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CN116589289A - Acid-resistant castable and preparation method thereof - Google Patents

Acid-resistant castable and preparation method thereof Download PDF

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CN116589289A
CN116589289A CN202310538855.9A CN202310538855A CN116589289A CN 116589289 A CN116589289 A CN 116589289A CN 202310538855 A CN202310538855 A CN 202310538855A CN 116589289 A CN116589289 A CN 116589289A
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acid
resistant
parts
powder
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朱国平
王立旺
彭晶晶
王琪
李新明
方利华
施展
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Zhejiang Kingcred New Material Co ltd
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Zhejiang Kingcred New Material Co ltd
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Abstract

本发明公开了一种耐酸浇注料及其制备方法。本发明以回收陶瓷、刚玉、焦宝石作为耐酸骨料,以硅微粉、活性氧化铝粉作为耐酸粉料,以硅溶胶作为结合剂,在此基础上添加铝酸盐水泥、水以及外加剂,制备的耐酸浇注料结构致密,具有强度高、耐磨性优异、抗渗透性好、热稳定性高、抗酸性好等优点,能够满足设备内衬的使用条件,可以有效保障设备安全稳定的运行,有助于取得良好的经济效益和社会效益。The invention discloses an acid-resistant pouring material and a preparation method thereof. In the present invention, recycled ceramics, corundum and coke gemstones are used as acid-resistant aggregates, silica micropowder and activated alumina powder are used as acid-resistant powders, silica sol is used as a binder, and aluminate cement, water and admixtures are added on this basis. The prepared acid-resistant castable has a dense structure and has the advantages of high strength, excellent wear resistance, good permeability resistance, high thermal stability, and good acid resistance. It can meet the use conditions of the equipment lining and effectively ensure the safe and stable operation of the equipment. , help to achieve good economic and social benefits.

Description

一种耐酸浇注料及其制备方法A kind of acid-resistant castable and preparation method thereof

技术领域technical field

本发明涉及一种耐酸浇注料及其制备方法,属于耐火材料领域。The invention relates to an acid-resistant castable and a preparation method thereof, belonging to the field of refractory materials.

背景技术Background technique

耐火材料可以分成定型耐火材料和不定型耐火材料。不定型耐火材料中使用最广泛的是浇注料。浇注料主要由耐火骨料、粉料、结合剂以及外加剂组成,具有较高的流动性,一般用浇筑方法施工,无需加热即可硬化。但用于冶金、医药、化工、石油等行业中的各种塔、炉、烟囱等设备内衬的耐火浇注料,因受到热应力的作用以及酸性水汽的侵蚀,在使用一段时间后就会损坏。Refractories can be divided into shaped refractories and unshaped refractories. Castables are the most widely used in unshaped refractories. The castable is mainly composed of refractory aggregate, powder, binder and admixture. It has high fluidity. It is generally constructed by pouring method and can be hardened without heating. However, the refractory castables used for the lining of various towers, furnaces, chimneys and other equipment in metallurgy, medicine, chemical industry, petroleum and other industries will be damaged after a period of use due to the effect of thermal stress and the erosion of acidic water vapor. .

申请公布号为CN115180964A的专利,公开了一种高强耐酸轻质浇注料,其组分为:莫来石质轻骨料、烧结板状刚玉、抗酸填充料、焦宝石、蓝晶石、二氧化硅微粉、锂辉石、工业氧化铝细粉、高铝水泥、一级高铝熟料粉、耐火纤维、外加剂。该浇筑料可以抵抗酸腐蚀但是抗渗透性不好,受到水汽侵蚀后容易开裂。The patent application publication No. CN115180964A discloses a high-strength acid-resistant lightweight castable. Silica micropowder, spodumene, industrial alumina fine powder, high alumina cement, first grade high alumina clinker powder, refractory fiber, admixture. The pouring material can resist acid corrosion but has poor permeability resistance, and it is easy to crack after being corroded by water vapor.

申请公布号为CN112573909A的专利,公开了一种基于纳米硅溶胶的陶瓷耐磨料,其组分为:耐磨骨料、钛铝酸钙、碳化硅、活性氧化铝粉、锆硅灰、A70水泥、硅溶胶、外加剂。该陶瓷耐磨料耐磨性优异但抗酸能力差,在受到酸性水汽侵蚀时损坏过快,影响设备寿命。The patent application publication number is CN112573909A discloses a ceramic wear-resistant material based on nano-silica sol, and its components are: wear-resistant aggregate, calcium aluminate titanate, silicon carbide, activated alumina powder, zirconium silica fume, A70 Cement, silica sol, admixtures. The ceramic wear-resistant material has excellent wear resistance but poor acid resistance, and it will be damaged too quickly when it is eroded by acidic water vapor, which will affect the life of the equipment.

发明内容Contents of the invention

本发明要解决上述问题,从而提供了一种耐酸浇注料。本发明以回收陶瓷、刚玉、焦宝石作为耐酸骨料,以硅微粉、活性氧化铝粉作为耐酸粉料,以硅溶胶作为结合剂,并在此基础上添加硅酸盐水泥、水以及外加剂。在制备时将各种材料按照粒径大小与各自的物性,配置成两个配方,一个配方以大中粒径材料为主,另一配方以中小粒径材料为主,分别制成不适合单用的两种浇筑料,然后将两种浇注料混合,制成所需的耐酸浇注料;优化了耐酸浇注料的结构,此方法制备的耐酸浇注料结构致密、强度高、耐磨性优异、热稳定性高、抗渗透性好、抗酸性好,可以满足设备内衬的使用条件,从而有效保障设备安全稳定的运行。The present invention aims to solve the above problems, thereby providing an acid-resistant castable. In the present invention, recycled ceramics, corundum, and coke gemstones are used as acid-resistant aggregates, silicon micropowder and activated alumina powder are used as acid-resistant powders, silica sol is used as a binder, and Portland cement, water and additives are added on this basis. . During the preparation, various materials are configured into two formulas according to the particle size and their respective physical properties. One formula is mainly composed of large and medium particle size materials, and the other is mainly composed of medium and small particle size materials. The two kinds of castables used, and then the two castables are mixed to make the required acid-resistant castable; the structure of the acid-resistant castable is optimized, and the acid-resistant castable prepared by this method has a compact structure, high strength, excellent wear resistance, It has high thermal stability, good permeability resistance and good acid resistance, which can meet the use conditions of the equipment lining, thus effectively ensuring the safe and stable operation of the equipment.

