CN108690240A - A kind of fire retardant and preparation method thereof - Google Patents
A kind of fire retardant and preparation method thereof Download PDFInfo
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- CN108690240A CN108690240A CN201810576620.8A CN201810576620A CN108690240A CN 108690240 A CN108690240 A CN 108690240A CN 201810576620 A CN201810576620 A CN 201810576620A CN 108690240 A CN108690240 A CN 108690240A
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- C08L19/00—Compositions of rubbers not provided for in groups C08L7/00 - C08L17/00
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- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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Abstract
The invention discloses a kind of fire retardant and preparation method thereof, the fire retardant is made of following raw material:Ethylene glycol ether acetate, Miglyol 812N, nonylphenol polyoxyethylene ether ammonium sulfate, polypropylene oxide triol, urea, aluminium hydroxide, antimony oxide, manganese oxide, diatomite, bleeding agent, the fire retardant by stirring, filtering and centrifugal drying and etc. be made, the fire retardant have high flame resistance.
Description
The application is application No. is 2017104836266, and the applying date is on 06 23rd, 2017, and invention and created name is
A kind of divisional application of the patent of " 3D printing consumptive material and preparation method thereof prepared by high level cycling and reutilization waste rubber ".
Technical field
The invention belongs to 3D printing consumptive material preparing technical fields, and in particular to a kind of high level cycling and reutilization waste rubber system
Standby 3D printing consumptive material and preparation method thereof.
Background technology
Rubber (Rubber):High elastic polymer material with reversible deformation.High resilience at room temperature, in very little
It can be generated under outer force effect compared with large deformation, remove resilient after external force.Rubber belongs to entirely without styling polymer, its glass
Glass transition temperature (Tg) is low, and molecular weight is often very big, is more than hundreds of thousands.
One word of rubber derives from Indian cau-uchu, means " tree to shed tears ".Natural rubber is exactly by Hevea rubber
The latex flowed out when tree rubber tapping is made after solidifying, drying.1770, Britain chemist J. Priestleys had found that rubber can
For wiping pencil writing, the material of this purposes was known as rubber at that time, this word is used till today always.The strand of rubber
It can be crosslinked, when the rubber after crosslinking is deformed by outer force effect, there is the ability restored rapidly, and there is good physics
Mechanical property and chemical stability.Rubber is the base stock of rubber industry, is widely used in manufacture tire, sebific duct, adhesive tape, cable
And other various rubber products.Rubber is divided into natural rubber and synthetic rubber by raw material.By form be divided into blocky raw rubber, latex,
Liquid rubber and powdered rubber.Latex is the colloidal aqueous dispersion of rubber;Liquid rubber is the oligomer of rubber, before unvulcanized
Generally sticky liquid;Powdered rubber be latex is processed into it is powdered, with sharp dispensing and processing and fabricating.The 1960s
The thermoplastic elastomer of exploitation is not necessarily to chemical cure, and the processing method for using thermoplastic shapes.Rubber by use be divided into for
Universal and two class of Special type.Insulator, it is not easy to it is conductive, but if get wet or different temperature if, it is possible to become
Conductor.Conduction is that the conduction of the electronics about substance interior molecules or ion is easy situation.
The Geim and Novoselov of Man Chesidun universities of Britain in 2004 remove high starch breeding by adhesive tape and obtain solely
Since vertical existing two-dimensional graphene (Gra-phene, GN) crystal, it is extremely concerned that graphene has become materials science field
One of research hotspot.Graphene, the actually graphite of monoatomic layer, it possesses unique two-dimensional structure and excellent power
, thermodynamics, optically and electrically performance.
It is also but most hard nano material that graphene, which is most thin in the world at present, it is almost fully transparent, to suction
2.3% light is received, thermal coefficient is up to 5300W/mk, is higher than carbon nanotube and diamond.Graphene is one kind by carbon atom
The new material of the individual layer laminated structure of composition has intensity height, large specific surface area, high chemical reactivity, the spy of high fillibility
Point.
With the fast development of auto industry, waste tire yield is more and more, and harm is increasing.The waste and old rubber in the whole world
Glue is increasing, and China is used as populous country in the world, and rubber-consumer amount is also giant.In the epoch for advocating low-carbon economy, regeneration
Glue comes into being.Meanwhile waste old belongs to industrial bazardous waste, it is to deteriorate natural environment, destroy vegetation growth, influence
Human health, most one of the Harmful Waste for jeopardizing ball ecological environment.Therefore, the rubber regeneration resource in China is made full use of, is delayed
Rubber sources shortage is solved, preserves the ecological environment, walks the Road of Cyclic Economy, there is far-reaching strategic importance for our countries.
3D printing is also known as rapid shaping technique, also referred to as increases material manufacturing technology, is that one kind not needing conventional tool, fixture
And lathe, but based on digital model file, using metal powder or plastics etc. there is the material of adhesion successively to print
To manufacture the technology of arbitrary shape article.There are many article that 3D printer can manufacture, such as aircraft, pistol, food, human body for another example
Organ, toy for children etc..3D printing technique is an important breakthrough of world's manufacturing technology field over the past two decades.It is mechanic
The multidisciplinary technology such as journey, computer technology, Numeric Control Technology, material science integrates.It is to beat that 3D printing, which is most difficult to most crucial technology,
Print the exploitation of material.Therefore the more various multi-functional 3D printing material of exploitation becomes hot spot and the pass of future studies and application
Key.
