Liquid phase synthesis method of high isotactic polybutene-1

A liquid-phase synthesis technology of isotactic polybutene, which is applied in the field of liquid-phase synthesis of high isotactic polybutene-1, can solve problems such as mass transfer, heat transfer difficulties, system stickiness, etc., and achieve simple process and high production efficiency High, guaranteed heat transfer effect

Active Publication Date: 2020-11-17
山东省滕州瑞达化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since polybutene-1 will swell in its monomer when the polymerization temperature is higher than 30°C, it will make the system sticky, resulting in difficulties in mass transfer and heat transfer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] In the ring pipe, the butene-1 monomer soaked by the dehydration molecular sieve and the desulfurization catalyst is first added, and then the supported Ziegler-Natta spherical catalyst (wherein the support is spherical MgCl 2 , the catalyst is TiCl 4 The mass content of Ti in the catalyzer is 2%; The inner electron donor is organosilane (the mol ratio of the inner electron donor and Ti is 10)), cocatalyst (alkyl aluminum) and the n-hexane of the outer electron donor Added in the loop reactor, wherein, the activity of the catalyst is 140kg / g polybutene-1 per gram of catalyst synthesis, the mass ratio of n-hexane / butene-1 monomer is 0.1, and the molar ratio of Al / Ti is 200 , the molar ratio of external electron donor / Ti is 10, the reaction temperature is programmed to change temperature in three stages, the temperature increase is 40°C, the partial pressure of the inert gas is adjusted to ensure that the pressure in the loop reactor remains constant, and in a reaction pr...

Embodiment 2

[0048] In the ring pipe, the butene-1 monomer soaked by the dehydration molecular sieve and the desulfurization catalyst is first added, and then the supported Ziegler-Natta spherical catalyst (wherein the support is spherical MgCl 2 , the catalyst is TiCl 4 The mass content of Ti in the catalyzer is 3%; The inner electron donor is organosilane (the mol ratio of the inner electron donor and Ti is 15)), cocatalyst (alkyl aluminum) and the n-hexane of the outer electron donor Added in the loop reactor, wherein, the activity of the catalyst is 170kg / g polybutene-1 per gram of catalyst synthesis, the mass ratio of n-hexane / butene-1 monomer is 0.08, and the molar ratio of Al / Ti is 250 , the molar ratio of the external electron donor / Ti is 15, the reaction temperature is programmed to change temperature in three stages, and the partial pressure of the inert gas is adjusted to ensure that the pressure in the loop reactor remains constant. In a reaction process, the temperature stages...

Embodiment 3

[0050] In the ring pipe, the butene-1 monomer soaked by the dehydration molecular sieve and the desulfurization catalyst is first added, and then the supported Ziegler-Natta spherical catalyst (wherein the support is spherical MgCl 2 , the catalyst is TiCl 4 The mass content of Ti in the catalyzer is 5%; The inner electron donor is the n-hexane of organosilane (the molar ratio of inner electron donor and Ti is 25)), cocatalyst (alkyl aluminum) and outer electron donor Join in the loop reactor, wherein, the activity of catalyst is that every gram of catalyst synthesizes 168kg / g polybutene-1, the mass ratio of n-hexane / butene-1 monomer is 0.01, and the molar ratio of Al / Ti is 300 , the molar ratio of the external electron donor / Ti is 25, the reaction temperature is programmed to change temperature in three stages, and the partial pressure of the inert gas is adjusted to ensure that the pressure in the loop reactor remains constant. In a reaction process, the temperature stages c...

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Abstract

The embodiment of the invention provides a liquid phase synthesis method of high isotactic polybutene-1 and belongs to the field of high-molecular polymer synthesis. With adoption of the liquid phase synthesis method of the high isotactic polybutene-1, a polymer with reasonable molecular weight distribution can be acquired according to the principle of reaction kinetics while the subsequent separation energy consumption is reduced. The liquid phase synthesis method of the high isotactic polybutene-1 comprises the following steps: adding a butane-1 monomer, a supported titanium catalyst, a cocatalyst, and mixed liquid of an electron donor and an inert solvent in a loop reactor sequentially, taking hydrogen as a molecular weight regulator and inert gas as a pressure regulator in the loop reactor, carrying out programmed temperature increasing within a preset temperature range under the condition of enabling the reaction pressure in the whole loop reactor to keep in a preset pressure range by regulating the partial pressure ratio of the inert gas, carrying out constant-pressure reaction for 1-4h, carrying out flash evaporation to remove the unreacted monomer, and obtaining the powdery high isotactic polybutene-1. The liquid phase synthesis method can be used for industrial production of the high isotactic polybutene-1.

Description

technical field [0001] The invention relates to the field of polymer synthesis, in particular to a liquid phase synthesis method of high isotactic polybutene-1. Background technique [0002] Isotactic polybutene polymer is a semi-crystalline polymer with butene-1 as a monomer, which naturally has physical properties similar to polyethylene and polypropylene polymers, and its outstanding creep resistance As well as the good mechanical properties displayed under heated conditions, it has unique advantages in the application of hot and cold water pipes, floor heating pipes, and packaging films. [0003] The traditional synthesis methods of isotactic polybutene-1 can be divided into gas-phase method and liquid-phase method. The gas-phase method is usually carried out with a gas-phase ebullating bed, but the gas-phase ebullating bed has high requirements for technology and equipment, and when solving the main problems affecting the reaction, the flow field and the size of the bu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F110/08C08F4/649C08F4/646C08F4/02C08F2/06
Inventor 齐世锋白锋李青海
Owner 山东省滕州瑞达化工有限公司
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