CN1223898A - 脱氯剂及其制备方法 - Google Patents
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Abstract
本发明的脱氯剂及其制备方法,是采用钙化合物、钠化合物、氢氧化铝、氢氧化铁为活性组成物,以无机粘土膨润土为载体,或者还加入胶体SiO2和扩孔剂,经混碾挤条后于80—120℃干燥,300—400℃焙烧制得的脱氯剂,其各组分的重量百分数按氧化物计分别为CaO10—40%、Na2O10—23%、Al2O35—11%、Fe2O311—24%、无机膨润土10—40%、胶体SiO2和扩孔剂分别为配料重量的0—5%。本发明的脱氯剂原料廉价易得,可将气体中HCl从1000ppm降至0.1ppm以下,此时穿透氯容达40—50m%,且耐水性好,可广泛用于石油化工和化肥工业中各种气体脱氯。
Description
本发明属于脱除化工原料气中氯化氢的气体净化剂及其制备方法。
在化肥工业和石油化工生产中，由于种种原因，原料气中或多或少含有氯化氢杂质。氯化氢对许多高效催化剂有毒害作用，极易造成催化剂中毒失活，同时还易腐蚀设备，生成盐类堵塞管线，生产中常常因为氯的危害而被迫减车、停车，严重影响了正常生产。
为解决此问题，须有效除去原料气中的氯化氢，国内外已相继研制出许多性能各异的脱氯剂并应用于生产中。US4762537利用活性氧化铝和Y沸石处理HCl小于100ppm的含氢重整气。US4639259将碱土金属负载在具有X-ρ-η物相结构的氧化铝上，氯容量可达13.8m％，净化度小于1ppm。US3935295则采用Ca(OH)2和ZnO混合，挤成条状物，可脱除微量氯和少量硫化氢，平均氯容达23.6m％。公开号CN1064099A将碱金属和碱土金属作为活性组分，混入天然无机粘土，可将原料气中HCl脱至0.5ppm，氯容量达35.2m％。公开号CN1147977则在碱金属或碱土金属中再引入锌化合物，可将原料气中氯脱除至0.1ppm以下，氯容量达30m％。此外，还有采用CuO-ZnO/Al2O3组分的脱氯剂，氯容量小于15m％。虽然脱氯剂品种和性能较早期有了很大发展，但在净化度、耐水性能上仍需改进提高。
本发明的目的在于提供一种新脱氯剂及其制备方法，该脱氯剂原料易得且制备容易，成本低而净化度好，氯容高，耐水性能佳，用于石油化工和化肥工业中各种含氯原料气的HCl脱除。
本发明的技术方案是：脱除化工原料气中氯化氢的脱氯剂是含有钙化合物如CaO、钠化合物如NaHCO3、Na2CO3、氢氧化铁Fe(OH)3、和氢氧化铝γ-AlOOH形成的活性组成物、无机粘土膨润土载体，其中，各组分的重量百分数按氧化物计分别为CaO 10-40％、Na2O 10-23％、Al2O3 5-11％、Fe2O3 11-24％、无机膨润土10-40％。
在本发明的脱氯剂中，为了使其具有更好的强度和耐水性，可在活性组成物和载体中加入组分重量百分数0-5％的胶体SiO2，为了使脱氯剂内部形成更多孔道，有利于传质的进行，提高氯容，可在活性组成物和载体中加入一定量的扩孔剂NH4HCO3或尿素，扩孔剂的添加量为配料总重量百分数的0-5％。
本脱氯剂的制备方法步骤是：
1、将氢氧化铁加水或者还加入配比量的胶体SiO2和扩孔剂NH4HCO3或尿素搅拌成悬浮液；
2、向上述悬浮液中加入配比量的氧化钙、碳酸钠或碳酸氢钠、氢氧化铝γ-AlOOH和膨润土混碾成膏状物，将此膏状物放置4小时以上；
3、将2所得膏状物挤条成型后于80-120℃干燥2小时以上，再在300-400℃焙烧2小时以上即得。
该脱氯剂侧压强度大于50N/cm。
氢氧化铁悬浮液由硫酸亚铁溶于水中，然后加氨水至pH≈7沉淀，过滤洗除SO4 2-后再加水制浆而成。
本发明的脱氯剂有如下特点：
1、净化度及氯容量高，在进口气中HCl含量100-1000ppm时，出口净化气中HCl含量小于0.1ppm，此时氯容量高达40-50％。
2、耐水性能好，在原料气水汽含量小于5％时性能不受影响。
3、原料廉价易得，工艺简单。
下面通过实施例进一步说明本脱氯剂的特点及制备。
实施例1
称取46.8g硫酸亚铁，溶于100mlH2O中，再逐步滴加3.0mol/L氨水并搅拌，至pH≈7.0，过滤洗涤至无SO4 2-，将滤饼加适量水打浆，使其分散，然后加入含11gCaO、39gNa2CO3、12gγ-AlOOH和32g膨润土的混合粉料，进行混碾成膏状物，将膏状物放置4小时以上后挤条成型，然后于80-120℃干燥2小时，300-400℃焙烧2小时即得脱氯剂A。