本发明解决上述问题的技术方案如下:The technical scheme that the present invention solves the above problems is as follows:

一种耐酸浇注料,包含如下重量份的组分:耐酸骨料45~75份,耐酸粉料15~35份,铝酸盐水泥5~10份,结合剂5~15份,水5~7份,外加剂3.02~6份;An acid-resistant castable, comprising the following components by weight: 45-75 parts of acid-resistant aggregate, 15-35 parts of acid-resistant powder, 5-10 parts of aluminate cement, 5-15 parts of binder, and 5-7 parts of water parts, admixture 3.02~6 parts;

所述耐酸骨料选自回收陶瓷、刚玉、焦宝石中的一种或多种;The acid-resistant aggregate is selected from one or more of recovered ceramics, corundum, and burnt gems;

所述耐酸粉料选自硅微粉、活性氧化铝粉中的一种或多种;The acid-resistant powder is selected from one or more of silicon micropowder and activated alumina powder;

所述结合剂是硅溶胶;The binding agent is silica sol;

所述外加剂包括耐高温纤维、分散剂、促凝剂。The admixture includes high temperature resistant fiber, dispersant and coagulant.

作为优选,所述耐酸骨料包括以下组分:Preferably, the acid-resistant aggregate includes the following components:

粒度3~5mm 25~35份;Particle size 3~5mm 25~35 parts;

粒度1~3mm 10~20 份;Particle size 1~3mm 10~20 parts;

粒度0.1~1mm 10~20份。Particle size 0.1~1mm 10~20 parts.

作为优选,所述耐酸粉料包括以下组分:Preferably, the acid-resistant powder comprises the following components:

硅微粉 10~20份;Silica powder 10~20 parts;

活性氧化铝粉 5~15 份。Activated alumina powder 5~15 parts.

作为优选,所述外加剂包括以下组分:Preferably, the admixture includes the following components:

耐高温纤维 3~5份;3~5 parts of high temperature resistant fiber;

分散剂 0.01~0.5份;Dispersant 0.01~0.5 parts;

促凝剂 0.01~0.5份。Coagulant 0.01~0.5 parts.

作为优选,所述回收陶瓷中氧化铝的含量大于90%。Preferably, the alumina content in the recycled ceramics is greater than 90%.

作为优选,所述刚玉为烧结刚玉。Preferably, the corundum is sintered corundum.

作为优选,所述硅微粉由高硅质废弃料粉末制成。Preferably, the silicon micropowder is made of high-siliceous waste powder.

作为优选,所述硅溶胶的SiO2固含量≥40%。Preferably, the SiO 2 solid content of the silica sol is ≥ 40%.

作为优选,所述分散剂为六偏磷酸钠、三聚磷酸钠、柠檬酸钠中的至少一种。Preferably, the dispersant is at least one of sodium hexametaphosphate, sodium tripolyphosphate and sodium citrate.

作为优选,所述促凝剂为氧化镁、氢氧化镁中的至少一种。Preferably, the coagulant is at least one of magnesium oxide and magnesium hydroxide.

回收陶瓷,主要成分为氧化铝和氧化硅,能够耐酸腐蚀;是高温烧制后的产物,具有优良的耐高温、抗磨损性能。Recycled ceramics, mainly composed of alumina and silicon oxide, can resist acid corrosion; they are products fired at high temperature, and have excellent high temperature resistance and wear resistance.

刚玉,主要成分为氧化铝,能够耐酸腐蚀;熔点高,耐高温;硬度大,抗磨损。Corundum, the main component is alumina, can resist acid corrosion; high melting point, high temperature resistance; high hardness, anti-wear.

焦宝石,具有耐高温、耐腐蚀、抗磨损的特点,能够提高耐酸浇注料的抗酸性、抗磨损性能。Jiaoge, with the characteristics of high temperature resistance, corrosion resistance and wear resistance, can improve the acid resistance and wear resistance of acid-resistant castables.

硅微粉,可以填充材料间的空隙;且因为经过烧制,物相能够保持相对的稳定。Microsilica powder can fill the gaps between materials; and because of firing, the phase can remain relatively stable.

活性氧化铝粉,能够增加浇注料的耐磨、耐高温、耐酸等性能。Activated alumina powder can increase the wear resistance, high temperature resistance, acid resistance and other properties of the castable.

铝酸盐水泥,能够增加浇注料的耐酸性、耐磨性。Aluminate cement can increase the acid resistance and wear resistance of castables.

硅溶胶,作为浇注料结合剂时,硅溶胶主要通过粒子之间的缩合反应(-Si-OH +HO-Si- = -Si-O-Si- + H2O)形成的三维网状结构为浇注料提供初始强度,同时硅溶胶中存在的纳米二氧化硅在热处理时也可与浇注料中的活性成分发生反应来改善浇注料的性能。Silica sol, when used as a castable binder, the three-dimensional network structure formed by the silica sol mainly through the condensation reaction between particles (-Si-OH + HO-Si- = -Si-O-Si- + H 2 O) is The castable provides initial strength, and the nano-silica present in the silica sol can also react with the active components in the castable to improve the performance of the castable during heat treatment.

