阅读说明：本技术 以锂皂石修饰的玄武岩纤维阻燃保温材料及其制备方法 (Hectorite-modified basalt fiber flame-retardant heat-insulation material and preparation method thereof ) 是由 苗世顶 李静瑶 魏存弟 张培萍 司集文 佐传潇 于 2020-12-29 设计创作，主要内容包括：本发明一种以锂皂石修饰的玄武岩纤维阻燃保温材料及其制备方法,包括锂皂石(Laponite)无机浸润剂、玄武岩纤维阻燃组分、树脂胶防水粘结组分、秸秆保温组分。该新型阻燃保温材料通过锂皂石修饰玄武岩纤维有效提高了普通玄武岩纤维的阻燃性能,同时使纤维表面更加粗糙化,提高施工相容性,可直接代替传统施工过程中的纤维网格布与后续砂浆层粘结；该发明又结合秸秆优良的保温隔热性能和来源丰富、造价低廉且可再生的资源优势,再配合环氧树脂的防水密封性能和增稠粘结性能,制备了一种阻燃性能更好、保温性能优良、施工相容性更好、造价更低的新型建筑材料。(The invention relates to a hectorite-modified basalt fiber flame-retardant heat-insulating material and a preparation method thereof. The novel flame-retardant heat-insulation material effectively improves the flame-retardant property of common basalt fibers by modifying the basalt fibers with the hectorite, simultaneously roughens the fiber surface, improves the construction compatibility, and can directly replace fiber mesh cloth in the traditional construction process to be bonded with a subsequent mortar layer; the invention combines the excellent heat-insulating property and resource advantages of rich sources, low cost and renewable resources of the straws, and prepares a novel building material with better flame retardant property, excellent heat-insulating property, better construction compatibility and lower cost by matching the waterproof sealing property and thickening bonding property of the epoxy resin.)

1. A basalt fiber flame-retardant heat-insulating material modified by hectorite is characterized by comprising the following components: laponite (Laponite) inorganic impregnating compound, basalt fiber flame-retardant component, resin adhesive waterproof bonding component and straw heat-insulating component.

2. The basalt fiber flame-retardant and heat-insulating material modified by laponite as claimed in claim 1, wherein: the Laponite inorganic impregnating compound is formed by uniformly dispersing 1-5% of Laponite nano particles with the particle size of less than 500nm in deionized water.

3. The basalt fiber flame-retardant and heat-insulating material modified by laponite as claimed in claim 1, wherein: the basalt fiber flame-retardant component is formed by spinning basalt after melting at 1400-1550 ℃, passing through platinum-rhodium alloy and infiltrating and drawing through an Laponite inorganic impregnating compound, and the thickness of the basalt fiber flame-retardant component is 1-3 mm.

4. The basalt fiber flame-retardant and heat-insulating material modified by laponite as claimed in claim 1, wherein: the resin adhesive waterproof bonding component is formed by doping 5-10 parts of diatomite into bisphenol A type bi-component epoxy resin adhesive, the bisphenol A type bi-component epoxy resin adhesive is formed by A component epoxy resin and B component curing agent, the epoxy value is 0.48-0.54 eq/100g, and the thickness is 1-3 mm.

5. The basalt fiber flame-retardant and heat-insulating material modified by laponite as claimed in claim 1, wherein: the straw heat-insulating component is a plate formed by uniformly mixing 40-70 parts of crushed corn straw skins and 30-60 parts of crushed straw pulp with 5-15 parts of vegetable glue, and the thickness of the plate is 5-10 cm.

6. The basalt fiber flame-retardant and heat-insulating material modified by laponite according to claim 5, wherein the vegetable gum is prepared from the following raw materials in parts by weight: 8-12 parts of Arabic gum, 7-9 parts of shellac, 10-13 parts of sodium carboxymethylcellulose and 65-75 parts of water.

7. The preparation method of the basalt fiber flame-retardant and heat-insulating material modified by the hectorite according to claims 1 to 6, which is characterized by comprising the following specific implementation steps:

(1) uniformly dispersing a certain amount of the Laponite nano particles into deionized water, and stirring for 3-5 hours by using a magnetic stirrer to prepare a hectorite inorganic impregnating compound for later use;

(2) the basalt is melted at high temperature and drawn into wires by platinum rhodium alloy, in the process, the impregnating compound obtained in the step (1) is used for impregnating into wires, the diameter is 12-18 mu m, and the linear density is 180-²Standby;

