CN111621146A - Low-water-absorption polyamide material and preparation method thereof - Google Patents
Low-water-absorption polyamide material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention relates to a polyamide material with low water absorption and a preparation method thereof, belonging to the technical field of high polymer materials. The material comprises the following components in parts by weight: 94-98 parts of polyamide resin, 1-3 parts of graft, 1-3 parts of alkyl phenolic vulcanized resin, 0.5-0.8 part of thermal stabilizing additive, 0.3-0.8 part of processing lubricant and 0.03-0.05 part of silicone oil. A certain amount of alkyl phenolic vulcanized resin and graft are added into polyamide resin, so that the water absorption rate of the finally prepared polyamide material can be effectively reduced, the problems of poor dimensional stability, mechanical property, electrical property and the like of the polyamide material due to hygroscopicity are solved, and the polyamide material has the advantages of small addition amount, high efficiency, low cost, no influence on material performance and the like. The material is simple in preparation method, easy to operate, low in equipment requirement and suitable for expanded production.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a low-water-absorption polyamide material and a preparation method thereof.
Background
Polyamide 6(PA6) and polyamide 66(PA66) have become one of the most widely used engineering plastics due to their excellent comprehensive properties, and are widely used in the fields of automobiles, aerospace, general machines, electronics and electrical products, instruments and meters, household appliances, office instruments and the like. However, in the later use process of the PA6 and PA66 products, due to the fact that-NHCO-groups in molecular chains have strong polarity, hydrogen bonds are easily formed with water molecules in the environment, the products have large water absorption rate, and the size stability, the mechanical property and the electrical property of the PA6 and PA66 products are poor, so that the use of the products is influenced.
In order to reduce the water absorption of PA6, PA66, researchers have proposed various solutions, mainly the following three methods: 1. adding fillers (glass fiber, talcum powder, montmorillonite, wollastonite and the like), and reducing the content of PA6 and PA66 in the composite material to reduce the water absorption; 2. adding low water absorption materials (polyolefin, polyketone, aromatic nylon, PPS, PPO and the like), and reducing water absorption by adding the low water absorption materials and PA6 and PA66 in the form of alloy; 3. the water absorption rate is reduced by adding a low water absorption auxiliary agent (a monomer which reacts with an amide group, an acid anhydride group which reacts with an amide group, a carboxylic acid group, a graft, a wax which functions as a barrier, a silicone, or the like) to reduce the formation of hydrogen bonds between the amide and water and to block the contact between water and the amide group. Although the methods can reduce the water absorption of PA6 and PA66, the methods have the problems of large addition amount of fillers and low water absorption materials, limited efficiency, influence on the performance of the whole material, high cost, color and the like, and limit the application range of PA6 and PA 66.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a polyamide material with low water absorption; the other purpose is to provide a preparation method of the polyamide material with low water absorption.
In order to achieve the purpose, the invention provides the following technical scheme:
1. a low water absorption polyamide material comprises the following components in parts by weight: 94-98 parts of polyamide resin, 1-3 parts of graft, 1-3 parts of alkyl phenolic vulcanized resin, 0.5-0.8 part of thermal stabilizing additive, 0.3-0.8 part of processing lubricant and 0.03-0.05 part of silicone oil.
Preferably, the polyamide resin is an aliphatic polyamide resin.
Preferably, the polyamide resin is one or more of polyamide 6(PA6) or polyamide 66(PA 66).
Preferably, the graft is one or more of ethylene-octene copolymer grafted maleic anhydride (POE-g-MAH), ethylene-octene copolymer grafted glycidyl methacrylate (POE-g-GMA), ethylene propylene diene monomer grafted maleic anhydride (EPDM-g-MAH), ethylene propylene diene monomer grafted glycidyl methacrylate (EPDM-g-GMA), polyethylene grafted maleic anhydride (PE-g-MAH), polyethylene grafted glycidyl methacrylate (PE-g-GMA), polypropylene grafted maleic anhydride (PP-g-MAH) or polypropylene grafted glycidyl methacrylate (PP-g-GMA).
Preferably, the content of hydroxymethyl in the alkylphenol aldehyde vulcanized resin is 4-15%.
Preferably, the alkyl phenol aldehyde vulcanized resin is one of octyl phenol aldehyde vulcanized resin or tert-butyl phenol aldehyde vulcanized resin.
Preferably, the thermal stabilizing auxiliary agent is one or more of antioxidant 1010, antioxidant 168, antioxidant 1098, antioxidant 1076, antioxidant H10 or antioxidant H161.
Preferably, the processing lubricant is one or more of polyethylene wax, silicone, hard zinc or hard calcium.
2. The preparation method of the low water absorption polyamide material comprises the following steps: the polyamide resin, the graft, the alkyl phenolic vulcanized resin, the thermal stabilizing additive, the processing lubricant and the silicone oil are uniformly mixed and then added into an extruder, and the mixture is melted, blended, extruded, drawn into strips, granulated and dried, so that the material is obtained.
