CN106554516A - A kind of preparation method of fire proofing material - Google Patents

A kind of preparation method of fire proofing material Download PDF

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Publication number
CN106554516A
CN106554516A CN201611059021.6A CN201611059021A CN106554516A CN 106554516 A CN106554516 A CN 106554516A CN 201611059021 A CN201611059021 A CN 201611059021A CN 106554516 A CN106554516 A CN 106554516A
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Prior art keywords
filtrate
weight
weight portions
preparation
flyash
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CN201611059021.6A
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Chinese (zh)
Inventor
储晓锋
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Jiangsu Dongsteel New Material Co Ltd
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Jiangsu Dongsteel New Material Co Ltd
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Priority to CN201611059021.6A priority Critical patent/CN106554516A/en
Publication of CN106554516A publication Critical patent/CN106554516A/en
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    • 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
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • 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
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • 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
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • 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
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/08Oxygen-containing compounds
    • 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
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic
    • C08K7/26Silicon- containing compounds
    • 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
    • C08K9/00Use of pretreated ingredients
    • C08K9/02Ingredients treated with inorganic substances
    • 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
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • 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
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2206Oxides; Hydroxides of metals of calcium, strontium or barium
    • 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
    • C08K2003/265Calcium, strontium or barium carbonate

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Fireproofing Substances (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention discloses a kind of preparation method of fire proofing material, flyash is mixed after extracting silicon, calcium by the present invention with auxiliary agent, new reinforcing agent is formed, the reinforcing agent of the present invention can effectively improve the stress at definite elongation and hardness of sizing material, improve wearability, heat resistance and flex cracking resistance, reduce setafter break, flyash is efficiently make use of, silicon, calcium is effectively combined, after testing, wherein the recovery rate of silicon is 76 85%, and the recovery rate of calcium is 73 80%.