Existing 3d printing rubber material the problems such as there is anti-flammability and poor mechanical properties, how graphene to be filled to rubber
It is modified in glue, prints rubber material to obtain 3d of good performance, become a kind of research tendency.
Invention content
The technical problem to be solved in the present invention is to provide 3D printing consumptions prepared by a kind of high level cycling and reutilization waste rubber
The problems such as material and preparation method thereof, there is anti-flammability and poor mechanical properties to solve existing 3d printing rubber material.The present invention
The 3D printing consumptive material good flame retardation effect for preparing of high level cycling and reutilization waste rubber, strong shock resistance, toughness is strong, is a kind of
The excellent fire-retardant graphene modified rubber material of performance, can be applicable, there is significant economic and social benefit.
In order to solve the above technical problems, the present invention uses following technical scheme:A kind of discarded rubber of high level cycling and reutilization
3D printing consumptive material prepared by glue is made as unit of parts by weight of following raw material:156~208 parts of waste rubber, graphene 2~
4 parts, 42~60 parts of polylactic acid, 26~35 parts of potassium tripolyphosphate, 25~38 parts of makrolon, glycerine glycerinate 22~30
Part, 16~20 parts of stearyl acrylate acid esters, 8~14 parts of carbon fiber, 5~8 parts of Fypro, 3~5 parts of carboxyethyl cellulose,
Surfactant 0.8~1.4
Part, 0.4~0.8 part of crosslinking agent, 0.3~0.4 part of catalyst, 0.5~0.8 part of plasticizer, dispersant 0.3~0.6
It is part, 0.3~0.5 part of tackifier, 0.9~1.5 part of curing agent, 0.3~0.5 part of antioxidant, 0.2~0.3 part of heat stabilizer, anti-ageing
0.7~1.3 part of agent, 1.5~2 parts of fire retardant, 0.6~1 part of smoke suppressant;The surfactant is PULLRONIC F68
Copolymer;The crosslinking agent is crosslinking aid S AC-100;The fire retardant is as unit of parts by weight, including following raw material:Ethylene glycol
72~90 parts of ethyl ether acetate ester, 26~30 parts of nonylphenol polyoxyethylene ether ammonium sulfate, gathers 35~42 parts of Miglyol 812N
23~28 parts of propylene oxide triol, 17~20 parts of urea, 13~15 parts of aluminium hydroxide, 14~16 parts of antimony oxide, manganese oxide
10~14 parts, 13~15 parts of diatomite, 2~3 parts of bleeding agent;The preparation method of the fire retardant, includes the following steps:(a) will
Nonylphenol polyoxyethylene ether ammonium sulfate, 350~420 parts of water are added in microwave reactor, are 300~500r/min in speed of agitator
Mixture A is made in 8~12min of lower stirring;(b) ethylene glycol ether acetate, octanoic acid are added into mixture A made from step a
Triglyceride DDD, polypropylene oxide triol, urea, aluminium hydroxide, antimony oxide, manganese oxide, diatomite, bleeding agent,
Speed of agitator is 200~400r/min, and microwave power is 300~350W, and temperature is that 1.5~2h is stirred at 90~95 DEG C, is made
Mixture B, the bleeding agent are penetrating agent JFC;(c) after being cooled to room temperature mixture B made from step b, by sediment mistake
Filter, in the case where rotating speed is 4000~5000r/min, fire retardant is made to water content≤1.2% in centrifugal drying;The smoke suppressant is with weight
Amount part is unit, including following raw material:45~60 parts of tributyltin oxide, 22~25 parts of molybdenum hydroxide, atlapulgite 17~22
Part, 13~16 parts of aluminium hydroxide, 8~10 parts of ammonium octamolybdate, 2.2~2.6 parts of stearic acid;The preparation method of the smoke suppressant, packet
Include following steps:(A) tributyltin oxide, molybdenum hydroxide, atlapulgite, aluminium hydroxide, ammonium octamolybdate, stearic acid are mixed,
It is 300~400r/min in speed of agitator, microwave power is 160~180W, and temperature is that 1.5~2h is stirred at 112~120 DEG C,
Mixture C is made;(B) after being cooled to room temperature mixture C made from step A, sediment is filtered, rotating speed be 4000~
Smoke suppressant is made to water content≤1.2% in centrifugal drying under 5000r/min.
The catalyst is vanadic anhydride.
Preferably, the plasticizer is citrate.
Preferably, the dispersant is dispersant 5040.
Preferably, the tackifier are butyl trimethoxy silane.
Preferably, the curing agent is epoxylite curing agent.
Preferably, the antioxidant is antioxidant 1076.
Preferably, the heat stabilizer is Dythal.
Preferably, the antiager is BASF UV-234 antiagers.
