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CN102173567A - Method for preparing fiber reinforced microcrystalline glass insulation material - Google Patents

Method for preparing fiber reinforced microcrystalline glass insulation material Download PDF

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CN102173567A
CN102173567A CN 201110023765 CN201110023765A CN102173567A CN 102173567 A CN102173567 A CN 102173567A CN 201110023765 CN201110023765 CN 201110023765 CN 201110023765 A CN201110023765 A CN 201110023765A CN 102173567 A CN102173567 A CN 102173567A
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slag
devitrified glass
glass
microcrystalline glass
glass waste
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CN102173567B (en
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汤李缨
程金树
何峰
全健
李宏
郑伟宏
陆平
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Wuhan University of Technology WUT
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Abstract

The invention relates to a method for preparing a fiber reinforced microcrystalline glass insulation material, which is characterized by comprising the following steps of: (1) firstly, obtaining a slag staple fiber through the centrifugal blowing process at a high-temperature liquid slag outlet of an industrial furnace; (2) pulverizing microcrystalline glass into 0.1-0.5 mm particles to obtain microcrystalline glass waste particles; (3) selecting the following raw materials for later use in percentage by weight: 23-35% of slag staple fiber, 60-75% of microcrystalline glass waste particles and 2-7% of foaming agent; uniformly mixing the slag staple fiber, the microcrystalline glass waste particles and the foaming agent to obtain a mixture; and (4) loading the mixture into a die, heating the die to 850-950 DEG C in a calcining kiln, maintaining the temperature for 1.0-2.0 h to perform calcine, annealing and cooling the die, taking the material out of the die to form the fiber reinforced microcrystalline glass insulation material. The method provided by the invention is simple, saves energy and resources and is beneficial to environmental protection.

Description

一种纤维增强微晶玻璃保温材料的制备方法A preparation method of fiber-reinforced glass-ceramic thermal insulation material

技术领域technical field

本发明属于材料制造技术领域,具体涉及利用液态工业炉渣和微晶玻璃废料制备一种纤维增强微晶玻璃保温材料的方法。The invention belongs to the technical field of material manufacture, and in particular relates to a method for preparing a fiber-reinforced glass-ceramic thermal insulation material by using liquid industrial slag and glass-ceramic waste.

背景技术Background technique

随着现代工业的迅猛发展,工业固体废弃物的排放量逐年增加,对环境造成了严重的污染和破坏。如何有效利用工业固体废弃物并保护环境,已受到人们的普遍关注。目前,高温磷渣、冶金炉渣出炉的方式是将液态炉渣导出并水淬,使其成为一定大小的固体颗粒。利用磷渣、冶金炉渣等固体废弃物为原料制备微晶玻璃的方法已有报道,其制备方法是将包括炉渣在内的各种原料按一定配比混合后高温熔制,再成型、烧结、晶化、退火,虽然这些方法可以利用固体废弃物,但材料制备工艺过程较复杂,需对混合料重新进行高温熔化,因此能耗高。此外,在建筑装饰微晶玻璃生产过程中,一些废品和切裁边角料通常是重新回炉高温熔化,消耗了大量能源。With the rapid development of modern industry, the discharge of industrial solid waste has increased year by year, causing serious pollution and damage to the environment. How to effectively utilize industrial solid waste and protect the environment has attracted widespread attention. At present, the method of producing high-temperature phosphorus slag and metallurgical slag is to export the liquid slag and water quench it to make it into solid particles of a certain size. The method of preparing glass-ceramic by using solid wastes such as phosphorus slag and metallurgical slag as raw materials has been reported. Crystallization and annealing, although these methods can use solid waste, the material preparation process is more complicated, and the mixture needs to be re-melted at high temperature, so the energy consumption is high. In addition, in the production process of architectural decorative glass-ceramics, some waste products and cutting scraps are usually returned to the furnace for high-temperature melting, which consumes a lot of energy.

