CN106046417A - Surface-coating type composite inorganic flame retardant, preparation method thereof and application of surface-coating type composite inorganic flame retardant to cable material - Google Patents
Surface-coating type composite inorganic flame retardant, preparation method thereof and application of surface-coating type composite inorganic flame retardant to cable material Download PDFInfo
- Publication number
- CN106046417A CN106046417A CN201610420806.5A CN201610420806A CN106046417A CN 106046417 A CN106046417 A CN 106046417A CN 201610420806 A CN201610420806 A CN 201610420806A CN 106046417 A CN106046417 A CN 106046417A
- Authority
- CN
- China
- Prior art keywords
- powder
- parts
- type composite
- fire retardant
- composite inorganic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/10—Metal compounds
- C08K3/14—Carbides
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
- H01B3/448—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from other vinyl compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
- H01B7/29—Protection against damage caused by extremes of temperature or by flame
- H01B7/295—Protection against damage caused by extremes of temperature or by flame using material resistant to flame
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2244—Oxides; Hydroxides of metals of zirconium
-
- 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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
Abstract
The invention relates to surface-coating type composite inorganic flame retardant and a preparation method thereof and belongs to the technical field of flame retardant. The flame retardant comprises, by weight, 20-40 parts of Al(OH)3-Zr(OH)2-Ti3C2 composite powder, 10-20 parts of aluminum hydroxide powder, 10-20 parts of magnesium hydroxide powder, 1-3 parts of cationic surfactant, 1-3 parts of anionic surfactant, 2-4 parts of coupling agent and 5-10 parts of water. The inorganic flame retardant is good in flame retarding effect and good in dispersity when being mixed with polymer.
Description
Technical field
The present invention relates to a kind of surface cladding type composite inorganic fire retardant, preparation method, belong to technical field of flame retardant.
Background technology
Fire retardant is one of important auxiliary agent of synthesis macromolecular material, adds fire retardant and macromolecular material is carried out fire-retardant place
Reason, can stop material combustion or delay spreading of the intensity of a fire, making synthetic material have flame retardancy, self-extinguishment and smoke elimination.With
Synthetic material be widely applied to and produce and live in closely-related all conglomeraties, such as building industry, plastic product industry, spin
Knitting industry, transport service, electronic apparatus industry, aerospace industry, the importance of fire retardant can not be ignored further.The progress of modern science and technology and generation
To safety and the attention of environmental conservation in the range of boundary, make people the highest to the flame-retardancy requirements of material, promote fire retardant
Development, production and popularization and application are developed rapidly, and the kind of fire retardant increases increasingly, yield steeply rises.At present, according to roughly
Estimating, the 65-70% of whole world fire retardant is for flame retardant plastics, and 20% is used for rubber, and 5% is used for textile, and 3% is used for coating, and 2% uses
In paper and timber.In recent years, day by day improving and the quick growth of plastics yield, whole world fire retardant along with fire safety standard
Consumption constantly increase.According to chemical composition, fire retardant can be divided into inorganic combustion inhibitor and organic fire-retardant, and inorganic combustion inhibitor is closing
Become in material, in addition to having flame retardant effect, also have the effect that suppression is fuming and hydrogen chloride generates, and give material non-toxic,
Non-corrosiveness and the advantage such as cheap.External industrially developed country inorganic combustion inhibitor consumption figure is significantly larger than organic fire-retardant,
As the consumption of industrially developed country's area inorganic combustion inhibitors such as the U.S., West Europe and Japan accounts for aggregate consumption about 60%, and China less than
10%, therefore the inorganic fire-retarded chaste tree of China's development is the most urgent, and has a high potential.Inorganic combustion inhibitor principal item has hydrogen-oxygen at present
Change aluminum, magnesium hydroxide, Phos, borate, stibium oxide etc..
Substantial amounts of water vapour, substantial amounts of water vapour energy accumulation of heat and dilution can be discharged during aluminum-magnesium series fire retardant decomposes
The concentration of polymer fuel gas, also can form noninflammability barrier between combustible source and host material thus reach fire-retardant mesh
's.It is also a kind of smoke suppressant simultaneously, because the gas discharged is steam, harmless to biology, corrosion-free to metal.So
Aluminum-magnesium series fire retardant is that having in plastic industry of generally acknowledging at present is fire-retardant, press down cigarette, the organic polymer of filling triple functions helps
Agent, is the organic polymer preferred material that realizes halogen-free flameproof.
