CN102408121A - Method for preparing magnesium hydroxide fire retardant with lithium carbonate by-product magnesium oxide slag - Google Patents
Method for preparing magnesium hydroxide fire retardant with lithium carbonate by-product magnesium oxide slag Download PDFInfo
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- CN102408121A CN102408121A CN2011102471392A CN201110247139A CN102408121A CN 102408121 A CN102408121 A CN 102408121A CN 2011102471392 A CN2011102471392 A CN 2011102471392A CN 201110247139 A CN201110247139 A CN 201110247139A CN 102408121 A CN102408121 A CN 102408121A
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- magnesium hydroxide
- slurry
- flame retardant
- manganese dioxide
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 81
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 80
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 80
- 239000003063 flame retardant Substances 0.000 title claims abstract description 79
- 239000002893 slag Substances 0.000 title claims abstract description 27
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000006227 byproduct Substances 0.000 title claims abstract description 15
- 239000000395 magnesium oxide Substances 0.000 title abstract description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title abstract 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title abstract 3
- 229910052808 lithium carbonate Inorganic materials 0.000 title abstract 2
- 239000012535 impurity Substances 0.000 claims abstract description 46
- 238000001035 drying Methods 0.000 claims abstract description 30
- 238000005406 washing Methods 0.000 claims abstract description 30
- 239000000047 product Substances 0.000 claims abstract description 27
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 18
- 238000006703 hydration reaction Methods 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 16
- 238000012216 screening Methods 0.000 claims abstract description 16
- 238000012545 processing Methods 0.000 claims abstract description 10
- 238000012986 modification Methods 0.000 claims abstract description 8
- 230000004048 modification Effects 0.000 claims abstract description 8
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 80
- 239000002002 slurry Substances 0.000 claims description 78
- 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 claims description 69
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 63
- 239000012065 filter cake Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- 239000008399 tap water Substances 0.000 claims description 12
- 235000020679 tap water Nutrition 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 239000004576 sand Substances 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 12
- 239000002699 waste material Substances 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000007822 coupling agent Substances 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 3
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 230000036571 hydration Effects 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000011347 resin Substances 0.000 abstract description 2
- 229920005989 resin Polymers 0.000 abstract description 2
- 239000000945 filler Substances 0.000 abstract 1
- 125000000962 organic group Chemical group 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 abstract 1
- 239000000463 material Substances 0.000 description 18
- 239000000779 smoke Substances 0.000 description 13
- 239000000243 solution Substances 0.000 description 13
- 229910052736 halogen Inorganic materials 0.000 description 12
- 150000002367 halogens Chemical class 0.000 description 12
- 239000011777 magnesium Substances 0.000 description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 8
- 229910052749 magnesium Inorganic materials 0.000 description 8
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 7
- 229910052796 boron Inorganic materials 0.000 description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 6
- 239000003112 inhibitor Substances 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 238000002386 leaching Methods 0.000 description 6
- 229910000077 silane Inorganic materials 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- -1 methacryloxy Chemical group 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 229920001296 polysiloxane Polymers 0.000 description 5
- UIDUKLCLJMXFEO-UHFFFAOYSA-N propylsilane Chemical compound CCC[SiH3] UIDUKLCLJMXFEO-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 241001131796 Botaurus stellaris Species 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 229910019440 Mg(OH) Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 159000000003 magnesium salts Chemical class 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- NFMWFGXCDDYTEG-UHFFFAOYSA-N trimagnesium;diborate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]B([O-])[O-].[O-]B([O-])[O-] NFMWFGXCDDYTEG-UHFFFAOYSA-N 0.000 description 2
- 229920002943 EPDM rubber Polymers 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 125000001118 alkylidene group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012757 flame retardant agent Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a method for preparing a magnesium hydroxide fire retardant with a lithium carbonate by-product magnesium oxide slag. Magnesium oxide slag is subjected to the procedures of impurity removal, grinding, screening, hydration, filtering, washing, drying and surface modification so as to obtain a magnesium hydroxide fire retardant, and waste residue generated from impurity removal can be crushed again and used as a raw material. The whole production process realizes zero discharge and reduces environmental pollution. Chemical bonding between a silane coupling agent and magnesium hydroxide generates the magnesium hydroxide fire retardant with weak surface polarity and good dispersibility. The inorganic terminal of the silane coupling agent is firstly hydrolyzed to form silanol which then reacts with the hydroxy on the filler surface. And the organic group at the other terminal of the coupling agent reacts with resin so as to form firm chemical combination. Thus, hydrophilic and oleophobic surface properties of magnesium hydroxide can be changed, the surface polarity of magnesium hydroxide is reduced, and the dispersibility as well as compatibility of magnesium hydroxide in a polymeric matrix can be improved. Therefore, the mechanical property of magnesium hydroxide in polymer product processing can be enhanced.
