A kind of preparation method of high regularity polybutene-1 powder

A high-specificity, polybutene technology, applied in the field of polybutene-1 powder and its preparation, can solve the problems of long polybutene-1 crystal transformation period and the like

Active Publication Date: 2017-06-16
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] One of the purposes of the present invention is to provide a method for preparing high isotactic polybutene-1 powder for the deficiencies of the current technology, and the second purpose of the present invention is to solve the problem of long polybutene-1 crystal transformation period

Method used

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  • A kind of preparation method of high regularity polybutene-1 powder
  • A kind of preparation method of high regularity polybutene-1 powder
  • A kind of preparation method of high regularity polybutene-1 powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1), preparation of catalytic components

[0048] (1) Vacuumize a 250ml three-necked flask, replace it with argon three times, add 3g (0.032mol) of anhydrous magnesium chloride under an argon atmosphere, 85ml (0.44mol) of inert solvent n-decane, 0.4g (0.0027mol) of phthalic anhydride mol), 35ml (0.22mol) of isooctyl alcohol, the system was heated up to 100°C for 2h, and naturally cooled to room temperature under the protection of argon to obtain alcohol and compound.

[0049] (2) Vacuumize the 500ml five-neck bottle, replace it with argon for 3 times, and add 50ml TiCl 4 , cooling down to -30°C--20°C in an ice-salt bath, drop the above-prepared alcohol compound into the five-necked bottle, and complete the dropwise addition within 2 hours.

[0050] (3) heat up to 80°C, keep warm for 2h,

[0051] (4) Remove the upper liquid after standing for 20 minutes. At this time, the temperature of the system is basically room temperature. Add 50ml of TiCl at this temperature 4 C...

Embodiment 2

[0057] (1), preparation of catalytic components

[0058] (1) Vacuumize a 250ml three-necked flask, replace it with argon three times, add 3g (0.032mol) of anhydrous magnesium chloride under an argon atmosphere, 85ml (0.44mol) of inert solvent n-decane, 0.4g (0.0027mol) of phthalic anhydride mol), 35ml (0.22mol) of isooctyl alcohol, the system was heated up to 100°C for 2h, and naturally cooled to room temperature under the protection of argon to obtain alcohol and compound.

[0059] (2) Vacuumize the 500ml five-neck bottle, replace it with argon for 3 times, and add 50ml TiCl 4 , cooling down to -30°C--20°C in an ice-salt bath, drop the above-prepared alcohol compound into the five-necked bottle, and complete the dropwise addition within 2 hours.

[0060] (3) heat up to 80°C, keep warm for 2h,

[0061] (4) Remove the upper liquid after standing for 20 minutes. At this time, the temperature of the system is basically room temperature. Add 50ml of TiCl at this temperature 4 C...

Embodiment 3

[0067] In a 2L stainless steel autoclave, after the system was replaced with nitrogen three times, 2.3ml of 1mol / L triethylaluminum solution was added successively under nitrogen protection (the solvent is n-hexane, the same as in the following examples), methylcyclohexyldimethoxy 0.075 mmol of silane, 20 mg of the supported Ziegler-Natta catalyst prepared in Example 1 (0.0076 mmol of titanium), 25 mg of lanthanum stearate and 25 mg of stearic acid, 473 g of propylene in liquid phase, pre-polymerized at 50° C. for 10 min. After the reaction, empty the propylene in the kettle, add 150g of butene-1 monomer, hydrogen 0.10MPa, polymerize at a constant temperature of 25°C for 8h, remove unreacted monomer by flash evaporation, and obtain polybutene-1 with a particle size of 0.1-3mm powder (such as figure 1 ), the catalyst activity is 4599g / g Cat, and the bulk density is 0.30g / cm 3 , the isotacticity of the polymer is 95.3%, the molecular weight distribution is 6.8, the polypropylen...

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Abstract

The invention relates to a preparation method of high-isotacticity polybutene-1 powder. The method comprises the following steps: sequentially adding a cocatalyst solution, an outer electron donor, a main catalyst, an assistant compound and a liquid-phase alpha-olefin into a tank reactor, prepolymerizing at 10-90 DEG C for 10-120 minutes, evacuating olefin gas, charging butylene-1 monomer and molecular weight regulator hydrogen gas, polymerizing at -10-90 DEG C for 1-20 hours, and carrying out flash evaporation on the unreacted monomer to obtain the high-isotacticity polybutene-1 powder. The polymerization method for synthesizing high-isotacticity polybutene-1 and powder thereof is simple in technique and easy to operate. The prepolymerization method solves the problem of difficulty in controlling the form of the polybutene-1 in the common catalytic polymerization method, and improves the problem of long crystal form transition period of the polybutene-1.

Description

[0001] Technical field: [0002] The invention relates to a polybutene-1 powder with high isotacticity and a preparation method thereof. [0003] technical background: [0004] High isotactic polybutene-1 has the characteristics of toughness, wear resistance, no scaling, high temperature resistance, non-toxicity, and excellent impact resistance. Compared with metal materials, the energy consumption of polybutene-1 pipes per unit volume is only 1 / 8-1 / 4 of steel and aluminum respectively; compared with other polyolefin materials, polybutene-1 can be used in Long-term use at 80-90°C, the upper limit of the service temperature can reach 110°C, it is an excellent material for hot water pipes. [0005] The traditional preparation method of high isotactic polybutene-1 includes gas phase method and liquid phase method. The gas phase polymerization process of polybutene-1 is usually carried out by gas phase fluidized bed process. As well as the Chinese patent CN 102040693 A, the buten...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F210/08C08F210/06C08F4/649
Inventor 刘宾元董小芳刘智博张莉杨敏崔晓鹏张广林
Owner HEBEI UNIV OF TECH
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