The present invention also provides a kind of preparation methods of 3D printing consumptive material prepared by high level cycling and reutilization waste rubber, including
Following steps:S1:It is dried to water content≤1% after waste rubber is cleaned, then smashes it through 200~300 mesh sieve, is made
Rubber powder;S2:Surfactant is added into rubber powder made from step S1, is 75~78 DEG C in temperature, rotating speed 180
1~1.5h is activated under~200r/min, and activating rubber powder end is made;S3:Graphene is crushed, 200~300 mesh sieve, system are crossed
Powder is obtained, gained powder is 6500~7500GS in magnetic field intensity, and ultrasonic power is 500~600W, and temperature is 55~58 DEG C,
Rotating speed is to stir 40~50min under 200~300r/min, and graphene energy powder is made;S4:Under nitrogen protection, to step
Graphene energy powder, polylactic acid, potassium tripolyphosphate, poly- carbonic acid made from step S3 are added in activating rubber powder end made from S2
Ester, glycerine glycerinate, stearyl acrylate acid esters, carbon fiber, Fypro, carboxyethyl cellulose, surfactant,
Crosslinking agent, catalyst, plasticizer, dispersant, tackifier are 265~272W in microwave power, and temperature is 136~142 DEG C, is turned
Speed is that 3~4h is stirred under 200~400r/min, and mixture I is made;S5:Solidification is added into mixture I made from step S4
Agent, antioxidant, heat stabilizer, antiager, fire retardant, smoke suppressant are 76~80 DEG C in temperature, and rotating speed is 100~200r/min
Mixture II is made in 1.5~2h of lower stirring;S6:Mixture II made from step S5 is put into screw extruding molding machine, in temperature
Degree is 192~205 DEG C, and rotating speed is, through squeezing strand, high level cycling and reutilization waste rubber system to be made under 110~120r/min
Standby 3D printing consumptive material.
Part material Action Specification:(1) polylactic acid has most good tensile strength and extensibility, and polylactic acid can also be each
Kind common process mode produces, such as:Extrusion molding, ejection formation, blowfilm shaping, foaming and vacuum forming are melted, with
Used polymer has similar molding condition extensively at present, it also has printing performance identical with conventional films in addition.
In this way, polylactic acid can answer the demand of variant industry, miscellaneous application product is made.
(2) potassium tripolyphosphate is usually used in material, the effects that playing quality improver, pH adjusting agent, metal-chelator.
(3) glycerine glycerinate can make lubricant, plasticiser, gelling agent, have hydrophilic and oleophylic double grading concurrently,
And have the characteristics that high temperature resistant, acidproof, and it is nontoxic, the industries such as 3d printings can be used safely in.
The invention has the advantages that:(1) fire-retardant graphene modified rubber material of the invention has high flame retardant
Energy and smoke suppressing effect, will not discharge poisonous and harmful substance, avoid the secondary injury to human body at high temperature.
(2) 3D printing consumptive material good flame retardation effect prepared by high level cycling and reutilization waste rubber of the invention, shock resistance energy
Power is strong, and toughness is strong, is a kind of excellent fire-retardant graphene modified rubber material of performance;In addition, by experimental comparison, polylactic acid, three
PA 800K, glycerine glycerinate play collaboration correlation in the present invention, anti-flammability, drawing to product of the present invention
Intensity, impact strength etc. is stretched to play the role of being obviously promoted.
(3) surfactant activation process is added after crushing waste rubber, is conducive to that it is compatible with other raw materials, carries
High syncretizing effect improves tensile strength, impact strength etc.;And there is no be added after first crushing waste rubber in the prior art
The step of surfactant activation process, but directly merged with other material compositions after directly crushing waste rubber and prepare 3D
Printing consumables, the performances such as the tensile strength being achieved in that, impact strength are poor.
Specific implementation mode
It for ease of more fully understanding the present invention, is illustrated by following embodiment, these embodiments belong to the present invention's
Protection domain, but do not limit the scope of the invention.
In embodiment, the 3D printing consumptive material that prepared by the high level cycling and reutilization waste rubber, as unit of parts by weight,
It is made of following raw material:156~208 parts of waste rubber, 2~4 parts of graphene, 42~60 parts of polylactic acid, potassium tripolyphosphate 26~
35 parts, 25~38 parts of makrolon, 22~30 parts of glycerine glycerinate, 16~20 parts of stearyl acrylate acid esters, carbon fiber 8
