WO2019052336A1 - 保温制品及其制备方法 - Google Patents

保温制品及其制备方法 Download PDF

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WO2019052336A1
WO2019052336A1 PCT/CN2018/102961 CN2018102961W WO2019052336A1 WO 2019052336 A1 WO2019052336 A1 WO 2019052336A1 CN 2018102961 W CN2018102961 W CN 2018102961W WO 2019052336 A1 WO2019052336 A1 WO 2019052336A1
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cement
graphene
weight
parts
agent
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PCT/CN2018/102961
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English (en)
French (fr)
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童裳慧
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中晶环境科技股份有限公司
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/08—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B18/02—Agglomerated materials, e.g. artificial aggregates
    • C04B18/027—Lightweight materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/04—Portland cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/06—Aluminous cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/30—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing magnesium cements or similar cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/30—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing magnesium cements or similar cements
    • C04B28/32—Magnesium oxychloride cements, e.g. Sorel cement
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/34—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
    • C04B2111/285—Intumescent materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
    • C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength

Definitions

  • the invention relates to an insulation product and a preparation method thereof, in particular to a self-insulation block and a preparation method thereof.
  • the self-insulation product is a new type of wall material which combines bearing and heat preservation, and has the advantages of low thermal conductivity, heat preservation, light weight, high strength and fire prevention.
  • the main measures to improve the thermal performance of self-insulating products include optimizing the block material composition and block hole structure, making blocks with different cavity structures, filling the cavity structure with thermal insulation products, and adopting composite structure composite thermal insulation products. .
  • the current main measures to improve the thermal performance of thermal insulation products are still relatively complicated, and it is difficult to achieve industrial production.
  • the insulation product still needs further improvement in terms of strength and thermal insulation properties.
  • Graphene is an ultra-thin nano-material composed of pure carbon atoms. It has an extra large specific surface area and its layered structure gives it superior infrared reflectance, excellent mechanical properties and mechanical properties.
  • the special properties of graphene can improve the performance of insulation products.
  • CN106280264A discloses an exterior wall insulation product having excellent mechanical properties, including: 25 to 55 parts by weight of expandable polystyrene, 25 to 35 parts by weight of polyurethane modified epoxy resin, and silicone modified phenolic resin.
  • the above materials completely mix the organic material and the inorganic material together, and the effect of the graphene cannot be fully exerted, so that the flame retarding property of the material is poor and the mechanical strength is not high.
  • Another object of the present invention is to provide a method for preparing a heat-insulating article which is advantageous for industrial scale production and which can obtain a heat-resistant product having good compressive strength and heat insulating properties.
  • the present invention provides a heat insulating article comprising a cement matrix and graphene-modified polystyrene particles; the graphene-modified polystyrene particles having a particle diameter of 2 mm or less and dispersed in the cement matrix;
  • the graphene-modified polystyrene particles are obtained by melt extrusion of graphene and polystyrene resin in the presence of an alkane blowing agent; wherein the weight ratio of graphene to polystyrene resin is 1:1.5 ⁇ 6.
  • the graphene-modified polystyrene particles have an apparent density of 0.025 to 0.035 g/cm 3 ; and the graphene has a purity of not less than 98% and a width of 15 ⁇ m or less. And the thickness is 1 to 3 nm.
  • the polystyrene resin is a flame retardant polystyrene resin
  • the alkane foaming agent is a pentane foaming agent
  • the weight ratio of the graphene-modified polystyrene particles to the cement matrix is 1:5.5 to 15.
  • the heat insulating article of the present invention is obtained by using a raw material comprising the following components:
  • Foam stabilizer 0.5 to 5 parts by weight
  • the cement is selected from the group consisting of magnesium oxysulfide cement, magnesium oxychloride cement, Portland cement, aluminate cement, sulphoaluminate cement, iron aluminate cement, fluoroaluminate One or more of salt cement and phosphate cement;
  • the cement foaming agent is one or more selected from the group consisting of hydrogen peroxide, sodium hydrogencarbonate, ammonium carbonate, azoformamide or azobisisobutyronitrile;
  • the foam stabilizer is selected from one or more of silicone amide, dodecyl dimethyl amine oxide, alkyl alcohol amide, polyacrylamide, polyvinyl alcohol, cellulose, and protein;
  • the agent is selected from one or more of calcium chloride, potassium chloride, sodium sulfate, calcium thiosulfate, triethanolamine or ammonium triisopropoxide;
  • the water reducing agent is selected from magnesium lignosulfonate, lignin
  • the cement is sulphur oxychloride cement
  • the cement foaming agent is hydrogen peroxide
  • the foam stabilizer is silicone amide
  • the early strength agent is triethanolamine
  • the water reducing agent is sodium lignosulfonate.