Description
Technical field
The present invention relates to a kind of preparation method of flame retardant of magnesium hydroxide, especially prepare the preparation method of flame retardant of magnesium hydroxide, belong to technical field of chemistry with Quilonum Retard by product Natural manganese dioxide slag.
Background technology
The magnesium hydrate powder material as inorganic, press down cigarette, nontoxic fire retardant, widespread use in the high polymeric fire-retardant field is applicable to the fire-retardant of macromolecular materials such as PP, PE, EVA, PVC, EPDM amine and unsaturated polyester and eliminates smoke.It has Heat stability is good, nontoxic, non-volatile, do not produce corrosive gases, the amount of being fuming few, do not produce characteristics such as secondary pollution, be the principal item of low-smoke non-halogen flame-retardant agent system.
Along with the develop rapidly and the environmental requirement of macromolecular material industrial application are increasingly high; It is increasing that market requires inorganic combustion inhibitor; Now the most salable is white lake; Have Heat stability is good, can promote that base material becomes advantages such as charcoal but Marinco H is compared with it, therefore the trend that replaces white lake arranged on fire-retardant market, market outlook are considerable.
Flame-proof magnesium hydroxide is different with Marinco H, pharmaceutical grade Marinco H as the fire retardant of filled and ordinary hydrogen Natural manganese dioxide, environmental protection, it requires, and flame-proof magnesium hydroxide will have the crystal formation rule, surface polarity is weak, specific surface area is little, good dispersivity, with characteristics such as the macromolecular material consistency is good.Otherwise, with the processing of high molecular material process in meet difficulty and can't use as fire retardant.
China is magnesium resource big country, and the magnesium resource reserves are huge in the especially western salt lake.The salt lake is rich magnesium salts lake in four Great Lakes such as the Inner Mongol, Xinjiang, Qinghai, Tibet, and wherein the relatively more concentrated area of magnesium resource is distributed in the Caidamu Basin, Qinghai.Promptly 3,700,000,000 tons of the magnesium salts total amounts of Qinghai Lake, wherein Cha Er sweat salt lake Marinco H reserves surpass 1,500,000,000 tons, occupy the second place of the world.But,, the exploitation of magnesium resource is only rested on the primary stage because salt lake resources exploitation for a long time mainly concentrates on resources such as potassium, lithium, boron.Wherein utilize salt lake resources to produce in the process of Quilonum Retard 10 tons of Natural manganese dioxide waste residues of 1 ton of Quilonum Retard by-product of every production.This not only causes the wasting of resources, mainly is the severe contamination that causes environment and salt lake brine resource.Therefore, in the development and use process in salt lake, strengthen the technical study of salt lake magnesium resource, multipath exploitation China magnesium based compound is very important, and seriation, the high added valueization of accelerating magnesium products are problem demanding prompt solutions.
Quilonum Retard production line by product is Natural manganese dioxide waste residue and hydrochloric acid, and by-product hydrochloric acid is used for removing the boron of bittern on the Quilonum Retard production line at present, also can be used as production marketing.The Natural manganese dioxide waste residue is the white solid granular product, about 100 orders of granularity.Staple is a Natural manganese dioxide, other be impurity such as magnesium borate and acid non-soluble substance, currently generally handle as producing waste residue, do not recycle, do not cause environmental pollution.
The Natural manganese dioxide waste residue is the white solid granular product, about 100 orders of granularity.Staple is a Natural manganese dioxide, other be impurity such as magnesium borate and acid non-soluble substance.
Summary of the invention
The problem that the present invention will solve is to above deficiency, and a kind of method for preparing flame retardant of magnesium hydroxide with Quilonum Retard by product Natural manganese dioxide slag is provided.Adopt this method to prepare Marinco H, solved the recycling problem of waste residue during Quilonum Retard is produced, reduced pollution, made full use of lithium, magnesium resource environment.
