CN113524623A - Method for improving impact performance of MCA flame-retardant PA66 - Google Patents
Method for improving impact performance of MCA flame-retardant PA66 Download PDFInfo
- Publication number
- CN113524623A CN113524623A CN202110609208.3A CN202110609208A CN113524623A CN 113524623 A CN113524623 A CN 113524623A CN 202110609208 A CN202110609208 A CN 202110609208A CN 113524623 A CN113524623 A CN 113524623A
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- Prior art keywords
- screw
- section
- head thread
- flame retardant
- double
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Links
- 239000003063 flame retardant Substances 0.000 title claims abstract description 46
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229920002302 Nylon 6,6 Polymers 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 238000001125 extrusion Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 230000007704 transition Effects 0.000 claims description 14
- 238000004898 kneading Methods 0.000 claims description 4
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 description 23
- 239000000463 material Substances 0.000 description 9
- 239000002131 composite material Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 238000001746 injection moulding Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 4
- 239000003963 antioxidant agent Substances 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- -1 carboxylic acid compound Chemical class 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000009818 secondary granulation Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/50—Details of extruders
- B29C48/505—Screws
- B29C48/64—Screws with two or more threads
- B29C48/655—Screws with two or more threads having three or more threads
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2077/00—Use of PA, i.e. polyamides, e.g. polyesteramides or derivatives thereof, as moulding material
Abstract
The invention discloses a method for improving impact performance of MCA flame retardant PA66, which comprises the following steps: 1) preparing raw materials according to a ratio; 2) putting the raw materials into a double-screw extruder for melt mixing, and extruding and granulating; wherein the length-diameter ratio of a screw of the double-screw extruder is 40-44:1, the temperature of a screw barrel is 260-450 ℃, and the rotating speed of the screw is 400-450 rpm; the double-screw extruder is characterized in that main threads are arranged in the whole screw process, and the double-screw extruder sequentially comprises a feeding section, a plasticizing section, a mixing section, an exhaust section and an extrusion section, wherein three-head thread elements are respectively arranged in the plasticizing section and the mixing section. The invention can improve the impact performance of MCA flame-retardant PA66 by more than 100%.
Description
Technical Field
The invention relates to a method for improving the impact performance of MCA flame-retardant PA66 (polyamide 66).
Background
The polyamide resin has excellent comprehensive properties such as good heat resistance, wear resistance, mechanical properties, barrier properties, chemical corrosion resistance and the like, and is widely applied to the fields of electric tools, electronic and electric appliances, connectors and the like. But the flame retardant rating of conventional PA66 can only reach V-2. To improve flame retardancy, MCA (melamine cyanurate) flame retardants are usually added.
The application of MCA flame retardant PA66 products requires solving two key problems: the first is the problem of flame retardant V0 grade, polyamide is used as a substrate, melamine cyanuric acid is used as a flame retardant, and MCA flame retardant polyamide composite material with flame retardant grade V0 can be obtained by adding more than 6 percent. However, the addition amount of MCA in the method is very high, and the toughness of the material is seriously influenced. The second is the problem of material toughness, and the material toughness is insufficient mainly because MCA flame retardant is not sufficiently dispersed, and the unnotched impact strength can only be generally 48-55J/m (ASTM D6110). In the prior art, PA66 powder and a powdery flame retardant are granulated to obtain flame retardant master batches, and then the flame retardant master batches and PA66 resin particles are subjected to secondary granulation, wherein the MCA flame retardant is subjected to two-time screw shearing dispersion, so that the dispersion is more uniform, and the toughness is improved.
In the prior art, a method for enhancing flame retardance is disclosed in, for example, CN201711422446.3, which discloses an MCA flame-retardant nylon 66 composite material and a preparation method thereof, wherein nylon 66 is used as a resin matrix, a market common MCA flame retardant is adopted, and at least one of a C8-C18 long carbon chain monobasic saturated carboxylic acid compound and a C8-C18 long carbon chain dibasic saturated carboxylic acid compound is used as a flame retardant stabilizer, so that the composite material reaches a stable V0 flame retardant grade.
