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Preparation method and application of MgCl2/silica gel carrier-supported metallocene catalyst

A metallocene catalyst and carrier-supported technology, which is applied in the field of polyolefin preparation, can solve problems such as difficult processing and low heat-sealing temperature, and achieve the effects of good processing performance, high activity and improved catalytic activity.

Inactive Publication Date: 2020-01-07
营口风光新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The metallocene polyethylene resin prepared by metallocene catalyst has the advantages of good transparency, good puncture resistance and low heat sealing temperature, but there are problems of processing difficulty

Method used

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  • Preparation method and application of MgCl2/silica gel carrier-supported metallocene catalyst
  • Preparation method and application of MgCl2/silica gel carrier-supported metallocene catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] MgCl 2 / Silica gel carrier loaded metallocene catalyst, the preparation method is as follows:

[0029] 1)MgCl 2 / Preparation and activation of silica gel support:

[0030] The 955 silica gel was calcined at 500° C. for 3 h under the protection of nitrogen to obtain activated 955 silica gel.

[0031] Take 50g MgCl 2 Dissolve in 300mL tetrahydrofuran, add 300g activated 955 silica gel, react at 30°C for 2h, filter to obtain MgCl 2 / Silicone carrier. MgCl will be obtained 2 / The silica gel carrier was calcined at 500°C for 3h to obtain activated MgCl 2 / Silicone carrier.

[0032] 2) After passing nitrogen into the 250ml reaction flask for 3-5 times, add 30g of the activated MgCl obtained in step 1) 2 / silica gel carrier, add 50mL toluene, heat up to 50°C, add 50mL of MAO toluene solution (containing MAO 15g) dropwise, react at 50°C for 4 hours, filter, and wash with 50mL toluene 3 times to obtain a supported cocatalyst slurry.

[0033] 3) Introduce nitrogen in...

Embodiment 2

[0035] MgCl 2 / Silica gel carrier loaded metallocene catalyst, the preparation method is as follows:

[0036] 1)MgCl 2 / Preparation and activation of silica gel support:

[0037] The 955 silica gel was calcined at 500° C. for 3 h under the protection of nitrogen to obtain activated 955 silica gel.

[0038] Take 50g MgCl 2 Dissolve in 300mL tetrahydrofuran, add 300g activated 955 silica gel, react at 30°C for 2h, filter to obtain MgCl 2 / Silicone carrier. MgCl will be obtained 2 / The silica gel carrier was calcined at 500°C for 3h to obtain activated MgCl 2 / Silicone carrier.

[0039] 2) After passing nitrogen into the 250ml reaction flask for 3-5 times, add 30g of the activated MgCl obtained in step 1) 2 / silica gel carrier, add 50mL toluene, heat up to 50°C, add dropwise 50mL of MAO toluene solution (containing MAO 15g), react at 50°C for 4 hours, filter, and wash with 50mL toluene 3 times to obtain a supported cocatalyst slurry.

[0040] 3) Nitrogen was introduce...

Embodiment 3-6

[0042] Polyethylene synthetic method, step is as follows:

[0043] In a 2L stainless steel autoclave, first pass in nitrogen for replacement 3-5 times, then pass in ethylene for replacement 3-5 times, then add 1L of n-hexane, 10g of polyethylene monomer as a seed, 10mmol of triethylaluminum , add catalyst, ethylene and 1-hexene as in Table 1, and react at 1.0 MPa and 90° C. for 1 hour. After the reaction, cool down, filter, and dry to obtain polyethylene powder. The results are shown in Table 1.

[0044] Table 1 aggregated data

[0045]

[0046] figure 1 Molecular weight distribution curve for the prepared polyethylene. Among the figure 1 is the polyethylene produced by the existing non-bridging metallocene catalyst; 2 is the MgCl prepared by the present invention 2 / Polyethylene prepared by supporting metallocene catalysts on silica gel carrier. Depend on figure 1 It can be seen that the molecular weight distribution of polyethylene prepared by using the supported ...

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Abstract

The invention relates to a preparation method and an application of a MgCl2 / silica gel carrier-supported metallocene catalyst. The preparation method comprises the following steps: a MgCl2 / silica gelcarrier and an organic solvent are taken, and are heated to 50 DEG C under the protection of nitrogen, a cocatalyst is added, a reaction is performed at 50 DEG C for 4 h, and the obtained reaction product is filtered and washed to obtain a supported cocatalyst slurry; and a toluene solution of a bridged metallocene compound is dropwise added into the obtained supported cocatalyst slurry under theprotection of nitrogen under a stirring condition, the obtained solution is stirred and reacted at 100 DEG C for 30 min, and the obtained reaction product is filtered and washed to obtain the MgCl2 / silica gel carrier-supported metallocene catalyst. Ethylene and 1-olefin are polymerized in the presence of the single MgCl2 / silica gel carrier-supported metallocene catalyst to obtain polyethylene witha wide molecular weight distribution. The polyethylene prepared by the method has the advantages of large melt flow ratio, good processability and wide molecular weight distribution.

Description

technical field [0001] The invention relates to the field of polyolefin preparation based on metallocene catalysts, in particular to a MgCl 2 / Preparation method and application of silica gel carrier supported metallocene catalyst. Background technique [0002] In the field of olefin polymerization, metallocene catalysts catalyze olefin polymerization to obtain polymers with narrow molecular weight distribution and narrow branch chain distribution. Due to the wide choice of catalyst ligands and the strong ability to regulate the polymer, the performance improvement of the polymer can be realized, making its application range wider and wider. [0003] The molecular weight and molecular weight distribution of polyolefins are key factors in determining physical properties and affecting workability, flow and mechanical properties. It is very important to improve the melt workability of the polymer by controlling the molecular weight distribution of the polymer. Therefore, it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F110/02C08F210/16C08F4/6592C08F4/02
CPCC08F110/02C08F210/16C08F4/02C08F4/65927C08F2500/04C08F2500/12C08F210/14
Inventor 王磊齐涛张文泉
Owner 营口风光新材料股份有限公司
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