Open a kind of inorganic combustion inhibitor of CN103450502A and preparation method thereof, be characterized in the component of inorganic combustion inhibitor by
Ultra-fine magnesium silicate, aluminium hydroxide, modifying agent form.The preparation method of the present invention, including selecting raw material, pretreatment of raw material, pulverizing
Process, the selection of modifying agent and process, modification.Modification is by this product microgranule above-mentioned, puts in modifying machine, with
Time modifying machine is heated up, make material temperature in modifying machine rise to 100 DEG C, be added dropwise to coupling machine agent, coupling agent addition after 10 minutes
It is 1.2%, when adding coupling agent, keeps the temperature at 100 DEG C, be incubated 30 minutes.CN101538419A disclose a kind of shepardite without
Machine fire retardant preparation technology, implements according to following steps: 1) process of shepardite crushing raw ore, it is respectively adopted jaw crusher, hammer
Formula disintegrating machine carries out two-stage break process to shepardite raw ore, and the shepardite particle diameter after crushing is less than 3mm；2) water after crushing
Magnesite carries out grinding in sending into high thin ball mill, the discharge outlet of high thin ball mill is sucked in superfine classifier by air-introduced machine；
3) shepardite after grinding is circulated three staged care in superfine classifier, and secondary grading is by the water magnesium after scalping
Stone sucks in superfine classifier again, and the shepardite after secondary grading carries out three classifications in sucking again superfine classifier, sorting
Slag charge out is discharged to the external world, and the shepardite after three classifications enters in product collector with air-flow, the water after three classifications
Magnesite average particle size is less than 5um.
But the flame retardant effect that above-mentioned aluminium hydroxide, magnesium hydroxide composite inorganic fire retardant exist is bad and polymer
Between the problem of bad dispersibility.
Summary of the invention
The technical problem to be solved is the aluminium hydroxide of routine, the existence of magnesium hydroxide composite inorganic fire retardant
Flame retardant effect is bad and the problem of bad dispersibility between polymer.
Technical scheme is:
A kind of surface cladding type composite inorganic fire retardant, includes Al (OH) by weight3-Zr(OH)2-Ti3C2Composite powder
Body 20～40 parts, aluminium hydroxide powder 10～20 parts, magnesium hydrate powder 10～20 parts, cationic surfactant 1～3 parts,
Anion surfactant 1～3 parts, coupling agent 2～4 parts, water 5～10 parts.
The granule mesh number of described aluminium hydroxide powder is between 400～800 mesh.
The granule mesh number of described magnesium hydrate powder is between 400～800 mesh.
Described anion surfactant is DBSA and sodium salt thereof.
Described cationic surfactant is hexadecyltrimethylammonium chloride.
Coupling agent refers to silane coupler.
Described Silane coupling agent KH550.
Al(OH)3-Zr(OH)2-Ti3C2The preparation method of composite granule comprises the steps:
S1 walks, by Ti3AlC2Powder body ball milling, then dry, obtain the ceramic powder of refinement；
S2 walks, and is taken by the ceramic powder of refinement in 2g～10g submergence 50mL～200mL hydrofluoric acid solution and reacts, and corrosion is produced
Thing deionized water cleans to neutral, then uses washes of absolute alcohol；Gained solid sample is dried, the pottery after being corroded
Powder body；
S3 walks, and the ceramic powder after being corroded by step (2) gained takes 15g～25g and puts in 2～4L dehydrated alcohol, stirring, then
Add aluminum nitrate powder and the 1～5 g ZrOCl of 5～20 g2Powder, then it is slowly added dropwise dilute hydrochloric acid 100～150ml, continue to stir
Mix reaction, use deionized water eccentric cleaning again with after dehydrated alcohol eccentric cleaning, solid sample is dried, obtains Al (OH)3-Zr
(OH)2-Ti3C2Composite.
In described S1 step, Ball-milling Time 1～10h, rotational speed of ball-mill 400r/min, ball material mass ratio 6:1；Dry temperature
Degree is 40～60 DEG C.
In described S2 step, the concentration 35～45wt% of hydrofluoric acid solution, the response time 6～12h.
In described S3 step, the mass concentration of dilute hydrochloric acid is 1～5wt%；Response time 6～12h；Drying temperature is 110
～120 DEG C.
The preparation method of described inorganic combustion inhibitor, comprises the steps:
1st step, by Al (OH)3-Zr(OH)2-Ti3C2Composite granule, anion surfactant, a part of water mix homogeneously；
2nd step, by the mixing of aluminium hydroxide powder, magnesium hydrate powder, cationic surfactant, coupling agent and remaining water all
Even；
3rd step, in the case of stirring is opened, in the mixture of the 1st step gained, is gradually added the mixture of the 2nd step gained,
After addition, negative pressure is dried, and obtains inorganic combustion inhibitor.
The application in cable material of the described surface cladding type composite inorganic fire retardant.
Described cable material refers to EVA material.