  • the heat insulating article of the present invention preferably, has a bulk density of 500 to 730 kg/m 3 , a compressive strength of 4.5 to 9 MPa, a thermal conductivity of 0.035 to 0.045 W/m ⁇ K, and a volume water absorption rate of 10 or less. %, and the fire level is A1.
  • the invention also provides a preparation method of the above thermal insulation article, comprising the following steps:
  • the melt blending is carried out using a twin-screw extruder; in the step (2), the static foaming time is 8 to 25 hours.
  • the curing time is 8 to 28 days.
  • the present invention melt-blends graphene and a polystyrene resin, and then foams to form graphene-modified polystyrene particles. This allows the graphene to be uniformly dispersed in the polystyrene particles.
  • As an effective nucleating agent graphene promotes cell nucleation and effectively controls the cell stability of polystyrene.
  • graphene effectively enhances the strength of polystyrene particles.
  • Graphene on the surface of polystyrene particles interacts with external additives such as foam stabilizer, early strength agent and water reducing agent, which effectively reduces the surface tension and effectively inhibits the expansion of polystyrene foam particles in the slurry.
  • graphene has specular reflection infrared properties, which can effectively improve the thermal insulation properties of thermal insulation products.
  • Figure 1 is a schematic view showing the structure of an insulated product of the present invention.
  • thermal insulation article of the present invention examples include, but are not limited to, self-insulating blocks and the like.
  • the thermal insulation article of the present invention comprises a cement matrix and graphene-modified polystyrene particles dispersed in a cement matrix.
  • the graphene-modified polystyrene particles are uniformly dispersed in the cement matrix. This can improve its strength and insulation properties.
  • the heat insulating article of the present invention comprises a cement matrix and graphene-modified polystyrene particles; the graphene-modified polystyrene particles have a particle diameter of 2 mm or less, and are dispersed in the cement In the matrix; the graphene-modified polystyrene particles are obtained by melt extrusion of graphene and polystyrene resin in the presence of an alkane blowing agent; wherein the weight ratio of graphene to polystyrene resin is 1:1.5 ⁇ 6.
  • the graphene-modified polystyrene particles may have a particle diameter of 0.1 to 2 mm, preferably 0.5 to 2 mm. Such a size range can take into account the strength and insulation properties of the insulation product.
  • the graphene-modified polystyrene particles may have an apparent density of from 0.025 to 0.035 g/cm 3 . This is advantageous for improving the strength of the heat insulating article.
  • the graphene may have a purity of not less than 98%, a width of 15 ⁇ m or less, and a thickness of 1 to 3 nm. According to an embodiment of the present invention, the graphene of the present invention has a purity of 99% or more, a width of 3 to 8 ⁇ m, and a thickness of 2 nm. Such graphene is more advantageous for improving the strength and thermal insulation properties of the thermal insulation article.
  • the graphene of the present invention can be obtained by a conventional method. For example, expandable flake graphite is obtained by the Hummers method.
  • the graphene of the present invention is not limited to the Hummers method graphene, and may be graphene obtained by a method such as chemical vapor deposition, SiC epitaxial growth, electrochemistry, mechanical exfoliation or the like.
  • the polystyrene resin may be a flame retardant polystyrene resin. Its purity is preferably 97% or more.
  • the alkane blowing agent may be a C3 to C8 alkane blowing agent, preferably a pentane blowing agent.
  • a pentane blowing agent composed of n-pentane and isopentane can be used.
  • the weight ratio of the graphene to the polystyrene resin may be 1:1.5 to 6, preferably 1:2 to 3.
  • the action of graphene can be fully exerted.
  • graphene particles can promote the nucleation of polystyrene resin cells, effectively control the cell stability, and thus improve the compressive strength of the heat-insulating products.
  • Graphene has a layered structure, which can effectively reduce the thermal conductivity of the heat-insulating product and provide a good heat preservation effect.
  • the weight ratio of the graphene-modified polystyrene particles to the cement matrix may be 1:5.5 to 15, preferably 1:6 to 10. This can take into account the thermal insulation properties and mechanical properties of the insulation products.