For overcoming the above problems; The present invention adopts following technical scheme: a kind of method for preparing flame retardant of magnesium hydroxide with Quilonum Retard by product Natural manganese dioxide slag; It is characterized in that: said preparation method for the Natural manganese dioxide slag through removal of impurities, grinding, screening, hydration reaction, filtration, washing, drying, surface-treated operation, obtain flame retardant of magnesium hydroxide;
A, removal of impurities operation are: at first; In blend tank, add tap water; Drop into the stirring of Natural manganese dioxide slag then and obtain slurry; Magnesian weight percent concentration is 20-30%, and slurry carries out rinsing and rotational flow separation through overflow groove, solid-liquid cyclone separator, removes buoyant impurity in the slurry and is insoluble to the particle of acid;
B, grinding, screening operation are: adopt disintegrating machine to grind in the slurry after the preliminary removal of impurities, through the slurry processing of sieving, remove the grains of sand and agglomerating Natural manganese dioxide then, the granularity of slurry is controlled at≤5 μ m;
C, hydration reaction operation are: in reaction kettle, carry out, add sodium hydroxide solution, be warming up to 100-200 ℃; Soaking time 3-8 hour, slurry basicity was controlled at NaOH≤2.5mol/L, obtained the flame retardant of magnesium hydroxide slurry; Under above condition, slurry hydration basicity, temperature are high more, and specific surface area is more little; Crystal formation is more regular, and product quality is high more.
D, filtration, washing, drying process are: the flame retardant of magnesium hydroxide slurry that obtains is placed in the plate and frame(type)filter press filter, obtain filter cake and filtrating, filtrating is sodium hydroxide solution; Can recycle, transfer to be used for the removal of impurities operation after dense, continue to be used for to allocate the basicity of slurry before the reaction; The filter cake water being washed, mainly is sodium hydroxide and the cl ions that contains in the washing leaching cake again, wash to pH value of filtrate less than 10; Washings reclaims and is used for the basicity of removal of impurities operation with the allotment slurry, adopts flash dryer that filter cake is carried out drying then, drying temperature 140-160 ℃; Air outlet temperature 115-145 ℃, obtain the former powder of flame retardant of magnesium hydroxide;
E, surface modification treatment operation are: the former powder of the flame retardant of magnesium hydroxide that obtains and silane coupling agent are joined height stir in the machine and stir; Be elevated to 60-100 ℃ to temperature then; Be incubated 10-30 minute, can obtain the flame retardant of magnesium hydroxide product of silane coupling agent surface-treated.Through after silane coupler modified, reduced product surface polarity, make Marinco H by the hydrophilic oleophylic that becomes, thereby improved the consistency of product and polymkeric substance.
The Natural manganese dioxide waste residue that obtains among the step a can pass through mechanical disintegration and reuse, and the washings washes in the steps d is alkalescence and can selects bittern to neutralize, and the Marinco H of generation can be used for preparing flame retardant of magnesium hydroxide.
Concrete chemical equation is following:
MgO+H
2O=?Mg(OH)
2
Mg
2B
2O
5+2NaOH+H
2O?=2Mg(OH)
2+2NaBO
2
YRSi(OX)
3+3H
2O?→YRSi(OH)
3+3XOH
YRSi(OH)
3+?Mg(OH)
2?→YRSiO
2?Mg?OH+2H
2O
What YR represented is organo-functional group, can be propyl group, vinyl, amino, epoxy group(ing), methacryloxy, and what OX represented is hydrolyzable group, and OX is generally methoxyl group, oxyethyl group, methoxy ethoxy, acetoxyl group, YRSiO
2Mg OH is the siloxanes that silanol and Marinco H react and take off two water and form.
The present invention adopts above technical scheme; Have the following advantages: the Natural manganese dioxide waste residue is through removal of impurities, grinding, screening, hydration reaction, filtration, washing, drying, surface-treated operation; Obtain flame retardant of magnesium hydroxide, the waste residue that removal of impurities produces can be pulverized once more as raw material and use, and the treated product that obtains of waste discharge that washing produces can be used for producing flame retardant of magnesium hydroxide; Whole process of production realizes zero release, has reduced the pollution to environment.
Silane coupling agent and Marinco H generation chemically bonded, thus obtain that surface polarity is weak, the flame retardant of magnesium hydroxide of good dispersivity.Have two active function groups in the molecular structure of silane coupling agent, one is the functional group that connects with Siliciumatom, claims inorganic end again, and another is the functional group that connects with alkylidene group.Inorganic end after hydrolysis with the Marinco H surface reaction, organic end then with the organic interface effect, thereby improved the effect between the matrix material component.When using as coupling agent, inorganic end at first hydrolysis forms silanol, and then with filling surface on hydroxyl reaction.The organic radical of the coupling agent the other end then with resin reaction, form firm Chemical bond.Thereby changed the surface properties of the hydrophilic oleophobic of Marinco H, reduced the surface polarity of Marinco H, improved its dispersiveness and consistency in polymeric matrix, thereby improved mechanical property and the mechanical property of Marinco H in polymeric articles processing.
