CN104560251B - Cleaning agent and use thereof - Google Patents
Cleaning agent and use thereof Download PDFInfo
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- CN104560251B CN104560251B CN201310512758.9A CN201310512758A CN104560251B CN 104560251 B CN104560251 B CN 104560251B CN 201310512758 A CN201310512758 A CN 201310512758A CN 104560251 B CN104560251 B CN 104560251B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
The invention relates to a cleaning agent and a use thereof. The cleaning agent is mainly used for solving the problems of high bulk density, low utilization rate and high industrial application cost of the cleaning agent in the prior art. The problems are well solved by use of the following technical scheme: the cleaning agent is prepared from the following components in percentage by weight: a) 20-95% of aurichalcite, and b) 5-80% of binder; and the cleaning agent can be applied to cleaning raw materials such as natural gas, synthetic gases, light gaseous/liquid hydrocarbons.
Description
Technical field
The present invention relates to a kind of cleanser and application thereof.
Background technology
The impurity such as sulfur, arsenic are widely present in the raw materials such as natural gas, synthesis gas, coal gas, lightweight liquid state hydro carbons, these are miscellaneous
The presence of matter can cause many catalyst poisoning inactivations, greatly shorten catalyst life, and even resulting in catalytic reaction cannot be normal
Carry out；Additionally, do not remove clean sulfur arsenic impurities can be a series of so as to bring as what is produced entering to be advanced in the composite of downstream
The aspect such as Environmental Health problem.Therefore, impurity the sponsoring for protection downstream unit such as high-efficiency high-accuracy ground removing sulfur arsenic
Agent and while improve downstream product quality have very important meaning.
Generally, the sulphur-containing substance present in the raw material of industry is mainly H2S and COS, for these sulphur-containing substances
Deep removal effect most preferably Zinc oxide desulfurizer.Zinc oxide desulfurization with its desulfurization precision it is high, easy to use, it is safe can
By, sulfur capacity it is high, play " checking on " and " protection " effect and occupy very important status, it be widely applied to synthesis ammonia,
The industries such as hydrogen manufacturing, Coal Chemical Industry, petroleum refinement, beverage production, to remove natural gas, petroleum distillate, casing-head gas, refinery gas, synthesis
Hydrogen sulfide and some organic sulfurs in the raw materials such as gas, carbon dioxide.Sulfur in unstripped gas can be removed to by zinc sulfide desulfurization
0.055mg/kg.Add CuO in normal temp zinc oxide desulfuriging agent to improve its desulphurizing ability.Zinc oxide desulfurizer is generally used for loss of essence
Sulfur process, it can also absorb general organosulfur compound.Arsenic impurities in the raw material of industry, generally with AsH3Form is present, work
The Hydrodearsenic Catalyst used in industry is substantially divided into copper system, lead system, four class of manganese systems and nickel system, wherein relatively conventional with copper system.Copper system takes off
Arsenical arsenic holds height, can carry out under room temperature, normal pressure and higher space velocity.Copper system Hydrodearsenic Catalyst is divided into metallic copper, CuO-Al again2O3、
CuO-ZnO-Al2O3Deng.When with CuO as active component, AsH3By Cu2+Low price or metallic state are reduced to, arsenic is combined with copper or swum
From into element state.The development trend of desulfurizing agent and Hydrodearsenic Catalyst be to low bulk density, low use temperature, high intensity and high sulfur capacity and
The direction that arsenic holds is developed.
Patent CN101591554A discloses a kind of room temperature composite sulfur arsenic cleanser and preparation method thereof, the sulfur arsenic cleanser
It is made up of carrier and active component, active component is lead oxide, magnetic iron oxide and copper oxide, and carrier is γ-Al2O3, the sulfur arsenic
Cleanser needs to activate 4 ~ 8 hours at 350 ~ 650 DEG C, can be seen that the oxide sulfur arsenic from its composition and preparation method and purifies
Agent heap density is high, and preparation process is complicated, and commercial Application is relatively costly.