Beneficial effect
The inorganic combustion inhibitor good flame retardation effect that the present invention provides, when mixing between polymer, dispersibility is excellent.
Detailed description of the invention
The inorganic combustion inhibitor that the present invention provides, includes Al (OH) by weight3-Zr(OH)2-Ti3C2Composite granule
20～40 parts, aluminium hydroxide powder 10～20 parts, magnesium hydrate powder 10～20 parts, cationic surfactant 1～3 parts, the moon
Ionic surface active agent 1～3 parts, coupling agent 2～4 parts, water 5～10 parts.
Wherein, cationic surfactant includes, such as, quaternary ammonium salt, such as hexadecyltrimethylammonium chloride, chlorination Laurel
Base trimethyl ammonium and ethyl sulfuric acid oleyl Methylethyl ammonium；And (polyoxyalkylenes) alkyl amino ether salt, such as (polyoxyethylene
Thiazolinyl) lauryl amino ether lactate, stearyl ether lactate, and (polyethylene oxide base) lauryl amino ether trimethyl
Phosphate.
Anion surfactant includes, such as, fatty acid and their salt, such as oleic acid, Palmic acid, enuatrol, palm fibre
Palmitic acid acid potassium, and triethanolamine oleate；Hydroxyl institute acids and their salt, such as hydroxyacetic acid, hydroxyacetic acid potassium, lactic acid and lactic acid
Potassium；Polyoxyalkylene alkyl acetic acid class and their salt, such as polyoxyalkylene three decyl ethers acetic acid and sodium salt thereof；Carboxyl-polysubstituted
The salt of aromatic compounds, such as trimellitic acid potassium and PMA potassium；Benzene sulfonamide acids and their salt, such as detergent alkylate
Sulfonic acid and sodium salt thereof；Polyoxyalkylene alkyl ethers sulfonic acid and their salt, such as polyethylene glycol oxide 2-ethylhexyl ether sulfonic acid and
Potassium salt；Higher fatty acid amides sulfonic acid and their salt, such as stearoyl N-methyltaurine and sodium salt thereof, lauroyl methyl taurine
And sodium salt, myristoyl methyl taurine and sodium salt and PMT and sodium salt thereof；N-acyl group sarcosinates
With their salt, such as Hamposyl L and sodium salt thereof；Alkyl phosphonic acid and their salt, such as octylphosphonate and potassium salt thereof；Virtue
Race's phosphonic acids and their salt, such as phenyl phosphonic acid esters and potassium salt thereof；Alkyl phosphonic acid phosphonate ester and their salt, such as 2-ethyl hexyl
Base phosphonic acids list-2-Octyl Nitrite and potassium salt thereof；Nitrogenous alkyl phosphonic acid and their salt, such as aminoethyl phosphonic acid and diethanolamine thereof
Salt；Alkyl sulfate and their salt, such as 2-ethyl hexyl sulfuric ester and sodium salt thereof；Polyoxyalkylene sulfuric acid ester and their salt,
Such as polyethylene glycol oxide 2-ethylhexyl ether sulfuric ester and sodium salt thereof；Alkyl phosphoric acid esters and their salt, such as base succinic acid salt,
Such as two-2-ethylhexyl sodium sulfo-succinate and dioctyl sodium sulfosuccinate；And long-chain N-acyl glutamate, such as the N-month
Osmanthus acyl monosodium glutamate and N-stearoyl-Pidolidone disodium.
Embodiment 1
Surface cladding type composite inorganic fire retardant, its constitutive material is: Al (OH) by weight3-Zr(OH)2-Ti3C2Multiple
Close powder body 20 parts, aluminium hydroxide powder 10 parts, magnesium hydrate powder 10 parts, cationic surfactant cetyl trimethyl chlorine
Change ammonium 3 parts, anion surfactant DBSA and sodium salt 3 parts, KH550 coupling agent 4 parts, 10 parts of water.
The granule mesh number of aluminium hydroxide powder is between 400～800 mesh；The granule mesh number of magnesium hydrate powder be 400～
Between 800 mesh.
Al(OH)3-Zr(OH)2-Ti3C2The preparation method of composite granule is: S1 walks, by Ti3AlC2Powder body ball milling, ball milling
Time 10h, rotational speed of ball-mill 400r/min, ball material mass ratio 6:1, then at 60 DEG C of drying, obtain the ceramic powder of refinement；S2
Step, takes the ceramic powder of refinement in 10g submergence 200mL hydrofluoric acid solution and reacts, concentration 35wt% of hydrofluoric acid solution, reaction
Time 6h, cleans corrosion product deionized water to neutral, then uses washes of absolute alcohol；Gained solid sample is dried,
Ceramic powder after being corroded；S3 walks, and the ceramic powder after being corroded by step (2) gained takes 15g and puts into 4L dehydrated alcohol
In, stirring, add aluminum nitrate powder and the 5 g ZrOCl of 20 g2Powder, then it is slowly added dropwise 5wt% dilute hydrochloric acid 150ml, continue
Stirring reaction 12h, uses deionized water eccentric cleaning again with after dehydrated alcohol eccentric cleaning, by solid sample 120 DEG C drying, to obtain final product
Al(OH)3-Zr(OH)2-Ti3C2Composite.
