CN109971148A - A kind of modified PC composite material and preparation method of environmental protection flame retardant - Google Patents
A kind of modified PC composite material and preparation method of environmental protection flame retardant Download PDFInfo
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- CN109971148A CN109971148A CN201910213670.4A CN201910213670A CN109971148A CN 109971148 A CN109971148 A CN 109971148A CN 201910213670 A CN201910213670 A CN 201910213670A CN 109971148 A CN109971148 A CN 109971148A
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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
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G79/00—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule
- C08G79/02—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule a linkage containing phosphorus
- C08G79/04—Phosphorus linked to oxygen or to oxygen and carbon
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
-
- 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
Abstract
The invention discloses a kind of modified PC composite material and preparation method of environmental protection flame retardant, which is prepared by following weight parts raw material: 10-70 parts of polycarbonate, 5-60 parts of carbon fiber, 5-60 parts of ABS resin, 0.1-3 parts of modified flame-retardant agent, 0.5-2 parts of sodium acrylate, 1-3 parts of silane coupling agent, 1-8 parts of nano montmorillonite；The invention, the viscosity of PC is reduced by the addition of carbon fiber, increase the mobility of melt, make composite material that there is excellent processing performance, but the toughness of PC/ carbon fiber blend is poor, carries out toughening by the way that ABS resin is added, the mobility and tensile strength of composite material are further enhanced, notch impact strength is also improved, and trielement composite material PC/ carbon fiber/ABS has the processing performance and mechanical property of excellent benefit simultaneously, is conducive to efficient industrialized production.
Description
Technical field
The present invention relates to technical field of composite materials, and in particular to a kind of modified PC composite material of environmental protection flame retardant and its preparation
Method.
Background technique
Polycarbonate (PC) refers to the general name of the quasi polymer in strand containing carbonate group, due to synthesis of bisphenol A
Type PC yield is maximum, purposes is most wide, and so-called polycarbonate is bisphenol A polycarbonate under normal circumstances.Due to poly- carbonic acid
Particularity on ester structure has become the general engineering plastic that growth rate is most fast in five large-engineering plastics.Polycarbonate is
A kind of thermoplastic engineering plastic of high comprehensive performance has impact flexibility outstanding, the transparency and dimensional stability, excellent
Mechanical strength, electrical insulating property, use temperature range is wide, good creep resistant, weatherability and self-extinguishment.Currently, polycarbonate
The fields such as electronics, electric appliance, automobile, optical material are widely used in by its excellent performance.But polycarbonate also have it is aobvious
The shortcomings that wanting, as contained a large amount of phenyl ring in its strand, molecular rigidity is big, and molecule space steric hindrance is big, leads to its melting temperature
Height, melt viscosity is big, and processing fluidity is poor；It is also easy to produce stress cracking to notch sensitive；Fatigue resistance, solvent resistance and resistance to
Mill property difference etc.；Material property is seriously affected, the application and development of polycarbonate are significantly limited.
Summary of the invention
In order to overcome above-mentioned technical problem, the purpose of the present invention is to provide a kind of modified PC composite materials of environmental protection flame retardant
And preparation method thereof, the addition of carbon fiber reduces the viscosity of PC, increases the mobility of melt, has composite material excellent
Processing performance, but the toughness of PC/ carbon fiber blend is poor, carry out toughening by the way that ABS resin is added, composite material
Mobility and tensile strength are further enhanced, and notch impact strength is also improved, trielement composite material PC/ carbon fiber
Dimension/ABS has the processing performance and mechanical property of excellent benefit simultaneously, is conducive to efficient industrialized production；
PC composite material is modified by the way that modified flame-retardant agent is added, modified flame-retardant agent is made of silicon, P elements, when
When silicon, phosphorus collective effect, the two plays the effect of cooperative flame retardant, and at high temperature, the formation of phosphorus energy catalysed promoted charcoal, silicon then increases
The thermal stability of charcoal, to have the function that synergistic is fire-retardant, PC composite material forms inner surface foaming, outer surface in burning
Fine and close continuous foamed char, flame retardant effect is more preferable, more environmentally-friendly；PC composite material is changed by the way that nano montmorillonite is added
Property, PC composite material anti-stress cracking performance can be enhanced, improve the barrier property and chemical resistance energy of material.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of modified PC composite material of environmental protection flame retardant, the composite material are prepared by following weight parts raw material: poly- carbonic acid
10-70 parts of ester, 5-60 parts of carbon fiber, 5-60 parts of ABS resin, 0.1-3 parts of modified flame-retardant agent, 0.5-2 parts of sodium acrylate, silane are even
Agent 1-3 parts, 1-8 parts of nano montmorillonite of connection；
A kind of preparation method of the modified PC composite material of environmental protection flame retardant, the composite material are prepared by the following method:
1) be dried: weighing the modified PC composite material each component of the environmental protection flame retardant as required, by polycarbonate,
ABS resin and carbon fiber are placed at 110-130 DEG C in vacuum drier 4 hours dry；
2) premix is prepared: at 800-1800 revs/min after the polycarbonate in step 1) after drying and carbon fiber are mixed
Lower mixed at high speed 5-8 minutes；Then being added has nano montmorillonite, mixed at high speed 5-8 minutes lower at 800-1800 revs/min；Finally
Modified flame-retardant agent, sodium acrylate, silane coupling agent is added, it is mixed at high speed 2-5 minutes lower at 800-1800 revs/min, it is premixed
Material；
3) it prepares composite material: the premix prepared in step 2) is fed into extruding pelletization in parallel dual-screw extruding machine,
The temperature of extrusion is 250-270 DEG C, and after expecting that grain is 2 hours dry under the conditions of 90-110 DEG C, with injection molding machine sample preparation, injection temperature is
220-260 DEG C, obtain the modified PC composite material of environmental protection flame retardant.
