CN113462117A - Preparation method of high-heat-resistance flame-retardant material - Google Patents
Preparation method of high-heat-resistance flame-retardant material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
- C08L55/02—ABS [Acrylonitrile-Butadiene-Styrene] 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
- B29B13/06—Conditioning or physical treatment of the material to be shaped by drying
- B29B13/065—Conditioning or physical treatment of the material to be shaped by drying of powder or pellets
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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
- B29B7/00—Mixing; Kneading
- B29B7/002—Methods
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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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- 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
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/17—Component parts, details or accessories; Auxiliary operations
- B29C45/76—Measuring, controlling or regulating
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- 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
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C2045/0096—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor drying the moulding material before injection, e.g. by heating
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- 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
- B29C2945/00—Indexing scheme relating to injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould
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Abstract
The invention discloses a preparation method of a high heat-resistant flame-retardant material, which comprises the following steps of S1: preparation of the premix: adding acrylonitrile-butadiene-styrene (ABS), a heat-resistant agent, high rubber powder, a compatibilizer, a flame-retardant system and other various processing aids into a high-speed mixer according to a proportion formula, mixing for 2min at the rotating speed of 400r/min, and mixing for 1min at the rotating speed of 1000r/min to obtain a premix. The high heat-resistant flame-retardant acrylonitrile-butadiene-styrene (ABS) material prepared by the two-step method has high heat resistance and flame retardance, the heat resistance of the acrylonitrile-butadiene-styrene (ABS) material is positively correlated with the heat resistance of the ABS material, the heat deformation temperature of the high heat-resistant flame-retardant acrylonitrile-butadiene-styrene (ABS) material is not obviously reduced by adding DBDPE, the bending strength, the tensile strength and the impact strength are slightly reduced, and the fluidity is obviously improved.
Description
Technical Field
The invention relates to the technical field of flame retardant material preparation, in particular to a preparation method of a high heat-resistant flame retardant material.
Background
Acrylonitrile-butadiene-styrene (ABS) plastic has the characteristics of both the rigidity and heat resistance of acrylonitrile, the gloss and processability of polystyrene, and the impact resistance of polybutadiene, and can be widely used in the fields of household appliances, office equipment, instruments, transportation, building materials, daily necessities, packaging materials, and the like. But Acrylonitrile Butadiene Styrene (ABS) has a Limiting Oxygen Index (LOI) of only 18%, and is a flammable material. In order to improve the combustion behavior, make it flame-retardant or self-extinguish when it is exposed to fire, acrylonitrile-butadiene-styrene (ABS) must be flame-retardant modified.
The flame-retardant material is a material which can inhibit or delay combustion and is not inflammable, and is widely applied to the fields of clothing, petroleum, chemical engineering, metallurgy, shipbuilding, fire fighting, national defense and the like.
The existing acrylonitrile-butadiene-styrene (ABS) plastic cannot have high heat resistance and flame retardant property, and cannot well meet the performance requirements when being applied to the fields of motors, hair dryers, power supply boxes, microwave ovens, electric cookers, power strips and the like.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation method of a high heat-resistant flame-retardant material.
The invention provides a preparation method of a high heat-resistant flame-retardant material, which is characterized by comprising the following steps:
s1: preparation of the premix: adding acrylonitrile-butadiene-styrene (ABS), a heat-resistant agent, high rubber powder, a compatibilizer and other various processing aids into a high-speed mixer according to a proportion formula, and mixing to obtain a premix;
s2: and (3) extruding and granulating: putting the premix into a double-screw extruder for extrusion granulation, and controlling the temperature of the double-screw extruder by 10 sections to prepare heat-resistant high-heat-resistant acrylonitrile-butadiene-styrene (ABS) master batch;
s3: secondary premixing: adding the high-heat-resistant acrylonitrile-butadiene-styrene (ABS) master batch in the S1, a DBDPE flame-retardant system, a compatibilizer and other various processing aids into a high-speed mixer according to the proportion of a formula for premixing, and putting the secondary premix into a double-screw extruder for extrusion granulation;
s4: injection molding: extruding and granulating, drying the heat-resistant agent high-heat-resistant acrylonitrile-butadiene-styrene (ABS) master batch prepared after secondary premixing at the temperature of 80 ℃ for 4h, and performing injection molding at the injection temperature of 180 ℃ and 210 ℃ by a precision injection molding machine;
s5: and (3) flame retardance detection: putting the existing flame-retardant materials of the same kind with different oxygen indexes in the market into a combustion cylinder of an oxygen index tester to measure the oxygen indexes at different temperatures and humidities, respectively obtaining oxygen index tables of the prepared and molded high heat-resistant flame-retardant materials with different oxygen indexes at different temperatures and humidities, and determining the oxygen index range in each oxygen index table; the high heat-resistant flame-retardant material is prepared by different proportions of 26, 32, 34, 38 and 43 in oxygen index, so that better performance of the flame-retardant material is obtained, and the high heat-resistant flame-retardant material is the optimal material proportion.
