WO2021022589A1 - 一种以金矿尾砂为原料的泡沫陶瓷及其制备方法 - Google Patents

一种以金矿尾砂为原料的泡沫陶瓷及其制备方法 Download PDF

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WO2021022589A1
WO2021022589A1 PCT/CN2019/101868 CN2019101868W WO2021022589A1 WO 2021022589 A1 WO2021022589 A1 WO 2021022589A1 CN 2019101868 W CN2019101868 W CN 2019101868W WO 2021022589 A1 WO2021022589 A1 WO 2021022589A1
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preparation
temperature
prepared
gold tailings
raw materials
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French (fr)
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孙晓刚
邱景平
邢军
王海龙
程春宏
赵英良
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东北大学
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    • C04B33/00—Clay-wares
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Definitions

  • the invention relates to the field of building materials, in particular to a foam ceramic using gold tailings as raw materials and a preparation method thereof.
  • Gold mine tailings are solid wastes generated after gold mine beneficiation. According to the "Annual Report on Comprehensive Utilization of Resources in China (2014)” released by the National Development and Reform Commission, in 2013, China's gold tailings produced 214 million tons of gold tailings. However, the comprehensive utilization rate of gold tailings is less than 20%, and as mining continues, the output of gold tailings will increase. On December 20, 2016, the State Council issued the “Thirteenth Five-Year Plan for Energy Conservation and Emission Reduction”, which clarified the energy-saving goals under the new normal of economic development, while vigorously developing a circular economy, and strengthening urban waste treatment and bulk solid waste. By 2020, the recycling rate of main waste will reach 54.6%.
  • the common building insulation materials are mineral wool rock wool, polyurethane foam, polystyrene foam board, aerated concrete, etc.
  • the current market is dominated by organic insulation materials, although they are lightweight , Good thermal insulation, simple production process, but it has the fatal flaws of poor fire resistance and high potential safety hazards.
  • organic thermal insulation materials have been hollowed, peeled, cracked, Problems such as water absorption and frost heave even cause the external wall insulation layer and finish layer to fall off as a whole.
  • ceramic foam has light weight, high strength, fire resistance, good thermal insulation performance, non-toxic, corrosion-resistant, non-absorbent, non-aging, and sticks to cement mortar.
  • the characteristics of good connection performance, using foam ceramics as external wall insulation materials can effectively solve the above problems.
  • the present invention provides a ceramic foam using gold tailings as raw materials and a preparation method thereof.
  • the purpose of the present invention is to provide a foam ceramic using gold tailings as a raw material and a preparation method thereof.
  • the foam ceramic has the characteristics of light weight, high strength and high tailings utilization rate.
  • One aspect of the present invention provides a foam ceramic using gold tailings as raw materials, prepared from the following mass percentages of raw materials: gold tailings 59.8%-74%, potash feldspar 5%-15%, albite 5%-20%, silicon carbide 0.2%-1%, bentonite 6%-9%, calcite 1%-4%.
  • Another aspect of the present invention provides a method for preparing foam ceramics based on the above-mentioned component raw materials, which includes the following steps:
  • Step 1 Weigh gold tailings, potash feldspar, albite, silicon carbide, bentonite, and calcite according to mass percentage;
  • Step 2 Use a ball mill for ball milling and mixing
  • Step 3 Put the ball-milled powder into a mold to flatten and compact to obtain a green body
  • Step 4 Send the green body into a high-temperature furnace for firing.
  • the second step specifically includes: putting the mixture into a planetary ball mill for ball milling for 1-2 hours, and then passing through a 200-mesh sieve.
  • the step 3 specifically includes putting the ball-milled powder into a corundum-mullite sagger with a thickness of 1mm and a refractoriness of 1260°C aluminum silicate paper on the inner wall and bottom surface, and then flattening and compacting it.
  • the powder volume is 40%-50% of the sagger volume.
