CN111138847B - Mixed antistatic semi-aromatic nylon resin and preparation method thereof - Google Patents
Mixed antistatic semi-aromatic nylon resin and preparation method thereof Download PDFInfo
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- CN111138847B CN111138847B CN201911400416.1A CN201911400416A CN111138847B CN 111138847 B CN111138847 B CN 111138847B CN 201911400416 A CN201911400416 A CN 201911400416A CN 111138847 B CN111138847 B CN 111138847B
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- aromatic nylon
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- polyacrylamide
- nylon resin
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
- B29B13/10—Conditioning or physical treatment of the material to be shaped by grinding, e.g. by triturating; by sieving; by filtering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/017—Additives being an antistatic agent
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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
- C08L2201/00—Properties
- C08L2201/04—Antistatic
Abstract
The invention belongs to the technical field of modification of engineering plastics, in particular relates to a mixed antistatic semi-aromatic nylon resin and a preparation method thereof, and aims to solve the problem of poor compatibility between conductive filler and a polymer matrix in the prior art. The invention provides ion transmission capacity by the polymer and inorganic salt together to prepare the permanent antistatic semi-aromatic nylon composite material with ion mixed conductive antistatic performance and compatibility.
Description
Technical Field
The invention belongs to the technical field of modification of engineering plastics, and particularly relates to a mixed antistatic semi-aromatic nylon resin and a preparation method thereof, which can be used for regulating and controlling antistatic performance of engineering plastics.
Background
Static electricity generated by interaction of friction or stripping and the like during processing and using of plastics not only can adsorb dust and pollutants, but also can easily generate electric shock phenomenon and even cause explosion accidents. In some electronic circuits, it has been found that some faulty integrated circuits are broken down by electrostatic discharge, and that the use of antistatic materials can avoid static damage to the microelectronic circuit.
The existing method for preparing the antistatic plastic mainly comprises two methods of surface treatment and mixing. The surface active agent and the conductive paint are coated on the surface of the plastic, and the conductive layer can be prepared on the surface of the plastic by electroplating and other methods. The kneading is to add a surfactant, carbon black, a conductive filler, a conductive polymer, and the like to the resin matrix. The most widely used method at present is to add conductive filler to prepare composite material, and the antistatic property of the composite material prepared by the conductive filler is influenced by the type, skeleton structure, dispersion property, surface state, addition concentration and the like of the conductive filler; and is also affected by the kind and structure of the plastic material. Conductive fillers are used in many cases in carbon black systems, metals, metal oxides, and the like. Of these three fillers, carbon black is used in the largest amount because of its low cost. But the three fillers have poor compatibility with the polymer matrix due to differences in physical properties.
Disclosure of Invention
Aiming at the problem of poor compatibility of conductive filler and polymer matrix in the prior art, the invention provides a mixed antistatic semi-aromatic nylon resin and a preparation method thereof, and the aim is to: the ionic polymer with better compatibility, the fast ion inorganic salt and the semi-aromatic nylon are mixed, so that the conductivity of the semi-aromatic nylon resin is improved, and the antistatic performance of the semi-aromatic nylon resin is further improved.
The technical scheme adopted by the invention is as follows:
the mixed antistatic semi-aromatic nylon resin comprises the following components in percentage by mass:
2-10% of polyacrylamide containing ions;
1-3% of inorganic salt;
87-97% of semi-aromatic nylon.
After the technical scheme is adopted, the ionic polymer, the fast ion inorganic salt and the semi-aromatic nylon are mixed in the preparation process of the mixed conductive antistatic semi-aromatic nylon resin, so that the defect of poor compatibility of the conductive filler and the resin matrix is overcome.
Preferably, the semi-aromatic nylon has a number average molecular weight of 17000-43000.
Preferably, the ion-containing polyacrylamide has a weight average molecular weight of 2.0X10 5 -2.0×10 7 。
Preferably, the ion-containing polyacrylamide is one or a combination of several of anionic polyacrylamide, cationic polyacrylamide or amphoteric polyacrylamide.
Preferably, the inorganic salt is one or a combination of several of lithium salt, sodium salt or silver salt.
Further preferably, the lithium salt is LiClO 4 The sodium salt is NaClO 4 The silver salt is AgI, ag 7 I 4 PO 4 Or Ag 3 One or a combination of several of S.