Patent CN102049236A discloses a kind of copper zinc ambient temperature desulfuration agent and preparation method thereof, and the desulfurizing agent is by alkali formula
Zinc carbonate, basic copper carbonate and binding agent composition, the preparation of the desulfurization sulfur agent is by commercially available basic zinc carbonate, basic carbonate
Copper, binding agent and water carry out mediating, molding, obtain after drying, and the desulfurizing agent is obtained by physical mixed, thus zinc-copper therein
Active component cannot play synergism, so as to cause its Sulfur capacity relatively low.
The content of the invention
The technical problem to be solved is that cleanser heap density is high in prior art, and utilization rate is low, commercial Application
A kind of relatively costly problem, there is provided new cleanser.The cleanser is for natural gas, synthesis gas, lightweight liquid state hydro carbons
Deng purification in when, low with heap density, utilization rate is high, commercial Application low cost advantage.
To solve above-mentioned technical problem, the technical solution used in the present invention is as follows：A kind of cleanser, with percentage by weight
Meter, including following components：A) 20 ~ 95% aurichalcite；B) 5 ~ 80% binding agent.
In above-mentioned technical proposal, in terms of cleanser percentage by weight, the preferred scope of aurichalcite is 35 ~ 65%；To purify
Agent percentage by weight meter, the preferred scope of binding agent is 15 ~ 35%；The binding agent is aluminium oxide, silicon oxide, alumina cement, fibre
At least one in dimension element, Kaolin, attapulgite, aluminosilicate cement, preferred aluminium oxide.
In above-mentioned technical proposal, it is preferable that the heap density of cleanser is less than 0.9kg/m3；
In above-mentioned technical proposal, it is preferable that the side pressure strength of cleanser is more than 70N/ grains.
In above-mentioned technical proposal, it is preferable that in terms of cleanser percentage by weight, cleanser is also comprising 7～23% ZnO and 8
~ 22 CuO.
In above-mentioned technical proposal, the preparation method of the cleanser is comprised the following steps successively：
(1) by copper nitrate, zinc nitrate, the water-soluble inorganic salt of aluminum nitrate and hydromassage, your ratio is counted：Cu/Zn is 0.1 ~ 2,；
Al/Zn is 0 ~ 0.7；(Cu+Zn+Al)/H2O mixes for 0.01 ~ 0.04 ratio, is uniformly mixing to obtain solution I；
(2) by least one and hydromassage that in sodium carbonate, sodium bicarbonate, ammonium carbonate than the ratio for 0.01 ~ 0.04
Mixing, is uniformly mixing to obtain solution II；
(3) by solution I and II mix homogeneously, at 40 ~ 90 DEG C, reaction obtains precipitate in 0.5 ~ 3 hour, will be precipitate washing dry
It is dry；
(4) precipitate, binding agent mixing are rolled into uniform, the water of 10 ~ 50 weight % of addition, pelletize；
(5) by the good material of pelletize at 110 ~ 300 DEG C, heat treatment 1 ~ 5 hour；
(6) lubricant compression molding is added to be cleanser.
In above-mentioned technical proposal, the lubricant is preferably at least in graphite, Pulvis Talci, sesbania powder and stearic acid
Kind.
Cleanser of the present invention, active component are aurichalcite ((Cu, Zn)5(CO3)2(OH)6), the oxygen in its structure
Atom is arranged in double-deck tightly packed mode, and bivalent cupric ion is at octahedral center, and divalent zinc ion is located at four sides position
Put, so that Cu, Zn can be spaced on atomic level each other, so as to ensure active center relative distribution, cleanser has
Higher specific surface area.Meanwhile, aurichalcite volume is larger, can produce larger duct, thus its heap is close in banking process
Degree is relatively low, and commercial Application cost is relatively low.