  • the step 4 specifically includes placing the prepared green body in a lift-type high-temperature sintering furnace, heating it from room temperature to 400-600°C at a heating rate of 10-15°C/min, holding it for 20-50 minutes, and then The heating rate is 5-10°C/min to 800-1000°C, and then the heating rate is 2-5°C/min to 1150-1200°C, holding for 30min-90min, and annealing after firing, first at 15-20 Cool down to 500-700°C at a rate of °C/min, keep for 30-60min, and then cool to room temperature with the furnace.
  • the present invention has the following technical effects:
  • the present invention uses gold tailings as the main raw material to prepare foam ceramics with excellent performance.
  • the addition amount of gold tailings is 59.8%-74%, which ensures the large use of gold tailings and reduces the impact of tailings on the ecological environment.
  • the impact provides new ideas for the bulk and high-value utilization of tailings;
  • the foam ceramic of the present invention has a bulk density of 400-750kg/cm 3 , a compressive strength of 3.5-8.0Mpa, an average bubble diameter of 1-3mm, good compressive strength of the product, uniform bubble distribution, and can be used as wall insulation material;
  • the present invention adopts a staged annealing method. Through rapid annealing, the integrity of the internal cell structure is ensured, the defects generated by the bubbles during the curing process are avoided, and the physical and chemical properties of the foam ceramic are further improved;
  • the present invention adopts the "one-step powder sintering method", through which gold tailings and other additives are evenly mixed, the source of raw materials is wide, the production cost is low, the process is simple, the firing cycle is short, the energy consumption is small, and it has significant economic benefits.
  • Figure 1 is an apparent structure diagram of the foamed ceramic prepared in Example 1 of the present invention.
  • Figure 2 is an apparent structure diagram of the foamed ceramic prepared in Example 2 of the present invention.
  • Figure 3 is an apparent structure diagram of the foamed ceramic prepared in Example 3 of the present invention.
  • Figure 4 is an apparent structure diagram of the foamed ceramic prepared in Example 4 of the present invention.
  • the present invention provides a foamed ceramic using gold tailings as raw materials and a preparation method thereof.
  • the gold tailings used in the embodiments include, by mass fraction, SiO 2 : 65%-75%; Al 2 O 3 : 10%-20%; CaO: 0.5%-3%; MgO: 0.1%-2%; Fe 2 O 3 : 2%-5%; K 2 O: 2%-5%; Na 2 O : 0.1%-2%; TiO 2 : 0.1%-2%; others 1%-5%.
  • the foam ceramic of this embodiment is prepared from the following mass percentages of raw materials: 59.8% gold tailings, 15% potash feldspar, 15% albite, 9% bentonite, 0.2% silicon carbide, and 1% calcite.
  • Firing Put the prepared green body into a lift-type high-temperature sintering furnace, heat up from room temperature to 400°C at a heating rate of 10°C/min, hold for 50 minutes, and then heat up to 800°C at a heating rate of 5°C/min. Subsequently, the temperature was raised to 1200°C at a heating rate of 5°C/min, and the temperature was kept for 30 minutes; after the firing, the temperature was lowered to 500°C at a rate of 20°C/min, the temperature was kept for 60 minutes, and then cooled to room temperature with the furnace.
  • the foam ceramic of this embodiment is prepared from the following mass percentages of raw materials: 64.5% of gold tailings, 5% of potash feldspar, 20% of albite, 8% of bentonite, 0.5% of silicon carbide, and 2% of calcite.
  • Forming Put the ball-milled powder into a corundum mullite sagger with a thickness of 1mm and a refractoriness of 1260°C aluminum silicate paper on the inner wall and bottom surface. After being flattened and compacted, the volume of the powder is casket. 40% of the bowl volume.
  • the foam ceramic of this embodiment is prepared from the following mass percentages of raw materials: 69.3% gold tailings, 15% potash feldspar, 5% albite, 7% bentonite, 0.7% silicon carbide, and 3% calcite.
  • the foam ceramic of this embodiment is prepared from the following mass percentages of raw materials: 74% gold tailings, 10% potash feldspar, 5% albite, 6% bentonite, 1% silicon carbide, and 4% calcite.
  • Firing Put the prepared green body into a lift-type high-temperature sintering furnace, heat up from room temperature to 600°C at a heating rate of 15°C/min, hold for 20 minutes, and then heat up to 1000°C at a heating rate of 10°C/min. Subsequently, the temperature was raised to 1150°C at a heating rate of 2°C/min, and the temperature was kept for 90 minutes; after the firing was completed, the temperature was lowered to 700°C at a rate of 15°C/min, and the temperature was kept for 30 minutes.