As a further scheme of the invention, in the S1, AS-MS-NB is adopted AS the heat-resistant agent, DBDPE is adopted AS the high rubber powder, HR181 is adopted AS the compatibilizer, and the proportion of acrylonitrile-butadiene-styrene (ABS), the heat-resistant agent, the high rubber powder and the compatibilizer is 60: 20: 12.5: 7.5.
as a further scheme of the invention, in the S1, the high-speed mixer is used for mixing for 2min at the working rotating speed of 400r/min and then is used for mixing for 1min at the rotating speed of 1000 r/min.
As a further proposal of the invention, the working conditions of the twin-screw extruder in S2 are as follows, the temperature is controlled at 270 ℃, the main machine rotating speed is 1020r/min, and the feeding rotating speed is 400 r/min.
As a further proposal of the invention, the barrel temperature of the twin-screw extruder in S3 is controlled in 10 sections, the temperature is controlled at 210 ℃ at 180 ℃, the main machine rotating speed is 1020r/min, and the feeding rotating speed is 400 r/min.
As a further aspect of the present invention, the flame retardancy test of S5 comprises the following specific procedures:
1) wherein the oxygen index tester is protected by the mixed gas of nitrogen and oxygen, and the temperature and humidity conditions are changed for testing;
2) carrying out difference operation on the oxygen indexes at different humidity and temperatures in the oxygen index table and the oxygen index values measured at the temperature of 25 ℃ and the humidity of 50% to obtain a difference table;
3) measuring the oxygen index of the flame-retardant material on site by using an oxygen index measuring instrument to obtain the oxygen index at the temperature and humidity, checking the oxygen index range corresponding to each oxygen index table in the step 1), and finding the oxygen index table containing the oxygen index measured on site or the oxygen index table with the closest value;
4) and obtaining the difference value under the temperature and the humidity by using a binary interpolation method according to an oxygen index table containing the oxygen index measured on site or a difference value table corresponding to the oxygen index table with the closest value, and performing addition and subtraction operation on the oxygen index measured on site and the difference value to obtain the actual oxygen index of the flame retardant material.
As a further scheme of the invention, the flow rate of the mixed gas is 10.1-11.2L/min.
As a further scheme of the invention, the detection size of the flame retardant material is that the length, width and height of the flame retardant material are both more than 10mm and less than 15mm, and the detection size can be controlled by the existing granulating equipment.
The beneficial effects of the invention are as follows:
the preparation method takes acrylonitrile-butadiene-styrene plastic (acrylonitrile-butadiene-styrene (ABS)) AS a substrate, takes styrene-N-phenylmaleimide-maleic anhydride terpolymer (AS-MS-NB) AS a heat-resistant agent, prepares high heat-resistant acrylonitrile-butadiene-styrene (ABS) master batch at 240-270 ℃ in a double screw extruder, mixes the master batch with a decabromodiphenylethane (DBDPE) flame-retardant system, prepares high heat-resistant flame-retardant acrylonitrile-butadiene-styrene (ABS) at 180-210 ℃ through the double screw extruder, prepares the high heat-resistant flame-retardant acrylonitrile-butadiene-styrene (ABS) material by the two-step method, has high heat resistance and flame-retardant property, has the content of the heat-resistant agent and the flame retardance prepared by the heat-resistant agent, and has positive correlation with the heat resistance of the acrylonitrile-butadiene-styrene (ABS) material, the heat distortion temperature of the high heat-resistant flame-retardant acrylonitrile-butadiene-styrene (ABS) is not obviously reduced by adding the DBDPE, the bending strength, the tensile strength and the impact strength are slightly reduced, the fluidity is obviously improved, and the high heat-resistant flame-retardant acrylonitrile-butadiene-styrene (ABS) can be widely applied to the fields of motors, hair dryers, power supply boxes, microwave ovens, electric rice cookers, plug boards and the like.