Description

A kind of preparation method of fire proofing material
Technical field
The invention mainly relates to flyash extraction and application field, more particularly to a kind of preparation method of fire proofing material.
Background technology
Shi Ge big coal countries of China, with coal as power generation substantially fuel.The energy industry stable development of China, generates electricity Ability annual growth is 7.3%, and developing rapidly for power industry brings sharply increasing for flyash discharge capacity, Hazards in Power Plant The flyash total amount discharged every year increases year by year, and nineteen ninety-five flyash discharge capacity is up to 1.25 hundred million tons, 2000 about 1.5 hundred million Ton, reached 300,000,000 tons by 2010, and the development of the national economy and ecological environment to China causes huge pressure.On the other hand, China is the limited country of a per capita resource reserve again, and the comprehensive utilization of flyash is turned waste into wealth, turned bane into boon, Become an important techno-economic policy in China's economic construction, be to solve China's power generation environmental pollution and resource shortage Between contradiction important means, and one of the task of the faced solution of power generation.Through exploitation, flyash is being built work, is being built The all departments such as material, water conservancy are widely used.20 century 70s, worldwide energy crisis, environmental pollution and mineral money The exhausted of source waits the research and development for consumingly exciting utilization of fly ash, repeatedly holds international flyash meeting, studies work Make increasingly deep, application aspect there has also been significant progress.Flyash becomes noticeable aboundresources, valency on international market Lattice are cheap, bring good to and remove all evil emerging building materials raw material and the raw material of chemical products, are favored by people.Research work to flyash Work mostly turns to application study by theoretical research, will particularly focus on Resource analysis and exploitation.Produced using flyash Product being continuously increased, technology is being constantly updated.Total utilization of PCA works compared with the past both at home and abroad, there occurs weight Big change, is mainly shown as:Flyash administer guiding theory from past simple environment angle change be the comprehensive regulation, Recycling;The approach of total utilization of PCA is in terms of past roadbed, embankment, concrete admixture, soil remediation etc. Application, develop in cement raw material, cement mixture, Large Hydro-Junction engineering, pump concrete, mass concrete system The advanced utilization ways such as product, senior filler.The activity of flyash is essentially from active SiO2(vitreum SiO2) and activity Al2O3 (vitreum Al2O3) hydration under certain alkalescence condition.Therefore, activity SiO in flyash2, activity Al2O3With F-CaO (free calcium oxide) be all activity advantageous component, sulphur in flyash a part with soluble plasters (CaSO4) Form is present, and its performance to flyash early strength has the sulphur in certain effect, therefore flyash to flyash activity to be also It is favourable to constitute.3% or so, its formation to gel is favourable to calcium content in flyash.Foreign countries exceed CaO content 10% flyash is referred to as C classes ash, and the low flyash with 10% is referred to as F classes ash.C classes ash itself has certain hydraulicity, Cement mixture can be made, F classes ash often makees concrete admixture, and heat of hydration when it is used than C class ash is low.
A small amount of MgO, Na in flyash2O、K2O etc. generates more vitreum, can promote alkali pasc reaction in hydration reaction. But when content of MgO is too high, adverse effect is brought to stability.
Unburned carbon granule in flyash is loose porous, is that a kind of inert substance is not only harmful to the activity of flyash, and Compacting to flyash is also unfavorable.Excessive Fe2O3It is also unfavorable to the activity of flyash.
The mineral composition of flyash:Due to each intergranular chemical composition of coal dust it is not fully consistent, therefore combustion process The flyash of middle formation defines different thing phases in the cooling procedure discharged.Such as:Silica and alumina content are higher Bead in iron ore, in addition, the content of crystalline mineral is relevant with flyash cooling velocity in flyash.In general, cool down During speed, vitreum content is more:Conversely, the easy crystallization of vitreum.It can be seen that, from thing phase, flyash is crystal ore deposit The mixture of thing and amorphous mineral.The fluctuation range of its mineral composition is larger.General crystalline mineral is quartz, mullite, oxygen Change iron, magnesia, quick lime and anhydrous gypsum etc., amorphous mineral is vitreum, amorphous carbon and secondary limonite, wherein glass Glass body content accounts for more than 50%.
The content of the invention
The object of the invention is exactly for the defect for making up prior art, there is provided a kind of preparation method of fire proofing material.
The present invention is achieved by the following technical solutions:
A kind of preparation method of fire proofing material, comprises the following steps:
(1)Flyash is mixed with the activator of its weight 1-2%, is stirred, at being placed in 600-700 DEG C, calcine 1-2 hours, Fine powder is worn into after cooling, 200-260 mesh sieves are crossed;
(2)Above-mentioned screening material is added in 2-3 times of deionized water, at 50-60 DEG C be incubated 30-40 minutes, filter, obtain filter residue and Calcic filtrate;
(3)The sodium hydroxide solution of addition 7-10mol/L in above-mentioned filter residue, the insulated and stirred 30-50 minute at 90-100 DEG C, Cold filtration, obtains siliceous filtrate, and described NaOH and the envelope-bulk to weight ratio of filter residue are 3-5ml:1g;
(4)Above-mentioned calcic filtrate, siliceous filtrate are mixed, is stirred, controlling reaction temperature is 80-90 DEG C, add reinforcement to help Agent, stirs, and is passed through CO2Content carries out carburizing reagent for the mixed gas of 70-80%, till precipitation is not further added by, stops Gas is only passed through, carbodiimide solution is obtained;
(5)Above-mentioned carbodiimide solution is heated to water at 100-110 DEG C to do, then through microwave drying, wears into fine powder, obtained final product.
A kind of preparation method of fire proofing material, step(1)Described in activator be made up of the raw material of following weight parts 's:Prodan 1-2 weight portions, calcium stearate 2-3 weight portions, sodium fluoride 2-4 weight portions.
A kind of preparation method of fire proofing material, step(4)Described in strengthening helping agent be by the raw material group of following weight parts Into:Phthalic acid ester 4-5 weight portions, sierozem power 3-4 weight portions, Tea Saponin 0.1-0.2 weight portions, silane coupler KH550 0.5-1 weight portions, fine silicon dioxide aeroge 1-2 weight portions, crystal whisker of hexa potassium titanate 1-2 weight portions;Described benefit The consumption of strong auxiliary agent is calcic filtrate, the 10-20% of siliceous filtrate mixed liquor weight.