Below in conjunction with embodiment the present invention is elaborated.
Embodiment
Embodiment 1, a kind ofly prepares the method for flame retardant of magnesium hydroxide with Quilonum Retard by product Natural manganese dioxide slag, and the Natural manganese dioxide slag obtains flame retardant of magnesium hydroxide through removal of impurities, grinding, screening, hydration reaction, filtration, washing, drying, surface-treated operation;
A, removal of impurities operation are: at first; In blend tank, add tap water; Drop into Natural manganese dioxide slag 100g stirring then and obtain slurry; Magnesian weight percent concentration is 20%, and slurry carries out rinsing and rotational flow separation through overflow groove, solid-liquid cyclone separator, removes buoyant impurity in the slurry and is insoluble to the particle of acid;
B, grinding, screening operation are: adopt disintegrating machine to grind in the slurry after the preliminary removal of impurities, through the slurry processing of sieving, remove the grains of sand and agglomerating Natural manganese dioxide then, the granularity of slurry is controlled at≤5 μ m;
C, hydration reaction operation are: in reaction kettle, carry out, adding concentration is the sodium hydroxide solution of 10.5mol/L, and adjustment slurry basicity is 0.2mol/L, is warming up to 100 ℃, and soaking time is 3h, obtains the flame retardant of magnesium hydroxide slurry;
D, filtration, washing, drying process are: the flame retardant of magnesium hydroxide slurry that obtains is placed in the plate and frame(type)filter press filter, obtain filter cake and filtrating, filtrating is sodium hydroxide solution; Can recycle, transfer to be used for the removal of impurities operation after dense, continue to be used for to allocate the basicity of slurry before the reaction; Filter cake being washed with tap water, mainly is sodium hydroxide and the cl ions that contains in the washing leaching cake again, wash to pH value of filtrate less than 10; Washings reclaims and is used for the basicity of removal of impurities operation with the allotment slurry, adopts flash dryer that filter cake is carried out drying then, 140 ℃ of drying temperatures; 115 ℃ of air outlet temperatures obtain the former powder of flame retardant of magnesium hydroxide;
E, surface modification treatment operation are: the former powder of the flame retardant of magnesium hydroxide that obtains and propyl silane coupling agent are joined height stir in the machine; Be elevated to 100 ℃ to temperature then; Be incubated 20 minutes, can obtain the flame retardant of magnesium hydroxide product of silane coupling agent surface-treated.
Through after silane coupler modified, reduced product surface polarity, make Marinco H by the hydrophilic oleophylic that becomes, thereby improved the consistency of product and polymkeric substance.
Through detecting the quality index of gained flame retardant of magnesium hydroxide such as following table:
| Project | Index |
| Marinco H content (%) | 95.30 |
| Moisture (%) | 0.35 |
| Muriate is (with Cl -Meter) content (%) | 0.18 |
| Boron is (with B 2O 3Meter) content (%) | 1.38 |
| Specific surface area (m 2/g) | 18 |
| Oil-absorption(number) (%) | 85 |
| Crystalline structure | The sheet aggregate |
Above gained flame retardant of magnesium hydroxide is applied to electric cable material with low smoke and halogen free, and the basic components of electric cable material with low smoke and halogen free is 10 parts of EVA, 6 parts of MPE, 120 parts of Marinco Hs, 10 parts of oxidation inhibitor, 1 part of silicone, 5 parts of other additives, and detected result is following:
| Content | Detect data |
| Tensile strength (MPa) | 11.30 |
| Elongation at break (%) | 170 |
| Oxygen index | 38 |
| Hardness | 89 |
| Volume specific resistance (Ω cm) | 3.2×10 15 |
| Melting index (g/10min) | 1.8 |
Embodiment 2, a kind ofly prepare the method for flame retardant of magnesium hydroxide with Quilonum Retard by product Natural manganese dioxide slag, and the Natural manganese dioxide slag obtains flame retardant of magnesium hydroxide through removal of impurities, grinding, screening, hydration reaction, filtration, washing, drying, surface-treated operation;
A, removal of impurities operation are: at first; In blend tank, add tap water; Drop into Natural manganese dioxide slag 100g stirring then and obtain slurry; Magnesian weight percent concentration is 23%, and slurry carries out rinsing and rotational flow separation through overflow groove, solid-liquid cyclone separator, removes buoyant impurity in the slurry and is insoluble to the particle of acid;
B, grinding, screening operation are: adopt disintegrating machine to grind in the slurry after the preliminary removal of impurities, through the slurry processing of sieving, remove the grains of sand and agglomerating Natural manganese dioxide then, the granularity of slurry is controlled at≤5 μ m;
C, hydration reaction operation are: in reaction kettle, carry out, adding concentration is the sodium hydroxide solution of 10.5mol/L, and adjustment slurry basicity is 1.0mol/L, is warming up to 130 ℃, and soaking time is 5h, obtains the flame retardant of magnesium hydroxide slurry;
