Copolymerized flame-retardant polyamide and preparation method thereof

A technology for copolymerizing flame retardant and polyamide is applied in the fields of copolymerization flame retardant polyamide and its preparation, the preparation of triblock phosphorus-containing copolymer flame retardant polyamide, and the preparation of flame retardant salt, which can solve the problem of long-term flame retardant effect, long-term flame retardant effect and high flame retardant effect. Affecting fabric dyeing properties, uneven distribution and other issues

A technology for copolymerizing flame retardant and polyamide is applied in the fields of copolymerization flame retardant polyamide and its preparation, the preparation of triblock phosphorus-containing copolymer flame retardant polyamide, and the preparation of flame retardant salt, which can solve the problem of long-term flame retardant effect, long-term flame retardant effect and high flame retardant effect. Affecting fabric dyeing properties, uneven distribution and other issues

CN112225892AActive Publication Date: 2021-01-15DONGHUA UNIV

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  • Copolymerized flame-retardant polyamide and preparation method thereof
  • Copolymerized flame-retardant polyamide and preparation method thereof
  • Copolymerized flame-retardant polyamide and preparation method thereof

Examples

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Effect test

Embodiment 1

[0055]A preparation method of copolymer flame-retardant polyamide 6 / 66, the steps are as follows:

[0056](1) Preparation of flame retardant salt;

[0057](1.1) Combine DOPO derivatives and diamine NH2R2NH2Mix at a molar ratio of 1:2.1, then add 25wt% of the total mass of the system as the reaction solvent, heating up (starting at 25°C) and stirring under nitrogen protection, the stirring speed is 100r / min, DOPO derivative The structural formula of is shown in formula (I), where R1For CH2, Diamine NH2R2NH2Hexamethylene diamine;

[0058]The preparation process of DOPO derivatives is as follows: Put DOPO-HQ and acid binding agent (triethylamine) into a three-necked flask, add solvent (ethanol) to dissolve, and add chloroacetate (methyl chloroacetate) dropwise at 100°C. ), after 14 hours of reaction, the solvent and unreacted chloroacetate are removed by rotary evaporation, the ester bond of the obtained intermediate is hydrolyzed by adding sodium hydroxide in ethanol, then hydrochloric acid is...

Embodiment 2

[0089]A preparation method of copolymer flame-retardant polyamide 6 / 66, the steps are as follows:

[0090](1) Preparation of flame retardant salt;

[0091](1.1) Combine DOPO derivatives and diamine NH2R2NH2Mix at a molar ratio of 1:2.02, and then add 26wt% of the total mass of the system as the reaction solvent. Under nitrogen protection, heat up (starting at 25°C) and stir. The stirring speed is 120r / min. DOPO derivative The structural formula of is shown in formula (I), where R1As (CH2)2, Diamine NH2R2NH2Is decane diamine;

[0092]The preparation process of DOPO derivatives is as follows: Put DOPO-HQ and acid binding agent (triethylamine) into a three-necked flask, add solvent (ethanol) to dissolve, and add chloropropionate (3-chloropropionate) dropwise at 100℃. After 14 hours of reaction, the solvent and unreacted chloropropionate were removed by rotary evaporation, and the ester bond of the obtained intermediate was hydrolyzed by adding sodium hydroxide in ethanol. After adding hydrochlo...

Embodiment 3

[0114]A preparation method of copolymer flame-retardant polyamide 6 / 66, the steps are as follows:

[0115](1) Preparation of flame retardant salt;

[0116](1.1) Combine DOPO derivatives and diamine NH2R2NH2Mix in a molar ratio of 1:2.15, and add 28wt% of the total mass of the system as the reaction solvent. Under nitrogen protection, heat up (starting at 25°C) and stir. The stirring speed is 115r / min. DOPO derivative The structural formula of is shown in formula (I), where R1As (CH2)3, Diamine NH2R2NH2Is propylene diamine;

[0117]The preparation process of DOPO derivatives is as follows: put DOPO-HQ and acid binding agent (triethylamine) into a three-necked flask, add solvent (ethanol) to dissolve, and add chlorobutyrate (4-chlorobutane) dropwise at 100℃. After the reaction for 14 hours, the solvent and unreacted chlorobutyrate are removed by rotary evaporation, and the ester bond of the obtained intermediate is hydrolyzed by adding sodium hydroxide in ethanol. After adding hydrochloric aci...

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Abstract

The invention relates to copolymerized flame-retardant polyamide and a preparation method thereof. The preparation method comprises the following steps: mixing a flame retardant salt with a polyamide6 oligomer and / or a polyamide 66 oligomer, and carrying out condensation polymerization to obtain copolymerized flame-retardant polyamide. The flame retardant salt is prepared from a DOPO derivative and diamine NH2R2NH2 through a high-temperature and high-pressure reaction. The temperature of the high temperature is 200-250 DEG C, and the pressure of the high pressure is 1.2-1.8 MPa. The structural formula of the finally obtained copolymerized flame-retardant polyamide is as follows. In the structural formula, x is the polymerization degree of the polyamide 6 oligomer, y is the polymerizationdegree of the polyamide 66 oligomer, and the structural formula of Rz is as follows. The preparation method disclosed by the invention is simple to operate, and the prepared product has excellent flame retardance, good impact resistance and processability.

Description

Technical field[0001]The invention belongs to the technical field of flame-retardant polyamide synthesis, and relates to a copolymerized flame-retardant polyamide and a preparation method thereof, in particular to a new preparation method of flame-retardant salt, and a preparation method of triblock phosphorus-containing copolymer flame-retardant polyamide .Background technique[0002]Polyamide 6 and polyamide 66 are the two varieties with the largest output and the most widely used in polyamide products. They are also widely used engineering plastics. They have high mechanical strength, good wear resistance, and good solvent resistance. However, the impact resistance of polyamide 6 is low; while polyamide 66 has a high melting point and a narrow processing temperature range, which limits the application of both in certain fields. Therefore, polyamide 6 and polyamide 66 are copolymerized and modified by the melt copolymerization method to prepare polyamide 6 / 66 composite materials, wh...

Claims

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Application Information

Patent Timeline
15 Jan 2021
Publication
CN112225892A
IPC
C08G69/42
CPC
C08G69/42
Inventors
肖茹; 郑裕磊