A kind of preparation method of fire proofing material, the filler of the present invention are mainly used in the elastomeric materials such as tire, sebific duct, sealing ring Reinforcement.
It is an advantage of the invention that:
Flyash through extracting silicon, mix with auxiliary agent after calcium, is formed new reinforcing agent by the present invention, and reinforcing agent of the invention can be with The stress at definite elongation and hardness of sizing material are improved effectively, improve wearability, heat resistance and flex cracking resistance, reduction pull apart permanent change Shape, efficiently make use of flyash, and silicon, calcium are effectively combined, and after testing, wherein the recovery rate of silicon is 76-85%, calcium Recovery rate is 73-80%.
Specific embodiment
Embodiment 1:
A kind of preparation method of fire proofing material, it is characterised in that comprise the following steps:
(1)Flyash is mixed with the activator of its weight 2%, is stirred, be placed in calcining 1-2 hours at 700 DEG C, after cooling Fine powder is worn into, 200 mesh sieves are crossed;
(2)Above-mentioned screening material is added in 2 times of deionized waters, at 59 DEG C, 37 minutes is incubated, is filtered, obtain filter residue and calcic filter Liquid;
(3)The sodium hydroxide solution of 7-10mol/L is added in above-mentioned filter residue, insulated and stirred 38 minutes, cooled at 98 DEG C Filter, obtains siliceous filtrate, and described NaOH and the envelope-bulk to weight ratio of filter residue are 4ml:1g;
(4)Above-mentioned calcic filtrate, siliceous filtrate are mixed, are stirred, controlling reaction temperature is 85 DEG C, adds strengthening helping agent, Stir, be passed through CO2Content is that 80% mixed gas carry out carburizing reagent, till precipitation is not further added by, stops being passed through Gas, obtains carbodiimide solution;
(5)Above-mentioned carbodiimide solution is heated to water at 106 DEG C to do, then through microwave drying, wears into fine powder, obtained final product.
A kind of preparation method of fire proofing material, step(1)Described in activator be made up of the raw material of following weight parts 's:1 weight portion of prodan, 2 weight portion of calcium stearate, 2 weight portion of sodium fluoride.
A kind of preparation method of fire proofing material, step(4)Described in strengthening helping agent be by the raw material group of following weight parts Into:5 weight portion of phthalic acid ester, 4 weight portion of sierozem power, 0.2 weight portion of Tea Saponin, 0.5 weight of Silane coupling agent KH550 Amount part, 2 weight portion of fine silicon dioxide aeroge, 1 weight portion of crystal whisker of hexa potassium titanate;The consumption of described strengthening helping agent is calcic Filtrate, the 19% of siliceous filtrate mixed liquor weight.
Embodiment 2
A kind of preparation method of fire proofing material, it is characterised in that comprise the following steps:
(1)Flyash is mixed with the activator of its weight 1%, is stirred, be placed in calcining 1-2 hours at 670 DEG C, after cooling Fine powder is worn into, 200 mesh sieves are crossed;
(2)Above-mentioned screening material is added in 2 times of deionized waters, at 50 DEG C, 30 minutes is incubated, is filtered, obtain filter residue and calcic filter Liquid;
(3)The sodium hydroxide solution of 7-10mol/L is added in above-mentioned filter residue, insulated and stirred 38 minutes, cooled at 98 DEG C Filter, obtains siliceous filtrate, and described NaOH and the envelope-bulk to weight ratio of filter residue are 3ml:1g;
(4)Above-mentioned calcic filtrate, siliceous filtrate are mixed, is stirred, controlling reaction temperature is 80-90 DEG C, add reinforcement to help Agent, stirs, and is passed through CO2Content is that 76% mixed gas carry out carburizing reagent, till precipitation is not further added by, is stopped Gas is passed through, carbodiimide solution is obtained;
(5)Above-mentioned carbodiimide solution is heated to water at 108 DEG C to do, then through microwave drying, wears into fine powder, obtained final product.
A kind of preparation method of fire proofing material, step(1)Described in activator be made up of the raw material of following weight parts 's:1 weight portion of prodan, 2 weight portion of calcium stearate, 3 weight portion of sodium fluoride.
A kind of preparation method of fire proofing material, step(4)Described in strengthening helping agent be by the raw material group of following weight parts Into:4 weight portion of phthalic acid ester, 3 weight portion of sierozem power, 0.17 weight portion of Tea Saponin, 0.9 weight of Silane coupling agent KH550 Amount part, 1 weight portion of fine silicon dioxide aeroge, 1 weight portion of crystal whisker of hexa potassium titanate;The consumption of described strengthening helping agent is calcic Filtrate, the 18% of siliceous filtrate mixed liquor weight.
Embodiment 3
A kind of preparation method of fire proofing material, it is characterised in that comprise the following steps:
(1)Flyash is mixed with the activator of its weight 2%, is stirred, be placed at 700 DEG C and calcine 1 hour, grind after cooling Into fine powder, 260 mesh sieves are crossed;
(2)Above-mentioned screening material is added in 2 times of deionized waters, at 60 DEG C, 40 minutes is incubated, is filtered, obtain filter residue and calcic filter Liquid;
(3)The sodium hydroxide solution of 7-10mol/l is added in above-mentioned filter residue, insulated and stirred 30 minutes, cooled at 100 DEG C Filter, obtains siliceous filtrate, and described NaOH and the envelope-bulk to weight ratio of filter residue are 5ml:1g;
(4)Above-mentioned calcic filtrate, siliceous filtrate are mixed, are stirred, controlling reaction temperature is 90 DEG C, adds strengthening helping agent, Stir, be passed through CO2Content is that 80% mixed gas carry out carburizing reagent, till precipitation is not further added by, stops being passed through Gas, obtains carbodiimide solution;
(5)Above-mentioned carbodiimide solution is heated to water at 110 DEG C to do, then through microwave drying, wears into fine powder, obtained final product.
A kind of preparation method of fire proofing material, step(1)Described in activator be made up of the raw material of following weight parts 's:1 weight portion of prodan, 3 weight portion of calcium stearate, 2 weight portion of sodium fluoride.
A kind of preparation method of fire proofing material, step(4)Described in strengthening helping agent be by the raw material group of following weight parts Into:4 weight portion of phthalic acid ester, 4 weight portion of sierozem power, 0.1 weight portion of Tea Saponin, 0.5 weight of Silane coupling agent KH550 Amount part, 1 weight portion of fine silicon dioxide aeroge, 1 weight portion of crystal whisker of hexa potassium titanate;The consumption of described strengthening helping agent is calcic Filtrate, the 10% of siliceous filtrate mixed liquor weight.