The preparation method of described inorganic combustion inhibitor, comprises the steps:
1st step, by Al (OH)3-Zr(OH)2-Ti3C2Composite granule, anion surfactant, a part of water mix homogeneously；
2nd step, by the mixing of aluminium hydroxide powder, magnesium hydrate powder, cationic surfactant, coupling agent and remaining water all
Even；
3rd step, in the case of stirring is opened, in the mixture of the 1st step gained, is gradually added the mixture of the 2nd step gained,
After addition, negative pressure is dried, and obtains inorganic combustion inhibitor.
Embodiment 2
Surface cladding type composite inorganic fire retardant, its constitutive material is: Al (OH) by weight3-Zr(OH)2-Ti3C2Multiple
Close powder body 40 parts, aluminium hydroxide powder 20 parts, magnesium hydrate powder 20 parts, cationic surfactant cetyl trimethyl chlorine
Change ammonium 3 parts, anion surfactant DBSA and sodium salt 3 parts, KH550 coupling agent 4 parts, 10 parts of water.
The granule mesh number of aluminium hydroxide powder is between 400～800 mesh；The granule mesh number of magnesium hydrate powder be 400～
Between 800 mesh.
Al(OH)3-Zr(OH)2-Ti3C2The preparation method of composite granule is: S1 walks, by Ti3AlC2Powder body ball milling, ball milling
Time 1h, rotational speed of ball-mill 400r/min, ball material mass ratio 6:1, then at 40 DEG C of drying, obtain the ceramic powder of refinement；S2
Step, takes the ceramic powder of refinement in 2g submergence 50mL hydrofluoric acid solution and reacts, and concentration 35wt% of hydrofluoric acid solution, during reaction
Between 6h, corrosion product deionized water is cleaned to neutral, then uses washes of absolute alcohol；Gained solid sample is dried,
Ceramic powder after corrosion；S3 walks, and the ceramic powder after being corroded by step (2) gained takes 15g and puts in 2L dehydrated alcohol,
Stirring, adds aluminum nitrate powder and the 1 g ZrOCl of 5 g2Powder, then it is slowly added dropwise 1wt% dilute hydrochloric acid 100ml, continue stirring
Reaction 6h, uses deionized water eccentric cleaning again with after dehydrated alcohol eccentric cleaning, by solid sample 110 DEG C drying, obtains Al
(OH)3-Zr(OH)2-Ti3C2Composite.
The preparation method of described inorganic combustion inhibitor, comprises the steps:
1st step, by Al (OH)3-Zr(OH)2-Ti3C2Composite granule, anion surfactant, a part of water mix homogeneously；
2nd step, by the mixing of aluminium hydroxide powder, magnesium hydrate powder, cationic surfactant, coupling agent and remaining water all
Even；
3rd step, in the case of stirring is opened, in the mixture of the 1st step gained, is gradually added the mixture of the 2nd step gained,
After addition, negative pressure is dried, and obtains inorganic combustion inhibitor.
Embodiment 3
Surface cladding type composite inorganic fire retardant, its constitutive material is: Al (OH) by weight3-Zr(OH)2-Ti3C2Multiple
Close powder body 30 parts, aluminium hydroxide powder 15 parts, magnesium hydrate powder 19 parts, cationic surfactant cetyl trimethyl chlorine
Change ammonium 2 parts, anion surfactant DBSA and sodium salt 2 parts, KH550 coupling agent 3 parts, 6 parts of water.
The granule mesh number of aluminium hydroxide powder is between 400～800 mesh；The granule mesh number of magnesium hydrate powder be 400～
Between 800 mesh.