The preferable scheme optimizes the components of the mixed antistatic semi-aromatic nylon resin, further enhances the conductivity and improves the antistatic performance.
The invention also provides a preparation method of the mixed antistatic semi-aromatic nylon resin, which comprises the following steps:
step 1, crushing and uniformly mixing the polyacrylamide containing ions and inorganic salt according to a proportion;
and 2, mixing the mixed raw material obtained in the step 1 with semi-aromatic nylon in proportion, extruding by using an extruder, and granulating to obtain the mixed antistatic semi-aromatic nylon resin.
According to the technical scheme, no organic solvent is introduced in the preparation process, so that the environment is prevented from being polluted by solvent volatilization, and the preparation method belongs to a clean preparation process.
Preferably, the specific process of crushing and uniformly mixing in the step 1 is as follows: mixing the polyacrylamide containing ions and inorganic salt in proportion, performing ultracentrifugal crushing by using an ultracentrifugal crusher provided with a screen, and performing ball milling mixing by using an omnibearing planetary ball mill.
Further preferably, the screen is trapezoid hole, the aperture is 0.08-0.25mm, the speed of ultracentrifugal crushing is 4000-16000rad/min, the omnibearing planetary ball mill is filled with inert gas for protection, the ball milling time is 1-3 hours, and the ball milling rotating speed is 100-500rad/min.
The preparation process of the mixed high-dielectric constant low-dielectric loss composite material in the preferred scheme is to carry out solid phase mixing by a plurality of methods, so that the defect that the common single physical method is difficult to uniformly mix can be overcome.
Preferably, the extruder in the step 2 adopts a miniature double-screw extruder, and the extrusion temperature is 170-310 ℃.
In summary, due to the adoption of the technical scheme, the beneficial effects of the invention are as follows:
1. the preparation process of the mixed conductive antistatic semi-aromatic nylon resin overcomes the defect of poor compatibility of the conductive filler and the resin matrix by mixing the ionic polymer, the fast ion inorganic salt and the semi-aromatic nylon.
2. The components of the mixed antistatic semi-aromatic nylon resin are optimized, so that the conductivity is further enhanced, and the antistatic performance is improved.
3. No organic solvent is introduced in the preparation process, so that the solvent is prevented from volatilizing to pollute the environment, and the preparation process belongs to a clean preparation process.
4. The preparation process of the mixed high-dielectric constant low-dielectric loss composite material is to carry out solid phase mixing by a plurality of methods, so that the defect that the common single physical method is difficult to uniformly mix can be overcome.
Detailed Description
All of the features disclosed in this specification, or all of the steps in a method or process disclosed, may be combined in any combination, except for mutually exclusive features and/or steps.
The mixed antistatic semi-aromatic nylon resin comprises the following components in percentage by mass:
2-10% of polyacrylamide containing ions;
1-3% of inorganic salt;
87-97% of semi-aromatic nylon.
As a preferred embodiment, the ion-containing polyacrylamide has a weight average molecular weight of 2.0X10 5 -2.0×10 7 . The average particle size of the ion-containing polyacrylamide is preferably less than 600 μm.
As a preferable scheme, the ion-containing polyacrylamide is one or a combination of several of anionic polyacrylamide, cationic polyacrylamide or amphoteric polyacrylamide.
As a preferred embodiment, the inorganic salt is one or a combination of several of lithium salt, sodium salt or silver salt.
As a preferred embodiment, the lithium salt is LiCIO 4 The sodium salt is NaCIO 4 The silver salt is AgI, ag 7 I 4 PO 4 Or Ag 3 One or a combination of several of S.
The invention also provides a preparation method of the mixed antistatic semi-aromatic nylon resin, which comprises the following steps:
step 1, crushing and uniformly mixing the polyacrylamide containing ions and inorganic salt according to a proportion;
and 2, mixing the mixed raw material obtained in the step 1 with semi-aromatic nylon in proportion, extruding by using an extruder, and granulating to obtain the mixed antistatic semi-aromatic nylon resin.
As a preferred embodiment, the inorganic salt and the ion-containing polyacrylamide are dried in vacuo at 100℃for 24 hours before use.
As a preferable scheme, the specific process of crushing and uniformly mixing in the step 1 is as follows: mixing the polyacrylamide containing ions and inorganic salt in proportion, performing ultracentrifugal crushing by using an ultracentrifugal crusher provided with a screen, and performing ball milling mixing by using an omnibearing planetary ball mill.
