CN101513605A - Method of preparing sulfur leaching mercury control activated carbon - Google Patents

Method of preparing sulfur leaching mercury control activated carbon Download PDF

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Publication number
CN101513605A
CN101513605A CNA2009100249314A CN200910024931A CN101513605A CN 101513605 A CN101513605 A CN 101513605A CN A2009100249314 A CNA2009100249314 A CN A2009100249314A CN 200910024931 A CN200910024931 A CN 200910024931A CN 101513605 A CN101513605 A CN 101513605A
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China
Prior art keywords
activated carbon
mercury
sulfur
active carbon
control activated
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Pending
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CNA2009100249314A
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Chinese (zh)
Inventor
施荫锐
刘军利
荀永葆
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NANJING ZHENGSEN CHEMICAL INDUSTRY Co Ltd
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NANJING ZHENGSEN CHEMICAL INDUSTRY Co Ltd
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Priority to CNA2009100249314A priority Critical patent/CN101513605A/en
Publication of CN101513605A publication Critical patent/CN101513605A/en
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Abstract

The invention relates to a method of preparing sulfur leaching mercury control activated carbon, which has the advantages of simple process and low cost. In the preparing method of the sulfur leaching mercury control activated carbon, the activated carbon is put in an enclosed vessel after being mixed with sulfur for 2-24 hours under 120-300 DEG C. The weight ratio of the activated carbon to the sulfur is from 1 to 0.02 to 1 to 0.6. The specific surface area of the activated carbon is from 200m<2>/g to 1300m<2>/g. The method of preparing the sulfur leaching mercury control activated carbon skillfully uses the sublimation ability and the low polarity and heats the sulfur in the enclosed vessel. The sulfur directly enters pores of the activated carbon and attaches into the pores of the activated carbon. When gas containing mercury enters the pores of the activated carbon, the mercury is captured by the sulfur, and mercury sulfide is formed. The preparing method has the advantages of simple process, low cost, high sulfur leaching amount and high mercury control efficiency. Compared with all the other methods, the preparing method is perfect and can easily recycle the mercury sulfide.

