CN105504597B - A kind of cable PVC material fire retardant - Google Patents
A kind of cable PVC material fire retardant Download PDFInfo
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- CN105504597B CN105504597B CN201610061380.9A CN201610061380A CN105504597B CN 105504597 B CN105504597 B CN 105504597B CN 201610061380 A CN201610061380 A CN 201610061380A CN 105504597 B CN105504597 B CN 105504597B
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- China
- Prior art keywords
- fire
- retardant
- cerium oxide
- fire retardant
- butyl titanate
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 27
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 26
- 239000004411 aluminium Substances 0.000 claims abstract description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 12
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- 229910052684 Cerium Inorganic materials 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- VWWHFOBVDHPEKJ-UHFFFAOYSA-N aluminum ethanol trinitrate Chemical compound C(C)O.[N+](=O)([O-])[O-].[Al+3].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] VWWHFOBVDHPEKJ-UHFFFAOYSA-N 0.000 claims description 5
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 239000002270 dispersing agent Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 abstract description 17
- 239000001301 oxygen Substances 0.000 abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 16
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 abstract 2
- 239000004800 polyvinyl chloride Substances 0.000 description 24
- 229920000915 polyvinyl chloride Polymers 0.000 description 23
- 239000004014 plasticizer Substances 0.000 description 10
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 5
- 239000003112 inhibitor Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 4
- 235000019504 cigarettes Nutrition 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000001629 suppression Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 230000000979 retarding effect Effects 0.000 description 2
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- YEAUATLBSVJFOY-UHFFFAOYSA-N tetraantimony hexaoxide Chemical compound O1[Sb](O2)O[Sb]3O[Sb]1O[Sb]2O3 YEAUATLBSVJFOY-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- NTWUDWUVKKRQRK-UHFFFAOYSA-N aluminum;cerium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Ce+3] NTWUDWUVKKRQRK-UHFFFAOYSA-N 0.000 description 1
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
- 239000008116 calcium stearate Substances 0.000 description 1
- 235000013539 calcium stearate Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- WLPSNBGDESCKIL-UHFFFAOYSA-N ethanol;titanium Chemical compound [Ti].CCO WLPSNBGDESCKIL-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- YCWSUKQGVSGXJO-NTUHNPAUSA-N nifuroxazide Chemical group C1=CC(O)=CC=C1C(=O)N\N=C\C1=CC=C([N+]([O-])=O)O1 YCWSUKQGVSGXJO-NTUHNPAUSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
-
- 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
- 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
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
- C08K2003/2213—Oxides; Hydroxides of metals of rare earth metal of cerium
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Insulated Conductors (AREA)
Abstract
The invention discloses a kind of novel cable PVC material fire retardant, the fire retardant includes aluminium titanates cerium oxide, and its dosage is 1 10wt% of PVC material gross weight.The aluminium titanates cerium oxide can be used cooperatively with other conventional PVC material fire retardants, have higher fire retardancy, and oxygen index (OI) can reach more than 35, have the characteristics of addition is small, environmentally friendly.
Description
Technical field
The invention belongs to cable special PVC additive, more particularly to a kind of fire retardant of cable PVC material.
Background technology
Polyvinyl chloride (PVC) resin has extensively as a kind of time-honored thermoplastic in wires and cables industry
Application.Such as present life by the use of 450V/750V and the electric wire and flexible cord of following insulation all much use PVC as base
Body resin.With extensive use of the flame retarding PVC composition for cable in fields such as electronic apparatus, computer, automobile and space flight, to cable
Anti-flammability also has higher and higher requirement.
PVC cables its flame resistance deficiency, can produce due to being wherein mixed with substantial amounts of plasticizer and other auxiliary agents in burning
Raw harmful HCl gases, HCl can also have very strong corrosiveness to metal., can also be because of except producing toxic gas
Some gas incomplete combustions and produce substantial amounts of smog, drastically influence the safety of life and property of the people.Therefore, research is opened
Send out cigarette low, the PVC cables of low toxicity turn into the urgent demand of cable-flame retardant industry, there is important social value.
In PVC cables, our generally uses add the method for fire retardant and flame-retardant plasticizer to realize its fire-retardant and suppression
The effect of cigarette.Specifically used method has following several：(1) conventional plasticizer is replaced with fire-retardant plasticizer.It is such as normal
Using triaryl phosphate and alkyl diaryl phosphate as plasticizer, they thermally decompose to generate not volatile in burning
Polyphosphoric acid, layer protecting film can be formed in the surface of solids, separate the contact with oxygen.(2) antimonial, metal hydrogen-oxygen are added
The inorganic combustion inhibitors such as compound.The aluminium hydroxide being usually added into also has obvious suppression cigarette effect.(3) it is higher in plasticizer loading
When using simultaneously add flame-retardant plasticizer, inorganic combustion inhibitor and fire-retardant filler method.(4) generally it is additionally added smoke suppressant.It is main
Be used for PVC cable material suppression cigarette has molybdenum trioxide and ammonium octamolybdate etc..We are frequently necessary to root in the formula of PVC cable material
The proportioning of suitable flame-retardant plasticizer and Conventional plasticizers is selected according to the different purposes of CABLE MATERIALS and fire-retardant demand, so can be with
Reach high cost performance.