Al(OH)3-Zr(OH)2-Ti3C2The preparation method of composite granule is: S1 walks, by Ti3AlC2Powder body ball milling, ball milling
Time 7h, rotational speed of ball-mill 400r/min, ball material mass ratio 6:1, then at 55 DEG C of drying, obtain the ceramic powder of refinement；S2
Step, takes the ceramic powder of refinement in 7g submergence 80mL hydrofluoric acid solution and reacts, and concentration 40wt% of hydrofluoric acid solution, during reaction
Between 8h, corrosion product deionized water is cleaned to neutral, then uses washes of absolute alcohol；Gained solid sample is dried,
Ceramic powder after corrosion；S3 walks, and the ceramic powder after being corroded by step (2) gained takes 20g and puts in 3L dehydrated alcohol,
Stirring, adds aluminum nitrate powder and the 4g ZrOCl of 14g2Powder, then it is slowly added dropwise 4wt% dilute hydrochloric acid 12ml, continue stirring anti-
Answer 10h, use deionized water eccentric cleaning again with after dehydrated alcohol eccentric cleaning, by solid sample 115 DEG C drying, obtain Al
(OH)3-Zr(OH)2-Ti3C2Composite.
The preparation method of described inorganic combustion inhibitor, comprises the steps:
1st step, by Al (OH)3-Zr(OH)2-Ti3C2Composite granule, anion surfactant, a part of water mix homogeneously；
2nd step, by the mixing of aluminium hydroxide powder, magnesium hydrate powder, cationic surfactant, coupling agent and remaining water all
Even；
3rd step, in the case of stirring is opened, in the mixture of the 1st step gained, is gradually added the mixture of the 2nd step gained,
After addition, negative pressure is dried, and obtains inorganic combustion inhibitor.
Reference examples 1
Difference with embodiment 3 is: is provided without Fluohydric acid. in the preparation of composite granule and corrodes.
Surface cladding type composite inorganic fire retardant, its constitutive material is: Al (OH) by weight3-Zr(OH)2-
Ti3C2Composite granule 30 parts, aluminium hydroxide powder 15 parts, magnesium hydrate powder 19 parts, cationic surfactant cetyl three
Ammonio methacrylate 2 parts, anion surfactant DBSA and sodium salt 2 parts thereof, KH550 coupling agent 3 parts, 6 parts of water.
The granule mesh number of aluminium hydroxide powder is between 400～800 mesh；The granule mesh number of magnesium hydrate powder be 400～
Between 800 mesh.
Al(OH)3-Zr(OH)2-Ti3C2The preparation method of composite granule is: S1 walks, by Ti3AlC2Powder body ball milling, ball milling
Time 7h, rotational speed of ball-mill 400r/min, ball material mass ratio 6:1, then at 55 DEG C of drying, obtain the ceramic powder of refinement；S2
Step, takes the ceramic powder of refinement 7g deionized water and cleans, then use washes of absolute alcohol；Gained solid sample is dried,
Ceramic powder after being processed；S3 walks, and the ceramic powder after being processed by step (2) gained takes 20g and puts into 3L dehydrated alcohol
In, stirring, add aluminum nitrate powder and the 4g ZrOCl of 14g2Powder, then it is slowly added dropwise 4wt% dilute hydrochloric acid 12ml, continue to stir
Mix reaction 10h, use deionized water eccentric cleaning again with after dehydrated alcohol eccentric cleaning, by solid sample 115 DEG C drying, obtain Al
(OH)3-Zr(OH)2-Ti3C2Composite.
The preparation method of described inorganic combustion inhibitor, comprises the steps:
1st step, by Al (OH)3-Zr(OH)2-Ti3C2Composite granule, anion surfactant, a part of water mix homogeneously；
2nd step, by the mixing of aluminium hydroxide powder, magnesium hydrate powder, cationic surfactant, coupling agent and remaining water all
Even；
3rd step, in the case of stirring is opened, in the mixture of the 1st step gained, is gradually added the mixture of the 2nd step gained,
After addition, negative pressure is dried, and obtains inorganic combustion inhibitor.
Reference examples 2
Difference with embodiment 3 is: in preparation method, anion surfactant is suitable with the addition of cationic surfactant
Sequence is reversed.
Surface cladding type composite inorganic fire retardant, its constitutive material is: Al (OH) by weight3-Zr(OH)2-
Ti3C2Composite granule 30 parts, aluminium hydroxide powder 15 parts, magnesium hydrate powder 19 parts, cationic surfactant cetyl three
Ammonio methacrylate 2 parts, anion surfactant DBSA and sodium salt 2 parts thereof, KH550 coupling agent 3 parts, 6 parts of water.
The granule mesh number of aluminium hydroxide powder is between 400～800 mesh；The granule mesh number of magnesium hydrate powder be 400～
Between 800 mesh.