Cleanser of the present invention can be used in the purifications of raw material such as natural gas, synthesis gas, lightweight liquid state hydro carbons, be used for
The impurity such as removing sulfur arsenic.It is 1500h in room temperature, normal pressure, volume space velocity-1Under conditions of, it is miscellaneous with sulfur containing variable concentrations, arsenic compound
By reactor, the Sulfur capacity of cleanser is up to more than 20% for the nitrogen or synthesis gas of matter.It is 3.0MPa, quality sky in room temperature, pressure
Speed is 3.5h-1Under conditions of, with the propylene liguid of sulfur containing variable concentrations, arsenic compound impurity by reactor, the sulfur of cleanser
Hold arsenic to hold also up to more than 20%.
Below by embodiment, the invention will be further elaborated.
Description of the drawings
Fig. 1 is the XRD diffraction spectrograms of cleaning up agent.(characteristic diffraction peak of aurichalcite in 2 θ=13.0 ± 0.2 °,
24.2 ± 0.2 ° and 32.9 ± 0.2 °)
Specific embodiment
【Comparative example 1】
The method of referenced patent CN101327419A embodiment 1 prepares cleanser, obtains sample sets into being shown in Table 1.
【Embodiment 1】
By 55 grams of zinc nitrate, 45 grams of copper nitrate and 450 grams of mixing and stirrings of water obtain metal salt solution, by sodium carbonate 49
Gram and 550 grams of mix homogeneously of water obtain sodium carbonate liquor, sodium carbonate liquor is sufficiently mixed with metal salt solution, 70 DEG C reactions
1 hour, precipitate is washed into drying, then add 2 grams of aluminium oxide, 1 gram of mixing of graphite is rolled, with precipitate and the gross weight of graphite
Amount percentages, add the water of 30 weight %, pelletize, and in 130 DEG C of heat treatments 5 hours, compression molding obtained sample sets prejudice
Table 1, the XRD spectra of sample are shown in Fig. 1.
【Embodiment 2】
By 55 grams of zinc nitrate, 45 grams of copper nitrate and 450 grams of mixing and stirrings of water obtain metal salt solution, by sodium carbonate 49
Gram and 550 grams of mix homogeneously of water obtain sodium carbonate liquor, sodium carbonate liquor is sufficiently mixed with metal salt solution, 70 DEG C reactions
1 hour, precipitate is washed into drying, then add 7 grams of aluminium oxide, 1 gram of mixing of graphite is rolled, with precipitate and the gross weight of graphite
Amount percentages, add the water of 30 weight %, pelletize, and in 130 DEG C of heat treatments 5 hours, compression molding obtained sample sets prejudice
Table 1.
【Embodiment 3】
By 55 grams of zinc nitrate, 45 grams of copper nitrate and 450 grams of mixing and stirrings of water obtain metal salt solution, by sodium carbonate 49
Gram and 550 grams of mix homogeneously of water obtain sodium carbonate liquor, sodium carbonate liquor is sufficiently mixed with metal salt solution, 70 DEG C reactions
1 hour, precipitate is washed into drying, then add 13 grams of aluminium oxide, 1 gram of mixing of graphite rolls, with the total of precipitate and graphite
Percentage by weight meter, adds the water of 30 weight %, pelletize, and in 130 DEG C of heat treatments 5 hours, compression molding obtained sample composition
It is shown in Table 1.
【Embodiment 4】
By 55 grams of zinc nitrate, 45 grams of copper nitrate and 450 grams of mixing and stirrings of water obtain metal salt solution, by sodium carbonate 49
Gram and 550 grams of mix homogeneously of water obtain sodium carbonate liquor, sodium carbonate liquor is sufficiently mixed with metal salt solution, 70 DEG C reactions
1 hour, precipitate is washed into drying, then add 21 grams of alumina cement, 1 gram of mixing of graphite rolls, with precipitate and graphite
Total weight percent meter, adds the water of 30 weight %, pelletize, and in 130 DEG C of heat treatments 5 hours, compression molding obtained sample sets
Into being shown in Table 1.
