CN111333371A - Process for preparing composite heat-insulating material by doping polylactic acid - Google Patents

Process for preparing composite heat-insulating material by doping polylactic acid Download PDF

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CN111333371A
CN111333371A CN202010156380.3A CN202010156380A CN111333371A CN 111333371 A CN111333371 A CN 111333371A CN 202010156380 A CN202010156380 A CN 202010156380A CN 111333371 A CN111333371 A CN 111333371A
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insulating material
heat
pressure
polylactic acid
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李孝林
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B26/00Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02Macromolecular compounds
    • C04B26/22Natural resins, e.g. rosin
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B20/00Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/02Treatment
    • C04B20/04Heat treatment
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24Macromolecular compounds
    • C04B24/28Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B24/283Polyesters
    • C04B24/285Polylactides
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02Compositions 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
    • C04B28/04Portland cements
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5076Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with masses bonded by inorganic cements
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/60After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
    • C04B41/61Coating or impregnation
    • C04B41/65Coating or impregnation with inorganic materials
    • C04B41/68Silicic acid; Silicates
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    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474Uses not provided for elsewhere in C04B2111/00
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    • C04B2111/00508Cement paints
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/30Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
    • C04B2201/32Mortars, 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

Abstract

The invention discloses a process for preparing a composite heat-insulating material by doping polylactic acid, which relates to the technical field of heat-insulating materials, and the process comprises the steps of carrying out swelling treatment on sepiolite fibers by high-temperature pressurization and depressurization operation, enlarging pore channel size, and loosening the structure of the sepiolite fibers so as to optimize the heat-insulating property of the sepiolite fibers; the novel composite thermal insulation material is prepared by compounding the inner layer thermal insulation material and the outer layer thermal insulation material, the thermal conductivity coefficient of the prepared composite thermal insulation material is as low as below 0.05W/(m.K), and the composite thermal insulation material is suitable for serving as a thermal insulation material for building decoration.

Description

Process for preparing composite heat-insulating material by doping polylactic acid
The technical field is as follows:
the invention relates to the technical field of heat-insulating materials, in particular to a process for preparing a composite heat-insulating material by doping polylactic acid.
Background art:
the heat insulating material includes inorganic material such as expanded perlite, aerated concrete, rock wool, glass wool, etc. and organic material such as polyurethane foam, polystyrene foam, etc. The quality of the heat insulation performance of these materials is mainly determined by the heat conductivity of the materials. The harder the material conducts heat (i.e., the lower the thermal conductivity), the better the thermal insulation performance.
In recent years, the application of straw as a processing raw material of heat insulation materials is more and more extensive, but compared with organic foam plastics, the heat insulation performance of straw materials is poorer, so that the raw material formula and the processing technology need to be improved to optimize the heat insulation performance.
The invention content is as follows:
the technical problem to be solved by the invention is to provide a process for preparing a composite heat-insulating material by doping polylactic acid, and the composite heat-insulating material with excellent heat-insulating property is prepared by compounding a heat-insulating inner layer material and an outer layer heat-insulating material.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a process for preparing a composite heat-insulating material by doping polylactic acid comprises the following process steps:
(1) puffing sepiolite fibers: putting the sepiolite fibers into a high-pressure kettle, heating to the temperature of 100-120 ℃, preserving heat, vacuumizing, filling nitrogen, pressurizing to 3-5MPa, maintaining pressure, reducing the pressure to 1-3MPa, maintaining pressure, reducing the pressure to normal pressure, and then transferring out;
(2) preparing an inner layer heat insulation material: paving the sepiolite fibers subjected to the bulking treatment in a mold, mixing polylactic acid and hydrogenated rosin pentaerythritol ester, heating to a molten state, injecting the mixture into the mold, and curing at room temperature to obtain an inner-layer heat-insulating material;
(3) preparing an outer-layer heat-preservation solution: adding asbestos wool, portland cement and white polyaluminium chloride into water, and uniformly mixing to obtain an outer-layer heat-preservation solution;
(4) forming the composite heat-insulating material: and coating the prepared outer layer heat-insulating liquid on the surface of the prepared inner layer heat-insulating material, heating and curing to form an outer layer heat-insulating material on the surface of the inner layer heat-insulating material, thus obtaining the composite heat-insulating material.
The pressure maintaining time after pressurization is 5-10 min.
The pressure maintaining time after the pressure reduction is 10-30 min.
