CN104560250B - Cleanser and preparation method thereof - Google Patents
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- CN104560250B CN104560250B CN201310512757.4A CN201310512757A CN104560250B CN 104560250 B CN104560250 B CN 104560250B CN 201310512757 A CN201310512757 A CN 201310512757A CN 104560250 B CN104560250 B CN 104560250B
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Abstract
The present invention relates to a kind of cleansers and preparation method thereof, mainly solve the problem of cleanser heap density in the prior art is high, and utilization rate is low, and commercial Application is of high cost.The present invention is by a kind of cleanser, by weight percentage, including following components：A) 20 ~ 95% Cu Zn Al ternary hydrotalcites；B) 5 ~ 80% binding agent；The hydrotalcite compound is two valency ion Zns2+、Cu2+, trivalent ion Al3+The ternary hydrotalcite of composition, molecular structure are [CuyZn(1‑x‑y)Alx(OH)2](CO3)x/2 .mH2O), x is the molar ratio of Al/ (Zn+Cu+Al), and x is 0.2 ~ 0.33；Cu/Zn (molar ratio)=0.1 ~ 2；M is hydration number, and m is 2 ~ 4 technical solution, preferably solves the problems, such as this, in the purification available for natural gas, synthesis gas, lightweight liquid state hydro carbons etc..
Description
Technical field
The present invention relates to a kind of cleansers and preparation method thereof.
Background technology
The impurity such as sulphur, 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 poisonings to inactivate, and greatly shorten catalyst life, and even resulting in catalysis reaction can not be normal
It carries out；It can be a series of so as to bring as production is into being advanced into the composite of downstream in addition, not removing clean sulphur arsenic impurities
Environmental Health etc. the problem of.Therefore, main reminder of the impurity such as sulphur arsenic for protection downstream unit is removed to high-efficiency high-accuracy
The agent and quality for improving downstream product simultaneously has very important meaning.
Under normal circumstances, 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 is high, easy to use, safe can
Lean on, sulfur capacity is high, plays " checking on " and " protection " acts on and occupy very important status, it be widely applied to synthesize 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 certain organic sulfurs in the raw materials such as gas, carbon dioxide.Sulphur in unstripped gas can be removed to by zinc sulphide desulfurization
0.055mg/kg.CuO is added in normal temp zinc oxide desulfuriging agent to improve its desulphurizing ability.It is de- that Zinc oxide desulfurizer is generally used for essence
Sulphur process, it can also absorb general organosulfur compound.Arsenic impurities in the raw material of industry, usually with AsH3Form exists, work
The Hydrodearsenic Catalyst used in industry substantially can be divided into copper system, four class of lead system, manganese systems and nickel system, wherein relatively conventional with copper system.Copper system takes off
Arsenical arsenic holds height, can be carried out under room temperature, normal pressure and higher space velocity.Copper system Hydrodearsenic Catalyst can be divided into metallic copper, CuO-Al again2O3、
CuO-ZnO-Al2O3Deng.When using CuO as active component, AsH3By Cu2+It is reduced at a low price or metallic state, arsenic is combined or swum with copper
From into element state.The development trend of desulfurizing agent and Hydrodearsenic Catalyst be to low bulk density, low temperature in use, 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 sulphur arsenic cleanser
It is made of carrier and active component, active component is lead oxide, magnetic iron oxide and copper oxide, and carrier is γ-Al2O3, the sulphur arsenic
Cleanser needs to activate 4 ~ 8 hours at 350 ~ 650 DEG C, and oxide sulphur arsenic purification is can be seen that from its composition and preparation method
Agent heap density is high, and preparation process is complicated, and commercial Application cost is higher.
Patent CN102049236A discloses a kind of copper zinc ambient temperature desulfuration agent and preparation method thereof, which 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 mediated, is molded, dry after obtain, which is obtained by physical mixed, thus zinc-copper therein
Active component can not play synergistic effect, relatively low so as to cause its Sulfur capacity.