D, filtration, washing, drying process are: the flame retardant of magnesium hydroxide slurry that obtains is placed in the plate and frame(type)filter press filter, obtain filter cake and filtrating, filtrating is sodium hydroxide solution; Can recycle, transfer to be used for the removal of impurities operation after dense, continue to be used for to allocate the basicity of slurry before the reaction; Filter cake being washed with tap water, mainly is sodium hydroxide and the cl ions that contains in the washing leaching cake again, wash to pH value of filtrate less than 10; Washings reclaims and is used for the basicity of removal of impurities operation with the allotment slurry, adopts flash dryer that filter cake is carried out drying then, 150 ℃ of drying temperatures; 125 ℃ of air outlet temperatures obtain the former powder of flame retardant of magnesium hydroxide;
E, surface modification treatment operation are: the former powder of the flame retardant of magnesium hydroxide that obtains and propyl silane coupling agent are joined height stir in the machine; Be elevated to 60 ℃ to temperature then; Be incubated 10 minutes, can obtain the flame retardant of magnesium hydroxide product of silane coupling agent surface-treated.Through after silane coupler modified, reduced product surface polarity, make Marinco H by the hydrophilic oleophylic that becomes, thereby improved the consistency of product and polymkeric substance.
Through detecting the quality index of gained flame retardant of magnesium hydroxide such as following table:
| Content | Detect data |
| Marinco H content (%) | 95.70 |
| Moisture (%) | 0.30 |
| Muriate is (with Cl -Meter) content (%) | 0.15 |
| Boron is (with B 2O 3Meter) content (%) | 0.76 |
| Specific surface area (m 2/g) | 16 |
| Oil-absorption(number) (%) | 78 |
| Crystalline structure | The sheet aggregate |
Above gained flame retardant of magnesium hydroxide is applied to electric cable material with low smoke and halogen free, and the basic components of electric cable material with low smoke and halogen free is 10 parts of EVA, 6 parts of MPE, 120 parts of Marinco Hs, 10 parts of oxidation inhibitor, 1 part of silicone, 5 parts of other additives, and detected result is following:
| Content | Detect data |
| Slight (MPa) stretches | 10.94 |
| Elongation at break (%) | 180 |
| Oxygen index | 38 |
| Hardness | 89 |
| Volume specific resistance (Ω cm) | 2.9×10 15 |
| Melting index (g/10min) | 2.1 |
Embodiment 3, a kind ofly prepare the method for flame retardant of magnesium hydroxide with Quilonum Retard by product Natural manganese dioxide slag, and the Natural manganese dioxide slag obtains flame retardant of magnesium hydroxide through removal of impurities, grinding, screening, hydration reaction, filtration, washing, drying, surface-treated operation;
A, removal of impurities operation are: at first; In blend tank, add tap water; Drop into Natural manganese dioxide slag 100g stirring then and obtain slurry; Magnesian weight percent concentration is 26%, and slurry carries out rinsing and rotational flow separation through overflow groove, solid-liquid cyclone separator, removes buoyant impurity in the slurry and is insoluble to the particle of acid;
B, grinding, screening operation are: adopt disintegrating machine to grind in the slurry after the preliminary removal of impurities, through the slurry processing of sieving, remove the grains of sand and agglomerating Natural manganese dioxide then, the granularity of slurry is controlled at≤5 μ m;
C, hydration reaction operation are: in reaction kettle, carry out, adding concentration is the sodium hydroxide solution of 10.5mol/L, and adjustment slurry basicity is 1.5mol/L, is warming up to 160 ℃, and soaking time is 8h, obtains the flame retardant of magnesium hydroxide slurry;
D, filtration, washing, drying process are: the flame retardant of magnesium hydroxide slurry that obtains is placed in the plate and frame(type)filter press filter, obtain filter cake and filtrating, filtrating is sodium hydroxide solution; Can recycle, transfer to be used for the removal of impurities operation after dense, continue to be used for to allocate the basicity of slurry before the reaction; Filter cake being washed with tap water, mainly is sodium hydroxide and the cl ions that contains in the washing leaching cake again, wash to pH value of filtrate less than 10; Washings reclaims and is used for the basicity of removal of impurities operation with the allotment slurry, adopts flash dryer that filter cake is carried out drying then, 155 ℃ of drying temperatures; 135 ℃ of air outlet temperatures obtain the former powder of flame retardant of magnesium hydroxide;
E, surface modification treatment operation are: the former powder of the flame retardant of magnesium hydroxide that obtains and propyl silane coupling agent are joined height stir in the machine; Be elevated to 70 ℃ to temperature then; Be incubated 30 minutes, can obtain the flame retardant of magnesium hydroxide product of silane coupling agent surface-treated.Through after silane coupler modified, reduced product surface polarity, make Marinco H by the hydrophilic oleophylic that becomes, thereby improved the consistency of product and polymkeric substance.
