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Copolymerized flame-retardant polyamide and preparation method thereof

A technology for copolymerization of flame retardant and polyamide, which is applied in the fields of copolymerization flame retardant polyamide and its preparation, preparation of flame retardant salt, and preparation of triblock phosphorus-containing copolymer flame retardant polyamide, and can solve the problem of easy flame retardant salt. Destruction, low reactivity, affecting the polymerization process, etc.

Active Publication Date: 2020-12-08
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patents (publication numbers CN106832911A, CN106633828A, CN106633043A, CN106675007A, etc.) all prepare phosphorus-containing copolymerized flame-retardant polyamide materials by copolymerization. When preparing flame retardant salts, they are all carried out at low temperature (60-90° C.) under normal pressure. The reactivity is low, and the molecular weight of the polymer is seriously reduced when the amount of flame retardant is large, and the flame retardant monomer and the diamine are not connected by covalent bonds under this condition, so in the later polymerization process, the flame retardant Salt is easily destroyed, thus affecting the polymerization process

Method used

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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

Experimental program
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Effect test

Embodiment 1

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

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

[0057](1.1) Mix N,N-bis(6-aminohexyl)phenylphosphoramide and adipic acid in an equimolar ratio, and then add 55wt% of the total mass of the system as the reaction solvent, and increase the temperature under nitrogen protection (The starting point of heating is 25°C) and stirring, the stirring speed is 50r / min, N,N-bis(6-aminohexyl)phenylphosphoramide is a mixture of the structure compound of formula (I) and the structure compound of formula (II) ;

[0058]The preparation process of N,N-bis(6-aminohexyl)phenylphosphoryl diamide is as follows: Dissolve hexamethylene diamine and phenylphosphoryl dichloride in an organic solvent (chloroform) at 25℃, and stir Next, add the organic solution of hexamethylene diamine to the organic solution of phenylphosphoryl dichloride. The molar ratio of phenylphosphoryl dichloride to hexamethylene diamine is 1:2. Af...

Embodiment 2

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

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

[0091](1.1) Mix N,N-bis(6-aminohexyl)phenyl phosphorodiamide and malonic acid in an equimolar ratio, and then add deionized water accounting for 56wt% of the total mass of the system as the reaction solvent, and proceed under nitrogen protection Increase the temperature (starting point is 25℃) and stir. The stirring speed is 70r / min. N,N-bis(6-aminohexyl)phenylphosphoramide is the difference between the structure compound of formula (I) and the structure compound of formula (II). mixture;

[0092]The preparation process of N,N-bis(6-aminohexyl)phenylphosphoryl diamide is as follows: Dissolve hexamethylene diamine and phenylphosphoryl dichloride in an organic solvent (acetonitrile) at 25°C. Add the organic solution of hexamethylene diamine dropwise to the organic solution of phenylphosphoryl dichloride. The molar ratio of phenylphosphoryl dichlor...

Embodiment 3

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

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

[0116](1.1) Mix N,N-bis(6-aminohexyl)phenyl phosphorodiamide and succinic acid in an equimolar ratio, and then add deionized water accounting for 58wt% of the total mass of the system as the reaction solvent, and proceed under nitrogen protection Raise the temperature (starting point is 25℃) and stir, the stirring speed is 65r / min, N,N-bis(6-aminohexyl)phenylphosphoramide is the difference between the structure compound of formula (I) and the structure compound of formula (II) mixture;

[0117]The preparation process of N,N-bis(6-aminohexyl)phenylphosphoramide is the same as in Example 1;

[0118](1.2) After the temperature rises to 213℃, keep the pressure at 1.75MPa, keep the temperature and keep the pressure for 2h;

[0119](1.3) Reduce the pressure to normal pressure within 0.8h, reduce the stirring speed to 50r / min, and vacuum to -0.07MPa for 0.6h...

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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 polyamide66 oligomer and / or a polyamide 6 oligomer, and carrying out condensation polymerization to obtain copolymerized flame-retardant polyamide; wherein the flame retardant salt is prepared from N, Ndi (6aminohexyl) phenyl phosphoramide and binary acid HOOCR1COOH through a high-temperature and high-pressure reaction; wherein the temperature of the high temperature is 210-220 DEG C, and the pressure of the high pressure is 1.7-1.9 MPa; wherein in the structural formula, x is the polymerization degree of the polyamide 66 oligomer, y is the polymerization degree of the polyamide 6 oligomer, and the structural formula of Rz1 is as follows: the structural formula of Rz2 is as follows: the preparation method disclosed by the invention is simple to operate, and the prepared product has excellent flameretardance, 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 66 and polyamide 6 are the two varieties with the largest output and the most widely used in polyamide products. They are also widely used engineering plastics on the market. They have high mechanical strength, good abrasion resistance, and good solvent resistance. characteristic. However, polyamide 66 has a high melting point and a narrow processing temperature range; while polyamide 6 has low impact resistance, which limits the application of both in certain fields. Therefore, by copolymerizing and modifying polyamide 66 and polyamide 6 by melt copolymerization to prepare polyamide 66 / 6, the ...

Claims

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Application Information

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IPC IPC(8): C08G69/42
CPCC08G69/42
Inventor 肖茹陈爽郑裕磊王星帅刘畅刘可李梦娇王华平
Owner DONGHUA UNIV
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