The present invention has excellent self-lubricating function, is added by adding carbon fiber, carbon fiber in polycarbonate
Enter in polymer, on the one hand increase the spacing between macromolecular, reduce intermolecular force: another aspect carbon fiber with polymerize
Active force between object macromolecular is also less than the active force between polymer macromolecule, itself rubs when reducing melt flows
Resistance is wiped, is reduced so as to cause apparent viscosity after carbon fiber is added in polycarbonate.In addition, carbon fiber can also improve poly- carbon
Adhesiveness between acid esters and metal, this is also one of the reason of causing fluidity of molten to improve.As carbon fiber content increases
After to a certain extent, the friction in melt between macromolecular and between macromolecular and carbon fiber, carbon fiber and carbon fiber gradually increases
Greatly, so mobility is also gradually reduced therewith, apparent viscosity is in increase tendency.But no matter gone back between carbon fiber and macromolecular
It is the active force that active force between carbon fiber is respectively less than between macromolecular, so the apparent viscosity of PC/ carbon fiber blend is total
It is less than the apparent viscosity of pure PC.Therefore, the addition of carbon fiber reduces the viscosity of PC, increases the mobility of melt, makes multiple
Condensation material has excellent processing performance.
The toughness of PC/ carbon fiber blend is poor, carries out toughening, the mobility of composite material by the way that ABS resin is added
It is further enhanced with tensile strength, notch impact strength is also improved, and trielement composite material PC/ carbon fiber/ABS is same
When processing performance and mechanical property with excellent benefit, be conducive to efficient industrialized production.
PC composite material is modified by the way that modified flame-retardant agent is added, when silicon, phosphorus collective effect, the two plays collaboration
Fire-retardant effect, at high temperature, the formation of phosphorus energy catalysed promoted charcoal, silicon then increase the thermal stability of charcoal, to reach synergistic resistance
The effect of combustion, PC composite material form inner surface foaming, the fine and close continuous foamed char in outer surface, flame retardant effect in burning
More preferably, more environmentally-friendly.
PC composite material is modified by the way that nano montmorillonite is added, PC composite material anti-stress cracking can be enhanced
Can, improve the barrier property and chemical resistance energy of material.
As a further solution of the present invention: the described composite material is prepared by following weight parts raw material: poly- carbonic acid
50 parts of ester, 30 parts of carbon fiber, 30 parts of ABS resin, 0.5 part of modified flame-retardant agent, 1 part of sodium acrylate, silane coupling agent 1 part, nanometer
5 parts of montmorillonite.
As a further solution of the present invention: the silane coupling agent is vinyltriethoxysilane, vinyl front three
At least one of oxysilane and vinyl three-beta-methoxy Ethoxysilane.
As a further solution of the present invention: the nano montmorillonite is prepared by following step:
In 180-200 DEG C of air blast bellows, montmorillonite tiling thickness 15-20mm to be dried 2 hours, taking-up sealing is spare,
Dewatered montmorillonite 65-75 parts and epoxides 25-35 parts are sequentially added in agitating device, is stirred 10-30 minutes,
After mixing, it is transported in double roll mill, is kneaded 10-20 minutes at 150-170 DEG C, is solidified into closely knit powdery
Nano montmorillonite both can be obtained in object, ultra-fine grinding.
