CN103816861B - The preparation method of attapulgite clay desulfurizing agent - Google Patents
The preparation method of attapulgite clay desulfurizing agent Download PDFInfo
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- CN103816861B CN103816861B CN201410102041.1A CN201410102041A CN103816861B CN 103816861 B CN103816861 B CN 103816861B CN 201410102041 A CN201410102041 A CN 201410102041A CN 103816861 B CN103816861 B CN 103816861B
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Abstract
The invention discloses the preparation method of the low attapulgite clay desulfurizing agent of a kind of desulphurization cost, comprise the steps: preparation 3% ~ 20% hydrochloric acid, get 30g attapulgite clay, mix by the ratio of solid-liquid mass ratio 1:3 ~ 1:5, soak 20 ~ 40 hours, microwave treatment 10 ~ 20 minutes, be washed with distilled water to PH=6 ~ 7 sedimentation, carry out suction filtration after removing upper liquid and obtain filter cake, filter cake is dried at 100 ~ 120 DEG C, be cooled to room temperature, dry cake is worn into 100 ~ 120 object powder, obtain modified attapulgite clay, by the modified attapulgite clay that obtains and active component Homogeneous phase mixing, adding appropriate distilled water makes clay and active component bind, and use tablet press machine granulation, activate under being placed in muffle furnace 500 ~ 700 DEG C of temperature again, make attapulgite clay desulfurizing agent finished product.Advantage is: utilize desulfurizing agent prepared by above-mentioned preparation method, and renewable use is with low cost, adsorption capacity, and desulfuration efficiency can reach more than 80%, effectively can remove the sulfide in gasoline and diesel oil.
Description
Technical field
The present invention relates to a kind of preparation method of desulfurizing agent, be related specifically to a kind of preparation method of attapulgite clay desulfurizing agent.
Background technology
The SOx that gasoline and the burning of diesel oil medium sulphide content generate is one of major pollutants, causes countries in the world extensive concern.At present, European and American developed countries to the sulfur content of vapour, diesel oil all to carry out strict restriction wherein sulfur in gasoline mass fraction be limited in 30 below μ g/g.Current desulfur technology is varied, respectively has its pluses and minuses.Hydrodesulfurization (HDS) is the effective technology removing sulphur from various petroleum distillate, greatly can reduce sulfur content, but it needs dedicated catalyst and high temperature, high-pressure process, equipment investment and operating cost high.About research existing more than the 50 year history so far of biological desulphurization, but until late 1980s, Kilbane has found can after the microorganism of selective fracture C-S key, biocatalytic desulfurization is just made to enter fast-developing period, but as a complete unit, it remains a developing technology.Non-hydrodesulfurization has advantage simply, easily and fast due to it, will be one of the dominant technology of 21 century gasoline desulfur.At present, adsorption desulfurizing agent is mainly with X-type molecular sieve, Y zeolite, Al
2o
3deng being carrier, adopting the preparation of the method such as Metal Supported, ion-exchange and obtaining, object improves its adsorption capacity and desulfuration selectivity.Existing adsorption desulfurizing agent is used for removing gasoline and diesel oil medium sulphide content cost is larger.
Summary of the invention
Technical problem to be solved by this invention is: the preparation method of the attapulgite clay desulfurizing agent providing a kind of desulphurization cost low.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: the preparation method of attapulgite clay desulfurizing agent, comprise the steps: preparation 3% ~ 20% hydrochloric acid, get 30g attapulgite clay, mix by the ratio of solid-liquid mass ratio 1:3 ~ 1:5, soak 20 ~ 40 hours, microwave treatment 10 ~ 20 minutes, be washed with distilled water to PH=6 ~ 7 sedimentation, carry out suction filtration after removing upper liquid and obtain filter cake, filter cake is dried at 100 ~ 120 DEG C, be cooled to room temperature, dry cake is worn into 100 ~ 120 object powder, obtain modified attapulgite clay, by the modified attapulgite clay that obtains and active component Homogeneous phase mixing, adding appropriate distilled water makes clay and active component bind, and use tablet press machine granulation, activate under being placed in muffle furnace 500 ~ 700 DEG C of temperature again, make attapulgite clay desulfurizing agent finished product.