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Abstract

一种以金矿尾砂为原料的泡沫陶瓷及制备方法，由如下质量百分数的原料制备而成：金矿尾砂59.8％-74％，钾长石5％-15％，钠长石5％-20％，碳化硅0.2％-1％，膨润土6％-9％，方解石1％-4％；制备方法包括：配料混合，球磨，压制成型，然后在1150-1200℃的空气气氛下烧结，保温时间为30min-90min，制得泡沫陶瓷。制备方法中金矿尾砂利用率高，制得的泡沫陶瓷轻质，高强。

Description

一种以金矿尾砂为原料的泡沫陶瓷及其制备方法 技术领域
本发明涉及建筑材料领域，具体为一种以金矿尾砂为原料的泡沫陶瓷及其制备方法。
背景技术
金矿尾砂是金矿选矿后产生的固体废弃物，据国家发改委发布《中国资源综合利用年度报告(2014)》统计，在2013年，中国黄金尾矿产生量就达到了2.14亿吨黄金尾矿，然而，黄金尾砂综合利用率则不到20％，并且随着开采的持续进行，黄金尾砂产量会越来越多。2016年12月20日，国务院印发了《“十三五”节能减排综合工作方案》，明确了经济发展新常态下的节能目标，同时大力发展循环经济，加强城市废弃物处理和大宗固体废弃物的综合利用，到2020年，主要废弃物循环利用率达到54.6％左右。
目前建筑保温材料中常见的有建筑保温中常见的材料有矿棉岩棉、聚氨酯泡沫塑料、聚苯乙烯泡沫板、加气混凝土等，目前市场中以有机保温材料为主，虽然其具有质轻、保温性好、生产工艺简单，但是其却有防火性能差、安全隐患大的致命缺陷，在实际应用中，大多数有机保温材料仅仅使用不到10年便出现了空鼓、剥落、开裂、吸水、冻胀等问题，甚至诱发外墙保温层及饰面层整体脱落。针对有机保温材料存在的问题，泡沫陶瓷作为一种新型的保温隔热墙体材料，具有轻质、高强、防火、保温性能好、无毒、耐腐蚀、不吸水，不老化、与水泥砂浆粘接性能良好的特点，采用泡沫陶瓷作为外墙保温材料能够有效解决以上问题。
鉴于泡沫陶瓷的良好的实用性，以及实现对废弃物的循环利用，本发明提供一种以金矿尾砂为原料的泡沫陶瓷及其制备方法。
发明概述
技术问题
问题的解决方案
技术解决方案
本发明的目的在于提供一种以金矿尾砂为原料的泡沫陶瓷及其制备方法，该泡沫陶瓷具有轻质、高强、尾砂利用率高的特点。
本发明一方面提供一种以金矿尾砂为原料的泡沫陶瓷，由如下质量百分数的原料制备而成：金矿尾砂59.8％-74％，钾长石5％-15％，钠长石5％-20％、碳化硅0.2％-1％、膨润土6％-9％、方解石1％-4％。
本发明另一方面提供一种基于上述组分原料制备泡沫陶瓷的方法，包括以下步骤：
步骤一：按质量百分比称取金矿尾砂、钾长石、钠长石、碳化硅、膨润土、方解石；
步骤二：采用球磨机进行球磨、混料；
步骤三：将球磨后的粉料放入模具中铺平压实得到生坯；
步骤四：将生坯送入高温炉内烧制。
优选的，所述步骤二具体为：将混合料放入行星球磨机中球磨1-2h，然后过200目筛。
优选的，所述步骤三具体为，将球磨后的粉料，放入到内壁及底面铺有厚度1mm、耐火度1260℃硅酸铝纸的刚玉莫来石匣钵中，铺平压实后，粉料体积为匣钵体积的40％-50％。
优选的，所述步骤四具体为，将制得的生坯置入升降式高温烧结炉内，自室温以10-15℃/min升温速率升温至400-600℃，保温20-50min，再以5-10℃/min升温速率升温至800-1000℃，随后以2-5℃/min升温速率升温至1150-1200℃，保温30min-90min，烧成结束后对其退火，先以15-20℃/min速率降温至500-700℃，保温30-60min，之后随炉冷却至室温。
发明的有益效果
有益效果
与现有技术相比，本发明具有以下技术效果：
(1)本发明以金矿尾砂主要原料，制备出性能优良的泡沫陶瓷，黄金尾砂添加量为59.8％-74％，保证了金矿尾砂的大量使用，减少尾砂对生态环境的影响， 为尾砂的大宗化、高值化利用提供了新思路；
(2)本发明所述的泡沫陶瓷体积密度为400-750kg/cm 3，抗压强度3.5-8.0Mpa，平均泡径1-3mm，产品抗压强度好，气泡分布均匀，可作为墙体保温材料；
(3)本发明采用分阶段退火方式，通过快速退火，保证了内部孔泡结构的完整性，避免了气泡在固化过程中产生的缺陷，进一步提高了泡沫陶瓷物理化学性能；
(4)本发明采用“一步粉末烧结法”，通过金矿尾砂与其他添加剂混合均匀，原料来源广泛，生产成本低，工艺简单，烧成周期短，能耗小，具有显著的经济效益。
对附图的简要说明
附图说明
图1是本发明实施例1所制备的泡沫陶瓷的表观结构图；
图2是本发明实施例2所制备的泡沫陶瓷的表观结构图；
图3是本发明实施例3所制备的泡沫陶瓷的表观结构图；
图4是本发明实施例4所制备的泡沫陶瓷的表观结构图。
发明实施例