As a further solution of the present invention: the modified flame-retardant agent is prepared by following step:
Step 1: in ventilating kitchen, in the tri- neck round bottom of 500mL that reflux condensing tube, thermometer and HCL absorption plant are housed
In flask, it is passed through nitrogen, 10-20 parts of pentaerythrites is then added, and phosphorus oxychloride 250mL is added, is then slowly stirred and rises
High-temperature is heated to 90 DEG C, and reaction was slowly warming up to 120 DEG C after 1 hour, after system is cooled to room temperature, by the mixing after reaction
Object obtains white sand shape solid product after filtering, and filters out the complete phosphorus oxychloride solvent of unreacted, after being recovered to drying
Reagent bottle in；Then solid product is washed with methylene chloride and acetone solvent, then is washed with ether, then quickly will
Product is put into vacuum oven to be dried 12 hours at 40-60 DEG C, obtains white sand shape solid product；
Step 2: equipped with mechanical agitator, thermometer, constant pressure funnel 250mL low-temp reaction kettle in, first plus
Enter excessive saturation NaOH solution, then utilizes and reaction system is maintained -8 DEG C of temperature, while being measured with the graduated cylinder after dry
The dichlorosilane of 40mL, is added in constant pressure funnel, and dichlorosilane is slowly added dropwise into the NaOH solution of saturation, quickly stirs
Solution is mixed, is dripped off in 1.5h to dichlorosilane, is continued after stirring 0.5h, stops reaction and obtains clear solution, it is cold to system
But to the HCI solution diluted in right amount after room temperature, is slowly added dropwise to obtained clear solution, the products of a large amount of whites are generated,
White depositions are washed after filtering, temperature be 40-60 DEG C, be dried in vacuo 12 hours, after obtain white solid powder；
Step 3: in draught cupboard, the tri- neck round bottom of 500mL equipped with reflux condensing tube, thermometer and HCI absorption plant is burnt
In bottle, after entire reaction unit is cooled to room temperature, 10-20 parts of white sand shape solid products are first weighed in a round bottom flask, so
300mL acetonitrile is measured with graduated cylinder afterwards and is added in round-bottomed flask；Under nitrogen atmosphere, temperature is warming up to 70 DEG C and is uniformly stirred
It mixes, is partially dissolved in acetonitrile to white sand shape solid product, 5-10 parts of white solid powders are added, after reaction 1.5 hours, then
It is gradually warmed up to 85 DEG C, determining in system, which does not have HCI gas to generate, stops reaction, and reactant obtains white powder production after filtering
Object is respectively washed three times with acetonitrile, acetone and ether, is 50-70 DEG C in temperature, is dried in vacuo 12 hours, can both obtain modified resistance
Fire agent.
As a further solution of the present invention: the partial size of the nano montmorillonite is 15-76um.
As a further solution of the present invention: in the step 1) vacuum drier include two support bases, regulating mechanism and
Drying cylinder is equipped with motor inside one support base, shaft is fixedly connected on the output shaft of the motor, the shaft is passed through
It wears drying cylinder and is connect with another support base bearing, the both ends of the shaft and drying cylinder pass through internal gear and external gear cooperation
Engagement connection, the two internal gear insertions are mounted on the both ends of drying cylinder, and two external gears are fixedly mounted in shaft, described
Regulating mechanism is uniformly installed, the regulating mechanism is located inside drying cylinder in shaft；
The regulating mechanism includes fixed plate, groove, pumping board, clamping plate and fastening bolt, and the inside of the fixed plate opens up
Fluted, inserted with pumping board in the groove, fastening bolt for driving two Boards wall pumping boards, fix by the top of the pumping board
It is connected with scraper plate.
As a further solution of the present invention: the bottom center of the drying cylinder offers discharge gate, the discharge gate
Two sides offer the condensation mouth of a river, be equipped at the top center of the drying cylinder and take out true tracheae, it is described to take out the one of true tracheae
Side offers feed inlet, and the top both ends of the drying cylinder offer heating steam port.
As a further solution of the present invention: being provided with teeth on the pumping board, clamping plate.
Beneficial effects of the present invention:
1, the addition of carbon fiber reduces the viscosity of PC, increases the mobility of melt, has composite material excellent
Processing performance, but the toughness of PC/ carbon fiber blend is poor, carries out toughening, the stream of composite material by the way that ABS resin is added
Dynamic property and tensile strength are further enhanced, and notch impact strength is also improved, and trielement composite material PC/ carbon fiber/
ABS has the processing performance and mechanical property of excellent benefit simultaneously, is conducive to efficient industrialized production；
2, PC composite material being modified by the way that modified flame-retardant agent is added, modified flame-retardant agent is made of silicon, P elements, when
When silicon, phosphorus collective effect, the two plays the effect of cooperative flame retardant, and at high temperature, the formation of phosphorus energy catalysed promoted charcoal, silicon then increases
The thermal stability of charcoal, to have the function that synergistic is fire-retardant, PC composite material forms inner surface foaming, outer surface in burning
Fine and close continuous foamed char, flame retardant effect is more preferable, more environmentally-friendly.
3, PC composite material is modified by the way that nano montmorillonite is added, PC composite material anti-stress cracking can be enhanced
Performance improves the barrier property and chemical resistance energy of material.
4, motor rotates, and drives shaft rotation, is provided with two external gears, external gear and drying cylinder both ends internal gear in shaft
Engagement connection, to drive drying cylinder to rotate, while shaft runs through drying cylinder, is uniformly equipped with regulating mechanism in shaft, adjusts
Mechanism is connect with scraper plate, can be not only stirred to material, so that drying is more full and uniform, while can will be in drying cylinder
It is glued on wall under viscous material extension, is convenient to clean, is easy to use, drive shaft and drying cylinder to rotate by a motor, more supernumerary segment
Energy；In the groove that plate insertion fixed plate is opened up, then rotational fastener bolt, two clamping plates of driving fix plate, pumping board,
It is provided with teeth on clamping plate, so that Boards wall pumping board more fastens, convenient for adjusting the length of scraper plate, does not have to model conveniently
Drying cylinder is dried.
Detailed description of the invention
The present invention will be further described below with reference to the drawings.
Fig. 1 is vacuum drier overall structure diagram of the present invention.
Fig. 2 is vacuum drier middle gear engaging structure schematic diagram of the present invention.
Fig. 3 is regulating mechanism mounting structure schematic diagram in vacuum drier of the present invention.
Fig. 4 is regulating mechanism overall structure diagram in vacuum drier of the present invention.
