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Plant oil benzoxazine copolymer elastomer preparation method

A technology of benzoxazine and elastomer, which is applied in the field of preparation of vegetable oil benzoxazine copolymer elastomer, can solve problems that have not yet been reported on polymer materials, achieve excellent thermal stability, reduce production costs, and structural rigidity strong effect

Inactive Publication Date: 2014-11-12
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The prior art has not yet involved reports on polymer materials formed by the copolymerization of polybenzoxazine and vegetable oil-based polymers

Method used

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  • Plant oil benzoxazine copolymer elastomer preparation method
  • Plant oil benzoxazine copolymer elastomer preparation method
  • Plant oil benzoxazine copolymer elastomer preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A kind of preparation method of soybean oil benzoxazine copolymer elastomer, comprises the steps:

[0030] (1) Ring-opening addition of part of the epoxy groups of epoxy soybean oil and ethylenediamine to obtain soybean oil-based prepolymer: when the epoxy soybean oil oil bath is heated to 85°C, add ethylenediamine and triethylamine Catalyst, the mass ratio of epoxidized soybean oil, ethylenediamine and triethylamine is 100:6.5:1.0, then the oil temperature is raised to 95°C, and the reaction is stopped after continuing the constant temperature reaction for 3.5 hours.

[0031] (2) Preparation method of amino-containing benzoxazine monomer

[0032] Using trifluoroacetic anhydride (TAFF) as amine protecting agent, a benzoxazine blocker retaining amino group was synthesized. The reaction equation is as follows:

[0033]

[0034] Dissolve 4-aminophenol in tetrahydrofuran, put it in an ice-water bath and stir for 30 minutes, add trifluoroacetic anhydride dropwise, the m...

Embodiment 2

[0045] (1) Ring-opening addition of some epoxy groups of epoxy soybean oil and triethylenetetramine to obtain soybean oil-based prepolymer. When the epoxidized soybean oil oil bath is heated to 120 DEG C, add triethylenetetramine and trimethylamine catalyst, the mass ratio of epoxidized soybean oil: triethylenetetramine: trimethylamine is 100: 2.5: 0.2, then the oil temperature rises Up to 125°C, continue the constant temperature reaction for 1.5 hours and then stop the reaction

[0046] (2) The preparation method of amino-containing benzoxazine.

[0047] Dissolve 2-aminophenol in tetrahydrofuran, put it in an ice-water bath and stir for 15 minutes, then add trifluoroacetic anhydride dropwise, 2-aminophenol: trifluoroacetic anhydride in a mass ratio of 100:250, and control the rate of addition in 60 minutes. The tetrahydrofuran was removed by evaporation, and ethyl acetate was added to dissolve the product, washed three times with saturated brine, dried by adding anhydrous so...

Embodiment 3

[0056] (1) Ring-opening addition of some epoxy groups of epoxy soybean oil and piperazine to obtain soybean oil-based prepolymer. When epoxy soybean oil oil bath is heated to 85 ℃, add piperazine and triethylamine catalyst, epoxy soybean oil: piperazine: the mass ratio of triethylamine is 100: 8.5: 1.0, then oil temperature is raised to 95°C, continue the constant temperature reaction for 3.5 hours, then stop the reaction.

[0057] (2) The preparation method of amino-containing benzoxazine.

[0058] Dissolve 3-aminophenol in tetrahydrofuran, put it in an ice-water bath and stir for 30 minutes, then add trifluoroacetic anhydride dropwise, 3-aminophenol: trifluoroacetic anhydride in a mass ratio of 100:250, and control the rate of addition to finish dropping in 30 minutes. The tetrahydrofuran was removed by evaporation, and ethyl acetate was added to dissolve the product, washed three times with saturated brine, dried by adding anhydrous sodium sulfate, filtered, and the solven...

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Abstract

The invention discloses preparation method of a plant oil benzoxazine copolymer elastomer. The elastomer is obtained by copolymerization of a plant-oil-based prepolymer, an amino-comprising benzoxazine monomer, a monocyclic benzoxazine monomer, and a bicyclic benzoxazine monomer. According to the invention, epoxy vegetable oil is heated to 85-120 DEG C in an oil bath, polyamine and tertiary amine catalyst are added, the oil temperature is increased to 95-125 DEG C, and constant-temperature reaction is carried out for 1.5-3.5h, such that the plant-oil-based prepolymer is prepared. The amino-comprising benzoxazine is prepared through a dehydration condensation reaction of an amino-substituted phenol compound, aniline and paraformaldehyde. Benzoxazine is prepared through a dehydration condensation reaction of a phenol compound, aniline and paraformaldehyde. According to the invention, the plant-oil-based prepolymer is adopted as a soft segment, polybenzoxazine is adopted as a hard segment, and the amino-comprising benzoxazine is adopted as a grafting agent, such that the prepared plant oil benzoxazine copolymer elastomer has the advantages of high modulus, high glass transition temperature, high hot strength, excellent thermal stability, and excellent thermal mechanical property.

Description

technical field [0001] The invention relates to a copolymer elastomer, in particular to a preparation method of a vegetable oil benzoxazine copolymer elastomer. The elastomer of the present invention is a polymer material formed by copolymerization of polybenzoxazine and vegetable oil-based polymer. Background technique [0002] Polymeric elastomers are copolymers (linear or low-density cross-linked) composed of soft segments and hard segments. They have high tensile modulus, excellent wear resistance, oil resistance, fatigue resistance, and vibration resistance. They are widely used It is a synthetic material with great development potential, which is used in many fields such as automobiles, construction, mining, aerospace, electronics, and medical equipment. The existing synthetic elastomer materials mainly include polyolefin, polyurethane, polyester, polyamide and so on. [0003] With the rapid consumption of petroleum resources, the preparation of renewable polymer ela...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/06C08G59/50C08G59/20
Inventor 司徒粤朱祖威黄洪
Owner SOUTH CHINA UNIV OF TECH
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