CN112795146B - Preparation method of laser-weldable black flame-retardant PBT (polybutylene terephthalate) composite material - Google Patents
Preparation method of laser-weldable black flame-retardant PBT (polybutylene terephthalate) composite material Download PDFInfo
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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Abstract
The invention relates to a preparation method of a laser-weldable black flame-retardant PBT composite material, which comprises the steps of adding a raw material I into a main side feeding port of a double-screw extruder, adding a raw material II into a 4-section side feeding port of the double-screw extruder, extruding and granulating, controlling the rotating speed of a screw machine of the double-screw extruder to be 180-600 revolutions per minute, and controlling the extruding temperature of the double-screw extruder to be 235-275 ℃ to prepare the laser-weldable black flame-retardant PBT composite material; the length-diameter ratio of the double-screw extruder is 40; according to the mass parts, the raw material I is a mixture of 70-90 parts of PBT resin A, 8-10 parts of flame retardant and 0.3-1.5 parts of black powder, and the raw material II is a mixture of 10-20 parts of PBT resin B and 0.2-3 parts of N-butyl Piaguacid sylvite; the laser-weldable black flame-retardant PBT composite material prepared by the invention has excellent laser welding capability, good temperature resistance, halogen-free flame retardance, meets the ROHS and Reach regulation requirements, and can be used for producing black parts with flame retardance requirements.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and relates to a preparation method of a laser-weldable black flame-retardant PBT composite material.
Background
In the plastic laser welding, plastic parts to be welded are clamped together, a laser beam in a short wave infrared region is directed to a part to be bonded, the laser beam passes through an upper layer material and is absorbed by a lower layer material, and the laser energy is absorbed to increase the temperature of the lower layer material and melt the upper layer and the lower layer plastic, so that the welding is completed. The technique of bonding thermoplastic sheets, films or molded parts together by melting the plastic contact surface with the heat generated by a laser beam. Advantages of laser welding applied to the fusion of plastic parts include: the welding is precise and firm; the seal is airtight and watertight, resin degradation is less during welding, debris generated is less, and the surfaces of the products can be tightly connected together around the weld; plastic residues can not be generated by laser welding, so that the laser welding method is more suitable for the pharmaceutical product industry, electronic sensors and the like; the laser welding process is applied to workpieces with small size or complex appearance structure.
The polybutylene terephthalate is a semi-crystalline thermoplastic polyester and has excellent performances of high heat resistance, fatigue resistance, self-lubrication and the like. However, compared to other crystalline materials such as polyamides, the polyester material PBT has a lower laser transparency, which is the main reason that although PBT material exhibits otherwise excellent properties (low water absorption, economy), it is still less adopted as a material for laser welding component at present. In the prior art, the laser welding capability of the PBT is generally improved by two ways, one way is to add an amorphous resin, for example, in patents CN104910620, CN108473668, CN109401219 and CN109233216, respectively, the amorphous resin is added to a semi-crystalline resin, so that the crystallization capability of the crystalline resin is weakened, and the laser transmittance is improved, but it is known that the addition of the amorphous resin directly affects the heat resistance of the material, and the application range of the material is limited. In addition, there are also added inorganic or organic nucleating agents, for example, patent CN102464870, although the semi-permeable effect of PBT is achieved, which reduces the difficulty of laser welding, but it cannot meet the use of parts required to have flame retardant requirements and is not suitable for black products.
More importantly, in the prior art, the PBT material related to laser welding is concentrated in a pure resin system or a reinforcing system, mainly because the flame retardance of the high polymer material is realized more by adding halogen flame retardants and phosphorus-nitrogen flame retardants, the addition amount of the flame retardants is large, and the flame retardants hinder and even absorb the laser permeability, so that the laser welding is difficult to realize, for example, the laser absorber applied in the patent CN107057349 is a common halogen-free flame retardant; on the other hand, in selecting a flame retardant which has less influence on the transparency of the material, the oligomeric aromatic phosphate tends to be selected more, for example, in patent CN1729243A, and the oligomeric aromatic phosphate is not only a flame retardant but also a plasticizer, so that the temperature resistance of the material is reduced sharply.
