CN111909501A - Permanent transparent flame-retardant PC (polycarbonate) and preparation method thereof - Google Patents
Permanent transparent flame-retardant PC (polycarbonate) and preparation method thereof Download PDFInfo
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- CN111909501A CN111909501A CN202010912556.3A CN202010912556A CN111909501A CN 111909501 A CN111909501 A CN 111909501A CN 202010912556 A CN202010912556 A CN 202010912556A CN 111909501 A CN111909501 A CN 111909501A
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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
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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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
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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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
- C08L2201/22—Halogen free composition
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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
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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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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Fireproofing Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to permanent transparent flame-retardant PC and a preparation method thereof. The raw materials and weight fraction include: 82.0-96.3 parts of polycarbonate, 2.0-10.0 parts of phosphorus-nitrogen flame retardant, 1.0-5.0 parts of toughening agent, 0.5-2.0 parts of antioxidant and 0.2-1.0 part of lubricant. The process comprises the following steps: uniformly mixing the pre-dried PC granules, the phosphorus-nitrogen flame retardant, the toughening agent and the antioxidant, putting the mixture into a torque rheometer for melt blending reaction, extruding and granulating by using a double-screw extruder, cooling and granulating to obtain the transparent flame-retardant PC. The flame retardant adopted by the invention is halogen-free and environment-friendly, and the PC and the flame retardant are subjected to ester exchange reaction to prepare the flame-retardant PC material, and the PC material has excellent and lasting flame retardant property, good comprehensive mechanical property and high light transmittance, and can meet the application in the field with high requirements on flame retardance and optical property.
Description
Technical Field
The invention relates to the field of modification of high polymer materials, and particularly relates to permanent transparent flame-retardant PC and a preparation method thereof.
Background
Polycarbonate (PC) is one of five engineering plastics, and is widely applied to the fields of buildings, electronic and electric appliances, aerospace, transportation and the like due to excellent comprehensive performance. PC has certain flame retardant property and certain char forming property during combustion, the Limiting Oxygen Index (LOI) of pure PC can reach 22-29%, and the grade of the PC can reach V-2 in a UL94 test. But when the PC is applied to televisions, computers, transformer coils, automobile parts, building materials and other fields with high requirement on high flame retardance, the PC still needs to be subjected to flame retardance modification.
Most of PC flame-retardant modification is carried out by adding sulfonate flame retardants, such as patents CN103602052B and CN106633762B, the sulfonate flame retardants have excellent flame-retardant PC performance, and can achieve good flame-retardant effect only by adding a small amount of the sulfonate flame retardants, but the sulfonate flame retardants are expensive, and the cost per ton is more than million, so the way of industrial popularization is far away. The phosphorus-containing flame retardant has good compatibility with PC and low price, and is widely used as the flame retardant of PC.
The patent (CN110551373A) discloses a high-performance halogen-free flame-retardant PC conductive material and a product thereof, wherein the high-performance halogen-free flame-retardant PC conductive material comprises PC resin, carbon black, hypophosphite flame retardant, phosphate flame retardant, organic silicon flame retardant and toughening agent, and is prepared by melt extrusion granulation. When the addition amount of the phosphorus-containing flame retardant is 15 parts, the vertical burning V-0 grade can be achieved, but the light transmittance of the PC composite material is influenced due to excessive carbon black content, so that the application range of PC is limited.
At present, PC flame retardant modification is basically an additive flame retardant, which migrates out of a polymer matrix along with the extension of the service time of the material after being added into the matrix, and cannot achieve the expected flame retardant effect.
Disclosure of Invention
Aiming at the problems, the invention provides a transparent flame-retardant PC and a preparation method thereof. Ester exchange reaction is carried out between ester in PC and ester or acid in the flame retardant, and the halogen-free flame retardant is connected to the molecular chain of the PC, so that the PC material is endowed with permanent flame retardant property.