The fire resistance of PVC cable material is typically to be weighed with oxygen index (OI), and oxygen index (OI) refers to allow required for sample burns
Minimum oxygen concentration.When oxygen index (OI) is bigger, anti-flammability is higher.Material of the usual oxygen index (OI) more than 30 just has certain
Anti-flammability.
Al (OH) is added in PVC cable material3, Sb2O3, the inorganic combustion inhibitor such as Firebrake ZB (ZB), their dosage is to PVC
Fire resistance influence it is very big.With Sb2O3Increase, the linear ascendant trend of limited oxygen index of PVC cable material, in nanometer
Sb2O3Addition be more than 1.5 parts when, nanometer Sb2O3Oxygen index (OI) contribution to PVC is more than micron order Sb2O3.But due to Sb2O3
Price costly, so typically adding Sb2O3Amount be not very high, as long as can guarantee that certain anti-flammability.And add
ZB may be used as antismoke agent, by ZB and Sb2O3Being used in combination will cause PVC cable material while with suitable oxygen index (OI)
Also there is low life smoke.
The content of the invention
The present inventor proposes to be used as high polymer especially PVC material fire retardant, the metatitanic acid using aluminium titanates-cerium oxide first
Aluminium-cerium oxide can be used cooperatively with other conventional PVC material fire retardants, have higher fire retardancy, and oxygen index (OI) can reach
To more than 35, there is the characteristics of addition is small, environmentally friendly.
The technical scheme is that be accomplished by the following way：
The invention discloses a kind of novel cable PVC material fire retardant, the fire retardant includes aluminium titanates-cerium oxide, and it is used
Measure as the 1-10wt% of PVC material gross weight, more preferably 3-5wt%.
The particle diameter of the aluminium titanates-cerium oxide fire-retardant particles is the fire-retardant particles of 10-100 microns.
The preparation method of the aluminium titanates-cerium oxide fire-retardant particles, comprises the following steps：Aluminum nitrate is dissolved in ethanol
Form aluminum nitrate ethanol solution；Butyl titanate is dissolved in ethanol formation butyl titanate ethanol solution, and to the metatitanic acid four
Butyl titanate quality 20-80% acetylacetone,2,4-pentanedione is added in butyl ester ethanol solution, is stirred vigorously 10-30min；Rubbed by aluminium, titanium
That ratio 2：1 is slowly added into the aluminum nitrate ethanol solution prepared in butyl titanate ethanol solution；It is mixed to add nitric acid regulation
Liquid pH value is closed to 5-7, polyethylene glycol is eventually adding and makees scattered pore creating material, dosage is the 0.5-5% of solvent volume, is stirred vigorously
To metatitanic acid Alumina gel；It is soluble in water with cerous nitrate, the cerous nitrate aqueous solution is formed, is precipitating reagent according to Ce using ammonium bicarbonate aqueous solution
And CO3 2-Mol ratio 1：2-3 is mixed, while the polyethylene glycol for adding mixed solution quality 1-2% is stirred vigorously as dispersant
10-30min, obtain cerous carbonate colloidal sol；By metatitanic acid Alumina gel and cerous carbonate colloidal sol according to the ratio that Ce and Al mol ratios are 0.1-10
Example mixing, and after being stirred vigorously 10-30min, drying is filtered, 1-5h is dried at 500-700 DEG C, crushes and obtains in ball mill
The aluminium titanates-cerium oxide fire-retardant particles.
The molecular weight of the polyethylene glycol is 200-4000.
It is preferred that the metatitanic acid Alumina gel and cerous carbonate colloidal sol mix according to the ratio that Ce and Al mol ratios are 0.5-2.
The acetylacetone,2,4-pentanedione is titanium hydrolysis inhibitor, and acetylacetone,2,4-pentanedione can chelate to form stable Ti chelator structure with titanium,
Effectively suppress the hydrolysis of titanium, ensure that the metatitanic acid Alumina gel of generation is uniform, there is good adsorption capacity.
Having the beneficial effect that relative to prior art of the invention：
It is using beneficial effect caused by above-mentioned technical proposal：Aluminium titanates-cerium oxide is developed as high polymer especially
It is the purposes of PVC material fire retardant, have developed new high polymer inorganic combustion inhibitor；(2) present invention addition small amount (1-
Aluminium titanates-cerium oxide 10wt.%) can reach flame retardant effect (oxygen index (OI) LOI >=40), compared with prior art, has and adds
Dosage is few, low to the mechanical property deterioration degree of material, or even can also improve the elongation at break of material；
Embodiment
The technical scheme of invention is described in detail with reference to specific embodiment.
