CN106007480B - A kind of preparation method of the fire retardant man-made stone containing magnesium aluminate spinel - Google Patents
A kind of preparation method of the fire retardant man-made stone containing magnesium aluminate spinel Download PDFInfo
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- CN106007480B CN106007480B CN201610456408.9A CN201610456408A CN106007480B CN 106007480 B CN106007480 B CN 106007480B CN 201610456408 A CN201610456408 A CN 201610456408A CN 106007480 B CN106007480 B CN 106007480B
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- aluminate spinel
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 32
- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000010982 man-made stone Substances 0.000 title claims abstract description 9
- -1 magnesium aluminate Chemical class 0.000 title claims description 26
- 239000011777 magnesium Substances 0.000 title claims description 15
- 239000011029 spinel Substances 0.000 title claims description 15
- 229910052749 magnesium Inorganic materials 0.000 title claims description 14
- 239000002969 artificial stone Substances 0.000 claims abstract description 19
- 229910026161 MgAl2O4 Inorganic materials 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 6
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000005011 phenolic resin Substances 0.000 claims abstract description 6
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 6
- 239000010453 quartz Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 14
- 239000002808 molecular sieve Substances 0.000 claims description 12
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 12
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 claims description 10
- 238000005498 polishing Methods 0.000 claims description 10
- 238000007711 solidification Methods 0.000 claims description 10
- 230000008023 solidification Effects 0.000 claims description 10
- 229920000877 Melamine resin Polymers 0.000 claims description 8
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 7
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 7
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000009938 salting Methods 0.000 claims description 6
- 239000003643 water by type Substances 0.000 claims description 6
- 229910015900 BF3 Inorganic materials 0.000 claims description 5
- 239000010445 mica Substances 0.000 claims description 5
- 229910052618 mica group Inorganic materials 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 3
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 claims 2
- 238000001914 filtration Methods 0.000 claims 1
- 229910001562 pearlite Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 19
- 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 abstract description 17
- 230000000694 effects Effects 0.000 abstract description 10
- 230000032683 aging Effects 0.000 abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 229910001051 Magnalium Inorganic materials 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 238000002242 deionisation method Methods 0.000 description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 206010030113 Oedema Diseases 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 239000012266 salt solution Substances 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- 229910020068 MgAl Inorganic materials 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000005034 decoration Methods 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 239000010451 perlite Substances 0.000 description 3
- 235000019362 perlite Nutrition 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000003712 anti-aging effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 235000019504 cigarettes Nutrition 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000004079 fireproofing Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 150000004291 polyenes Chemical class 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- DMGNFLJBACZMRM-UHFFFAOYSA-N O[P] Chemical compound O[P] DMGNFLJBACZMRM-UHFFFAOYSA-N 0.000 description 1
- 241000907903 Shorea Species 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003124 biologic agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011365 complex material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 235000003642 hunger Nutrition 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 230000003434 inspiratory effect Effects 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000000941 radioactive substance Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 125000005624 silicic acid group Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000037351 starvation Effects 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B26/12—Condensation polymers of aldehydes or ketones
- C04B26/122—Phenol-formaldehyde condensation polymers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/0093—Aluminates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00017—Aspects relating to the protection of the environment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The preparation method of the present invention relates to a kind of fire retardant man-made stone containing magnoferrite, the nano magnalium spinelle MgAl2O4With special structure, good inorganic nanometer oxide material can be used as, it is added in talcum powder/phenolic resin/quartz, improve the heat resistance and intensity of artificial stone, the ageing time for reducing artificial stone can keep non-degradable for a long time under high temperature action, and can also keep preferable flame retardant effect, increase carbon left, greatly improves LOI loss on ignition indexes.
Description
Technical field
The present invention relates to a kind of preparation methods of the fire retardant man-made stone comprising nano magnalium spinelle, belong to construction material neck
Domain.
Background technology
With the promotion of people's living standard, the improvement of living conditions, interior decoration industry is grown rapidly, decoration material
Dosage is very big, wherein stone material be it is a kind of most generally use, one of most basic building materials are widely used in ground, metope and table top
Mat formation.Lithotome cost of winning is high, pollution is big, and contains a large amount of naturally occurring radioactive substances, to human health damage compared with
Greatly.With the continuous development of Material Field, the performance of artificial stone material is gradually improved, close to be even more than lithotome,
Increasingly received by market and user, is widely used in cabinet, bathroom, ground, wall decoration.But current artificial stone
Material still has that intensity is low, abrasion-resistant surface is poor, flame-proof heat-resistant performance is not strong, the disadvantage of surface gloss difference.
