CN111664493B - Quick-heating floor heating module - Google Patents

Quick-heating floor heating module Download PDF

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CN111664493B
CN111664493B CN202010441684.4A CN202010441684A CN111664493B CN 111664493 B CN111664493 B CN 111664493B CN 202010441684 A CN202010441684 A CN 202010441684A CN 111664493 B CN111664493 B CN 111664493B
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phosphogypsum
quick
floor heating
heating module
graphite
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CN111664493A (en
Inventor
朱国飞
施辉朝
张启卫
杨步雷
徐韦洪
杨永彬
李贵汶
彭步平
安光文
宋维相
姚孟林
韦明志
王琴
何珍
张燕
米林
徐虎
刘小成
罗进峰
崔俊新
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Guizhou Kailin Phosphogypsum Integration Utilization Co ltd
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Guizhou Kailin Phosphogypsum Integration Utilization Co ltd
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24HEATING; RANGES; VENTILATING
    • F24DDOMESTIC- OR SPACE-HEATING SYSTEMS, e.g. CENTRAL HEATING SYSTEMS; DOMESTIC HOT-WATER SUPPLY SYSTEMS; ELEMENTS OR COMPONENTS THEREFOR
    • F24D3/00Hot-water central heating systems
    • F24D3/12Tube and panel arrangements for ceiling, wall, or underfloor heating
    • F24D3/14Tube and panel arrangements for ceiling, wall, or underfloor heating incorporated in a ceiling, wall or floor
    • F24D3/148Tube and panel arrangements for ceiling, wall, or underfloor heating incorporated in a ceiling, wall or floor with heat spreading plates
    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04FFINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F15/00Flooring
    • E04F15/02Flooring or floor layers composed of a number of similar elements
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24HEATING; RANGES; VENTILATING
    • F24DDOMESTIC- OR SPACE-HEATING SYSTEMS, e.g. CENTRAL HEATING SYSTEMS; DOMESTIC HOT-WATER SUPPLY SYSTEMS; ELEMENTS OR COMPONENTS THEREFOR
    • F24D2220/00Components of central heating installations excluding heat sources
    • F24D2220/20Heat consumers
    • F24D2220/2081Floor or wall heating panels

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  • Engineering & Computer Science (AREA)
  • Architecture (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Civil Engineering (AREA)
  • Structural Engineering (AREA)
  • Floor Finish (AREA)

Abstract

The invention belongs to the field of building materials, and particularly relates to a quick-heating gypsum floor heating module; by activating the phosphogypsum, preparing the heat conduction material and combining with a convenient and simple preparation method, the floor heating module which has the average heat conductivity of 2.41W/(m.k), good heat preservation effect and simple installation is produced by using the industrial byproduct gypsum, so that the utilization rate of the phosphogypsum is increased, and the environmental pollution is reduced.

