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Fluorine-containing water-resistant polyamide 6 and preparation method thereof

A technology of polyamide and water resistance, which is applied in the field of fluorine-containing water-resistant polyamide 6 and its preparation, can solve the problems of dimensional stability decline, material volume expansion, and size reduction, and achieve a balance between mechanical properties, high modulus, and space The effect of high steric hindrance

Inactive Publication Date: 2021-06-25
JIAXING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In order to solve the problems of polyamide 6 resin in the prior art, such as material volume expansion, modulus decrease, and dimensional stability decrease caused by water absorption, the present invention provides a fluorine-containing water-resistant polyamide 6 and a preparation method thereof
In the present invention, a fluorine-containing chain extender is prepared by a one-step reaction between a diamino fluorine-containing compound containing a water-resistant benzene ring structure and a dibasic acid, and a large amount of fluorine-containing chain extender is introduced into the main chain of the polyamide resin through a polymerization reaction with a polyamide prepolymer. The fluorine-containing chain extender of sexual functional groups can improve the water resistance of polyamide materials, and solve the problems of material volume expansion, modulus decrease, and dimensional stability decrease of polyamide 6 resins caused by water absorption; the fluorine-containing water-resistant polyamide of the present invention can simultaneously Can maintain good mechanical properties

Method used

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  • Fluorine-containing water-resistant polyamide 6 and preparation method thereof
  • Fluorine-containing water-resistant polyamide 6 and preparation method thereof
  • Fluorine-containing water-resistant polyamide 6 and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] A preparation method of fluorine-containing water-resistant polyamide 6, the specific steps are as follows:

[0052] (1) 2,2-bis[4-(4-aminophenoxybenzene)]hexafluoropropane with a molar ratio of 1:1 and malonic acid in dicyclohexylcarbodiimide and 4-N,N -Under the action of lutidine, react at a temperature of 110°C for 1 hour, and then vacuum-dry at 60°C for 2 hours to obtain a fluorine-containing chain extender; wherein, malonic acid: dicyclohexylcarbodiimide: 4- The molar ratio of N,N-lutidine is 1:0.5:1;

[0053] The structural formula of the obtained fluorine-containing chain extender is: m is 43, molecular weight is 26015Da;

[0054] (2) Use caprolactam, water, phosphoric acid, and tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] pentaerythritol ester as raw materials at a temperature of 220°C and a vacuum of -0.05MPa Reaction for 10 minutes, and then precondensation reaction for 1.5 hours under a pressure of 0.3 MPa to obtain a prepolymer of polyamid...

Embodiment 2

[0066] A preparation method of fluorine-containing water-resistant polyamide 6, the specific steps are as follows:

[0067] (1) 2,2'-bis(trifluoromethyl)diaminobiphenyl and succinic acid at a molar ratio of 1:1 in dicyclohexylcarbodiimide and 4-N,N-lutidine Under the action of , react at a temperature of 100°C for 1h, and then vacuum dry at 60°C for 2h to obtain a fluorine-containing chain extender; wherein,

[0068] The molar ratio of succinic acid: dicyclohexylcarbodiimide: 4-N,N-lutidine is 1:0.5:1;

[0069] The structural formula of the obtained fluorine-containing chain extender is: m is 50, molecular weight is 22050Da;

[0070] (2) Use caprolactam, water, boric acid, and 2,6-p-di-tert-butyl-p-cresol as raw materials, react for 10 minutes at a temperature of 235°C, and a vacuum of -0.05MPa, and then under the condition of a pressure of 0.3MPa Precondensation reaction 0.5h, obtains the prepolymer of polyamide 6;

[0071] Wherein, the mass ratio of caprolactam, boric a...

Embodiment 3

[0078] A preparation method of fluorine-containing water-resistant polyamide 6, the specific steps are as follows:

[0079] (1) 2,2'-bis(4-aminophenyl)hexafluoropropane and glutaric acid at a molar ratio of 1:1 in dicyclohexylcarbodiimide and 4-N,N-lutidine Under the action of , react at a temperature of 110°C for 1h, and then vacuum-dry at 60°C for 2h to obtain a fluorine-containing chain extender; wherein,

[0080] The molar ratio of glutaric acid: dicyclohexylcarbodiimide: 4-N,N-lutidine is 1:0.5:1;

[0081] The structural formula of the obtained fluorine-containing chain extender is: m is 27, molecular weight is 12582Da;

[0082] (2) Use caprolactam, water, phosphoric acid ester, and 2,6-tert-butyl-4-methylphenol as raw materials, react at a temperature of 230°C and a vacuum of -0.05MPa for 10min, and then Precondensation reaction 1h under condition, obtain the prepolymer of polyamide 6;

[0083] Wherein, the mass ratio of caprolactam, phosphoric acid ester and water ...

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Abstract

The invention relates to fluorine-containing water-resistant polyamide 6 and a preparation method thereof, and the method comprises the following steps: adding a fluorine-containing chain extender into a prepolymer of polyamide 6, and carrying out polymerization reaction to prepare the fluorine-containing water-resistant polyamide 6. The structural formula of the fluorine-containing chain extender is shown in the specification, wherein X is a group containing a benzene ring, an ether bond, tertiary-butyl carbon and sulfuryl, Y is methylene containing 1-9 carbon atoms, and m is 10-50. The addition amount of the fluorine-containing chain extender is 10-50wt% of the feeding mass of caprolactam. The structural formula of the prepared fluorine-containing water-resistant polyamide 6 is shown in the specification, wherein the ratio of m to n to p is (10-50):(95-250):(150-250). According to the method disclosed by the invention, the interface compatibility between polyamide and a fluorine-containing polymer and the like is better improved by forming a fluorine-containing block copolymer through a polymerization reaction, and the prepared fluorine-containing water-resistant polyamide 6 is good in mechanical property and stress creep resistance caused by water absorption.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a fluorine-containing water-resistant polyamide 6 and a preparation method thereof. Background technique [0002] The molecular structure of polyamide contains amino groups and carbonyl groups that are easy to form hydrogen bonds with water molecules, and the resulting material is easy to absorb water (polyamide can absorb up to 10wt.% of moisture from humid air), resulting in a plasticizing effect, resulting in volume expansion of the material , The modulus decreases, the creep under the stress is obvious, and the dimensional stability decreases. The water absorption rate of nylon 6 in water is 8.5% to 10%, and the water absorption rate in air is 1.8% to 2.9%. Therefore, it is necessary to reduce the water absorption of polyamide. [0003] There are three effective ways to obtain water-resistant nylon: 1. Filling and modification of inorganic materials to reduce the co...

Claims

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Application Information

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IPC IPC(8): C08G69/42
CPCC08G69/42
Inventor 胡英颜志勇王晓馨姚勇波李喆生俊露
Owner JIAXING UNIV
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