Invention content
For many deficiencies existing for existing artificial stone, the present invention provides a kind of fire retardant man-made stone containing magnesium aluminate spinel
Preparation method, be prepared in accordance with the following steps：
（1）Prepare compound magnesium aluminate spinel MgAl2O4；
（2）By 70-90 parts of talcum powder, 50-60 parts of phenolic resin, 6-10 parts of boron trifluoride, 10-20 parts of white carbon, pearl
25-30 parts of rock powder end, 5-15 parts of melamine, 5-15 parts of triethyl phosphate, 5-15 parts of hydroxyapatite, 5-15 parts of mica sheet,
50-70 parts quartzy, 5-10 parts of molecular sieve SBA-15 and step（1）Obtained MgAl2O4 10-20 parts of mixing, pour into high-speed stirred
Machine is first used 1000 revs/min of speed to stir 30 minutes, is then stirred with 3000 revs/min of speed at 50 DEG C at room temperature
The batch mixing stirred evenly is discharged, is uniformly taped against on making sheet mold by 30min, and then making sheet mold is placed in vacuum environment and is done
Dry curing molding, the artificial stone blank being removed from the molds after solidification carries out fixed thick, polishing to blank, polishing treatment is hindered
Fire artificial stone.
Wherein, the step（1）Middle MgAl2O4Preparation method be：0.02molMg (NO are weighed respectively3)2· 6H2O、
0.04molAl(NO3)3 9H2O is dissolved in 50ml deionization oedema, matches to obtain mixing salt solution, takes 0.04molNa2CO3、
0.06molNaOH is dissolved in 50ml deionized waters, and then quickly stirring, is added aqueous slkali by salting liquid, pH is made to be maintained at 9-11,
It is uniformly mixed, precipitation is filtered, deionized water is washed till neutrality, 8-10h is dried in 80-100 DEG C of baking oven, then at 800-1000 DEG C
Muffle kiln roasting 4-6h.
Wherein, the preparation process of the SBA-15 molecular sieves is：Under conditions of 35-40 DEG C, by three block surface-active
Agent P123 is dissolved in appropriate amount of deionized water, and ethyl orthosilicate (TEOS), hydrochloric acid (HCl) are added thereto, stirs to continuing vigorous
For 24 hours, it is packed into 100-180 DEG C of crystallization in polytetrafluoroethylene (PTFE) bottle for 24 hours, to be filtered, washed and dried, 5-8h is finally calcined at 550 DEG C, so
After be filtered, washed and dried, obtained white powder is SBA-15, and the molar ratio of each raw material is about TEOS：P123：HCl：
H2O=1：0.017：5.88：136.
Wherein, step（2）Middle dry solidification forming temperature is 50-65 DEG C, preferably 55-60 DEG C.
Wherein, magnesium aluminate spinel average grain diameter is 20-65nm, preferably 25-45nm.
Beneficial effects of the present invention：
Phosphorus and phosphorus-containing compound fire retardant are listed as three big flame-retardant systems with halogen system, inorganic system.Triethyl phosphate, hydroxyl phosphorus
The flame retardant effect of the phosphorus series compounds such as lime stone is preferable, because the metaphosphoric acid generated when burning can be grouped to stable poly state, at
For the protective layer of burning point, the contact by combustion things with oxygen can be completely cut off.The phosphoric acid and poly-metaphosphoric acid of generation are all then strong acid, are had
Very strong dehydration property can make polymer dehydration carbonization, and form charring layer in polymer surfaces, reach starvation and prevent combustion
The purpose of burning.