In order to achieve the aim, the invention provides transparent flame-retardant PC and a preparation method thereof, wherein the transparent flame-retardant PC comprises the following components in parts by weight:
the invention provides a transparent flame-retardant PC and a preparation method thereof, which are carried out according to the following steps:
putting PC granules into a vacuum oven in advance for drying to fully remove moisture, uniformly mixing the dried PC, the phosphorus-nitrogen flame retardant, the toughening agent and the antioxidant by using a high-speed mixer, then putting the mixture into a torque rheometer for melt blending, adding the ester exchanger after blending for 2min for continuing melt blending, discharging the mixture rapidly after the reaction is finished, putting the mixture into ice water for cooling, putting the cooled raw materials into a vacuum oven at 120 ℃ for drying for 8h, extruding and granulating by using a double-screw extruder, bracing, cooling and dicing to obtain the transparent flame-retardant PC, and carrying out laser cutting on the PC to obtain a test sample strip.
Further, the PC is bisphenol A type PC resin;
further, the phosphorus-nitrogen flame retardant is at least one of melamine polyphosphate, ethylene diamine tetramethylene phosphonic acid, amino trimethylene phosphonic acid, diethylene triamine pentamethylene phosphonic acid, hexamethylene diamine tetramethylene phosphonic acid and the like;
further, the toughening agent is at least one of EMA, MBS and POE;
further, the antioxidant is at least one of antioxidant 168, antioxidant 1010, antioxidant 1076, antioxidant 5057, and antioxidant 3114;
further, the lubricant is pentaerythritol stearate;
further, the temperature of the vacuum oven is 100-120 ℃, and the processing time is 12-24 h;
further, the ester exchanger is tetrabutyl titanate;
further, the mixing temperature of the torque rheometer is 250-300 ℃, the rotating speed is 60-100 r/min, and the reaction time is 40-80 min;
further, the length-diameter ratio of the double-screw extruder is 36-44, the rotating speed of the screw extruder is 200-300 rpm, the temperature of the first zone is 100-110 ℃, the temperature of the second zone is 130-150 ℃, the temperature of the third zone is 160-180 ℃, the temperature of the fourth zone is 180-190 ℃, the temperature of the fifth zone is 190-200 ℃, the temperature of the sixth zone is 200-210 ℃, the temperature of the seventh zone is 200-210 ℃, the temperature of the head is 210-230 ℃, the residence time is 2min, and the pressure is 10-15 MPa.
The invention has the beneficial effects that:
1. the flame retardant adopted by the invention is halogen-free, environment-friendly and compounded with the concept of green development.
2. The flame-retardant PC material prepared by the method has lasting flame-retardant performance, does not migrate out along with the service time of the PC, and has good flame-retardant effect.
3. The invention can keep higher light transmittance while obtaining high-performance flame-retardant PC, the light transmittance of the flame-retardant PC is up to more than 88%, and the haze is lower than 5%, so that the application of PC products in the field of optical transparency is not influenced.
4. The transparent flame-retardant PC prepared by the invention has excellent flame-retardant property, excellent comprehensive mechanical property, simple and convenient preparation method and low cost, and is expected to be produced industrially in a large scale.
Detailed Description
The technical solutions implemented by the present invention will be clearly and completely described below by way of examples, and it is obvious that the described examples are only a part of the examples of the present invention, and not all of the examples. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Putting bisphenol A type PC granules into a 100 ℃ vacuum oven for 24 hours in advance to fully remove moisture, uniformly mixing dried PC, melamine polyphosphate, EMA, an antioxidant 168 and pentaerythritol stearate by using a high-speed mixer, putting the mixture into a torque rheometer with the temperature of 250 ℃ and the rotating speed of 80r/min for melt blending, adding tetrabutyl titanate for continuous melt blending after 2 minutes of blending, finishing reaction after 50 minutes, quickly discharging and putting the mixture into ice water for cooling, putting the cooled raw material into a 120 ℃ vacuum oven for drying for 8 hours, and carrying out extrusion granulation by using a double-screw extruder with the length-diameter ratio of 36, the rotating speed of 250rpm and the pressure of 10MPa, wherein the first-zone temperature of the double-screw extruder is 100 ℃, the second-zone temperature of the double-screw extruder is 130 ℃, the third-zone temperature of 160 ℃, the fourth-zone temperature of the double-zone temperature of 185 ℃, the fifth-zone temperature of the double-zone temperature of 200 ℃ and the seventh-zone, And (3) the temperature of a machine head is 210 ℃, the retention time is 2min, the transparent flame-retardant PC can be obtained after the stretching, cooling and grain cutting, and the test sample band can be obtained by performing laser cutting on the PC.