In figure: 1, support base；2, regulating mechanism；3, scraper plate；4, drying cylinder；5, discharge gate；6, the mouth of a river is condensed；7, internal tooth
Wheel；8, shaft；9, motor；10, steam port is heated；11, feed inlet；12, true tracheae is taken out；13, external gear；21, fixed plate；22,
Groove；23, pumping board；24, clamping plate；25, fastening bolt.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, all other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of modified PC composite material of environmental protection flame retardant, the composite material are prepared by following weight parts raw material: poly- carbonic acid
30 parts of ester, 10 parts of carbon fiber, 10 parts of ABS resin, 0.1 part of modified flame-retardant agent, 0.5 part of sodium acrylate, vinyl triethoxyl silicon
1 part of alkane, 1 part of nano montmorillonite；
A kind of preparation method of the modified PC composite material of environmental protection flame retardant, the composite material are prepared by the following method:
1) it is dried: the modified PC composite material each component of environmental protection flame retardant is weighed as required, by polycarbonate, ABS resin
It is placed at 110 DEG C in vacuum drier with carbon fiber 4 hours dry；
2) premix is prepared: after the polycarbonate after drying in step 1) and carbon fiber are mixed under 800 revs/min at a high speed
Mixing 5 minutes；Then be added have nano montmorillonite, 800 revs/min lower mixed at high speed 5 minutes；Be eventually adding modified flame-retardant agent,
Sodium acrylate, vinyltriethoxysilane, it is mixed at high speed 2-5 minutes lower at 800 revs/min, obtain premix；
3) it prepares composite material: the premix prepared in step 2) is fed into extruding pelletization in parallel dual-screw extruding machine,
The temperature of extrusion is 250 DEG C, and after expecting that grain is 2 hours dry under the conditions of 90 DEG C, with injection molding machine sample preparation, injection temperature is 220 DEG C, is obtained
To the modified PC composite material of environmental protection flame retardant.
The nano montmorillonite is prepared by following step:
In 180 DEG C of air blast bellows, montmorillonite tiling thickness 15mm is dried 2 hours, taking-up sealing is spare, will be dehydrated
65 parts and 25 parts of epoxides of montmorillonite afterwards sequentially add in agitating device, are stirred 10 minutes, after mixing, by it
It is transported in double roll mill, is kneaded 10 minutes at 150 DEG C, is solidified into closely knit powder, nanometer both can be obtained in ultra-fine grinding
Montmorillonite, the partial size of nano montmorillonite are 15um.
The modified flame-retardant agent is prepared by following step:
Step 1: in ventilating kitchen, in the tri- neck round bottom of 500mL that reflux condensing tube, thermometer and HCL absorption plant are housed
In flask, it is passed through nitrogen, 10 parts of pentaerythrites is then added, and phosphorus oxychloride 250mL is added, is then slowly stirred and increases temperature
Degree is heated to 90 DEG C, and reaction was slowly warming up to 120 DEG C after 1 hour, and after system is cooled to room temperature, the mixture after reaction is passed through
White sand shape solid product is obtained after crossing suction filtration, filters out the complete phosphorus oxychloride solvent of unreacted, the examination after being recovered to drying
In agent bottle；Then solid product is washed with methylene chloride and acetone solvent, then is washed with ether, then quickly by product
It is put into vacuum oven and is dried 12 hours at 40-60 DEG C, obtain white sand shape solid product；
Step 2: equipped with mechanical agitator, thermometer, constant pressure funnel 250mL low-temp reaction kettle in, first plus
Enter excessive saturation NaOH solution, then utilizes and reaction system is maintained -8 DEG C of temperature, while being measured with the graduated cylinder after dry
The dichlorosilane of 40mL, is added in constant pressure funnel, and dichlorosilane is slowly added dropwise into the NaOH solution of saturation, quickly stirs
Solution is mixed, is dripped off in 1.5h to dichlorosilane, is continued after stirring 0.5h, stops reaction and obtains clear solution, it is cold to system
But to the HCI solution diluted in right amount after room temperature, is slowly added dropwise to obtained clear solution, the products of a large amount of whites are generated,
White depositions are washed after filtering, temperature be 40 DEG C, be dried in vacuo 12 hours, after obtain white solid powder；
Step 3: in draught cupboard, the tri- neck round bottom of 500mL equipped with reflux condensing tube, thermometer and HCI absorption plant is burnt
In bottle, after entire reaction unit is cooled to room temperature, first weighs 10 parts of white sand shape solid products in a round bottom flask, then use
Graduated cylinder measures 300mL acetonitrile and is added in round-bottomed flask；Under nitrogen atmosphere, temperature is warming up to 70 DEG C and uniform stirring, to
White sand shape solid product is partially dissolved in acetonitrile, and 5 parts of white solid powders are added, after reaction 1.5 hours, then are gradually warmed up
To 85 DEG C, determining in system, which does not have HCI gas to generate, stops reaction, and reactant obtains white powder product after filtering, uses second
Nitrile, acetone and ether respectively wash three times, are 50 DEG C in temperature, are dried in vacuo 12 hours, modified flame-retardant agent both can be obtained.