Melamine has the advantages that Halogen, low toxicity, low cigarette, and nitrogenous flame ratardant is preferable in the flame retardant effect of polyester plastics,
It is especially combined with phosphorus flame retardant, Intumscent Flame Retardant System can be formed, by the synergistic effect of the two, can be greatly improved
The flame retardant effect of polyalkenylesters hydrocarbon artificial stone.The application uses melamine and is applied in combination with triethyl phosphate, hydroxyapatite,
And the ratio of three is adjusted, so that three is played synergistic effect, forms Intumscent Flame Retardant System, experiments have shown that, three（Melamine
Amine：Triethyl phosphate：Hydroxyapatite）Best mass ratio is 1:1:1, flame retardant effect can be greatly improved.Nano inorganic oxygen
Compound is the good selection of fire retardant, such as nano magnesia, and nano zine oxide etc. all can serve as nano inorganic oxide resistance
Combustion agent is added in polyene ester material.Due to nano effect, Preparing Organic-inorganic Nano Hybrid Material have more conventional polymer/
Filler compound is incomparable a little, for example density is small, high mechanical strength, inspiratory and permeability, especially heat-resisting
Property and anti-flammability can be greatly improved.Further, some scholars study the clays class laminar silicic acids such as concave convex rod, montmorillonite
The flame retardant property of salt nanocomposite, above-mentioned inorganic material have different degrees of flame retardant effect.Perovskite structure oxide
ABO3 has unique optics, electricity and magnetic performance, is widely used in terms of biological agent ceramics, has thermal stability
It is good, at low cost, absorption oxygen can be carried out according to B selections, A, B atom, which can be mentioned, adjusts Lattice Oxygen quantity and activity.Mesh
It is preceding that resistance is used as using the more excellent nano-perovskite material of structure or similar polymetallic metal composite oxide not yet
Combustible material.
The aerial burning of high-molecular compound is a kind of very fierce oxidation reaction, belongs to chain reaction course.
It is proliferated a large amount of active hydroxyl free radicals in combustion process, when hydroxyl free radical and high-molecular compound meet, generates hydrocarbon
Compound free radical and water, in the presence of oxygen, hydrocarbon radical decomposition, and form new hydroxyl free radical.So
Cycle, makes combustion reaction constantly continue.The mechanism of action of fire retardant is more complicated, including many factors, but mainly by adopting
Burn cycle is prevented with either physically or chemically.
The present invention uses magnesium aluminate spinel as inorganic nano flame retardant constituent for the first time, by itself and molecular sieve SBA-15 and point
Polyene material is added in spar together, is mixed to form fire-retardant compounding agent, moreover it is possible to which the intensity for further increasing complex material compensates for point
The defect of flexible difference, forms hard and soft complementation in son sieve material, and inorganic material is carried out skeletonizing or intercalation, forms spatial stability
Structure controls the migration rate of space charge, improves charge movement rate, is conducive to capture or detrapping, avoids charge
Polymerization improves flame retardant property to avoid making the artificial stone materials such as its aging, the inflammable usually problem, increases intensity, increases
Add carbon left, it is ageing-resistant to improve LOI indexes.
The artificial stone of the present invention due to using dimension stone of magnesia alumina spinel for the first time, using its advantage space structure, and and SBA-
15 molecular sieves are compound, and a part can generate more inorganic nano flame-retardant composition, remove from and be individually added into inorganic nano magnesia
Equal inorganic anti-flaming materials, another part can utilize the skeleton structure of space omission and SBA-15 molecular sieves, optimize polymeric material
The carbon-forming performance of material improves LOI indexes, and the organic backbone in SBA-15 molecular sieves can be further multiple with polyene material
It closes, is conducive to comprehensive covering of fire proofing, greatly improves flame retardant property.Aging can be substantially reduced, the resistance to of artificial stone is improved
High temperature, use intensity and resistance to flame retardant property.
The application has studied including composite material MgAl2O4With molecular sieve SBA-15 to the fire-retardant and power of quartzy composite material
Performance is learned, by thering are limited oxygen index, vertical combustion and mechanical property tests to measure, it is known that composite material combination property is excellent, property
Energy stabilization, oxygen index (OI) height, good flame retardation effect, effect are lasting, cheap;It is non-toxic by non-volatile, smog is small, the compound resistance
Combustible material has fire-retardant, suppression cigarette and the function of reducing toxic gas concurrently, and being a kind of non-environmental-pollution fire proofing has commercial Application
Foreground.
Specific implementation mode
The present invention will be further described in detail with reference to the specific embodiments.
