CN1040865C - 从盐酸中除去不希望颜色的方法 - Google Patents
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- CN1040865C CN1040865C CN95190500A CN95190500A CN1040865C CN 1040865 C CN1040865 C CN 1040865C CN 95190500 A CN95190500 A CN 95190500A CN 95190500 A CN95190500 A CN 95190500A CN 1040865 C CN1040865 C CN 1040865C
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- hydrochloric acid
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 21
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 16
- 150000002367 halogens Chemical class 0.000 claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 15
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 9
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005342 ion exchange Methods 0.000 claims abstract description 4
- 230000002829 reductive effect Effects 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052801 chlorine Inorganic materials 0.000 abstract description 9
- 239000000460 chlorine Substances 0.000 abstract description 9
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 abstract description 8
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052794 bromium Inorganic materials 0.000 abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 abstract description 5
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract description 3
- 238000004040 coloring Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- RBLWMQWAHONKNC-UHFFFAOYSA-N hydroxyazanium Chemical compound O[NH3+] RBLWMQWAHONKNC-UHFFFAOYSA-N 0.000 description 2
- -1 hydroxylammonium ion Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treatment Of Sludge (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Silver Salt Photography Or Processing Solution Therefor (AREA)
- Optical Filters (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Catalysts (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
从盐酸中脱除如铁和卤素的带色物质的方法。在卤素中尤其是氯和溴对颜色的贡献最多。优选用过滤和离子交换先从盐酸中除去铁。然后，向酸中加入含氮还原剂。优选使用含羟胺化合物，更优选使用盐酸羟胺。还原剂的加入量是按化学计量过量。
Description
通过破坏氯代烃生产盐酸所得的产品，由于其它杂质：铁、游离溴和游离氯的存在而带黄色。这种带色的酸限制了它们在工业上的应用和具有较低的价值。为提高这种酸的使用价值，有必要采取简单而经济的方法从酸中除去颜色。
以前已知一些从HCl中除去这类化合物的方法。美国专利4,349,525描述一种从碱性氯化物和硫酸的反应生产的盐酸的纯化方法。此方法发现该颜色是Br2造成的，和同时除去的SO2也使颜色水平进一步降低。根据此专利的方法，是用情性气体和氧气的吹洗来纯化此酸。这可得到无色的酸。但由于要使用气提塔和供给足量的惰性气体和氧，此方法是很昂贵的。
从欧洲专利申请0506050已知一种从盐酸中除去氟、溴、碘和它们的氢化物的方法。此方法是这样进行的：第一步加入化学计量过量的可溶解氯盐，使它们的氟化物沉淀从而除去HF和氟化物。然后，蒸馏酸。为除去Br2碘、溴化物和碘化物要加入使生成元素的溴或碘所需量的氯和然后用水蒸汽气提除去这些杂质。这是很广泛使用的和昂贵的处理工序。
本发明的目的是开发一种有效除去带色物质的方法，此方法是价廉的、易于操作和对于内、外环境都是安全的。同时，此方法也不会造成待处理的酸中又产生不希望的反应产物。
这些和其它发明目的可以通过下述方法和应用来实现。所附权利要求书也进一步限定和规定本发明的特征。
本发明是涉及从盐酸中除去铁和卤素这样的带色物质的方法。在这些卤素中对颜色作出贡献的尤其是氯和溴。首先最好通过过滤或离子交换从盐酸中除去铁，和然后向酸中加入含氮还原剂。对于该含氮还原剂优选使用含羟胺的化合物，更优选使用盐酸羟胺(氯化羟铵)。加入还原剂的量为化学计量过量。
例如通过过滤和离子交换可首先从酸中除去铁。对所生产的盐酸的分析表明除铁之后黄色的主要来源是如游离氯和溴的卤素。已发现可加入还原剂使残留的游离氯和溴被还原。
可接受的还原剂必须具备以下性能：
1.高效。该化合物应尽可能有效地与氯和溴反应。
2.低价格。
3.易于操作。该化合物应该是可泵送的或易于使之泵送的(溶于水的)。
4.对工作场地和外部环境无害。
5.在盐酸中不产生不希望的反应产物。
这些要求导致去调查在具有低分子量的众多简单化合物中的可能入选者。考察了几个含氮还原剂。可以提及下述的一些实际化合物：有机胺，肼和含羟胺(羟铵)的化合物。最实际的化合物是肼和羟胺。肼是有活性的但对环境有害。而发现羟胺可满足全部要求。并发现盐酸羟胺是最有效的和在实例中使用作为例示。
在盐酸中的羟胺是以羟铵离子NNOH+形式存在。游离卤素与羟胺之间最可能的反应如下所述，其中反应1是占优势的：
1.