实施例2
称取46.8g硫酸亚铁，溶于100ml水中，再逐步滴加3,0mol/L氨水，搅拌至pH≈7.0，过滤洗涤至无SO4 2-，将滤饼加含有2gNH4HCO3和5ml 20m％胶体SiO2的混合溶液再制浆，使Fe(OH)3分散，然后加入含11gCaO、39gNa2CO3、12gγ-AlOOH和20g膨润土的混合粉料，进行混碾成膏状物，将膏状物放置5-6小时后挤条成型，然后于80-120℃干燥2小时，300-400℃焙烧2小时即得脱氯剂B。
实施例3
称取46.8g硫酸亚铁按实施例1所述的方法制成氢氧化铁浆料，再混入25gCaO、30gNa2CO3、19gγ-AlOOH和10g膨润土，混碾后放置6小时，于80-120℃干燥2小时，300-400℃焙烧2小时即得脱氯剂C。
实施例4
称取72.8g硫酸亚铁，按实施例1或2制成氢氧化铁沉淀，加入含2g尿素和3ml胶体SiO2(20m％)的混合溶液的水制成氢氧化铁浆料，再混入38gCaO、15gNa2CO3、9gγ-AlOOH和10g膨润土，混碾后放置5-6小时挤条，于80-120℃干燥2小时以上，300-400℃焙烧2小时以上，得脱氯剂D。
实施例5
称取39.8g硫酸亚铁，按实施例1所述方法制成氢氧化铁浆料，再混入17gCaO、36gNa2CO3、16gγ-AlOOH和15g膨润土，充分混碾后放置6-7小时后挤条成型，在80-120℃干燥2小时，300-400℃焙烧2小时，得脱氯剂E。
实施例6
本实施例为脱氯剂A-E脱除HCl性能的测试结果。脱氯剂强度测试在智能强度仪上测量，以测压强度(或抗碎强度)计。脱氯性能测试在φ10mm不锈钢反应器中进行，将脱氯剂A-E碎成20-40目的小颗粒，各取2.0ml装入反应器中，气体为H2-N2混合气，体积空速1000-3000h-1、配入HCl量为1000ppm，反应温度100-300℃，压力常压，氯容量以出口气体中HCl大于0.1ppm时的脱氯剂吸附量表示，即穿透氯容。
氯化氢的测量采用碱液吸收，分光光度法测定，氯容测定采用将穿透后样品粉碎干燥，称量后水浸，测定水中氯含量，然后计算得，氯的分析亦为分光光度法。其结果如表1。
表1
| 脱氯剂 | 强度N/cm | 空速h-1 | 反应温度℃ | 氯容m％ |
| ABCDE | 4655636259 | 300030003000300030001000 | 100200200100100300 | 39.847.644.343.945.850.2 |
Claims (4)
1、一种脱氯剂，其特征是含有CaO、Na2CO3或NaHCO3、Fe(OH)3、和γ-AlOOH形成的活性组成物和无机粘土膨润土载体，其中各组分的重量百分数按氧化物计分别为CaO 10-40％、Na2O 10-23％、Al2O3 5-11％、Fe2O3 11-24％、无机膨润土10-40％。
2、如权利要求1所述的脱氯剂，其特征是还含有胶体SiO2，胶体SiO2为组分重量百分数的0-5％。
3、权利要求1或2所述脱氯剂的制备方法，其特征是步骤为：
(1)将Fe(OH)3加水，或者还加入配比量的胶体SiO2和配料总重量百分数的0-5％的扩孔剂NH4HCO3或尿素，搅拌成胶体悬浮液；
(2)向(1)所得悬浮液中加入配比量的CaO、Na2CO3或NaHCO3、r-AlOOH及膨润土，混碾成膏状物，然后，放置4小时以上；
(3)将膏状物挤条成型后于80-120℃干燥2小时以上，再在300-400℃焙烧2小时以上即得。
4、如权利要求3所述的制备方法，其特征是氢氧化铁悬浮液由硫酸亚铁溶于水中，然后加氨水至pH≈7沉淀，过滤洗除SO4 2-后再加水制浆而成。
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100354030C (zh) * | 2004-11-01 | 2007-12-12 | 中国科学院生态环境研究中心 | 一种脱氯剂及其制备方法 |
| CN100453147C (zh) * | 2005-12-07 | 2009-01-21 | 西北化工研究院 | 催化重整再生气脱氯剂及制备方法 |