Embodiment 2
A kind of modified PC composite material of environmental protection flame retardant, the composite material are prepared by following weight parts raw material: poly- carbonic acid
50 parts of ester, 30 parts of carbon fiber, 30 parts of ABS resin, 0.5 part of modified flame-retardant agent, 1 part of sodium acrylate, silane coupling agent 1 part, nanometer
5 parts of montmorillonite；
A kind of preparation method of the modified PC composite material of environmental protection flame retardant, the composite material are prepared by the following method:
1) it is dried: the modified PC composite material each component of environmental protection flame retardant is weighed as required, by polycarbonate, ABS resin
It is placed at 120 DEG C in vacuum drier with carbon fiber 4 hours dry；
2) prepare premix: polycarbonate and carbon fiber after will be dry in step 1) be high under 1000 revs/min after mixing
Speed mixing 7 minutes；Then be added have nano montmorillonite, 1000 revs/min lower mixed at high speed 7 minutes；It is eventually adding modified flame-retardant
Agent, sodium acrylate, vinyltriethoxysilane, 1000 revs/min lower mixed at high speed 3 minutes, obtain premix；
3) it prepares composite material: the premix prepared in step 2) is fed into extruding pelletization in parallel dual-screw extruding machine,
The temperature of extrusion is 260 DEG C, and after expecting that grain is 2 hours dry under the conditions of 100 DEG C, with injection molding machine sample preparation, injection temperature is 240 DEG C,
Obtain the modified PC composite material of environmental protection flame retardant.
The nano montmorillonite is prepared by following step:
In 190 DEG C of air blast bellows, montmorillonite tiling thickness 18mm is dried 2 hours, taking-up sealing is spare, will be dehydrated
70 parts and 30 parts of epoxides of montmorillonite afterwards sequentially add in agitating device, are stirred 20 minutes, after mixing, by it
It is transported in double roll mill, is kneaded 15 minutes at 160 DEG C, is solidified into closely knit powder, nanometer both can be obtained in ultra-fine grinding
Montmorillonite, the partial size of nano montmorillonite are 50um.
The modified flame-retardant agent is prepared by following step: identical as 1 preparation method of embodiment.
Embodiment 3
A kind of modified PC composite material of environmental protection flame retardant, the composite material are prepared by following weight parts raw material: poly- carbonic acid
70 parts of ester, 60 parts of carbon fiber, 60 parts of ABS resin, 3 parts of modified flame-retardant agent, 2 parts of sodium acrylate, vinyltriethoxysilane 3
Part, 8 parts of nano montmorillonite；
A kind of preparation method of the modified PC composite material of environmental protection flame retardant, the composite material are prepared by the following method:
1) it is dried: the modified PC composite material each component of environmental protection flame retardant is weighed as required, by polycarbonate, ABS resin
It is placed at 130 DEG C in vacuum drier with carbon fiber 4 hours dry；
2) prepare premix: polycarbonate and carbon fiber after will be dry in step 1) be high under 1800 revs/min after mixing
Speed mixing 8 minutes；Then be added have nano montmorillonite, 1800 revs/min lower mixed at high speed 8 minutes；It is eventually adding modified flame-retardant
Agent, sodium acrylate, vinyltriethoxysilane, 1800 revs/min lower mixed at high speed 5 minutes, obtain premix；
3) it prepares composite material: the premix prepared in step 2) is fed into extruding pelletization in parallel dual-screw extruding machine,
The temperature of extrusion is 270 DEG C, and after expecting that grain is 2 hours dry under the conditions of 110 DEG C, with injection molding machine sample preparation, injection temperature is 260 DEG C,
Obtain the modified PC composite material of environmental protection flame retardant.
The nano montmorillonite is prepared by following step:
In 200 DEG C of air blast bellows, montmorillonite tiling thickness 20mm is dried 2 hours, taking-up sealing is spare, will be dehydrated
75 parts and 35 parts of epoxides of montmorillonite afterwards sequentially add in agitating device, are stirred 30 minutes, after mixing, by it
It is transported in double roll mill, is kneaded 20 minutes at 170 DEG C, is solidified into closely knit powder, nanometer both can be obtained in ultra-fine grinding
Montmorillonite, the partial size of nano montmorillonite are 76um.
The modified flame-retardant agent is prepared by following step: identical as 1 preparation method of embodiment.
Comparative example 1:
A kind of modified PC composite material of environmental protection flame retardant, the composite material are prepared by following weight parts raw material: poly- carbonic acid
30 parts of ester, 10 parts of carbon fiber, 10 parts of ABS resin, 0.1 part of fire retardant, 0.5 part of sodium acrylate, vinyltriethoxysilane 1
Part, 1 part of nano montmorillonite；
A kind of preparation method of the modified PC composite material of environmental protection flame retardant, the composite material are prepared by the following method:
1) it is dried: the modified PC composite material each component of environmental protection flame retardant is weighed as required, by polycarbonate, ABS resin
It is placed at 110-130 DEG C in vacuum drier with carbon fiber 4 hours dry；
2) premix is prepared: after the polycarbonate after drying in step 1) and carbon fiber are mixed under 800 revs/min at a high speed
Mixing 5 minutes；Then being added has nano montmorillonite, mixed at high speed 5-8 minutes lower at 800 revs/min；It is eventually adding fire retardant, third
Olefin(e) acid sodium, vinyltriethoxysilane, 800 revs/min lower mixed at high speed 2 minutes, obtain premix；
3) it prepares composite material: the premix prepared in step 2) is fed into extruding pelletization in parallel dual-screw extruding machine,
The temperature of extrusion is 250 DEG C, and after expecting that grain is 2 hours dry under the conditions of 90 DEG C, with injection molding machine sample preparation, injection temperature is 220 DEG C, is obtained
To the modified PC composite material of environmental protection flame retardant.