Embodiment 1
（1）Prepare compound magnesium aluminate spinel MgAl2O4：
(a)MgAl2O4It prepares：0.02molMg (NO are weighed respectively3)2· 6H2O、0.04molAl(NO3)3·9H2O is dissolved in
50ml deionization oedema matches to obtain mixing salt solution, 0.04molNa2CO3,0.06molNaOH is taken to be dissolved in 50ml deionized waters,
Then quickly stirring, is added aqueous slkali by salting liquid, PH is made to be maintained at 9-11, is uniformly mixed, and precipitation is filtered, deionization washing
To neutrality.8h is dried in 80 DEG C of baking ovens.Then in 800 DEG C of Muffle kiln roasting 4-6h.
(b) prepared by SBA-15：Under conditions of 40 DEG C, three block surfactant P123 is dissolved in appropriate amount of deionized water,
Ethyl orthosilicate (TEOS), hydrochloric acid (HCl) are added thereto, stirs to continuing vigorous for 24 hours, is packed into 120 in polytetrafluoroethylene (PTFE) bottle
DEG C crystallization for 24 hours, is filtered, washed and dried, and 6h is finally calcined at 550 DEG C, is then filtered, washed and dried, obtained white powder
End is SBA-15, spare；
（2）By 70 parts of talcum powder, 50 parts of phenolic resin, 6 parts of boron trifluoride, 10 parts of white carbon, 25 parts of perlite powder,
5 parts of melamine, 5 parts of triethyl phosphate, 5 parts of hydroxyapatite, 5 parts of mica sheet, quartz 50 parts, 5 parts of molecular sieve SBA-15 and
The MgAl that above-mentioned steps obtain2O4 10 parts of mixing, pour into homogenizer, first 1000 revs/min of speed are used to stir at room temperature
It mixes 30 minutes, 30min is then stirred with 3000 revs/min of speed at 50 DEG C, the batch mixing stirred evenly is discharged, is uniformly taped against
On making sheet mold, making sheet mold is then placed in vacuum environment the dry solidification at 50 DEG C and is molded, solidification is removed from the molds
Artificial stone blank afterwards carries out fixed thick, polishing to blank, polishing treatment obtains fire retardant man-made stone.
Embodiment 2
（1）Prepare compound magnesium aluminate spinel MgAl2O4：
(a)MgAl2O4It prepares：Weigh respectively 0.02molMg (NO3) 2 6H2O, 0.04molAl (NO3) 3 9H2O be dissolved in
50ml deionization oedema matches to obtain mixing salt solution, 0.04molNa2CO3,0.06molNaOH is taken to be dissolved in 50ml deionized waters,
Then quickly stirring, is added aqueous slkali by salting liquid, PH is made to be maintained at 9-11, is uniformly mixed, and precipitation is filtered, deionization washing
To neutrality.10h is dried in 100 DEG C of baking ovens.Then in 800 DEG C of Muffle kiln roasting 4h.
(b) prepared by SBA-15：Under conditions of 40 DEG C, three block surfactant P123 is dissolved in appropriate amount of deionized water,
Ethyl orthosilicate (TEOS), hydrochloric acid (HCl) are added thereto, stirs to continuing vigorous for 24 hours, is packed into 120 in polytetrafluoroethylene (PTFE) bottle
DEG C crystallization for 24 hours, is filtered, washed and dried, and 6h is finally calcined at 550 DEG C, is then filtered, washed and dried, obtained white powder
End is SBA-15, spare；
（2）By 80 parts of talcum powder, 55 parts of phenolic resin, 8 parts of boron trifluoride, 15 parts of white carbon, 28 parts of perlite powder,
10 parts of melamine, 10 parts of triethyl phosphate, 10 parts of hydroxyapatite, 10 parts of mica sheet, quartzy 60 parts, molecular sieve SBA-15 8
The MgAl that part and above-mentioned steps obtain2O415 parts of mixing, pour into homogenizer, first use 1000 revs/min of speed at room temperature
Degree stirring 30 minutes, then stirs 30min at 50 DEG C with 3000 revs/min of speed, the batch mixing stirred evenly is discharged, uniformly
It is taped against on making sheet mold, then making sheet mold is placed in vacuum environment and is molded in 60 DEG C of dry solidifications, be removed from the molds solid
Artificial stone blank after change carries out fixed thick, polishing to blank, polishing treatment obtains fire retardant man-made stone.
