CN106882827A - It is desuifurized and preparation method thereof for the modified oxidized magnesium of synergistic flame-retarded resin - Google Patents

It is desuifurized and preparation method thereof for the modified oxidized magnesium of synergistic flame-retarded resin Download PDF

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Publication number
CN106882827A
CN106882827A CN201510944025.1A CN201510944025A CN106882827A CN 106882827 A CN106882827 A CN 106882827A CN 201510944025 A CN201510944025 A CN 201510944025A CN 106882827 A CN106882827 A CN 106882827A
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China
Prior art keywords
desuifurized
modified oxidized
preparation
oxidized magnesium
magnesium
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Pending
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CN201510944025.1A
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Chinese (zh)
Inventor
王福明
曾凡东
林宇
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YINGKOU BOHAI TECHNOLOGY Co Ltd
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YINGKOU BOHAI TECHNOLOGY Co Ltd
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Priority to CN201510944025.1A priority Critical patent/CN106882827A/en
Publication of CN106882827A publication Critical patent/CN106882827A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/78Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
    • C01F7/784Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
    • C01F7/785Hydrotalcite
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Fireproofing Substances (AREA)

Abstract

The present invention provides that a kind of modified oxidized magnesium for synergistic flame-retarded resin is desuifurized and preparation method thereof, and the modified oxidized specific preparation method of magnesium waste residue is comprised the following steps:The preparation of aluminum salt solution:Weigh a certain amount of Al (OH)3And NaOH, deionized water is added, heating is boiled, and aluminate solution is obtained.The preparation of modified oxidized magnesium waste residue:Weigh quantitative NaCO3And MgO is desuifurized, add in aluminum salt solution, be sufficiently stirred for, make to be well mixed, ensure the pH value of mixed solution, by mixed solution being sufficiently stirred for, under conditions of reflux condensation mode, react certain hour, then suction filtration, washing, dries, and finally grinds, and obtains modified oxidized magnesium desulfurization slag.The desuifurized water resistance that improve waste residue of modified oxidized magnesium, stability prepared by the present invention, cost is significantly less than in the market like product, with the good market competitiveness.

Description

It is desuifurized and preparation method thereof for the modified oxidized magnesium of synergistic flame-retarded resin
Technical field
The present invention relates to field of fine chemical, more particularly to a kind of modified oxidized magnesium for synergistic flame-retarded resin It is desuifurized and preparation method thereof.
Background technology
In recent years, magnesium oxide flue gas desulfurization technology, a large amount of waste residues that desulfurization is produced gradually are carried out by coal-burning power plant (MDWR) containing magnesium sulfite, magnesium sulfate, magnesium hydroxide, magnesia etc., can be produced with calcination and regeneration Sulfuric acid, but energy consumption is higher and easily causes secondary pollution;Or for producing fertiliser containing magnesium, but content of magnesium is low, produces Product added value is relatively low;Or waste residue is directly arranged outward or filled, it will cause environmental pollution.How effectively to process, Using waste residue and to obtain economic benefit higher and good social benefit be problem demanding prompt solution.
Magnesia, aluminum oxide and iron, calcium, silicon compound for containing in desuifurized etc. are to prepare class neatly The raw material of stone (HTLcs).Due to houghite have can modulation chemical composition and the structure of uniqueness, therefore, Can be used as plastics, rubber, the fire-retardant, stable of chemical fibre Polymer material, insulation, coloring, uvioresistant Etc. multi-functional filling modifier.If being modified desuifurized production houghite and applying, will obtain Good Social benefit and economic benefit.Have not yet to see research in this respect and application report.Prepare neatly Generally using coprecipitation, its synthetic system mainly has stone class compound:
MgCl2/AlCl3/NaOH/Na2CO3;Mg(NO3)2/Al(NO3)3/NaOH/Na2CO3; MgSO4/Al2SO4/NaOH/Na2CO3Deng such synthetic method consumes substantial amounts of NaOH simultaneously in the reaction Generate the NaCl, NaNO of low value3Or Na2SO4And largely discharge, one side cost is of a relatively high, separately On the one hand environmental pollution is caused.
The content of the invention
It is an object of the present invention to be directed to the existing utilization of resources fully, synthetic method imperfection etc. is carried Go out and magnesia FGD waste residue is modified, life is reacted using the MgO in waste residue and sodium aluminate aqueous solution Into the modified waste residue containing houghite, reaction filtrate can all recycle, and the class neatly that will be prepared Stone is used for synergistic fire retarding epoxide resin.
To achieve the above object, the technical solution adopted by the present invention is:It is a kind of for synergistic flame-retarded resin Modified oxidized magnesium is desuifurized and preparation method thereof, comprises the following steps:
(1), the preparation of aluminum salt solution:
Weigh a certain amount of Al (OH)3And NaOH, a certain amount of deionized water is added, heating is boiled, and is obtained Aluminate solution, it is stand-by.
(2) preparation of modified oxidized magnesium waste residue:
Weigh quantitative NaCO3And MgO is desuifurized, it is separately added into aluminum salt solution, is sufficiently stirred for, Make to be well mixed, it is ensured that the pH value of mixed solution, by mixed solution being sufficiently stirred for, reflux condensation mode Under the conditions of, certain hour is reacted, then suction filtration, washing is dried, and is finally ground, and obtains modified oxidized Magnesium desulfurization slag.
Further, the mass ratio of the raw material is:Al(OH)39~11 parts;10~12 parts of NaOH; 4~5 parts of NaCO3;7~8 parts of MgO;110~130 parts of deionized water.
Further, the solution pH value should be controlled between 11~12.
Further, the reflux condensation mode time is 6h.
Further, the condition of affiliated drying process is dry 20~24h at 70~80 DEG C.
Another object of the present invention additionally provides desuifurized the answering in synergistic is fire-retardant of the modified oxidized magnesium With a certain amount of modified oxidized magnesium of addition is desuifurized, and fire retarding epoxide resin oxygen index (OI) can bring up to 25%~30%.
Beneficial effect:Modified oxidized magnesium prepared by the present invention is desuifurized, improves the water resistance of waste residue, steady It is qualitative, and make it that good fire-retardant, smoke suppressing is provided with to macromolecules such as epoxy resin.It has magnalium The performance of hydrotalcite, and cost is significantly less than in the market like product, with the good market competitiveness. With the popularization of magnesium oxide flue gas desulfurization technology and desuifurized modification technology, huge economy, society will be produced Meeting, environmental benefit.
Specific embodiment
The present invention is further described with reference to embodiments:
Embodiment
Weigh 10.4g Al (OH)3With 12g NaOH, it is put into beaker, adds the deionized water of 125mL, Solution boiling is heated to, to prepare aluminate solution.Separately weigh 4.3g Na2CO3With containing 7.5g MgO's It is desuifurized to be added in beaker, it is sufficiently stirred for, make to be well mixed.The pH value for determining mixed solution is about 12, mixed solution is poured into the there-necked flask of 500mL, being sufficiently stirred for, under conditions of reflux condensation mode, instead 6h is answered, then suction filtration, washed, 70 DEG C dry 24h, finally grind.
2g fire retardants are added in 10g epoxy resin, 1g curing agent second two is added after stirring Amine, stirring is injected in homemade aluminum alloy trough, and 24h, 80 DEG C of curing oven 2h are solidified at room temperature.Treat Required batten is trimmed to after being fully cured carries out fire resistance test.
By limiting oxygen index determination, after adding modified oxidized magnesium desuifurized, the oxygen index (OI) of flame-retarded resin is by 21% 25% is brought up to, its fire resistance and smoke suppressing effect been significantly enhanced.
Finally it should be noted that:Various embodiments above is merely illustrative of the technical solution of the present invention, rather than to it Limitation;Although being described in detail to the present invention with reference to foregoing embodiments, the ordinary skill of this area Personnel should be understood:It can still modify to the technical scheme described in foregoing embodiments, or Equivalent is carried out to which part or all technical characteristic;And these modifications or replacement, do not make phase Answer the scope of the essence disengaging various embodiments of the present invention technical scheme of technical scheme.