The pressure of the pressurization is preferably 4 to 5 MPa.
The pressure for reducing the pressure is preferably 1-2 MPa.
The mass ratio of the sepiolite fibers to the polylactic acid to the hydrogenated rosin pentaerythritol ester is 15-50:1-10: 1-10.
The mass ratio of the water, the asbestos wool, the portland cement and the white polyaluminium chloride is 20-100:5-20:5-20: 1-10.
The temperature of the heating and curing is 60-80 ℃.
The thickness ratio of the inner layer heat-insulating material to the outer layer heat-insulating material is 5-10: 1-5.
The sepiolite fiber is a natural mineral fiber, is a fibrous variant of sepiolite mineral, has high specific surface area and large porosity, is usually used as an adsorbent, a reinforcing agent and a filler, and utilizes the specific structure of the sepiolite fiber as a preparation raw material of an inner heat-insulating layer material.
The polylactic acid is a polymer obtained by polymerizing lactic acid serving as a main raw material, and is a novel biodegradable material. The hydrogenated rosin pentaerythritol ester has good adhesion and is generally used as a tackifying resin of solvent adhesives and pressure-sensitive adhesives. According to the invention, polylactic acid and hydrogenated rosin pentaerythritol ester are used for bonding sepiolite fibers, so that the forming of the inner-layer heat-insulating material is facilitated.
Asbestos wool is silicate mineral fiber widely used for building fireproof plates, and has good tensile strength, heat insulation and corrosion resistance. The white polyaluminium chloride belongs to an inorganic high-molecular coagulant, has high electric neutralization and bridging effects on colloids and particles in water, can remove micro-toxic substances and heavy metal ions, and is usually used for sewage treatment. The invention is beneficial to preparing the outer layer heat insulation material by asbestos wool, Portland cement and polyaluminium chloride, and obviously optimizes the heat insulation performance of the prepared composite heat insulation material.
The asbestos wool has certain heat preservation and insulation functions, and is pretreated in order to further optimize the heat preservation and insulation performance.
The technical problem to be solved by the invention can also be realized by adopting the following technical scheme:
a process for preparing a composite heat-insulating material by doping polylactic acid comprises the following process steps:
(1) puffing sepiolite fibers: putting the sepiolite fibers into a high-pressure kettle, heating to the temperature of 100-120 ℃, preserving heat, vacuumizing, filling nitrogen, pressurizing to 3-5MPa, maintaining pressure, reducing the pressure to 1-3MPa, maintaining pressure, reducing the pressure to normal pressure, and then transferring out;
(2) preparing an inner layer heat insulation material: paving the sepiolite fibers subjected to the bulking treatment in a mold, mixing polylactic acid and hydrogenated rosin pentaerythritol ester, heating to a molten state, injecting the mixture into the mold, and curing at room temperature to obtain an inner-layer heat-insulating material;
(3) pretreatment of asbestos wool: placing the asbestos wool in a microwave high-pressure reactor, performing microwave high-pressure treatment under the pressure of 2-3MPa, the microwave frequency of 2450MHz and the microwave power of 500-;
(4) preparing an outer-layer heat-preservation solution: adding the pretreated asbestos wool, Portland cement and white polyaluminium chloride into water, and uniformly mixing to obtain an outer-layer heat-preservation solution;
(5) forming the composite heat-insulating material: and coating the prepared outer layer heat-insulating liquid on the surface of the prepared inner layer heat-insulating material, heating and curing to form an outer layer heat-insulating material on the surface of the inner layer heat-insulating material, thus obtaining the composite heat-insulating material.
The pressure maintaining time after pressurization is 5-10 min.
The pressure maintaining time after the pressure reduction is 10-30 min.
The pressure of the pressurization is preferably 4 to 5 MPa.
The pressure for reducing the pressure is preferably 1-2 MPa.
The mass ratio of the sepiolite fibers to the polylactic acid to the hydrogenated rosin pentaerythritol ester is 15-50:1-10: 1-10.
The microwave high-pressure treatment time is 5-15 min.
The mass ratio of the water, the asbestos wool, the portland cement and the white polyaluminium chloride is 20-100:5-20:5-20: 1-10.
The temperature of the heating and curing is 60-80 ℃.
The thickness ratio of the inner layer heat-insulating material to the outer layer heat-insulating material is 5-10: 1-5.