【Embodiment 5】
By 55 grams of zinc nitrate, 45 grams of copper nitrate and 450 grams of mixing and stirrings of water obtain metal salt solution, by sodium carbonate 49
Gram and 550 grams of mix homogeneously of water obtain sodium carbonate liquor, sodium carbonate liquor is sufficiently mixed with metal salt solution, 70 DEG C reactions
1 hour, precipitate is washed into drying, then add 32 grams of cellulose, 1 gram of mixing of graphite rolls, with the total of precipitate and graphite
Percentage by weight meter, adds the water of 30 weight %, pelletize, and in 130 DEG C of heat treatments 5 hours, compression molding obtained sample composition
It is shown in Table 1.
【Embodiment 6】
By 55 grams of zinc nitrate, 45 grams of copper nitrate and 450 grams of mixing and stirrings of water obtain metal salt solution, by sodium carbonate 49
Gram and 550 grams of mix homogeneously of water obtain sodium carbonate liquor, sodium carbonate liquor is sufficiently mixed with metal salt solution, 70 DEG C reactions
1 hour, precipitate is washed into drying, then add 49 grams of aluminium oxide, 1 gram of mixing of graphite rolls, with the total of precipitate and graphite
Percentage by weight meter, adds the water of 30 weight %, pelletize, and in 130 DEG C of heat treatments 5 hours, compression molding obtained sample composition
It is shown in Table 1.
【Embodiment 7】
By 55 grams of zinc nitrate, 45 grams of copper nitrate and 450 grams of mixing and stirrings of water obtain metal salt solution, by sodium carbonate 49
Gram and 550 grams of mix homogeneously of water obtain sodium carbonate liquor, sodium carbonate liquor is sufficiently mixed with metal salt solution, 70 DEG C reactions
1 hour, precipitate is washed into drying, then add 74 grams of aluminium oxide, 1 gram of mixing of graphite rolls, with the total of precipitate and graphite
Percentage by weight meter, adds the water of 30 weight %, pelletize, and in 130 DEG C of heat treatments 5 hours, compression molding obtained sample composition
It is shown in Table 1.
【Embodiment 8】
By 55 grams of zinc nitrate, 45 grams of copper nitrate and 450 grams of mixing and stirrings of water obtain metal salt solution, by sodium carbonate 49
Gram and 550 grams of mix homogeneously of water obtain sodium carbonate liquor, sodium carbonate liquor is sufficiently mixed with metal salt solution, 70 DEG C reactions
1 hour, precipitate is washed into drying, then add 160 grams of aluminium oxide, 1 gram of mixing of graphite rolls, with the total of precipitate and graphite
Percentage by weight meter, adds the water of 30 weight %, pelletize, and in 130 DEG C of heat treatments 5 hours, compression molding obtained sample composition
It is shown in Table 1.
【Embodiment 9】
By 55 grams of zinc nitrate, 45 grams of copper nitrate, it is molten that 12 grams of aluminum nitrate and 450 grams of mixing and stirrings of water obtain slaine
49 grams of sodium carbonate and 550 grams of mix homogeneously of water are obtained sodium carbonate liquor, sodium carbonate liquor are fully mixed with metal salt solution by liquid
Close, react 1 hour at 70 DEG C, precipitate is washed into drying, then add 8 grams of aluminium oxide, 1 gram of mixing of graphite to roll, to precipitate
The total weight percent meter of thing and graphite, adds the water of 30 weight %, pelletize, in 300 DEG C of heat treatments 5 hours, compression molding,
Sample sets are obtained into being shown in Table 1.
【Embodiment 10】
By 55 grams of zinc nitrate, 45 grams of copper nitrate, it is molten that 12 grams of aluminum nitrate and 450 grams of mixing and stirrings of water obtain slaine
49 grams of sodium carbonate and 550 grams of mix homogeneously of water are obtained sodium carbonate liquor, sodium carbonate liquor are fully mixed with metal salt solution by liquid
Close, react 1 hour at 70 DEG C, precipitate is washed into drying, then add 8 grams of aluminium oxide, 1 gram of mixing of graphite to roll, to precipitate
The total weight percent meter of thing and graphite, adds the water of 30 weight %, pelletize, in 270 DEG C of heat treatments 5 hours, compression molding,
Sample sets are obtained into being shown in Table 1.
