微波硬化水玻璃砂应用的关键技术基础
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摘要
微波加热硬化水玻璃砂可充分发挥水玻璃的粘结效率，具有水玻璃加入量低、强度高、硬化时间短、旧砂溃散及再生回用性好、清洁生产等一系列优势。本文针对微波硬化水玻璃砂应用的关键问题开展了如下研究：
1、试验研究了普通微波硬化水玻璃砂的加热特征、强度特征和存放特征，分析了加热时间和功率、水玻璃加入量、水玻璃模数、存放时间和存放环境等对砂型强度的影响，研究了砂型抗湿性差、强度快速下降的原因，并通过测试微波加热作用下型砂试样的温度场分布，探索了微波加热硬化水玻璃砂的传热特征。
2、针对造型模具要求高的问题，开展了四种少模或无模硬化新工艺的系统研究：
（1）研究了二次微波硬化水玻璃砂新工艺的特征及其影响因素。结果表明，10-30s微波初次硬化可达到15KPa的脱模强度，90-100s的二次无模具直接微波硬化能达到可使用强度，该工艺具有模具要求低、直接加热、硬化效率高等优点。
（2）研究了有机酯―微波复合硬化水玻璃砂工艺。测试了有机酯加入量、加热时间、微波功率等对砂型强度和抗湿性的影响。该工艺能提高砂型的抗湿性能，硬化过程中生成的三水醋酸钠晶体和甘油、高模数水玻璃等疏水性物质保护了粘结桥。
（3）研究了CO_2―微波复合硬化水玻璃砂工艺。测试了CO_2吹气流量、吹气时间、微波硬化时间、微波功率等对砂型强度和抗湿性的影响。发现该工艺能提高砂型的抗吸湿性能，硬化产生的十水碳酸钠和高模数水玻璃保护了粘结桥。
（4）研究了热空气―微波复合硬化水玻璃砂工艺。测试结果表明，该工艺硬化时间较慢，砂型的抗湿性较差，需要热空气保温设备。
3、结合水玻璃本身的特征（富含硅原子或者硅氧键、本身即为表面活性剂），开展了微波硬化水玻璃砂的抗吸湿性材料及其方法的研究；开发了三类水玻璃砂抗吸湿涂料（层）。
（1）对粘结剂或原砂进行改性以提高型砂的抗吸湿性。采用纳米氮化硅、纳米碳化硅、纳米绢云母等无机硅质粉末改性水玻璃；甲基硅酸钠、甲基硅油的液体有机硅及烷基苯磺酸钠、Span-80等表面活性剂改性原砂，添加了改性剂的砂型恒湿瓶4h存放强度较未改性砂型大都能提高90%左右。
（2）开发了以PbO-ZnO低温陶瓷粉为骨料的醇基涂料来改善砂型的抗湿性，点火烧结后，生成了Al_2TiO_5、NaAlO_2、PbTiO_3等物质，涂覆了涂料的水玻璃砂样恒湿瓶4h存放强度较普通砂样提高了将近2.33倍。
（3）研究了在水玻璃砂型表面生成低共熔体锂盐涂层的方法，来提高砂型的抗湿性。首先在水玻璃砂型表面喷涂0.38LiOH-0.62LiNO_3混合锂盐（共熔点温度最低只有175.7℃）饱和水溶液，再将砂型放入微波炉加热硬化制得表面有致密混合锂盐涂层的水玻璃砂型。砂型硬化温度高达370℃，远高于普通微波硬化砂型（110℃），表面涂层处理的砂型恒湿瓶4h存放强度较未处理的提高了将近2倍。
（4）以PbO-ZnO系低温陶瓷粉为骨料，再加入3.5%V2O_5、2.5%Al_2O_3、2.5%TiO_2及20%的0.38LiOH-0.62LiNO_3混合锂盐而制备了低温涂料，在微波烧结和硬化作用下，表面具有低温涂料的砂样在恒湿瓶中存放4h的强度较未处理提高6倍多，砂型被Zn_2TiO_4、Pb_5O_8、PbTiO_3、PbSiO_3、Pb_6Al_2Si6O_21和Al_2SiO_5等无机物质的致密熔体包裹。该涂层开始烧结温度仅为259.6℃，砂型的硬化温度高达390℃。
4、针对目前水玻璃砂工艺应用仍未很好解决的旧砂再生问题，提出了生物再生水玻璃旧砂新方法，初步研究了水玻璃旧砂生物再生的可行性及其影响因素。
对比了谷皮菱形藻、直链藻和小环藻再生水玻璃旧砂污水的效果，结果表明谷皮菱形藻的效果最好。利用水玻璃旧砂湿法再生污水培养经过耐碱驯化的谷皮菱形藻，确定了回收效率的各种影响条件的单因素最佳值：温度25℃，光强5000lux，光照时间14h/d，氮浓度80mg/L，磷浓度50mg/L，氮磷比14:1，Fe3+浓度2.28mg/L，Mg2+浓度16mg/L。对部分影响因子进行了优化，并对污水循环问题也进行了研究。
Sodium silicate sand cured with microwave can exert adequately the bondingpotential of binder and so the sand mould with low binder addition would achieve higherstrength and better collapsibility. Beside these, microwave curing possesses manyadvantages such as fast curing, clean production, and so on.The dissertation had carriedout in order to solve the key problems of this microwave curing process.
(1). The heating, strength and storage characteristics of the traditional microwavecuring process for sodium silicate sand were investigated, and the curing time, microwavepower, binder addition and modulus, storage time and circumstance would influence thesand mould strength. Especially, the mechanism of humidity absorption of sodium silicatesand cured with microwave was analyzed.The temperature field distribution of standardcylindrical sand specimen was studied, and the results showed that there was a positivetemperature gradient from inside to outside within the samples of sodium silicate sandsamples cured with microwave. Furthermore, heat transfer formula was deduced.