Through detecting the quality index of gained flame retardant of magnesium hydroxide such as following table:
| Content | Detect data |
| Marinco H content (%) | 96.20 |
| Moisture (%) | 0.28 |
| Muriate is (with Cl -Meter) content (%) | 0.10 |
| Boron is (with B 2O 3Meter) content (%) | 0.53 |
| Specific surface area (m 2/g) | 13 |
| Oil-absorption(number) (%) | 73 |
| Crystalline structure | The sheet aggregate |
Above gained flame retardant of magnesium hydroxide is applied to electric cable material with low smoke and halogen free, and the basic components of electric cable material with low smoke and halogen free is 10 parts of EVA, 6 parts of MPE, 120 parts of Marinco Hs, 10 parts of oxidation inhibitor, 1 part of silicone, 5 parts of other additives, and detected result is following:
| Content | Detect data |
| Slight (MPa) stretches | 10.95 |
| Elongation at break (%) | 193 |
| Oxygen index | 38 |
| Hardness | 87 |
| Volume specific resistance (Ω cm) | 2.6×10 15 |
| Melting index (g/10min) | 2.3 |
Embodiment 4, a kind ofly prepare the method for flame retardant of magnesium hydroxide with Quilonum Retard by product Natural manganese dioxide slag, and the Natural manganese dioxide slag obtains flame retardant of magnesium hydroxide through removal of impurities, grinding, screening, hydration reaction, filtration, washing, drying, surface-treated operation;
A, removal of impurities operation are: at first; In blend tank, add tap water; Drop into Natural manganese dioxide slag 100g stirring then and obtain slurry; Magnesian weight percent concentration is 28%, and slurry carries out rinsing and rotational flow separation through overflow groove, solid-liquid cyclone separator, removes buoyant impurity in the slurry and is insoluble to the particle of acid;
B, grinding, screening operation are: adopt disintegrating machine to grind in the slurry after the preliminary removal of impurities, through the slurry processing of sieving, remove the grains of sand and agglomerating Natural manganese dioxide then, the granularity of slurry is controlled at≤5 μ m;
C, hydration reaction operation are: in reaction kettle, carry out, adding concentration is the sodium hydroxide solution of 10.5mol/L, and adjustment slurry basicity is 2.0mol/L, is warming up to 180 ℃, and soaking time is 7h, obtains the flame retardant of magnesium hydroxide slurry;
D, filtration, washing, drying process are: the flame retardant of magnesium hydroxide slurry that obtains is placed in the plate and frame(type)filter press filter, obtain filter cake and filtrating, filtrating is sodium hydroxide solution; Can recycle, transfer to be used for the removal of impurities operation after dense, continue to be used for to allocate the basicity of slurry before the reaction; Filter cake being washed with tap water, mainly is sodium hydroxide and the cl ions that contains in the washing leaching cake again, wash to pH value of filtrate less than 10; Washings reclaims and is used for the basicity of removal of impurities operation with the allotment slurry, adopts flash dryer that filter cake is carried out drying then, 160 ℃ of drying temperatures; 145 ℃ of air outlet temperatures obtain the former powder of flame retardant of magnesium hydroxide;
E, surface modification treatment operation are: the former powder of the flame retardant of magnesium hydroxide that obtains and propyl silane coupling agent are joined height stir in the machine; Be elevated to 85 ℃ to temperature then; Be incubated 30 minutes, can obtain the flame retardant of magnesium hydroxide product of silane coupling agent surface-treated.Through after silane coupler modified, reduced product surface polarity, make Marinco H by the hydrophilic oleophylic that becomes, thereby improved the consistency of product and polymkeric substance.