耐高温纤维,长时间高温下,仍可以维持一般力学性能,用作浇注料的增强材料,可以增强其结构强度。High temperature resistant fibers can still maintain general mechanical properties under high temperature for a long time, and can be used as reinforcing materials for castables to enhance their structural strength.

分散剂,在硅溶胶结合剂中的作用是分散在溶胶粒子周围,通过提高浇注料中基质的Zeta电位,调节胶粒之间的距离,提高溶胶的稳定性,以此来调节浇注料的流动性。Dispersant, the function of the silica sol binder is to disperse around the sol particles, and adjust the flow of the castable by increasing the Zeta potential of the matrix in the castable, adjusting the distance between the colloidal particles, and improving the stability of the sol sex.

促凝剂,可以夺取硅溶胶粒子表面的H+,促进硅溶胶粒子间的硅羟基缩合反应,加快硅氧烷网络的形成,提升浇注料的凝结速度,提高初始强度。Coagulation accelerator can capture H + on the surface of silica sol particles, promote the condensation reaction of silanol groups between silica sol particles, accelerate the formation of siloxane network, increase the coagulation speed of castables, and increase the initial strength.

本发明所述的耐酸浇注料的制备方法,包括以下步骤:The preparation method of acid-resistant castable of the present invention comprises the following steps:

S1、将回收陶瓷、刚玉、焦宝石、硅微粉、活性氧化铝粉、铝酸盐水泥、水、硅溶胶、耐高温纤维、分散剂、促凝剂,在搅拌器内搅拌均匀,得到混合物料1;本步骤中,粒度0.1~5mm的耐酸骨料用量占耐酸骨料总量的75~90%,耐酸粉料用量占耐酸粉料总量的15~25%,铝酸盐水泥用量占铝酸盐水泥总量的80~95%,硅溶胶用量占硅溶胶总量的5~15%,耐高温纤维用量占耐高温纤维总量的70~85%,分散剂用量占分散剂总量的70~85%,促凝剂用量占促凝剂总量的70~85%,水用量占水总量的40~60%;S1. Stir the recycled ceramics, corundum, coke gemstone, silica micropowder, activated alumina powder, aluminate cement, water, silica sol, high temperature resistant fiber, dispersant, and coagulant in the mixer evenly to obtain a mixed material 1; In this step, the amount of acid-resistant aggregate with a particle size of 0.1-5mm accounts for 75-90% of the total amount of acid-resistant aggregate, the amount of acid-resistant powder accounts for 15-25% of the total amount of acid-resistant powder, and the amount of aluminate cement accounts for 10% of the total amount of acid-resistant powder. 80~95% of the total amount of salt cement, the amount of silica sol accounts for 5~15% of the total amount of silica sol, the amount of high temperature resistant fiber accounts for 70~85% of the total amount of high temperature resistant fiber, and the amount of dispersant accounts for 5% of the total amount of dispersant 70~85%, the amount of coagulant accelerator accounts for 70~85% of the total amount of coagulant accelerator, and the amount of water accounts for 40~60% of the total amount of water;

S2、将刚玉、焦宝石、硅微粉、活性氧化铝粉、铝酸盐水泥、水、硅溶胶、耐高温纤维、分散剂、促凝剂,在搅拌器内搅拌均匀,得到混合物料2;本步骤中,耐酸骨料、耐酸粉料、铝酸盐水泥、硅溶胶、耐高温纤维、分散剂、促凝剂、水的用量均为余量;S2. Stir corundum, coke gemstone, silica micropowder, activated alumina powder, aluminate cement, water, silica sol, high temperature resistant fiber, dispersant, and coagulant in a mixer evenly to obtain a mixture 2; In the step, the amount of acid-resistant aggregate, acid-resistant powder, aluminate cement, silica sol, high-temperature-resistant fiber, dispersant, coagulant, and water is the balance;

S3、将混合物料1与混合物料2进一步混合均匀,得到浇注料。S3, further mixing the mixed material 1 and the mixed material 2 evenly to obtain a castable.

作为上述技术方案的优选,步骤S1中,回收陶瓷的粒度为3~5mm,使用量占回收陶瓷总量的95%以上;刚玉的粒度为1~3mm,使用量占刚玉总量的75~85%;焦宝石的粒度为0.1~1mm,使用量占焦宝石总量的45~55%;硅微粉使用量占硅微粉总量的15~25%;活性氧化铝粉使用量占活性氧化铝粉总量的15~25%。As an optimization of the above-mentioned technical solution, in step S1, the particle size of recovered ceramics is 3-5mm, and the usage amount accounts for more than 95% of the total amount of recycled ceramics; the particle size of corundum is 1-3mm, and the usage amount accounts for 75-85% of the total amount of corundum. %; the particle size of coke gemstones is 0.1~1mm, and the usage amount accounts for 45~55% of the total amount of coke gemstones; the usage amount of microsilica powder accounts for 15~25% of the total amount of microsilica powder; the usage amount of activated alumina powder accounts for 15~25% of the total amount.

本发明具有以下的有益效果:The present invention has following beneficial effect:

1、本发明制备的耐酸浇注料结构致密、强度高、耐磨性优异,可以满足设备内衬的使用条件;1. The acid-resistant castable prepared by the present invention has a compact structure, high strength and excellent wear resistance, which can meet the conditions of use for equipment linings;

2、本发明制备的耐酸浇注料热稳定性高,在生产温度改变时也能够与设备贴合;2. The acid-resistant castable prepared by the present invention has high thermal stability and can be bonded to equipment when the production temperature changes;

3、本发明制备的耐酸浇注料吸水率低,抗渗透性好,可以防止设备内衬开裂,延长设备寿命;3. The acid-resistant castable prepared by the present invention has low water absorption and good permeability resistance, which can prevent the equipment lining from cracking and prolong the life of the equipment;

4、本发明制备的耐酸浇注料抗酸性好,可以抵抗酸性气体侵蚀,能够有效保障设备安全稳定的运行。4. The acid-resistant castable prepared by the present invention has good acid resistance, can resist acid gas erosion, and can effectively ensure safe and stable operation of equipment.