Preferably, the extruder is a co-rotating twin-screw extruder, and the length-diameter ratio is 40.
Preferably, the thread combination of the co-rotating twin-screw extruder is as follows: 48 × 3, 32, 22 × 2, K48 × 30 °, 22, K32 × 45 °, K22 × 60 °, K22 × 60 °, 22, K32 × 45 °, K22 × 60 °, 32, K32 × 90 °, 11L, 48 × 3, 32 × 2, 22 × 3, K32 × 45 °, K22 × 60 °, 22, K32 × 45 ° L, 22, K32 × 45 °, K22 × 60 °, 22, K32 × 90 °, 11L, 48 × 4, 32 × 4, 22 × 3, and a screw head.
Preferably, the temperature of each section of the extruder from the main feed inlet to the head is as follows: 50 ℃, 90-150 ℃, 220-270 ℃, 230-270 ℃ and 220-260 ℃.
Preferably, the rotating speed of the extruder is 250-300 r/min.
The invention has the beneficial effects that: the invention provides a polyamide material with low water absorption and a preparation method thereof, wherein a certain amount of alkyl phenolic vulcanized resin and graft are added into polyamide resin, so that the water absorption of the finally prepared polyamide material can be effectively reduced, the problems of poor dimensional stability, mechanical property, electrical property and the like of the polyamide material due to hygroscopicity are solved, and the polyamide material has the advantages of small addition amount, high efficiency, low cost, no influence on material performance and the like. Wherein, hydroxymethyl and phenolic groups in the alkyl phenolic vulcanized resin can take precedence over water to act with amide groups in the polyamide resin, so that the formation of hydrogen bonds between the amide groups and water molecules is effectively reduced, and the water absorption of the finally prepared polyamide material is reduced. In addition, the addition of the graft can increase the compatibility of the alkylphenol aldehyde vulcanized resin and the polyamide resin, thereby on one hand, increasing the contact of hydroxymethyl and phenol groups in the alkylphenol aldehyde vulcanized resin and amide groups in the polyamide resin, ensuring that the hydroxymethyl and phenol groups in the alkylphenol aldehyde vulcanized resin can act with the amide groups in the polyamide resin to the maximum extent, and further ensuring the low water absorption rate of the finally prepared polyamide material; on the other hand, the alkyl phenolic vulcanized resin is uniformly dispersed in the polyamide resin, so that the mechanical property of the finally prepared polyamide material can be ensured. The material is simple in preparation method, easy to operate, low in equipment requirement and suitable for expanded production.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
A low water absorption polyamide material comprises the following components in parts by weight: PA 696 parts, POE-g-MAH 2 parts, octyl phenolic vulcanized resin 2 parts with 10 percent of hydroxymethyl content, antioxidant H100.4 parts, silicone 0.5 part and silicone oil 0.03 part.
Example 2
The difference from example 1 is PA 698, POE-g-MAH 1 and octyl phenol-formaldehyde vulcanized resin with 10% hydroxymethyl.
Example 3
The difference from example 1 is PA 694 parts, POE-g-MAH 3 parts, and octyl phenol novolac sulfide resin having a methylol group content of 10% 3 parts.
Example 4
The difference from example 1 is that POE-g-MAH was replaced with EPDM-g-MAH.
Example 5
The difference from example 2 is that POE-g-MAH was replaced with EPDM-g-MAH.
Example 6
The difference from example 3 is that POE-g-MAH was replaced with EPDM-g-MAH.
Example 7 to example 12
PA6 was replaced with PA66 in all of examples 1 to 6.
Comparative example 1
The difference from example 1 is that the octyl phenol novolac resin was replaced with a phenol novolac resin.
Comparative example 2
The difference from example 1 is PA 698 and 0 part of octyl phenol-formaldehyde curing resin with 10% of hydroxymethyl group.
Comparative example 3
The difference from example 7 is that the octyl phenol novolac resin was replaced with a phenol novolac resin.
Comparative example 4
The difference from example 7 is PA 6698 parts, 0 part of octyl phenol-formaldehyde curing resin with 10% hydroxymethyl group.
The polyamide materials with low water absorption in examples 1 to 6 and the polyamide materials in comparative examples 1 to 2 were prepared as follows: the preparation method comprises the following steps of uniformly stirring and mixing polyamide resin, a graft, alkyl phenolic vulcanized resin, a heat stabilizing auxiliary agent, a processing lubricant and silicone oil, adding the mixture into a co-rotating double-screw extruder with the length-diameter ratio (L/D) of 40, and carrying out melting, blending, extruding, drawing, granulating and drying, wherein the screw thread combination of the extruder is as follows: 48 × 3, 32, 22 × 2, K48 × 30 °, 22, K32 × 45 °, K22 × 60 °, K22 × 60 °, 22, K32 × 45 °, K22 × 60 °, 32, K32 × 90 °, 11L, 48 × 3, 32 × 2, 22 × 3, K32 × 45 °, K22 × 60 °, 22, K32 × 45 ° L, 22, K32 × 45 °, K22 × 60 °, 22, K32 × 90 °, 11L, 48 × 4, 32 × 4, 22 × 3, a screw head; the temperature of each section from the main feed inlet to the head of the extruder is as follows: 50 ℃, 90 ℃, 220 ℃, 230 ℃, 220 ℃, and the rotation speed of the extruder is 300 r/min.