Invention content
The technical problems to be solved by the invention are that cleanser heap density is high in the prior art, and utilization rate is low, commercial Application
The problem of cost is higher provides a kind of new cleanser.The cleanser is for natural gas, synthesis gas, lightweight liquid state hydro carbons
When purification in when, have heap density low, utilization rate is high, commercial Application advantage at low cost.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：A kind of cleanser, with weight percent
Meter, including following components：A) 20 ~ 95% Cu-Zn-Al ternary hydrotalcites；B) 5 ~ 80% binding agent；The hydrotalcite chemical combination
Object is two valency ion Zns2+、Cu2+, trivalent ion Al3+The ternary hydrotalcite of composition, molecular structure are [CuyZn(1-x-y)Alx
(OH)2](CO3)x/2 .mH2O), x is the molar ratio of Al/ (Zn+Cu+Al), and x is 0.2 ~ 0.33；Cu/Zn (molar ratio)=0.1 ~ 2；m
For hydration number, m is 2 ~ 4.
In above-mentioned technical proposal, preferably Cu/Zn (molar ratio)=0.5 ~ 1；In terms of cleanser weight percent, Cu-Zn-Al
The preferred scope of ternary hydrotalcite is 30 ~ 85%；In terms of cleanser weight percent, the preferred scope of the binding agent for 10 ~
50%；The binding agent is aluminium oxide, in silica, alumina cement, cellulose, kaolin, attapulgite, alumino-silicate cement
At least one, 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 75N/.
In above-mentioned technical proposal, it is preferable that in terms of cleanser weight percent, cleanser further include 10 ~ 30% ZnO and
10 ~ 30% CuO.
The preparation method of cleanser described in above-mentioned technical proposal, includes 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 0.5 ~ 0.9；(Cu+Zn+Al)/H2The ratio that O is 0.01 ~ 0.04 mixes, and is uniformly mixing to obtain solution I；
(2) by least one of sodium carbonate, sodium bicarbonate, ammonium carbonate and hydromassage that than the ratio for 0.01 ~ 0.04
Mixing, is uniformly mixing to obtain solution II；
(3) solution I and II is uniformly mixed, at 40 ~ 90 DEG C, reaction obtains sediment in 0.5 ~ 3 hour, sediment is washed dry
It is dry；
(4) sediment, binding agent, mix lubricant are rolled to the water for uniformly adding in 10 ~ 50 weight %, are granulated.
(5) it by the material being granulated at 110 ~ 300 DEG C, is heat-treated 1 ~ 5 hour；
(6) compression molding is cleanser.
In above-mentioned technical proposal, the lubricant is at least one of graphite, talcum powder, sesbania powder and stearic acid.
Cleanser of the present invention, active component are Cu-Zn-Al ternary hydrotalcites [CuyZn(1-x-y)Alx(OH)2]
(CO3)x/2 .mH2O), hydrotalcite is layer structure, has higher specific surface area, is conducive to the dispersion in activated centre.Therefore, it uses
Cleanser prepared by hydrotalcite has higher specific surface area, and active component relative distribution, effective rate of utilization is high, has relatively strong net
Change ability.Meanwhile hydrotalcite volume is larger, and larger duct can be generated in banking process, thus its heap density is relatively low, industry
Application cost is relatively low.
Cleanser of the present invention can be used in the purification of natural gas, synthesis gas, lightweight liquid state hydro carbons etc., can remove original
The impurity such as the sulphur arsenic in material.In room temperature, normal pressure, volume space velocity 1500h-1Under conditions of, to contain various concentration sulphur, arsenic compound
The nitrogen or synthesis gas of impurity are held by reactor, the Sulfur capacity arsenic of cleanser up to more than 20%.Room temperature, pressure 3.0MPa,
Mass space velocity is 3.5h-1Under conditions of, reactor, purification are passed through with the propylene liguid of sulphur containing various concentration, arsenic compound impurity
The Sulfur capacity arsenic of agent holds also up to more than 20%.
The present invention will be further described below by way of examples.
Description of the drawings
Fig. 1 is the XRD diffraction spectrograms of cleaning up agent.(characteristic diffraction peak of Cu-Zn-Al ternary hydrotalcites is in 2 θ=11.7
± 0.2 ° and 23.5 ± 0.2 °)
Specific embodiment
【Comparative example 1】
1 sample of comparative example is copper aluminum hydrotalcite.
