CN1039219C - 一种雾化法生产水合硅酸的方法 - Google Patents
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Abstract
一种雾化法生产水合硅酸的方法,系用芒硝为原料联产硅酸钠和水合硅酸的无机化工生产工艺方法,该工艺方法是一种以生产与三废治理相结合的联产方法,该工艺是在生产过程中将回收的SO2制成的硫酸与液体硅酸钠在雾化反应器中进行喷雾反应生产精细水合硅酸,生产中所排放的废水经过真空浓缩、干燥、生成无水芒硝并用作生产硅酸钠的原料补充。该工艺方法设计新颖、产品精细质量高,废水、废气得以回收利用,值得推广普及。
Description
本发明的一种雾化法生产水合硅酸的方法属一种综合利用的无机化工联产工艺。
硅酸钠的传统生产方法是纯碱法。经检索尚未见到用芒硝作原料联产硅酸钠、水合硅酸及沸石催化剂的生产工艺,亦未见到直接在生产工艺过程中回收二氧化硫,经催化转换为硫酸直接作原料反应生成水合硅酸和芒硝,且生成的芒硝又可直接作补充原料,投入本生产工艺的实例。
本必明的目的是提出一种在工业生产中不仅能达到生产硅酸钠、水合硅酸及沸石催化剂的工业目的,而且在生产过程中将生产与环境治理相结合,能有效解决化工“三废”对环境污染问题的用芒硝法联产硅酸钠、水合硅酸及沸石催化剂工艺方法。
本发明的联产工艺的总体设想是:用芒硝、石英砂为原料。以碳热还原法制备固体硅酸钠并经水解成为液体硅酸钠,再将液体硅酸钠与硫酸反应制成的水合硅酸经老化成硅溶胶,再与偏铝酸钠反应制成沸石原粉,再将经干燥后的沸石原料在90±5℃条件下与碱土金属或稀土金属的氢氧化物或氯化物催化剂进行离子交换合成各种类型的沸石催化剂,经造粒、干燥、活化后成为成品。
本发明的联产工艺的特征是:将碳热还原法生产硅酸钠的生产过程中排放出的二氧化硫气体吸收转换生成硫酸,该硫酸与液体硅酸钠反应生成水合硅酸和芒硝,成品的水合硅酸可作为产品上市,也可深加工,作为吸附剂或催化剂的载体,还可当作原料合成沸石,而无水芒硝则可作为生产硅酸钠的原料补充。如此综合利用联产,达到工业生产良性循环的目的。
附图1是本发明的联产工艺流程图。
本联产工艺是以石英砂、碳粉和替代纯碱的芒硝为原料,以碳热还原法在1400℃高温炉内溶融生成固体硅酸钠,继而将固体硅酸钠固体投入密封容器内通入蒸汽加压水解,得到液体硅酸钠成品作为生产水合硅酸及沸石催化剂的主要原料,而生产硅酸钠所排放的含硫气体经催化转化成硫酸,作为生产水合硅酸及沸石催化剂的原料。
联产方法及工艺流程:
一、硅酸钠(Na2SiO3)
这种以芒硝生产硅酸钠的联产工艺流程, 其化学反应表达式如下:
其特征是选用含量为95%以上的细度为40目的无水芒硝作为基准物料和含量为97%以上,水份不大于1%,细度为40~60目的二氧化硅为原料,同时加入固定碳含量为70%以上,细度为20~40目,含硫量不大于0.05%,比热大于或等于7000大卡/千克的碳粉作还原剂按照纯物质摩尔比计算配量,模数即SiO2/Na2O×1.032,以2.8模数的硅酸钠的配料比为例:Na2SiO4∶SiO2∶C=(1.0+20%)∶1∶1∶(0.095+5%)进行配量,经粉碎后均匀混合,在特制的硅酸钠加热反射炉内持继稳定加热到1380℃~1400℃长达0.5~1小时,继而将熔融的硅酸钠水淬成固体碎块,继而再投放入4Kg/cm2压力,120℃的蒸汽球内溶解液化成液体硅酸钠。
二、回收SO2气体生产硫酸
用芒硝生产硅酸钠在反应中会排放大量SO2气体,本工艺采用相应技术措施以利用SO2气体作原料生成硫酸,其化学反应方程式是: 或
2、
其技术措施是回收加热反应炉中排放的二氧化硫气体,经净化塔、干燥塔,在转化塔内,在钾——钒沸石催化剂作用下,经氧化反应生成三氧化硫,再经吸收转化成硫酸。
三、水合硅酸(SiO2·nH2O)
用硫酸法生产水合硅酸是在常压下将浓度为95%的硫酸用水稀释至50%与2.8M40度玻尔浓度的液体硅酸钠采用喷雾方式在搅拌式反应器中进行反应化合为硅酸与芒硝的混合物料,再经老化、水洗、过滤、氨浸,PH值为5~8条件下的水洗、干燥、粉碎而得到成品,其化学反应式如下:
1、
生成的硅凝胶加热干燥即得水合硅酸(白炭黑)
成品水合硅酸经粉碎至320目包装,上市作为合成橡胶的补强剂或吸附剂和催化剂载体;在本联产工艺中生成的水合硅酸或硅溶胶用作沸石催化剂的原料。
本工序中第一次水洗、过滤的水溶液为玻尔浓度20~25的芒硝水,经真空浓缩、干燥而得到无水芒硝成品,即可提供用作生产硅酸钠的原料补充。
四、沸石催化剂(分子筛催化剂)
水合硅酸法(硅溶胶法)是用水合硅酸与偏铝酸钠为原料在常压下,以水热法合成沸石,本联产工艺中是选用高硅沸石,按不同类型催化剂的要求,用离子交换的方法合成多功能沸石催化剂。
本工艺首先合成Na-Y型沸石
Na2O∶Al2O3∶6SiO2(1∶1∶6)
干燥后的原粉经20%氨水(NH3·H2O)浸泡水洗干燥后与30%硝酸银水溶液在85℃温度下进行离子交换2小时,经水洗、干燥后分别用20%的钼酸铵和氯化镍溶液交换4小时,水洗、干燥后用30%的氢氧化铼溶液在90℃恒温下进行交换4小时,水洗、干燥后用150℃蒸汽活化2小时后用20%的洋甘土造粒在600℃~700℃温度下灼烧活化4小时即为成品。
用水合硅酸和偏铝酸钠合成沸石粉用20%氧化钙溶液50℃交换4小时,水洗、干燥后、氨浸2小时,水洗后用9%的氢氧化铼溶液交换合成中孔稀土沸石催化剂或用1%镧、铈的氢氧化物或氯化物水溶液合成,经造粒、干燥在600℃~700℃温度下活化成产品。