本发明的实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。
本发明提供了一种以金矿尾砂为原料的泡沫陶瓷及其制备方法，实施例中所采用的金矿尾砂其组分按质量分数计包括，SiO 2：65％-75％；Al 2O 3：10％-20％；CaO：0.5％-3％；MgO：0.1％-2％；Fe 2O 3：2％-5％；K 2O：2％-5％；Na 2O：0.1％-2％；TiO 2：0.1％-2％；其他1％-5％。
实施例1
本实施例的泡沫陶瓷，由如下质量百分数的原料制备而成：金矿尾砂59.8％、钾长石15％、钠长石15％、膨润土9％、碳化硅0.2％、方解石1％。
本实施例的金矿尾砂制备泡沫陶瓷制备方法，包括以下步骤：
1.混料：将金矿尾砂、钾长石、钠长石、碳化硅、膨润土、方解石按质量百分比称取配合料；
2.粉磨：将混合料放入行星球磨机中球磨1h，然后过200目筛；
3.成型：将球磨后的粉料，放入到内壁及底面铺有厚度1mm、耐火度1260℃硅酸铝纸的刚玉莫来石匣钵中，铺平压实后，粉料体积为匣钵体积的45％；
4.烧制：将制得的生坯置入升降式高温烧结炉内，自室温以10℃/min升温速率升温至400℃，保温50min，再以5℃/min升温速率升温至800℃，随后以5℃/min升温速率升温至1200℃，保温30min；烧成结束后对其退火，先以20℃/min速率降温至500℃，保温60min，之后随炉冷却至室温。
实施例2
本实施例的泡沫陶瓷，由如下质量百分数的原料制备而成：金矿尾砂64.5％、钾长石5％、钠长石20％、膨润土8％、碳化硅0.5％、方解石2％。
实施例的金矿尾砂制备泡沫陶瓷制备方法，包括以下步骤：
1.混料：将金矿尾砂、钾长石、钠长石、碳化硅、膨润土、方解石按质量百分比称取配合料。
2.粉磨：将混合料放入行星球磨机中球磨1h，然后过200目筛。
3.成型：将球磨后的粉料，放入到内壁及底面铺有厚度1mm、耐火度1260℃硅酸铝纸的刚玉莫来石匣钵中，铺平压实后，粉料体积为匣钵体积的40％。
4.烧制：将制得的生坯置入升降式高温烧结炉内，自室温以12℃/min升温速率升温至450℃，保温40min，再以7℃/min升温速率升温至850℃，随后以4℃/min升温速率升温至1180℃，保温50min；烧成结束后对其退火，先以18℃/min速率降温至550℃，保温50min，之后随炉冷却至室温。
实施例3
本实施例的泡沫陶瓷，由如下质量百分数的原料制备而成：金矿尾砂69.3％、钾长石15％、钠长石5％、膨润土7％、碳化硅0.7％、方解石3％。
实施例的金矿尾砂制备泡沫陶瓷制备方法，包括以下步骤：
1.混料：将金矿尾砂、钾长石、钠长石、碳化硅、膨润土、方解石按质量百分 比称取配合料。
2.粉磨：将混合料放入行星球磨机中球磨1h，然后过200目筛；
3.成型：将球磨后的粉料，放入到内壁及底面铺有厚度1mm、耐火度1260℃硅酸铝纸的刚玉莫来石匣钵中，铺平压实后，粉料体积为匣钵体积的50％；
4.烧制：将制得的生坯置入升降式高温烧结炉内，自室温以14℃/min升温速率升温至550℃，保温30min，再以8℃/min升温速率升温至950℃，随后以3℃/min升温速率升温至1170℃，保温70min；烧成结束后对其退火，先以17℃/min速率降温至650℃，保温40min，之后随炉冷却至室温。
实施例4
本实施例的泡沫陶瓷，由如下质量百分数的原料制备而成：金矿尾砂74％、钾长石10％、钠长石5％、膨润土6％、碳化硅1％、方解石4％。
实施例的金矿尾砂制备泡沫陶瓷制备方法，包括以下步骤：
1.混料：将金矿尾砂、钾长石、钠长石、碳化硅、膨润土、方解石按质量百分比称取配合料；
2.粉磨：将混合料放入行星球磨机中球磨1h，然后过200目筛；
3.成型：将球磨后的粉料，放入到内壁及底面铺有厚度1mm、耐火度1260℃硅酸铝纸的刚玉莫来石匣钵中，铺平压实后，粉料体积为匣钵体积的40％；
4.烧制：将制得的生坯置入升降式高温烧结炉内，自室温以15℃/min升温速率升温至600℃，保温20min，再以10℃/min升温速率升温至1000℃，随后以2℃/min升温速率升温至1150℃，保温90min；烧成结束后对其退火，先以15℃/min速率降温至700℃，保温30min，之后随炉冷却至室温。
各实施例制备的泡沫陶瓷的表观结构图如图1-4所示，对各实施例中制备的泡沫陶瓷进行性能测试，结果参见表1：
表1泡沫陶瓷性能测试表
[Table 1]
Figure PCTCN2019101868-appb-000001
以上技术方案阐述了本发明的技术思路，不能以此限定本发明的保护范围，凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上技术方案所作的任何改动及修饰，均属于本发明技术方案的保护范围。