2.
剩余的羟胺可能按下式反应岐化为N2O和NH4 +：
产生颜色的组分因此还原为无色的氯化物和溴化物。为验证这试剂可否除去酸的颜色和除去颜色到多大程度已进行还原实验。检验需要消耗大量的试剂也是必要的。
盐酸的色值(the colour numbers)是用LOVIBOND 2000色辉计(比色计)测定的。带色程度以霾值(Hazen)表示的。
实验1
进行了实验室实验。使用样品体积为200毫升的清净无色的玻璃瓶。温度为20-22℃和在实验期间玻瓶是不避光的。每升盐酸加入3毫摩尔盐酸羟胺。这相当于208.5毫克H3NOHCl。盐酸比重约为1.16和含有以氯计为110ppm的卤素。结果示于表1。
表1
| 酸 | 加入H3NOHCl后的时间 | 色值Hazen |
| HCl HRA | 100-125 | |
| HCl HRA+H3NOHCl | 10分钟 | 175-200 |
| HCl HRA+H3NOHCl | 30分钟 | 225 |
| HCl HRA+H3NOHCl | 50分钟 | 150 |
| HCl HRA+H3NOHCl | 80分钟 | 70 |
| HCl HRA+H3NOHCl | 155分钟 | 30-40 |
| HCl HRA+H3NOHCl | 1昼夜 | 15-20 |
| HCl HRA+H3NOHCl | 3昼夜 | 15-20 |
| HCl HRA+H3NOHCl | 4昼夜 | 15-20 |
| HCl HRA+H3NOHCl | 5昼夜 | 15-20 |
| HCl HRA+H3NOHCl | 6昼夜 | 15-20 |
从表中可见，在20℃一昼夜后色值从100-125 Hazen减至15-20 Hazen。也可以看出：在加入还原剂后第1个半小时颜色的强度基本上是增加的。
以实验室小试为基础，将实验扩大进行。但这并未给出预期的结果。在加入羟胺时酸并未变得清澈和无色。
因此，又进行一些试验。从生产现场取来10升盐酸用于全部实验。在进行实验之前先完成如下分析。结果见表2。
表2
| ％ HCl | 氯 | Fe | 色值 | TSS* |
| 33.05 | 97ppm | 0.56ppm | 100Hazen | 2ppm |
*总悬浮固体
实验2
必须检验温度的因素。取盐酸试样冷却至0℃和向100毫升盐酸试样中加入0.3毫升25％的盐酸羟胺溶液。这相当于750毫克/升酸。此试样再放回冰箱中保持同样温度，和在30分钟后和60分钟后分别测量色值。在60分钟后试样完全为无色。此时用碘量法分析卤素含量＜1ppm。在同样温度贮存9昼夜之后试样仍是无色的。
相同的实验在22℃下完成。结果表明30分钟后酸变为无色。此时卤素含量经分析小于1ppm。
两个检验温度均得到相同结果-无色的酸，但为使酸无色所需的时间随温度的增加而减少。
也应指出，为快速有效，还原剂与试样的充分混合是重要的。
实验3
搅拌下将还原剂(盐酸羟胺)以4个不同浓度(187，375，750和1000mg/升)加到酸中。在第1个30分钟是每5分钟间隔测量一次色值，在第2个30分钟是每10分钟间隔测量一次色值和在此后2.5小时内是每隔半小时测量一次。温度为22℃。-187mg/升：此剂量表现为3.5小时后色值增加至225Hazen。颜色并不消失。1小时后分析卤素为85ppm。-375mg/升：此剂量表现为25分钟后色值增加至300Hazen。此后色值减小和在120分钟后为20Hazen。1小时后分析卤素为8ppm。-750mg/升：此剂量表现为5分钟后色值达最大值250Hazen，但30分钟后急剧下降至20Hazen分析卤素含量小于1ppm。-1000mg/升：此剂量表现为与750mg/升相同的结果。-5000mg/升：此剂量表现为反应很快进行，酸变得清澈和无色，为20Hazen和无再变色的指示。
从上述结果可见，正确的剂量是375-750mg/升之间，即对此卤素含量而言大约500mg/升。此剂量使酸在约30-40分钟后变清澈和氯含量小于1ppm。使用此剂量，也包括卤素含量/颜色的自然变化可能发生和混合不及大规模那样好。
还原剂加入的量将取决于酸中存在的卤素含量。但是一般而言可以说，加入的还原剂的量相对于化学计量而言是过量的，这样可获得期望的效果。
按照本发明可以得到一个简便经济的方法。此方法可用于工业规模，并可得到可出售的产品。
Claims (3)
1.从盐酸中脱除如铁和卤素的带色物质的方法，其特征是，从盐酸中先除去存在的铁和然后向酸中加入超化学计量的含羟基胺的化合物形式的还原剂。
2.权利要求1的方法，其特征是将盐酸羟胺用作还原剂。
3.权利要求1的方法，其特征是除去铁的方法是过滤和离子交换。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| NO942074 | 1994-06-03 | ||
| NO19942074A NO179243B1 (no) | 1994-06-03 | 1994-06-03 | Fremgangsmate for a fjerne uonsket farge fra saltsyre, samt anvendelse av hydroksylaminhydroklorid for a fjerne uonsket farge fra saltsyre |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1128978A CN1128978A (zh) | 1996-08-14 |