Description

The preparation method of sulfur leaching mercury control activated carbon
Technical field
The present invention relates to a kind of preparation method of sulfur leaching mercury control activated carbon.
Background technology
The harmful element mercury vapour can enter in all gases with various approach, such as air, oxygen, chlorine, carbon dioxide, natural gas, oil gas, artificial synthesis gas, burnt gas or the like.No matter all need remove mercury from environmental angle or food security.Mercury is a kind of trace element in the coal, and in coal combustion process, mercury can enter in the atmosphere, is present in the atmosphere for a long time.Harmful element mercury all has mercury to enter atmosphere when metal smelt, smelting iron and steel, cement industry, chlorine industry, waste incineration, oil combustion.China in 2003 total amount of being discharged into mercury in the atmosphere has reached 650 tons according to statistics.So the present invention seeks to from gas, to remove a kind of good adsorption agent of mercury,, promptly be the safety of human survival with protection environment and the safety that reaches food.
Gas phase method for removing hydrargyrum in the past has following several:
(a) allow and contain mercury gas and be absorbed by potassium sulfate solution and form HgSO 4, drop into K again 2S, K 2S and H gSO 4Form HgS and be recovered, or allow and contain mercury gas and absorb by solid calcium hydroxide, activated charcoal, active carbon, these method demercuration efficient are low.
(b) use H 2SO 4, oxidant such as nitric acid, persulfuric acid silver, NH 2NH 2The 2HCl Immesion active carbon is removed the mercury in the gas, improves the adsorption capacity of active carbon to mercury, but complex process, cost height, efficient are not high.
(c) flood potassium triiodide with active carbon, cost is too high.
(d) element sulphur is dissolved in Immesion active carbon behind carbon disulfide or the chloroform, after carbon disulfide, the chloroform evaporation, becomes sulfur leaching mercury control activated carbon.Because Sulfur capacity is easy and mercury generation chemical reaction, generates HgS, owing to the porous adsorptivity of sulfur leaching mercury control activated carbon, not only can effectively adsorb and contain mercury gas, and increase the contact area of sulphur and mercury greatly simultaneously, thereby can high-efficiency mercury removal.Wherein soak sulfur content (be the quality of dipping sulphur on the unit mass active carbon, unit is 100%) and directly determined the demercuration efficient of sulfur leaching mercury control activated carbon, it is high more to soak sulfur content, and demercuration efficient is good more.But this method need reclaim the solvent condenses that evaporates, and continues to use complex process, cost height.
Summary of the invention
The invention provides a kind of preparation method of sulfur leaching mercury control activated carbon, technology is simple, cost is low.
The preparation method of described sulfur leaching mercury control activated carbon is: active carbon is mixed being placed in the airtight container with sulphur, kept 2~24 hours down at 120~300 ℃.
The mass ratio of active carbon and sulphur is 1: 0.02 to 1: 0.6.
The specific area of active carbon is 200m 2/ g is to 1300m 2/ g.
Those of ordinary skills can pass through simple experiment, determine the reasonable volume of described closed container.
The present invention utilizes the sublimability and the low polarity of sulphur dexterously, heats in closed container, and sulphur directly enters in the active carbon hole, invests in the active carbon hole, enters in the active carbon hole when containing mercury gas, and mercury is caught by sulphur, forms mercuric sulphide.Technology of the present invention is simple, and cost is low, soaks the sulfur content height, so demercuration efficient height, and is all better than above-mentioned all methods before, and can easily reclaim mercuric sulphide.
The specific embodiment
The present invention is described in detail below in conjunction with embodiment.Wherein soak sulfur content and make sulphur become SO2, be transformed into H2SO3 again,, measure sulfur content with the titration of standard iodine solution with firing method; Mercury content adopts the coal-fired flue-gas mercury vapourmeter of Suzhou high official position instrument plant to measure.Except that particularly pointing out, the specific area of used basic active carbon is 1100m 2/ g.
Embodiment 1
Take by weighing basic active carbon 30g, add 11g sulphur, under solid state, mix, be heated to 200 ℃ and kept 4 hours, obtain the sulfur leaching mercury control activated carbon product, record that to soak sulfur content be 23.8%.
Embodiment 2
Take by weighing basic active carbon 300g, add 90g sulphur, under solid state, mix, be heated to 180 ℃ and kept 8 hours, obtain the sulfur leaching mercury control activated carbon product, record that to soak sulfur content be 20.0%.
Embodiment 3
Take by weighing basic active carbon 3000g, add 600g sulphur, under solid state, mix, be heated to 190 ℃ and kept 10 hours, obtain the sulfur leaching mercury control activated carbon product, record that to soak sulfur content be 15.0%.
Embodiment 4
Take by weighing basic active carbon 6000g, add 800g sulphur, under solid state, mix, be heated to 220 ℃ and kept 20 hours, obtain the sulfur leaching mercury control activated carbon product, record that to soak sulfur content be 9.0%.
Embodiment 5
Take by weighing basic active carbon 7000g, add 900g sulphur, under solid state, mix, be heated to 250 ℃ and kept 20 hours, obtain the sulfur leaching mercury control activated carbon product, record that to soak sulfur content be 8.35%.
Embodiment 6
Take by weighing basic active carbon 100g, add 4g sulphur, under solid state, mix, be heated to 300 ℃ and kept 20 hours, obtain the sulfur leaching mercury control activated carbon product, record that to soak sulfur content be 2.0%.
Embodiment 7
Take by weighing basic active carbon 600g and add 100g sulphur again, mix under solid state, be heated to 200 ℃ and kept 20 hours, soaking sulfur content is 10%.
Embodiment 8
Taking by weighing specific area is 200m 2/ g active carbon 100g adds 2g sulphur, mixes under solid state, is heated to 130 ℃ and keeps 4 hours, obtains the sulfur leaching mercury control activated carbon product, records that to soak sulfur content be 0.2%.
Embodiment 9
Taking by weighing specific area is 500m 2/ g active carbon 100g adds 3g sulphur, mixes under solid state, is heated to 150 ℃ and keeps 6 hours, obtains the sulfur leaching mercury control activated carbon product, records that to soak sulfur content be 0.5%.
Embodiment 10
Taking by weighing specific area is 800m 2/ g active carbon 100g adds 5g sulphur, mixes under solid state, is heated to 160 ℃ and keeps 7 hours, obtains the sulfur leaching mercury control activated carbon product, records that to soak sulfur content be 1.0%.
Embodiment 11
Taking by weighing specific area is 1300m 2/ g active carbon 300g adds 90g sulphur, mixes under solid state, is heated to 150 ℃ and keeps 6 hours, obtains the sulfur leaching mercury control activated carbon product, records that to soak sulfur content be 21%.
Application Example 1
Gained sulfur leaching mercury control activated carbon product of the present invention and basic active carbon are carried out following test respectively:
Get the 100mg active carbon, place in the absorber of coal-fired flue-gas mercury vapourmeter,, when exit concentration is 0.003mg/m3, test the mercury adsorbance when inlet mercury concentration is 243.5mg/m3.Test result is shown in Table 1.
Application Example 2
Gained sulfur leaching mercury control activated carbon product of the present invention and basic active carbon are carried out following test respectively:
Get the 100mg active carbon, place in the absorber of coal-fired flue-gas mercury vapourmeter,, when exit concentration is 0.003mg/m3, test the mercury adsorbance when inlet mercury concentration is 62.5mg/m3.Test result is shown in Table 2.
By table 1 and table 2 as can be seen, gained sulfur leaching mercury control activated carbon product of the present invention improves greatly with respect to the mercury adsorption efficiency of basic active carbon.This be because, adopt the present invention, can effectively sulphur be invested in the active carbon space, handle when containing mercury gas, effect is very good.
Table 1
Active carbon The mercury adsorbance
The basis active carbon 3.83mg/100%
Embodiment 4 34.5mg/900%
Table 2
Active carbon The mercury adsorbance
The basis active carbon 4.01mg/100%
Embodiment 1 87.4mg/2180%
Embodiment 2 79.0mg/1970%
Embodiment 3 54.1mg/1349%
Embodiment 5 35.1mg/875%
Embodiment 6 9.1mg/227%