  • the heat insulating article can be obtained by using a raw material comprising the following components:
  • Graphene modified polystyrene particles 5 to 15 parts by weight, preferably 8 to 10 parts by weight;
  • the foam stabilizer is 0.5 to 5 parts by weight, preferably 1 to 3 parts by weight;
  • the early strength agent is 0.5 to 2 parts by weight, preferably 0.6 to 1 part by weight;
  • the water reducing agent is used in an amount of 0.5 to 3 parts by weight, preferably 0.6 to 1 part by weight.
  • the cement substrate of the present invention is produced by using a raw material comprising the following components: 60 parts by weight of cement, 30 parts by weight of fly ash, 50 parts by weight of water, and graphene-modified polystyrene particles 10 Parts by weight, 3 parts by weight of the cement foaming agent, 1.6 parts by weight of the foam stabilizer, 0.8 parts by weight of the early strengthening agent, and 0.6 parts by weight of the water reducing agent.
  • the cement blowing agent may be selected from one or more of hydrogen peroxide, sodium hydrogencarbonate, ammonium carbonate, azoformamide or azobisisobutyronitrile; preferably hydrogen peroxide.
  • the foam stabilizer of the present invention may be selected from one or more of silicone amide, dodecyl dimethyl amine oxide, alkyl alcohol amide, polyacrylamide, polyvinyl alcohol, cellulose, and protein.
  • the protein of the invention may be an animal protein or a vegetable protein.
  • the foam stabilizer of the present invention is preferably selected from the group consisting of silicone amide, lauryl dimethyl amine oxide, and polyvinyl alcohol; more preferably, silicone amide.
  • the early strength agent of the present invention may be selected from one or more of calcium chloride, potassium chloride, sodium sulfate, calcium thiosulfate, triethanolamine or triisopropanolamine; preferably triethanolamine.
  • the water reducing agent of the present invention may be selected from one or more of magnesium lignosulfonate, sodium lignosulfonate, melamine formaldehyde resin, and naphthalene-containing water reducing agent; preferably magnesium lignosulfonate or lignosulfonic acid sodium.
  • the cement is selected from the group consisting of magnesium oxysulfide cement, magnesium oxychloride cement, Portland cement, aluminate cement, sulphoaluminate cement, iron aluminate cement, fluoroaluminate cement, phosphate.
  • the cement of the invention is selected from the group consisting of magnesium oxysulfate cement or aluminate cement.
  • the cement is sulphur oxychloride cement
  • the cement foaming agent is hydrogen peroxide
  • the foam stabilizer is silicone amide
  • the early strength agent is triethanolamine
  • the aqueous agent is sodium lignosulfonate.
  • the heat insulating article of the present invention is prepared by using a raw material comprising the following components: 60 parts by weight of magnesium oxysulfide cement, 30 parts by weight of fly ash, 50 parts by weight of water, graphene modified polyphenylene. 10 parts by weight of ethylene particles, 3 parts by weight of hydrogen peroxide, 1.6 parts by weight of silicone amide, 0.8 parts by weight of triethanolamine, and 0.6 parts by weight of sodium lignosulfonate.
  • the heat insulating product of the present invention may have a bulk density of 500 to 730 kg/m 3 , a compressive strength of 4.5 to 9 MPa, a thermal conductivity of 0.035 to 0.045 W/m ⁇ K, a volume water absorption rate of 10% or less, and a fireproof rating of A1.
  • the heat insulating article of the present invention has a bulk density of 650 to 700 kg/m 3 , a compressive strength of 8 to 9 MPa, a thermal conductivity of 0.035 to 0.043 W/m ⁇ K, a volume water absorption rate of ⁇ 9.5%, and a fireproof rating of A1.
  • the bulk density has the meanings well known in the art and will not be described again here.
  • the method for preparing the heat insulating article of the present invention comprises a graphene-modified polystyrene particle forming step and a forming step.
  • the graphene-modified polystyrene particles of the present invention are formed by melt-blending polystyrene resin and graphene at 120 to 150 ° C, then adding an alkane foaming agent, and extruding and granulating to obtain graphene modified poly Styrene particles.
  • alkane blowing agents are particularly suitable for improving insulation properties and strength.
  • the melt blending is carried out using a twin screw extruder.
  • the melt blending temperature is preferably from 130 to 135 °C. Such conditions are advantageous for the uniform dispersion of graphene in the polystyrene resin, thereby improving the strength and thermal insulation properties of the thermal insulation article.
  • the cement substrate forming step of the invention is: mixing cement, fly ash and graphene modified polystyrene particles to obtain a premix; then, the cement foaming agent, the foam stabilizer, the early strength agent, the water reducing agent and Water is added to the premix, and uniformly mixed to obtain a slurry; the slurry is poured into a mold for molding, static foaming, demoulding, and curing to form an insulation product.