Al(OH)3-Zr(OH)2-Ti3C2The preparation method of composite granule is: S1 walks, by Ti3AlC2Powder body ball milling, ball milling
Time 7h, rotational speed of ball-mill 400r/min, ball material mass ratio 6:1, then at 55 DEG C of drying, obtain the ceramic powder of refinement；S2
Step, takes the ceramic powder of refinement in 7g submergence 80mL hydrofluoric acid solution and reacts, and concentration 40wt% of hydrofluoric acid solution, during reaction
Between 8h, corrosion product deionized water is cleaned to neutral, then uses washes of absolute alcohol；Gained solid sample is dried,
Ceramic powder after corrosion；S3 walks, and the ceramic powder after being corroded by step (2) gained takes 20g and puts in 3L dehydrated alcohol,
Stirring, adds aluminum nitrate powder and the 4g ZrOCl of 14g2Powder, then it is slowly added dropwise 4wt% dilute hydrochloric acid 12ml, continue stirring anti-
Answer 10h, use deionized water eccentric cleaning again with after dehydrated alcohol eccentric cleaning, by solid sample 115 DEG C drying, obtain Al
(OH)3-Zr(OH)2-Ti3C2Composite.
The preparation method of described inorganic combustion inhibitor, comprises the steps:
1st step, by Al (OH)3-Zr(OH)2-Ti3C2Composite granule, cationic surfactant, a part of water mix homogeneously；
2nd step, by the mixing of aluminium hydroxide powder, magnesium hydrate powder, anion surfactant, coupling agent and remaining water all
Even；
3rd step, in the case of stirring is opened, in the mixture of the 1st step gained, is gradually added the mixture of the 2nd step gained,
After addition, negative pressure is dried, and obtains inorganic combustion inhibitor.
Performance test
Following formula is used to prepare EVA cable material: product is filled the plastic formula of EVA CABLE MATERIALS and is: fire retardant 100 parts,
EVA140 part, each 1.5 parts of antioxidant, compatilizer, lubricant；Preparation method be raw material is mixed after, then at double screw extruder
In carry out extrusion molding.
Material property parameter such as following table:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Reference examples 1 | Reference examples 2 | |
| Oxygen index (OI) LOI, % | 35.8 | 36.4 | 36.8 | 32.1 | 31.9 |
| Hot strength Mpa | 12.9 | 12.4 | 13.2 | 11.8 | 11.5 |
| Elongation at break % | 200 | 205 | 215 | 178 | 182 |
As can be seen from the table, the material that the present invention provides has preferable fire resistance, after applying simultaneously in EVA material,
EVA material can be kept to have preferable tensile property；In reference examples 1, due to not to Ti3AlC2Powder body carries out Fluohydric acid. and carries out
Corrosion treatmentCorrosion Science, causes its particle surface pattern bad, can not form preferable clad structure when mixing with other component, lead
Cause fire resistance bad；In reference examples 2, owing to cationic surfactant is mutually exchanged with anion surfactant,
Due to cationic surfactant can not with composite granule preferably Electrostatic Absorption, result in cationic surfactant with cloudy from
Action effect between sub-surface activating agent weakens, and the mechanical performance that result in EVA material declines.
Claims (10)
1. a surface cladding type composite inorganic fire retardant, it is characterised in that include Al (OH) by weight3-Zr
(OH)2-Ti3C2Composite granule 20～40 parts, aluminium hydroxide powder 10～20 parts, magnesium hydrate powder 10～20 parts, cation form
Face activating agent 1～3 parts, anion surfactant 1～3 parts, coupling agent 2～4 parts, water 5～10 parts.
Surface cladding type composite inorganic fire retardant the most according to claim 1, it is characterised in that described aluminium hydrate powder
The granule mesh number of body is between 400～800 mesh.
Surface cladding type composite inorganic fire retardant the most according to claim 1, it is characterised in that described hydroxide magnesium powder
The granule mesh number of body is between 400～800 mesh.
Surface cladding type composite inorganic fire retardant the most according to claim 1, it is characterised in that described anionic surface
Activating agent is DBSA and sodium salt thereof；Described cationic surfactant is hexadecyltrimethylammonium chloride.
Surface cladding type composite inorganic fire retardant the most according to claim 1, it is characterised in that.
Surface cladding type composite inorganic fire retardant the most according to claim 1, it is characterised in that coupling agent refers to that silane is even
Connection agent KH550.
Surface cladding type composite inorganic fire retardant the most according to claim 1, it is characterised in that Al (OH)3-Zr(OH)2-
Ti3C2The preparation method of composite granule comprises the steps: that S1 walks, by Ti3AlC2Powder body ball milling, then dry, obtain thin
The ceramic powder changed；S2 walks, and is taken by the ceramic powder of refinement in 2g～10g submergence 50mL～200mL hydrofluoric acid solution and reacts,
Corrosion product deionized water is cleaned to neutral, then uses washes of absolute alcohol；Gained solid sample is dried, is corroded
After ceramic powder；S3 walks, and the ceramic powder after being corroded by step (2) gained takes 15g～25g and puts into 2～4L dehydrated alcohol
In, stirring, add aluminum nitrate powder and the 1～5 g ZrOCl of 5～20 g2Powder, then be slowly added dropwise dilute hydrochloric acid 100～
150ml, continues stirring reaction, uses deionized water eccentric cleaning again with after dehydrated alcohol eccentric cleaning, dried by solid sample, i.e.