本工艺可用离子交换法合成含钾、钒、钡等碱金属或稀土氯化物的沸石催化剂。
Claims (3)
1、一种雾化法生产水合硅酸的方法,是用芒硝为原料,以碳热还原法,在1400℃反应炉中与二氧化硅溶融,经水淬、加压、水解工艺生成液态硅酸钠,生产水合硅酸的方法,其特征是以50%浓度的硫酸与2.8M40玻尔浓度的液体硅酸钠在搅拌式雾化反应器中采用喷雾的方式进行反应,老化、氨浸,反应PH值5-8条件下进行水洗、干燥、粉碎至高目数,包装成产品,生产硅酸钠反应生成的SO2气体及生产过程中排放的芒硝水均被回收利用。
2、如权利要求1所述的一种雾化法生产水合硅酸的方法,其特征是所述SO2的回收利用是在碳热还原法生产硅酸钠过程中排放的SO2气体经净化塔、干燥塔,在转化塔内,在钾-钒沸石催化剂作用下,经氧化反应生成三氧化硫,再经吸收转化成硫酸。
3、如权利要求1所述的一种雾化法生产水合硅酸的方法,其特征是所述生产过程中排放芒硝水的回收利用是将排放的芒硝水经真空浓缩、干燥转化成无水芒硝并做为生产硅酸钠的原料补充。
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US20080202387A1 (en) * | 2005-06-08 | 2008-08-28 | Yuanjian Lu | Process For Producing Silica and Sodium Sulfite With Sodium Sulfate |
CN1331744C (zh) * | 2005-06-08 | 2007-08-15 | 德固赛嘉联白炭黑(南平)有限公司 | 一种用硫酸钠法生产白炭黑和亚硫酸钠的工艺 |
CN107827119B (zh) * | 2017-11-07 | 2020-04-24 | 陆植才 | 一种活性白土两段活化生产工艺 |
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US2724701A (en) * | 1951-10-25 | 1955-11-22 | Grace W R & Co | Preparation of silicic acid sols |
US3492089A (en) * | 1968-11-26 | 1970-01-27 | Universal Oil Prod Co | Crystalline aluminosilicate faujasite manufacture |
US3492090A (en) * | 1966-04-07 | 1970-01-27 | Mobil Oil Corp | Process for producing faujasite |
CN1044931A (zh) * | 1989-02-16 | 1990-08-29 | 赵双根 | 用芒硝一步法连续生产钠碱的方法 |
CN1051709A (zh) * | 1989-11-09 | 1991-05-29 | 埃卡诺贝尔公司 | 硅溶胶,生产硅溶胶的方法及硅溶胶的用途 |
CN1053044A (zh) * | 1990-12-07 | 1991-07-17 | 贺江波 | 一种制备沉淀水合二氧化硅的方法 |
CN1065440A (zh) * | 1991-04-03 | 1992-10-21 | 大连理工大学 | 溶液诱发浓酸制白炭黑 |
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Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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US2724701A (en) * | 1951-10-25 | 1955-11-22 | Grace W R & Co | Preparation of silicic acid sols |
US3492090A (en) * | 1966-04-07 | 1970-01-27 | Mobil Oil Corp | Process for producing faujasite |
US3492089A (en) * | 1968-11-26 | 1970-01-27 | Universal Oil Prod Co | Crystalline aluminosilicate faujasite manufacture |
CN1044931A (zh) * | 1989-02-16 | 1990-08-29 | 赵双根 | 用芒硝一步法连续生产钠碱的方法 |
CN1051709A (zh) * | 1989-11-09 | 1991-05-29 | 埃卡诺贝尔公司 | 硅溶胶,生产硅溶胶的方法及硅溶胶的用途 |
CN1053044A (zh) * | 1990-12-07 | 1991-07-17 | 贺江波 | 一种制备沉淀水合二氧化硅的方法 |
CN1065440A (zh) * | 1991-04-03 | 1992-10-21 | 大连理工大学 | 溶液诱发浓酸制白炭黑 |
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