A kind of solid composition and its preparation method and application
A solid composition and compound technology, applied in the field of application as a carrier for olefin polymerization catalysts, can solve the problems of inert dispersion media increasing solvent recovery costs, reducing carrier single-pot yield, etc., achieving good particle shape and increasing single-pot yield , the effect of high stereoregularity
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[0068] In a preferred embodiment, the preparation method of the solid composition may include:
[0069] (i) In a closed container, heat the mixture of magnesium halide, organic alcohol and at least one polymer dispersion stabilizer to 30-160°C, preferably 40-120°C, and react for 0.1-5 hours, preferably 0.5 -2 hours, a magnesium halide alcoholate solution is formed, wherein, based on each mole of magnesium, the amount of the organic alcohol is 3-30 moles, preferably 4-25 moles; the amount of the polymer dispersion stabilizer is the The total amount of the magnesium halide and the organic alcohol is 0.1-10% by weight, preferably 0.2-5% by weight.
[0070] (ii) under stirring, add the alkylene oxide compound represented by the above formula (2) to the above magnesium halide alcoholate solution, and react at 30-160°C (preferably 40-120°C) for 0.1-5 hours, It is preferably 0.3-1 hour to form solid composition granules, wherein the amount of the alkylene oxide compound is 1-10 mole...
Embodiment 1-17
[0080] These examples are used to illustrate the solid compositions of the present invention and their preparation methods.
[0081] In a 500mL airtight reactor, sequentially add magnesium chloride, organic alcohol (R 1 OH) and polymer dispersion stabilizer, heated up to the reaction temperature (T) under stirring, after constant temperature reaction for 1 hour, added alkylene oxide compound (E), maintained the temperature for 0.5 hour reaction, filtered off the liquid, and washed with hexane 5 times, vacuum-dried to obtain solid composition particles, the specific preparation conditions are shown in Table 1, so as to prepare spherical solid compositions A1-A17 respectively, wherein, the average particle diameter (D50) and particle diameter of these solid compositions The distribution values (SPAN) are shown in Table 1, the solid composition A1 1 H-NMR spectrum as figure 1 As shown, the solid composition A2 1 H-NMR spectrum as figure 2 As shown, the solid composition A1...
Embodiment 18
[0115] This example is used to illustrate the application of the solid composition of the present invention.
[0116] (1) Preparation of solid catalyst
[0117] Into a 300mL glass reaction bottle, 100ml of titanium tetrachloride was added sequentially, cooled to -20°C, 8g of the solid composition A1 prepared in Example 1 above was added, and the temperature was raised to 110°C. During the heating process, 1.5 ml of diisobutyl phthalate was added, the liquid was filtered off, washed twice with titanium tetrachloride, washed three times with hexane, and dried in vacuum to obtain a solid catalyst Cat-1.
[0118] (2) Propylene liquid phase bulk polymerization
[0119] The liquid-phase bulk polymerization of propylene was carried out in a 5L stainless steel autoclave. Under the protection of nitrogen, add 5ml triethylaluminum hexane solution (concentration: 0.5mmol / ml) and 1ml cyclohexylmethyldimethoxysilane (CHMMS) hexane solution (concentration: 0.1mmol / ml) to the reaction kett...
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Abstract
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