具体实施方式Detailed ways

实施例1Example 1

一种耐酸浇注料,按重量份配比称取原料:3~5mm回收陶瓷25份、1~3mm烧结刚玉10份、0.1~1mm焦宝石10份、活性氧化铝粉15份、硅微粉20份、铝酸盐水泥10份、硅溶胶10份、水6份、高温纤维5份、六偏磷酸钠0.06份、氧化镁0.02份。 An acid-resistant castable, the raw materials are weighed according to the weight ratio: 25 parts of 3~5mm recycled ceramics, 10 parts of 1~3mm sintered corundum, 10 parts of 0.1~1mm coke gem, 15 parts of activated alumina powder, 20 parts of silicon micropowder , 10 parts of aluminate cement, 10 parts of silica sol, 6 parts of water, 5 parts of high-temperature fiber, 0.06 part of sodium hexametaphosphate, and 0.02 part of magnesium oxide.

所述耐酸浇注料的制备方法包括以下步骤:The preparation method of described acid-resistant castable comprises the following steps:

S1、取25份3~5mm回收陶瓷、8份1~3mm烧结刚玉、5份0.1~1mm焦宝石、4份硅微粉、3份活性氧化铝粉、9份铝酸盐水泥、3份水、1份硅溶胶、4份耐高温纤维、0.05份六偏磷酸钠、0.015份氧化镁,在搅拌器内搅拌均匀,得到混合物料1;S1. Take 25 parts of 3~5mm recycled ceramics, 8 parts of 1~3mm sintered corundum, 5 parts of 0.1~1mm coke gem, 4 parts of silica powder, 3 parts of activated alumina powder, 9 parts of aluminate cement, 3 parts of water, 1 part of silica sol, 4 parts of high-temperature-resistant fiber, 0.05 part of sodium hexametaphosphate, and 0.015 part of magnesium oxide were stirred evenly in the mixer to obtain the mixed material 1;

S2、取2份1~3mm烧结刚玉、5份0.1~1mm焦宝石、16份硅微粉、12份活性氧化铝粉、1份铝酸盐水泥、3份水、9份硅溶胶、1份耐高温纤维、0.01份六偏磷酸钠、0.005份氧化镁,在搅拌器内搅拌均匀,得到混合物料2;S2. Take 2 parts of 1~3mm sintered corundum, 5 parts of 0.1~1mm coke gem, 16 parts of silicon micropowder, 12 parts of activated alumina powder, 1 part of aluminate cement, 3 parts of water, 9 parts of silica sol, 1 part of resistant High-temperature fiber, 0.01 part of sodium hexametaphosphate, and 0.005 part of magnesium oxide were stirred evenly in a mixer to obtain a mixture 2;

S3、将混合物料1与混合物料2进一步混合均匀,得到浇注料;S3, further mixing the mixed material 1 and the mixed material 2 evenly to obtain a castable;

S4、将所述浇筑料按需要浇注成型。S4. Casting the pouring material as required.

将浇注料倒入160mm×40 mm×40 mm的模具中,振动成型后,常温下养护24 h后,脱模再养护24 h,将浇注料在电炉内进行110℃×24h的烘干处理和1100 ℃×3 h的热处理后,根据 GB/T4513.6-2017进行物理性能测试;根据GB/T 17601-2008进行耐酸性能检测。Pour the castable into a mold of 160 mm × 40 mm × 40 mm. After vibration molding, it is cured at room temperature for 24 h, demolded and cured for another 24 h. The castable is dried in an electric furnace at 110°C × 24 h and After heat treatment at 1100 ℃ for 3 h, the physical performance test was carried out according to GB/T4513.6-2017; the acid resistance test was carried out according to GB/T 17601-2008.

检测结果为:110℃×24h烘干:体积密度1.12g/cm3,抗折强度30.2Mpa,耐压强度170.9Mpa,体积吸水率4.2%;1100℃×3h热处理:线变化-0.07%;耐硫酸侵蚀:质量损失比0.43%。The test results are: 110℃×24h drying: bulk density 1.12g/cm 3 , flexural strength 30.2Mpa, compressive strength 170.9Mpa, volume water absorption 4.2%; 1100℃×3h heat treatment: linear change -0.07%; Sulfuric acid attack: the mass loss ratio is 0.43%.

实施例2Example 2

一种耐酸浇注料,按重量份配比称取原料:3~5mm回收陶瓷30份、1~3mm烧结刚玉15份、0.1~1mm焦宝石15份、活性氧化铝粉10份、硅微粉15份、铝酸盐水泥6份、硅溶胶9份、水6份、高温纤维5份、六偏磷酸钠0.06份、氧化镁0.02份。 An acid-resistant castable, the raw materials are weighed according to the weight ratio: 30 parts of 3~5mm recycled ceramics, 15 parts of 1~3mm sintered corundum, 15 parts of 0.1~1mm coke gem, 10 parts of activated alumina powder, 15 parts of silicon micropowder , 6 parts of aluminate cement, 9 parts of silica sol, 6 parts of water, 5 parts of high-temperature fiber, 0.06 part of sodium hexametaphosphate, and 0.02 part of magnesium oxide.

