CN1234808C - Desulfate adsorbing agent for deep purifying sulfide in fuel oil and preparation process thereof - Google Patents
Desulfate adsorbing agent for deep purifying sulfide in fuel oil and preparation process thereof Download PDFInfo
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- CN1234808C CN1234808C CN 200410018733 CN200410018733A CN1234808C CN 1234808 C CN1234808 C CN 1234808C CN 200410018733 CN200410018733 CN 200410018733 CN 200410018733 A CN200410018733 A CN 200410018733A CN 1234808 C CN1234808 C CN 1234808C
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- hydrotalcite
- polynite
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- sulfide
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Abstract
The present invention relates to a devulcanization adsorbent used for the deep purification of sulfide in fuel oil and a preparation method thereof, which belongs to the technology for the purification of impurities in fuel oil. The adsorbent selects montmorillonite or hydrotalcite or other pillared compounds as a raw material which is prepared into the powder of montmorillonite or hydrotalcite or other pillared compounds by the technologies of layer assembly and interfacial assembly. The process of the preparation method comprises: selecting montmorillonite or hydrotalcite; preparing the adsorbent by the interfacial assembly technology combined with a plasma technology and a microwave irradiation technology. The present invention has the advantages that the adsorbent can be used at room temperature, and has good use effect and the function of deeply purifying sulfide in fuel oil.
Description
Technical field
The present invention relates to a kind of desulfuration adsorbent that is used for oil fuel sulfide deep purifying and preparation method thereof, belong to fuel well cuts purification techniques.
Background technology
The sulfur-containing oxide that sulfurous fuels burning back forms causes topsoil such as acid rain human beings'health and development all to be caused great threat, and for this reason, the U.S., Europe, Japan etc. have proposed the rules of deep desulfuration production " clean fuel ".Reach the expection desulfurization level, present production equipment need enlarge 5-15 doubly, therefore, the complicated organosulfur compound that is difficult to remove at the HDS method such as thiophene phenol, dibenzo thiophene phenol etc. especially condensed ring class sulfocompound carry out deep desulfuration " green " technology---the adsorption desulfurize method causes people's common concern.Many scholars carried out adopt modified zeolite, solid adsorbent, porous polymer, etc. the research of absorption sulfide, these materials have good adsorption to sulfide in the oil fuel.
Summary of the invention
The object of the present invention is to provide a kind of desulfuration adsorbent that is used for deep purifying oil fuel sulfide and preparation method thereof.Described desulfuration adsorbent adsorbs sulfide at ambient temperature in non-aqueous system, with sulfide absorption in the oil fuel and reach the purification purpose, the preparation method is simple.
The present invention is realized by following technical proposals.A kind of preparation method who is used for the desulfuration adsorbent of deep purifying oil fuel sulfide, described desulfuration adsorbent is polynite or hydrotalcite layer-pillared compound powder, its preparation process comprises selects polynite or hydrotalcite, utilize plasma technique and microwave irradiation technology, it is characterized in that comprising the following steps:
1.TiCl
4Be dissolved in the HCl solution of 0.1-5mol/L concentration, then through diluting to such an extent that contain the pillaring solution that Ti concentration is 0.4-0.9mol/L.
2. polynite or hydrotalcite are according to the ratio formulated suspension of quality 1%-5%, pillaring solution slowly is added dropwise to institute joins in the suspension, stir while dripping, after stirring end, suspension is placed pressure vessel, under 0-5MPa pressure and 10-180 ℃ of temperature condition, left standstill 0-48 hour respectively, leach then, under 100-120 ℃ of condition, dry.
3. sample is placed muffle furnace, any under room temperature-860 ℃ condition or the heating of a plurality of temperature range 1-5 hour, furnace cooling.
4. polynite or the hydrotalcite with roasting is immersed in respectively under room temperature in ammonium copper sulfate solution, silver nitrate solution, cerous nitrate solution or the gadolinium oxide solution of 0.01mol/L-0.5mol/L, soaked 1-48 hour, filter and take out, sample was placed low-temperature plasma 1-60 minute.
5. above sample was shone 1-60 minute oven dry under the microwave of 370W.
6. polynite that step 5 is obtained or hydrotalcite place muffle furnace to heat 1-8 hour down in 300-400 ℃, make desulfuration adsorbent.
If set by step in 4 with being dipped in the silver nitrate solution of polynite or hydrotalcite, add quality 5-10% formaldehyde, soaks after 1-48 hour,, left standstill 5 hours in 70-90 ℃ of following lucifuge, filter and take out, oven dry gets the argentiferous desulfuration adsorbent.
The invention has the advantages that can use at ambient temperature, result of use is good, have function sulfide deep purifying in the oil fuel.
Embodiment
Embodiment 1:
TiCl just
4Be dissolved in the HCl solution of 3mol/L, then through diluting to such an extent that Ti concentration is 0.86mol/L; HCl concentration is the pillaring solution of 0.7mol/L, in Ti/ polynite=20meq/g or in Ti/ hydrotalcite=20meq/g ratio pillaring solution is slowly dripped in 2% (wt) polynite or hydrotalcite suspension that are made under constantly stirring, after stirring, leave standstill 12h, solid-liquid separation again, simultaneously with distilled water wash for several times to not having the Cl ion and in 100 ℃ of oven dry down.At last in 600 ℃-650 ℃ following calcining 5h, through grind the titanium pillared montmorillonite, titanium pillared montmorillonite or the titanium pillared hydrotalcite concentration with 4% (wt) is immersed in respectively in the ammonium copper sulfate solution of 0.1mol/L, leave standstill 12h after, filtering, dry in 100 ℃.Result of study shows that desulfuration adsorbent has good adsorption effect to sulfide in the oil fuel.