发明内容Contents of the invention

针对现有工业固体废弃物和微晶玻璃废料利用技术的不足,本发明的目的在于提供一种纤维增强微晶玻璃保温材料的制备方法,该方法工艺简单、节能,节约资源,利于环保。Aiming at the deficiencies of existing industrial solid waste and glass-ceramic waste utilization technologies, the purpose of the present invention is to provide a preparation method of fiber-reinforced glass-ceramic thermal insulation material, which is simple in process, energy-saving, resource-saving, and environmentally friendly.

为实现上述目的,本发明的技术方案是:一种纤维增强微晶玻璃保温材料的制备方法,其特征在于它包括如下步骤:In order to achieve the above object, the technical solution of the present invention is: a preparation method of fiber-reinforced glass-ceramic thermal insulation material, which is characterized in that it comprises the following steps:

1)首先在工业炉的高温液态炉渣(如磷渣、钢渣)出口,通过离心喷吹工艺获得炉渣短纤维;1) First, at the outlet of the high-temperature liquid slag (such as phosphorus slag, steel slag) of the industrial furnace, the slag short fiber is obtained through the centrifugal injection process;

2)将微晶玻璃废料粉碎成0.1~0.5mm的颗粒,得到微晶玻璃废料颗粒;2) crushing the glass-ceramic waste into particles of 0.1 to 0.5 mm in size to obtain glass-ceramic waste particles;

3)按各原料所占重量百分数为:炉渣短纤维23~35%、微晶玻璃废料颗粒60~75%、发泡剂2~7%,选取炉渣短纤维、微晶玻璃废料颗粒和发泡剂,备用;将炉渣短纤维、微晶玻璃废料颗粒和发泡剂混合均匀,得到混合料;3) According to the percentage by weight of each raw material: short slag fibers 23-35%, glass-ceramic waste particles 60-75%, foaming agent 2-7%, select slag short fibers, glass-ceramic waste particles and foaming agent, for subsequent use; mixing slag short fibers, glass-ceramic waste particles and foaming agent evenly to obtain a mixture;

4)将混合料放进模具中,然后置于烧成窑加热至850℃~950℃(室温至700℃升温速率为4~6℃/分钟,700℃以上升温速率为6~8℃/分钟)、保温1.0~2.0小时进行烧成;然后经退火、冷却(以15~20℃/分钟的降温速度降至600℃,再以0.7~1.2℃/分钟的降温速度降至250℃,然后以5~7℃/分钟的降温速度冷却至60℃),取出脱模,即获得纤维增强微晶玻璃保温材料。4) Put the mixture into the mold, and then place it in a firing kiln and heat it to 850°C-950°C (the heating rate from room temperature to 700°C is 4-6°C/min, and the heating rate above 700°C is 6-8°C/min ), heat preservation for 1.0-2.0 hours for firing; then annealing and cooling (down to 600°C at a cooling rate of 15-20°C/min, then down to 250°C at a cooling rate of 0.7-1.2°C/min, and then Cool down to 60°C at a cooling rate of 5-7°C/min), take it out and demould, and obtain a fiber-reinforced glass-ceramic thermal insulation material.

所述高温液态炉渣为高温液态磷渣或高温液态钢渣。The high-temperature liquid slag is high-temperature liquid phosphorus slag or high-temperature liquid steel slag.

所述微晶玻璃废料为建筑装饰用微晶玻璃废品或建筑装饰用微晶玻璃切裁的边角料。The glass-ceramics waste is waste glass-ceramics for architectural decoration or leftovers of glass-ceramics for architectural decoration.

所述发泡剂为碳粉、白云石、云母中的任意一种或任意二种以上(含任意二种)的混合物,任意二种以上(含任意二种)混合时为任意配比。The foaming agent is any one of carbon powder, dolomite, and mica, or a mixture of any two or more (including any two), and any two or more (including any two) are mixed in any proportion.