As a preferable scheme, the screen is trapezoid hole, the aperture is 0.08-0.25mm, and 0.08, 0.12, 0.20 or 0.25mm can be selected, and the sample injection size of ultracentrifuge crushing is less than 10mm. The diameter of the rotary cutter is 99mm, the speed of the ultracentrifuge crushing is 4000-16000rad/min, and the time is 2-12min. The omnibearing planetary ball mill is filled with inert gas for protection, the ball milling time is 1-3 hours, and the ball milling rotating speed is 100-500rad/min.
As a preferred embodiment, the extruder in step 2 is a micro twin screw extruder, and the extrusion temperature is 170-310 ℃.
The technical scheme of the invention is further described through specific examples.
Example 1
The technical scheme of the invention is not limited to the following specific embodiments.
Weighing anionic PAM 220g with number average molecular weight of 30 ten thousand, and semi-aromatic nylon 2kg with number average molecular weight of 37000, wherein the molecular formula of semi-aromatic nylon is H- [ NH (CH) 2 ) 5 CO-NH(CH 2 ) 6 NH-OCC 6 H 4 CO-] n OH, dried in vacuo at 100deg.C for 24h before use.
The LiClO is subjected to 4 And feeding PAM into an ultracentrifuge pulverizer, selecting an ultracentrifuge pulverizer with a diameter of 99mm and a 12-tooth rotary cutter, pulverizing and mixing for 3min, sieving with a 125 μm trapezoid-hole sieve, and repeating for 3 times. Under the protection of nitrogen atmosphere, sending the ultracentrifuge mixed sample into a planetary ball mill protected by nitrogen, ball milling for 3 hours, mixing with semi-aromatic nylon, and sending into a double-screw hot press for extrusion, wherein the extrusion temperature is 280 ℃. Weighing and putting an appropriate amount of extrusion materials into a polytetrafluoroethylene die, and hot-pressing for 10min at 280 ℃ and under the pressure of 12MPa to obtain uniform antistatic semi-aromatic nylon. Through testing, the conductivity of the embodiment can reach 10 -10 s cm -1 Has good antistatic performance.
Example 2
The technical scheme of the invention is not limited to the following specific embodiments.
40g of LiClO4 and 2kg of semiaromatic nylon with a number average molecular weight of 37000 are weighed, the molecular formula of the semiaromatic nylon is H- [ NH (CH 2) 5CO-NH (CH 2) 6NH-OCC6H4CO- ] nOH, and the semiaromatic nylon is dried in vacuum at 100 ℃ for 24 hours before use.
The LiClO4 and the anionic PAM with the number average molecular weight of 30 ten thousand are fed into an ultracentrifuge pulverizer, and the materials are crushed and mixed by ultracentrifuge pulverization with a diameter of 99mm and a 12-tooth rotary cutter for 3min, pass through a trapezoid hole screen with the aperture of 125 mu m, and repeat for 3 times. Under the protection of nitrogen atmosphere, sending the ultracentrifuge mixed sample into a planetary ball mill protected by nitrogen, ball milling for 3 hours, mixing with semi-aromatic nylon, and sending into a double-screw hot press for extrusion, wherein the extrusion temperature is 280 ℃. Weighing and putting an appropriate amount of extrusion materials into a polytetrafluoroethylene die, and hot-pressing for 10min at 280 ℃ and under the pressure of 12MPa to obtain uniform antistatic semi-aromatic nylon. Through testing, the conductivity of the embodiment can reach 10 -8 S cm -1 Has good antistatic performance.
Example 3
The technical scheme of the invention is not limited to the following specific embodiments.
40g LiClO was weighed out 4 220g of anionic PAM with a number average molecular weight of 30 ten thousand and 2kg of semiaromatic nylon with a number average molecular weight of 37000, the semiaromatic nylon being dividedThe sub-formula is H- [ NH (CH 2) 5CO-NH (CH 2) 6NH-OCC6H4CO ]]nOH, dried in vacuo at 100deg.C for 24h before use.