(3) stranding the basalt fiber filaments obtained in the step (2) through a stranding machine and then spinning to form basalt fiber cloth, wherein the thickness of the woven cloth is 2-5mm for later use;

(4) weighing corn straw skins and straw pulp according to a proportion, drying, mixing, cutting into sections, and crushing by a ball mill until the width is 1-3mm and the length is 1-5cm for later use;

(5) weighing arabic gum, shellac, sodium carboxymethylcellulose and water in proportion, and mixing uniformly to prepare vegetable gum for use;

(6) mixing the straws obtained in the step (4) and the step (5) with the vegetable gum according to a proportion, uniformly stirring and placing into a mold for later use;

(7) placing the sample obtained in the step (6) on a hot press, and hot-pressing at 90-150 ℃ and 0.5-5MPa for 20-60min to form for later use;

(8) uniformly mixing the epoxy resin of the component A, the curing agent of the component B and the diatomite in the bisphenol A type bi-component epoxy resin adhesive in proportion for later use;

(9) uniformly coating the epoxy resin glue obtained in the step (8) on the surface of the straw board obtained in the step (7) for standby;

(10) and (4) immediately sticking the basalt fiber woven fabric in the step (3) on the surface of the plate obtained in the step (9), and performing hot pressing on the basalt fiber woven fabric in a hot press for 3-15min at 40-80 ℃ under the pressure of 0.2-1MPa to obtain the basalt fiber composite plate.

Technical Field

The invention discloses a hectorite-modified basalt fiber flame-retardant heat-insulation material and a preparation method thereof, belongs to a heat-insulation system used on the outer side of a building wall structure, and also provides a preparation method thereof, belonging to the technical field of building materials.

Background

The current building energy-saving level of China is far lower than that of developed countries, the unit area energy consumption is still 3-5 times of that of developed countries with similar climates, and wall heat preservation is an important link for realizing building energy saving. The currently common external wall thermal insulation materials are inorganic and organic. For a Chinese patent with an organic heat-insulating material granted patent number ZL200910071491.8, a novel organic heat-insulating material is invented by utilizing corn straws and polystyrene particles, the material has excellent heat-insulating property, saves resources and is low in cost, but the flame retardant property of the material cannot meet the requirement of fire-retardant grade A, and a fire disaster is easily caused; an inorganic foaming basalt thermal insulation material and a basalt rock wool sandwich thermal insulation board are developed for Chinese invention type patents with patent numbers of inorganic thermal insulation materials ZL201310528477.2 and ZL201110152574.7, the inorganic foaming basalt thermal insulation material and the basalt rock wool sandwich thermal insulation board all have excellent thermal insulation performance and flame retardant performance, but the production process of foaming basalt is difficult to control, and basalt rock wool, glass rock wool and the like have the defects of large water absorption rate and easy pulverization, and in addition, compared with various inorganic thermal insulation mortars, the thermal insulation performance is poor and the self weight is large. Therefore, the novel external wall thermal insulation material is still an important task of building energy conservation by utilizing the advantages of the existing renewable resources in China and combining the respective performance characteristics of basalt fibers and straws. (ii) a

The Laponite (Laponite) used in the present invention is oneAn artificially synthesized clay material with hectorite structure is a water-containing layered silicate mineral with trioctahedral structure and has a chemical formula of Si₈[(Mg_5.5Li_0.4)H₄O_{2 4}]^0.7-Na^0.7+I.e. the octahedral central ion is Mg⁺²And Li⁺Sandwiched between four tetrahedral silicon atom layers, these groups are balanced by 20 oxygen atoms and 4 hydroxyl groups, and Na is contained between layers⁺The layered structure of (1). The clay mineral is considered as a flame retardant with excellent performance, and the flame retardant mechanism is that firstly, the nano-sheet layer of the clay plays a key gas barrier role in the decomposition and combustion of materials [ juxianjian and the like, the flame retardant mechanism of minerals in high polymer materials and research progress thereof, 2007](ii) a Secondly, the clay mineral forms a high-performance carbonized silicate structure on the surface of the material in the combustion process of the clay mineral, so that outward diffusion of volatilizable products generated by thermal decomposition of unburned parts and inward diffusion of external oxygen are prevented; meanwhile, structural iron in clay minerals has a trapping effect on free radicals, the mass loss rate of the materials is reduced, and the materials are flame-retardant [ Wanglinjiang et al, application prospects and problems of clay mineral materials in flame-retardant technology, 2011](ii) a Because Laponite is water-containing clay and exists in the form of interlayer water and crystal water, the interlayer water is neutral water molecules between the structural layers in the crystal lattice, and the electric price of the structural layers is not balanced, the interlayer water can adsorb other metal cations and then adsorb the water molecules, so that water molecule layers are formed between the adjacent structural layers, interlayer water is greatly escaped when the structural layers are heated to about 110 ℃ under normal pressure, the crystal lattice of the mineral is not damaged after water loss, and the mineral can absorb water again; crystal water (OH)^-The form exists on a certain coordination position in the crystal lattice, is firmly connected with other ions, and can escape only when the structure is damaged at high temperature of 600-1000 ℃, so that the fire resistance of the basalt fiber modified by the Laponite can be further improved.