Under the microwave high-pressure treatment, the pores in the asbestos wool are further enlarged, and the heat preservation and insulation performance is further optimized.
Although polylactic acid can promote the adhesion of sepiolite fibers, the polylactic acid does not have a certain heat preservation and insulation effect per se, so that the polylactic acid is modified.
The technical problem to be solved by the invention can also be realized by adopting the following technical scheme:
a process for preparing a composite heat-insulating material by doping polylactic acid comprises the following process steps:
(1) puffing sepiolite fibers: putting the sepiolite fibers into a high-pressure kettle, heating to the temperature of 100-120 ℃, preserving heat, vacuumizing, filling nitrogen, pressurizing to 3-5MPa, maintaining pressure, reducing the pressure to 1-3MPa, maintaining pressure, reducing the pressure to normal pressure, and then transferring out;
(2) preparing modified polylactic acid: dissolving polylactic acid in acetone, adding 3-hydroxy magnesium butyrate and concentrated sulfuric acid, heating to reflux, carrying out heat preservation reaction, carrying out reduced pressure concentration after the reaction is finished so as to recover acetone, adding water into the concentrate, stirring, standing, filtering, and drying at low temperature to obtain modified polylactic acid;
(3) preparing an inner layer heat insulation material: paving the sepiolite fibers subjected to the puffing treatment in a mold, mixing the prepared modified polylactic acid and hydrogenated rosin pentaerythritol ester, heating to a molten state, injecting into the mold, and curing at room temperature to obtain an inner layer heat-insulating material;
(4) preparing an outer-layer heat-preservation solution: adding asbestos wool, portland cement and white polyaluminium chloride into water, and uniformly mixing to obtain an outer-layer heat-preservation solution;
(5) forming the composite heat-insulating material: and coating the prepared outer layer heat-insulating liquid on the surface of the prepared inner layer heat-insulating material, heating and curing to form an outer layer heat-insulating material on the surface of the inner layer heat-insulating material, thus obtaining the composite heat-insulating material.
The pressure maintaining time after pressurization is 5-10 min.
The pressure maintaining time after the pressure reduction is 10-30 min.
The pressure of the pressurization is preferably 4 to 5 MPa.
The pressure for reducing the pressure is preferably 1-2 MPa.
The mass ratio of the polylactic acid to the magnesium 3-hydroxybutyrate to the concentrated sulfuric acid is 50-100:5-20: 0.5-3.
The mass ratio of the sepiolite fibers to the modified polylactic acid to the hydrogenated rosin pentaerythritol ester is 15-50:1-10: 1-10.
The mass ratio of the water, the asbestos wool, the portland cement and the white polyaluminium chloride is 20-100:5-20:5-20: 1-10.
The temperature of the heating and curing is 60-80 ℃.
The thickness ratio of the inner layer heat-insulating material to the outer layer heat-insulating material is 5-10: 1-5.
According to the invention, the 3-hydroxybutyrate magnesium is used as a polylactic acid modifier, and the hydroxyl are subjected to etherification reaction to modify polylactic acid, so that the polylactic acid has a certain heat preservation and insulation effect, and the heat preservation and insulation performance of the prepared composite heat preservation and insulation material is optimized.
The invention has the beneficial effects that:
(1) the invention carries out bulking treatment on the sepiolite fibers by high-temperature pressurization and depressurization operation, enlarges pore path size, and loosens the sepiolite fiber structure, thereby optimizing the heat insulation performance;
(2) the novel composite thermal insulation material is prepared by compounding the inner layer thermal insulation material and the outer layer thermal insulation material, the thermal conductivity coefficient of the prepared composite thermal insulation material is as low as below 0.05W/(m.K), and the prepared composite thermal insulation material is suitable for serving as a thermal insulation material for building decoration.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Sepiolite fibers and asbestos fibers were purchased from Shijiazhuang Majon building materials, Inc.
Polylactic acid was purchased from Zhejiang Haizhen biomaterial GmbH.
The hydrogenated rosin pentaerythritol ester was purchased from Guangzhou Songbao chemical Co., Ltd.
Portland cement was purchased from Oshun Cement, Inc., of Tangshan.
White polyaluminum chloride was purchased from Henan Zhengyuan chemical Co., Ltd.
Magnesium 3-hydroxybutyrate was purchased from Hippocampus Chemicals, Inc.