【Embodiment 11】
By 55 grams of zinc nitrate, 45 grams of copper nitrate, it is molten that 12 grams of aluminum nitrate and 450 grams of mixing and stirrings of water obtain slaine
49 grams of sodium carbonate and 550 grams of mix homogeneously of water are obtained sodium carbonate liquor, sodium carbonate liquor are fully mixed with metal salt solution by liquid
Close, react 1 hour at 70 DEG C, precipitate is washed into drying, then add 8 grams of aluminium oxide, 1 gram of mixing of graphite to roll, to precipitate
The total weight percent meter of thing and graphite, adds the water of 30 weight %, pelletize, in 230 DEG C of heat treatments 5 hours, compression molding,
Sample sets are obtained into being shown in Table 1.
【Embodiment 12】
By 55 grams of zinc nitrate, 45 grams of copper nitrate, it is molten that 12 grams of aluminum nitrate and 450 grams of mixing and stirrings of water obtain slaine
49 grams of sodium carbonate and 550 grams of mix homogeneously of water are obtained sodium carbonate liquor, sodium carbonate liquor are fully mixed with metal salt solution by liquid
Close, react 1 hour at 70 DEG C, precipitate is washed into drying, then add 8 grams of aluminium oxide, 1 gram of mixing of graphite to roll, to precipitate
The total weight percent meter of thing and graphite, adds the water of 30 weight %, pelletize, in 210 DEG C of heat treatments 5 hours, compression molding,
Sample sets are obtained into being shown in Table 1.
Table 1
【Embodiment 13】
Cleanser prepared by above-described embodiment is ground into into the granule of 20 ~ 40 mesh, the reaction that internal diameter is 1cm is filled it into
In device, it is 1500h in room temperature, normal pressure, volume space velocity-1Under conditions of, it is logical with the nitrogen of sulfur containing variable concentrations, arsenic compound impurity
The reactor is crossed, the cleanser is evaluated, as a result as shown in table 2.
Table 2
【Embodiment 14】
Cleanser prepared by above-described embodiment is ground into into the granule of 20 ~ 40 mesh, the reaction that internal diameter is 1cm is filled it into
In device, it is 1500h in room temperature, normal pressure, volume space velocity-1Under conditions of, with sulfur containing variable concentrations, the synthesis gas of arsenic compound impurity
By the reactor, the cleanser is evaluated, as a result as shown in table 3.
Table 3
【Embodiment 15】
Cleanser prepared by above-described embodiment is ground into into the granule of 20 ~ 40 mesh, the reaction that internal diameter is 1cm is filled it into
In device, it is 3.5h in room temperature, pressure 3.0MPa, mass space velocity-1Under conditions of, with sulfur containing variable concentrations, arsenic compound impurity
Propylene liguid is evaluated to the cleanser, as a result as shown in table 4 by the reactor.
Table 4
Claims (9)
1. a kind of cleanser, by weight percentage, including following components：
A) 20～95% aurichalcite；
B) 5～80% binding agent；
The preparation method of the cleanser is comprised the following steps successively：
(1) by copper nitrate, zinc nitrate, the water-soluble inorganic salt of aluminum nitrate and hydromassage, your ratio is counted：Cu/Zn is 0.1～2；
Al/Zn is 0～0.7；(Cu+Zn+Al)/H2O is 0.01～0.04 ratio mixing, is uniformly mixing to obtain solution I；
(2) by least one and hydromassage in sodium carbonate, sodium bicarbonate, ammonium carbonate, you are mixed than the ratio for 0.01～0.04
Close, be uniformly mixing to obtain solution II；
(3) by solution I and II mix homogeneously, at 40～90 DEG C, reaction obtains precipitate in 0.5～3 hour, will be precipitate washing dry
It is dry；
(4) precipitate, binding agent mixing are rolled into uniform, the water of 10～50 weight % of addition, pelletize；
(5) by the good material of pelletize at 110～300 DEG C, heat treatment 1～5 hour；
(6) lubricant compression molding is added to be cleanser.