450 grams of 45 grams of copper nitrate, 56 grams of aluminum nitrate and water are mixed evenly to obtain metal salt solution, by 50 grams of sodium carbonate
It is uniformly mixed with 550 grams of water and obtains sodium carbonate liquor, sodium carbonate liquor and metal salt solution are sufficiently mixed, in 70 DEG C of reactions 1
Hour, sediment is washed into drying, then adds in 2.2 grams of aluminium oxide, 1 gram of mixing of graphite rolls, with the total of sediment and graphite
Weight percent meter adds the water of 30 weight %, is granulated, dry, and 110 DEG C are heat-treated 5 hours, and compression molding obtains sample sets
Into being shown in Table 1.
【Comparative example 2】
2 sample of comparative example is zinc-aluminum hydrotalcite.
450 grams of 55 grams of zinc nitrate, 56 grams of aluminum nitrate and water are mixed evenly to obtain metal salt solution, by 50 grams of sodium carbonate
It is uniformly mixed with 550 grams of water and obtains sodium carbonate liquor, sodium carbonate liquor and metal salt solution are sufficiently mixed, in 70 DEG C of reactions 1
Hour, sediment is washed into drying, then adds in 2.2 grams of aluminium oxide, 1 gram of mixing of graphite rolls, with the total of sediment and graphite
Weight percent meter adds the water of 30 weight %, is granulated, dry, and 110 DEG C are heat-treated 5 hours, and compression molding obtains sample sets
Into being shown in Table 1.
【Embodiment 1】
By 55 grams of zinc nitrate, 45 grams of copper nitrate, 450 grams of 56 grams of aluminum nitrate and water are mixed evenly to obtain metal salt molten
550 grams of 69 grams of sodium carbonate and water are uniformly mixed and obtain sodium carbonate liquor by liquid, and sodium carbonate liquor and metal salt solution is fully mixed
It closes, is reacted 1 hour at 70 DEG C, sediment is washed into drying, then add in 3.2 grams of aluminium oxide, 1 gram of mixing of graphite rolls, with heavy
The total weight percent meter of starch and graphite adds the water of 30 weight %, is granulated, dry, and 110 DEG C are heat-treated 5 hours, tabletting
Molding, obtains sample composition and is shown in Table 1, the XRD spectra of sample is shown in Fig. 1.
【Embodiment 2】
By 55 grams of zinc nitrate, 45 grams of copper nitrate, 450 grams of 56 grams of aluminum nitrate and water are mixed evenly to obtain metal salt molten
550 grams of 69 grams of sodium carbonate and water are uniformly mixed and obtain sodium carbonate liquor by liquid, and sodium carbonate liquor and metal salt solution is fully mixed
It closes, is reacted 1 hour at 70 DEG C, sediment is washed into drying, then add in 15 grams of aluminium oxide, 1 gram of mixing of graphite rolls, with precipitation
The total weight percent meter of object and graphite adds the water of 30 weight %, is granulated, dry, and 110 DEG C are heat-treated 5 hours, tabletting into
Type obtains sample composition and is shown in Table 1.
【Embodiment 3】
By 55 grams of zinc nitrate, 20 grams of copper nitrate, 450 grams of 56 grams of aluminum nitrate and water are mixed evenly to obtain metal salt molten
550 grams of 69 grams of sodium carbonate and water are uniformly mixed and obtain sodium carbonate liquor by liquid, and sodium carbonate liquor and metal salt solution is fully mixed
It closes, is reacted 1 hour at 70 DEG C, sediment is washed into drying, then add in 35 grams of aluminium oxide, 1 gram of mixing of graphite rolls, with precipitation
The total weight percent meter of object and graphite adds the water of 30 weight %, is granulated, dry, and 110 DEG C are heat-treated 5 hours, tabletting into
Type obtains sample composition and is shown in Table 1.
【Embodiment 4】
By 55 grams of zinc nitrate, 5 grams of copper nitrate, 450 grams of 56 grams of aluminum nitrate and water are mixed evenly to obtain metal salt solution,
550 grams of 69 grams of sodium carbonate and water are uniformly mixed and obtain sodium carbonate liquor, sodium carbonate liquor and metal salt solution are sufficiently mixed,
It is reacted 1 hour at 70 DEG C, sediment is washed into drying, then add in 70 grams of aluminium oxide, 1 gram of mixing of graphite rolls, with sediment
With the total weight percent meter of graphite, the water of 30 weight % is added, is granulated, dry, 110 DEG C are heat-treated 5 hours, compression molding,
It obtains sample composition and is shown in Table 1.