本发明的有益效果是:一是直接将工业炉的高温液态炉渣(磷渣、钢渣)制成短纤维作为原料,节约资源,利于环保;二是纤维状炉渣(炉渣短纤维)起到材料骨架结构的作用,与颗粒状微晶玻璃相结合,提高了整体强度。三是原料不需高温熔化,工艺过程简单并节省了大量能源。四是微晶玻璃废料因其本身已是微晶玻璃则不需再晶化,只需烧成而大大缩短了制备时间。The beneficial effects of the present invention are: firstly, the high-temperature liquid slag (phosphorus slag, steel slag) of the industrial furnace is directly made into short fibers as raw materials, which saves resources and is beneficial to environmental protection; The role of the structure, combined with the granular glass-ceramics, increases the overall strength. The third is that the raw materials do not need to be melted at high temperature, the process is simple and a large amount of energy is saved. The 4th, glass-ceramic waste material does not need recrystallization because of itself already is glass-ceramics, only needs to burn and has shortened preparation time greatly.

与其它保温材料相比,本发明材料具有纤维增强和微晶增强的双重特性,其抗折强度高、化学稳定性好、隔热性能好,使用温度范围广,可用于建筑物及工业设备的保温。Compared with other thermal insulation materials, the material of the present invention has dual characteristics of fiber reinforcement and microcrystalline reinforcement, high flexural strength, good chemical stability, good heat insulation performance, and wide service temperature range, and can be used for building and industrial equipment. insulation.

具体实施方式Detailed ways

为了更好地理解本发明,下面结合实施例进一步阐明本发明的内容,但本发明的内容不仅仅局限于下面的实施例。In order to better understand the present invention, the content of the present invention is further illustrated below in conjunction with the examples, but the content of the present invention is not limited to the following examples.

实施例1:Example 1:

一种纤维增强微晶玻璃保温材料的制备方法,它包括如下步骤:A method for preparing a fiber-reinforced glass-ceramic thermal insulation material, comprising the steps of:

1)首先在工业炉的高温液态炉渣出口(在制磷电炉出渣口),通过离心喷吹工艺获得炉渣短纤维;1) First, at the high-temperature liquid slag outlet of the industrial furnace (at the slag outlet of the phosphorus-making electric furnace), the slag short fibers are obtained through a centrifugal blowing process;

2)将微晶玻璃废料(建筑装饰用微晶玻璃切裁的边角料)粉碎成0.1~0.2mm的颗粒,得到微晶玻璃废料颗粒;2) Crushing the glass-ceramic waste (cutting scraps of glass-ceramics for architectural decoration) into particles of 0.1-0.2 mm to obtain glass-ceramic waste particles;

3)按各原料所占重量百分数为:炉渣短纤维35%、微晶玻璃废料颗粒61%、发泡剂(碳粉)4%,选取炉渣短纤维、微晶玻璃废料颗粒和发泡剂,备用;将炉渣短纤维、微晶玻璃废料颗粒和发泡剂混合均匀,得到混合料;3) According to the percentage by weight of each raw material: short slag fibers 35%, glass-ceramic waste particles 61%, blowing agent (carbon powder) 4%, choose short slag fibers, glass-ceramic waste particles and blowing agent, Standby; mixing slag short fibers, glass-ceramic waste particles and foaming agent evenly to obtain a mixture;

4)将混合料放进模具中,然后置于烧成窑加热至850℃(室温至700℃升温速率为5℃/分钟,700℃以上升温速率为8℃/分钟)、保温1.0小时进行烧成,利用纤维界面易于析晶的原理,短时间内形成大量纤维状微晶玻璃,而微晶玻璃粒料软化并出现部分液相,烧结成一整体材料,同时由于发泡剂的作用,在材料中形成一定量封闭气孔;然后经退火、冷却(以15℃/分钟的降温速度降至600℃,再以1℃/分钟的降温速度降至250℃,然后以5℃/分钟的降温速度冷却至60℃),取出脱模,即获得纤维增强微晶玻璃保温材料。4) Put the mixture into the mold, then place it in a firing kiln and heat it to 850°C (the temperature rise rate is 5°C/minute from room temperature to 700°C, and the temperature rise rate is 8°C/minute above 700°C), and keep it warm for 1.0 hours for firing Formation, using the principle that the fiber interface is easy to crystallize, a large amount of fibrous glass-ceramics is formed in a short period of time, and the glass-ceramics grains soften and part of the liquid phase appears, and are sintered into a whole material. A certain amount of closed pores are formed in the middle; then annealed and cooled (down to 600°C at a cooling rate of 15°C/min, then down to 250°C at a cooling rate of 1°C/min, and then cooled at a cooling rate of 5°C/min to 60°C), take it out and demould, and obtain fiber-reinforced glass-ceramic thermal insulation material.

