CN1768905A - Dechlorination agent and preparation method thereof - Google Patents

Dechlorination agent and preparation method thereof Download PDF

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Publication number
CN1768905A
CN1768905A CN 200410088724 CN200410088724A CN1768905A CN 1768905 A CN1768905 A CN 1768905A CN 200410088724 CN200410088724 CN 200410088724 CN 200410088724 A CN200410088724 A CN 200410088724A CN 1768905 A CN1768905 A CN 1768905A
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China
Prior art keywords
antichlor
calcium
deionized water
naoh
titration
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CN 200410088724
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Chinese (zh)
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CN100354030C (en
Inventor
郑明辉
马小东
刘文彬
张兵
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Research Center for Eco Environmental Sciences of CAS
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Research Center for Eco Environmental Sciences of CAS
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Priority to CNB2004100887242A priority Critical patent/CN100354030C/en
Publication of CN1768905A publication Critical patent/CN1768905A/en
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Publication of CN100354030C publication Critical patent/CN100354030C/en
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Abstract

The invention provides a dechlorinating agent and it's preparing method. Said dechlorinating agent uses the nanometer ferro-calcium composite metallic oxide superfine powder as active component while its components comprises: CaO and Ca2Fe2O5, or Fe2O3 and CaFe2O4. And the mol ratio between calcium and iron atom is 6:1-1:1. The preparing method is that using NaOH, KOH or dense NH3 as titrant, to titrate the mixture of ferric iron salt and calcium salt in water-bath and 30-100Deg. C, to be completely deposited, and washing, filtering, drying and milling the deposition to be sintered at 500-900Deg. C. Said invention has high effect, lower cost and simple operation which can apply removing chlorine in variable organic chloride.