Embodiment 2:
With TiCl
4Be dissolved in the HCl solution of 3mol/L, then through diluting to such an extent that Ti concentration is 0.86mol/L; HCl concentration is the pillaring solution of 0.7mol/L, in Ti/ polynite=20meq/g or in Ti/ hydrotalcite=20meq/g ratio pillaring solution is slowly dripped in 2% (wt) polynite or hydrotalcite suspension that are made under constantly stirring, after stirring, leave standstill 12h, solid-liquid separation again, simultaneously with distilled water wash for several times to not having the Cl ion and in 100 ℃ of oven dry down.Calcine 5h down in 600 ℃-650 ℃ at last, through grind titanium pillared montmorillonite or titanium pillared hydrotalcite, titanium pillared montmorillonite or the titanium pillared hydrotalcite concentration with 4% (wt) is immersed in respectively in the silver nitrate solution of 0.1mol/L, after leaving standstill 12h, filtering, in 370 watts of microwave oven internal radiations 10 minutes.Result of study shows that desulfuration adsorbent has good adsorption effect to sulfide in the oil fuel.
Claims (1)
1, a kind of preparation method who is used for the desulfuration adsorbent of deep purifying oil fuel sulfide, described desulfuration adsorbent is polynite or hydrotalcite layer-pillared compound powder, its preparation process comprises selects polynite or hydrotalcite, utilize plasma technique and microwave irradiation technology, it is characterized in that comprising the following steps:
(1) with TiCl
4Be dissolved in the HCl solution of 0.1-5mol/L concentration, then through diluting to such an extent that contain the pillaring solution that Ti concentration is 0.4-0.9mol/L;
(2) with polynite or hydrotalcite ratio formulated suspension according to quality 1-5%, pillaring solution slowly is added dropwise to institute joins in the suspension, stir while dripping, after stirring end, suspension is placed pressure vessel, under 0-5MPa pressure and 10-180 ℃ of temperature condition, left standstill 0-48 hour respectively, leach then, under 100-120 ℃ of condition, dry;
(3) sample is placed muffle furnace, any under room temperature-860 ℃ condition or the heating of a plurality of temperature range 1-5 hour, furnace cooling;
(4) polynite or the hydrotalcite with roasting is immersed in respectively under room temperature in ammonium copper sulfate solution, silver nitrate solution, cerous nitrate solution or the gadolinium oxide solution of 0.01mol/L-0.5mol/L, soaked 1-48 hour, filter and take out, sample was placed low-temperature plasma 1-60 minute;
(5) above sample was shone 1-60 minute oven dry under the microwave of 370W;
(6) polynite that step (5) is obtained or hydrotalcite place muffle furnace to heat 1-8 hour down in 300-400 ℃, make desulfuration adsorbent;
(7) if in (4) polynite or hydrotalcite are dipped in the silver nitrate solution set by step, add quality 5-10% formaldehyde, soak after 1-48 hour, left standstill 5 hours in 70-90 ℃ of following lucifuge, to filter and take out, oven dry gets the argentiferous desulfuration adsorbent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410018733 CN1234808C (en) | 2004-03-11 | 2004-03-11 | Desulfate adsorbing agent for deep purifying sulfide in fuel oil and preparation process thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410018733 CN1234808C (en) | 2004-03-11 | 2004-03-11 | Desulfate adsorbing agent for deep purifying sulfide in fuel oil and preparation process thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1560199A CN1560199A (en) | 2005-01-05 |
| CN1234808C true CN1234808C (en) | 2006-01-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200410018733 Expired - Fee Related CN1234808C (en) | 2004-03-11 | 2004-03-11 | Desulfate adsorbing agent for deep purifying sulfide in fuel oil and preparation process thereof |
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| CN (1) | CN1234808C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100382886C (en) * | 2005-05-26 | 2008-04-23 | 天津大学 | Adsorption material for removing copper and lead from plant medicine and preparation method thereof |
| CN103084147B (en) * | 2011-11-08 | 2015-02-25 | 纳科石油化工有限公司 | Iron oxide magnetic nano particle, preparation method and application method thereof in desulfurization |
| CN103381353B (en) * | 2013-07-17 | 2015-07-08 | 常州大学盱眙凹土研发中心 | Preparation method of clay base gasoline desulfurization adsorbent |
| CN105709750B (en) * | 2014-12-04 | 2018-01-16 | 中国石油化工股份有限公司 | A kind of copper pillared montmorillonite catalyst and its preparation method and application |
| CN110813313B (en) * | 2019-11-11 | 2022-03-04 | 安徽理工大学 | Silver oxide/layered double-metal hydroxide compound and preparation and application thereof |
| CN112391193B (en) * | 2020-11-12 | 2022-07-08 | 大连大学 | Method for adsorbing and removing dibenzothiophene |
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2004
- 2004-03-11 CN CN 200410018733 patent/CN1234808C/en not_active Expired - Fee Related
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