【Embodiment 5】
By 55 grams of zinc nitrate, 90 grams of copper nitrate, 450 grams of 56 grams of aluminum nitrate and water are mixed evenly to obtain metal salt molten
550 grams of 69 grams of sodium carbonate and water are uniformly mixed and obtain sodium carbonate liquor by liquid, and sodium carbonate liquor and metal salt solution is fully mixed
It closes, is reacted 1 hour at 70 DEG C, sediment is washed into drying, then add in 240 grams of aluminium oxide, 1 gram of mixing of graphite rolls, with heavy
The total weight percent meter of starch and graphite adds the water of 30 weight %, is granulated, dry, and 110 DEG C are heat-treated 5 hours, tabletting
Molding, obtains sample composition and is shown in Table 1.
【Embodiment 6】
By 55 grams of zinc nitrate, 45 grams of copper nitrate, 450 grams of 39 grams of aluminum nitrate and water are mixed evenly to obtain metal salt molten
550 grams of 69 grams of sodium carbonate and water are uniformly mixed and obtain sodium carbonate liquor by liquid, and sodium carbonate liquor and metal salt solution is fully mixed
It closes, is reacted 1 hour at 70 DEG C, sediment is washed into drying, then add in 15 grams of alumina cement, 1 gram of mixing of graphite rolls, with heavy
The total weight percent meter of starch and graphite adds the water of 30 weight %, is granulated, dry, and 110 DEG C are heat-treated 5 hours, tabletting
Molding, obtains sample composition and is shown in Table 1.
【Embodiment 7】
By 55 grams of zinc nitrate, 45 grams of copper nitrate, 450 grams of 70 grams of aluminum nitrate and water are mixed evenly to obtain metal salt molten
550 grams of 69 grams of sodium carbonate and water are uniformly mixed and obtain sodium carbonate liquor by liquid, and sodium carbonate liquor and metal salt solution is fully mixed
It closes, is reacted 1 hour at 70 DEG C, sediment is washed into drying, then add in 15 grams of kaolin, 1 gram of mixing of graphite rolls, with precipitation
The total weight percent meter of object and graphite adds the water of 30 weight %, is granulated, dry, and 110 DEG C are heat-treated 5 hours, tabletting into
Type obtains sample composition and is shown in Table 1.
【Embodiment 8】
By 55 grams of zinc nitrate, 90 grams of copper nitrate, 650 grams of 56 grams of aluminum nitrate and water are mixed evenly to obtain metal salt molten
700 grams of 69 grams of sodium carbonate and water are uniformly mixed and obtain sodium carbonate liquor by liquid, and sodium carbonate liquor and metal salt solution is fully mixed
It closes, is reacted 1 hour at 70 DEG C, sediment is washed into drying, then add in 240 grams of aluminium oxide, 1 gram of mixing of graphite rolls, with heavy
The total weight percent meter of starch and graphite adds the water of 30 weight %, is granulated, dry, and 190 DEG C are heat-treated 5 hours, tabletting
Molding, obtains sample composition and is shown in Table 1.
【Embodiment 9】
By 55 grams of zinc nitrate, 90 grams of copper nitrate, 450 grams of 56 grams of aluminum nitrate and water are mixed evenly to obtain metal salt molten
550 grams of 69 grams of sodium carbonate and water are uniformly mixed and obtain sodium carbonate liquor by liquid, and sodium carbonate liquor and metal salt solution is fully mixed
It closes, is reacted 1 hour at 70 DEG C, sediment is washed into drying, then add in 240 grams of aluminium oxide, 1 gram of mixing of graphite rolls, with heavy
The total weight percent meter of starch and graphite adds the water of 30 weight %, is granulated, dry, and 230 DEG C are heat-treated 5 hours, tabletting
Molding, obtains sample composition and is shown in Table 1.
【Embodiment 10】
By 55 grams of zinc nitrate, 90 grams of copper nitrate, 450 grams of 56 grams of aluminum nitrate and water are mixed evenly to obtain metal salt molten
550 grams of 69 grams of sodium carbonate and water are uniformly mixed and obtain sodium carbonate liquor by liquid, and sodium carbonate liquor and metal salt solution is fully mixed
It closes, is reacted 1 hour at 70 DEG C, sediment is washed into drying, then add in 240 grams of aluminium oxide, 1 gram of mixing of graphite rolls, with heavy
The total weight percent meter of starch and graphite adds the water of 30 weight %, is granulated, dry, and 270 DEG C are heat-treated 5 hours, tabletting
Molding, obtains sample composition and is shown in Table 1.