~14 parts, 5~8 parts of Fypro, 3~5 parts of carboxyethyl cellulose, 0.8~1.4 part of surfactant, crosslinking agent 0.4~
0.8 part, it is 0.3~0.4 part of catalyst, 0.5~0.8 part of plasticizer, 0.3~0.6 part of dispersant, 0.3~0.5 part of tackifier, solid
0.9~1.5 part of agent, 0.3~0.5 part of antioxidant, 0.2~0.3 part of heat stabilizer, 0.7~1.3 part of antiager, fire retardant 1.5
~2 parts, 0.6~1 part of smoke suppressant;The surfactant is Pluronic F68;The crosslinking agent is crosslinking
Agent SAC-100;The catalyst is vanadic anhydride;The plasticizer is citrate;The dispersant is dispersant 5040;
The tackifier are butyl trimethoxy silane;The curing agent is epoxylite curing agent;The antioxidant is antioxidant
1076;The heat stabilizer is Dythal;The antiager is BASF UV-234 antiagers;It is described fire-retardant
Agent is as unit of parts by weight, including following raw material:72~90 parts of ethylene glycol ether acetate, Miglyol 812N 35~42
Part, 26~30 parts of nonylphenol polyoxyethylene ether ammonium sulfate, 23~28 parts of polypropylene oxide triol, 17~20 parts of urea, hydroxide
13~15 parts of aluminium, 14~16 parts of antimony oxide, 10~14 parts of manganese oxide, 13~15 parts of diatomite, 2~3 parts of bleeding agent;It is described
Smoke suppressant is as unit of parts by weight, including following raw material:45~60 parts of tributyltin oxide, 22~25 parts of molybdenum hydroxide, activity
17~22 parts of carclazyte, 13~16 parts of aluminium hydroxide, 8~10 parts of ammonium octamolybdate, 2.2~2.6 parts of stearic acid;The high level cycle is again
Using the preparation method of 3D printing consumptive material prepared by waste rubber, include the following steps:S1:It is dried to after waste rubber is cleaned
Water content≤1% then smashes it through 200~300 mesh sieve, and rubber powder is made;S2:To rubber powder made from step S1
Middle addition surfactant is 75~78 DEG C in temperature, and rotating speed is that 1~1.5h is activated under 180~200r/min, and activation rubber is made
Rubber powder end;S3:Graphene is crushed, cross 200~300 mesh sieve, be made powder, gained powder magnetic field intensity be 6500~
7500GS, ultrasonic power be 500~600W, temperature be 55~58 DEG C, rotating speed be 200~300r/min under, stirring 40~
Graphene energy powder is made in 50min;S4:Under nitrogen protection, step is added into activating rubber powder end made from step S2
Graphene energy powder, polylactic acid, potassium tripolyphosphate, makrolon, glycerine glycerinate, stearyl acrylate made from S3
Acid esters, carbon fiber, Fypro, carboxyethyl cellulose, surfactant, crosslinking agent, catalyst, plasticizer, dispersant, increasing
Stick is 265~272W in microwave power, and temperature is 136~142 DEG C, and rotating speed is that 3~4h is stirred under 200~400r/min, system
Obtain mixture I;S5:Into mixture I made from step S4 be added curing agent, antioxidant, heat stabilizer, antiager, fire retardant,
Smoke suppressant is 76~80 DEG C in temperature, and rotating speed is that 1.5~2h is stirred under 100~200r/min, and mixture II is made;The resistance
The preparation method for firing agent, includes the following steps:(a) by 350~420 parts of nonylphenol polyoxyethylene ether ammonium sulfate, water addition microwaves
In reactor, 8~12min is stirred in the case where speed of agitator is 300~500r/min, mixture A is made;(b) to made from step a
In mixture A be added ethylene glycol ether acetate, Miglyol 812N, polypropylene oxide triol, urea, aluminium hydroxide,
Antimony oxide, manganese oxide, diatomite, bleeding agent, speed of agitator be 200~400r/min, microwave power be 300~
350W, temperature are that 1.5~2h is stirred at 90~95 DEG C, and mixture B is made, and the bleeding agent is penetrating agent JFC;(c) by step b
After mixture B obtained is cooled to room temperature, sediment is filtered, in the case where rotating speed is 4000~5000r/min, centrifugal drying is to containing
Fire retardant is made in water≤1.2%;The preparation method of the smoke suppressant, includes the following steps:(A) by tributyltin oxide, hydrogen
Molybdenum oxide, atlapulgite, aluminium hydroxide, ammonium octamolybdate, stearic acid mixing are 300~400r/min, microwave work(in speed of agitator
Rate is 160~180W, and temperature is that 1.5~2h is stirred at 112~120 DEG C, and mixture C is made;(B) it will be mixed made from step A
After object C is cooled to room temperature, sediment is filtered, rotating speed be 4000~5000r/min under centrifugal drying to water content≤
1.2%, smoke suppressant is made;S6:Mixture II made from step S5 is put into screw extruding molding machine, temperature be 192~
205 DEG C, rotating speed is, through squeezing strand, 3D printing prepared by high level cycling and reutilization waste rubber to be made under 110~120r/min
Consumptive material.
Below by more specifically examples illustrate the present invention.