Description

Quick-heating floor heating module
Technical Field
The invention belongs to the field of building materials, and particularly relates to a quick-heating floor heating module.
Background
The floor heating module is one of main optional components at the tail end of a floor heating system. The auxiliary materials such as the insulation board, the reflection film and the staple bolt in the traditional floor heating system are replaced, and the installation procedure of the floor heating system is greatly simplified. However, floor heating modules made of different materials and in different forms have respective advantages and also have various defects, such as high manufacturing cost, relatively weak compressive strength and the like of a composite module, and the modules made of plastics or PVC have poor fireproof performance, serious fire hazard, short service life and the like.
Phosphogypsum is a solid by-product generated when phosphorite is treated by sulfuric acid in the production of phosphoric acid, about 4-5 tons of phosphogypsum are generated when 1 ton of phosphoric acid is produced, the main component of the phosphogypsum is calcium sulfate dihydrate, and in addition, a small amount of phosphorite, phosphoric acid, fluoride, organic matters, potassium, sodium and other components are contained. The phosphogypsum is one of the by-product gypsums with the largest discharge capacity, and most of the phosphogypsum is stored in a stacking and placing mode due to low utilization rate, so that the ecological environments such as atmosphere, soil, underground water and the like in a stacking land and nearby areas are seriously harmed by improper treatment. Therefore, how to improve the utilization rate of the phosphogypsum is a problem which needs to be solved urgently at present.
Disclosure of Invention
The invention provides a quick-heating floor heating module for solving the problems.
The method is realized by the following technical scheme:
a quick-heating floor heating module comprises the following steps:
1. activating the phosphogypsum:
a. mixing and crushing lime and phosphogypsum according to the mass ratio of 1-2:5-10, adding resin which is 7-14% of the mass of the phosphogypsum and is soaked in an alkaline solution and then dried, and calcining for 20-40min at the temperature of 150-;
b. and (b) adding water with the mass 2-3 times of that of the step (a), cooling, simultaneously dripping hydrogen peroxide with the water weight 30-35% and sodium alginate with the water weight 16-25%, fully stirring, standing, screening to remove agglomerated impurities, and drying the residual phosphogypsum to obtain the activated phosphogypsum.
2. Preparing a heat conduction material:
soaking graphite in methanol of the same amount, drying, soaking in molten silicon dioxide for 12-24h, taking out the graphite, cleaning with steam, drying, and pulverizing to obtain the graphite-silicon intercalation material.
3. Preparing a quick-heating floor heating module:
mixing the activated phosphogypsum and a heat conduction material according to a mass ratio of 10-15:2-4, heating to 90-120 ℃, adding the auxiliary material A, uniformly mixing, adding the auxiliary material B and water when the temperature is reduced to 50-60 ℃, stirring for 10-15min, and casting and molding;
furthermore, the auxiliary material A is one of aggregate-free materials, vitrified microbeads, polyphenyl granules and fine sand stones;
and the auxiliary material B is one or a combination of more of polypropylene fiber, retarder, water reducer and cement.
In conclusion, the beneficial effects of the invention are as follows: according to the invention, by activating the phosphogypsum, preparing the heat conduction material and combining a convenient and simple preparation method, the floor heating module which has the average heat conductivity of 2.41W/(m.k), good heat insulation effect and simple installation is produced by using the industrial byproduct gypsum, so that the utilization rate of the phosphogypsum is increased, and the environmental pollution is reduced.
The traditional pretreatment method for the phosphogypsum is to carry out washing and screening firstly, and compared with the traditional method, when the phosphogypsum is activated, lime, resin and the phosphogypsum are mixed and calcined firstly, and then water is added for sedimentation and washing. When phosphogypsum is directly subjected to hydration pretreatment in a traditional treatment mode, phosphorus impurities can hinder phosphogypsum from being hydrated, so that the product structure is loose, the strength is reduced, the treated phosphogypsum is used as a raw material for preparing a floor heating module, the module is easy to crack when being pressed, the water consumption for washing is large, the energy consumption is high, the investment is large, a large amount of wastewater containing pollutants can be generated, and the wastewater can be discharged only by secondary treatment. If the calcining mode is adopted, the calcining is mostly carried out at a high temperature of more than 400 ℃, the energy consumption is large, and pyrophosphate converted from eutectic phosphorus impurities cannot be completely removed in the subsequent steps. In the application, the intermediate-temperature rapid calcination is firstly carried out, and then the water is added for sedimentation and washing, so that not only is the sequence of the treatment steps