Claims (3)

1, a kind of preparation method of sulfur leaching mercury control activated carbon is characterized in that active carbon mixed with sulphur being placed in the closed container, keeps 2~24 hours down at 120~300 ℃.
2, the preparation method of sulfur leaching mercury control activated carbon as claimed in claim 1, the mass ratio that it is characterized in that active carbon and sulphur is 1: 0.02 to 1: 0.6.
3, the preparation method of sulfur leaching mercury control activated carbon as claimed in claim 1 or 2, the specific area that it is characterized in that active carbon is 200m 2/ g is to 1300m 2/ g.
CNA2009100249314A 2009-02-27 2009-02-27 Method of preparing sulfur leaching mercury control activated carbon Pending CN101513605A (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101844074A (en) * 2010-05-20 2010-09-29 宁夏华辉活性炭股份有限公司 Method for preparing activated carbon used for flue gas demercuration
CN102078797A (en) * 2010-12-16 2011-06-01 浙江天蓝环保技术有限公司 Modified magnetic catalyst for demercuration of flue gas as well as preparation method and application thereof
CN102247823A (en) * 2011-04-29 2011-11-23 叶向荣 Preparation method of sulfurizing porous nanometer material for high-efficiency hydrargyrum removal
CN103977763A (en) * 2014-06-04 2014-08-13 武汉市天虹仪表有限责任公司 Preparation method of efficient adsorbent for gaseous mercury sampling
CN104014304A (en) * 2013-12-04 2014-09-03 中国科学院过程工程研究所 Nitric acid modified activated carbon adsorbent for demercuration of flue gas, and preparation method and application thereof
CN105921107A (en) * 2016-05-18 2016-09-07 天津普瑞特净化技术有限公司 Active-carbon composite mercury removing agent and preparing technology thereof
CN106237985A (en) * 2016-08-16 2016-12-21 四川师范大学 A kind of straw base selectivity removal of mercury material and its preparation method and application
CN106914215A (en) * 2015-12-28 2017-07-04 沈阳中科环境工程科技开发有限公司 Modified dipping sulfur molecule sieve mercury removal agent of one kind and preparation method thereof and special purpose device
CN106996884A (en) * 2017-02-27 2017-08-01 深圳中物安防科技有限公司 A kind of explosive gas phase detecting devices verification product and preparation method thereof
CN109799322A (en) * 2019-03-12 2019-05-24 中国华能集团清洁能源技术研究院有限公司 A kind of multifunctional coal gasification experiment test device
CN112642413A (en) * 2020-12-10 2021-04-13 北京清新环境技术股份有限公司 Preparation method and product of mercury removal adsorbent based on active coke
CN115318248A (en) * 2022-08-19 2022-11-11 宁夏华辉环保科技股份有限公司 Accurate temperature-control sulfur-carrying activated carbon and preparation method thereof

