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Hydrophobic organosilicon/polyamide 6block copolymers and in situ preparation method thereof

A technology of block copolymer and polyamide, applied in the field of hydrophobic silicone/polyamide 6 block copolymer and its in-situ preparation, can solve the problem of poor product stability, poor compatibility of polyamide, difficult blending, etc. question

Inactive Publication Date: 2011-08-17
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are usually two methods for the block copolymerization modification of polyamides. One is to prepare polyamide oligomers with terminal functionalization (such as terminal hydroxylation and terminal carboxylation), and then combine them with other structural monomers or segments Reaction to prepare block copolymers, such as copolymerization modification of polyamide and polyether diol, etc., the disadvantage of this method is that the oligomer system has poor compatibility and the polycondensation reaction time is long
Relatively speaking, there are few studies on silicone-modified polyamides, because it has poor compatibility with polyamides, and it is difficult to carry out simple blending, and the two polymers are coupled and connected by chemical reactions, due to the generated Si- O-C is easy to hydrolyze, resulting in poor product stability

Method used

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  • Hydrophobic organosilicon/polyamide 6block copolymers and in situ preparation method thereof
  • Hydrophobic organosilicon/polyamide 6block copolymers and in situ preparation method thereof
  • Hydrophobic organosilicon/polyamide 6block copolymers and in situ preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 50g of ε-caprolactam into the reactor, start stirring and heating, after the ε-caprolactam is completely melted and the temperature reaches above 105°C, and control the temperature in the reactor between 105°C, start vacuuming until the pressure is less than 4mm Hg Dehydrate for more than 30 minutes, then lower the temperature and keep the temperature at 75°C, release the vacuum, add 1.1206g of 2,4-toluene diisocyanate, 3.1387g of double-terminated hydrocarbon hydroxyl polysiloxane (molecular weight: 1000g / mol) and dibutyl dilaurate Acid tin 0.003ml, react for 2 hours. The temperature was raised to 110°C, and the reaction was carried out for 2 hours. Add 0.8485 g of the reactant of sodium hydroxide and ε-caprolactam, stir and mix evenly, pour into a mold preheated to 165°C and polymerize for more than 40 minutes, then cool and demould.

[0029] The conversion rate of the copolymer obtained by polymerization is measured by an extraction method, and the conversion ra...

Embodiment 2

[0031] Add 50g of ε-caprolactam into the reactor, start stirring and heating, after the ε-caprolactam is completely melted and the temperature reaches above 105°C, and control the temperature in the reactor between 110°C, start vacuuming until the pressure is less than 4mm Hg Dehydrate for more than 30 minutes, then lower the temperature and keep the temperature at 80°C, release the vacuum, add 1.8677g of 2,4-toluene diisocyanate, 5.2313g of double-terminated hydrocarbon hydroxyl polysiloxane (molecular weight: 1000g / mol) and dibutyl dilaurate Acid tin 0.003ml, reacted for 2.5 hours. The temperature was raised to 110°C, and the reaction was carried out for 2.5 hours. Add 1.4142 g of the reactant of sodium hydroxide and ε-caprolactam, stir and mix evenly, pour into a mold preheated to 150°C and polymerize for more than 40 minutes, then cool and demould.

[0032] The conversion rate of the copolymer obtained by polymerization is measured by an extraction method, and the convers...

Embodiment 3

[0034] Add 50g of ε-caprolactam into the reactor, start stirring and heating, after the ε-caprolactam is completely melted and the temperature reaches above 105°C, and control the temperature in the reactor between 115°C, start vacuuming until the pressure is less than 4mm Hg Dehydrate for more than 30 minutes, then lower the temperature and keep the temperature at 82°C, release the vacuum, add 0.2979g of 2,4-toluene diisocyanate, 2.2518g of double-ended ether hydroxypolysiloxane (molecular weight: 2700g / mol) and dibutyl dilaurate Acid tin 0.003ml, react for 3 hours. The temperature was raised to 110°C, and the reaction was carried out for 3 hours. Add 0.2255 g of the reactant of sodium hydroxide and ε-caprolactam, stir and mix evenly, pour into a mold preheated to 170°C and polymerize for more than 40 minutes, and then cool and demould.

[0035] The conversion rate of the copolymer obtained by polymerization is measured by an extraction method, and the conversion rates of ca...

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Abstract

The invention discloses a method for preparing a hydrophobic organosilicon / polyamide 6 block copolymer at original position taking end hydroxyl organic silicone oil, diisocyanate and epsilon-caprolactam as raw materials. The method comprises the following steps: adding the diisocyanate into melted dehydrated epsilon-caprolactam, adding the end hydroxyl organic silicone oil for carrying out a hydroxyl-isocyanic acid radical reaction after even mixing to generate end isocyanic acid radical organic silicone oil, then heating up the end isocyanic acid radical organic silicone oil to carry out thereaction of epsilon-caprolactam sealing the end isocyanic acid radical to obtain acylated caprolactam which contains the organic silicone oil and has the action of anionic polymerization catalysis promotion; and finally, adding an epsilon-caprolactam anionic polymerization catalyst to polymerize the rest epsilon-caprolactam to obtain the hydrophobic organosilicon / polyamide 6 block copolymer, wherein the weight ratio of the organic silicone oil to the polyamide 6 is between 4.5 and 40 to 100. The copolymer can be directly cast and formed or be mixed with polyamides for modification. The copolymer has the functions of improving the surface hydrophobicity of materials, and improving the surface lubricity and tenacity.

Description

technical field [0001] The present invention relates to a kind of in-situ preparation method of hydrophobic organosilicon / polyamide 6 block copolymer, specifically, it is a kind of co-catalyst that first prepares ε-caprolactam anion polymerization by taking hydroxyl-terminated organosilicon oil as raw material, and then A method for in situ initiating anionic polymerization of ε-caprolactam together with an anionic polymerization catalyst to prepare organosilicone oil and polyamide 6 block copolymer. technical background [0002] Polyamide is one of the most important varieties of engineering plastics. It has been widely used in industries such as automobiles, electrical appliances, communications, electronics, and machinery. The rapid development of these industries has put forward new and higher requirements for its performance and functions. Block copolymerization modification is one of the effective ways to improve its performance and functionalization. Block copolymeriz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/455
Inventor 翁盛光陈建定夏浙安贡鸾鸾
Owner EAST CHINA UNIV OF SCI & TECH