The hectorite used in the invention can modify basalt fibers because when the Laponite is dispersed in water, the Laponite can be hydrated and expanded into a sol containing hydroxyl, so that the Laponite can be directly used as a wetting agent in a drawing process, can interact with functional groups on the fiber surface to form a film, is uniformly coated on the fiber surface, increases the roughness and the alkali resistance of the fiber, has better bonding effect with a cement substrate interface, improves the construction compatibility, and replaces the complicated procedure of singly modifying the basalt fibers in the traditional industry.

The corn straw used in the invention has rich resources in China, the internal structure of the straw has rich pores, the heat conductivity coefficient is lower, and the straw is a material with excellent heat insulation performance, so that the corn straw used as a building material not only saves energy, but also protects the environment. However, the straw has the defects of inflammability, easy water absorption and the like, so that the fireproof components formed by the flame retardant property obtained by utilizing the modified basalt fiber mutually make up for the shortages, can resist the temperature as high as 600 ℃, has the strength 5-10 times that of an EPS heat-insulating board, and can also play a role in protection under the environments of humidity, steam, alkalinity, smog and chemical gas. Meanwhile, the basalt fiber woven fabric can replace the process of independently pasting fiber gridding cloth in construction, so that the construction period is saved, and the manufacturing cost is saved.

In conclusion, the basalt fiber flame-retardant heat-insulating material modified by the hectorite is a novel multifunctional material which has excellent flame-retardant property, better heat-insulating property, stable strength and reduced construction procedures.

Disclosure of Invention

The technical problem to be solved is as follows:

1. the invention provides a basalt fiber flame-retardant heat-insulating material modified by hectorite, which aims to further improve the fire resistance of the heat-insulating material.

2. The invention provides a hectorite-modified basalt fiber flame-retardant heat-insulating material, and aims to solve the problem of poor construction compatibility caused by smooth surface of basalt fiber.

3. The invention provides a hectorite-modified basalt fiber flame-retardant heat-insulating material, and aims to solve the problems of great weight, high water absorption rate or poor heat-insulating property of the traditional inorganic heat-insulating material.

4. The invention provides a hectorite-modified basalt fiber flame-retardant heat-insulation material and aims to solve the technical problem of complex external wall heat-insulation construction procedures.

5. The invention further provides a preparation method of the hectorite-modified basalt fiber flame-retardant heat-insulating material, and aims to solve the problems that the heat-insulating material is high in cost and not beneficial to industrial production.

The technical scheme is as follows:

in order to meet the technical requirements, the invention provides a hectorite-modified basalt fiber flame-retardant heat-insulating material and a preparation method thereof, which can replace external wall heat-insulating materials such as EPS boards, polyurethane foam boards, heat-insulating mortar and the like, and have excellent flame retardance, waterproofness, strength, alkali resistance and surface bonding property. The method is realized by the following technical scheme:

a hectorite-modified basalt fiber flame-retardant heat-insulation material comprises the following components: the composite material comprises an Laponite inorganic impregnating compound, a basalt fiber woven fabric flame-retardant component, a resin adhesive waterproof bonding component and a straw heat-insulating component.

1. Preferably, the Laponite inorganic impregnating compound is a sol-type impregnating compound formed by uniformly dispersing 1-5% of Laponite nano particles with the particle size of less than 500nm in deionized water.

2. Preferably, the basalt fiber flame-retardant component is formed by spinning and weaving basalt after melting at 1400-1550 ℃ and infiltrating and drawing by a laponite inorganic impregnating compound, and the thickness is 1-3 mm.

3. Preferably, the resin adhesive waterproof bonding component is formed by mixing bisphenol A type bi-component epoxy resin and 5-10 parts of diatomite, the epoxy value of the resin adhesive is 0.48-0.54 eq/100g, and the thickness of the resin adhesive is 1-3 mm.