Example 1
(1) Puffing sepiolite fibers: putting the sepiolite fibers into a high-pressure kettle, heating to 110 ℃, preserving heat, vacuumizing, filling nitrogen, pressurizing to 5MPa, maintaining pressure for 10min, reducing pressure to 2MPa, maintaining pressure for 20min, reducing pressure to normal pressure, and transferring out;
(2) preparing an inner layer heat insulation material: spreading 50 parts of the sepiolite fibers subjected to the puffing treatment in a mold, mixing 5 parts of polylactic acid and 4 parts of hydrogenated rosin pentaerythritol ester, heating to a molten state, injecting into the mold, and curing at 25 ℃ for 8 hours to obtain an inner layer heat-insulating material;
(3) preparing an outer-layer heat-preservation solution: adding 20 parts of asbestos wool, 12 parts of Portland cement and 5 parts of white polyaluminium chloride into 40 parts of water, and uniformly mixing to obtain an outer-layer heat-preservation solution;
(4) forming the composite heat-insulating material: and coating the prepared outer layer heat-insulating liquid on the surface of the prepared inner layer heat-insulating material, heating to 65 ℃ and curing for 8h, and forming an outer layer heat-insulating material with the thickness of 4mm on the surface of the inner layer heat-insulating material with the thickness of 10mm to obtain the composite heat-insulating material.
Example 2
Example 2 differs from example 1 only in that the amount of sepiolite fibers was replaced by 40 parts.
(1) Puffing sepiolite fibers: putting the sepiolite fibers into a high-pressure kettle, heating to 110 ℃, preserving heat, vacuumizing, filling nitrogen, pressurizing to 5MPa, maintaining pressure for 10min, reducing pressure to 2MPa, maintaining pressure for 20min, reducing pressure to normal pressure, and transferring out;
(2) preparing an inner layer heat insulation material: paving 40 parts of the sepiolite fibers subjected to the puffing treatment in a mold, mixing 5 parts of polylactic acid and 4 parts of hydrogenated rosin pentaerythritol ester, heating to a molten state, injecting into the mold, and curing at 25 ℃ for 8 hours to obtain an inner layer heat-insulating material;
(3) preparing an outer-layer heat-preservation solution: adding 20 parts of asbestos wool, 12 parts of Portland cement and 5 parts of white polyaluminium chloride into 40 parts of water, and uniformly mixing to obtain an outer-layer heat-preservation solution;
(4) forming the composite heat-insulating material: and coating the prepared outer layer heat-insulating liquid on the surface of the prepared inner layer heat-insulating material, heating to 65 ℃ and curing for 8h, and forming an outer layer heat-insulating material with the thickness of 4mm on the surface of the inner layer heat-insulating material with the thickness of 10mm to obtain the composite heat-insulating material.
Example 3
Example 3 differs from example 1 only in that asbestos wool was pretreated.
(1) Puffing sepiolite fibers: putting the sepiolite fibers into a high-pressure kettle, heating to 110 ℃, preserving heat, vacuumizing, filling nitrogen, pressurizing to 5MPa, maintaining pressure for 10min, reducing pressure to 2MPa, maintaining pressure for 20min, reducing pressure to normal pressure, and transferring out;
(2) preparing an inner layer heat insulation material: spreading 50 parts of the sepiolite fibers subjected to the puffing treatment in a mold, mixing 5 parts of polylactic acid and 4 parts of hydrogenated rosin pentaerythritol ester, heating to a molten state, injecting into the mold, and curing at 25 ℃ for 8 hours to obtain an inner layer heat-insulating material;
(3) pretreatment of asbestos wool: placing asbestos wool in a microwave high-pressure reactor, performing microwave high-pressure treatment for 10min under the conditions of 3MPa of pressure, 2450MHz of microwave frequency and 500W of microwave power, reducing the pressure to normal pressure, and then transferring out;
(4) preparing an outer-layer heat-preservation solution: adding 20 parts of the pretreated asbestos wool, 12 parts of Portland cement and 5 parts of white polyaluminium chloride into 40 parts of water, and uniformly mixing to obtain an outer-layer heat-preservation solution;
(5) forming the composite heat-insulating material: and coating the prepared outer layer heat-insulating liquid on the surface of the prepared inner layer heat-insulating material, heating to 65 ℃ and curing for 8h, and forming an outer layer heat-insulating material with the thickness of 4mm on the surface of the inner layer heat-insulating material with the thickness of 10mm to obtain the composite heat-insulating material.