所述耐酸浇注料的制备方法包括以下步骤:The preparation method of described acid-resistant castable comprises the following steps:

S1、取30份3~5mm回收陶瓷、12份1~3mm烧结刚玉、7.5份0.1~1mm焦宝石、3份硅微粉、2份活性氧化铝粉、5份铝酸盐水泥、3份水、1份硅溶胶、4份耐高温纤维、0.05份六偏磷酸钠、0.015份氧化镁,在搅拌器内搅拌均匀,得到混合物料1;S1. Take 30 parts of 3~5mm recycled ceramics, 12 parts of 1~3mm sintered corundum, 7.5 parts of 0.1~1mm coke gem, 3 parts of silica powder, 2 parts of activated alumina powder, 5 parts of aluminate cement, 3 parts of water, 1 part of silica sol, 4 parts of high-temperature-resistant fiber, 0.05 part of sodium hexametaphosphate, and 0.015 part of magnesium oxide were stirred evenly in the mixer to obtain the mixed material 1;

S2、取3份1~3mm烧结刚玉、7.5份0.1~1mm焦宝石、12份硅微粉、8份活性氧化铝粉、1份铝酸盐水泥、3份水、8份硅溶胶、1份耐高温纤维、0.01份六偏磷酸钠、0.005份氧化镁,在搅拌器内搅拌均匀,得到混合物料2;S2. Take 3 parts of 1~3mm sintered corundum, 7.5 parts of 0.1~1mm coke gem, 12 parts of silicon micropowder, 8 parts of activated alumina powder, 1 part of aluminate cement, 3 parts of water, 8 parts of silica sol, 1 part of resistant High-temperature fiber, 0.01 part of sodium hexametaphosphate, and 0.005 part of magnesium oxide were stirred evenly in a mixer to obtain a mixture 2;

S3、将混合物料1与混合物料2进一步混合均匀,得到浇注料;S3, further mixing the mixed material 1 and the mixed material 2 evenly to obtain a castable;

S4、将所述浇筑料按需要浇注成型。S4. Casting the pouring material as required.

将浇注料倒入 160mm×40 mm×40 mm的模具中,振动成型后,常温下养护24 h后,脱模再养护24 h,将浇注料在电炉内进行110℃×24h的烘干处理和1100 ℃×3 h的热处理后,根据GB/T4513.6-2017,进行物理性能测试;根据GB/T 17601-2008进行耐酸性能检测。Pour the castable into a mold of 160 mm × 40 mm × 40 mm. After vibration molding, it is cured at room temperature for 24 h, demolded and cured for another 24 h. The castable is dried in an electric furnace at 110°C × 24 h and After heat treatment at 1100 ℃ for 3 h, the physical performance test was carried out according to GB/T4513.6-2017; the acid resistance test was carried out according to GB/T 17601-2008.

检测结果为:110℃×24h烘干:体积密度0.95g/cm3,抗折强度34.6Mpa,耐压强度179.8Mpa,体积吸水率3.3%;1100℃×3h热处理:线变化-0.02%;耐硫酸侵蚀:质量损失比0.38%。The test results are: 110℃×24h drying: bulk density 0.95g/cm 3 , flexural strength 34.6Mpa, compressive strength 179.8Mpa, volume water absorption 3.3%; 1100℃×3h heat treatment: linear change -0.02%; Sulfuric acid attack: the mass loss ratio is 0.38%.

实施例3Example 3

一种耐酸浇注料,按重量份配比称取原料:3~5mm回收陶25份、1~3mm烧结刚玉20份、0.1~1mm焦宝石20份、活性氧化铝粉5份、硅微粉10份、铝酸盐水泥10份、硅溶胶10份、水6份、高温纤维5份、六偏磷酸钠0.06份、氧化镁0.02份。 An acid-resistant castable, the raw materials are weighed according to the weight ratio: 25 parts of 3~5mm recycled pottery, 20 parts of 1~3mm sintered corundum, 20 parts of 0.1~1mm coke gem, 5 parts of activated alumina powder, 10 parts of silicon micropowder , 10 parts of aluminate cement, 10 parts of silica sol, 6 parts of water, 5 parts of high-temperature fiber, 0.06 part of sodium hexametaphosphate, and 0.02 part of magnesium oxide.

所述耐酸浇注料的制备方法包括以下步骤:The preparation method of described acid-resistant castable comprises the following steps:

S1、取25份3~5mm回收陶瓷、16份1~3mm烧结刚玉、10份0.1~1mm焦宝石、2份硅微粉、1份活性氧化铝粉、9份铝酸盐水泥、3份水、1份硅溶胶、4份耐高温纤维、0.05份六偏磷酸钠、0.015份氧化镁,在搅拌器内搅拌均匀,得到混合物料1;S1. Take 25 parts of 3~5mm recycled ceramics, 16 parts of 1~3mm sintered corundum, 10 parts of 0.1~1mm coke gem, 2 parts of silica powder, 1 part of activated alumina powder, 9 parts of aluminate cement, 3 parts of water, 1 part of silica sol, 4 parts of high-temperature-resistant fiber, 0.05 part of sodium hexametaphosphate, and 0.015 part of magnesium oxide were stirred evenly in the mixer to obtain the mixed material 1;

S2、取4份1~3mm烧结刚玉、10份0.1~1mm焦宝石、8份硅微粉、4份活性氧化铝粉、1份铝酸盐水泥、3份水、9份硅溶胶、1份耐高温纤维、0.01份六偏磷酸钠、0.005份氧化镁,在搅拌器内搅拌均匀,得到混合物料2;S2. Take 4 parts of 1~3mm sintered corundum, 10 parts of 0.1~1mm coke gem, 8 parts of silicon micropowder, 4 parts of activated alumina powder, 1 part of aluminate cement, 3 parts of water, 9 parts of silica sol, 1 part of resistant High-temperature fiber, 0.01 part of sodium hexametaphosphate, and 0.005 part of magnesium oxide were stirred evenly in a mixer to obtain a mixture 2;

S3、将混合物料1与混合物料2进一步混合均匀,得到浇注料;S3, further mixing the mixed material 1 and the mixed material 2 evenly to obtain a castable;

S4、将所述浇筑料按需要浇注成型。S4. Casting the pouring material as required.