Claims (4)

1. a kind of preparation method of fire proofing material, it is characterised in that comprise the following steps:
(1)Flyash is mixed with the activator of its weight 1-2%, is stirred, at being placed in 600-700 DEG C, calcine 1-2 hours, Fine powder is worn into after cooling, 200-260 mesh sieves are crossed;
(2)Above-mentioned screening material is added in 2-3 times of deionized water, at 50-60 DEG C be incubated 30-40 minutes, filter, obtain filter residue and Calcic filtrate;
(3)The sodium hydroxide solution of addition 7-10mol/L in above-mentioned filter residue, the insulated and stirred 30-50 minute at 90-100 DEG C, Cold filtration, obtains siliceous filtrate, and described NaOH and the envelope-bulk to weight ratio of filter residue are 3-5ml:1g;
(4)Above-mentioned calcic filtrate, siliceous filtrate are mixed, is stirred, controlling reaction temperature is 80-90 DEG C, add reinforcement to help Agent, stirs, and is passed through CO2Content carries out carburizing reagent for the mixed gas of 70-80%, till precipitation is not further added by, stops Gas is only passed through, carbodiimide solution is obtained;
(5)Above-mentioned carbodiimide solution is heated to water at 100-110 DEG C to do, then through microwave drying, wears into fine powder, obtained final product.
2. a kind of preparation method of fire proofing material according to claim 1, it is characterised in that step(1)Described in activation Agent is made up of the raw material of following weight parts:Prodan 1-2 weight portions, calcium stearate 2-3 weight portions, sodium fluoride 2-4 weights Amount part.
3. a kind of preparation method of fire proofing material according to claim 1, it is characterised in that step(4)Described in reinforcement Auxiliary agent is made up of the raw material of following weight parts:Phthalic acid ester 4-5 weight portions, sierozem power 3-4 weight portions, Tea Saponin 0.1-0.2 weight portions, Silane coupling agent KH550 0.5-1 weight portions, fine silicon dioxide aeroge 1-2 weight portions, six metatitanic acids Potassium whisker 1-2 weight portions;The consumption of described strengthening helping agent is calcic filtrate, the 10-20% of siliceous filtrate mixed liquor weight.
4. the preparation method of a kind of fire proofing material according to claim 1, it is characterised in that the filler of the present invention is mainly used In the reinforcement of the elastomeric materials such as tire, sebific duct, sealing ring.
CN201611059021.6A 2016-11-28 2016-11-28 A kind of preparation method of fire proofing material Pending CN106554516A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107118510A (en) * 2017-06-20 2017-09-01 合肥博之泰电子科技有限公司 It is a kind of for fire proofing material of fire engineering and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104891838A (en) * 2015-05-19 2015-09-09 河北工程大学 Method for extracting silicon and calcium from fly ash for filler reinforcing

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104891838A (en) * 2015-05-19 2015-09-09 河北工程大学 Method for extracting silicon and calcium from fly ash for filler reinforcing

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107118510A (en) * 2017-06-20 2017-09-01 合肥博之泰电子科技有限公司 It is a kind of for fire proofing material of fire engineering and preparation method thereof

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