Drawings
FIG. 1 is a process flow chart of a method for preparing a high heat-resistant flame-retardant material according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1
Referring to fig. 1, a preparation method of a high heat-resistant flame-retardant material adopts a two-step preparation process, the high heat-resistant acrylonitrile-butadiene-styrene (ABS) master batch in example 1, a DBDPE flame-retardant system, a compatibilizer and other various processing aids are added into a high-speed mixer according to a formula ratio for premixing (process conditions are the same as above), the premix is put into a double-screw extruder for extrusion granulation, the temperature of the double-screw extruder barrel is controlled in 10 sections, the temperature is controlled at 180 ℃ and 210 ℃, the main machine rotation speed is 1020r/min, and the feeding rotation speed is 400 r/min. Extruding and granulating, drying the prepared high-heat-resistant flame-retardant acrylonitrile-butadiene-styrene (ABS) plastic particles for 4 hours at the temperature of 80 ℃, and performing injection molding by a precision injection molding machine (the injection molding temperature is 180-;
the preparation method comprises the steps of adding acrylonitrile-butadiene-styrene (ABS), a heat-resistant agent, high rubber powder, a DBDPE flame-retardant system, a compatibilizer and other various processing aids into a high-speed mixer according to a certain proportion, mixing for 2min at the rotating speed of 400r/min, mixing for 1min at the rotating speed of 1000r/min to obtain a premix, putting the premix into a double-screw extruder for extrusion granulation, controlling the temperature of the double-screw extruder barrel at 10 sections, controlling the temperature at 240 ℃ and 270 ℃, controlling the rotating speed of a main machine at 1020r/min and the rotating speed of material intolerance at 400r/min, and extruding and granulating the prepared high heat-resistant flame-retardant acrylonitrile-butadiene-styrene (ABS) plastic particles.
Wherein the injection temperature of the injection molding machine is 180-210 ℃. The drying temperature of the plastic particles is 80 ℃, and the drying time is 4 hours. The mixture is mixed at a rotation speed of 400r/min for 2min and then at a rotation speed of 1000r/min for 1 min. The temperature of each section of the double-screw extruder barrel is 180-210 ℃. The method not only solves the problem of dispersion of the heat-resistant agent in the matrix resin, but also solves the problem of sensitivity of the flame retardant to the processing temperature. Firstly, a heat-resistant agent is well dispersed in an ABS system under a higher temperature condition through a screw rod with strong shearing, and then the screw rod with weak shearing is selected to prepare the flame-retardant heat-resistant ABS at a lower temperature. All components of the system are uniformly dispersed, so that all properties of the prepared high-heat-resistance flame-retardant ABS are greatly improved, especially the heat resistance and the flame retardance. Along with the increase of the content of the heat-resistant agent, the heat resistance of the prepared heat-resistant ABS master batch is continuously increased. When the mass fraction of the heat-resistant agent is 5%, the heat distortion temperature of the high heat-resistant ABS master batch is only 86 ℃, and the corresponding Vicat softening temperature is only 97 ℃, but when the mass fraction of the heat-resistant agent is 30%, the heat distortion temperature of the high heat-resistant ABS master batch is as high as 117 ℃, the corresponding Vicat softening temperature is 131 ℃, and the ball indentation temperature and the Vicat softening temperature are basically similar.
DBDPE has an extremely high melting point and is basically insoluble in the resin, so that the DBDPE can be added into the resin to enable the resin to have a higher heat distortion temperature and be difficult to bloom, and particularly, the DBDPE can be added into ABS to obviously improve the heat resistance of the ABS, so that DBDPE is selected as a flame retardant of high-heat-resistance ABS. The high heat-resistant ABS master batches with different heat-resistant agent contents are prepared at a screw rod with higher processing temperature and stronger shearing by compounding a heat-resistant agent and ABS matrix resin, the prepared master batches with different heat-resistant agent contents are blended with a DBDPE/Sb2O3 flame-retardant system, a high heat-resistant flame-retardant ABS material with specified heat-resistant temperature is prepared at a screw rod with lower processing temperature and weaker shearing, and the high heat-resistant flame-retardant ABS material can be applied to the fields of motors, hair dryers, power boxes, microwave ovens, electric cookers, plug boards and the like which need heat resistance and flame retardance instead of flame-retardant PC or flame-retardant PC/ABS.