Laser welding has certain limitations on the welding of black materials, and it is difficult to weld the black materials together, mainly when the upper layer is made of black parts, because the black materials absorb laser energy very obviously, so that the black materials cannot reach the interface of the welding materials. For example, in patent CN106317864, nigrosine is added to realize the permeability of a black nylon material, but nigrosine is not suitable for a polyester material, and mainly, amine groups in nigrosine react with terminal hydroxyl groups and terminal carboxyl groups in a PBT resin, which results in degradation of PBT. For example, in patent CN109233216, the laser welding of black materials is implemented by using an alloy manner and an ultramarine blue dye, but the ultramarine blue dye is an inorganic material, still has a certain absorption capacity for laser, and the alloy manner directly affects the heat resistance and mechanical properties of the material, and does not have a flame retardant property. Therefore, no relevant technical report is found about the flame-retardant PBT obtained by black laser welding.
Disclosure of Invention
The invention aims to solve the technical problem that black PBT is hardly welded by laser in the prior art, and provides a preparation method of a laser-weldable black flame-retardant PBT composite material.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a laser-weldable black flame-retardant PBT composite material comprises the steps of adding a raw material I into a main feeding port of a double-screw extruder, adding a raw material II into a side feeding port at 4 sections of the double-screw extruder, extruding and granulating, controlling the rotating speed of a screw machine of the double-screw extruder to be 180-600 r/min, and controlling the extruding temperature of the double-screw extruder to be 235-275 ℃ to prepare the laser-weldable black flame-retardant PBT composite material; the length-diameter ratio of the double-screw extruder is 40; according to the mass parts, the raw material I is a mixture of 70-90 parts of PBT resin A, 8-10 parts of flame retardant and 0.3-1.5 parts of black powder, and the raw material II is a mixture of 10-20 parts of PBT resin B and 0.2-3 parts of N-butyl Piaguacid sylvite;
the PBT resin A is a PBT resin with the intrinsic viscosity of 1.0-1.1 dl/g and the terminal carboxyl group content of 10-11 mol/t; the use of the PBT with the medium intrinsic viscosity avoids the problem that the PBT with the high intrinsic viscosity has high viscosity and is difficult to disperse, ensures that the bulk nucleating agent input from three sections is fully dispersed into a resin matrix, avoids overhigh local crystalline phase caused by uneven crystallization, and reduces the laser transmittance; the problems of low mechanical property and poor flame retardant property caused by low molecular weight of the low intrinsic viscosity PBT are avoided;
the PBT resin B is a PBT resin with the intrinsic viscosity of 0.82-0.85 dl/g and the carboxyl end group content of 18-22 mol/t; the application of high-end carboxyl group content and low intrinsic viscosity is mainly used for improving the reaction activity of the PBT resin and N-butyl-Piguate potassium salt and ensuring the size of the formed body crystal nucleus, so that the formed body crystal nucleus can be fully dispersed into the PBT resin, and the permeability is improved. Compared with an inorganic nucleating agent, the PBT resin is prevented from being rapidly crystallized due to larger molecular weight, so that the formed crystal is smaller and the light transmission is better;
the black toner is compounded by perylene red toner, indanthrene blue toner and isoindoline yellow toner in a mass ratio of 1 (0.6-0.8) to (0.9-1.2), does not affect the laser permeability, realizes the laser welding of black materials, simultaneously avoids the absorption of carbon black and ultramarine blue inorganic toner on laser, avoids the degradation of alkaline toners such as aniline black and the like on PBT resin, and ensures the material performance.
As a preferred technical scheme:
according to the preparation method, the raw material I is a mixture obtained by mixing the PBT resin A, the flame retardant and the black powder for 2-5 minutes by a high-speed mixer.
In the above-mentioned production method, the raw material II is a mixture of the PBT resin B and the N-butylpipecacid potassium salt mixed in a high-speed mixer for 2 to 5 minutes, and fed by an auxiliary twin-screw extruder through a 4-stage side feed port of the twin-screw extruder.