(2). Four less-using mould, even non-mould moulding processing were developed tosolve the problem of high-performance mould in the microwave oven, that was the firstcuring for demoulding and the second microwave curing for service strength.
1).Twice microwave curing processing: The sodium silicate sand specimens werecured in microwave oven for10-30s to the stripping strength of15KPa, and then the sandand mould were taken out from microwave oven, and the sand specimens were demoulded,after which the sand specimens were cured for90-100s in the microwave oven to the sandservice strength, and this processing could greatly decrease the requirements on the mouldmaterial and increase the efficiency of curing.
2).Ester―microwave composite curing: The sodium silicate sand specimens werecured by ester fistly for demoulding. A system research of influence factors, included esteraddition, curing time and power, on the strength and moisture resistance properties of thisnew process were investigated. The humidity resistance of the sodium silicate sand wasimproved after the production of hydrophobic materials, glycerol and sodium acetatetrihydrate and high-modulus sodium silicate from the ester curing process.
3).CO_2―microwave composite curing: The sodium silicate sand specimens werecured by CO_2fistly.The influence factors, included CO_2gassing flow and time, curingtime and power, on the strength and moisture resistance properties of this new processwere investigated. The humidity resistance of the sodium silicate sand was improved afterthe production of hydrophobic materials, sodium carbonate decahydrate and high-modulussodium silicate from the CO_2curing process.
4).Hot air―microwave composite curing: The sodium silicate sand specimens werecured by hot air fistly.But the demoulding time was longer and humidity resistance wasworse, and the thermal insulating equipment was complex.
(3).The new modifiers and three coatings were developed to solve the high moistureabsorbability of sodium silicate sand cured with microwave.
1).Many modifiers, such as nano Si3N4, SiC, sericite and methyl sodium silicate,methyl silicone oil and sodium dodecyl sulphate, span-80, were used to improve humidityresistance. The results show that: the4h storage strength in humidistat with0.2%nanoSi3N4increased about93.7%in which the modifier was the minimum, and the modifiedsodium silicate sand with15%methyl silicone oil increased about129.52%in which themodified effect was the best.
