Preparation method of organic vehicle olefin polymerization catalyst

A technology of olefin polymerization and organic carrier, which is applied in the field of organic carrier preparation, can solve the problems of large particle size and distribution, and achieve the effects of uniform particle size, easy filtration, and increased yield

Active Publication Date: 2015-04-22
PETROCHINA CO LTD
23 Cites 5 Cited by

AI-Extracted Technical Summary

Problems solved by technology

However, the particle size and distribution of the particles prepared by the suspension polymerization method are large, and the particle size can re...
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Method used

As can be seen from Table 1, the present invention adopts metal oxide template reagent to prepare organic carrier and compares the method for not using metal oxide template reagent, can improve the productive rate of the polymer particle that improves preparation, makes the polymer of preparation It is easier to filter, increases the specific surface area of ​​the porous organic carrier, and can also increase its pore volume. After the metal oxide nanoparticles are ultrasonically dispersed to refine the metal oxide particles, the prepared or...
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Abstract

The invention relates to a preparation method of an organic vehicle olefin polymerization catalyst. The preparation method of the organic vehicle olefin polymerization catalyst comprises the following steps: mixing alcohol with water, thus obtaining a dispersion liquid; adding a reactive monomer into the dispersion liquid, thus obtaining mixed solution; adding a stabilizer, metal oxide particles and a free radical initiator into the mixed solution, heating to 60-85 DEG C, stirring while reacting for 3-12 hours to obtain a reaction product, washing the obtained reaction product, and drying, thus obtaining a copolymer containing metallic oxide, wherein metal in the metal oxide is one or combination of more than one of metal ions in families VIII, IB, IIB and IIA; and removing metallic oxide in the copolymer containing metallic oxide, washing and drying, thus obtaining the organic vehicle olefin polymerization catalyst. The preparation method of the organic vehicle olefin polymerization catalyst has the advantages that the form and the specific surface area of an organic vehicle can be regulated, and thus the organic vehicle can be separated out from a system relatively easily, solid particles can be filtered out relatively easily, the yield of a reaction monomer is increased, and the organic vehicle with the narrow particle size distribution is obtained.

Technology Topic

IonOlefin polymerization +10

Image

  • Preparation method of organic vehicle olefin polymerization catalyst
  • Preparation method of organic vehicle olefin polymerization catalyst
  • Preparation method of organic vehicle olefin polymerization catalyst

Examples

  • Experimental program(22)

Example Embodiment

[0034] Example 1
[0035] This embodiment provides a method for preparing an organic carrier for an olefin polymerization catalyst, comprising the following steps:
[0036] In a 250mL glass reactor, add 108mL ethanol and 12mL deionized water;
[0037] Add 3.8g divinylbenzene (55wt%) and 2.4g hydroxyethyl methacrylate reaction monomer, stir at room temperature for 5min;
[0038] Add iron ferric oxide nanoparticles (particle size: 20nm) accounting for 5% of the total mass of the reaction monomers and polyvinyl alcohol (the degree of polymerization is 1788) accounting for 2% of the total mass of the reaction monomers, and stir for 1 hour at 50° C. Vinyl alcohol stabilizer dissolved;
[0039] Add AIBN accounting for 2% of the total mass of the reaction monomer, raise the temperature to 70°C, react for 3 hours, raise the temperature to 80°C, and react for 5 hours, the stirring speed is 360 rpm, using ethanol/water (1:1) Mixed solvent washes 3 times, uses 400 order 316 stainless steel filter net multi-layers to filter (filtering in all following examples all is to use this method to filter), after drying, obtain 4.8g gray porous organic carrier A1 containing ferric oxide -1.
[0040] Take 3.3g of the dried A1-1 carrier, use 20mL of 36.5wt% concentrated hydrochloric acid and 100mL of alcohol/water system acid solvent (mass ratio 1:1), wash at 70°C for 2h, the solution turns from gray black to Yellow, after filtering, wash with a small amount of the above acid solvent for 0.5h, then wash with alcohol/water (mass ratio 1:1) system solvent for 3 times, filter and dry to obtain 2.8g white porous P(DVB-co-HEMA) Organic vehicle A1-2.

Example Embodiment

[0041] Example 2
[0042] This embodiment provides a method for preparing an organic carrier for an olefin polymerization catalyst, comprising the following steps:
[0043] In a 250mL glass reactor, add 126mL ethanol and 14mL deionized water;
[0044] Add 4.6g divinylbenzene (55wt%) and 3.1g hydroxyethyl methacrylate (98wt%) reaction monomer, and stir at room temperature for 5min;
[0045] Add iron ferric oxide nanoparticles (20nm in particle size) accounting for 3% of the total mass of the reaction monomers and polyvinyl alcohol (1788 degree of polymerization) accounting for 2% of the total mass of the reaction monomers, stir at 50° C. for 1 h, and polymerize Vinyl alcohol stabilizer dissolved;
[0046] Add AIBN accounting for 2% of the total mass of the reaction monomer, raise the temperature to 70°C, react for 3 hours, then raise the temperature to 80°C, react for 5 hours, stir at 360 rpm, wash 3 times with ethanol, and dry 5.0 g of gray porous organic carrier A2-1 containing ferric oxide was obtained.
[0047] Take 3.0g of the dried A2-1 carrier, use 20mL of 36.5% concentrated hydrochloric acid and 100mL of alcohol/water system acid solvent (mass ratio 1:1), wash at 70°C for 2h, the solution turns from gray black to yellow, after filtration , washed with a small amount of the above acid solvent for 0.5h, then washed 3 times with the solvent of the alcohol/water (mass ratio 1:1) system, and obtained 2.7g white porous P(DVB-co-HEMA) organic carrier A2- 2.

Example Embodiment

[0048] Example 3
[0049] This embodiment provides a method for preparing an organic carrier for an olefin polymerization catalyst, the steps of which are basically the same as those in Example 2, except that the amount of ferric iron tetroxide nanoparticles becomes 1.5% of the total mass of the reaction monomers, 4.0 g of porous organic carrier containing ferric oxide was prepared as A3-1.
[0050] Take 2.8g of the dried A3-1 carrier, use 20mL of 36.5% concentrated hydrochloric acid and 100mL of alcohol/water system acid solvent (mass ratio 1:1), wash at 70°C for 2h, the solution turns from gray black to yellow, filter Finally, wash 0.5h with a small amount of above-mentioned acid solvent, then wash 3 times with the solvent of alcohol/water (mass ratio 1:1) system, obtain 2.4g white porous P (DVB-co-HEMA) organic carrier A3 after filtering and drying -2.

PUM

PropertyMeasurementUnit
Particle size20.0nm

Description & Claims & Application Information

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