Example 4
Example 4 differs from example 1 only in that the polylactic acid is subjected to modification treatment.
(1) Puffing sepiolite fibers: putting the sepiolite fibers into a high-pressure kettle, heating to 110 ℃, preserving heat, vacuumizing, filling nitrogen, pressurizing to 5MPa, maintaining pressure for 10min, reducing pressure to 2MPa, maintaining pressure for 20min, reducing pressure to normal pressure, and transferring out;
(2) preparing modified polylactic acid: dissolving 75 parts of polylactic acid in acetone, adding 16 parts of magnesium 3-hydroxybutyrate and 1 part of concentrated sulfuric acid, heating to reflux, then carrying out heat preservation reaction for 5 hours, carrying out reduced pressure concentration after the reaction is finished to recover acetone, adding water into the concentrate, stirring, standing, filtering, and drying at low temperature to obtain modified polylactic acid;
(3) preparing an inner layer heat insulation material: spreading 50 parts of the sepiolite fibers subjected to the puffing treatment in a mold, mixing 5 parts of the prepared modified polylactic acid and 4 parts of hydrogenated rosin pentaerythritol ester, heating to a molten state, injecting into the mold, and curing for 8 hours at 25 ℃ to obtain an inner layer heat insulation material;
(4) preparing an outer-layer heat-preservation solution: adding 20 parts of asbestos wool, 12 parts of Portland cement and 5 parts of white polyaluminium chloride into 40 parts of water, and uniformly mixing to obtain an outer-layer heat-preservation solution;
(5) forming the composite heat-insulating material: and coating the prepared outer layer heat-insulating liquid on the surface of the prepared inner layer heat-insulating material, heating to 65 ℃ and curing for 8h, and forming an outer layer heat-insulating material with the thickness of 4mm on the surface of the inner layer heat-insulating material with the thickness of 10mm to obtain the composite heat-insulating material.
Comparative example 1
Comparative example 1 differs from example 1 only in that no white polyaluminum chloride was added in the preparation of the outer insulation.
(1) Puffing sepiolite fibers: putting the sepiolite fibers into a high-pressure kettle, heating to 110 ℃, preserving heat, vacuumizing, filling nitrogen, pressurizing to 5MPa, maintaining pressure for 10min, reducing pressure to 2MPa, maintaining pressure for 20min, reducing pressure to normal pressure, and transferring out;
(2) preparing an inner layer heat insulation material: spreading 50 parts of the sepiolite fibers subjected to the puffing treatment in a mold, mixing 5 parts of polylactic acid and 4 parts of hydrogenated rosin pentaerythritol ester, heating to a molten state, injecting into the mold, and curing at 25 ℃ for 8 hours to obtain an inner layer heat-insulating material;
(3) preparing an outer-layer heat-preservation solution: adding 20 parts of asbestos wool and 12 parts of portland cement into 40 parts of water, and uniformly mixing to obtain an outer-layer heat-preservation solution;
(4) forming the composite heat-insulating material: and coating the prepared outer layer heat-insulating liquid on the surface of the prepared inner layer heat-insulating material, heating to 65 ℃ and curing for 8h, and forming an outer layer heat-insulating material with the thickness of 4mm on the surface of the inner layer heat-insulating material with the thickness of 10mm to obtain the composite heat-insulating material.
Comparative example 2
Comparative example 2 differs from example 1 only in that the sepiolite fibers were not bulked.
(1) Preparing an inner layer heat insulation material: paving 50 parts of sepiolite fibers in a mold, mixing 5 parts of polylactic acid and 4 parts of hydrogenated rosin pentaerythritol ester, heating to a molten state, injecting into the mold, and curing at 25 ℃ for 8 hours to obtain an inner layer heat-insulating material;
(2) preparing an outer-layer heat-preservation solution: adding 20 parts of asbestos wool, 12 parts of Portland cement and 5 parts of white polyaluminium chloride into 40 parts of water, and uniformly mixing to obtain an outer-layer heat-preservation solution;
(3) forming the composite heat-insulating material: and coating the prepared outer layer heat-insulating liquid on the surface of the prepared inner layer heat-insulating material, heating to 65 ℃ and curing for 8h, and forming an outer layer heat-insulating material with the thickness of 4mm on the surface of the inner layer heat-insulating material with the thickness of 10mm to obtain the composite heat-insulating material.