Wherein, fire retardant is urea formaldehyde, acrylic resin, sodium metasilicate, calcium nitrate, polypropylene, polystyrene, polychlorostyrene second
Alkene, polyamide, vinylacetate it is one or more；
The nano montmorillonite is prepared by following step: identical as 1 preparation method of embodiment.
The test of PC composite property:
PC composite material prepared by embodiment 1-3 and comparative example 1 is put into carbon tetrachloride and is impregnated 48 hours, is observed
The PC composite material surface crackle of the face checking phenomenon of PC composite material, embodiment 1-3 preparation is slightly deepened, and crackle is tiny
Reticular structure, and had peeling phenomenon in comparative example 1；It, can to illustrate that nano montmorillonite is modified PC composite material
To enhance PC composite material anti-stress cracking performance, the barrier property and chemical resistance energy of material are improved.
Embodiment 1-3 and PC composite material prepared by comparative example 1 and traditional handicraft are tested for the property, test knot
Fruit is as illustrated in chart 1:
Table 1
As upper table 1 it is found that PC composite material prepared by embodiment 1-3 and comparative example 1 have good tensile strength and
Impact strength is but the embodiment 1-3 because joined carbon fiber, ABS resin and nano montmorillonite in PC composite material
The anti-flammability of the PC composite material of preparation is more better than comparative example 1, be because embodiment 1-3 in joined modified flame-retardant agent,
Modified flame-retardant agent is made of phosphorus, element silicon, and when silicon, phosphorus collective effect, the two plays the effect of cooperative flame retardant, at high temperature,
The formation of phosphorus energy catalysed promoted charcoal, silicon then increases the thermal stability of charcoal, to have the function that synergistic is fire-retardant, PC composite material exists
When burning, inner surface foaming is formed, the fine and close continuous foamed char in outer surface, flame retardant effect is more preferable, more environmentally-friendly.
Please refer to shown in Fig. 1-4: in step 1) vacuum drier include two support bases 1, regulating mechanism 2 and drying cylinder 4, one
Motor 9 is installed inside support base 1, is fixedly connected with shaft 8 on the output shaft of motor 9, shaft 8 through drying cylinder 4 and with it is another
The connection of one support base, 1 bearing, shaft 8 passes through internal gear 7 with the both ends of drying cylinder 4 and 13 fit engagement of external gear is connect, and two
Internal gear 7 is embedded in the both ends for being mounted on drying cylinder 4, and two external gears 13 are fixedly mounted in shaft 8, are uniformly equipped in shaft 8
Regulating mechanism 2, regulating mechanism 2 are located inside drying cylinder 4；Regulating mechanism 2 includes fixed plate 21, groove 22, pumping board 23, clamping plate 24
With fastening bolt 25, the inside of fixed plate 21 opens up fluted 22, and inserted with pumping board 23 in groove 22, fastening bolt 25 is for driving
The dynamic fixed pumping board 23 of two clamping plates 24, the top of pumping board 23 is fixedly connected with scraper plate 3；The bottom center of drying cylinder 4 offers row
Material mouth 5, the two sides of discharge gate 5 offer the condensation mouth of a river 6, are equipped at the top center of drying cylinder 4 and take out true tracheae 12, take out true
The side of tracheae 12 offers feed inlet 11, and the top both ends of drying cylinder 4 offer heating steam port 10；Pumping board 23, clamping plate
Teeth are provided on 24, so that the fixed pumping board 23 of clamping plate 24 more fastens.
Working principle: motor 9 rotates, and shaft 8 is driven to rotate, and is provided with two external gears 13 in shaft 8, external gear 13 and dry
Dry 4 both ends internal gear 7 of cylinder engagement connection, to drive drying cylinder 4 to rotate, while shaft 8 is uniform on drying cylinder 4, shaft 8
Regulating mechanism 2 is installed, regulating mechanism 2 is connect with scraper plate 3, can be not only stirred to material, so that drying is more abundant
Uniformly, it while can will be glued on 4 inner wall of drying cylinder under viscous material extension, be convenient to clean, be easy to use, pass through 9 band of motor
Turn axis 8 and drying cylinder 4 rotate, more energy saving；Pumping board 23 is inserted into the groove 22 that fixed plate 21 opens up, then rotational fastener
Bolt 25, two clamping plates 24 of driving fix pumping board 23, are provided with teeth on pumping board 23, clamping plate 24, so that clamping plate 24 is fixed
Pumping board 23 more fastens, and convenient for adjusting the length of scraper plate 3, the convenient drying cylinder 4 for not having to model is dried.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
Above content is only citing made for the present invention and explanation, affiliated those skilled in the art are to being retouched
The specific embodiment stated does various modifications or additions or is substituted in a similar manner, and without departing from invention or surpasses
More range defined in the claims, is within the scope of protection of the invention.