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101844074B (en) * 2010-05-20 2012-06-27 宁夏华辉活性炭股份有限公司 Method for preparing activated carbon used for flue gas demercuration
CN101844074A (en) * 2010-05-20 2010-09-29 宁夏华辉活性炭股份有限公司 Method for preparing activated carbon used for flue gas demercuration
CN102078797A (en) * 2010-12-16 2011-06-01 浙江天蓝环保技术有限公司 Modified magnetic catalyst for demercuration of flue gas as well as preparation method and application thereof
CN102247823A (en) * 2011-04-29 2011-11-23 叶向荣 Preparation method of sulfurizing porous nanometer material for high-efficiency hydrargyrum removal
CN102247823B (en) * 2011-04-29 2012-12-19 叶向荣 Preparation method of sulfurizing porous nanometer material for high-efficiency hydrargyrum removal
CN104014304A (en) * 2013-12-04 2014-09-03 中国科学院过程工程研究所 Nitric acid modified activated carbon adsorbent for demercuration of flue gas, and preparation method and application thereof
CN103977763A (en) * 2014-06-04 2014-08-13 武汉市天虹仪表有限责任公司 Preparation method of efficient adsorbent for gaseous mercury sampling
CN103977763B (en) * 2014-06-04 2016-03-16 武汉市天虹仪表有限责任公司 A kind of preparation method of the high-efficiency adsorbent for gaseous mercury sampling
CN106914215A (en) * 2015-12-28 2017-07-04 沈阳中科环境工程科技开发有限公司 Modified dipping sulfur molecule sieve mercury removal agent of one kind and preparation method thereof and special purpose device
CN105921107A (en) * 2016-05-18 2016-09-07 天津普瑞特净化技术有限公司 Active-carbon composite mercury removing agent and preparing technology thereof
CN106237985A (en) * 2016-08-16 2016-12-21 四川师范大学 A kind of straw base selectivity removal of mercury material and its preparation method and application
CN106237985B (en) * 2016-08-16 2018-08-31 四川师范大学 A kind of stalk based selective removal of mercury material and its preparation method and application
CN106996884A (en) * 2017-02-27 2017-08-01 深圳中物安防科技有限公司 A kind of explosive gas phase detecting devices verification product and preparation method thereof
CN109799322A (en) * 2019-03-12 2019-05-24 中国华能集团清洁能源技术研究院有限公司 A kind of multifunctional coal gasification experiment test device
CN112642413A (en) * 2020-12-10 2021-04-13 北京清新环境技术股份有限公司 Preparation method and product of mercury removal adsorbent based on active coke
CN115318248A (en) * 2022-08-19 2022-11-11 宁夏华辉环保科技股份有限公司 Accurate temperature-control sulfur-carrying activated carbon and preparation method thereof

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Open date: 20090826