Embodiment 3
（1）Prepare compound magnesium aluminate spinel MgAl2O4；
(a)MgAl2O4It prepares：0.02molMg (NO3) is weighed respectively2 6H2O、0.04molAl(NO3) 3 9H2O are dissolved in
50ml deionization oedema matches to obtain mixing salt solution, 0.04molNa2CO3,0.06molNaOH is taken to be dissolved in 50ml deionized waters,
Then quickly stirring, is added aqueous slkali by salting liquid, PH is made to be maintained at 9-11, is uniformly mixed, and precipitation is filtered, deionization washing
To neutrality.10h is dried in 80 DEG C of baking ovens.Then in 800 DEG C of Muffle kiln roasting 6h.
(b) prepared by SBA-15：Under conditions of 40 DEG C, three block surfactant P123 is dissolved in appropriate amount of deionized water,
Ethyl orthosilicate (TEOS), hydrochloric acid (HCl) are added thereto, stirs to continuing vigorous for 24 hours, is packed into 120 in polytetrafluoroethylene (PTFE) bottle
DEG C crystallization for 24 hours, is filtered, washed and dried, and 6h is finally calcined at 550 DEG C, is then filtered, washed and dried, obtained white powder
End is SBA-15, spare；
（2）By 90 parts of talcum powder, 60 parts of phenolic resin, 10 parts of boron trifluoride, 20 parts of white carbon, 30 parts of perlite powder,
15 parts of melamine, 15 parts of triethyl phosphate, 15 parts of hydroxyapatite, 15 parts of mica sheet, quartzy 70 parts, molecular sieve SBA-15
10 parts of MgAl obtained with above-mentioned steps2O420 parts of mixing, pour into homogenizer, first use 1000 revs/min at room temperature
Speed stirs 30 minutes, then stirs 30min at 50 DEG C with 3000 revs/min of speed, the batch mixing stirred evenly is discharged,
It is even to be taped against on making sheet mold, then making sheet mold is placed in vacuum environment and is molded in 65 DEG C of dry solidifications, is removed from the molds
Artificial stone blank after solidification carries out fixed thick, polishing to blank, polishing treatment obtains fire retardant man-made stone.
Comparative example 1
It is added without nano magnalium spinelle, other experiment parameters are the same as embodiment 1.
Comparative example 2
SBA-15 materials are added without, other experiment parameters are the same as embodiment 1.
Comparative example 3
The magnesium aluminate spinel of the present invention is replaced using concave convex rod, other experiment parameters are the same as embodiment 1.
Comparative example 4
The SBA-15 for replacing the present invention is sieved using common molecular, other experiment parameters are the same as embodiment 1.
Specific detection
Detect the tensile strength (σ t/MPa) of above-mentioned anti-aging artificial stone, elongation at break (δ/ %), carbon left, hardness,
Then above-mentioned anti-aging artificial stone is carried out hot air aging by LOI indexes all over the world by 250 DEG C × 30, then detect tensile strength
Conservation rate (E1/ %) and elongation at break conservation rate (E2/ %), concrete outcome is shown in Table 1.
The each Testing index of 1 artificial stone of table
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | |
| Carbon left, wt% | 18.6 | 196 | 20.1 | 1.19 | 2.1 | 4.4 | 1.5 |
| Hardness, ShoreA | 96 | 95 | 95 | 84 | 75 | 76 | 72 |
| Tensile strength, MPa | 52 | 50 | 48 | 45 | 35 | 46 | 43 |
| Elongation at break % | 550 | 521 | 500 | 380 | 395 | 420 | 405 |
| LOI | 39.3 | 37.5 | 39.0 | 19.1 | 20.1 | 25.1 | 27.4 |
| 250 DEG C × 30 days, LOI | 33.8 | 34.1 | 33.5 | 14.3 | 11.2 | 10.5 | 12.7 |
| 250 DEG C × 30 days, E1/ % | 97.4 | 95.3 | 97.6 | 77.5 | 72.5 | 73.6 | 80.3 |
| 250 DEG C × 30 days, E2/ % | 90.7 | 90.5 | 94.0 | 62.9 | 61.9 | 62.5 | 70.4 |
There are the above results to can be seen that by the way that magnesium aluminate spinel and molecular sieve SBA-15 is added, advantageously reduces insulation material
The density for expecting LDPE/EVA/PVC systems, improves the heat resistance and intensity of insulating materials, reduces the ageing time of insulating materials, carry
High LOI indexes have good anti-flammability, improve carbon left, can keep under high temperature action for a long time（250 DEG C × 30 days）No
Degradation, and by for a long time（250 DEG C × 30 days）Still have higher LOI indexes, flame retardant property still preferable.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those skilled in the art within the technical scope disclosed by the invention, can without the variation that creative work is expected or
It replaces, should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be limited with claims
Subject to fixed protection domain.