In addition, CN201911147736.0 discloses a heat-resistant oxygen aging-resistant low-precipitation MCA flame-retardant PA66 composite material and application thereof. The composite material comprises 85-91 parts of PA66 resin, 8-12 parts of MCA flame retardant, 0.6-1.0 part of hollow glass bead, 0.3-0.6 part of antioxidant, 0.2-0.3 part of flame retardant stabilizer and 0.3-0.6 part of zinc borate. The invention takes PA66 as a resin matrix, adopts a common MCA flame retardant in the market, and combines hollow glass beads, anhydrous zinc borate and stearate as a flame retardant stabilizer, so that the composite material reaches the UL94V0 grade and is less in precipitation.
All the above are to improve the performance of MCA flame retardant PA66 by improving the components.
Disclosure of Invention
The invention mainly aims to provide a method for improving the impact performance of MCA flame-retardant PA 66. The invention is promoted by adopting a process mode.
A method for improving the impact performance of MCA flame-retardant PA66 comprises the following steps:
1) preparing raw materials according to a ratio;
2) putting the raw materials into a double-screw extruder for melt mixing, and extruding and granulating; wherein the length-diameter ratio of a screw of the double-screw extruder is 40-44:1, the temperature of a screw barrel is 260-450 ℃, and the rotating speed of the screw is 400-450 rpm;
the whole process of a screw of the double-screw extruder is provided with main threads, and the double-screw extruder sequentially comprises a feeding section, a plasticizing section, a mixing section, an exhaust section and an extrusion section, wherein three-head thread elements are respectively arranged in the plasticizing section and the mixing section; the large-diameter and small-diameter central lines of the three-head thread element are overlapped, and the large-diameter and small-diameter central lines are also overlapped with the rotating central line of the three-head thread element; when the screw element rotates in the cylinder, the clearance between 3 screw edges and the inner wall of the cylinder is always kept to be less than 0.2mm, wherein the total length of the three-start screw element of the plasticizing section is 20-60% of the length of the plasticizing section; the total length of the mixing section three-start thread element is 5-20% of the length of the mixing section.
In a preferred embodiment, a three-head thread element is arranged in the middle of the plasticizing section, and transition elements which are in transition with the two-head thread are respectively arranged in front of and behind the three-head thread; the middle of the mixing section is provided with a three-head thread element, and the front and the back of the three-head thread are respectively provided with a transition element which is in transition with the two-head thread.
In a preferred embodiment, the total length of the triple-start threaded element of the plasticizing section is 30-50% of the length of the plasticizing section.
In a preferred embodiment, the total length of the mixing section triple start screw element is 5-15% of the length of the mixing section.
In a preferred embodiment, the kneading disk angle of the triple flight is 40-50.
In the present invention, the transition member has three ends at one end connected to the three-start threaded member and two ends at the other end connected to the two-start threaded member
Compared with the background technology, the technical scheme has the following advantages:
1. in the double-screw extruder, 20-60% of the plasticizing section and 5-20% of the double-thread element in the mixing section are replaced by the triple-thread element, so that the material can meet the toughness requirement through one-time extrusion, and the manufacturing cost and the formula cost are directly reduced.
2. Higher average shear rate and shear force can be applied to the materials, so that the MCA flame retardant is dispersed more fully, the unnotched impact strength of the material can reach more than 100J/m (ASTM D6110), and the toughness is improved by at least one time.