  • the types and amounts of the above raw materials are as described above and will not be described herein.
  • the manner of mixing is not particularly limited. For example, these materials are stirred in a high speed mixer.
  • the mold is based on actual needs.
  • the time for standing foaming can be controlled from 8 to 25 hours, preferably from 12 to 20 hours.
  • the curing time can be controlled from 8 to 28 days, preferably from 10 to 15 days. Such conditional control can improve the strength of the insulation article.
  • the graphene in the following examples has a purity of not less than 98%, a width of 15 ⁇ m or less, a thickness of 1 to 3 nm, a cement of magnesium oxysulfide cement, a cement foaming agent of hydrogen peroxide, a foam stabilizer of silicone amide, and an early strength agent.
  • Triethanolamine the water reducing agent is sodium lignosulfonate.
  • the bulk density is determined by Appendix A of GB/T 29060-2012; the compressive strength is measured by GB/T 4111-2013; the thermal conductivity is measured by GB/T 13475-2008; the volumetric water absorption is determined by JC/T 641-2008.
  • the thermal insulation product has a bulk density of 650 kg/m 3 , a compressive strength of 8.5 MPa, a thermal conductivity of 0.043 W/m ⁇ k, a volumetric water absorption of 9.3%, and a fire rating of A1.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
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  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
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Abstract

提供一种保温制品及其制备方法。该保温制品包括水泥基体和石墨烯改性聚苯乙烯颗粒；该颗粒的粒径小于等于2mm，并且分散在水泥基体中；该颗粒是通过石墨烯和聚苯乙烯树脂在烷烃发泡剂的存在下熔融挤出得到的；其中，石墨烯与聚苯乙烯树脂的重量配比为1:1.5～6。该保温制品的强度和保温性能得到提高。

Description

保温制品及其制备方法 技术领域