2).The alcohol-based coating made of PbO-ZnO low-temperature ceramic powder(aggregate) was fired to form coating in the sodium silicate sand. The results show thathumidity resistance of the sodium silicate sand had significantly greater improvement aftersurface coating, the4hour storage strength can be increased by2.33times. And three newkinds of phase were produced: Al_2TiO_5, NaAlO_2, and PbTiO_3, which were the mainreasons for humidity resistance of sodium silicate sand increased by surface coating.
3).The coating of eutectic lithium salts (0.38LiOH-0.62LiNO_3) were sprayed on thesurface of water glass sand and then sintered by the microwave energy to obtain glassymembrane for its lowest eutectic point of175.7℃，so the humidity resistance of waterglass sand cured with microwave was improved greatly. The results showed that the curingtemperature of coating sand mould was about370℃，which was higher than thetemperature (110℃) of common one by the microwave energy，and the strength of coatingsand mould was higher than common one. The4h storage strength of coating sand mould in humidistat with relative humidity of98-100%increased by two times comparing withthe common microwave curing one.
4).The microwave low-temperature coating, which was made of PbO-ZnO ceramicpowder,3.5%V2O_5,2.5%Al_2O_3,2.5%TiO_2,20%0.38LiOH-0.62LiNO_3eutectic lithiumsalts could produce Zn_2TiO_4, Pb_5O_8, PbTiO_3, PbSiO_3, Pb_6Al_2Si6O_21and Al_2SiO_5in thesurface of the sodium silicate sand mould cured with microwave, and the coatingbeginning sintering temperature was259.6℃, but the curing temperature was390℃. The4h storage strength of coating sand mould in humidistat with relative humidity of98-100%increased by six times comparing with the common microwave curing one.
4. A new process of wet reclamation by biologically treating the waste waterproduced during the wet reclamation process of used sand was studied in this dissertation.Comparing three diatom species of Melosira varians, Cyclotella hebeiana and Nitzschiapalae (for short N. palea below), and N. palea was seleted as the optimum diatom to treatthe waste water. So the domestication was used in the N. palea and many influence factorson the reclaimation were investigated as following: temperature25℃, irradiance5000lux,illumination time14h/d, N concentration80mg/L, P concentration50mg/L, N: P14:1,Fe3+concentration2.28mg/L, Mg2+concentration16mg/L, thus a optimized research wasdone to get the best reclamation effect on basis of these data.And the waste water cyclemethod was tested.
1、试验研究了普通微波硬化水玻璃砂的加热特征、强度特征和存放特征，分析了加热时间和功率、水玻璃加入量、水玻璃模数、存放时间和存放环境等对砂型强度的影响，研究了砂型抗湿性差、强度快速下降的原因，并通过测试微波加热作用下型砂试样的温度场分布，探索了微波加热硬化水玻璃砂的传热特征。
2、针对造型模具要求高的问题，开展了四种少模或无模硬化新工艺的系统研究：
（1）研究了二次微波硬化水玻璃砂新工艺的特征及其影响因素。结果表明，10-30s微波初次硬化可达到15KPa的脱模强度，90-100s的二次无模具直接微波硬化能达到可使用强度，该工艺具有模具要求低、直接加热、硬化效率高等优点。
（2）研究了有机酯―微波复合硬化水玻璃砂工艺。测试了有机酯加入量、加热时间、微波功率等对砂型强度和抗湿性的影响。该工艺能提高砂型的抗湿性能，硬化过程中生成的三水醋酸钠晶体和甘油、高模数水玻璃等疏水性物质保护了粘结桥。