Through detecting the quality index of gained flame retardant of magnesium hydroxide such as following table:
| Content | Detect data |
| Marinco H content (%) | 96.75 |
| Moisture (%) | 0.27 |
| Muriate is (with Cl -Meter) content (%) | 0.09 |
| Boron is (with B 2O 3Meter) content (%) | 0.39 |
| Specific surface area (m 2/g) | 11 |
| Oil-absorption(number) (%) | 65 |
| Crystalline structure | The sheet dispersion-s |
Above gained flame retardant of magnesium hydroxide is applied to electric cable material with low smoke and halogen free; The basic components of electric cable material with low smoke and halogen free is 10 parts of EVA, 6 parts of MPE, 120 parts of Marinco Hs, 10 parts of oxidation inhibitor, 1 part of silicone, 5 parts of other additives; Be weight part more than, detected result is following:
| Content | Detect data |
| Slight (MPa) stretches | 10.52 |
| Elongation at break (%) | 208 |
| Oxygen index | 38 |
| Hardness | 85 |
| Volume specific resistance (Ω cm) | 2.4×10 15 |
| Melting index (g/10min) | 3.0 |
Embodiment 5, a kind ofly prepare the method for flame retardant of magnesium hydroxide with Quilonum Retard by product Natural manganese dioxide slag, and the Natural manganese dioxide slag obtains flame retardant of magnesium hydroxide through removal of impurities, grinding, screening, hydration reaction, filtration, washing, drying, surface-treated operation;
A, removal of impurities operation are: at first; In blend tank, add tap water; Drop into Natural manganese dioxide slag 100g stirring then and obtain slurry; Magnesian weight percent concentration is 30%, and slurry carries out rinsing and rotational flow separation through overflow groove, solid-liquid cyclone separator, removes buoyant impurity in the slurry and is insoluble to the particle of acid;
B, grinding, screening operation are: adopt disintegrating machine to grind in the slurry after the preliminary removal of impurities, through the slurry processing of sieving, remove the grains of sand and agglomerating Natural manganese dioxide then, the granularity of slurry is controlled at≤5 μ m;
C, hydration reaction operation are: in reaction kettle, carry out, adding concentration is the sodium hydroxide solution of 10.5mol/L, and adjustment slurry basicity is 2.5mol/L, is warming up to 200 ℃, and soaking time is 6h, obtains the flame retardant of magnesium hydroxide slurry;
D, filtration, washing, drying process are: the flame retardant of magnesium hydroxide slurry that obtains is placed in the plate and frame(type)filter press filter, obtain filter cake and filtrating, filtrating is sodium hydroxide solution; Can recycle, transfer to be used for the removal of impurities operation after dense, continue to be used for to allocate the basicity of slurry before the reaction; Filter cake being washed with tap water, mainly is sodium hydroxide and the cl ions that contains in the washing leaching cake again, wash to pH value of filtrate less than 10; Washings reclaims and is used for the basicity of removal of impurities operation with the allotment slurry, adopts flash dryer that filter cake is carried out drying then, 160 ℃ of drying temperatures; 145 ℃ of air outlet temperatures obtain the former powder of flame retardant of magnesium hydroxide;
E, surface modification treatment operation are: the former powder of the flame retardant of magnesium hydroxide that obtains and propyl silane coupling agent are joined height stir in the machine; Be elevated to 100 ℃ to temperature then; Be incubated 30 minutes, can obtain the flame retardant of magnesium hydroxide product of silane coupling agent surface-treated.Through after silane coupler modified, reduced product surface polarity, make Marinco H by the hydrophilic oleophylic that becomes, thereby improved the consistency of product and polymkeric substance.
Through detecting the quality index of gained flame retardant of magnesium hydroxide such as following table:
| Content | Detect data |
| Marinco H content (%) | 98.20 |
| Moisture (%) | 0.25 |
| Muriate is (with Cl -Meter) content (%) | 0.07 |
| Boron is (with B 2O 3Meter) content (%) | 0.25 |
| Specific surface area (m 2/g) | 8 |
| Oil-absorption(number) (%) | 56 |
| Crystalline structure | Hexagonal flake, single dispersion |
Above gained flame retardant of magnesium hydroxide is applied to electric cable material with low smoke and halogen free; The basic components of electric cable material with low smoke and halogen free is 10 parts of EVA, 6 parts of MPE, 120 parts of Marinco Hs, 10 parts of oxidation inhibitor, 1 part of silicone, 5 parts of other additives; Be weight part more than, detected result is following:
| Content | Detect data |
| Slight (MPa) stretches | 11.20 |
| Elongation at break (%) | 220 |
| Oxygen index | 39 |
| Hardness | 82 |
| Volume specific resistance (Ω cm) | 2.1×10 15 |
| Melting index (g/10min) | 3.6 |
More than test can be found out, produces flame retardant of magnesium hydroxide with preparation method of the present invention, and its Marinco H content is high, uses above flame retardant of magnesium hydroxide in electric cable material with low smoke and halogen free, and the performance of CABLE MATERIALS is good, and the effect of embodiment 5 is best.