所得到的纤维增强微晶玻璃保温材料的性能指标为:密度1.7g/cm3,抗折强度30MPa,吸水率<0.12%,耐酸性0.011%,耐碱性0.014%,使用温度-50℃~600℃。The performance indicators of the obtained fiber-reinforced glass-ceramic insulation material are: density 1.7g/cm 3 , flexural strength 30MPa, water absorption < 0.12%, acid resistance 0.011%, alkali resistance 0.014%, service temperature -50℃~ 600°C.

实施例2:Example 2:

一种纤维增强微晶玻璃保温材料的制备方法,它包括如下步骤:A method for preparing a fiber-reinforced glass-ceramic thermal insulation material, comprising the steps of:

1)首先在工业炉的高温液态炉渣出口(即炼钢炉出渣口),通过离心喷吹工艺获得炉渣短纤维;1) First, at the high-temperature liquid slag outlet of the industrial furnace (that is, the slag outlet of the steelmaking furnace), the slag short fibers are obtained through a centrifugal injection process;

2)将微晶玻璃废料(即建筑装饰用微晶玻璃废品)粉碎成0.2~0.3mm的颗粒,得到微晶玻璃废料颗粒;2) Crushing the glass-ceramic waste (ie glass-ceramic waste for architectural decoration) into particles of 0.2-0.3 mm to obtain glass-ceramic waste particles;

3)按各原料所占重量百分数为:炉渣短纤维30%、微晶玻璃废料颗粒64%、发泡剂(白云石)6%,选取炉渣短纤维、微晶玻璃废料颗粒和发泡剂,备用;将炉渣短纤维、微晶玻璃废料颗粒和发泡剂混合均匀,得到混合料;3) according to the percentage by weight of each raw material: short slag fibers 30%, glass-ceramic waste particles 64%, blowing agent (dolomite) 6%, select short slag fibers, glass-ceramics waste particles and blowing agent, Standby; mixing slag short fibers, glass-ceramic waste particles and foaming agent evenly to obtain a mixture;

4)将混合料放进模具中,然后置于烧成窑加热至880℃(室温至700℃升温速率为4℃/分钟,700℃~880℃升温速率为7℃/分钟)、保温1.5小时进行烧成,利用纤维界面易于析晶的原理,短时间内形成大量纤维状微晶玻璃,而微晶玻璃粒料软化并出现部分液相,烧结成一整体材料,同时由于发泡剂的作用,在材料中形成一定量封闭气孔;然后经退火、冷却(以18℃/分钟的降温速度降至600℃,再以0.8℃/分钟的降温速度降至250℃,然后以6℃/分钟的降温速度冷却至60℃),取出脱模,即获得纤维增强微晶玻璃保温材料。4) Put the mixture into the mold, then place it in a firing kiln and heat it to 880°C (the temperature rise rate is 4°C/min from room temperature to 700°C, and the temperature rise rate is 7°C/min from 700°C to 880°C), and keep warm for 1.5 hours Sintering, using the principle that the fiber interface is easy to crystallize, a large amount of fibrous glass-ceramics is formed in a short time, and the glass-ceramic grains soften and part of the liquid phase appears, and sintered into a whole material. At the same time, due to the action of the foaming agent, A certain amount of closed pores are formed in the material; then annealed and cooled (down to 600°C at a cooling rate of 18°C/min, then down to 250°C at a cooling rate of 0.8°C/min, and then at a cooling rate of 6°C/min speed cooling to 60°C), take out and demould, and obtain fiber-reinforced glass-ceramic insulation material.