（3）研究了CO_2―微波复合硬化水玻璃砂工艺。测试了CO_2吹气流量、吹气时间、微波硬化时间、微波功率等对砂型强度和抗湿性的影响。发现该工艺能提高砂型的抗吸湿性能，硬化产生的十水碳酸钠和高模数水玻璃保护了粘结桥。
（4）研究了热空气―微波复合硬化水玻璃砂工艺。测试结果表明，该工艺硬化时间较慢，砂型的抗湿性较差，需要热空气保温设备。
3、结合水玻璃本身的特征（富含硅原子或者硅氧键、本身即为表面活性剂），开展了微波硬化水玻璃砂的抗吸湿性材料及其方法的研究；开发了三类水玻璃砂抗吸湿涂料（层）。
（1）对粘结剂或原砂进行改性以提高型砂的抗吸湿性。采用纳米氮化硅、纳米碳化硅、纳米绢云母等无机硅质粉末改性水玻璃；甲基硅酸钠、甲基硅油的液体有机硅及烷基苯磺酸钠、Span-80等表面活性剂改性原砂，添加了改性剂的砂型恒湿瓶4h存放强度较未改性砂型大都能提高90%左右。
（2）开发了以PbO-ZnO低温陶瓷粉为骨料的醇基涂料来改善砂型的抗湿性，点火烧结后，生成了Al_2TiO_5、NaAlO_2、PbTiO_3等物质，涂覆了涂料的水玻璃砂样恒湿瓶4h存放强度较普通砂样提高了将近2.33倍。
（3）研究了在水玻璃砂型表面生成低共熔体锂盐涂层的方法，来提高砂型的抗湿性。首先在水玻璃砂型表面喷涂0.38LiOH-0.62LiNO_3混合锂盐（共熔点温度最低只有175.7℃）饱和水溶液，再将砂型放入微波炉加热硬化制得表面有致密混合锂盐涂层的水玻璃砂型。砂型硬化温度高达370℃，远高于普通微波硬化砂型（110℃），表面涂层处理的砂型恒湿瓶4h存放强度较未处理的提高了将近2倍。
（4）以PbO-ZnO系低温陶瓷粉为骨料，再加入3.5%V2O_5、2.5%Al_2O_3、2.5%TiO_2及20%的0.38LiOH-0.62LiNO_3混合锂盐而制备了低温涂料，在微波烧结和硬化作用下，表面具有低温涂料的砂样在恒湿瓶中存放4h的强度较未处理提高6倍多，砂型被Zn_2TiO_4、Pb_5O_8、PbTiO_3、PbSiO_3、Pb_6Al_2Si6O_21和Al_2SiO_5等无机物质的致密熔体包裹。该涂层开始烧结温度仅为259.6℃，砂型的硬化温度高达390℃。
4、针对目前水玻璃砂工艺应用仍未很好解决的旧砂再生问题，提出了生物再生水玻璃旧砂新方法，初步研究了水玻璃旧砂生物再生的可行性及其影响因素。
对比了谷皮菱形藻、直链藻和小环藻再生水玻璃旧砂污水的效果，结果表明谷皮菱形藻的效果最好。利用水玻璃旧砂湿法再生污水培养经过耐碱驯化的谷皮菱形藻，确定了回收效率的各种影响条件的单因素最佳值：温度25℃，光强5000lux，光照时间14h/d，氮浓度80mg/L，磷浓度50mg/L，氮磷比14:1，Fe3+浓度2.28mg/L，Mg2+浓度16mg/L。对部分影响因子进行了优化，并对污水循环问题也进行了研究。
Sodium silicate sand cured with microwave can exert adequately the bondingpotential of binder and so the sand mould with low binder addition would achieve higherstrength and better collapsibility. Beside these, microwave curing possesses manyadvantages such as fast curing, clean production, and so on.The dissertation had carriedout in order to solve the key problems of this microwave curing process.
(1). The heating, strength and storage characteristics of the traditional microwavecuring process for sodium silicate sand were investigated, and the curing time, microwavepower, binder addition and modulus, storage time and circumstance would influence thesand mould strength. Especially, the mechanism of humidity absorption of sodium silicatesand cured with microwave was analyzed.The temperature field distribution of standardcylindrical sand specimen was studied, and the results showed that there was a positivetemperature gradient from inside to outside within the samples of sodium silicate sandsamples cured with microwave. Furthermore, heat transfer formula was deduced.
(2). Four less-using mould, even non-mould moulding processing were developed tosolve the problem of high-performance mould in the microwave oven, that was the firstcuring for demoulding and the second microwave curing for service strength.
1).Twice microwave curing processing: The sodium silicate sand specimens werecured in microwave oven for10-30s to the stripping strength of15KPa, and then the sandand mould were taken out from microwave oven, and the sand specimens were demoulded,after which the sand specimens were cured for90-100s in the microwave oven to the sandservice strength, and this processing could greatly decrease the requirements on the mouldmaterial and increase the efficiency of curing.