changed, but also the process is improved, the lime is added, the pH value of the phosphogypsum is effectively balanced, meanwhile, effective calcium oxide and magnesium oxide contained in the phosphogypsum and resin form a cross-linked component in the subsequent calcination, and pyrophosphate generated in the calcination of the phosphogypsum can be wrapped so as to be completely removed in the subsequent calcination. Meanwhile, the material is blended with resin and calcined, so that the strength is improved, the density is reduced, and the material with light weight and high strength is formed. By adopting a medium-temperature quick calcining mode, eutectic impurities in phosphogypsum crystal lattices can be decomposed, organic impurities can also be decomposed along with the rise of temperature, the decomposed impurities are wrapped by the bonding components formed by lime, and meanwhile, the thermal conductivity of the composite material after calcining is improved. And the water washing is carried out, the added water amount is much less than that of the traditional method, the investment is reduced, the impurities can be further adsorbed and wrapped by adding hydrogen peroxide and sodium alginate, the separation is convenient, the wastewater does not contain impurities such as phosphorus, fluoride and the like, the secondary treatment is not needed, the cost is reduced, and the environment is not stressed. The heat conduction material prepared by graphite-silicon intercalation is added when the floor heating module is prepared, the intercalation treatment is carried out by an impregnation method, the intercalation degree can be effectively controlled, the operation is simple, the heat conduction speed of the floor heating module is accelerated after the intercalation, the hardness, the oxidation resistance and the corrosion resistance of the floor heating module are increased, the service life of the floor heating module is effectively prolonged, and the potential safety hazard is reduced.
Detailed Description
The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.
Example 1
A quick-heating floor heating module comprises the following steps:
1. activating the phosphogypsum:
a. mixing and crushing lime and phosphogypsum according to the mass ratio of 1.5:7, adding resin accounting for 10 percent of the mass of the phosphogypsum, and calcining for 30min at the temperature of 170 ℃;
furthermore, the resin is obtained by soaking in a sodium hydroxide solution for 12h, drying and crushing.
b. And (b) adding water with the mass 3 times that of the phosphogypsum mixture in the step (a) for cooling, simultaneously dripping hydrogen peroxide with the weight 32% of the water and sodium alginate with the weight 20%, fully stirring, standing, screening out agglomerated impurities, and drying the residual phosphogypsum to obtain the activated phosphogypsum.
2. Preparing a heat conduction material:
soaking graphite in methanol of the same amount, drying, soaking in molten silicon dioxide for 18h, taking out the graphite, cleaning with steam, drying, and pulverizing to obtain the graphite-silicon intercalation material.
3. Preparing a quick-heating floor heating module:
mixing the activated phosphogypsum and a heat conduction material according to the mass ratio of 12:3, heating to 110 ℃, adding vitrified micro bubbles accounting for 15% of the mass of the activated phosphogypsum, uniformly mixing, adding an auxiliary material B accounting for 3% of the mass of the activated phosphogypsum and water when the temperature is reduced to 55 ℃, stirring for 15min, and casting and molding;
furthermore, the auxiliary material B is formed by mixing polypropylene fiber and a retarder in equal proportion.
Example 2
A quick-heating floor heating module comprises the following steps:
1. activating the phosphogypsum:
a. mixing and crushing lime and phosphogypsum according to the mass ratio of 2:10, adding resin with the mass of 14% of the phosphogypsum, and calcining for 20min at the temperature of 200 ℃;
furthermore, the resin is obtained by soaking in potassium hydroxide solution for 8h, drying and crushing.
b. And (b) adding water with the mass 3 times that of the phosphogypsum mixture in the step (a) for cooling, dripping hydrogen peroxide with the weight 35% of that of the water and sodium alginate with the weight 25%, fully stirring, standing, screening out agglomerated impurities, and drying the residual phosphogypsum to obtain the activated phosphogypsum.
2. Preparing a heat conduction material:
soaking graphite in methanol of the same amount, drying, soaking in molten silicon dioxide for 24h, taking out the graphite, cleaning with steam, drying, and pulverizing to obtain the graphite-silicon intercalation material.
3. Preparing a quick-heating floor heating module:
mixing the activated phosphogypsum and a heat conduction material according to a mass ratio of 15:4, heating to 120 ℃, adding polyphenyl particles accounting for 20% of the mass of the activated phosphogypsum, uniformly mixing, adding an auxiliary material B accounting for 5% of the mass of the activated phosphogypsum and water when the temperature is reduced to 60 ℃, stirring for 15min, and casting and molding;
and the auxiliary material B is prepared by mixing a water reducing agent and cement according to the proportion of 1: 5.
Example 3
A quick-heating floor heating module comprises the following steps:
1. activating the phosphogypsum:
a. mixing and crushing lime and phosphogypsum according to the mass ratio of 1:5, adding resin accounting for 7 percent of the mass of the phosphogypsum, and calcining at the temperature of 150 ℃ for 40min;
furthermore, the resin is obtained by soaking in a sodium carbonate solution for 48 hours, drying and crushing.
b. And (b) adding water with the mass 2 times that of the phosphogypsum mixture in the step (a) for cooling, simultaneously dripping hydrogen peroxide with the weight 30% of that of water and sodium alginate with the weight 16%, fully stirring, standing, screening out agglomerated impurities, and drying the residual phosphogypsum to obtain the activated phosphogypsum.
2. Preparing a heat conduction material:
soaking graphite in methanol of the same amount, drying, soaking in molten silicon dioxide for 12h, taking out the graphite, cleaning with steam, drying, and pulverizing to obtain the graphite-silicon intercalation material.
3. Preparing a quick-heating floor heating module:
mixing the activated phosphogypsum and a heat conduction material according to the mass ratio of 10:2, heating to 90 ℃, adding a non-aggregate material accounting for 7 percent of the mass of the activated phosphogypsum, uniformly mixing, adding an auxiliary material B accounting for 6 percent of the mass of the activated phosphogypsum and water when the temperature is reduced to 50 ℃, stirring for 10min, and casting and molding;
further, the auxiliary material B is formed by mixing polypropylene fiber, retarder and cement according to the proportion of 1:0.3: 4.
Physical and chemical property experiment of floor heating module
1.1 Experimental methods
Experiments 1-3: under the same conditions as those of the embodiment 1, the heat conduction materials are respectively replaced by graphite-Yb, graphite-Cl and graphite-benzene intercalation materials to prepare the floor heating module;
experiment 4: under the same conditions as those of the embodiment 1, a floor heating module is prepared by pretreating phosphogypsum in a water washing mode;
experiment 5: under the same conditions as those of the embodiment 1, the floor heating module is prepared by pretreating phosphogypsum in a mode of calcining at 400 ℃ for 30 min;
the thermal conductivity and Mohs hardness were measured and compared with those of example 1, and the results are shown in Table 1.
1.2 results of the experiment
TABLE 1
Item Thermal conductivity W/(m.k) Mohs hardness
Example 1 2.41 3
Experiment 1 10.33 >2
Experiment 2 4.28 >2
Experiment 3 3.17 >2
Experiment 4 2.07 2
Experiment 5 1.95 2
Second, testing the effect of heat transfer speed
2.1 Experimental methods
Experiment 6-10: the floor heating modules prepared in experiments 1 to 5 are taken to be 1 square meter each, a floor heating pipe and a wood floor made of the same material are paved in a closed space with the same volume, the time required for the temperature in the closed space to reach 22 ℃ and the temperature change within 12 hours after the temperature is reached are tested under the conditions of 60 ℃ water temperature and 10 ℃ room temperature, and the results are shown in table 2 compared with the example 1.
2.2 results of the experiment
TABLE 2
Figure BDA0002504404790000061
Third, toxicity test of cigarette
3.1 Experimental methods
Experiments 11-15: selecting 5 mice with the weight of 18-24g, carrying out sex randomization, taking the floor heating module prepared in the experiment 1-5 as a material, carrying out a smoke toxicity test according to the GB/T20285-.
The concentration of the smoke is set to be 25mg/L for 30min of contamination experiment, if the mice do not die in the contamination period (including within 1h after contamination), the anesthesia is judged to be qualified under the level, if the mice do not die after 30min of contamination, the weight is not reduced or is reduced, but the body weight is recovered within 3 days, the irritation is judged to be qualified. The status of the mice was recorded within 30min, and the body weight of the mice before the experiment was compared with that of example 1 after 1h, and the results are shown in Table 3.
3.2 results of the experiment
TABLE 3
Item 30min 1h 1d 2d 3d
Example 1 Activity mitigation Body weight not changing Body weight not changing Increase by 0.2g Increase by 0.5g
Experiment 11 Shortness of breath 0.4g lightening 0.6g lightening 0.9g lightening 1.2g lightening
Experiment 12 Shortness of breath 0.3g lightening 0.7g lightening 1.1g lightening 1.5g lightening
Experiment 13 Death of mice - - - -
Experiment 14 Restlessness and restlessness Body weight not changing 0.3g lightening 0.5g lightening 0.8g lightening
Experiment 15 Restlessness and restlessness Body weight not changing 0.4g lightening 0.3g lightening 0.1g lightening
According to the three experimental results, the ground heating module prepared by the application has good heat insulation effect and high heat transfer speed, and the heat transfer speed is higher after the heat conduction material is replaced, but the danger coefficient is also higher by combining a smoke toxicity experiment, so that more harmful substances can be generated when a fire disaster happens. Although the heat preservation effect of the floor heating module prepared by treating the phosphogypsum by the traditional method is not much different from that of the floor heating module, the heat transfer speed is slow, and the heat radiation speed to a room is slow in practical application.