Example 2
A preparation method of a high heat-resistant flame-retardant material adopts a two-step preparation process, the high heat-resistant acrylonitrile-butadiene-styrene (ABS) master batch in the embodiment 1, an LDPE/red phosphorus alloy system, a compatibilizer and other various processing aids are added into a high-speed mixer according to the formula proportion for premixing (the process conditions are the same as above), the premix is put into a double-screw extruder for extrusion granulation, the temperature of the double-screw extruder is controlled in 10 sections, the temperature is controlled at 180-210 ℃, the rotating speed of a main machine is 1020r/min, and the feeding rotating speed is 400 r/min. Extruding and granulating, drying the prepared high-heat-resistant flame-retardant acrylonitrile-butadiene-styrene (ABS) plastic particles for 4 hours at the temperature of 80 ℃, and performing injection molding by a precision injection molding machine (the injection molding temperature is 180-;
the flame retardant system is an LDPE/red phosphorus alloy system, wherein the red phosphorus alloy adopts the following components of HT2951, LDPE: HT2951 is 10:3, the flame retardant mechanism of the red phosphorus alloy is that red phosphorus is mainly oxidized under the actual flame condition to generate phosphorus oxide phosphoric acid and phosphoric acid derivatives, the generated phosphorus oxide promotes the dehydration and carbonization of resin, so that the flammable cracking products are reduced, meanwhile, a layer of glassy melt is formed on the surface of the resin due to the generation of phosphoric acid-phosphorous acid polymetaphosphoric acid, the heat transfer of flame to the surface of the polymer and the outward diffusion of the decomposition products from the surface of the polymer are prevented to form an oxygen-blocking barrier layer, so that the spread of the flame is inhibited, and on the other hand, the process has the heat absorption effect, reduces the thermal oxidation of the polymer and achieves the purpose of flame retardant.
Example 3
A preparation method of a high heat-resistant flame-retardant material adopts a two-step preparation process, the high heat-resistant acrylonitrile-butadiene-styrene (ABS) master batch in the embodiment 1, an LDPE/APP flame-retardant system, a compatibilizer and other various processing aids are added into a high-speed mixer according to the formula proportion for premixing (the process conditions are the same as above), the premix is put into a double-screw extruder for extrusion granulation, the temperature of the double-screw extruder is controlled by 10 sections, the temperature is controlled at 180-210 ℃, the main machine rotating speed is 1020r/min, and the feeding rotating speed is 400 r/min. Extruding and granulating, drying the prepared high-heat-resistant flame-retardant acrylonitrile-butadiene-styrene (ABS) plastic particles for 4 hours at the temperature of 80 ℃, and performing injection molding by a precision injection molding machine (the injection molding temperature is 180-;
the flame retardant system is an LDPE/APP flame retardant system, wherein the flame retardant effect of APP is that polyphosphoric acid and NH are generated when the APP is subjected to thermal decomposition, the polyphosphoric acid can be used as a dehydrating agent to dehydrate and carbonize a polymer to form a carbonized layer, the released NH can be used as a foaming agent to expand the carbonized layer, and the added hydroxyl-containing pentaerythritol is more beneficial to the formation of the carbonized layer. A
Example 4
A preparation method of a high heat-resistant flame-retardant material adopts a two-step preparation process, the high heat-resistant acrylonitrile-butadiene-styrene (ABS) master batch in the embodiment 1, an LDPE/ATH flame-retardant system, a compatibilizer and other various processing aids are added into a high-speed mixer according to the formula proportion for premixing (the process conditions are the same as above), the premix is put into a double-screw extruder for extrusion granulation, the temperature of the double-screw extruder is controlled in 10 sections, the temperature is controlled at 180-210 ℃, the rotating speed of a main machine is 1020r/min, and the feeding rotating speed is 400 r/min. Extruding and granulating, drying the prepared high-heat-resistant flame-retardant acrylonitrile-butadiene-styrene (ABS) plastic particles for 4 hours at the temperature of 80 ℃, and performing injection molding by a precision injection molding machine (the injection molding temperature is 180-;
the flame retardant system is LDPE/ATH flame retardant structure, and the flame retardant mechanism is that the ATH releases crystal water after being heated, and the heat absorption capacity is about 2.09kJ/g, so that the ATH filled in the PE absorbs part of heat released in the combustion process when being decomposed, the temperature of high polymer is reduced, the degradation speed is reduced, and in addition, the water vapor released by the decomposition of the ATH dilutes the concentration of combustible gas in a flame zone and has a certain cooling effect. The ATH also helps to form a charring layer during combustion, which can not only prevent the entry of heat and oxygen, but also prevent the escape of small molecule combustible gas.