In the preparation method, the length-diameter ratio of the auxiliary twin-screw extruder is 45. The extrusion temperature of the auxiliary double-screw extruder is 230-240 ℃, and the screw rotating speed is 250 r/min. The high-length-diameter ratio double-screw extruder is used as an auxiliary feeding system, and the lower rotating speed is used as an auxiliary material, so that the retention time of the PBT resin in the double-screw extruder is prolonged, sufficient reaction activity and reaction amount are ensured, and the formation and crystal nucleus are more sufficient.
The combination of the two twin-screw extruders mainly aims to directly introduce a body crystal phase point into a main material system and avoid the phenomenon that secondary crystallization of PBT forms large crystals, thereby influencing light transmission. If a reactant of PBT and N-butyl-Piguate potassium salt is prepared in advance, the reactant can be recrystallized after water is discharged and cooled, and the reactant needs to be melted at high temperature when the twin-screw is applied again, so that the reactant can be dispersed unevenly again, the crystalline phase is enlarged, and the light transmittance is influenced.
According to the preparation method, the used flame retardant is bis (phenoxy) polyphosphazene, the compatibility with PBT resin is good, the flame retardant efficiency is high, the laser transmittance is not influenced like halogen-antimony and phosphorus-nitrogen flame retardants, and the material temperature resistance is not influenced like a phosphate flame retardant having a plasticizing effect.
According to the preparation method, when the laser-weldable black flame-retardant PBT composite material is subjected to injection molding to form a product with the thickness of 2.0mm, the near infrared transmittance of more than or equal to 57% is achieved at 980 nm.
According to the preparation method, the flame retardant grade of the laser-weldable black flame-retardant PBT composite material is 3.0mm V0 grade and 1.6mm V2 grade according to UL94 standard.
The invention uses the screw with high length-diameter ratio and low rotating speed, ensures that the PBT with high end carboxyl content and low intrinsic viscosity reacts with the N-butyl-Piaguacid sylvite to form enough nucleation points, and directly conveys the nucleation points to the double-screw extruder, thereby avoiding secondary crystallization and large crystal formation of the PBT to influence the laser permeability; the application of the bis (phenoxy) polyphosphazene flame retardant with transparency avoids the influence of the application of other types of flame retardants on the laser transmittance; the black powder is formed by compounding three primary colors, the laser permeability is not influenced, and the laser welding of the black material is realized.
Has the beneficial effects that:
compared with the prior art, the laser-weldable black flame-retardant PBT composite material prepared by the invention has excellent laser welding capability, good temperature resistance, no halogen and flame retardance, meets the ROHS and Reach regulation requirements, can be used for producing parts with flame-retardant black requirements, and has the following advantages:
(1) The PBT resin with high carboxyl content and the high length-diameter ratio extruder are selected for application, so that the reaction activity and the reaction quantity of the PBT resin and the N-butyl-Piagonic acid potassium salt are improved, the self nucleation of the PBT resin is realized, the introduction of other nucleating agents which additionally influence the permeability is avoided, the crystal nucleus is smaller, and the laser transmittance is higher.
(2) The two twin-screw extruders are combined, the PBT resin after reaction is directly added into the main feeder, and the phenomenon that the PBT forms large crystals due to secondary crystallization and melting processes after the resin after reaction is cooled so as to influence light transmission is avoided.
(3) The bis (phenoxy) polyphosphazene is used as a main flame retardant, has good compatibility with PBT resin and high flame retardant efficiency, and does not influence the laser transmittance. The halogen-antimony and phosphorus-nitrogen flame retardants do not influence the laser permeability, and the phosphate flame retardants have plasticizing effect and do not influence the temperature resistance of the material.
(4) The perylene red toner, the danline blue toner and the isoindoline yellow toner are combined together, so that the laser permeability is not influenced, and the laser welding of the black material is realized. Meanwhile, the strong absorption effect of carbon black and ultramarine inorganic toner on laser is avoided, the degradation effect of toner such as aniline black on PBT resin is also avoided, and the material performance is ensured.
Detailed Description
The present invention will be further described with reference to the following embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention can be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the claims appended to the present application.