Detailed Description
In the following examples and comparative examples, the equipment, model and manufacturer used were as follows:
| name of instrument | Model number | Manufacturer of the product |
| High-speed mixer | SHR200 | Suzhou Song Yuan |
| Co-rotating parallel double-screw extruder | RTX-65 | South Beijing ruiya |
| Pendulum impact testing machine | ZBC8400-C | Metas (R) device |
| Electronic universal tester | AGS-X-10KN | Shimadzu |
| Melt flow rate meter | MFI-2322S | Jin Jian |
| Injection molding machine | EM80-V | Haitian injection molding machine |
| Glow wire testing machine | AUTO-ZRSA | Odysseia wound |
| Water vertical combustion testing machine | AUTO-SPA | Odysseia wound |
The formula is as follows: 90 percent of PA66 resin particles, 0.5 percent of antioxidant, 0.5 percent of MCA powder flame retardant and 9 percent of MCA powder flame retardant.
The process flow of the material is as follows: mixing the surface materials, granulating by an extruder, injecting a sample strip, and testing physical properties.
Stirring 90% of PA66 resin particles, 0.5% of antioxidant and 0.5% of lubricant for 2min by a high-speed mixer to obtain a mixture, separately feeding the mixture and 9% of MCA powder flame retardant by a scale, respectively, putting the mixture into a double-screw extruder for melt mixing, and extruding and granulating to obtain the high-toughness MCA flame-retardant PA66 composite material; wherein the length-diameter ratio of the screw of the double-screw extruder is 40:1, the temperature of the screw cylinder is 260-270 ℃, and the rotating speed of the screw is 400-450 rpm.
The flame-retardant PA66 mechanical property sample is prepared by an injection molding machine, and the injection molding temperature is shown in the following table:
TABLE 1 flame retardant PA66 sample injection moulding process conditions
Performance testing
(1) The impact performance is tested according to the ISO179-1 standard;
(2) the bending strength is tested according to ISO178 standard;
(3) the tensile strength is tested according to ISO527-2 standard;
(4) the melt flow rate volume method is tested according to the ISO1133 standard;
(5) the flammability index is tested according to the IEC60695 standard;
(6) the vertical method for testing the combustion performance of the plastic is carried out according to the IEC60695 and UL94 standards.
Example 1
The screws of the twin-screw extruder are constituted by screw elements. The screw elements and their specifications are shown in Table 2
TABLE 2 specification of threaded elements
1) In "K45/5/72", 45 denotes the number of kneading disk turns, 5 denotes the number of kneading disks, 72 denotes the total length of the elements 72mm, and the like;
2) in "72/72", the former 72 means a pitch of 72mm, the latter 72 means a length of 72mm, and the like;
3) in the "" 44/22L ", L" refers to a left-handed threaded element, and the like;
4) in "K45/5/563 Fe", 3Fe means a triple-start threaded element; the tables "N-3 Fe" and "3 Fe-N" refer to transition elements with the double-start threaded element.
TABLE 3 screw combinations before and after adjustment and extrusion Process conditions
"X2" and "X3" indicate two or three of the elements, respectively.
As can be seen from Table 3, the impact strength of the material is obviously improved and the toughness is improved by more than 1 time by correspondingly replacing the original double-thread element with the triple-thread element.
2.2 comparison of physical Properties before and after adjustment of screw elements
TABLE 4 comparison of physical Properties before and after screw element adjustment
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims and their equivalents.
Claims (10)
1. A method for improving the impact performance of MCA flame-retardant PA66 comprises the following steps:
1) preparing raw materials according to a ratio;
2) putting the raw materials into a double-screw extruder for melt mixing, and extruding and granulating; wherein the length-diameter ratio of a screw of the double-screw extruder is 40-44:1, the temperature of a screw barrel is 260-450 ℃, and the rotating speed of the screw is 400-450 rpm;
the whole process of a screw of the double-screw extruder is provided with main threads, and the double-screw extruder sequentially comprises a feeding section, a plasticizing section, a mixing section, an exhaust section and an extrusion section, wherein three-head thread elements are respectively arranged in the plasticizing section and the mixing section; the total length of the three-head thread element of the plasticizing section is 20-60% of the length of the screw of the plasticizing section; the total length of the three-head thread element of the mixing section is 5-20% of the length of the screw of the mixing section; the large-diameter and small-diameter central lines of the three-head thread element are overlapped, and the large-diameter and small-diameter central lines are also overlapped with the rotating central line of the three-head thread element; when the screw element rotates in the cylinder, the clearance between 3 screw edges and the inner wall of the cylinder is always kept less than 0.2 mm.