4. Preferably, the straw heat-insulating component is a plate formed by mixing 40-70 parts of crushed corn straw skins and 30-60 parts of crushed straw pulp and then uniformly mixing with 5-15 parts of vegetable glue, and the thickness of the plate is 5-10 cm.

5. Preferably, the vegetable gum is prepared from the following raw materials in parts by weight: 8-12 parts of Arabic gum, 7-9 parts of shellac, 10-13 parts of sodium carboxymethylcellulose and 65-75 parts of water.

The preparation method comprises the following steps:

the preparation method of the hectorite-modified basalt fiber flame-retardant heat-insulating material comprises the following specific implementation steps of:

(1) uniformly dispersing the weighed Laponite particles in deionized water, and stirring for 3-5h by using a magnetic stirrer to prepare a hectorite inorganic impregnating compound for later use;

(2) the basalt is melted at the high temperature of 1400-1600 ℃ and is drawn by platinum-rhodium alloy, in the process, the impregnating compound obtained in the step (1) is infiltrated into filaments, the diameter is 12-18 mu m, and the linear density is 180-220g/m²Standby;

(3) stranding the basalt fiber filaments obtained in the step (2) through a stranding machine and then spinning to form basalt fiber cloth, wherein the thickness of the woven cloth is 2-5mm for later use;

(4) drying the corn straw skin and the straw pulp, mixing, cutting into sections, and crushing by a ball mill until the width is 1-3mm and the length is 1-5cm for later use;

(5) weighing arabic gum, shellac, sodium carboxymethylcellulose and water in proportion, and mixing uniformly to prepare vegetable gum for use;

(6) mixing the straws obtained in the step (4) and the step (5) with the vegetable gum according to a proportion, uniformly stirring and placing into a mold for later use;

(7) placing the sample obtained in the step (6) on a hot press, and hot-pressing at 90-150 ℃ and 0.5-5MPa for 20-60min to form for later use;

(8) uniformly mixing the epoxy resin of the component A, the curing agent of the component B and the diatomite in the bisphenol A type bi-component epoxy resin adhesive in proportion for later use;

(9) uniformly coating the epoxy resin adhesive obtained in the step (8) on the surface of the straw board obtained in the step (7) for standby;

(10) and (4) immediately sticking the basalt fiber woven fabric in the step (3) on the surface of the plate obtained in the step (9), and performing hot pressing on the basalt fiber woven fabric in a hot press for 3-15min at 40-80 ℃ under the pressure of 0.2-1MPa to obtain the basalt fiber composite plate.

The invention has the following positive effects:

compared with the prior art, the invention provides a hectorite-modified basalt fiber flame-retardant heat-insulating material and a preparation method thereof, and the positive effects are as follows:

1. the fire resistance and the caking property of the basalt fiber modified by the Laponite nano particles are improved.

2. The straw has the advantages of excellent heat preservation and heat insulation performance, rich resources, low manufacturing cost and renewable resources, and waste resources are effectively utilized, so that the energy is saved and the environment is protected.

3. The fiber woven cloth can directly replace the externally hung fiber gridding cloth in the traditional external wall heat insulation construction, and is directly bonded with the plastering mortar layer, so that the construction procedures are reduced, the construction period is shortened, and the manufacturing cost is reduced.

4. The novel material has simple preparation process, waste utilization and environmental protection, and has remarkable social benefit.

Drawings

FIG. 1 is SEM image of the surface of basalt fiber without laponite modification, the surface is smooth, the basalt fiber is not tightly bonded with cement mortar in later construction, and the flame retardance depends on the fiber.

FIG. 21 is an SEM image of basalt fiber treated by the hectorite inorganic impregnating compound, the surface of the basalt fiber is slightly rough, the later bonding effect with cement is good, and the flame retardant property is slightly improved.

FIG. 34 is an SEM image of basalt fiber treated by the laponite inorganic impregnating compound, the surface is very rough, the later construction compatibility is obviously improved, and the flame retardance is obviously improved.

Detailed Description

The present invention is further illustrated by the following examples, which do not limit the present invention in any way, and any modifications or changes that can be easily made by a person skilled in the art to the present invention will fall within the scope of the claims of the present invention without departing from the technical solution of the present invention.

Example 1:

weighing 1.5 parts of Laponite nano particles, uniformly dispersing the Laponite nano particles in deionized water, stirring the mixture by using a magnetic stirrer for 3 hours, melting basalt at the high temperature of 1520 ℃, infiltrating the basalt into filaments by using the impregnating compound in the platinum-rhodium alloy drawing process, and then weaving the basalt fiber filaments into basalt fiber cloth with the thickness of 1 +/-0.2 mm. Mixing 90 parts of corn straw and 10 parts of vegetable gum, carrying out hot press molding for 20min at 90 ℃ and 2MPa, uniformly coating resin gum with the thickness of 1 +/-0.2 mm on the surface of the mixture, pasting basalt fiber cloth, and then carrying out hot press for 6min at 50 ℃ and 0.5 MPa.