Claims (5)
1. a kind of preparation method of the fire retardant man-made stone containing magnesium aluminate spinel, which is characterized in that be prepared in accordance with the following steps：
（1）Prepare compound magnesium aluminate spinel MgAl2O4；
（2）By 70-90 parts of talcum powder, 50-60 parts of phenolic resin, 6-10 parts of boron trifluoride, 10-20 parts of white carbon, crushed crude pearlite
25-30 parts last, 5-15 parts of melamine, 5-15 parts of triethyl phosphate, 5-15 parts of hydroxyapatite, 5-15 parts of mica sheet, quartz
50-70 parts, 5-10 parts of molecular sieve SBA-15 and step（1）Obtained MgAl2O4 10-20 parts of mixing, pour into homogenizer,
It first uses 1000 revs/min of speed to stir at room temperature 30 minutes, is then stirred with 3000 revs/min of speed at 50 DEG C
The batch mixing stirred evenly is discharged, is uniformly taped against on making sheet mold by 30min, and then making sheet mold is placed in vacuum environment and is done
Dry curing molding, the artificial stone blank being removed from the molds after solidification carries out fixed thick, polishing to blank, polishing treatment is hindered
Fire artificial stone.
2. preparation method as described in claim 1, which is characterized in that the step（1）Middle MgAl2O4Preparation method be：Point
Also known as take 0.02mol Mg (NO3)2· 6H2O、0.04mol Al(NO3)3· 9H2O is dissolved in 50ml deionized waters, matches mixed
Salting liquid is closed, 0.04mol Na are taken2CO3, 0.06mol NaOH be dissolved in 50ml deionized waters, then quickly stirring, by salting liquid
Aqueous slkali is added, pH is made to be maintained at 9-11, is uniformly mixed, will precipitation filtering, deionized water is washed till neutrality, in 80-100 DEG C of baking oven
8-10h is dried, then in 800-1000 DEG C of Muffle kiln roasting 4-6h.
3. preparation method as claimed in claim 1 or 2, which is characterized in that step（2）Middle dry solidification forming temperature is 50-
65℃。
4. preparation method as claimed in claim 1 or 2, which is characterized in that step（2）Middle dry solidification forming temperature is 55-
60℃。
5. preparation method as described in claim 1, which is characterized in that magnesium aluminate spinel average grain diameter is 20-65nm.
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| CN201610456408.9A CN106007480B (en) | 2016-06-22 | 2016-06-22 | A kind of preparation method of the fire retardant man-made stone containing magnesium aluminate spinel |
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| JPH1025146A (en) * | 1996-07-09 | 1998-01-27 | M R C Du Pont Kk | Flame retardant acrylic artificial marble |
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| JP4562929B2 (en) * | 2001-02-14 | 2010-10-13 | 独立行政法人農業・食品産業技術総合研究機構 | Cement composition |
| CN1536031A (en) * | 2003-04-11 | 2004-10-13 | 陈书怡 | Polycrystalline state composite and its preparation method |
| CN104710169B (en) * | 2015-03-17 | 2017-12-15 | 武汉科技大学 | A kind of magnesium aluminate spinel superfine powder and preparation method thereof |
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- 2016-06-22 CN CN201810325700.6A patent/CN108483993A/en not_active Withdrawn
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| JPH1025146A (en) * | 1996-07-09 | 1998-01-27 | M R C Du Pont Kk | Flame retardant acrylic artificial marble |
| CN102167540A (en) * | 2010-12-23 | 2011-08-31 | 广州戈兰迪高分子材料有限公司 | Anti-static flame-retardant quartz stone product and manufacturing method thereof |
| CN103396040A (en) * | 2013-07-15 | 2013-11-20 | 肇庆富盛复合材料有限公司 | Artificial solid plane materiel and manufacturing method thereof |
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