S5: and (3) flame retardance detection: putting the existing flame-retardant materials of the same kind with different oxygen indexes in the market into a combustion cylinder of an oxygen index tester to measure the oxygen indexes at different temperatures and humidities, respectively obtaining oxygen index tables of the prepared and molded high heat-resistant flame-retardant materials with different oxygen indexes at different temperatures and humidities, and determining the oxygen index range in each oxygen index table; the high heat-resistant flame-retardant material is prepared by different proportions of 26, 32, 34, 38 and 43 in oxygen index respectively; the detection process is as follows:
1) wherein the flow rate of the mixed gas of nitrogen and oxygen in the oxygen index tester is 10.1-11.2L/min, and the size of the flame-retardant material is 100mm multiplied by 10 mm;
2) carrying out difference operation on the oxygen indexes at different humidity and temperatures in the oxygen index table and the oxygen index values measured at the temperature of 25 ℃ and the humidity of 50% to obtain a difference table;
3) measuring the oxygen index of the flame-retardant material on site by using an oxygen index measuring instrument to obtain the oxygen index at the temperature and humidity, checking the oxygen index range corresponding to each oxygen index table in the step 1), and finding the oxygen index table containing the oxygen index measured on site or the oxygen index table with the closest value;
4) and obtaining the difference value under the temperature and the humidity by using a binary interpolation method according to an oxygen index table containing the oxygen index measured on site or a difference value table corresponding to the oxygen index table with the closest value, and performing addition and subtraction operation on the oxygen index measured on site and the difference value to obtain the actual oxygen index of the flame retardant material.
The raw materials and equipment used in the method are as follows:
raw material ABS: 8434,
n-phenylmaleimide terpolymer (AS-MS-NB)
DBDPE：4010。
High-speed mixer: SHR-100A, Kodak machines, Inc., Zhang Jiangsu Kong City;
a double-screw extruder: model SHJ-30, south kyo ruiya polymer equipment ltd;
an injection molding machine: type B-920, Zhejiang Haitian injection molding machine, Inc.;
melt Flow Rate (MFR) meter: model ZR21452, Meister Industrial systems (China) Ltd.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. The preparation method of the high-heat-resistance flame-retardant material is characterized by comprising the following steps of:
s1: preparation of the premix: adding acrylonitrile-butadiene-styrene (ABS), a heat-resistant agent, high rubber powder, a compatibilizer and other various processing aids into a high-speed mixer according to a proportion formula, and mixing to obtain a premix;
s2: and (3) extruding and granulating: putting the premix into a double-screw extruder for extrusion granulation, and controlling the temperature of the double-screw extruder by 10 sections to prepare heat-resistant high-heat-resistant acrylonitrile-butadiene-styrene (ABS) master batch;
s3: secondary premixing: adding the high-heat-resistant acrylonitrile-butadiene-styrene (ABS) master batch in the S1, a DBDPE flame-retardant system, a compatibilizer and other various processing aids into a high-speed mixer according to the proportion of a formula for premixing, and putting the secondary premix into a double-screw extruder for extrusion granulation;
s4: injection molding: extruding and granulating, drying the heat-resistant agent high-heat-resistant acrylonitrile-butadiene-styrene (ABS) master batch prepared after secondary premixing at the temperature of 80 ℃ for 4h, and performing injection molding at the injection temperature of 180 ℃ and 210 ℃ by a precision injection molding machine;
s5: and (3) flame retardance detection: putting the existing flame-retardant materials of the same kind with different oxygen indexes in the market into a combustion cylinder of an oxygen index tester to measure the oxygen indexes at different temperatures and humidities, respectively obtaining oxygen index tables of the prepared and molded high heat-resistant flame-retardant materials with different oxygen indexes at different temperatures and humidities, and determining the oxygen index range in each oxygen index table; the high heat-resistant flame-retardant material is prepared by different proportions of 26, 32, 34, 38 and 43 in oxygen index, so that better performance of the flame-retardant material is obtained, and the high heat-resistant flame-retardant material is the optimal material proportion.