获得的纤维增强微晶玻璃保温材料的性能指标为:1.8g/cm3,抗折强度35MPa,吸水率<0.10%,耐酸性0.010%,耐碱性0.013%,使用温度-50℃~600℃。The performance indicators of the obtained fiber-reinforced glass-ceramic insulation material are: 1.8g/cm 3 , flexural strength 35MPa, water absorption <0.10%, acid resistance 0.010%, alkali resistance 0.013%, service temperature -50℃~600℃ .

实施例3:Example 3:

一种纤维增强微晶玻璃保温材料的制备方法,它包括如下步骤:A method for preparing a fiber-reinforced glass-ceramic thermal insulation material, comprising the steps of:

1)首先在工业炉的高温液态炉渣出口(在制磷电炉出渣口),通过离心喷吹工艺获得炉渣短纤维;1) First, at the high-temperature liquid slag outlet of the industrial furnace (at the slag outlet of the phosphorus-making electric furnace), the slag short fibers are obtained through a centrifugal blowing process;

2)将微晶玻璃废料粉碎成0.3~0.4mm的颗粒,得到微晶玻璃废料颗粒;2) crushing the waste glass-ceramics into particles of 0.3-0.4 mm to obtain waste glass-ceramics granules;

3)按各原料所占重量百分数为:炉渣短纤维23%、微晶玻璃废料颗粒75%、发泡剂(云母)2%,选取炉渣短纤维、微晶玻璃废料颗粒和发泡剂,备用;将炉渣短纤维、微晶玻璃废料颗粒和发泡剂混合均匀,得到混合料;3) According to the percentage by weight of each raw material: short slag fibers 23%, glass-ceramic waste particles 75%, foaming agent (mica) 2%, select short slag fibers, glass-ceramic waste particles and foaming agent, and reserve ; mix the slag short fiber, glass-ceramic waste particles and foaming agent evenly to obtain a mixture;

4)将混合料放进模具中,然后置于烧成窑加热至900℃(室温至700℃升温速率为6℃/分钟,700℃以上升温速率为8℃/分钟)、保温1.5小时进行烧成;然后经退火、冷却(以20℃/分钟的降温速度降至600℃,再以0.7℃/分钟的降温速度降至250℃,然后以5℃/分钟的降温速度冷却至60℃),取出脱模,即获得纤维增强微晶玻璃保温材料。4) Put the mixture into the mold, then place it in a firing kiln and heat it to 900°C (the temperature rise rate is 6°C/min from room temperature to 700°C, and the temperature rise rate is 8°C/min above 700°C), and keep it warm for 1.5 hours for firing into; then annealed and cooled (down to 600°C at a cooling rate of 20°C/min, then down to 250°C at a cooling rate of 0.7°C/min, and then cooled to 60°C at a cooling rate of 5°C/min), Take it out and demould, and obtain the fiber-reinforced glass-ceramic thermal insulation material.

获得的纤维增强微晶玻璃保温材料的性能指标为:1.9g/cm3,抗折强度36MPa,吸水率<0.11%,耐酸性0.010%,耐碱性0.013%,使用温度-50℃~600℃。The performance indicators of the obtained fiber-reinforced glass-ceramic insulation material are: 1.9g/cm 3 , flexural strength 36MPa, water absorption <0.11%, acid resistance 0.010%, alkali resistance 0.013%, service temperature -50℃~600℃ .

实施例4:Example 4:

一种纤维增强微晶玻璃保温材料的制备方法,它包括如下步骤:A method for preparing a fiber-reinforced glass-ceramic thermal insulation material, comprising the steps of:

1)首先在工业炉的高温液态炉渣出口(即炼钢炉出渣口),通过离心喷吹工艺获得炉渣短纤维;1) First, at the high-temperature liquid slag outlet of the industrial furnace (that is, the slag outlet of the steelmaking furnace), the slag short fibers are obtained through a centrifugal injection process;

2)将微晶玻璃废料粉碎成0.4~0.5mm的颗粒,得到微晶玻璃废料颗粒;2) crushing the waste glass-ceramics into particles of 0.4-0.5 mm to obtain waste glass-ceramics granules;