Claims (6)

1. A quick-heating floor heating module is characterized in that the raw material is made of activated phosphogypsum; the activated phosphogypsum is obtained by activating an industrial byproduct gypsum phosphogypsum;
the activation treatment comprises the following steps:
a. mixing and crushing lime and phosphogypsum, adding resin which is soaked by alkali solution and then dried, and calcining for 20-40min at the temperature of 150-200 ℃;
b. and c, adding water with the mass of 2-3 times in the step a, cooling, simultaneously performing sedimentation washing, screening out agglomerated impurities, and drying the residual phosphogypsum to obtain the activated phosphogypsum.
2. The quick-heating floor heating module of claim 1, wherein the sedimentation washing is performed by adding water and simultaneously dropping hydrogen peroxide and sodium alginate, fully stirring and standing.
3. A method for manufacturing a quick-heating floor heating module according to claim 1, comprising the steps of: mixing the activated phosphogypsum with a heat conduction material, heating to 90-120 ℃, adding the auxiliary material A, uniformly mixing, adding the auxiliary material B and water when the temperature is reduced to 50-60 ℃, stirring for 10-15min, and casting and molding.
4. The preparation method of the quick-heating floor heating module as claimed in claim 3, wherein the auxiliary material A is one of aggregate-free material, vitrified micro bubbles, polyphenyl granules and fine sand;
and the auxiliary material B is one or a combination of more of polypropylene fiber, retarder, water reducer and cement.
5. The method for manufacturing a quick-heating floor heating module as claimed in claim 3, wherein the heat conductive material is a graphite-silicon intercalation material.
6. The preparation method of the quick-heating floor heating module according to claim 5, wherein the preparation method of the graphite-silicon intercalation material comprises the following steps: soaking graphite in methanol, drying, soaking in molten silicon dioxide for 12-24 hr, taking out graphite, cleaning with steam, drying, and pulverizing.
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CN112679182B (en) * 2020-12-24 2022-08-23 贵州磷镁材料有限公司 Preparation and construction method of heat-preservation sound-insulation floor heating terrace

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CN101349099A (en) * 2007-07-20 2009-01-21 柯海艇 Graphitic contented gravel ground warming energy-saving substrate
CN102503341A (en) * 2011-11-23 2012-06-20 苏勇 Ardealite building material and preparation method thereof
CN104628276A (en) * 2015-02-02 2015-05-20 河南聚能新型建材有限公司 Phosphogypsum treatment method
CN104710158A (en) * 2015-02-04 2015-06-17 贵州开磷集团股份有限公司 Ardealite substrate wood-like floor and preparation method thereof
CN108178555A (en) * 2018-02-07 2018-06-19 成都新柯力化工科技有限公司 A kind of fire-retardant composite decorative building floor of ardealite base and preparation method

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Publication number Priority date Publication date Assignee Title
CN100567192C (en) * 2008-07-04 2009-12-09 昆明理工大学 A method for preparing modified phosphogypsum by calcining without water washing
GB2466391B (en) * 2009-10-15 2010-10-20 Michael Trevor Berry Phase change materials with improved fire-retardant properties
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Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101349099A (en) * 2007-07-20 2009-01-21 柯海艇 Graphitic contented gravel ground warming energy-saving substrate
CN102503341A (en) * 2011-11-23 2012-06-20 苏勇 Ardealite building material and preparation method thereof
CN104628276A (en) * 2015-02-02 2015-05-20 河南聚能新型建材有限公司 Phosphogypsum treatment method
CN104710158A (en) * 2015-02-04 2015-06-17 贵州开磷集团股份有限公司 Ardealite substrate wood-like floor and preparation method thereof
CN108178555A (en) * 2018-02-07 2018-06-19 成都新柯力化工科技有限公司 A kind of fire-retardant composite decorative building floor of ardealite base and preparation method

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