| CN101804298A (zh) * | 2010-04-10 | 2010-08-18 | 太原理工大学 | 一种氯气捕消剂的制备方法 |
| CN103127903A (zh) * | 2013-03-22 | 2013-06-05 | 沈阳三聚凯特催化剂有限公司 | 一种常温脱氯剂 |
| CN103316624A (zh) * | 2013-06-08 | 2013-09-25 | 华烁科技股份有限公司 | 一种脱磷剂及其制备方法 |
| CN109382388A (zh) * | 2017-08-07 | 2019-02-26 | 中国石化扬子石油化工有限公司 | 一种由废脱氯剂制备新鲜脱氯剂的方法 |
| CN115869900A (zh) * | 2022-12-27 | 2023-03-31 | 上海恒业微晶材料科技股份有限公司 | 一种复合型脱氯剂及其制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4639259A (en) * | 1985-10-09 | 1987-01-27 | Kaiser Aluminum & Chemical Corporation | Promoted scavenger for purifying HCl-contaminated gases |
| US4762537A (en) * | 1985-11-07 | 1988-08-09 | Aluminum Company Of America | Adsorbent for HCl comprising alumina and acid-treated Y zeolite |
| CN1064099A (zh) * | 1992-03-21 | 1992-09-02 | 南京化工学院 | 脱氯剂 |
| CN1088388C (zh) * | 1996-04-26 | 2002-07-31 | 湖北省化学研究所 | 精脱氯剂及制备方法 |
-
1998
- 1998-11-24 CN CN98121676A patent/CN1095388C/zh not_active Expired - Lifetime
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100354030C (zh) * | 2004-11-01 | 2007-12-12 | 中国科学院生态环境研究中心 | 一种脱氯剂及其制备方法 |
| CN100453147C (zh) * | 2005-12-07 | 2009-01-21 | 西北化工研究院 | 催化重整再生气脱氯剂及制备方法 |
| CN101804298A (zh) * | 2010-04-10 | 2010-08-18 | 太原理工大学 | 一种氯气捕消剂的制备方法 |
| CN101804298B (zh) * | 2010-04-10 | 2013-03-27 | 太原理工大学 | 一种氯气捕消剂的制备方法 |
| CN103127903A (zh) * | 2013-03-22 | 2013-06-05 | 沈阳三聚凯特催化剂有限公司 | 一种常温脱氯剂 |
| CN103316624A (zh) * | 2013-06-08 | 2013-09-25 | 华烁科技股份有限公司 | 一种脱磷剂及其制备方法 |
| CN103316624B (zh) * | 2013-06-08 | 2015-03-04 | 华烁科技股份有限公司 | 一种脱磷剂及其制备方法 |
| CN109382388A (zh) * | 2017-08-07 | 2019-02-26 | 中国石化扬子石油化工有限公司 | 一种由废脱氯剂制备新鲜脱氯剂的方法 |
| CN115869900A (zh) * | 2022-12-27 | 2023-03-31 | 上海恒业微晶材料科技股份有限公司 | 一种复合型脱氯剂及其制备方法 |
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|---|---|
| CN1095388C (zh) | 2002-12-04 |
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