Claims (10)
1. a kind of modified PC composite material of environmental protection flame retardant, which is characterized in that the composite material is prepared by following weight parts raw material
It arrives: 10-70 parts of polycarbonate, 5-60 parts of carbon fiber, 5-60 parts of ABS resin, 0.1-3 parts of modified flame-retardant agent, sodium acrylate 0.5-2
Part, 1-3 parts of silane coupling agent, 1-8 parts of nano montmorillonite；
The modified flame-retardant agent is prepared by following step:
Step 1: in ventilating kitchen, in the 500mL three neck round bottom that reflux condensing tube, thermometer and HCl absorption plant are housed
In, it is passed through nitrogen, 10-20 parts of pentaerythrites is then added, and phosphorus oxychloride 250mL is added, is then slowly stirred and increases temperature
Degree is heated to 90 DEG C, and reaction was slowly warming up to 120 DEG C after 1 hour, and after system is cooled to room temperature, the mixture after reaction is passed through
White sand shape solid product is obtained after crossing suction filtration, then solid product is washed with methylene chloride and acetone solvent, then uses
Product, is then quickly put into vacuum oven and dries 12 hours at 40-60 DEG C, obtain white sand shape solid by ether washing
Product；
Step 2: equipped with mechanical agitator, thermometer, constant pressure funnel 250mL low-temp reaction kettle in, be first added
Then the saturation NaOH solution of amount utilizes reaction system maintaining -8 DEG C of temperature, while measuring 40mL with the graduated cylinder after dry
Dichlorosilane, be added in constant pressure funnel, dichlorosilane be slowly added dropwise into the NaOH solution of saturation, quickly stir molten
Liquid drips off in 1.5h to dichlorosilane, continues after stirring 0.5h, stops reaction and obtains clear solution, is cooled to system
After room temperature, the HCI solution diluted in right amount is slowly added dropwise to obtained clear solution, generates the product of a large amount of whites, white
Sediment is washed after filtering, temperature be 40-60 DEG C, be dried in vacuo 12 hours, after obtain white solid powder；
Step 3: in draught cupboard, the 500mL three neck round bottom equipped with reflux condensing tube, thermometer and HCI absorption plant
In, after entire reaction unit is cooled to room temperature, first weigh 10-20 parts of white sand shape solid products in a round bottom flask, then
300mL acetonitrile is measured with graduated cylinder and is added in round-bottomed flask；Under nitrogen atmosphere, temperature is warming up to 70 DEG C and uniform stirring,
It is partially dissolved in acetonitrile to white sand shape solid product, 5-10 parts of white solid powders is added, after reaction 1.5 hours, then by
85 DEG C are gradually warming up to, determining in system, which does not have HCI gas to generate, stops reaction, and reactant obtains white powder production after filtering
Object is respectively washed three times with acetonitrile, acetone and ether, is 50-70 DEG C in temperature, is dried in vacuo 12 hours, can both obtain modified resistance
Fire agent.
2. the modified PC composite material of a kind of environmental protection flame retardant according to claim 1, which is characterized in that the described composite material
Be prepared by following weight parts raw material: 50 parts of polycarbonate, 30 parts of carbon fiber, 30 parts of ABS resin, 0.5 part of modified flame-retardant agent,
1 part of sodium acrylate, 1 part of silane coupling agent, 5 parts of nano montmorillonite.
3. the modified PC composite material of a kind of environmental protection flame retardant according to claim 1, which is characterized in that the silane coupling agent
For at least one of vinyltriethoxysilane, vinyltrimethoxysilane and vinyl three-beta-methoxy Ethoxysilane.
4. a kind of preparation method of the modified PC composite material of environmental protection flame retardant, which is characterized in that the composite material passes through following methods
It is prepared:
1) be dried: the modified PC composite material of environmental protection flame retardant according to claim 1 weighs each component, by polycarbonate,
ABS resin and carbon fiber are placed at 110-130 DEG C in vacuum drier 4 hours dry；
2) prepare premix: polycarbonate and carbon fiber after will be dry in step 1) be high under 800-1800 revs/min after mixing
Speed mixing 5-8 minutes；Then being added has nano montmorillonite, mixed at high speed 5-8 minutes lower at 800-1800 revs/min；It is eventually adding
Modified flame-retardant agent, sodium acrylate, silane coupling agent, it is mixed at high speed 2-5 minutes lower at 800-1800 revs/min, obtain premix；
3) it prepares composite material: extruding pelletization in the premix feeding parallel dual-screw extruding machine prepared in step 2) squeezes out
Temperature be 250-270 DEG C, grain is expected under the conditions of 90-110 DEG C after dry 2 hours, with injection molding machine sample preparation, injection temperature 220-
260 DEG C, obtain the modified PC composite material of environmental protection flame retardant.
5. a kind of preparation method of the modified PC composite material of environmental protection flame retardant according to claim 4, which is characterized in that described
Nano montmorillonite is prepared by following step:
In 180-200 DEG C of air blast bellows, montmorillonite tiling thickness 15-20mm is dried 2 hours, taking-up sealing is spare, will take off
65-75 parts and epoxides 25-35 parts of montmorillonite after water sequentially add in agitating device, are stirred 10-30 minutes, mix
It after uniformly, is transported in double roll mill, is kneaded 10-20 minutes at 150-170 DEG C, is solidified into closely knit powder, surpass
It is finely divided, nano montmorillonite both can be obtained.