Comparative example 3
Comparative example 3 differs from example 1 only in that no outer insulation was prepared.
(1) Puffing sepiolite fibers: putting the sepiolite fibers into a high-pressure kettle, heating to 110 ℃, preserving heat, vacuumizing, filling nitrogen, pressurizing to 5MPa, maintaining pressure for 10min, reducing pressure to 2MPa, maintaining pressure for 20min, reducing pressure to normal pressure, and transferring out;
(2) preparing an inner layer heat insulation material: 50 parts of the sepiolite fibers subjected to the puffing treatment are flatly laid in a mould, 5 parts of polylactic acid and 4 parts of hydrogenated rosin pentaerythritol ester are mixed and then heated to a molten state, the mixture is injected into the mould, and the mixture is solidified for 8 hours at 25 ℃ to obtain an inner layer heat-insulating material with the thickness of 10 mm;
the thermal conductivity of the heat insulating materials manufactured in the above examples and comparative examples was measured in accordance with GB/T10294-2008, and the measurement results are shown in Table 1.
TABLE 1 measurement results of thermal conductivity
Group of Thermal conductivity W/(m.K)
Example 1 0.043
Example 2 0.048
Example 3 0.036
Example 4 0.032
Comparative example 1 0.057
Comparative example 2 0.086
Comparative example 3 0.114
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (9)

1. A process for preparing a composite heat-insulating material by doping polylactic acid is characterized by comprising the following process steps:
(1) puffing sepiolite fibers: putting the sepiolite fibers into a high-pressure kettle, heating to the temperature of 100-120 ℃, preserving heat, vacuumizing, filling nitrogen, pressurizing to 3-5MPa, maintaining pressure, reducing the pressure to 1-3MPa, maintaining pressure, reducing the pressure to normal pressure, and then transferring out;
(2) preparing an inner layer heat insulation material: paving the sepiolite fibers subjected to the bulking treatment in a mold, mixing polylactic acid and hydrogenated rosin pentaerythritol ester, heating to a molten state, injecting the mixture into the mold, and curing at room temperature to obtain an inner-layer heat-insulating material;
(3) preparing an outer-layer heat-preservation solution: adding asbestos wool, portland cement and white polyaluminium chloride into water, and uniformly mixing to obtain an outer-layer heat-preservation solution;
(4) forming the composite heat-insulating material: and coating the prepared outer layer heat-insulating liquid on the surface of the prepared inner layer heat-insulating material, heating and curing to form an outer layer heat-insulating material on the surface of the inner layer heat-insulating material, thus obtaining the composite heat-insulating material.
2. The process for preparing the composite heat-insulating material by doping the polylactic acid according to claim 1, which is characterized in that: the pressure maintaining time after pressurization is 5-10 min.
3. The process for preparing the composite heat-insulating material by doping the polylactic acid according to claim 1, which is characterized in that: the pressure maintaining time after the pressure reduction is 10-30 min.
4. The process for preparing the composite heat-insulating material by doping the polylactic acid according to claim 1, which is characterized in that: the pressure of the pressurization is preferably 4 to 5 MPa.
5. The process for preparing the composite heat-insulating material by doping the polylactic acid according to claim 1, which is characterized in that: the pressure for reducing the pressure is preferably 1-2 MPa.
6. The process for preparing the composite heat-insulating material by doping the polylactic acid according to claim 1, which is characterized in that: the mass ratio of the sepiolite fibers to the polylactic acid to the hydrogenated rosin pentaerythritol ester is 15-50:1-10: 1-10.
7. The process for preparing the composite heat-insulating material by doping the polylactic acid according to claim 1, which is characterized in that: the mass ratio of the water, the asbestos wool, the portland cement and the white polyaluminium chloride is 20-100:5-20:5-20: 1-10.
8. The process for preparing the composite heat-insulating material by doping the polylactic acid according to claim 1, which is characterized in that: the temperature of the heating and curing is 60-80 ℃.
9. The process for preparing the composite heat-insulating material by doping the polylactic acid according to claim 1, which is characterized in that: the thickness ratio of the inner layer heat-insulating material to the outer layer heat-insulating material is 5-10: 1-5.
CN202010156380.3A 2020-03-06 2020-03-06 Process for preparing composite heat-insulating material by doping polylactic acid Withdrawn CN111333371A (en)

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