstract

The invention discloses a liquid-liquid mixing device, the device includes a cylinder body (1) and a stirring device (4) arranged in the cylinder body (1); the cylinder body (1) is separated into a plurality of mixed spaces by separating discs (2) along the axial direction, the stirring device (4) is provided with a stirring paddle (5) corresponding to each mixed space, the device is characterized in that: each mixed space is provided with a baffle plate (3), and the separate disc (2) is provided with a diversion hole (2-2). The invention also provides a polymer solution processing method using the liquid-liquid mixing device. The method is as follows: a catalyst-containing polymer solution with polymerization activity and a polar liquid are respectively mixed or mixed in advance, and the mixture is added into the liquid-liquid mixing device via an upper liquid inlet of the liquid-liquid mixing device for step-by-step mixing. The liquid-liquid mixing device has the advantages of simple process, low cost and high mixing efficiency.

Description

technical field

[0001] The invention relates to a treatment device for polymer solution containing catalyst, which is suitable for the dispersion of rubber polymer solution and the separation of catalyst therein, more specifically, it relates to the rubber polymer solution containing catalyst and immiscible other A liquid mixing and dispersing device and a catalyst separation method therein. Background technique

[0002] In the field of synthesis of synthetic rubber elastomers, homogeneous solution polymerization is usually used, and batch or continuous solution polymerization is carried out by polymerizing monomers, catalysts or initiators (such as Ziegler-Natta series nickel, vanadium, or titanium series catalyst systems). .

[0003] In the production of elastomeric polymers using Ziegler-Natta, the amount of catalyst remaining in the polymer is higher due to the generally lower catalytic efficiency. First of all, when the residual catalyst such as nickel, vanadium, tita...

Examples

Embodiment 1

[0051] use Figure 1-3 The liquid-liquid mixing device shown includes: a cylinder body 1, a partition plate 2, a baffle plate 3, a stirring device 4, a stirring paddle 5, a stirring shaft 6, a venting balance pipe 7, a sight glass 8, a temperature measuring component 9, and a safety valve 10. The upper end head 11, the lower end head 12, the liquid inlet N1 and the liquid outlet N2. Wherein, the separation disc 2 has a central hole 2-1 and a flow guide hole 2-2.

[0052] The cylinder body 1 is divided into three mixing spaces in the axial direction by the partition plate 2 .

[0053] The disk surface of the separating disk 2 is horizontal, and the plate surface of the baffle plate 3 is vertical.

[0054] There is a gap between the baffle plate 3 and the inner wall of the cylinder body 1 . The ratio of the length of the gap along the radial direction of the cylinder 1 to the inner diameter of the cylinder 1 is 0.03:1.

[0055] In each mixing space, the ratio of the width of...

Embodiment 2

[0069] In a 5L polymerization kettle, a butadiene-styrene copolymer was synthesized with n-butyllithium as an initiator and a mixture of cyclohexane and n-hexane (the weight percent of cyclohexane was 87%) as a solvent. The copolymer concentration is 10.0% by weight based on the whole polymerization system, the number average molecular weight of the copolymer is 55,000, and the weight ratio of styrene to butadiene monomer units is 3:7. Triisobutylaluminum (Yanshan Synthetic Rubber Factory, industrial grade, concentration 3g / L) and nickel naphthenate (Yanshan Synthetic Rubber Factory, industrial grade, concentration 4g / L) are 4 according to the molar ratio (based on metal): 1 mix, add it to the butadiene-styrene block copolymer solution obtained above, and stir well. Finally, 1200 mL of a butadiene-styrene copolymer solution containing a hydrogenation catalyst was added into a 20 L autoclave for hydrogenation reaction. The hydrogenation reaction temperature is controlled at ab...

Embodiment 3

[0074] Adopt the device and method identical with embodiment 1, difference is:

[0075] There is no gap between the baffle plate 3 and the inner wall of the cylinder body 1 .

[0076] The residual metal content in the dry glue was determined by plasma emission spectrometry IPC, and the results are shown in Table 3.

technical field

[0001] The invention relates to a treatment device for polymer solution containing catalyst, which is suitable for the dispersion of rubber polymer solution and the separation of catalyst therein, more specifically, it relates to the rubber polymer solution containing catalyst and immiscible other A liquid mixing and dispersing device and a catalyst separation method therein. Background technique

[0002] In the field of synthesis of synthetic rubber elastomers, homogeneous solution polymerization is usually used, and batch or continuous solution polymerization is carried out by polymerizing monomers, catalysts or initiators (such as Ziegler-Natta series nickel, vanadium, or titanium series catalyst systems). .

[0003] In the production of elastomeric polymers using Ziegler-Natta, the amount of catalyst remaining in the polymer is higher due to the generally lower catalytic efficiency. First of all, when the residual catalyst such as nickel, vanadium, tita...

Examples

Embodiment 1

[0051] use Figure 1-3 The liquid-liquid mixing device shown includes: a cylinder body 1, a partition plate 2, a baffle plate 3, a stirring device 4, a stirring paddle 5, a stirring shaft 6, a venting balance pipe 7, a sight glass 8, a temperature measuring component 9, and a safety valve 10. The upper end head 11, the lower end head 12, the liquid inlet N1 and the liquid outlet N2. Wherein, the separation disc 2 has a central hole 2-1 and a flow guide hole 2-2.

[0052] The cylinder body 1 is divided into three mixing spaces in the axial direction by the partition plate 2 .

[0053] The disk surface of the separating disk 2 is horizontal, and the plate surface of the baffle plate 3 is vertical.

[0054] There is a gap between the baffle plate 3 and the inner wall of the cylinder body 1 . The ratio of the length of the gap along the radial direction of the cylinder 1 to the inner diameter of the cylinder 1 is 0.03:1.

[0055] In each mixing space, the ratio of the width of...

Embodiment 2

[0069] In a 5L polymerization kettle, a butadiene-styrene copolymer was synthesized with n-butyllithium as an initiator and a mixture of cyclohexane and n-hexane (the weight percent of cyclohexane was 87%) as a solvent. The copolymer concentration is 10.0% by weight based on the whole polymerization system, the number average molecular weight of the copolymer is 55,000, and the weight ratio of styrene to butadiene monomer units is 3:7. Triisobutylaluminum (Yanshan Synthetic Rubber Factory, industrial grade, concentration 3g / L) and nickel naphthenate (Yanshan Synthetic Rubber Factory, industrial grade, concentration 4g / L) are 4 according to the molar ratio (based on metal): 1 mix, add it to the butadiene-styrene block copolymer solution obtained above, and stir well. Finally, 1200 mL of a butadiene-styrene copolymer solution containing a hydrogenation catalyst was added into a 20 L autoclave for hydrogenation reaction. The hydrogenation reaction temperature is controlled at ab...

Embodiment 3

[0074] Adopt the device and method identical with embodiment 1, difference is:

[0075] There is no gap between the baffle plate 3 and the inner wall of the cylinder body 1 .

[0076] The residual metal content in the dry glue was determined by plasma emission spectrometry IPC, and the results are shown in Table 3.

Images