6. a kind of preparation method of the modified PC composite material of environmental protection flame retardant according to claim 4, which is characterized in that described
Modified flame-retardant agent is prepared by following step:
Step 1: in ventilating kitchen, in the 500mL three neck round bottom that reflux condensing tube, thermometer and HCL absorption plant are housed
In, it is passed through nitrogen, 10-20 parts of pentaerythrites is then added, and phosphorus oxychloride 250mL is added, is then slowly stirred and increases temperature
Degree is heated to 90 DEG C, and reaction was slowly warming up to 120 DEG C after 1 hour, and after system is cooled to room temperature, the mixture after reaction is passed through
White sand shape solid product is obtained after crossing suction filtration, filters out the complete phosphorus oxychloride solvent of unreacted, the examination after being recovered to drying
In agent bottle；Then solid product is washed with methylene chloride and acetone solvent, then is washed with ether, then quickly by product
It is put into vacuum oven and is dried 12 hours at 40-60 DEG C, obtain white sand shape solid product；
Step 2: equipped with mechanical agitator, thermometer, constant pressure funnel 250mL low-temp reaction kettle in, be first added
Then the saturation NaOH solution of amount utilizes reaction system maintaining -8 DEG C of temperature, while measuring 40mL with the graduated cylinder after dry
Dichlorosilane, be added in constant pressure funnel, dichlorosilane be slowly added dropwise into the NaOH solution of saturation, quickly stir molten
Liquid drips off in 1.5h to dichlorosilane, continues after stirring 0.5h, stops reaction and obtains clear solution, is cooled to system
After room temperature, the HCI solution diluted in right amount is slowly added dropwise to obtained clear solution, generates the product of a large amount of whites, white
Sediment is washed after filtering, temperature be 40-60 DEG C, be dried in vacuo 12 hours, after obtain white solid powder；
Step 3: in draught cupboard, the 500mL three neck round bottom equipped with reflux condensing tube, thermometer and HCI absorption plant
In, after entire reaction unit is cooled to room temperature, first weigh 10-20 parts of white sand shape solid products in a round bottom flask, then
300mL acetonitrile is measured with graduated cylinder and is added in round-bottomed flask；Under nitrogen atmosphere, temperature is warming up to 70 DEG C and uniform stirring,
It is partially dissolved in acetonitrile to white sand shape solid product, 5-10 parts of white solid powders is added, after reaction 1.5 hours, then by
85 DEG C are gradually warming up to, determining in system, which does not have HCI gas to generate, stops reaction, and reactant obtains white powder production after filtering
Object is respectively washed three times with acetonitrile, acetone and ether, is 50-70 DEG C in temperature, is dried in vacuo 12 hours, can both obtain modified resistance
Fire agent.
7. a kind of preparation method of the modified PC composite material of environmental protection flame retardant according to claim 4, which is characterized in that described
The partial size of nano montmorillonite is 15-76um.
8. a kind of preparation method of the modified PC composite material of environmental protection flame retardant according to claim 4, which is characterized in that described
Vacuum drier includes two support bases (1), regulating mechanism (2) and drying cylinder (4) in step 1), and a support base (1) is internal
It is equipped with motor (9), is fixedly connected with shaft (8) on the output shaft of the motor (9), the shaft (8) runs through drying cylinder (4)
And connect with another support base (1) bearing, the both ends of the shaft (8) and drying cylinder (4) pass through internal gear (7) and external gear
(13) fit engagement connects, and two internal gear (7) insertions are mounted on the both ends of drying cylinder (4), and two external gears (13) are solid
Dingan County is uniformly equipped with regulating mechanism (2), the regulating mechanism (2) is located at drying on shaft (8) on the shaft (8)
Cylinder (4) is internal；
The regulating mechanism (2) includes fixed plate (21), groove (22), pumping board (23), clamping plate (24) and fastening bolt (25), institute
The inside for stating fixed plate (21) opens up fluted (22), and inserted with pumping board (23) in the groove (22), fastening bolt (25) is used
Fixed pumping board (23) in driving two clamping plates (24), the top of the pumping board (23) is fixedly connected with scraper plate (3).
9. a kind of preparation method of the modified PC composite material of environmental protection flame retardant according to claim 8, which is characterized in that described
The bottom center of drying cylinder (4) offers discharge gate (5), and the two sides of the discharge gate (5) offer the condensation mouth of a river (6),
It is equipped at the top center of the drying cylinder (4) and takes out true tracheae (12), the side for taking out true tracheae (12) offers charging
Mouth (11), the top both ends of the drying cylinder (4) offer heating steam port (10).
10. a kind of preparation method of the modified PC composite material of environmental protection flame retardant according to claim 8, which is characterized in that institute
State pumping board (23), clamping plate is provided with teeth on (24).
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| CN116144095A (en) * | 2023-04-19 | 2023-05-23 | 河北兴航线缆有限公司 | Crosslinked polyethylene halogen-free flame-retardant cable and preparation method thereof |
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