Example 2
Putting bisphenol A type PC granules into a vacuum oven at 110 ℃ in advance for 15 hours to fully remove moisture, uniformly mixing the dried PC, ethylenediamine tetramethylene phosphonic acid, MBS, antioxidant 1010 and pentaerythritol stearate by using a high-speed mixer, putting the mixture into a torque rheometer at the temperature of 280 ℃ and the rotating speed of 100r/min for melt blending, adding tetrabutyl titanate for continuous melt blending after 2min blending, and after 60min, finishing the reaction, quickly discharging the materials and putting the materials into ice water for cooling. Drying the cooled raw materials in a vacuum oven at 120 ℃ for 8h, extruding and granulating in a double-screw extruder with the length-diameter ratio of 40, the rotation speed of 280rpm and the pressure of 12MPa, wherein the first-zone temperature of the double-screw extruder is 105 ℃, the second-zone temperature of the double-screw extruder is 140 ℃, the third-zone temperature of the double-screw extruder is 165 ℃, the fourth-zone temperature of the double-screw extruder is 185 ℃, the fifth-zone temperature of the double-screw extruder is 195 ℃, the sixth-zone temperature of the double-screw extruder is 205 ℃, the seventh-zone temperature of the double-screw extruder is 205 ℃, the head temperature of the double-screw extruder is 220 ℃, and the residence time is 2min, and the transparent flame-.
Example 3
Putting bisphenol A type PC granules into a 120 ℃ vacuum oven for 12 hours in advance to fully remove moisture, uniformly mixing the dried PC, aminotrimethylene phosphonic acid, POE, an antioxidant 1076 and pentaerythritol stearate by using a high-speed mixer, putting the mixture into a torque rheometer with the temperature of 300 ℃ and the rotating speed of 60r/min for melt blending, adding tetrabutyl titanate for continuous melt blending after blending for 2 minutes, finishing the reaction after 80 minutes, quickly discharging, and putting the mixture into ice water for cooling. Drying the cooled raw materials in a vacuum oven at 120 ℃ for 8h, extruding and granulating in a double-screw extruder with the length-diameter ratio of 42, the rotating speed of 300rpm and the pressure of 13MPa, wherein the first-zone temperature of the double-screw extruder is 110 ℃, the second-zone temperature of the double-screw extruder is 140 ℃, the third-zone temperature of the double-screw extruder is 170 ℃, the fourth-zone temperature of the double-screw extruder is 190 ℃, the fifth-zone temperature of the double-screw extruder is 200 ℃, the sixth-zone temperature of the double-screw extruder is 210 ℃, the seventh-zone temperature of the double-screw extruder is 210 ℃, the head temperature of the double-screw extruder is 220 ℃, and the residence time is 2min, bracing, cooling and dicing.
Example 4
Putting bisphenol A type PC granules into a 115 ℃ vacuum oven for 18 hours in advance to fully remove moisture, uniformly mixing the dried PC, diethylenetriamine pentamethylene phosphonic acid, EMA and POE in a mass ratio of 1:2, an antioxidant 5057 and pentaerythritol stearate by using a high-speed mixer, putting the mixture into a torque rheometer at 290 ℃ and 85r/min for melt blending, adding tetrabutyl titanate for continuous melt blending after blending for 2min, after 70min, finishing the reaction, quickly discharging the materials, and putting the materials into ice water for cooling. Drying the cooled raw materials in a vacuum oven at 120 ℃ for 8 hours, extruding and granulating in a double-screw extruder with the length-diameter ratio of 44, the rotating speed of 300rpm and the pressure of 10-15 MPa, wherein the first-zone temperature of the double-screw extruder is 108 ℃, the second-zone temperature of the double-screw extruder is 135 ℃, the third-zone temperature of the double-screw extruder is 163 ℃, the fourth-zone temperature of the double-screw extruder is 186 ℃, the fifth-zone temperature of the double-screw extruder is 200 ℃, the sixth-zone temperature of the double-screw extruder is 205 ℃, the seventh-zone temperature of the double-screw extruder is 210 ℃, the head temperature of the double-screw extruder is 225 ℃ and the retention time of.