Obtain Al (OH)3-Zr(OH)2-Ti3C2Composite.
Surface cladding type composite inorganic fire retardant the most according to claim 1, it is characterised in that in described S1 step,
Ball-milling Time 1～10h, rotational speed of ball-mill 400r/min, ball material mass ratio 6:1；Drying temperature is 40～60 DEG C；Described S2
In step, the concentration 35～45wt% of hydrofluoric acid solution, the response time 6～12h；In described S3 step, the mass concentration of dilute hydrochloric acid
It is 1～5wt%；Response time 6～12h；Drying temperature is 110～120 DEG C.
9. the preparation method of the surface cladding type composite inorganic fire retardant described in any one of claim 1～8, it is characterised in that
Comprise the steps: the 1st step, by Al (OH)3-Zr(OH)2-Ti3C2Composite granule, anion surfactant, a part of water are mixed
Close uniformly；2nd step, mixes aluminium hydroxide powder, magnesium hydrate powder, cationic surfactant, coupling agent and remaining water
Close uniformly；3rd step, in the case of stirring is opened, in the mixture of the 1st step gained, is gradually added the mixing of the 2nd step gained
Thing, after addition, negative pressure is dried, and obtains inorganic combustion inhibitor.
10. the application in cable material of the surface cladding type composite inorganic fire retardant described in any one of claim 1～8；Institute
The cable material stated refers to EVA material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610420806.5A CN106046417A (en) | 2016-06-15 | 2016-06-15 | Surface-coating type composite inorganic flame retardant, preparation method thereof and application of surface-coating type composite inorganic flame retardant to cable material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610420806.5A CN106046417A (en) | 2016-06-15 | 2016-06-15 | Surface-coating type composite inorganic flame retardant, preparation method thereof and application of surface-coating type composite inorganic flame retardant to cable material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106046417A true CN106046417A (en) | 2016-10-26 |
Family
ID=57168163
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610420806.5A Pending CN106046417A (en) | 2016-06-15 | 2016-06-15 | Surface-coating type composite inorganic flame retardant, preparation method thereof and application of surface-coating type composite inorganic flame retardant to cable material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106046417A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107994186A (en) * | 2017-11-10 | 2018-05-04 | 江苏华富储能新技术股份有限公司 | A kind of lithium battery organo-mineral complexing membrane and preparation method |
| CN107994185A (en) * | 2017-11-10 | 2018-05-04 | 江苏华富储能新技术股份有限公司 | A kind of lithium battery and preparation method using organo-mineral complexing membrane |
| KR20190102680A (en) * | 2018-02-27 | 2019-09-04 | 현대하이켐(주) | Method for preparing phosphor-nitrogen flame retardant |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1492005A (en) * | 2003-08-29 | 2004-04-28 | 杨治富 | Surface treating coupling agent for natural magnesium hydroxide organic flame-retardant powder |
| KR100498226B1 (en) * | 2004-06-17 | 2005-07-01 | 진성산업(주) | Fire retardant coating composition and coating method thereof |
| CN1654597A (en) * | 2005-03-04 | 2005-08-17 | 北京化工大学 | Process for preparing nano inorganic compound flame retardant by transfer method |
| JPWO2009128306A1 (en) * | 2008-04-16 | 2011-08-04 | 株式会社Ｈｉ−Ｖａｎ | Flame retardant composite material |
| CN103041837A (en) * | 2011-10-17 | 2013-04-17 | 中国石油化工股份有限公司 | Preparation method of spherical hydrogenation catalyst |
| CN104086849A (en) * | 2014-06-24 | 2014-10-08 | 淮北市天相电缆有限责任公司 | Low-smoke, halogen-free and flame-retardant cable material used for coal mine, and preparation method thereof |
| CN104528721A (en) * | 2014-12-23 | 2015-04-22 | 陕西科技大学 | Preparation method of flaky two-dimensional nano-titanium carbide nanometre material |
-
2016
- 2016-06-15 CN CN201610420806.5A patent/CN106046417A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1492005A (en) * | 2003-08-29 | 2004-04-28 | 杨治富 | Surface treating coupling agent for natural magnesium hydroxide organic flame-retardant powder |
| KR100498226B1 (en) * | 2004-06-17 | 2005-07-01 | 진성산업(주) | Fire retardant coating composition and coating method thereof |
| CN1654597A (en) * | 2005-03-04 | 2005-08-17 | 北京化工大学 | Process for preparing nano inorganic compound flame retardant by transfer method |