Table 1
【Embodiment 11】
Cleanser prepared by above-described embodiment is ground into the particle of 20 ~ 40 mesh, fills it into the reaction that internal diameter is 1cm
In device, in room temperature, normal pressure, volume space velocity 1500h-1Under conditions of, led to the nitrogen of sulphur containing various concentration, arsenic compound impurity
The reactor is crossed, which is evaluated, the results are shown in Table 2.
Table 2
【Embodiment 12】
Cleanser prepared by above-described embodiment is ground into the particle of 20 ~ 40 mesh, fills it into the reaction that internal diameter is 1cm
In device, in room temperature, normal pressure, volume space velocity 1500h-1Under conditions of, with sulphur containing various concentration, the synthesis gas of arsenic compound impurity
By the reactor, which is evaluated, the results are shown in Table 3.
Table 3
【Embodiment 13】
Cleanser prepared by above-described embodiment is ground into the particle of 20 ~ 40 mesh, fills it into the reaction that internal diameter is 1cm
In device, in room temperature, pressure 3.0MPa, mass space velocity 3.5h-1Under conditions of, with sulphur containing various concentration, arsenic compound impurity
Propylene liguid is evaluated the cleanser, the results are shown in Table 4 by the reactor.
Table 4
Claims (7)
1. a kind of purposes of cleanser, cleanser is used in the purification of lightweight liquid state hydrocarbon raw material, removes the sulphur arsenic in raw material
Impurity；The cleanser, it is by weight percentage, composed of the following components：
A) 20~95% Cu-Zn-Al hydrotalcite compounds；
B) 5~80% binding agent；
The hydrotalcite compound is two valency ion Zns2+、Cu2+, trivalent ion Al3+The ternary hydrotalcite of composition, molecular structure are
[CuyZn(1-x-y)Alx(OH)2](CO3)x/2.mH2O), x is the molar ratio of Al/ (Zn+Cu+Al), and x is 0.2~0.33；Cu/Zn
(molar ratio)=0.1~2；M is hydration number, and m is 2~4.
2. the purposes of cleanser according to claim 1, it is characterised in that in terms of cleanser weight percent, hydrotalcite chemical combination
The content of object is 40~80%.
3. the purposes of cleanser according to claim 1, it is characterised in that in terms of cleanser weight percent, binding agent contains
Measure is 10~50%.
4. the purposes of cleanser according to claim 1, it is characterised in that Cu/Zn (molar ratio)=0.5~1.
5. the purposes of cleanser according to claim 1, it is characterised in that the binding agent is aluminium oxide, silica, alumina
At least one of cement, cellulose, kaolin, attapulgite, alumino-silicate cement.
6. the purposes of cleanser according to claim 5, it is characterised in that the binding agent is aluminium oxide.
7. the purposes of cleanser according to claim 1, it is characterised in that the heap density of cleanser is less than 0.9kg/m3；Side pressure
Intensity is more than 75N/.
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| CN106606926A (en) * | 2015-10-22 | 2017-05-03 | 中国石油化工股份有限公司 | Room temperature fine desulfurization method |
| US10882801B2 (en) | 2016-01-04 | 2021-01-05 | Saudi Arabian Oil Company | Methods for gas phase oxidative desulphurization of hydrocarbons using CuZnAl catalysts promoted with group VIB metal oxides |
| 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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| CN1037778C (en) * | 1992-11-28 | 1998-03-18 | 大阪瓦斯株式会社 | Method for desulfurization of hydrocarbon |
| US7431825B2 (en) * | 2003-12-05 | 2008-10-07 | Intercat, Inc. | Gasoline sulfur reduction using hydrotalcite like compounds |
| JP2005345448A (en) * | 2004-06-07 | 2005-12-15 | National Institute For Materials Science | Adsorbent for radioactive element-containing waste, and method of immobilizing radioactive element |
| US7749376B2 (en) * | 2005-08-15 | 2010-07-06 | Sud-Chemie Inc. | Process for sulfur adsorption using copper-containing catalyst |
| CN1919447A (en) * | 2006-08-16 | 2007-02-28 | 天津化工研究设计院 | Preparation process of flue gas desulfurization and denitration material |
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