Embodiment 1
A kind of 3D printing consumptive material prepared by high level cycling and reutilization waste rubber, as unit of parts by weight, by following raw material
It is made:182 parts of waste rubber, 3 parts of graphene, 55 parts of polylactic acid, 32 parts of potassium tripolyphosphate, 33 parts of makrolon, glycerine three
26 parts of monoglyceride, 18 parts of stearyl acrylate acid esters, 12 parts of carbon fiber, 6 parts of Fypro, 4 parts of carboxyethyl cellulose, surface
1.2 parts of activating agent, 0.6 part of crosslinking agent, 0.3 part of catalyst, 0.6 part of plasticizer, 0.5 part of dispersant, 0.4 part of tackifier, solidification
1.2 parts of agent, 0.4 part of antioxidant, 0.2 part of heat stabilizer, 1 part of antiager, 1.8 parts of fire retardant, 0.9 part of smoke suppressant;The surface
Activating agent is Pluronic F68;The crosslinking agent is crosslinking aid S AC-100;The catalyst is five oxidations
Two vanadium;The plasticizer is citrate;The dispersant is dispersant 5040;The tackifier are butyl trimethoxy silicon
Alkane;The curing agent is epoxylite curing agent;The antioxidant is antioxidant 1076;The heat stabilizer is that dibasic is adjacent
Phthalic acid lead;The antiager is BASF UV-234 antiagers;The fire retardant is as unit of parts by weight, including following original
Material:82 parts of ethylene glycol ether acetate, 38 parts of Miglyol 812N, 28 parts of nonylphenol polyoxyethylene ether ammonium sulfate, polyoxy
Change 25 parts of propylene triol, 190 parts of urea, 14 parts of aluminium hydroxide, 15 parts of antimony oxide, 12 parts of manganese oxide, 14 parts of diatomite, ooze
Saturating 2.5 parts of agent;The smoke suppressant is as unit of parts by weight, including following raw material:55 parts of tributyltin oxide, molybdenum hydroxide 23
Part, 19 parts of atlapulgite, 15 parts of aluminium hydroxide, 9 parts of ammonium octamolybdate, 2.5 parts of stearic acid;The high level cycling and reutilization discards rubber
The preparation method of 3D printing consumptive material prepared by glue, includes the following steps:S1:Water content is dried to after waste rubber is cleaned is
1%, 200 mesh sieve are then smashed it through, rubber powder is made;S2:Surface is added into rubber powder made from step S1 to live
Property agent, temperature be 76 DEG C, rotating speed be 190r/min under activate 1.3h, be made activating rubber powder end;S3:Graphene is crushed,
200 mesh sieve to be crossed, powder is made, gained powder is 7000GS in magnetic field intensity, and ultrasonic power 550W, temperature is 56 DEG C,
Rotating speed is to stir 45min under 200r/min, and graphene energy powder is made;S4:Under nitrogen protection, to made from step S2
Graphene energy powder made from step S3, polylactic acid, potassium tripolyphosphate, makrolon, the third three are added in activating rubber powder end
Alcohol glycerinate, stearyl acrylate acid esters, carbon fiber, Fypro, carboxyethyl cellulose, surfactant, crosslinking agent,
Catalyst, plasticizer, dispersant, tackifier are 270W in microwave power, and temperature is 140 DEG C, and rotating speed is to be stirred under 300r/min
Mixture I is made in 3.5h;S5:Into mixture I made from step S4 be added curing agent, antioxidant, heat stabilizer, antiager,
Fire retardant, smoke suppressant are 78 DEG C in temperature, and rotating speed is to stir 1.8h under 150r/min, and mixture II is made;The fire retardant
Preparation method includes the following steps:(a) nonylphenol polyoxyethylene ether ammonium sulfate, 380 parts of water are added in microwave reactor,
Speed of agitator is to stir 10min under 400r/min, and mixture A is made;
(b) ethylene glycol ether acetate, Miglyol 812N, polyoxygenated are added into mixture A made from step a
Propylene triol, urea, aluminium hydroxide, antimony oxide, manganese oxide, diatomite, bleeding agent are 300r/min in speed of agitator,
Microwave power is 320W, and temperature is to stir 1.8h at 92 DEG C, and mixture B is made, and the bleeding agent is penetrating agent JFC;It (c) will step
After mixture B made from rapid b is cooled to room temperature, sediment is filtered, is centrifugal drying under 4500r/min to water content in rotating speed
It is 1.2%, fire retardant is made;The preparation method of the smoke suppressant, includes the following steps:(A) by tributyltin oxide, hydroxide
Molybdenum, atlapulgite, aluminium hydroxide, ammonium octamolybdate, stearic acid mixing, speed of agitator be 360r/min, microwave power 170W,
Temperature is to stir 1.8h at 118 DEG C, and mixture C is made;(B) it after being cooled to room temperature mixture C made from step A, will precipitate
Object filters, and in the case where rotating speed is 450r/min, centrifugal drying to water content is 1.2%, and smoke suppressant is made;S6:Made from step S5
Mixture II is put into screw extruding molding machine, is 200 DEG C in temperature, and rotating speed is, through squeezing strand, height to be made under 110r/min
It is worth 3D printing consumptive material prepared by cycling and reutilization waste rubber.