2. The preparation method of the high heat-resistant flame-retardant material according to claim 1, wherein the heat-resistant agent in S1 is AS-MS-NB, the high rubber powder is DBDPE, the compatibilizer is HR181, and the ratio of acrylonitrile-butadiene-styrene (ABS), the heat-resistant agent, the high rubber powder and the compatibilizer is 60: 20: 12.5: 7.5.
3. the method for preparing a high heat-resistant flame-retardant material according to claim 1, wherein the high-speed mixer in S1 is used for mixing at a working speed of 400r/min for 2min and then at a working speed of 1000r/min for 1 min.
4. The method as claimed in claim 1, wherein the twin-screw extruder in S2 is controlled at a temperature of 240 ℃ and 270 ℃ and at a main machine rotation speed of 1020r/min and at a feeding rotation speed of 400 r/min.
5. The method as claimed in claim 1, wherein the barrel temperature of the twin-screw extruder in S3 is controlled in 10 stages, the temperature is controlled at 210 ℃ and 180 ℃ respectively, the main machine rotation speed is 1020r/min, and the feeding rotation speed is 400 r/min.
6. The method for preparing a high heat-resistant flame-retardant material according to claim 1, wherein the flame retardancy of S5 is tested by the following specific procedures:
1) wherein the oxygen index tester is protected by the mixed gas of nitrogen and oxygen, and the temperature and humidity conditions are changed for testing;
2) carrying out difference operation on the oxygen indexes at different humidity and temperatures in the oxygen index table and the oxygen index values measured at the temperature of 25 ℃ and the humidity of 50% to obtain a difference table;
3) measuring the oxygen index of the flame-retardant material on site by using an oxygen index measuring instrument to obtain the oxygen index at the temperature and humidity, checking the oxygen index range corresponding to each oxygen index table in the step 1), and finding the oxygen index table containing the oxygen index measured on site or the oxygen index table with the closest value;
4) and obtaining the difference value under the temperature and the humidity by using a binary interpolation method according to an oxygen index table containing the oxygen index measured on site or a difference value table corresponding to the oxygen index table with the closest value, and performing addition and subtraction operation on the oxygen index measured on site and the difference value to obtain the actual oxygen index of the flame retardant material.
7. The method for preparing a high heat-resistant flame-retardant material according to claim 6, wherein the flow rate of the mixed gas is 10.1-11.2L/min.
8. The preparation method of the high heat-resistant flame-retardant material according to claim 6, wherein the detection size of the flame-retardant material is that the length, width and height of the flame-retardant material are both more than 10mm and less than 15mm, and the detection size can be controlled by the existing granulation equipment.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643507A (en) * | 2012-05-10 | 2012-08-22 | 金发科技股份有限公司 | Extremely-high-temperature-resistant anti-flaming ABS (Acrylonitrile Butadiene Styrene) composition as well as preparation method and applications thereof |
| CN104374867A (en) * | 2014-11-24 | 2015-02-25 | 重庆消防安全技术研究服务有限责任公司 | Flame retardant material and method for quickly detecting oxygen index of product on site |
| CN105524396A (en) * | 2015-11-11 | 2016-04-27 | 陕西聚洁瀚化工有限公司 | Preparation method for high-heat-resistance flame-retardant material |
| US20170355847A1 (en) * | 2014-12-31 | 2017-12-14 | Shanghai Kumhosunny Plastics Co., Ltd | Low-gloss heat-resistant abs resin composition and its preparation method |
-
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643507A (en) * | 2012-05-10 | 2012-08-22 | 金发科技股份有限公司 | Extremely-high-temperature-resistant anti-flaming ABS (Acrylonitrile Butadiene Styrene) composition as well as preparation method and applications thereof |
| CN104374867A (en) * | 2014-11-24 | 2015-02-25 | 重庆消防安全技术研究服务有限责任公司 | Flame retardant material and method for quickly detecting oxygen index of product on site |
| US20170355847A1 (en) * | 2014-12-31 | 2017-12-14 | Shanghai Kumhosunny Plastics Co., Ltd | Low-gloss heat-resistant abs resin composition and its preparation method |
| CN105524396A (en) * | 2015-11-11 | 2016-04-27 | 陕西聚洁瀚化工有限公司 | Preparation method for high-heat-resistance flame-retardant material |
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