Description

A kind of antichlor and preparation method thereof
Technical field
The present invention relates to a kind of organic chloride antichlor, specifically, relate to a kind of nanometer calcium iron composite metal oxide superfine powder that removes chlorine in the organic chloride.
The invention still further relates to the preparation method of above-mentioned antichlor.
Background technology
Organochlorine compound is the important compound of a class, is widely used for various chemical raw materials, reagent.The some of them compound not only has higher toxicity, and is difficult to degraded in environment, and ecological environment and health are constituted a threat to.Significant to its disinfection.Have and studies show that dechlorination is a kind of effective processing means.
In recent years, existing many dechlorination technology are published.Adopting natural sepiolite, alkali metal and alkaline earth metal compounds as Chinese patent 1334139 is active component, and to the high-temperature gas dechlorination, its chlorosity reaches 36%.Chinese patent 1147977 antichlors with receive, the compound of calcium and zinc is the active component of antichlor, with kaolin or rectorite, bentonite, diatomite is that carrier adds suitable quantity of water and directly mixes extrusion modling, make the chlorine<0.1ppm in its Purge gas again through roasting.Chinese patent 1353005 solid dechlorinating agent active components are calcium hydroxide or calcium hydroxide and calcium carbonate or sodium carbonate and calcium carbonate, can be used for removing hydrogen chloride in gas under the high temperature.Chinese patent 1064099 is the active component of antichlor with alkali metal compound or alkaline earth metal compound, is binding agent with the natural inorganic clay, adds the direct batch mixing moulding of an amount of water, makes antichlor through roasting again and can be used for gas purification.Chinese patent 1223898 antichlors with calcium compound, to receive compound, aluminium hydroxide, iron hydroxide be active constituent, is carrier with inorganic clay, bentonite, perhaps also adds colloid SiO 2And spreading agent, make through moulding, drying, roasting.Its chlorosity reaches 40-50%.It is active component that Chinese patent antichlor 1178133 adopts sodium carbonates, calcium carbonate and magnesia, carries out compositely, is carrier with inorganic clay, bentonite, diatomite or kaolin, adds modified additive, and through mixed grind, extruded moulding, drying, roasting are made again.Chinese patent 1481942 provides a method, and its key step is in the aqueous solution of the 2-10% of 0.05-0.5% alkaline earth metal compound inorganic base, under the condition of 160-280 ℃, 1.0-5.0Mpa and inert gas organic waste materials is handled.It is the alkaline-earth metal antichlor of carrier that U.S. Pat 4639259 adopts aluminium oxide, and penetrating chlorosity is 20%.U.S. Pat 3935295 is formed antichlor with zinc oxide and alkaline-earth metal, and below 500 ℃, chlorosity is 10-35%.
It is active component that above antichlor adopts alkali metal and alkaline earth metal compounds mostly, and its dechlorination efficiency is lower.Chief reason is to be carried on that active component kind on the carrier is single, content is lower.
Summary of the invention
The object of the present invention is to provide a kind of antichlor that is applicable to organochlorine compound.
Another object of the present invention is to provide the preparation method of above-mentioned antichlor.
Antichlor provided by the invention has overcome known antichlor active component mainly based on alkali metal, alkaline-earth metal and compound thereof, and content is lower, activity is single, the defective of dechlorination effect difference, and has the dechlorination efficiency height, the advantage that cost is low.
For achieving the above object, antichlor provided by the invention is with the active component of nanometer calcium iron composite metal oxide superfine powder as antichlor.Species in the antichlor can comprise CaO and Ca 2Fe 2O 5Or Fe 2O 3With CaFe 2O 4Wherein the mol ratio of calcium and iron is 6 in the antichlor: 1-1: 1.
The method of the above-mentioned antichlor of preparation provided by the invention, its key step is:
With NaOH or KOH or dense NH 3Be titrant, the mixed solution to trivalent iron salt and calcium salt under the condition of water bath with thermostatic control carries out titration, and it is precipitated fully.Precipitation is made antichlor through washing, filtration, oven dry, grinding, roasting.The concentration of above-mentioned trivalent iron salt, calcium salt and titrant is 0.05-2mol/L.The bath temperature of drop reaction is 30-100 ℃.The rate of titration of drop reaction is 10-30ml/min.After filtration, deionized water washing, wash as dispersant with ethanol or methyl alcohol.Bake out temperature is 50-250 ℃, and the time is 12-48 hour.Sintering temperature is 500-900 ℃, and roasting time is 2-8 hour.
By above-mentioned disclosed technical scheme as seen, antichlor of the present invention is the nanometer calcium iron composite metal oxide powder that adopts the method preparation of co-precipitation.By the synergy between the calcium ferriferous oxide, improve dechlorination ability to organochlorine compound, the patented technology of enumerating in this and the background technology has significant difference.
Antichlor of the present invention can be used for removing of chlorine in the various organochlorine compounds.
The specific embodiment
Be better understanding content of the present invention, the present invention is further illustrated below by embodiment, but the cited case does not limit protection scope of the present invention.
Embodiment 1
7.2 gram NaOH are dissolved in 370 ml deionized water 16.8 gram Ca (NO 3) 2.4H 2O and 5.1 gram Fe (NO 3) 3.9H 2O is dissolved in 320 ml deionized water, and vigorous stirring under 30 ℃ of water-baths treats that solution is mixed into an even phase, carry out titration with above-mentioned NaOH solution, the speed of control titration is 10ml/min, after precipitation is complete, the gained precipitation is successively with deionized water, absolute ethyl alcohol washs, and puts into 120 ℃ of baking ovens, dry 20 hours, take out, place muffle furnace,, get antichlor of the present invention in 500 ℃ of roastings 8 hours.It consists of CaO and Ca 2Fe 2O 5
Embodiment 2
7.3 gram NaOH are dissolved in 370 ml deionized water 12.7 gram Ca (NO 3) 2.4H 2O and 10.1 gram Fe (NO 3) 3.9H 2O is dissolved in 320 ml deionized water, and vigorous stirring under 100 ℃ of water-baths treats that solution is mixed into an even phase, carry out titration with above-mentioned NaOH solution, the speed of control titration is 20ml/min, after precipitation is complete, the gained precipitation is successively with deionized water, absolute ethyl alcohol washs, and puts into 50 ℃ of baking ovens, dry 48 hours, take out, place muffle furnace,, get antichlor of the present invention in 600 ℃ of roastings 4 hours.It consists of CaO and Ca 2Fe 2O 5
Embodiment 3
7.5 gram NaOH are dissolved in 370 ml deionized water 4.3 gram Ca (NO 3) 2.4H 2O and 20.3 gram Fe (NO 3) 3.9H 2O is dissolved in 320 ml deionized water, and vigorous stirring under 50 ℃ of water-baths treats that solution is mixed into an even phase, carry out titration with above-mentioned NaOH solution, the speed of control titration is 10ml/min, after precipitation is complete, the gained precipitation is successively with deionized water, absolute methanol washs, and puts into 120 ℃ of baking ovens, dry 20 hours, take out, place muffle furnace,, get antichlor of the present invention in 600 ℃ of roastings 4 hours.It consists of Fe 2O 3With CaFe 2O 4