将浇注料倒入 160mm×40 mm×40 mm的模具中,振动成型后,常温下养护24 h后,脱模再养护24 h,将浇注料在电炉内进行110℃×24h的烘干处理和1100 ℃×3 h的热处理后,根据GB/T4513.6-2017,进行物理性能测试;根据GB/T 17601-2008进行耐酸性能检测。Pour the castable into a mold of 160 mm × 40 mm × 40 mm. After vibration molding, it is cured at room temperature for 24 h, demolded and cured for another 24 h. The castable is dried in an electric furnace at 110°C × 24 h and After heat treatment at 1100 ℃ for 3 h, the physical performance test was carried out according to GB/T4513.6-2017; the acid resistance test was carried out according to GB/T 17601-2008.

检测结果为:110℃×24h烘干:体积密度1.09g/cm3,抗折强度32.1Mpa,耐压强度174.2Mpa,体积吸水率3.8%;1100℃×3h热处理:线变化-0.05%;耐硫酸侵蚀:质量损失比0.41%。The test results are: 110℃×24h drying: bulk density 1.09g/cm 3 , flexural strength 32.1Mpa, compressive strength 174.2Mpa, volume water absorption 3.8%; 1100℃×3h heat treatment: linear change -0.05%; Sulfuric acid attack: the mass loss ratio is 0.41%.

对比例1Comparative example 1

一种耐酸浇注料,按重量份配比称取原料:3~5mm回收陶瓷30份、1~3mm烧结刚玉15份、0.1~1mm焦宝石15份、活性氧化铝粉10份、硅微粉15份、铝酸盐水泥6份、硅溶胶9份、水6份、高温纤维5份、六偏磷酸钠0.06份、氧化镁0.02份。 An acid-resistant castable, the raw materials are weighed according to the weight ratio: 30 parts of 3~5mm recycled ceramics, 15 parts of 1~3mm sintered corundum, 15 parts of 0.1~1mm coke gem, 10 parts of activated alumina powder, 15 parts of silicon micropowder , 6 parts of aluminate cement, 9 parts of silica sol, 6 parts of water, 5 parts of high-temperature fiber, 0.06 part of sodium hexametaphosphate, and 0.02 part of magnesium oxide.

所述耐酸浇注料的制备方法包括以下步骤:The preparation method of described acid-resistant castable comprises the following steps:

S1、取30份3~5mm回收陶瓷、15份1~3mm烧结刚玉、15份0.1~1mm焦宝石、5份铝酸盐水泥、3份水、1份硅溶胶、4份耐高温纤维、0.05份六偏磷酸钠、0.015份氧化镁,在搅拌器内搅拌均匀,得到混合物料1;S1. Take 30 parts of 3~5mm recycled ceramics, 15 parts of 1~3mm sintered corundum, 15 parts of 0.1~1mm coke gem, 5 parts of aluminate cement, 3 parts of water, 1 part of silica sol, 4 parts of high temperature resistant fiber, 0.05 1 part of sodium hexametaphosphate, 0.015 part of magnesium oxide, stirred uniformly in a mixer to obtain the mixed material 1;

S2、取15份硅微粉、10份活性氧化铝粉、1份铝酸盐水泥、3份水、8份硅溶胶、1份耐高温纤维、0.01份六偏磷酸钠、0.005份氧化镁,在搅拌器内搅拌均匀,得到混合物料2;S2, get 15 parts of silica powder, 10 parts of activated alumina powder, 1 part of aluminate cement, 3 parts of water, 8 parts of silica sol, 1 part of high temperature resistant fiber, 0.01 part of sodium hexametaphosphate, 0.005 part of magnesium oxide, in Stir evenly in the mixer to obtain the mixed material 2;

S3、将混合物料1与混合物料2进一步混合均匀,得到浇注料;S3, further mixing the mixed material 1 and the mixed material 2 evenly to obtain a castable;

S4、将所述浇筑料按需要浇注成型。S4. Casting the pouring material as required.

将浇注料倒入160mm×40 mm×40 mm的模具中,振动成型后,常温下养护24 h后,脱模再养护24 h,将浇注料在电炉内进行110℃×24h的烘干处理和1100 ℃×3 h的热处理后,根据GB/T4513.6-2017,进行物理性能测试;根据GB/T 17601-2008进行耐酸性能检测。Pour the castable into a mold of 160 mm × 40 mm × 40 mm. After vibration molding, it is cured at room temperature for 24 h, demolded and cured for another 24 h. The castable is dried in an electric furnace at 110°C × 24 h and After heat treatment at 1100 ℃ for 3 h, the physical performance test was carried out according to GB/T4513.6-2017; the acid resistance test was carried out according to GB/T 17601-2008.

检测结果为:110℃×24h烘干:体积密度1.23g/cm3,抗折强度26.8Mpa,耐压强度162.2Mpa,体积吸水率4.5%;1100℃×3h热处理:线变化-0.10%;耐硫酸侵蚀:质量损失比0.54%。The test results are: 110℃×24h drying: bulk density 1.23g/cm 3 , flexural strength 26.8Mpa, compressive strength 162.2Mpa, volume water absorption 4.5%; 1100℃×3h heat treatment: linear change -0.10%; Sulfuric acid attack: the mass loss ratio is 0.54%.