2).Ester―microwave composite curing: The sodium silicate sand specimens werecured by ester fistly for demoulding. A system research of influence factors, included esteraddition, curing time and power, on the strength and moisture resistance properties of thisnew process were investigated. The humidity resistance of the sodium silicate sand wasimproved after the production of hydrophobic materials, glycerol and sodium acetatetrihydrate and high-modulus sodium silicate from the ester curing process.
3).CO_2―microwave composite curing: The sodium silicate sand specimens werecured by CO_2fistly.The influence factors, included CO_2gassing flow and time, curingtime and power, on the strength and moisture resistance properties of this new processwere investigated. The humidity resistance of the sodium silicate sand was improved afterthe production of hydrophobic materials, sodium carbonate decahydrate and high-modulussodium silicate from the CO_2curing process.
4).Hot air―microwave composite curing: The sodium silicate sand specimens werecured by hot air fistly.But the demoulding time was longer and humidity resistance wasworse, and the thermal insulating equipment was complex.
(3).The new modifiers and three coatings were developed to solve the high moistureabsorbability of sodium silicate sand cured with microwave.
1).Many modifiers, such as nano Si3N4, SiC, sericite and methyl sodium silicate,methyl silicone oil and sodium dodecyl sulphate, span-80, were used to improve humidityresistance. The results show that: the4h storage strength in humidistat with0.2%nanoSi3N4increased about93.7%in which the modifier was the minimum, and the modifiedsodium silicate sand with15%methyl silicone oil increased about129.52%in which themodified effect was the best.
2).The alcohol-based coating made of PbO-ZnO low-temperature ceramic powder(aggregate) was fired to form coating in the sodium silicate sand. The results show thathumidity resistance of the sodium silicate sand had significantly greater improvement aftersurface coating, the4hour storage strength can be increased by2.33times. And three newkinds of phase were produced: Al_2TiO_5, NaAlO_2, and PbTiO_3, which were the mainreasons for humidity resistance of sodium silicate sand increased by surface coating.
3).The coating of eutectic lithium salts (0.38LiOH-0.62LiNO_3) were sprayed on thesurface of water glass sand and then sintered by the microwave energy to obtain glassymembrane for its lowest eutectic point of175.7℃，so the humidity resistance of waterglass sand cured with microwave was improved greatly. The results showed that the curingtemperature of coating sand mould was about370℃，which was higher than thetemperature (110℃) of common one by the microwave energy，and the strength of coatingsand mould was higher than common one. The4h storage strength of coating sand mould in humidistat with relative humidity of98-100%increased by two times comparing withthe common microwave curing one.
4).The microwave low-temperature coating, which was made of PbO-ZnO ceramicpowder,3.5%V2O_5,2.5%Al_2O_3,2.5%TiO_2,20%0.38LiOH-0.62LiNO_3eutectic lithiumsalts could produce Zn_2TiO_4, Pb_5O_8, PbTiO_3, PbSiO_3, Pb_6Al_2Si6O_21and Al_2SiO_5in thesurface of the sodium silicate sand mould cured with microwave, and the coatingbeginning sintering temperature was259.6℃, but the curing temperature was390℃. The4h storage strength of coating sand mould in humidistat with relative humidity of98-100%increased by six times comparing with the common microwave curing one.
4. A new process of wet reclamation by biologically treating the waste waterproduced during the wet reclamation process of used sand was studied in this dissertation.Comparing three diatom species of Melosira varians, Cyclotella hebeiana and Nitzschiapalae (for short N. palea below), and N. palea was seleted as the optimum diatom to treatthe waste water. So the domestication was used in the N. palea and many influence factorson the reclaimation were investigated as following: temperature25℃, irradiance5000lux,illumination time14h/d, N concentration80mg/L, P concentration50mg/L, N: P14:1,Fe3+concentration2.28mg/L, Mg2+concentration16mg/L, thus a optimized research wasdone to get the best reclamation effect on basis of these data.And the waste water cyclemethod was tested.
引文
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