Example 5
Putting the bisphenol A type PC granules into a vacuum oven at 120 ℃ for 14 hours in advance to fully remove moisture, and adding the dried PC, hexamethylenediamine tetramethylidene phosphonic acid, EMA: MBS: POE (poly ethylene ether) 1:1:1 (wt%), antioxidant 3114 and pentaerythritol stearate are uniformly mixed by a high-speed mixer, then are placed in a torque rheometer with the temperature of 300 ℃ and the rotating speed of 100r/min for melt blending, tetrabutyl titanate is added for continuous melt blending after blending for 2min, and after 55min, after the reaction is finished, quickly discharging and cooling in ice water, placing the cooled raw materials in a vacuum oven at 120 ℃ for drying for 8h, extruding and granulating in a double-screw extruder with the length-diameter ratio of 44, the rotating speed of 260rpm and the pressure of 12MPa, wherein the first-zone temperature of the double-screw extruder is 108 ℃, the second-zone temperature of 140 ℃, the third-zone temperature of 165 ℃, the fourth-zone temperature of 188 ℃, the fifth-zone temperature of 196 ℃, the sixth-zone temperature of 206 ℃, the seventh-zone temperature of 210 ℃, the head temperature of 230 ℃ and the residence time of 2min, drawing strips, cooling and granulating, and obtaining the transparent flame-retardant PC, and preparing a test sample strip by laser cutting the PC.
Soxhlet extraction test: the transparent flame-retardant PC prepared in the examples 1 to 5 is respectively put into a good solvent of a flame retardant for reflux Soxhlet extraction, and after extraction for 5 days, the transparent flame-retardant PC is taken out, cleaned by deionized water, and subjected to UL-94 vertical combustion test after vacuum drying to evaluate the flame-retardant performance.
DSC test: a transparent flame-retardant PC prepared in examples 1 to 5 was pulverized and placed in an aluminum crucible of a DSC, and a nitrogen atmosphere was opened, temperature-controlled according to the following procedure, and 2 cycles of scanning were performed: (1) constant temperature lmin at 30 ℃; (2) keeping the temperature at 30-300 ℃, 5 ℃/min (3) and 300 ℃ for 3 min; (4) 300-30 ℃ and 5 ℃/min.
TABLE 1 flame retardant, optical, mechanical Properties test results for transparent flame retardant PC's in examples 1-5
As can be seen from Table 1, the permanent transparent flame-retardant PC prepared by the invention has excellent comprehensive performance, when the addition amount of the reactive phosphorus-nitrogen flame retardant is 2 parts, the PC composite material can reach UL-94(1.6mm) V-0 grade, and the PC composite material keeps excellent optical transparency and comprehensive mechanical properties, and can meet the application in the fields of electronic appliances and the like with higher requirements on flame retardance and optical properties.