对比例2Comparative example 2

一种耐酸浇注料,按重量份配比称取原料:3~5mm回收陶瓷30份、1~3mm烧结刚玉15份、0.1~1mm焦宝石15份、活性氧化铝粉10份、硅微粉15份、铝酸盐水泥6份、硅溶胶9份、水6份、高温纤维5份、六偏磷酸钠0.06份、氧化镁0.02份。 An acid-resistant castable, the raw materials are weighed according to the weight ratio: 30 parts of 3~5mm recycled ceramics, 15 parts of 1~3mm sintered corundum, 15 parts of 0.1~1mm coke gem, 10 parts of activated alumina powder, 15 parts of silicon micropowder , 6 parts of aluminate cement, 9 parts of silica sol, 6 parts of water, 5 parts of high-temperature fiber, 0.06 part of sodium hexametaphosphate, and 0.02 part of magnesium oxide.

所述耐酸浇注料的制备方法包括以下步骤:The preparation method of described acid-resistant castable comprises the following steps:

S1、取30份3~5mm回收陶瓷、15份1~3mm烧结刚玉、15份0.1~1mm焦宝石、取15份硅微粉、10份活性氧化铝粉、6份铝酸盐水泥、5份耐高温纤维、0.06份六偏磷酸钠、0.02份氧化镁,在搅拌器内搅拌均匀,得到混合物料1;S1. Take 30 parts of 3~5mm recycled ceramics, 15 parts of 1~3mm sintered corundum, 15 parts of 0.1~1mm burnt gemstones, 15 parts of silicon micropowder, 10 parts of activated alumina powder, 6 parts of aluminate cement, 5 parts of High-temperature fiber, 0.06 part of sodium hexametaphosphate, and 0.02 part of magnesium oxide were stirred evenly in the mixer to obtain the mixed material 1;

S2、向所述混合物料1中加入由6份水、9份硅溶胶组成的混合物料2,混合均匀,得到浇注料;S2. Add the mixed material 2 consisting of 6 parts of water and 9 parts of silica sol to the mixed material 1, and mix evenly to obtain a castable;

S3、将所述浇筑料按需要浇注成型。S3. Casting the pouring material as required.

将浇注料倒入160mm×40 mm×40 mm的模具中,振动成型后,常温下养护24 h后,脱模再养护24 h,将浇注料在电炉内进行110℃×24h的烘干处理和1100 ℃×3 h的热处理后,根据 GB/T4513.6-2017,进行物理性能测试;根据GB/T 17601-2008进行耐酸性能检测。Pour the castable into a mold of 160 mm × 40 mm × 40 mm. After vibration molding, it is cured at room temperature for 24 h, demolded and cured for another 24 h. The castable is dried in an electric furnace at 110°C × 24 h and After heat treatment at 1100 ℃ for 3 h, the physical performance test was carried out according to GB/T4513.6-2017; the acid resistance test was carried out according to GB/T 17601-2008.

检测结果为:110℃×24h烘干:体积密度1.35g/cm3,抗折强度23.4Mpa,耐压强度154.5Mpa,体积吸水率4.6%;1100℃×3h热处理:线变化-0.14%;耐硫酸侵蚀:质量损失比0.68%。The test results are: 110℃×24h drying: bulk density 1.35g/cm 3 , flexural strength 23.4Mpa, compressive strength 154.5Mpa, volume water absorption 4.6%; 1100℃×3h heat treatment: linear change -0.14%; Sulfuric acid attack: the mass loss ratio is 0.68%.

表1:实施例1~3与对比例1~2的部分组分对比表Table 1: Partial component comparison table of embodiments 1~3 and comparative examples 1~2

表2:实施例1~3与对比例1~2的性能对比表Table 2: Performance comparison table of Examples 1~3 and Comparative Examples 1~2

从表2可以看出,经110℃×24h烘干处理后,实施例1~3的体积密度、抗折强度、耐压强度均好于对比例1~2,说明实施例1~3的强度、耐磨性优于对比例1~2。It can be seen from Table 2 that after drying at 110°C×24h, the bulk density, flexural strength, and compressive strength of Examples 1-3 are all better than those of Comparative Examples 1-2, indicating that the strength of Examples 1-3 is , Abrasion resistance is better than Comparative Examples 1~2.

从表2可以看出,经110℃×24h烘干处理后,实施例1~3的体积吸水率低于对比例1~2浇注料,说明实施例1~3的抗渗透性、致密性好于对比例1~2。It can be seen from Table 2 that after drying at 110℃×24h, the volume water absorption rate of Examples 1~3 is lower than that of Comparative Examples 1~2 castables, indicating that Examples 1~3 have good permeability resistance and compactness In comparative example 1~2.

从表2可以看出,经1100℃×3h热处理后,实施例1~3的线变化均好于对比例1~2,说明实施例1~3的热稳定性优于对比例1~2。It can be seen from Table 2 that after heat treatment at 1100°C × 3h, the linear changes of Examples 1-3 are better than those of Comparative Examples 1-2, indicating that the thermal stability of Examples 1-3 is better than that of Comparative Examples 1-2.

从表2可以看出,实施例1~3抗酸性好于对比例1~2。As can be seen from Table 2, the acid resistance of Examples 1-3 is better than that of Comparative Examples 1-2.

从表2可以看出,实施例2的强度、耐磨性、抗渗透性、致密性、热稳定性、抗酸性均是最好的。It can be seen from Table 2 that the strength, wear resistance, penetration resistance, compactness, thermal stability and acid resistance of Example 2 are all the best.