Embodiment 2
A kind of 3D printing consumptive material prepared by high level cycling and reutilization waste rubber, as unit of parts by weight, by following raw material
It is made:158 parts of waste rubber, 2 parts of graphene, 44 parts of polylactic acid, 26 parts of potassium tripolyphosphate, 25 parts of makrolon, glycerine three
22 parts of monoglyceride, 16 parts of stearyl acrylate acid esters, 8 parts of carbon fiber, 5 parts of Fypro, 3 parts of carboxyethyl cellulose, surface
0.8 part of activating agent, 0.4 part of crosslinking agent, 0.3 part of catalyst, 0.5 part of plasticizer, 0.3 part of dispersant, 0.3 part of tackifier, solidification
0.9 part of agent, 0.3 part of antioxidant, 0.2 part of heat stabilizer, 0.7 part of antiager, 1.5 parts of fire retardant, 0.6 part of smoke suppressant;The table
Face activating agent is Pluronic F68;The crosslinking agent is crosslinking aid S AC-100;The catalyst is five oxygen
Change two vanadium;The plasticizer is citrate;The dispersant is dispersant 5040;The tackifier are butyl trimethoxy silicon
Alkane;The curing agent is epoxylite curing agent;The antioxidant is antioxidant 1076;The heat stabilizer is that dibasic is adjacent
Phthalic acid lead;The antiager is BASF UV-234 antiagers;The fire retardant is as unit of parts by weight, including following original
Material:72 parts of ethylene glycol ether acetate, 35 parts of Miglyol 812N, 26 parts of nonylphenol polyoxyethylene ether ammonium sulfate, polyoxy
Change 23 parts of propylene triol, 17 parts of urea, 13 parts of aluminium hydroxide, 14 parts of antimony oxide, 10 parts of manganese oxide, 13 parts of diatomite, ooze
Saturating 2 parts of agent;The smoke suppressant is as unit of parts by weight, including following raw material:45 parts of tributyltin oxide, 22 parts of molybdenum hydroxide,
17 parts of atlapulgite, 13 parts of aluminium hydroxide, 8 parts of ammonium octamolybdate, 2.2 parts of stearic acid;The high level cycling and reutilization waste rubber
The preparation method of the 3D printing consumptive material of preparation, includes the following steps:S1:Water content is dried to after waste rubber is cleaned is
0.8%, 200 mesh sieve are then smashed it through, rubber powder is made;S2:Surface is added into rubber powder made from step S1
Activating agent is 75 DEG C in temperature, and rotating speed is to activate 1.5h under 180r/min, and activating rubber powder end is made;S3:By Graphene powder
It is broken, 200 mesh sieve are crossed, powder is made, gained powder is 6500GS, ultrasonic power 500W, temperature 55 in magnetic field intensity
DEG C, rotating speed is to stir 50min under 200r/min, and graphene energy powder is made;S4:Under nitrogen protection, it is made to step S2
Activating rubber powder end in graphene energy powder, polylactic acid, potassium tripolyphosphate, makrolon, third made from step S3 is added
Triol glycerinate, stearyl acrylate acid esters, carbon fiber, Fypro, carboxyethyl cellulose, surfactant, crosslinking
Agent, catalyst, plasticizer, dispersant, tackifier are 265W in microwave power, and temperature is 136 DEG C, and rotating speed is under 200r/min
4h is stirred, mixture I is made;S5:Curing agent, antioxidant, heat stabilizer, anti-ageing is added into mixture I made from step S4
Agent, fire retardant, smoke suppressant are 76 DEG C in temperature, and rotating speed is to stir 2h under 100r/min, and mixture II is made;The fire retardant
Preparation method, include the following steps:(a) nonylphenol polyoxyethylene ether ammonium sulfate, 350 parts of water are added in microwave reactor,
12min is stirred in the case where speed of agitator is 300r/min, mixture A is made;(b) second two is added into mixture A made from step a
Alcohol ethyl ether acetate ester, Miglyol 812N, polypropylene oxide triol, urea, aluminium hydroxide, antimony oxide, manganese oxide,
Diatomite, bleeding agent are 200r/min in speed of agitator, and microwave power 300W, temperature is to stir 2h at 90 DEG C, and mixing is made
Object B, the bleeding agent are penetrating agent JFC;(c) after being cooled to room temperature mixture B made from step b, sediment is filtered,
Rotating speed is that centrifugal drying to water content is 1% under 4000r/min, and fire retardant is made;The preparation method of the smoke suppressant, including with
Lower step:(A) tributyltin oxide, molybdenum hydroxide, atlapulgite, aluminium hydroxide, ammonium octamolybdate, stearic acid are mixed, is being stirred
Mix rotating speed is 300r/min, and microwave power 160W, temperature is to stir 2h at 112 DEG C, and mixture C is made;(B) by step A systems
After the mixture C obtained is cooled to room temperature, sediment is filtered, in the case where rotating speed is 4000r/min, centrifugal drying to water content is
1%, smoke suppressant is made;S6:Mixture II made from step S5 is put into screw extruding molding machine, is 192 DEG C in temperature, turns
Speed is, through squeezing strand, 3D printing consumptive material prepared by high level cycling and reutilization waste rubber to be made under 1100r/min.