| CN1040865C true CN1040865C (zh) | 1998-11-25 |
Family
ID=19897144
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95190500A Expired - Fee Related CN1040865C (zh) | 1994-06-03 | 1995-05-31 | 从盐酸中除去不希望颜色的方法 |
Country Status (12)
| Country | Link |
|---|---|
| US (1) | US6290927B1 (zh) |
| EP (1) | EP0725759B1 (zh) |
| JP (1) | JPH08509455A (zh) |
| CN (1) | CN1040865C (zh) |
| AT (1) | ATE184860T1 (zh) |
| AU (1) | AU2684395A (zh) |
| DE (1) | DE69512378T2 (zh) |
| ES (1) | ES2138215T3 (zh) |
| NO (1) | NO179243B1 (zh) |
| PL (1) | PL179886B1 (zh) |
| RU (1) | RU2107020C1 (zh) |
| WO (1) | WO1995033680A1 (zh) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10101394A1 (de) * | 2001-01-15 | 2002-07-18 | Bayer Ag | Verfahren zur Verwertung von Abfallsalzmischungen von HALEX-Reaktionen |
| JP2007022956A (ja) * | 2005-07-15 | 2007-02-01 | Mitsubishi Gas Chem Co Inc | 高純度アミノメチレンホスホン酸の製造方法 |
| WO2014203276A2 (en) | 2013-06-17 | 2014-12-24 | Reliance Industries Limited | A process for the removal of metal contaminants from fluids |
| CN108383083A (zh) * | 2018-03-16 | 2018-08-10 | 三峡大学 | 一种负载型盐酸脱色剂及其制备方法和脱色工艺 |
| CN108435137A (zh) * | 2018-03-16 | 2018-08-24 | 三峡大学 | 一种盐酸脱色及盐酸金属离子脱除的负载型试剂及制备方法 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6136102A (ja) * | 1984-07-27 | 1986-02-20 | Asahi Glass Co Ltd | 塩化水素中に含まれる弗化水素の除去法 |
| EP0506050A1 (de) * | 1991-03-27 | 1992-09-30 | QVF Glastechnik GmbH | Verfahren zur Herstellung einer von Fremdhalogenen gereinigten Salzsäure |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1770010A (en) * | 1927-04-27 | 1930-07-08 | British Dyestuffs Corp Ltd | Removal of free chlorine and bromine from fluid mixtures |
| US2787525A (en) * | 1952-01-23 | 1957-04-02 | Columbia Southern Chem Corp | Removal of free chlorine from hci |
| US2787523A (en) * | 1952-02-23 | 1957-04-02 | Columbia Southern Chem Corp | Removal of chlorine from hci |
| US3855400A (en) * | 1972-02-10 | 1974-12-17 | Hooker Chemicals Plastics Corp | Purification of hydrochloric acid |
| DE2836580C3 (de) * | 1978-08-21 | 1981-11-05 | Chemische Werke Hüls AG, 4370 Marl | Verfahren zur Trennung von Chlorwasserstoff und Bromwasserstoff |