In the embodiment of the invention:
the PBT resin A is PBT TH6100 produced by Xinjiang blue mountain Tunghe; the intrinsic viscosity is 1.0 to 1.3dl/g, and the content of terminal carboxyl is 10 to 11mol/t.
The PBT resin B is PBT KH2083 produced by Yingkou Kanghui petrochemical; the intrinsic viscosity is 0.82-0.85 dl/g, and the content of terminal carboxyl is 18-22 mol/t.
The N-butyl Piguate potassium salt is HK195 produced by Dongguan tri-hydrate chemical industry;
the fire retardant bis (phenoxy) polyphosphazene is SPB100 produced by Japan Otsuka chemistry;
the perylene red toner is L3875 (CAS.5521-31-3) produced by BASF;
the blue toner of the cathelicidin class is L6470 (CAS.81-77-6) produced by BASF;
the isoindoline yellow toner can be L2140HD (CAS. 36888-99-0) produced by BASF.
And (3) transmittance test: the prepared composite material is dried in a 110 ℃ oven for 6 hours, and is injection molded into a sample plate with the size of 80mm multiplied by 2mm by an injection molding machine, wherein the injection molding temperature is 250 ℃, and the mold temperature is 100 ℃. The transmittance at 980nm was measured by a NIRQuest 256.1 near infrared spectrometer from Ulmus optical instruments (Shanghai) Ltd.
And (3) testing the flame retardant property: the composite material obtained above was dried in an oven at 110 ℃ for 6 hours, and injection-molded into 130 mm. Times.13 mm. Times.1.6 mm and 130 mm. Times.13 mm. Times.3.0 mm, respectively, using an injection-molding machine, at 250 ℃ and 100 ℃ in a mold. The flame retardant performance was tested according to the U.S. UL94 standard.
Example 1
A preparation method of a laser-weldable black flame-retardant PBT composite material comprises the following specific steps:
(1) Preparing raw materials;
according to the mass parts, 70 parts of PBT TH6100 resin, 8 parts of flame retardant (di (phenoxy) polyphosphazene) (SPB 100) and 0.3 part of black powder are mixed for 2 minutes by a high-speed mixer, and the obtained mixture is taken as a raw material I;
wherein the black toner is compounded by perylene red toner, indanthrene blue toner and isoindoline yellow toner in a mass ratio of 1.6;
mixing 10 parts of PBT KH2083 resin and 0.2 part of N-butyl potassium biguate salt for 2 minutes by a high-speed mixer according to parts by weight to obtain a mixture serving as a raw material II;
(2) Adding a raw material I into a main side feeding port of the double-screw extruder, adding a raw material II into a 4-section side feeding port of the double-screw extruder, extruding and granulating to prepare the black flame-retardant PBT composite material capable of being subjected to laser welding;
the length-diameter ratio of a screw machine of the double-screw extruder is 40, the rotating speed is 180 r/min, and the temperature is 235 ℃;
the raw material II is conveyed to a 4-section side feeding port of the double-screw extruder by an auxiliary double-screw extruder and is added; the length-diameter ratio of the auxiliary double-screw extruder is 45, the extrusion temperature is 230 ℃, and the screw rotating speed is 250 r/min.
When the prepared black flame-retardant PBT composite material capable of being welded by laser is subjected to injection molding to form a product with the thickness of 2.0mm, the near-infrared transmittance of 65 percent is achieved at 980 nm; the flame retardant grade of the laser-weldable black flame-retardant PBT composite material is 3.0mm V0 grade and 1.6mm V2 grade according to the UL94 standard.