Embodiment 3
A kind of 3D printing consumptive material prepared by high level cycling and reutilization waste rubber, as unit of parts by weight, by following raw material
It is made:205 parts of waste rubber, 4 parts of graphene, 60 parts of polylactic acid, 35 parts of potassium tripolyphosphate, 38 parts of makrolon, glycerine three
30 parts of monoglyceride, 20 parts of stearyl acrylate acid esters, 14 parts of carbon fiber, 8 parts of Fypro, 5 parts of carboxyethyl cellulose, surface
1.4 parts of activating agent, 0.8 part of crosslinking agent, 0.4 part of catalyst, 0.8 part of plasticizer, 0.6 part of dispersant, 0.5 part of tackifier, solidification
1.5 parts of agent, 0.5 part of antioxidant, 0.3 part of heat stabilizer, 1.3 parts of antiager, 2 parts of fire retardant, 1 part of smoke suppressant;It lives on the surface
Property agent be Pluronic F68;The crosslinking agent is crosslinking aid S AC-100;The catalyst is five oxidations two
Vanadium;The plasticizer is citrate;The dispersant is dispersant 5040;The tackifier are butyl trimethoxy silane;
The curing agent is epoxylite curing agent;The antioxidant is antioxidant 1076;The heat stabilizer is dibasic neighbour's benzene
Diformazan lead plumbate;The antiager is BASF UV-234 antiagers;The fire retardant is as unit of parts by weight, including following original
Material:90 parts of ethylene glycol ether acetate, 42 parts of Miglyol 812N, 30 parts of nonylphenol polyoxyethylene ether ammonium sulfate, polyoxy
Change 28 parts of propylene triol, 20 parts of urea, 15 parts of aluminium hydroxide, 16 parts of antimony oxide, 14 parts of manganese oxide, 15 parts of diatomite, ooze
Saturating 3 parts of agent;The smoke suppressant is as unit of parts by weight, including following raw material:60 parts of tributyltin oxide, 25 parts of molybdenum hydroxide,
22 parts of atlapulgite, 16 parts of aluminium hydroxide, 10 parts of ammonium octamolybdate, 2.6 parts of stearic acid;The high level cycling and reutilization waste rubber
The preparation method of the 3D printing consumptive material of preparation, includes the following steps:S1:Water content is dried to after waste rubber is cleaned is
0.6%, 300 mesh sieve are then smashed it through, rubber powder is made;S2:Surface is added into rubber powder made from step S1
Activating agent is 78 DEG C in temperature, and rotating speed is to activate 1.5h under 200r/min, and activating rubber powder end is made;S3:By Graphene powder
It is broken, 300 mesh sieve are crossed, powder is made, gained powder is 7500GS, ultrasonic power 600W, temperature 58 in magnetic field intensity
DEG C, rotating speed is to stir 40min under 300r/min, and graphene energy powder is made;S4:Under nitrogen protection, it is made to step S2
Activating rubber powder end in graphene energy powder, polylactic acid, potassium tripolyphosphate, makrolon, third made from step S3 is added
Triol glycerinate, stearyl acrylate acid esters, carbon fiber, Fypro, carboxyethyl cellulose, surfactant, crosslinking
Agent, catalyst, plasticizer, dispersant, tackifier are 272W in microwave power, and temperature is 142 DEG C, and rotating speed is under 400r/min
3h is stirred, mixture I is made;S5:Curing agent, antioxidant, heat stabilizer, anti-ageing is added into mixture I made from step S4
Agent, fire retardant, smoke suppressant are 80 DEG C in temperature, and rotating speed is to stir 1.5h under 200r/min, and mixture II is made;It is described fire-retardant
The preparation method of agent, includes the following steps:(a) by 420 parts of nonylphenol polyoxyethylene ether ammonium sulfate, water addition microwave reactors
In, 8min is stirred in the case where speed of agitator is 500r/min, mixture A is made;(b) second is added into mixture A made from step a
Glycol ether acetate, Miglyol 812N, polypropylene oxide triol, urea, aluminium hydroxide, antimony oxide, oxidation
Manganese, diatomite, bleeding agent are 400r/min in speed of agitator, and microwave power 350W, temperature is to stir 1.5h at 95 DEG C, is made
Mixture B is obtained, the bleeding agent is penetrating agent JFC;(c) after being cooled to room temperature mixture B made from step b, by sediment
Filtering, in the case where rotating speed is 5000r/min, centrifugal drying to water content is 0.8%, and fire retardant is made;The preparation side of the smoke suppressant
Method includes the following steps:(A) by tributyltin oxide, molybdenum hydroxide, atlapulgite, aluminium hydroxide, ammonium octamolybdate, stearic acid
Mixing is 400r/min in speed of agitator, and microwave power 180W, temperature is to stir 1.5h at 120 DEG C, and mixture C is made;
(B) after being cooled to room temperature mixture C made from step A, sediment is filtered, the centrifugal drying in the case where rotating speed is 5000r/min
It is 1% to water content, smoke suppressant is made;S6:Mixture II made from step S5 is put into screw extruding molding machine, in temperature
It it is 205 DEG C, rotating speed is, through squeezing strand, 3D printing consumption prepared by high level cycling and reutilization waste rubber to be made under 120r/min
Material.
Comparative example 1
It prepares raw material and preparation method is substantially the same manner as Example 3, difference is that comparative example 1 is added to polylactic acid less
60 parts.
Comparative example 2
It prepares raw material and preparation method is substantially the same manner as Example 3, difference is that comparative example 2 is added to trimerization phosphorus less
35 parts of sour potassium.
Comparative example 3
It prepares raw material and preparation method is substantially the same manner as Example 3, difference is that comparative example 3 is added to glycerine less
30 parts of glycerinate.
Comparative example 4
It prepares raw material and preparation method is substantially the same manner as Example 3, difference is that comparative example 4 is added to polylactic acid less
60 parts, 35 parts of potassium tripolyphosphate, 30 parts of glycerine glycerinate.
Comparative example 5
It prepares raw material and preparation method is substantially the same manner as Example 3, difference is that 5 raw material of comparative example is added to table less
1.4 parts of face activating agent;Preparation method has lacked the activation process of step S2.