本发明涉及一种保温制品及其制备方法，尤其是一种自保温砌块及其制备方法。
背景技术
目前，建筑节能越来越受到人们的关注。结构节能一体化成为建材发展和应用的重要方向。现有的保温体系存在裂缝、脱落、施工工艺复杂、不易粘结合外墙等问题。自保温制品是一种集承重和保温于一体的新型墙体材料，具有导热系数低、保温、质轻、强度高、防火等优点。目前，提高自保温制品的热工性能的主要措施包括优化砌块材料成分和砌块孔结构，做含有不同空腔结构的砌块，在空腔结构中填充保温制品，采用组合结构复合保温制品。但是，目前改进保温制品热工性能的主要措施仍然较为复杂，较难实现工业化生产。另外，保温制品在强度和保温性能等方面仍然需要进一步的提高。
石墨烯是一种纯碳原子组成的超薄纳米材料，具有超大的比表面积，其层状结构赋予其具有优越的反射红外线性能、卓越的力学性能和机械性能。利用石墨烯的特殊性能，可以改善保温制品性能。例如，CN106280264A公开了一种具有优异力学性能的外墙板保温制品，包括：可发性聚苯乙烯25～55重量份，聚氨酯改性环氧树脂25～35重量份，有机硅改性酚醛树脂35～45重量份，改性石墨粉8～12重量份，双三丁基酚聚氧乙烯醚1.5～2.5重量份，环氧大豆油3～4重量份，云母粉4～8重量份，石墨烯纳米片8～12重量份，硅酸钙6～10重量份，氧化铝2～4重量份，硅酸钠3～5重量份，氧化镁2～3重量份，煅烧陶土4～12重量份，磷酸1.5～2.5重量份，对甲磺酸1.5～ 2.5重量份，物理发泡剂2～3重量份，水35～55重量份。但是上述材料将有机材料和无机材料完全混合在一起，无法将石墨烯的作用充分发挥，从而使得该材料的阻燃性能较差、力学强度也不高。
发明内容
本发明的一个目的是提供一种保温制品，其具有良好的抗压强度和保温性能。
本发明的另一个目的在于提供一种保温制品的制备方法，其利于工业规模化生产，并能够获得良好的抗压强度和保温性能的保温制品。
本发明提供一种保温制品，其包括水泥基体和石墨烯改性聚苯乙烯颗粒；所述石墨烯改性聚苯乙烯颗粒的粒径小于等于2mm，并且其分散在所述水泥基体中；所述石墨烯改性聚苯乙烯颗粒是通过石墨烯和聚苯乙烯树脂在烷烃发泡剂的存在下熔融挤出得到的；其中，石墨烯与聚苯乙烯树脂的重量配比为1:1.5～6。
根据本发明的保温制品，优选地，所述石墨烯改性聚苯乙烯颗粒的表观密度为0.025～0.035g/cm 3；且所述石墨烯的纯度不小于98％，宽度小于等于15μm，且厚度为1～3nm。
根据本发明的保温制品，优选地，所述聚苯乙烯树脂为阻燃聚苯乙烯树脂；且所述烷烃发泡剂为戊烷发泡剂。
根据本发明的保温制品，优选地，所述石墨烯改性聚苯乙烯颗粒与所述水泥基体的重量配比为1:5.5～15。
根据本发明的保温制品，优选地，所述保温制品采用包括如下组分的原料制得：
水泥 35～90重量份，
粉煤灰 25～55重量份，
石墨烯改性聚苯乙烯颗粒 5～15重量份，
水 35～90重量份，
水泥发泡剂 2～7重量份，
稳泡剂 0.5～5重量份，
早强剂 0.5～2重量份，和
减水剂 0.5～3重量份。
根据本发明的保温制品，优选地，所述水泥选自硫氧镁水泥、氯氧镁水泥、硅酸盐水泥、铝酸盐水泥、硫铝酸盐水泥、铁铝酸盐水泥、氟铝酸盐水泥、磷酸盐水泥中的一种或多种；所述水泥发泡剂选自双氧水、碳酸氢钠、碳酸铵、偶氮甲酰胺或偶氮二异丁腈中的一种或多种；所述稳泡剂选自硅酮酰胺、十二烷基二甲基氧化胺、烷基醇酰胺、聚丙烯酰胺、聚乙烯醇、纤维素、蛋白质中的一种或多种；所述早强剂选自氯化钙、氯化钾、硫酸钠、硫代硫酸钙、三乙醇胺或三异丙醇铵中的一种或多种；所述减水剂选自木质素磺酸镁、木质素磺酸钠、三聚氰胺甲醛树脂、含萘减水剂中的一种或多种。
根据本发明的保温制品，优选地，所述水泥为硫氧镁水泥；所述水泥发泡剂为双氧水；所述稳泡剂为硅酮酰胺；所述早强剂为三乙醇胺；且所述减水剂为木质素磺酸钠。
根据本发明的保温制品，优选地，所述保温制品的容重为500～730kg/m 3，抗压强度为4.5～9MPa，导热系数为0.035～0.045W/m·K，体积吸水率小于等于10％，且防火级别为A1级。
本发明还提供上述保温制品的制备方法，包括如下步骤：