3)按各原料所占重量百分数为:炉渣短纤维33%、微晶玻璃废料颗粒60%、发泡剂7%(碳粉4%,白云石3%),选取炉渣短纤维、微晶玻璃废料颗粒和发泡剂,备用;将炉渣短纤维、微晶玻璃废料颗粒和发泡剂混合均匀,得到混合料;3) According to the percentage by weight of each raw material: short slag fiber 33%, glass-ceramic waste particles 60%, foaming agent 7% (carbon powder 4%, dolomite 3%), select slag short fiber, glass-ceramic Waste granules and foaming agent are used for standby; slag short fibers, glass-ceramic waste particles and foaming agent are evenly mixed to obtain a mixture;

4)将混合料放进模具中,然后置于烧成窑加热至950℃(室温至700℃升温速率为5℃/分钟,700℃~950℃升温速率为8℃/分钟)、保温2.0小时进行烧成;然后经退火、冷却(以16℃/分钟的降温速度降至600℃,再以1.2℃/分钟的降温速度降至250℃,然后以6℃/分钟的降温速度冷却至60℃),取出脱模,即获得纤维增强微晶玻璃保温材料。4) Put the mixture into the mold, then place it in a firing kiln and heat it to 950°C (the temperature rise rate is 5°C/min from room temperature to 700°C, and the temperature rise rate is 8°C/min from 700°C to 950°C), and keep warm for 2.0 hours Firing; then annealed, cooled (down to 600°C at a cooling rate of 16°C/min, then down to 250°C at a cooling rate of 1.2°C/min, and then cooled to 60°C at a cooling rate of 6°C/min ), take out the demoulding, and obtain the fiber-reinforced glass-ceramic thermal insulation material.

获得的纤维增强微晶玻璃保温材料的性能指标为:1.7g/cm3,抗折强度30MPa,吸水率<0.15%,耐酸性0.011%,耐碱性0.014%,使用温度-50℃~600℃。The performance indicators of the obtained fiber-reinforced glass-ceramic insulation material are: 1.7g/cm 3 , flexural strength 30MPa, water absorption <0.15%, acid resistance 0.011%, alkali resistance 0.014%, service temperature -50℃~600℃ .

Claims (4)

1. the preparation method of a fiber reinforcement devitrified glass lagging material is characterized in that it comprises the steps:
1) at first in the high-temperature liquid state slag outlet of industrial furnace, obtains the slag staple fibre by centrifugal blowing process;
2) the devitrified glass waste material is ground into the particle of 0.1~0.5mm, obtains devitrified glass waste material particle;
3) by the shared weight percentage of each raw material be: slag staple fibre 23~35%, devitrified glass waste material particle 60~75%, whipping agent 2~7%, choose slag staple fibre, devitrified glass waste material particle and whipping agent, standby; Slag staple fibre, devitrified glass waste material particle and whipping agent are mixed, obtain compound;
4) compound is put in the mould, placed calcining kiln to be heated to 850 ℃~950 ℃, insulation then and burnt till in 1.0~2.0 hours; Through annealing, cooling, take out the demoulding then, promptly obtain fiber reinforcement devitrified glass lagging material.
2. the preparation method of a kind of fiber reinforcement devitrified glass lagging material according to claim 1 is characterized in that: described high-temperature liquid state slag is high-temperature liquid state phosphorus slag or high-temperature liquid state slag.
3. the preparation method of a kind of fiber reinforcement devitrified glass lagging material according to claim 1 is characterized in that: described devitrified glass waste material is the scrap stock of architectural decoration devitrified glass waste product or architectural decoration devitrified glass cutting.
4. the preparation method of a kind of fiber reinforcement devitrified glass lagging material according to claim 1, it is characterized in that: described whipping agent is any one or any mixture more than two kinds in carbon dust, rhombspar, the mica, and any is any proportioning when mixing more than two kinds.
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CN103742757A (en) * 2013-09-11 2014-04-23 太仓派欧技术咨询服务有限公司 Preparation device and preparation method for glass fiber core material pulp
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CN1868946A (en) * 2006-06-06 2006-11-29 武汉理工大学 Waste residue microcrystal glass and its preparation method
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