Example 2
A preparation method of a laser-weldable black flame-retardant PBT composite material comprises the following specific steps:
(1) Preparing raw materials;
mixing 72 parts of PBT TH6100 resin, 8 parts of flame retardant (di (phenoxy) polyphosphazene) (SPB 100) and 0.5 part of black powder for 2 minutes by a high-speed mixer, and taking the obtained mixture as a raw material I;
wherein the black toner is compounded by perylene red toner, silthiophane blue toner and isoindoline yellow toner in a mass ratio of 1;
mixing 12 parts of PBT KH2083 resin and 0.5 part of N-butyl potassium biguate in parts by mass for 2 minutes by using a high-speed mixer to obtain a mixture serving as a raw material II;
(2) Adding a raw material I into a main side feeding port of the double-screw extruder, adding a raw material II into a 4-section side feeding port of the double-screw extruder, extruding and granulating to prepare the black flame-retardant PBT composite material capable of being subjected to laser welding;
the length-diameter ratio of a screw machine of the double-screw extruder is 40, the rotating speed is 280 revolutions per minute, and the temperature is 240 ℃;
the raw material II is conveyed to a 4-section side feeding port of the double-screw extruder by an auxiliary double-screw extruder and is added; the length-diameter ratio of the auxiliary double-screw extruder is 45, the extrusion temperature is 233 ℃, and the screw rotating speed is 250 r/min.
When the prepared black flame-retardant PBT composite material capable of being welded by laser is subjected to injection molding to form a product with 2.0mm, the product has a near-infrared transmittance of 62% at 980 nm; the flame retardant grade of the laser-weldable black flame-retardant PBT composite material is 3.0mm V0 grade and 1.6mm V2 grade according to the UL94 standard.
Example 3
A preparation method of a laser-weldable black flame-retardant PBT composite material comprises the following specific steps:
(1) Preparing raw materials;
according to the mass parts, 75 parts of PBT TH6100 resin, 8 parts of flame retardant (di (phenoxy) polyphosphazene) (SPB 100) and 0.7 part of black powder are mixed for 3 minutes by a high-speed mixer, and the obtained mixture is used as a raw material I;
wherein the black toner is compounded by perylene red toner, indanthrene blue toner and isoindoline yellow toner in a mass ratio of 1.6;
mixing 14 parts of PBT KH2083 resin and 1 part of N-butyl Piguate potassium salt for 3 minutes by a high-speed mixer according to parts by weight to obtain a mixture serving as a raw material II;
(2) Adding a raw material I into a main side feeding port of the double-screw extruder, adding a raw material II into a 4-section side feeding port of the double-screw extruder, extruding and granulating to prepare the black flame-retardant PBT composite material capable of being subjected to laser welding;
the length-diameter ratio of a screw machine of the double-screw extruder is 40, the rotating speed is 350 r/min, and the temperature is 245 ℃;
the raw material II is conveyed to a 4-section side feeding port of the double-screw extruder by an auxiliary double-screw extruder and is added; the length-diameter ratio of the auxiliary double-screw extruder is 45, the extrusion temperature is 235 ℃, and the screw rotating speed is 250 r/min.
When the prepared black flame-retardant PBT composite material capable of being welded by laser is subjected to injection molding to form a product with 2.0mm, the product has a near-infrared transmittance of 57% at 980 nm; the flame retardant grade of the laser-weldable black flame-retardant PBT composite material is 3.0mm V0 grade and 1.6mm V2 grade according to the UL94 standard.
Example 4
A preparation method of a laser-weldable black flame-retardant PBT composite material comprises the following specific steps:
(1) Preparing raw materials;
mixing 80 parts of PBT TH6100 resin, 9 parts of flame retardant (di (phenoxy) polyphosphazene) (SPB 100) and 0.9 part of black powder by a high-speed mixer for 3 minutes, and taking the obtained mixture as a raw material I;
wherein the black toner is compounded by perylene red toner, silthiophane blue toner and isoindoline yellow toner in a mass ratio of 1.6;
mixing 16 parts of PBT KH2083 resin and 1.2 parts of N-butyl potassium biguate in parts by weight by a high-speed mixer for 3 minutes to obtain a mixture serving as a raw material II;
(2) Adding a raw material I into a main side feeding port of a double-screw extruder, adding a raw material II into a 4-section side feeding port of the double-screw extruder, extruding and granulating to prepare the black flame-retardant PBT composite material capable of being subjected to laser welding;
the length-diameter ratio of a screw machine of the double-screw extruder is 40, the rotating speed is 400 r/min, and the temperature is 250 ℃;
the raw material II is conveyed to a 4-section side feeding port of the double-screw extruder by an auxiliary double-screw extruder and is added; the length-diameter ratio of the auxiliary double-screw extruder is 45, the extrusion temperature is 236 ℃, and the screw rotating speed is 250 r/min.