Claims (4)

1, a kind of antichlor, its activity consists of CaO and Ca 2Fe 2O 5Or Fe 2O 3With CaFe 2O 4The mol ratio of calcium and iron is 6 in the antichlor: 1-1: 1.
2, prepare the method for the described antichlor of claim 1, it is characterized in that, with NaOH or KOH solution or the dense NH of concentration 0.05-2mol/L 3Be titrant, the mixed solution to trivalent iron salt and/or calcium salt under 30-100 ℃ of water-bath carries out titration, and it is precipitated fully, filter, the deionized water washing, 50-250 ℃ of oven dry 12-48 hour, 500-900 ℃ roasting 2-8 hour, make antichlor.
3, the described preparation method of claim 2 is characterized in that, rate of titration is 10-30ml/min.
4, the described preparation method of claim 2 is characterized in that, precipitates after the deionized water washing again with ethanol or methanol wash.
CNB2004100887242A 2004-11-01 2004-11-01 Dechlorination agent and preparation method thereof Expired - Fee Related CN100354030C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB2004100887242A CN100354030C (en) 2004-11-01 2004-11-01 Dechlorination agent and preparation method thereof

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Application Number Priority Date Filing Date Title
CNB2004100887242A CN100354030C (en) 2004-11-01 2004-11-01 Dechlorination agent and preparation method thereof

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CN1768905A true CN1768905A (en) 2006-05-10
CN100354030C CN100354030C (en) 2007-12-12

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101274211B (en) * 2008-05-23 2011-03-30 北京三聚环保新材料股份有限公司 High-temperature dechlorinating agent and preparing method thereof
CN102513111A (en) * 2011-10-30 2012-06-27 中国科学院西双版纳热带植物园 CaFe2O4 type magnetic solid catalyst and application thereof
CN101954166B (en) * 2009-07-16 2012-07-04 中国科学院大连化学物理研究所 Method for degrading aryl halide organic pollutants
CN102824718A (en) * 2012-09-07 2012-12-19 桂林市产品质量监督检验所 Compound catalytic dechlorinating agent
CN105617853A (en) * 2015-12-30 2016-06-01 沈阳三聚凯特催化剂有限公司 Gaseous phase dechlorinating agent and preparation method thereof
CN105749855A (en) * 2014-12-19 2016-07-13 中国石油天然气股份有限公司 Liquid-phase antichlor and preparation method and application thereof

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08504665A (en) * 1992-12-18 1996-05-21 ジ ユニバシティー オブ ウエスタン オーストラリア How to treat toxic substances
CN1088388C (en) * 1996-04-26 2002-07-31 湖北省化学研究所 Refined antichlor and method for preparing same
CN1095388C (en) * 1998-11-24 2002-12-04 湖北省化学研究所 Dechlorinating agent and its preparing method
CN1302834C (en) * 2003-10-31 2007-03-07 中国科学院生态环境研究中心 Method for dechloridizing organochloric compound

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101274211B (en) * 2008-05-23 2011-03-30 北京三聚环保新材料股份有限公司 High-temperature dechlorinating agent and preparing method thereof
CN101954166B (en) * 2009-07-16 2012-07-04 中国科学院大连化学物理研究所 Method for degrading aryl halide organic pollutants
CN102513111A (en) * 2011-10-30 2012-06-27 中国科学院西双版纳热带植物园 CaFe2O4 type magnetic solid catalyst and application thereof
CN102824718A (en) * 2012-09-07 2012-12-19 桂林市产品质量监督检验所 Compound catalytic dechlorinating agent
CN102824718B (en) * 2012-09-07 2015-04-15 桂林市产品质量监督检验所 Compound catalytic dechlorinating agent
CN105749855A (en) * 2014-12-19 2016-07-13 中国石油天然气股份有限公司 Liquid-phase antichlor and preparation method and application thereof
CN105749855B (en) * 2014-12-19 2018-12-25 中国石油天然气股份有限公司 Liquid phase antichlor and its preparation method and application
CN105617853A (en) * 2015-12-30 2016-06-01 沈阳三聚凯特催化剂有限公司 Gaseous phase dechlorinating agent and preparation method thereof
CN105617853B (en) * 2015-12-30 2018-08-03 沈阳三聚凯特催化剂有限公司 A kind of gas phase antichlor and preparation method thereof

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