The preparation of aluminium titanates-cerium oxide fire-retardant particles：Aluminum nitrate is dissolved in formation aluminum nitrate ethanol solution in ethanol；Titanium
Sour four butyl esters are dissolved in formation butyl titanate ethanol solution in ethanol, and add metatitanic acid into the butyl titanate ethanol solution
The acetylacetone,2,4-pentanedione of four butyl ester quality 20%, is stirred vigorously 10-30min；By aluminium, titanium mol ratio 2：The 1 aluminum nitrate second that will be prepared
Alcoholic solution is slowly added into butyl titanate ethanol solution；Add nitric acid and adjust mixed liquor pH value to 7, be eventually adding poly- second two
Alcohol makees scattered pore creating material, and dosage is the 1% of solvent volume, is stirred vigorously to obtain metatitanic acid Alumina gel；It is soluble in water with cerous nitrate, shape
It is precipitating reagent according to Ce and CO using ammonium bicarbonate aqueous solution into the cerous nitrate aqueous solution3 2-Mol ratio 1：2 mixing, while add mixing
The polyethylene glycol of solution quality 1% is stirred vigorously 30min, obtains cerous carbonate colloidal sol as dispersant；By metatitanic acid Alumina gel and carbon
Sour cerium colloidal sol mixes according to the ratio that Ce and Al mol ratios are 1, and after being stirred vigorously 10min, filters drying, is done at 550 DEG C
Dry 5h, crushed in ball mill and obtain the aluminium titanates-cerium oxide fire-retardant particles.
Embodiment 1
Aluminium titanates-cerium oxide the fire retardant, dosage 5wt% are added in PVC high polymers.
Embodiment 2
Aluminium titanates-cerium oxide the fire retardant, dosage 2wt% are added in PVC high polymers.
Comparative example 1
Aluminium titanates-cerium oxide fire retardant is not added, and other components and embodiment 1 are identical
Performance test：
As the basic recipe corresponding to each embodiment, other additives, such as plasticizer are added according to conventional amount used and formula
(DOP), organic tin stabilizer, coupling agent, calcium stearate, stearic acid, then by said components, machinery stirs in high-speed mixer
Mix uniformly, be kneaded on double track kneading machine and be pressed into standard-sized sample.And sample is entered according to ASTMD2863-2000
Row oxygen index (OI) is tested.
| Oxygen index (OI) | Flame retarding efficiency | |
| Embodiment 1 | 36 | 1.5 |
| Embodiment 2 | 38 | 1.6 |
| Comparative example 1 | 21 | 0.1 |
From table 1 it follows that being compared with blank PVC material, the sample oxygen that with the addition of aluminium titanates-cerium oxide fire retardant refers to
Number greatly improves, and with the increase of dosage, oxygen index (OI) also increases.
The present invention can be summarized with others without prejudice to the concrete form of the spirit or essential characteristics of the present invention.The present invention's
All embodiments can only all be considered the description of the invention rather than limitation, and every technique according to the invention content is made
Any trickle amendment or equivalent substitution gone out, is belonged within technical scheme.
Claims (4)
1. a kind of cable PVC material fire retardant, the fire retardant is aluminium titanates-cerium oxide fire-retardant particles, and its dosage is PVC material
The 1-10wt% of gross weight, the preparation method of the aluminium titanates-cerium oxide fire-retardant particles comprise the following steps：Aluminum nitrate is molten
Aluminum nitrate ethanol solution is formed in ethanol；Butyl titanate is dissolved in ethanol formation butyl titanate ethanol solution, and to institute
The acetylacetone,2,4-pentanedione that butyl titanate quality 20-80% is added in butyl titanate ethanol solution is stated, is stirred vigorously 10-30min；Press
Aluminium, titanium mol ratio 2：1 is slowly added into the aluminum nitrate ethanol solution prepared in butyl titanate ethanol solution；Add nitric acid
Mixed liquor pH value is adjusted to 5-7, polyethylene glycol is eventually adding and makees scattered pore creating material, dosage is the 0.5-5% of solvent volume, acutely
Stirring obtains metatitanic acid Alumina gel；It is soluble in water with cerous nitrate, the cerous nitrate aqueous solution is formed, using ammonium bicarbonate aqueous solution as precipitating reagent
According to Ce and HCO3 -Mol ratio 1：2-3 is mixed, while adds mixed solution quality 1-2% polyethylene glycol as dispersant, play
Strong stirring 10-30min, obtains cerous carbonate colloidal sol；According to Ce and Al mol ratios it is 0.1- by metatitanic acid Alumina gel and cerous carbonate colloidal sol
10 ratio mixing, and after being stirred vigorously 10-30min, drying is filtered, 1-5h, the powder in ball mill are dried at 500-700 DEG C
It is broken to obtain the aluminium titanates-cerium oxide fire-retardant particles.
2. fire retardant according to claim 1, it is characterised in that the particle diameter of the aluminium titanates-cerium oxide fire-retardant particles is
10-100 microns.
3. fire retardant according to claim 1, it is characterised in that the molecular weight of the polyethylene glycol is 200-4000.
4. fire retardant according to claim 1, it is characterised in that the metatitanic acid Alumina gel and cerous carbonate colloidal sol according to Ce and
The ratio that Al mol ratios are 0.5-2 mixes.
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