When the prepared laser-weldable black flame-retardant PBT composite material is subjected to injection molding to form a product with 2.0mm, the product has 58% near-infrared transmittance at 980 nm; the flame retardant grade of the laser-weldable black flame-retardant PBT composite material is 3.0mm V0 grade and 1.6mm V2 grade according to the UL94 standard.
Example 5
A preparation method of a laser-weldable black flame-retardant PBT composite material comprises the following specific steps:
(1) Preparing raw materials;
according to the mass parts, 84 parts of PBT TH6100 resin, 9 parts of flame retardant (di (phenoxy) polyphosphazene) (SPB 100) and 1 part of black powder are mixed for 4 minutes by a high-speed mixer, and the obtained mixture is taken as a raw material I;
wherein the black toner is compounded by perylene red toner, silthiophane blue toner and isoindoline yellow toner in a mass ratio of 1;
mixing 18 parts of PBT KH2083 resin and 1.5 parts of N-butyl Piguate potassium salt for 4 minutes by a high-speed mixer according to parts by weight to obtain a mixture serving as a raw material II;
(2) Adding a raw material I into a main side feeding port of the double-screw extruder, adding a raw material II into a 4-section side feeding port of the double-screw extruder, extruding and granulating to prepare the black flame-retardant PBT composite material capable of being subjected to laser welding;
the length-diameter ratio of a screw machine of the double-screw extruder is 40, the rotating speed is 500 revolutions per minute, and the temperature is 255 ℃;
the raw material II is conveyed to a 4-section side feeding port of the double-screw extruder by an auxiliary double-screw extruder and is added; the length-diameter ratio of the auxiliary double-screw extruder is 45, the extrusion temperature is 237 ℃, and the screw rotating speed is 250 r/min.
When the prepared laser-weldable black flame-retardant PBT composite material is subjected to injection molding to form a product with 2.0mm, the product has 61% of near-infrared transmittance at 980 nm; the flame retardant grade of the laser-weldable black flame-retardant PBT composite material is 3.0mm V0 grade and 1.6mm V2 grade according to UL94 standard.
Example 6
A preparation method of a laser-weldable black flame-retardant PBT composite material comprises the following specific steps:
(1) Preparing raw materials;
mixing 88 parts of PBT TH6100 resin, 10 parts of flame retardant (di (phenoxy) polyphosphazene) (SPB 100) and 1.2 parts of black powder by a high-speed mixer for 4 minutes to obtain a mixture as a raw material I;
wherein the black toner is compounded by perylene red toner, indanthrene blue toner and isoindoline yellow toner in a mass ratio of 1.7;
mixing 19 parts of PBT KH2083 resin and 2 parts of N-butyl potassium biguate salt for 4 minutes by a high-speed mixer according to parts by weight to obtain a mixture serving as a raw material II;
(2) Adding a raw material I into a main side feeding port of a double-screw extruder, adding a raw material II into a 4-section side feeding port of the double-screw extruder, extruding and granulating to prepare the black flame-retardant PBT composite material capable of being subjected to laser welding;
the length-diameter ratio of a screw machine of the double-screw extruder is 40, the rotating speed is 550 revolutions per minute, and the temperature is 260 ℃;
the raw material II is conveyed to a 4-section side feeding port of the double-screw extruder by an auxiliary double-screw extruder and is added; the length-diameter ratio of the auxiliary double-screw extruder is 45, the extrusion temperature is 239 ℃, and the screw rotating speed is 250 r/min.
When the prepared laser-weldable black flame-retardant PBT composite material is subjected to injection molding to form a product with 2.0mm, the product has 60% near-infrared transmittance at 980 nm; the flame retardant grade of the laser-weldable black flame-retardant PBT composite material is 3.0mm V0 grade and 1.6mm V2 grade according to UL94 standard.