Claims (7)

1. a kind of modified oxidized magnesium for synergistic flame-retarded resin is desuifurized and preparation method thereof, its feature It is to comprise the following steps:
(1), the preparation of aluminum salt solution:
Weigh a certain amount of Al (OH)3And NaOH, a certain amount of deionized water is added, heating is boiled, and aluminium is obtained Acid salt solution, it is stand-by;
(2) preparation of modified oxidized magnesium waste residue:
Weigh quantitative NaCO3And MgO is desuifurized, it is separately added into aluminum salt solution, is sufficiently stirred for, Make to be well mixed, it is ensured that the pH value of mixed solution, by mixed solution being sufficiently stirred for, reflux condensation mode Under the conditions of, certain hour is reacted, then suction filtration, washing is dried, and is finally ground, and obtains modified oxidized Magnesium desulfurization slag.
2. a kind of modified oxidized magnesium for synergistic flame-retarded resin is desuifurized according to claim 1 And preparation method thereof, it is characterised in that the mass ratio of the raw material is:Al(OH)39~11 parts;NaOH 10~12 parts;4~5 parts of NaCO3;7~8 parts of MgO;110~130 parts of deionized water.
3. a kind of modified oxidized magnesium for synergistic flame-retarded resin is desuifurized according to claim 1 And preparation method thereof, it is characterised in that the solution pH value should be controlled between 11~12.
4. according to claim 1 a kind of modified oxidized magnesium for synergistic flame-retarded resin it is desuifurized and Its preparation method, it is characterised in that the reflux condensation mode time is 6h.
5. according to claim 1 a kind of modified oxidized magnesium for synergistic flame-retarded resin it is desuifurized and Its preparation method, it is characterised in that the condition of affiliated drying process is dry 20~24h at 70~80 DEG C.
6. a kind of low freezing point diesel fuel antiwear additive, it is characterised in that using claim 1-7 any one institute State preparation method to be prepared from, consisting of Mg6Al2(OH)16CO3 2-·4H2O, also contains Si, Ca, The elements such as Fe, its structural formula is represented by
[M2+1-xM3+x(OH)2][A2-]x/2·mH2O,
Wherein M2+It is Mg2+, Ca2+Deng bivalent cation, M3+It is Al3+, Fe3+Deng Tricationic, A2-It is CO3 2-, SiO3 2-Deng dianion.
7. the desuifurized application in synergistic is fire-retardant of modified oxidized magnesium described in claim 6, its feature exists In the modified oxidized magnesium of addition is desuifurized, and fire retarding epoxide resin oxygen index (OI) can bring up to 25%~30%.
CN201510944025.1A 2015-12-16 2015-12-16 It is desuifurized and preparation method thereof for the modified oxidized magnesium of synergistic flame-retarded resin Pending CN106882827A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113716588A (en) * 2021-08-17 2021-11-30 湖南恒光化工有限公司 Low-cost preparation method of magnesium-aluminum hydrotalcite

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113716588A (en) * 2021-08-17 2021-11-30 湖南恒光化工有限公司 Low-cost preparation method of magnesium-aluminum hydrotalcite

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Application publication date: 20170623