(1)将聚苯乙烯树脂和石墨烯在120～150℃下熔融共混，然后加入烷烃发泡剂，挤出造粒得到石墨烯改性聚苯乙烯颗粒；
(2)将水泥、粉煤灰、石墨烯改性聚苯乙烯颗粒混合均匀得到预混料；然后将水泥发泡剂、稳泡剂、早强剂、减水剂和水加入该预混料，混合均匀得到料浆；将所述料浆浇筑至模具中成型、静置发泡、 脱模和养护，从而形成保温制品。
根据本发明的制备方法，优选地，在步骤(1)中，所述的熔融共混采用双螺杆挤出机进行；在步骤(2)中，所述静置发泡的时间为8～25h，所述养护的时间为8～28天。
本发明将石墨烯与聚苯乙烯树脂熔融共混，然后经过发泡形成石墨烯改性聚苯乙烯颗粒。这可以使得石墨烯均匀分散于聚苯乙烯颗粒中。石墨烯作为有效成核剂，促进泡孔成核，有效控制聚苯乙烯的泡孔稳定性；而且石墨烯有效增强了聚苯乙烯颗粒的强度。聚苯乙烯颗粒表面的石墨烯与稳泡剂、早强剂和减水剂等外加助剂相互作用，有效降低了表面张力，有效抑制了聚苯乙烯发泡颗粒在料浆中上浮。此外，石墨烯具有镜面反射红外线性能，可以有效提高保温制品的保温性能。
附图说明
图1、本发明的一种保温制品的结构示意图。
具体实施方式
下面结合具体实施例对本发明作进一步的说明，但本发明的保护范围并不限于此。
<保温制品>
本发明的保温制品的实例包括但不限于自保温砌块等。本发明的保温制品包括水泥基体和分散在水泥基体中的石墨烯改性聚苯乙烯颗粒。作为优选，石墨烯改性聚苯乙烯颗粒均匀分散在水泥基体中。这样可以改善其强度和保温性能。根据本发明的一个实施方式，本发明的保温制品包括水泥基体和石墨烯改性聚苯乙烯颗粒；所述石墨烯 改性聚苯乙烯颗粒的粒径小于等于2mm，并且其分散在所述水泥基体中；所述石墨烯改性聚苯乙烯颗粒是通过石墨烯和聚苯乙烯树脂在烷烃发泡剂的存在下熔融挤出得到的；其中，石墨烯与聚苯乙烯树脂的重量配比为1:1.5～6。在本发明中，所述石墨烯改性聚苯乙烯颗粒的粒径可以为0.1～2mm，优选为0.5～2mm。这样的尺寸范围可以兼顾保温制品的强度和保温性能。
在本发明中，所述石墨烯改性聚苯乙烯颗粒的表观密度可以为0.025～0.035g/cm 3。这样有利于改善保温制品的强度。
在本发明中，石墨烯的纯度可以不小于98％，宽度可以小于等于15μm，厚度可以为1～3nm。根据本发明的一个实施方式，本发明的石墨烯的纯度为99％以上，宽度为3～8μm，厚度为2nm。这样的石墨烯更加有利于改善保温制品的强度和保温性能。本发明的石墨烯可以采用常规方法获得。例如，将可膨胀鳞片石墨经Hummers法获得石墨烯。本发明的石墨烯不限于Hummers法石墨烯，还可以是化学气相沉积、SiC外延生长、电化学、机械剥离等方法获得的石墨烯。
在本发明中，所述聚苯乙烯树脂可以为阻燃聚苯乙烯树脂。其纯度优选大于等于97％。烷烃发泡剂可以为C3～C8的烷烃发泡剂，优选为戊烷发泡剂。例如，可以采用正戊烷和异戊烷组成的戊烷发泡剂。
在本发明中，石墨烯和聚苯乙烯树脂的重量配比可以为1:1.5～6，优选为1:2～3。将二者配比控制在上述范围，可以使得石墨烯的作用充分发挥。石墨烯颗粒作为成核剂，可以促进聚苯乙烯树脂泡孔成核，有效控制泡孔稳定性，从而改善保温制品的抗压强度。石墨烯具有层状结构，可以有效降低保温制品的导热系数，起到良好的保温效果。
在本发明中，所述石墨烯改性聚苯乙烯颗粒与所述水泥基体的重量配比可以为1:5.5～15，优选为1:6～10。这样可以兼顾保温制品的保温性能和力学性能。
在本发明中，保温制品可以采用包括如下组分的原料制得：
水泥35～90重量份，优选为60～80重量份；
粉煤灰25～55重量份，优选为30～35重量份；
石墨烯改性聚苯乙烯颗粒5～15重量份，优选为8～10重量份；
水35～90重量份，优选为50～80重量份；
水泥发泡剂2～7重量份，优选为3～5重量份；
稳泡剂0.5～5重量份，优选为1～3重量份；
早强剂0.5～2重量份，优选为0.6～1重量份；和
减水剂0.5～3重量份，优选为0.6～1重量份。
采用上述范围的原料，可以进一步改善保温制品的强度，并改善保温性能。根据本发明的一个具体实施方式，本发明的水泥基体采用包括如下组分的原料制得：水泥60重量份，粉煤灰30重量份，水50重量份，石墨烯改性聚苯乙烯颗粒10重量份，水泥发泡剂3重量份，稳泡剂1.6重量份，早强剂0.8重量份，减水剂0.6重量份。