2. The method of claim 1, wherein the impact strength of the MCA flame retardant PA66 is improved by: a three-head thread element is arranged in the middle of the plasticizing section, and transition elements which are in transition with the two-head thread are respectively arranged at the front and the rear of the three-head thread; the middle of the mixing section is provided with a three-head thread element, and the front and the back of the three-head thread are respectively provided with a transition element which is in transition with the two-head thread.
3. The method of claim 2, wherein the impact strength of the MCA flame retardant PA66 is improved by: the total length of the three-head thread element of the plasticizing section is 30-50% of the length of the screw of the plasticizing section.
4. The method of claim 3, wherein the impact strength of the MCA flame retardant PA66 is improved by: the total length of the three-head thread element of the mixing section is 5-15% of the length of the screw of the mixing section.
5. The method of claim 3 or 4, wherein the impact strength of the MCA flame retardant PA66 is improved by: the kneading disc angle of the three-start screw is 40-50.
6. The method of any one of claims 1 to 4, wherein the impact strength of the MCA flame retardant PA66 is improved by: one end of the transition element is three-head and is connected with the three-head thread element, and the other end of the transition element is two-head and is connected with the two-head thread element.
7. The method of claim 1, wherein the impact strength of the MCA flame retardant PA66 is improved by: the screw combinations in the plasticizing section were as follows:
K45/5/72N-3Fe；K45/5/56 3Fe；K45/5/56 3Fe；
K60/4/44 3Fe；K60/4/44 3Fe-N；44/22L，
wherein 3Fe refers to a triple threaded element and N-3Fe and 3Fe-N refer to transition elements with the double threaded element.
8. The method of claim 7, wherein the impact strength of the MCA flame retardant PA66 is improved by: the screw combination of the mixing section is as follows:
96/96X3；72/72；56/56X2；K45/5/56N-3Fe
K45/5/56 3Fe；K45/5/44 3Fe；K45/5/44 3Fe-N
44/22L；96/96X2；56/56X2
K45/5/44；44/44；K45/5/44；44/44
wherein 3Fe refers to a triple threaded element and N-3Fe and 3Fe-N refer to transition elements with the double threaded element.
9. The method of claim 1, wherein the impact strength of the MCA flame retardant PA66 is improved by: the screw combination of the feeding section is as follows: 56/56A; 96/96X 2; 96/48, respectively; 72/72, respectively; 56/56.
10. The method of claim 1, wherein the impact strength of the MCA flame retardant PA66 is improved by: the screw combination of the exhaust section is as follows: 44/22L; 96/96X 2; 72/72, respectively; the screw combination of the extrusion section is as follows: 64/64, respectively; 56/56, respectively; 44/44X 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110609208.3A CN113524623A (en) | 2021-06-01 | 2021-06-01 | Method for improving impact performance of MCA flame-retardant PA66 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110609208.3A CN113524623A (en) | 2021-06-01 | 2021-06-01 | Method for improving impact performance of MCA flame-retardant PA66 |
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| CN113524623A true CN113524623A (en) | 2021-10-22 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113969057A (en) * | 2021-10-27 | 2022-01-25 | 金旸（厦门）新材料科技有限公司 | Phosphonate flame-retardant system polyamide material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113969057A (en) * | 2021-10-27 | 2022-01-25 | 金旸（厦门）新材料科技有限公司 | Phosphonate flame-retardant system polyamide material and preparation method thereof |
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Application publication date: 20211022 |