In order to solve the problems of the technologies described above better, the further technical scheme that the present invention adopts is: described active component is iron oxide or titanium oxide.
In order to solve the problems of the technologies described above better, the further technical scheme that the present invention adopts is: described active component and the mixed proportion of modified attapulgite clay are 1:19.
Advantage of the present invention is: the preparation method technique of above-mentioned attapulgite clay desulfurizing agent is simple, utilizes desulfurizing agent prepared by above-mentioned preparation method, renewable use, with low cost, adsorption capacity, desulfuration efficiency can reach more than 80%, effectively can remove the sulfide in gasoline and diesel oil.
Detailed description of the invention
Particular content of the present invention is described in detail below by specific embodiment.
The preparation method of attapulgite clay desulfurizing agent, comprise the steps: preparation 3% ~ 20% hydrochloric acid, get 30g attapulgite clay, mix by the ratio of solid-liquid mass ratio 1:3 ~ 1:5, soak 20 ~ 40 hours, microwave treatment 10 ~ 20 minutes, be washed with distilled water to PH=6 ~ 7 sedimentation, carry out suction filtration after removing upper liquid and obtain filter cake, filter cake is dried at 100 ~ 120 DEG C, be cooled to room temperature, dry cake is worn into 100 ~ 120 object powder, obtain modified attapulgite clay, by the modified attapulgite clay that obtains and active component Homogeneous phase mixing, adding appropriate distilled water makes clay and active component bind, and use tablet press machine granulation, activate under being placed in muffle furnace 500 ~ 700 DEG C of temperature again, make attapulgite clay desulfurizing agent finished product.Described active component is iron oxide or titanium oxide.Described active component and the mixed proportion of modified attapulgite clay are 1:19.
Embodiment 1:
The preparation method of attapulgite clay desulfurizing agent, comprise the steps: preparation 3% hydrochloric acid, get 30g attapulgite clay, mix by the ratio of solid-liquid mass ratio 1:3, soak 20 hours, microwave treatment 10 minutes, be washed with distilled water to PH=7 sedimentation, carry out suction filtration after removing upper liquid and obtain filter cake, filter cake is dried at 120 DEG C, be cooled to room temperature, dry cake is worn into 120 object powder, obtain modified attapulgite clay, the modified attapulgite clay obtained is mixed with the ratio uniform of 19:1 with active component iron oxide, adding appropriate distilled water makes clay and active component bind, and use tablet press machine granulation, activate under being placed in muffle furnace 500 DEG C of temperature again, make attapulgite clay desulfurizing agent finished product.
Embodiment 2:
The preparation method of attapulgite clay desulfurizing agent, comprise the steps: preparation 10% hydrochloric acid, get 30g attapulgite clay, mix by the ratio of solid-liquid mass ratio 1:4, soak 40 hours, microwave treatment 20 minutes, be washed with distilled water to PH=6 sedimentation, carry out suction filtration after removing upper liquid and obtain filter cake, filter cake is dried at 100 DEG C, be cooled to room temperature, dry cake is worn into 100 object powder, obtain modified attapulgite clay, the modified attapulgite clay obtained is mixed with the ratio uniform of 19:1 with active component iron oxide, adding appropriate distilled water makes clay and active component bind, and use tablet press machine granulation, activate under being placed in muffle furnace 600 DEG C of temperature again, make attapulgite clay desulfurizing agent finished product.
Embodiment 3:
The preparation method of attapulgite clay desulfurizing agent, comprise the steps: preparation 15% hydrochloric acid, get 30g attapulgite clay, mix by the ratio of solid-liquid mass ratio 1:5, soak 30 hours, microwave treatment 15 minutes, be washed with distilled water to PH=7 sedimentation, carry out suction filtration after removing upper liquid and obtain filter cake, filter cake is dried at 110 DEG C, be cooled to room temperature, dry cake is worn into 110 object powder, obtain modified attapulgite clay, the modified attapulgite clay obtained is mixed with the ratio uniform of 19:1 with active component titanium oxide, adding appropriate distilled water makes clay and active component bind, and use tablet press machine granulation, activate under being placed in muffle furnace 700 DEG C of temperature again, make attapulgite clay desulfurizing agent finished product.