在本发明中，水泥发泡剂可以选自双氧水、碳酸氢钠、碳酸铵、偶氮甲酰胺或偶氮二异丁腈中的一种或多种；优选为双氧水。本发明的稳泡剂可以选自硅酮酰胺、十二烷基二甲基氧化胺、烷基醇酰胺、聚丙烯酰胺、聚乙烯醇、纤维素、蛋白质中的一种或多种。本发明的蛋白质可以为动物蛋白或植物蛋白。本发明的稳泡剂优选自硅酮酰胺、十二烷基二甲基氧化胺、聚乙烯醇；更优选为硅酮酰胺。本发明的早强剂可以选自氯化钙、氯化钾、硫酸钠、硫代硫酸钙、三乙醇胺或三异丙醇胺中的一种或多种；优选为三乙醇胺。本发明的减水剂可以选自木质素磺酸镁、木质素磺酸钠、三聚氰胺甲醛树脂、含萘减水剂中的一种或多种；优选为木质素磺酸镁、木质素磺酸钠。采用上述组分，有利于改善保温制品的强度和保温性能。
在本发明中，所述水泥选自硫氧镁水泥、氯氧镁水泥、硅酸盐水 泥、铝酸盐水泥、硫铝酸盐水泥、铁铝酸盐水泥、氟铝酸盐水泥、磷酸盐水泥中的一种或多种。作为优选，本发明的水泥选自硫氧镁水泥或铝酸盐水泥。本申请发现，将硫氧镁水泥等和石墨烯改性聚苯乙烯颗粒配合使用，可以显著改善保温制品的综合性能。
根据本发明的一个具体实施方式，所述水泥为硫氧镁水泥；所述水泥发泡剂为双氧水；所述稳泡剂为硅酮酰胺；所述早强剂为三乙醇胺；且所述减水剂为木质素磺酸钠。采用上述原料，可以使得保温制品的综合性能更好。
根据本发明的一个具体实施方式，本发明的保温制品采用包括如下组分的原料制得：硫氧镁水泥60重量份，粉煤灰30重量份，水50重量份，石墨烯改性聚苯乙烯颗粒10重量份，双氧水3重量份，硅酮酰胺1.6重量份，三乙醇胺0.8重量份，和木质素磺酸钠0.6重量份。
本发明的保温制品的容重可以为500～730kg/m 3，抗压强度为4.5～9MPa，导热系数为0.035～0.045W/m·K，体积吸水率小于等于10％，防火级别为A1级。优选地，本发明的保温制品的容重650～700kg/m 3，抗压强度为8～9MPa，导热系数为0.035～0.043W/m·K，体积吸水率≤9.5％，防火级别为A1级。容重具有本领域熟知的含义，这里不再赘述。
<制备方法>
本发明的保温制品的制备方法包括石墨烯改性聚苯乙烯颗粒形成步骤和成型步骤。
本发明的石墨烯改性聚苯乙烯颗粒形成步骤为：将聚苯乙烯树脂和石墨烯在120～150℃下熔融共混，然后加入烷烃发泡剂，挤出造粒得到石墨烯改性聚苯乙烯颗粒。本申请发现，烷烃发泡剂特别适合于改善保温性能和强度。根据本发明的一个实施方式，熔融共混采用双 螺杆挤出机进行。熔融共混温度优选为130～135℃。这样的条件有利于石墨烯均匀分散在聚苯乙烯树脂中，从而提高保温制品的强度和保温性能。
本发明的水泥基体形成步骤为：将水泥、粉煤灰、石墨烯改性聚苯乙烯颗粒混合均匀得到预混料；然后将水泥发泡剂、稳泡剂、早强剂、减水剂和水加入该预混料，混合均匀得到料浆；将所述料浆浇筑至模具中成型、静置发泡、脱模和养护，从而形成保温制品。上述原料的种类和用量如前所述，这里不再赘述。混合的方式并没有特别限定。例如，将这些原料在高速搅拌机中进行搅拌。模具根据实际需要而定。静置发泡的时间可以控制在8～25h，优选为12～20h。养护的时间可以控制在8～28天，优选为10～15天。这样的条件控制可以改善保温制品的强度。
以下实施例和对比例中的“重量份”表示重量份，除非特别声明。
以下实施例中的石墨烯的纯度不小于98％、宽度小于等于15μm、厚度1～3nm，水泥为镁氧硫水泥，水泥发泡剂为双氧水，稳泡剂为硅酮酰胺，早强剂为三乙醇胺，减水剂为木质素磺酸钠。
以下实施例的成品采用如下方法进行测试：
容重采用GB/T 29060-2012附录A进行测定；抗压强度采用GB/T 4111-2013进行测定；导热系数采用GB/T 13475-2008进行测定；体积吸水率采用JC/T 641-2008测定。
实施例1
(1)将聚苯乙烯树脂10重量份和石墨烯5重量份经双螺杆挤出机在135℃下熔融共混，加入戊烷发泡剂，挤出造粒得到聚苯乙烯颗粒，筛分，得到粒径≤2mm的石墨烯改性聚苯乙烯颗粒。