In the hydration reaction operation, when temperature is higher than 200 ℃, cause product to stick together, the quality product variation, when slurry basicity is higher than 2.5mol/L, basicity is high more, and slurry viscosity is big more, and heat-up rate is very slow, and stirs relatively difficulty.
Claims (1)
1. method for preparing flame retardant of magnesium hydroxide with Quilonum Retard by product Natural manganese dioxide slag; It is characterized in that: said preparation method for the Natural manganese dioxide slag through removal of impurities, grinding, screening, hydration reaction, filtration, washing, drying, surface-treated operation, obtain flame retardant of magnesium hydroxide;
A, removal of impurities operation are: at first; In blend tank, add tap water; Drop into the stirring of Natural manganese dioxide slag then and obtain slurry; Magnesian weight percent concentration is 20-30%, and slurry carries out rinsing and rotational flow separation through overflow groove, solid-liquid cyclone separator, removes buoyant impurity in the slurry and is insoluble to the particle of acid;
B, grinding, screening operation are: adopt disintegrating machine to grind in the slurry after the preliminary removal of impurities, through the slurry processing of sieving, remove the grains of sand and agglomerating Natural manganese dioxide then, the granularity of slurry is controlled at≤5 μ m;
C, hydration reaction operation are: in reaction kettle, carry out, add sodium hydroxide solution, be warming up to 100-200 ℃, soaking time 3-8 hour, slurry basicity was controlled at NaOH≤2.5mol/L, obtained the flame retardant of magnesium hydroxide slurry;
D, filtration, washing, drying process are: the flame retardant of magnesium hydroxide slurry that obtains is placed in the plate and frame(type)filter press filter; Obtain filter cake and filtrating, the filter cake water washed, wash to pH value of filtrate less than 10; Adopt flash dryer that filter cake is carried out drying then; Drying temperature 140-160 ℃, air outlet temperature 115-145 ℃, obtain the former powder of flame retardant of magnesium hydroxide;
E, surface modification treatment operation are: the former powder of the flame retardant of magnesium hydroxide that obtains and silane coupling agent are joined height stir in the machine and stir; Be elevated to 60-100 ℃ to temperature then; Be incubated 10-30 minute, obtain the flame retardant of magnesium hydroxide product of silane coupling agent surface-treated.
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| CN105984890A (en) * | 2015-02-26 | 2016-10-05 | 宝山钢铁股份有限公司 | Method for producing flame retardant grade magnesium hydrate from oriented silicon steel magnesium oxide waste |
| CN107722774A (en) * | 2017-10-23 | 2018-02-23 | 河北晨阳工贸集团有限公司 | A kind of flame-retardant water burnt-in sand coating and preparation method thereof |
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| CN104332672A (en) * | 2014-10-09 | 2015-02-04 | 超威电源有限公司 | Washing method of lead-acid storage battery waste lead paste |
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| CN107722774A (en) * | 2017-10-23 | 2018-02-23 | 河北晨阳工贸集团有限公司 | A kind of flame-retardant water burnt-in sand coating and preparation method thereof |
| CN113046098A (en) * | 2019-12-27 | 2021-06-29 | 江苏艾特克阻燃材料有限公司 | Magnesium-boron composite flame retardant and preparation method thereof |
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| CN111450724B (en) * | 2020-04-15 | 2022-05-03 | 山东格润德环保科技有限公司 | Magnesium hydroxide suspension with low impurity content and preparation method thereof |
| CN113929970A (en) * | 2021-11-24 | 2022-01-14 | 北京工业职业技术学院 | Preparation method of magnesium hydroxide coated zinc oxide composite powder |
| CN113929970B (en) * | 2021-11-24 | 2023-03-10 | 北京工业职业技术学院 | Preparation method of magnesium hydroxide coated zinc oxide composite powder |
| CN115527703A (en) * | 2022-09-01 | 2022-12-27 | 北京市昆仑线缆制造有限公司 | Halogen-free low-smoke A-level flame-retardant efficient energy-saving wire for home decoration |
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Application publication date: 20120411 |