The LiClO is subjected to 4 And feeding PAM into an ultracentrifuge pulverizer, selecting an ultracentrifuge pulverizer with a diameter of 99mm and a 12-tooth rotary cutter, pulverizing and mixing for 3min, sieving with a 125 μm trapezoid-hole sieve, and repeating for 3 times. Under the protection of nitrogen atmosphere, sending the ultracentrifuge mixed sample into a planetary ball mill protected by nitrogen, ball milling for 3 hours, mixing with semi-aromatic nylon, and sending into a double-screw hot press for extrusion, wherein the extrusion temperature is 280 ℃. Weighing and putting an appropriate amount of extrusion materials into a polytetrafluoroethylene die, and hot-pressing for 10min at 280 ℃ and under the pressure of 12MPa to obtain uniform antistatic semi-aromatic nylon. Through testing, the conductivity of the embodiment can reach 10 -7 S cm -1 Has good antistatic performance.
The foregoing examples merely represent specific embodiments of the present application, which are described in more detail and are not to be construed as limiting the scope of the present application. It should be noted that, for those skilled in the art, several variations and modifications can be made without departing from the technical solution of the present application, which fall within the protection scope of the present application.
Claims (4)
1. The mixed antistatic semi-aromatic nylon resin is characterized by comprising the following components in percentage by mass:
2-10% of polyacrylamide containing ions;
1-3% of inorganic salt;
semi-aromatic nylon, 87-97%;
the weight average molecular weight of the ion-containing polyacrylamide is 2.0X10 5 -2.0×10 7 ；
The polyacrylamide containing ions is one or a combination of a plurality of anionic polyacrylamide, cationic polyacrylamide or amphoteric polyacrylamide;
the inorganic salt is LiClO 4 ；
The preparation method of the mixed antistatic semi-aromatic nylon resin comprises the following steps:
step 1, crushing and uniformly mixing the polyacrylamide containing ions and inorganic salt according to a proportion;
and 2, mixing the mixed raw material obtained in the step 1 with semi-aromatic nylon in proportion, extruding by using an extruder, and granulating to obtain the mixed antistatic semi-aromatic nylon resin.
2. The mixed antistatic semi-aromatic nylon resin according to claim 1, wherein the specific process of crushing and uniformly mixing in the step 1 is as follows: mixing the polyacrylamide containing ions and inorganic salt in proportion, performing ultracentrifugal crushing by using an ultracentrifugal crusher provided with a screen, and performing ball milling mixing by using an omnibearing planetary ball mill.
3. A hybrid antistatic semi-aromatic nylon resin according to claim 2, characterized in that: the screen is trapezoid hole, aperture is 0.08-0.25mm, speed of ultracentrifugal crushing is 4000-16000rad/min, the omnibearing planetary ball mill is filled with inert gas for protection, ball milling time is 1-3 hours, and ball milling rotating speed is 100-500rad/min.
4. A hybrid antistatic semi-aromatic nylon resin according to claim 2, characterized in that: and 2, adopting a miniature double-screw extruder as the extruder in the step 2, wherein the extrusion temperature is 170-310 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911400416.1A CN111138847B (en) | 2019-12-29 | 2019-12-29 | Mixed antistatic semi-aromatic nylon resin and preparation method thereof |
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| CN201911400416.1A CN111138847B (en) | 2019-12-29 | 2019-12-29 | Mixed antistatic semi-aromatic nylon resin and preparation method thereof |
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| CN111138847A CN111138847A (en) | 2020-05-12 |
| CN111138847B true CN111138847B (en) | 2023-05-19 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1752142A (en) * | 2005-08-19 | 2006-03-29 | 华南理工大学 | Preparation method of nylon 6/polyelectrolyte anti electrostatic composite material and anti electrostatic mother particle |
| CN106356194A (en) * | 2016-11-24 | 2017-01-25 | 东莞理工学院 | Polyacrylamide (PAM) solid compound polymer electrolyte and preparation method thereof |
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- 2019-12-29 CN CN201911400416.1A patent/CN111138847B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1752142A (en) * | 2005-08-19 | 2006-03-29 | 华南理工大学 | Preparation method of nylon 6/polyelectrolyte anti electrostatic composite material and anti electrostatic mother particle |
| CN106356194A (en) * | 2016-11-24 | 2017-01-25 | 东莞理工学院 | Polyacrylamide (PAM) solid compound polymer electrolyte and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王国建 等.抗静电剂.《功能高分子材料》.华东理工大学出版社,2006,(第一版), * |
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