The polyamide materials with low water absorption in examples 7 to 12 and the polyamide materials in comparative examples 3 to 4 were prepared as follows: the preparation method comprises the following steps of uniformly stirring and mixing polyamide resin, a graft, alkyl phenolic vulcanized resin, a heat stabilizing auxiliary agent, a processing lubricant and silicone oil, adding the mixture into a co-rotating double-screw extruder with the length-diameter ratio (L/D) of 40, and carrying out melting, blending, extruding, drawing, granulating and drying, wherein the screw thread combination of the extruder is as follows: 48 × 3, 32, 22 × 2, K48 × 30 °, 22, K32 × 45 °, K22 × 60 °, K22 × 60 °, 22, K32 × 45 °, K22 × 60 °, 32, K32 × 90 °, 11L, 48 × 3, 32 × 2, 22 × 3, K32 × 45 °, K22 × 60 °, 22, K32 × 45 ° L, 22, K32 × 45 °, K22 × 60 °, 22, K32 × 90 °, 11L, 48 × 4, 32 × 4, 22 × 3, a screw head; the temperature of each section from the main feed inlet to the head of the extruder is as follows: 50 ℃, 150 ℃, 260 ℃, 250 ℃ and the rotation speed of the extruder is 300 r/min.
The low water absorption polyamide materials of examples 1 to 12 and the polyamide materials of comparative examples 1 to 4 were tested for tensile strength, impact strength, notched impact strength, flexural modulus, heat distortion temperature, density and water absorption, and the test results are shown in table 1.
TABLE 1
As can be seen from table 1, the materials of examples 1 to 6 and examples 7 to 12 all had low water absorption when the alkylphenol curing resin was added.
The water absorption of the materials of comparative example 1, comparative example 1 and comparative example 2 was found to be lower for the material of example 1 with the addition of the alkylphenol formaldehyde curing resin than for the material with the addition of the phenol novolac resin and the material without the phenol novolac resin, and similarly, the water absorption of the materials of comparative example 7, comparative example 3 and comparative example 4 was found to be lower for the material of example 7 with the addition of the alkylphenol formaldehyde curing resin than for the material with the addition of the phenol novolac resin and the material without the phenol novolac resin.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.
Claims (10)
1. A low water absorption polyamide material is characterized by comprising the following components in parts by weight: 94-98 parts of polyamide resin, 1-3 parts of graft, 1-3 parts of alkyl phenolic vulcanized resin, 0.5-0.8 part of thermal stabilizing additive, 0.3-0.8 part of processing lubricant and 0.03-0.05 part of silicone oil.
2. A low water absorption polyamide material as claimed in claim 1, wherein the polyamide resin is an aliphatic polyamide resin.
3. A low water absorption polyamide material as claimed in claim 2, wherein the polyamide resin is one or more of polyamide 6 or polyamide 66.
4. A low water absorption polyamide material as claimed in claim 1, wherein the graft is one or more of ethylene-octene copolymer grafted maleic anhydride, ethylene-octene copolymer grafted glycidyl methacrylate, ethylene-propylene-diene monomer grafted maleic anhydride, ethylene-propylene-diene monomer grafted glycidyl methacrylate, polyethylene grafted maleic anhydride, polyethylene grafted glycidyl methacrylate, polypropylene grafted maleic anhydride or polypropylene grafted glycidyl methacrylate.
5. A low water absorption polyamide material as claimed in claim 1, wherein the methylol content of the alkylphenol-formaldehyde curing resin is 4-15%.
6. The low water absorption polyamide material of claim 1, wherein the thermal stabilizing aid is one or more of antioxidant 1010, antioxidant 168, antioxidant 1098, antioxidant 1076, antioxidant H10 or antioxidant H161.
7. A low water absorption polyamide material as claimed in claim 1, wherein the processing lubricant is one or more of polyethylene wax, silicone, hard zinc or hard calcium.
8. A process for the preparation of a polyamide material with low water absorption according to any of claims 1 to 7, characterized in that it comprises the following steps: the polyamide resin, the graft, the alkyl phenolic vulcanized resin, the thermal stabilizing additive, the processing lubricant and the silicone oil are uniformly mixed and then added into an extruder, and the mixture is melted, blended, extruded, drawn into strips, granulated and dried, so that the material is obtained.
9. The method of claim 8, wherein the temperature of the extruder in each section from the main feed port to the head is: 50 ℃, 90-150 ℃, 220-270 ℃, 230-270 ℃ and 220-260 ℃.
10. The method as claimed in claim 8, wherein the rotation speed of the extruder is 250-300 r/min.
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