Example 2:

weighing 2 parts of Laponite nano particles, uniformly dispersing the Laponite nano particles in deionized water, stirring the mixture by using a magnetic stirrer for 5 hours, melting basalt at 1520 ℃ and infiltrating the basalt into filaments by using the impregnating compound in the platinum-rhodium alloy drawing process, and then spinning the filaments to form basalt fiber cloth with the thickness of 1 +/-0.2 mm. Mixing 85 parts of corn straw and 15 parts of vegetable gum, carrying out hot press molding for 40min at 100 ℃ and under the pressure of 3MPa, uniformly coating resin gum with the thickness of 2 +/-0.2 mm on the surface of the corn straw, pasting basalt fiber cloth, and then carrying out hot press for 10min at 50 ℃ and under the pressure of 0.5 MPa.

Example 3:

weighing 2 parts of Laponite nano particles, uniformly dispersing the Laponite nano particles in deionized water, stirring the mixture by using a magnetic stirrer for 5 hours, melting basalt at 1520 ℃ and infiltrating the basalt into filaments by using the impregnating compound in the platinum-rhodium alloy drawing process, and then spinning the filaments to form basalt fiber cloth with the thickness of 2 +/-0.2 mm. Mixing 92 parts of corn straw and 8 parts of vegetable gum, carrying out hot press molding for 40min at 110 ℃ under the pressure of 3MPa, uniformly coating resin gum with the thickness of 2 +/-0.2 mm on the surface of the mixture, pasting basalt fiber cloth, and then carrying out hot press for 10min at 50 ℃ under the pressure of 0.8 MPa.

Example 4:

weighing 4 parts of Laponite nano particles, uniformly dispersing the Laponite nano particles in deionized water, stirring the mixture by using a magnetic stirrer for 5 hours, melting basalt at 1520 ℃ and infiltrating the basalt into filaments by using the impregnating compound in the platinum-rhodium alloy drawing process, and then spinning the filaments to form basalt fiber cloth with the thickness of 1 +/-0.2 mm. Mixing 88 parts of corn straw and 12 parts of vegetable gum, hot-pressing at 100 ℃ and 3MPa for 40min, uniformly coating resin gum with the thickness of 1 +/-0.2 mm on the surface of the mixture, pasting basalt fiber cloth, and then hot-pressing at 50 ℃ and 0.6MPa for 10 min.

Example 5:

weighing 4 parts of Laponite nano particles, uniformly dispersing the Laponite nano particles in deionized water, stirring the mixture by using a magnetic stirrer for 5 hours, melting basalt at 1520 ℃ and infiltrating the basalt into filaments by using the impregnating compound in the platinum-rhodium alloy drawing process, and then spinning the filaments to form basalt fiber cloth with the thickness of 1 +/-0.2 mm. Mixing 90 parts of corn straw and 10 parts of vegetable gum, carrying out hot press molding for 40min at 100 ℃ and 2.5MPa, uniformly coating resin gum with the thickness of 2 +/-0.2 mm on the surface of the mixture, pasting basalt fiber cloth, and then carrying out hot press for 10min at 40 ℃ and 0.6 MPa.

Test example:

the performance experiments were performed on the basalt fiber novel flame-retardant and heat-insulating material modified with laponite, prepared in examples 1-5. The method for detecting the combustion performance is carried out according to GB/T8626-2007 flammability test method of building materials, the thermal insulation performance is measured according to GB50411-2007 construction quality acceptance criteria of building energy conservation engineering, the strength detection method is carried out according to GB/T8813-2008 determination of compression performance of rigid foam plastics, the water absorption determination is carried out according to GB/T8810-2005 determination of water absorption of rigid foam plastics, and the test results are shown in Table 1 and figure 1.

TABLE 1 values of Performance measurements of the examples

Examples	Oxygen index (%)	Thermal conductivity (W/(m.K))	Compressive Strength (KPa)	Water absorption (%)
					Example 1	66	0.0523	350	0.9
Example 2	69	0.0519	340	0.8
					Example 3	77	0.0492	360	0.8
Example 4	76	0.0516	350	0.9
					Example 5	77	0.0512	350	0.8