Claims (6)

  1. 一种以金矿尾砂为原料的泡沫陶瓷，其特征在于，由如下质量百分数的原料制备而成：金矿尾砂59.8％-74％，钾长石5％-15％，钠长石5％-20％、碳化硅0.2％-1％、膨润土6％-9％、方解石1％-4％。
  2. 一种制备如权利要求1所述的以金矿尾砂为原料的泡沫陶瓷的方法，其特征在于，包括以下步骤：
    步骤一：按质量百分比称取金矿尾砂、钾长石、钠长石、碳化硅、膨润土、方解石；
    步骤二：采用球磨机进行球磨、混料；
    步骤三：将球磨后的粉料放入模具中铺平压实得到生坯；
    步骤四：将生坯送入高温炉内烧制。
  3. 如权利要求2所述的制备方法，其特征在于，所述步骤二具体为：将混合料放入行星球磨机中球磨1-2h，然后过200目筛。
  4. 如权利要求2所述的制备方法，其特征在于，所述步骤三具体为，将球磨后的粉料，放入到内壁及底面铺有厚度1mm、耐火度1260℃硅酸铝纸的刚玉莫来石匣钵中，铺平压实后，粉料体积为匣钵体积的40％-50％。
  5. 如权利要求2所述的制备方法，其特征在于，所述步骤四具体为，将制得的生坯置入升降式高温烧结炉内，自室温以10-15℃/min升温速率升温至400-600℃，保温20-50min，再以5-10℃/min升温速率升温至800-1000℃，随后以2-5℃/min升温速率升温至1150-1200℃，保温30min-90min，烧成结束后对其退火，先以15-20℃/min速率降温至500-700℃，保温30-60min，之后随炉冷却至室温。
  6. 如权利要求2所述的制备方法，其特征在于，所制备的泡沫陶瓷体积密度为400-750kg/cm 3，抗压强度3.5-8.0Mpa，导热系数为0.042-0.065W/(m·k)；孔隙率为54.7％-65.3％。
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