Embodiment 4:
The preparation method of attapulgite clay desulfurizing agent, comprise the steps: preparation 20% hydrochloric acid, get 30g attapulgite clay, mix by the ratio of solid-liquid mass ratio 1:5, soak 40 hours, microwave treatment 18 minutes, be washed with distilled water to PH=7 sedimentation, carry out suction filtration after removing upper liquid and obtain filter cake, filter cake is dried at 100 DEG C, be cooled to room temperature, dry cake is worn into 120 object powder, obtain modified attapulgite clay, the modified attapulgite clay obtained is mixed with the ratio uniform of 19:1 with active component titanium oxide, adding appropriate distilled water makes clay and active component bind, and use tablet press machine granulation, activate under being placed in muffle furnace 700 DEG C of temperature again, make attapulgite clay desulfurizing agent finished product.
Claims (1)
1. the preparation method of attapulgite clay desulfurizing agent, is characterized in that: comprise the steps: preparation 3% ~
10% hydrochloric acid, gets 30g attapulgite clay, mixes by the ratio of solid-liquid mass ratio 1:3 ~ 1:4, soaks 20 ~ 40
Hour, microwave treatment 10 ~ 20 minutes, is washed with distilled water to pH=6 ~ 7 sedimentation, carries out after removing upper liquid
Suction filtration obtains filter cake, is dried by filter cake, is cooled to room temperature, dry cake is worn into 100 ~ 120 orders at 100 ~ 120 DEG C
Powder, obtain modified attapulgite clay, by the modified attapulgite clay that obtains and active component Homogeneous phase mixing,
Adding appropriate distilled water makes clay and active component bind, and uses tablet press machine granulation, then is placed in muffle furnace
Activate at 500 ~ 600 DEG C of temperature, make attapulgite clay desulfurizing agent finished product;
Described active component is iron oxide;
Described active component and the mixed proportion of modified attapulgite clay are 1:19.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104109012A (en) * | 2014-07-22 | 2014-10-22 | 肥东县丰宝种养殖有限责任公司 | Shii-take culture medium with mushroom dreg as raw material and preparation method of shii-take |
| CN105435736A (en) * | 2015-12-04 | 2016-03-30 | 盐城市兰丰环境工程科技有限公司 | Method for preparing modified attapulgite sulfur-transfer additive |
| CN106732592A (en) * | 2016-12-14 | 2017-05-31 | 湘潭大学 | A kind of method that the method for modifying and microwave irradiation of sepiolite prepare Cu sepiolites |
| CN108176385A (en) * | 2018-01-26 | 2018-06-19 | 山东星火科学技术研究院 | A kind of gasoline desulfurizer |
Citations (3)
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| CN1039139A (en) * | 1989-06-29 | 1990-01-24 | 谢两雄 | The mark printing method of baling strips |
| CN102059115A (en) * | 2010-12-20 | 2011-05-18 | 上海纳米技术及应用国家工程研究中心有限公司 | CO normal-temperature catalytic oxidation catalyst and preparation method thereof |
| CN102874826A (en) * | 2012-10-18 | 2013-01-16 | 南京信息工程大学 | Purification technical method for attapulgite clay |
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| ES2401799B1 (en) * | 2011-08-08 | 2014-06-03 | Acciona Infraestructuras, S.A. | PROCEDURE FOR THE PREPARATION OF AN ADDITIVE THAT INCLUDES SUPPORTED AND DISPERSED TIO2 PARTICLES |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039139A (en) * | 1989-06-29 | 1990-01-24 | 谢两雄 | The mark printing method of baling strips |
| CN102059115A (en) * | 2010-12-20 | 2011-05-18 | 上海纳米技术及应用国家工程研究中心有限公司 | CO normal-temperature catalytic oxidation catalyst and preparation method thereof |
| CN102874826A (en) * | 2012-10-18 | 2013-01-16 | 南京信息工程大学 | Purification technical method for attapulgite clay |
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| Title |
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| Dynamic Adsorption of Microwave Modified Attapulgite on Micro-polluted Phenol Wastewater;Chunsheng LEI et al.;《Resources and Environment》;20121231;第13卷(第11期);第2385-2388页 * |
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