相较于对比例1采用的将大粒径材料与小粒径材料分别混匀后再制成浇注料的制备方法,和对比例2采用的将所有固体原料混匀后再加湿料的制备方法,本发明将各种材料按照粒径大小与各自的物性,配置成两个配方,一个配方以大中粒径材料为主,另一配方以中小粒径材料为主,分别制成不适合单用的两种浇筑料,然后将两种浇注料混合,制成所需的耐酸浇注料;优化了耐酸浇注料的结构,使结构更加致密,使耐酸浇注料的性能得到了提升。Compared with the preparation method of mixing large particle size materials and small particle size materials separately and then making castables in Comparative Example 1, and the preparation method of mixing all solid raw materials before adding wet materials in Comparative Example 2 In the present invention, various materials are configured into two formulas according to the particle size and their respective physical properties. One formula is mainly composed of large and medium particle size materials, and the other is mainly composed of medium and small particle size materials. The two kinds of castables are used, and then the two kinds of castables are mixed to make the required acid-resistant castable; the structure of the acid-resistant castable is optimized to make the structure more compact, and the performance of the acid-resistant castable is improved.

结合以上对比数据,本发明制备的耐酸浇注料结构致密、强度高、耐磨性优异、抗渗透性好、热稳定性高、抗酸性好,这些优点能够很好的满足设备内衬的使用条件,可以有效保障设备安全稳定的运行,有助于取得良好的经济效益和社会效益。Combined with the above comparative data, the acid-resistant castable prepared by the present invention has a compact structure, high strength, excellent wear resistance, good permeability resistance, high thermal stability, and good acid resistance. These advantages can well meet the use conditions of equipment linings , can effectively guarantee the safe and stable operation of the equipment, and help to achieve good economic and social benefits.

Claims (10)

1. An acid-resistant castable is characterized in that: comprises the following components in parts by weight: 45-75 parts of acid-resistant aggregate, 15-35 parts of acid-resistant powder, 5-10 parts of aluminate cement, 5-15 parts of binding agent, 5-7 parts of water and 3.02-6 parts of additive;
the acid-resistant aggregate is selected from one or more of recycled ceramics, corundum and flint clay;
the acid-resistant powder is one or more selected from silicon micropowder and activated alumina powder;
the binding agent is silica sol;
the additive comprises high temperature resistant fiber, dispersing agent and coagulant.
2. An acid resistant castable according to claim 1, wherein: the acid-resistant aggregate comprises the following components:
25-35 parts of granularity of 3-5 mm;
10-20 parts of particles with the granularity of 1-3 mm;
10-20 parts of particles with the granularity of 0.1-1 mm.
3. An acid resistant castable according to claim 1, wherein: the acid-resistant powder comprises the following components:
10-20 parts of silicon micropowder;
5-15 parts of active alumina powder.
4. An acid resistant castable according to claim 1, wherein: the additive comprises the following components:
3-5 parts of high-temperature resistant fibers;
0.01-0.5 parts of dispersing agent;
0.01-0.5 parts of coagulant.
5. An acid resistant castable according to claim 1, wherein: the content of alumina in the reclaimed ceramic is more than 90%; the corundum is sintered corundum; the silicon micropowder is made from high-siliceous waste powder.
6. An acid resistant castable according to claim 1, wherein: siO of the silica sol 2 The solid content is more than or equal to 40 percent.
7. An acid resistant castable according to claim 1, wherein: the dispersing agent is at least one of sodium hexametaphosphate, sodium tripolyphosphate and sodium citrate.
8. An acid resistant castable according to claim 1, wherein: the coagulant is at least one of magnesium oxide and magnesium hydroxide.
9. The method for preparing the acid-resistant castable according to any one of claims 1 to 8, wherein the method is characterized by comprising the following steps: the method comprises the following steps:
s1, uniformly stirring recycled ceramics, corundum, flint clay, silica micropowder, activated alumina powder, aluminate cement, water, silica sol, high-temperature resistant fibers, a dispersing agent and a coagulant in a stirrer to obtain a mixed material 1; in the step, the acid-resistant aggregate with the granularity of 0.1-5 mm accounts for 75-90% of the total acid-resistant aggregate, the acid-resistant powder accounts for 15-25% of the total acid-resistant powder, the aluminate cement accounts for 80-95% of the total aluminate cement, the silica sol accounts for 5-15% of the total silica sol, the high-temperature resistant fiber accounts for 70-85% of the total high-temperature resistant fiber, the dispersant accounts for 70-85% of the dispersant, the coagulant accounts for 70-85% of the total coagulant, and the water accounts for 40-60% of the total water;
s2, uniformly stirring corundum, flint clay, silica micropowder, activated alumina powder, aluminate cement, water, silica sol, high-temperature resistant fiber, dispersing agent and coagulant in a stirrer to obtain a mixed material 2; in the step, the dosages of acid-resistant aggregate, acid-resistant powder, aluminate cement, silica sol, high-temperature resistant fiber, dispersing agent, coagulant and water are the rest;
and S3, further uniformly mixing the mixed material 1 and the mixed material 2 to obtain the castable.
10. The method for preparing the acid-resistant castable according to claim 9, wherein: in the step S1, the granularity of the recovered ceramic is 3-5 mm, and the usage amount of the recovered ceramic is more than 95% of the total amount of the recovered ceramic; the granularity of the corundum is 1-3 mm, and the usage amount of the corundum accounts for 75-85% of the total amount of the corundum; the granularity of the flint clay is 0.1-1 mm, and the usage amount of the flint clay accounts for 45-55% of the total amount of the flint clay; the usage amount of the silicon micro powder is 15-25% of the total amount of the silicon micro powder; the usage amount of the activated alumina powder is 15-25% of the total amount of the activated alumina powder.
CN202310538855.9A 2023-05-15 2023-05-15 Acid-resistant castable and preparation method thereof Pending CN116589289A (en)

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