(2)将水泥60重量份、粉煤灰30重量份、石墨烯改性聚苯乙烯颗粒10重量份经高速搅拌机搅拌混合，加入水泥发泡剂3重量份、稳泡剂1.6重量份、早强剂0.8重量份、减水剂0.6重量份、水50重量份的混合溶液，高速搅拌得到料浆，浇筑入模具中成型、静置发泡12h、脱模、养护10天，得到保温制品(参见图1)。养护期间须保持产品表面潮湿，确保产品达到最终强度。
该保温制品的容重为650kg/m 3，抗压强度为8.5MPa，导热系数为0.043W/m·k，体积吸水率为9.3％，防火等级为A1级。
本发明并不限于上述实施方式，在不背离本发明的实质内容的情况下，本领域技术人员可以想到的任何变形、改进、替换均落入本发明的范围。

Claims (10)

  1. 一种保温制品，其特征在于，其包括水泥基体和石墨烯改性聚苯乙烯颗粒；所述石墨烯改性聚苯乙烯颗粒的粒径小于等于2mm，并且其分散在所述水泥基体中；所述石墨烯改性聚苯乙烯颗粒是通过石墨烯和聚苯乙烯树脂在烷烃发泡剂的存在下熔融挤出得到的；其中，石墨烯与聚苯乙烯树脂的重量配比为1:1.5～6。
  2. 根据权利要求1所述的保温制品，其特征在于，所述石墨烯改性聚苯乙烯颗粒的表观密度为0.025～0.035g/cm 3；且所述石墨烯的纯度不小于98％，宽度小于等于15μm，且厚度为1～3nm。
  3. 根据权利要求1所述的保温制品，其特征在于，所述聚苯乙烯树脂为阻燃聚苯乙烯树脂；且所述烷烃发泡剂为戊烷发泡剂。
  4. 根据权利要求1所述的保温制品，其特征在于，所述石墨烯改性聚苯乙烯颗粒与所述水泥基体的重量配比为1:5.5～15。
  5. 根据权利要求1所述的保温制品，其特征在于，所述保温制品采用包括如下组分的原料制得：
    水泥35～90重量份，
    粉煤灰25～55重量份，
    石墨烯改性聚苯乙烯颗粒5～15重量份，
    水35～90重量份，
    水泥发泡剂2～7重量份，
    稳泡剂0.5～5重量份，
    早强剂0.5～2重量份，和
    减水剂0.5～3重量份。
  6. 根据权利要求5所述的保温制品，其特征在于：
    所述水泥选自硫氧镁水泥、氯氧镁水泥、硅酸盐水泥、铝酸盐水泥、硫铝酸盐水泥、铁铝酸盐水泥、氟铝酸盐水泥、磷酸盐水泥中的 一种或多种；
    所述水泥发泡剂选自双氧水、碳酸氢钠、碳酸铵、偶氮甲酰胺或偶氮二异丁腈中的一种或多种；
    所述稳泡剂选自硅酮酰胺、十二烷基二甲基氧化胺、烷基醇酰胺、聚丙烯酰胺、聚乙烯醇、纤维素、蛋白质中的一种或多种；
    所述早强剂选自氯化钙、氯化钾、硫酸钠、硫代硫酸钙、三乙醇胺或三异丙醇胺中的一种或多种；和
    所述减水剂选自木质素磺酸镁、木质素磺酸钠、三聚氰胺甲醛树脂、含萘减水剂中的一种或多种。
  7. 根据权利要求5所述的保温制品，其特征在于，所述水泥为硫氧镁水泥；所述水泥发泡剂为双氧水；所述稳泡剂为硅酮酰胺；所述早强剂为三乙醇胺；且所述减水剂为木质素磺酸钠。
  8. 根据权利要求1～7任一项所述的保温制品，其特征在于，所述保温制品的容重为500～730kg/m 3，抗压强度为4.5～9MPa，导热系数为0.035～0.045W/m·K，体积吸水率小于等于10％，且防火级别为A1级。
  9. 根据权利要求5～7任一项所述的保温制品的制备方法，其特征在于，包括如下步骤：
    (1)将聚苯乙烯树脂和石墨烯在120～150℃下熔融共混，然后加入烷烃发泡剂，挤出造粒得到石墨烯改性聚苯乙烯颗粒；
    (2)将水泥、粉煤灰、石墨烯改性聚苯乙烯颗粒混合均匀得到预混料；然后将水泥发泡剂、稳泡剂、早强剂、减水剂和水加入该预混料，混合均匀得到料浆；将所述料浆浇筑至模具中成型、静置发泡、脱模和养护，从而形成保温制品。
  10. 根据权利要求9所述的制备方法，其特征在于，在步骤(1)中，所述的熔融共混采用双螺杆挤出机进行；在步骤(2)中，所述 静置发泡的时间为8～25h，所述养护的时间为8～28天。
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