TABLE 2 DSC test results of transparent flame retardant PC in examples 1-5
| Tm1 | Tm2 | Tm | Tc1 | Tc2 | Tc | |
| Example 1 | 225.8 | 193.4 | 32.4 | 188.6 | 159.7 | 28.9 |
| Example 2 | 223.7 | 189.5 | 34.2 | 187.5 | 159.9 | 27.6 |
| Example 3 | 223.4 | 190.6 | 32.8 | 186.8 | 158.2 | 28.6 |
| Example 4 | 224.8 | 191.4 | 33.4 | 188.2 | 158.5 | 29.7 |
| Example 5 | 221.4 | 189.3 | 32.1 | 187.2 | 158.1 | 29.1 |
Tm1And Tm2Respectively represents the melting temperature in the first and second heating processes, Tc1And Tc2Respectively representing the crystallization temperature during the first and second temperature reduction. Commonly available Tm＝Tm1-Tm2，Tc＝Tc1-Tc2To indicate the degree of transesterification, TmAnd TcThe larger the value of (A) is, the larger the degree of reaction is. Examples 1 to 5TmHas a value of 30 or more, TcThe numerical value of (A) is more than 25, which proves that the degree of ester exchange between the PC and the flame retardant is larger, and the flame retardant is successfully grafted to the PC molecular chain.
Claims (10)
1. A transparent flame retardant PC characterized in that: the composition comprises the following components in parts by weight: 82.0-96.3 parts of PC, 2.0-10.0 parts of phosphorus-nitrogen flame retardant, 1.0-5.0 parts of toughening agent, 0.5-2.0 parts of antioxidant and 0.2-1.0 part of lubricant.
2. A transparent flame retardant PC characterized in that: the preparation method comprises the following steps:
putting PC granules into a vacuum oven in advance for drying to fully remove moisture, uniformly mixing the dried PC, the phosphorus-nitrogen flame retardant, the toughening agent and the antioxidant by using a high-speed mixer, then putting the mixture into a torque rheometer for melt blending, adding the ester exchanger after blending for 2min for continuing melt blending, discharging the mixture rapidly after the reaction is finished, putting the mixture into ice water for cooling, putting the cooled raw materials into a vacuum oven at 120 ℃ for drying for 8h, extruding and granulating by using a double-screw extruder, bracing, cooling and dicing to obtain the transparent flame-retardant PC, and carrying out laser cutting on the PC to obtain a test sample strip.
3. The transparent flame retardant PC of claim 1, wherein: the PC is bisphenol A type PC resin.
4. The transparent flame retardant PC of claim 1, wherein: the phosphorus-nitrogen flame retardant is at least one of melamine polyphosphate, ethylene diamine tetramethylene phosphonic acid, amino trimethylene phosphonic acid, diethylene triamine pentamethylene phosphonic acid, hexamethylene diamine tetramethylmethylene phosphonic acid and the like.
5. The transparent flame retardant PC of claim 1, wherein: the toughening agent is at least one of EMA, MBS and POE.
6. The transparent flame retardant PC of claim 1, wherein: the antioxidant is at least one of antioxidant 168, antioxidant 1010, antioxidant 1076, antioxidant 5057, and antioxidant 3114.
7. The transparent flame retardant PC of claim 1, wherein: the lubricant is pentaerythritol stearate.
8. The transparent flame retardant PC of claim 2, wherein: the temperature of the vacuum oven is 100-120 ℃, and the processing time is 12-24 h; the ester exchanger is tetrabutyl titanate.
9. The transparent flame retardant PC of claim 2, wherein: the mixing temperature of the torque rheometer is 250-300 ℃, the rotating speed is 60-100 r/min, and the reaction time is 40-80 min.
10. The transparent flame retardant PC of claim 2, wherein: the length-diameter ratio of the double-screw extruder is 36-44, the rotating speed of the screw extruder is 200-300 rpm, the temperature of a first zone is 100-110 ℃, the temperature of a second zone is 130-150 ℃, the temperature of a third zone is 160-180 ℃, the temperature of a fourth zone is 180-190 ℃, the temperature of a fifth zone is 190-200 ℃, the temperature of a sixth zone is 200-210 ℃, the temperature of a seventh zone is 200-210 ℃, the temperature of a head is 210-230 ℃, the retention time is 2min, and the pressure is 10-15 MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202010912556.3A CN111909501A (en) | 2020-09-03 | 2020-09-03 | Permanent transparent flame-retardant PC (polycarbonate) and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010912556.3A CN111909501A (en) | 2020-09-03 | 2020-09-03 | Permanent transparent flame-retardant PC (polycarbonate) and preparation method thereof |
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Application publication date: 20201110 |