Example 7
A preparation method of a laser-weldable black flame-retardant PBT composite material comprises the following specific steps:
(1) Preparing raw materials;
mixing 90 parts of PBT TH6100 resin, 10 parts of flame retardant (bis (phenoxy) polyphosphazene) (SPB 100) and 1.5 parts of black powder for 5 minutes by a high-speed mixer, and taking the obtained mixture as a raw material I;
wherein the black toner is compounded by perylene red toner, silthiophane blue toner and isoindoline yellow toner in a mass ratio of 1.8;
mixing 20 parts of PBT KH2083 resin and 3 parts of N-butyl Piguate potassium salt for 5 minutes by a high-speed mixer according to the mass parts, and taking the obtained mixture as a raw material II;
(2) Adding a raw material I into a main side feeding port of a double-screw extruder, adding a raw material II into a 4-section side feeding port of the double-screw extruder, extruding and granulating to prepare the black flame-retardant PBT composite material capable of being subjected to laser welding;
the length-diameter ratio of a screw machine of the double-screw extruder is 40, the rotating speed is 600 revolutions per minute, and the temperature is 275 ℃;
the raw material II is conveyed to a 4-section side feeding port of the double-screw extruder by an auxiliary double-screw extruder and is added; the length-diameter ratio of the auxiliary double-screw extruder is 45, the extrusion temperature is 240 ℃, and the screw rotating speed is 250 r/min.
When the prepared laser-weldable black flame-retardant PBT composite material is subjected to injection molding to form a product with 2.0mm, the product has 59% of near-infrared transmittance at 980 nm; the flame retardant grade of the laser-weldable black flame-retardant PBT composite material is 3.0mm V0 grade and 1.6mm V2 grade according to UL94 standard.
Claims (6)
1. A preparation method of a laser-weldable black flame-retardant PBT composite material is characterized by comprising the following steps: adding a raw material I into a main side feeding port of a double-screw extruder, adding a raw material II into a 4-section side feeding port of the double-screw extruder, extruding and granulating, controlling the rotating speed of a screw machine of the double-screw extruder to be 180-600 revolutions per minute, and controlling the extruding temperature of the double-screw extruder to be 235-275 ℃, thus preparing the black flame-retardant PBT composite material capable of being subjected to laser welding;
the length-diameter ratio of the double-screw extruder is 40;
the raw material I is a mixture of 70-90 parts of PBT resin A, 8-10 parts of flame retardant and 0.3-1.5 parts of black powder, and the raw material II is a mixture of 10-20 parts of PBT resin B and 0.2-3 parts of N-butyl-potassium pipecolite;
the raw material II is conveyed to a 4-section side feeding port of the double-screw extruder by an auxiliary double-screw extruder and is added;
the length-diameter ratio of the auxiliary double-screw extruder is 45;
the extrusion temperature of the auxiliary double-screw extruder is 230-240 ℃, and the screw rotating speed is 250 revolutions per minute;
the PBT resin A is a PBT resin with the intrinsic viscosity of 1.0-1.1 dl/g and the terminal carboxyl group content of 10-11 mol/t;
the PBT resin B is a PBT resin with the intrinsic viscosity of 0.82-0.85 dl/g and the terminal carboxyl group content of 18-22 mol/t;
the black toner is compounded by perylene red toner, indanthrene blue toner and isoindoline yellow toner in a mass ratio of 1 (0.6-0.8) to (0.9-1.2).
2. The process according to claim 1, wherein the starting material I is a mixture of the PBT resin A, the flame retardant and the black powder for 2 to 5 minutes.
3. The process according to claim 1, wherein the starting material II is a mixture of PBT resin B and N-butylpyramidate potassium salt for 2 to 5 minutes.
4. The method of claim 1, wherein the flame retardant is bis (phenoxy) polyphosphazene.
5. The preparation method according to claim 1, wherein the laser-weldable black flame-retardant PBT composite material has a near-infrared transmittance of 57% or more at 980nm when injection-molded into a product having a thickness of 2.0 mm.
6. The method of claim 1, wherein the flame retardant grade of the laser weldable black flame retardant PBT composite is 3.0mm V0 grade and 1.6mm V2 grade according to UL94 standard.
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