Silica gel carrier, silica gel-loaded alkyl aluminometallocene catalyst, long-chain branched polyethylene and preparation method and application of long-chain branched polyethylene

A kind of alkylaluminum metallocene, long-chain branching technology, applied in the long-chain branched polyethylene and its preparation, the field of alkylaluminum metallocene catalyst

Active Publication Date: 2020-06-05
SHANGHAI HONGAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are also a large number of patents referring to self-made silica gel, such as the Chinese patents with publication numbers CN109833859A, CN109833917A, CN109835908A, CN108794667A, CN108970647A and CN109833857A and U.S. Patent No. 6,169,154, etc., which do not involve how to make silica gel carrier-loaded metallocene catalysts for the preparation Contents of long chain branched polyethylene containing other comonomers

Method used

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  • Silica gel carrier, silica gel-loaded alkyl aluminometallocene catalyst, long-chain branched polyethylene and preparation method and application of long-chain branched polyethylene
  • Silica gel carrier, silica gel-loaded alkyl aluminometallocene catalyst, long-chain branched polyethylene and preparation method and application of long-chain branched polyethylene
  • Silica gel carrier, silica gel-loaded alkyl aluminometallocene catalyst, long-chain branched polyethylene and preparation method and application of long-chain branched polyethylene

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preparation example Construction

[0049] The invention provides a preparation method of a silica gel carrier, comprising the steps of:

[0050] The sodium silicate aqueous solution and organosilicone are mixed to obtain a silicon source solution; the organosilanol has a structure shown in any one of formulas I to III:

[0051] SiR 1 n (OH) 4-n Formula I, SiR 1 p R 2 q (OH) 4-p-q Formula II or SiR 1 R 2 R 3 (OH) Formula III, wherein n is 1, 2 or 3, p and q are independently 1 or 2, and 4-p-q>0, R 1 , R 2 and R 3 are independently alkyl, aryl, alkoxy, phenol or amine;

[0052] Adding the silicon source solution and the acid solution dropwise into water at the same time to obtain a hydrated silica gel; then adjusting the pH value of the hydrated silica gel to 9-10, and then performing thermal aging to obtain a silica gel precursor;

[0053] The silica gel precursor is sequentially acidified, washed and dried to obtain a silica gel carrier; the acidification solution for acidification is a strong oxi...

Embodiment 1

[0114] Concentration is the sodium silicate aqueous solution of 40wt% and [(Me 3 Si)PhN]Si(OH) 3 Mix to obtain the silicon source solution, wherein in the silicon source solution [(Me 3 Si)PhN]Si(OH) 3 The concentration is 0.1wt%;

[0115] 10L of the silicon source solution and 1.2L of aqueous hydrochloric acid solution with a concentration of 16wt% were added dropwise to 5L of water at 55°C at a rate of 15 mL / min and 1.8mL / min respectively; The pH value of the glue is 9.4±0.1. After continuing to stir at constant temperature for 3.5 hours, let it stand for 96 hours to age, then pour off the solvent in the reaction solution obtained from aging, wash the obtained solid with water, and cut it into a volume of 0.50±0.01cm 3 The small piece, obtains the silica gel precursor;

[0116] Soak the silica gel precursor in aqua regia, soak at 10°C for 72h, then pour off the aqua regia, and wash the obtained solid with pure water with a conductivity of 5 μS / cm to obtain a crude silica...

Embodiment 2

[0120] The silica gel carrier was prepared by the method of Example 1, the difference being that the organic silanol [(Me 3 Si)PhN]Si(OH) 3 Replace with [(Me 3 Si)PhN]SiMe(OH) 2 , and the obtained silica gel support was designated as HPS-2.

[0121] The specific surface area of ​​the silica gel carrier obtained in this embodiment is 285 ± 5m by using the BET test method. 2 / g, the average pore diameter is 24.58±1.0nm, and the pore volume is 1.69±0.05mL / g. The sodium ion content measured by atomic absorption spectrometry was 250±10ppm.

[0122] The silica gel carrier obtained in this example was crushed, graded and screened, and tested by a laser particle size analyzer to obtain a silica gel carrier with an average particle size of 48.72±2.5 μm for use (the microscopic appearance is as follows: figure 2 shown).

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Abstract

The invention provides a silica gel carrier, a silica gel loaded metallocene catalyst, a preparation method of the silica gel loaded metallocene catalyst, and a preparation method and application of long-chain branched polyethylene, and belongs to the technical field of polymer preparation. Organic silanol is used as an additive; the organic silanol is used as a terminal group blocking agent whensilicon hydroxyl is dehydrated to form silica sol, on one hand, the organic silanol contains an organic group with adjustable stereo steric hindrance, and on the other hand, the organic group also hashydrophobicity, so that the condensation reaction of the silicon hydroxyl can be effectively blocked, and further, an expected porous structure is effectively formed; the hydrated silica gel can be solidified through thermal aging, so that a silica gel precursor with a stable structure is obtained, the obtained silica gel precursor is acidified, organic groups on organosilanol are converted intohydroxyl groups, unreacted raw materials and byproducts are removed through washing, and then the silica gel carrier is obtained through drying. The confinement effect of the silica gel carrier obtained by the method can be matched with metallocene to promote the formation of long-chain branched polyethylene.

Description

technical field [0001] The invention relates to the technical field of polymer preparation, in particular to a silica gel carrier and a silica gel-supported alkyl aluminum metallocene catalyst, long-chain branched polyethylene, and a preparation method and application thereof. Background technique [0002] Polyethylene long-chain branching means that the molecular weight of the branched chain is greater than the minimum entanglement molecular weight of polyethylene molecular chains. This polymer is called long-chain branched polyethylene (LCB-PE). When the branch length of long-chain branched polyethylene exceeds the critical molecular chain length of polyethylene, the branched chain will enhance the entanglement between the molecular chains, thus showing high melt strength at low shear rates, while the branched chain It also reduces the hydrodynamic volume of polyethylene and thus exhibits high shear thinning behavior at high shear rates. Long-chain branched polyethylene h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/02C08F4/6592C08F210/16C08F210/14
CPCC08F4/025C08F4/6592C08F210/16C08F210/14
Inventor 彭晓琪叶建忠姜海军金建耀丁炎彭彦博
Owner SHANGHAI HONGAN CHEM
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