2. cleanser according to claim 1, it is characterised in that in terms of cleanser percentage by weight, the content of aurichalcite is
35～65%.
3. cleanser according to claim 1 or claim 2, it is characterised in that in terms of cleanser percentage by weight, the content of binding agent
For 15～35%.
4. cleanser according to claim 3, its feature in terms of cleanser percentage by weight, also comprising 7～23% ZnO
With 8～22% CuO.
5. cleanser according to claim 1, it is characterised in that the binding agent is aluminium oxide, silicon oxide, alumina cement, fibre
At least one in dimension element, Kaolin, attapulgite, aluminosilicate cement.
6. cleanser according to claim 5, it is characterised in that the binding agent is aluminium oxide.
7. cleanser according to claim 1, it is characterised in that the heap density of cleanser is less than 0.9kg/m3, side pressure strength is big
In 70N/ grains.
8. cleanser according to claim 1, it is characterised in that the lubricant is graphite, Pulvis Talci, sesbania powder and Hard Fat
At least one in acid.
9. the cleanser described in any one of claim 1～8 is used for the purification of natural gas, synthesis gas, lightweight liquid state hydro carbons
In.
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| CN201310512758.9A CN104560251B (en) | 2013-10-28 | 2013-10-28 | Cleaning agent and use thereof |
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| CN104560251B true CN104560251B (en) | 2017-04-19 |
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| CN113522004A (en) * | 2021-08-11 | 2021-10-22 | 中建材蚌埠玻璃工业设计研究院有限公司 | CIGS tail gas purifying agent and preparation method thereof |
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|---|---|---|---|---|
| US5302569A (en) * | 1991-08-17 | 1994-04-12 | Hoechst Aktiengesellschaft | Copper/zinc oxide/aluminum oxide-containing catalysts |
| CN1256970A (en) * | 1998-11-16 | 2000-06-21 | 中国石油化工集团公司 | Processf or preparing copper-containing catalyst |
| CN101262928A (en) * | 2005-08-12 | 2008-09-10 | Sk能源株式会社 | Desulfurizing agent for removing organic sulfur compounds, preparation method thereof and method for removing organic sulfur compounds using the same |
| CN101652176A (en) * | 2007-04-10 | 2010-02-17 | 出光兴产株式会社 | Catalyst precursor and catalyst using the same |
| CN102091526A (en) * | 2009-12-09 | 2011-06-15 | 北京三聚环保新材料股份有限公司 | Normal-temperature desulfurizer and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101988065B1 (en) * | 2011-07-27 | 2019-06-11 | 사우디 아라비안 오일 컴퍼니 | Catalytic compositions useful in removal of sulfur compounds from gaseous hydrocarbons, processes for making these and uses thereof |
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- 2013-10-28 CN CN201310512758.9A patent/CN104560251B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5302569A (en) * | 1991-08-17 | 1994-04-12 | Hoechst Aktiengesellschaft | Copper/zinc oxide/aluminum oxide-containing catalysts |
| CN1256970A (en) * | 1998-11-16 | 2000-06-21 | 中国石油化工集团公司 | Processf or preparing copper-containing catalyst |
| CN101262928A (en) * | 2005-08-12 | 2008-09-10 | Sk能源株式会社 | Desulfurizing agent for removing organic sulfur compounds, preparation method thereof and method for removing organic sulfur compounds using the same |
| CN101652176A (en) * | 2007-04-10 | 2010-02-17 | 出光兴产株式会社 | Catalyst precursor and catalyst using the same |
| CN102091526A (en) * | 2009-12-09 | 2011-06-15 | 北京三聚环保新材料股份有限公司 | Normal-temperature desulfurizer and preparation method thereof |
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