| JPWO2009128306A1 (en) * | 2008-04-16 | 2011-08-04 | 株式会社Ｈｉ−Ｖａｎ | Flame retardant composite material |
| CN103041837A (en) * | 2011-10-17 | 2013-04-17 | 中国石油化工股份有限公司 | Preparation method of spherical hydrogenation catalyst |
| CN104086849A (en) * | 2014-06-24 | 2014-10-08 | 淮北市天相电缆有限责任公司 | Low-smoke, halogen-free and flame-retardant cable material used for coal mine, and preparation method thereof |
| CN104528721A (en) * | 2014-12-23 | 2015-04-22 | 陕西科技大学 | Preparation method of flaky two-dimensional nano-titanium carbide nanometre material |
Non-Patent Citations (3)
| Title |
|---|
| 《无机化学》编写组: "《无机化学》", 30 September 1983, 山东科学技术出版社 * |
| 化学工业部天津化工研究院等: "《化工产品手册-无机化工产品》", 31 October 1993, 化学工业出版社 * |
| 孙积辉: "《药物化学》", 30 November 1986, 人民卫生出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107994186A (en) * | 2017-11-10 | 2018-05-04 | 江苏华富储能新技术股份有限公司 | A kind of lithium battery organo-mineral complexing membrane and preparation method |
| CN107994185A (en) * | 2017-11-10 | 2018-05-04 | 江苏华富储能新技术股份有限公司 | A kind of lithium battery and preparation method using organo-mineral complexing membrane |
| KR20190102680A (en) * | 2018-02-27 | 2019-09-04 | 현대하이켐(주) | Method for preparing phosphor-nitrogen flame retardant |
| KR102134264B1 (en) | 2018-02-27 | 2020-07-15 | 현대하이켐(주) | Method for preparing phosphor-nitrogen flame retardant |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103740231B (en) | A kind of water expansion cable nano fire-retardant coating and preparation method thereof | |
| CN106046417A (en) | Surface-coating type composite inorganic flame retardant, preparation method thereof and application of surface-coating type composite inorganic flame retardant to cable material | |
| CN105256572B (en) | Halogen-free flame retardant coating adhesive and preparing method thereof | |
| CN109517220A (en) | A kind of preparation method of nanometer of tinbase expanding fire retardant | |
| CN102241931A (en) | Environment-friendly type flame-retarding and smoke-suppressing paint and preparation method thereof | |
| CN105037960A (en) | Hydrolysis-resistant cable material for automobile and preparation method of hydrolysis-resistant cable material | |
| CN102719154B (en) | Flame-retardant heat-insulating coating and preparation method thereof | |
| CN103540053A (en) | Heat and flame resistant polyvinyl chloride power cord sheath material and preparation method thereof | |
| CN104804293A (en) | Locomotive fatigue resistant cable material and preparation method thereof | |
| CN104650683A (en) | Environmentally-friendly fireproof coating and preparation method thereof | |
| CN105314959B (en) | A kind of preparation method of Building Fire Protection ornament materials | |
| CN101659833A (en) | Fireproofing paint for steel structure and preparation method thereof | |
| CN104893169A (en) | Lubrication plastic for sealing element | |
| CN105110357A (en) | Method used for preparing magnesium hydroxide fire retardant from magnesium salt | |
| CN104650728A (en) | Wear-resistant scrub-resistant waterproof paint and preparation method thereof | |
| CN104744763A (en) | Antistatic fire retardant master batch for modification of polyethylene | |
| CN109810545A (en) | A kind of single layer nanometer basic zirconium phosphate modified heavy magnesium hydroxide and preparation method thereof | |
| CN109988336A (en) | A kind of preparation method of Modification of Montmorillonite nano-aluminum hydroxide composite inorganic fire retardant | |
| CN109651849A (en) | A kind of preparation method of flame-retardant cable wollastonite surface cladded aluminium hydroxide | |
| CN104804339A (en) | Locomotive fluoroplastic cable material and preparation method thereof | |
| CN1492005A (en) | Surface treating coupling agent for natural magnesium hydroxide organic flame-retardant powder | |
| CN103992067A (en) | Lightweight partition plate made by using vanadium tailings, and making method thereof | |
| CN111302824B (en) | Preparation method of environment-friendly efficient flame-retardant wall material and prepared material | |
| CN113831590A (en) | Flame-retardant smoke-suppressing mineral complex and preparation method and application thereof | |
| CN106117604A (en) | The preparation method of absorbent-type attapulgite ground mass fire proofing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161026 |
|
| RJ01 | Rejection of invention patent application after publication |