3D printing consumptive material warp prepared by high level cycling and reutilization waste rubber prepared by the present embodiment 1-3 and comparative example 1-4
Detection, performance are as shown in the table:
As seen from the above table, the 3D printing consumptive material good flame retardation effect that prepared by high level cycling and reutilization waste rubber of the invention,
Strong shock resistance, toughness is strong, is a kind of excellent fire-retardant graphene modified rubber material of performance;By experimental comparison, polylactic acid,
Potassium tripolyphosphate, glycerine glycerinate play collaboration correlation in the present invention, to anti-flammability, tensile strength, resist
Impact strength etc. plays the role of being obviously promoted;Surfactant activation process is added after waste rubber is crushed, is conducive to
It is compatible with other raw materials, improves syncretizing effect, improves tensile strength, impact strength etc.;And after waste rubber is crushed
It is directly merged with other material compositions and prepares 3D printing consumptive material, the performances such as the tensile strength being achieved in that, impact strength are poor.
The specific implementation of the invention is not to be limited to these illustrations for the above content, and technology belonging to the present invention is led
For the those of ordinary skill in domain, without departing from the inventive concept of the premise, a number of simple deductions or replacements can also be made,
It all shall be regarded as belonging to present invention scope of patent protection determined by the appended claims.
Claims (8)
1. a kind of fire retardant, which is characterized in that the fire retardant is as unit of parts by weight, including following raw material:Ethylene glycol ethyl ether
72~90 parts of acetate, 35~42 parts of Miglyol 812N, 26~30 parts of nonylphenol polyoxyethylene ether ammonium sulfate, polyoxygenated
23~28 parts of propylene triol, 17~20 parts of urea, 13~15 parts of aluminium hydroxide, 14~16 parts of antimony oxide, manganese oxide 10~
14 parts, 13~15 parts of diatomite, 2~3 parts of bleeding agent.
2. fire retardant according to claim 1, which is characterized in that the flame retardant component is:Ethylene glycol ether acetate
82 parts, 38 parts of Miglyol 812N, 28 parts of nonylphenol polyoxyethylene ether ammonium sulfate, 25 parts of polypropylene oxide triol, urea
190 parts, 14 parts of aluminium hydroxide, 15 parts of antimony oxide, 12 parts of manganese oxide, 14 parts of diatomite, 2.5 parts of bleeding agent.
3. fire retardant according to claim 1, which is characterized in that the flame retardant component is:Ethylene glycol ether acetate
72 parts, 35 parts of Miglyol 812N, 26 parts of nonylphenol polyoxyethylene ether ammonium sulfate, 23 parts of polypropylene oxide triol, urea
17 parts, 13 parts of aluminium hydroxide, 14 parts of antimony oxide, 10 parts of manganese oxide, 13 parts of diatomite, 2 parts of bleeding agent.
4. fire retardant according to claim 1, which is characterized in that the flame retardant component is:Ethylene glycol ether acetate
90 parts, 42 parts of Miglyol 812N, 30 parts of nonylphenol polyoxyethylene ether ammonium sulfate, 28 parts of polypropylene oxide triol, urea
20 parts, 15 parts of aluminium hydroxide, 16 parts of antimony oxide, 14 parts of manganese oxide, 15 parts of diatomite, 3 parts of bleeding agent.
5. a kind of preparation method of fire retardant is used to prepare claim 1-4 any one of them fire retardants, which is characterized in that
The preparation method of the fire retardant, includes the following steps:
(a) nonylphenol polyoxyethylene ether ammonium sulfate, 350~420 parts of water are added in microwave reactor, are 300 in speed of agitator
8~12min is stirred under~500r/min, and mixture A is made;
(b) ethylene glycol ether acetate, Miglyol 812N, polypropylene oxide are added into mixture A made from step a
Triol, urea, aluminium hydroxide, antimony oxide, manganese oxide, diatomite, bleeding agent are 200~400r/min in speed of agitator,
Microwave power is 300~350W, and temperature is that 1.5~2h is stirred at 90~95 DEG C, and mixture B is made, and the bleeding agent is infiltration
Agent JFC;
(c) after being cooled to room temperature mixture B made from step b, sediment is filtered, is 4000~5000r/min in rotating speed
Fire retardant is made to water content≤1.2% in lower centrifugal drying.
6. the preparation method of fire retardant according to claim 5, which is characterized in that the water in (a) step is 380 parts, is stirred
Mix rotating speed is 400r/min, mixing time 10min, and (b) speed of agitator in step is 300r/min, and microwave power is
320W, temperature are 92 DEG C, mixing time 1.8h, and (c) rotating speed in step is 4500r/min, and centrifugal drying to water content is
1.2%.
7. the preparation method of fire retardant according to claim 5, which is characterized in that the water in (a) step is 350 parts, is stirred
Mix rotating speed is 300r/min, mixing time 12min, and (b) speed of agitator in step is 200r/min, and microwave power is
300W, temperature are 90 DEG C, mixing time 2h, and (c) rotating speed in step is 4000r/min, and centrifugal drying to water content is
1%.
8. the preparation method of fire retardant according to claim 5, which is characterized in that the water in (a) step is 420 parts, is stirred
Mix rotating speed is 500r/min, mixing time 8min, and (b) speed of agitator in step is 400r/min, microwave power 350W,
Temperature is 95 DEG C, mixing time 1.5h, and (c) rotating speed in step is 5000r/min, and centrifugal drying to water content is 0.8%.
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Application publication date: 20181023 |