| US4349525A (en) * | 1981-04-21 | 1982-09-14 | Chisso Corporation | Process for purifying hydrochloric acid produced from alkali chloride and sulfuric acid |
| JPH02233503A (ja) * | 1989-03-06 | 1990-09-17 | Daiso Co Ltd | 塩酸の精製方法 |
| DE4344200C2 (de) | 1993-12-23 | 1995-11-30 | Schering Ag | Verfahren zur Salzsäuregewinnung aus brom- und jodhaltigen Rauchgasen |
-
1994
- 1994-06-03 NO NO19942074A patent/NO179243B1/no not_active IP Right Cessation
-
1995
- 1995-05-31 JP JP8500697A patent/JPH08509455A/ja active Pending
- 1995-05-31 EP EP95922008A patent/EP0725759B1/en not_active Expired - Lifetime
- 1995-05-31 AT AT95922008T patent/ATE184860T1/de not_active IP Right Cessation
- 1995-05-31 DE DE69512378T patent/DE69512378T2/de not_active Expired - Fee Related
- 1995-05-31 RU RU96104255A patent/RU2107020C1/ru not_active IP Right Cessation
- 1995-05-31 US US08/586,874 patent/US6290927B1/en not_active Expired - Fee Related
- 1995-05-31 CN CN95190500A patent/CN1040865C/zh not_active Expired - Fee Related
- 1995-05-31 AU AU26843/95A patent/AU2684395A/en not_active Abandoned
- 1995-05-31 WO PCT/NO1995/000085 patent/WO1995033680A1/en active IP Right Grant
- 1995-05-31 PL PL95312777A patent/PL179886B1/pl not_active IP Right Cessation
- 1995-05-31 ES ES95922008T patent/ES2138215T3/es not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6136102A (ja) * | 1984-07-27 | 1986-02-20 | Asahi Glass Co Ltd | 塩化水素中に含まれる弗化水素の除去法 |
| EP0506050A1 (de) * | 1991-03-27 | 1992-09-30 | QVF Glastechnik GmbH | Verfahren zur Herstellung einer von Fremdhalogenen gereinigten Salzsäure |
Also Published As
| Publication number | Publication date |
|---|---|
| NO179243C (no) | 1996-09-04 |
| DE69512378D1 (de) | 1999-10-28 |
| EP0725759B1 (en) | 1999-09-22 |
| DE69512378T2 (de) | 2000-04-06 |
| WO1995033680A1 (en) | 1995-12-14 |
| PL312777A1 (en) | 1996-05-13 |
| RU2107020C1 (ru) | 1998-03-20 |
| ES2138215T3 (es) | 2000-01-01 |
| ATE184860T1 (de) | 1999-10-15 |
| NO179243B1 (no) | 1996-09-23 |
| AU2684395A (en) | 1996-01-04 |
| JPH08509455A (ja) | 1996-10-08 |
| NO179243B (no) | 1996-05-28 |
| EP0725759A1 (en) | 1996-08-14 |
| NO942074D0 (no) | 1994-06-03 |
| PL179886B1 (pl) | 2000-11-30 |
| CN1128978A (zh) | 1996-08-14 |
| NO942074A (no) | 1995-12-04 |
| US6290927B1 (en) | 2001-09-18 |
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