CN104096565A - Carbonyl sulfide hydrolyst and preparation method thereof - Google Patents
Carbonyl sulfide hydrolyst and preparation method thereof Download PDFInfo
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- CN104096565A CN104096565A CN201410369381.0A CN201410369381A CN104096565A CN 104096565 A CN104096565 A CN 104096565A CN 201410369381 A CN201410369381 A CN 201410369381A CN 104096565 A CN104096565 A CN 104096565A
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Abstract
The invention provides a carbonyl sulfide hydrolyst and a preparation method thereof. The method comprises the steps as follows: firstly, a carrier is dipped into a reactive metal saline solution for enabling reactive metal saline ions to be dispersed uniformly on the surface of the carrier; secondly, when the carrier is dipped for a certain period of time, the dipping amount of the reactive metal saline ions reaches saturation, an inorganic alkaline liquid is dripped gradually and slowly into the solution, and the pH value is controlled well, and metal ions and hydroxyl are combined to facilitate the formation of countless small granules to be adhered to the inner surface and the outer surface of the carrier. In the method for preparing a carbonyl sulfide hydrolyst in the prior art, the process of dipping a carrier carrying metallic compounds in a dipping manner again into an alkaline liquid can lead to heavy loss of the metallic compounds, so that the capacity of the active components on a final carrier is greatly lowered, the sulphur capacity of the carbonyl sulfide hydrolyst is lower, and the desulphurization efficiency is lower. Comparing with the method in the prior art, the carbonyl sulfide hydrolyst prepared by the method provided by the invention is excellent in the dispersity and the capacity of the active components on the inner surface and the outer surface of the carrier, high in sulphur capacity, and high in desulphurization efficiency.
Description
Technical field
The present invention relates to a kind of hydrolytic catalyst of carbonyl sulfur and preparation method thereof, belong to carbonyl sulfide hydrolysis catalysis technical field.
Background technology
Taking coal, coke, natural gas and oil etc. as raw material produce material gas in all containing organic sulfur, but organic sulfur particularly cos COS existence not only contaminated environment, corrosion pipeline equipment, affect quality of chemical products, and can cause the poisoning and deactivation of catalyst in subsequent production process, therefore the technology that removes of cos is paid much attention to.Because cos is neutrality or faintly acid, its chemical property torpescence, be difficult to use the method that removes hydrogen sulfide to be removed, thereby in current industrial production, utilize the catalyzing hydrolysis of cos to remove cos and be proved to be one of effective method, its fundamental reaction principle is: under the effect of hydrolytic catalyst of carbonyl sulfur, cos COS first reacts and changes into H with water
2s, adopts desulfurizing agent to remove H afterwards
2s.
Chinese patent literature CN101590395A discloses a kind of preparation method of hydrolytic catalyst of carbonyl sulfur, comprises the following steps: the activation of (1) carrier; (2) active metallic compound is dissolved in and in solvent, is mixed with maceration extract; (3) by the described maceration extract that after activation in step (1), carrier impregnation obtains in step (2), after filtration, obtain load after dry and have the carrier of active metallic compound; (4) there is the carrier impregnation of active metallic compound in inorganic alkaline solution by obtaining described load in step (3), through filtering, being dried, then after roasting, obtain hydrolytic catalyst of carbonyl sulfur finished product.Said method is by being first carried on active metallic compound on carrier, and then have the carrier of active metallic compound with inorganic base liquid dip loading, can avoid first load alkaline matter to flood active metallic ion again time, metal ion and alkaline matter generate and are difficult for molten metal hydroxides and are only attached to carrier surface and are difficult to enter the defect in carrier duct.But, said method, the carrier of metallic compound on dip loading be impregnated in the process in alkali lye again, can cause metallic compound to run off serious, and the load capacity of active component on final carrier is reduced greatly, cause the Sulfur capacity of hydrolytic catalyst of carbonyl sulfur lower, desulfuration efficiency is low.
Summary of the invention
When technical problem to be solved by this invention is that art methods is prepared hydrolytic catalyst of carbonyl sulfur, the carrier of metallic compound on dip loading be impregnated in the process in alkali lye again, can cause metallic compound to run off serious, the load capacity of active component on final carrier is reduced greatly, cause the Sulfur capacity of hydrolytic catalyst of carbonyl sulfur lower, desulfuration efficiency is low, thereby proposes hydrolytic catalyst of carbonyl sulfur that a kind of Sulfur capacity is high and preparation method thereof.
For solving the problems of the technologies described above, the present invention is achieved by the following technical solutions:
The preparation method who the invention provides a kind of hydrolytic catalyst of carbonyl sulfur, it comprises the steps:
(1) by the water-soluble soluble metallic salt maceration extract that is mixed with;
(2) by carrier impregnation in described maceration extract and the volume ratio of controlling solid-liquid be 1:2-1:3, soak 20-40min;
(3) in above-mentioned system, slowly drip inorganic alkaline solution, and after regulating pH to be 7.5,15-30min, filter, dry, obtain described hydrolytic catalyst of carbonyl sulfur.
Front being also provided with of step (1), carrier is carried out to pretreated step, specifically comprise: carrier is immersed to diluted acid and soak 12-18h, and the volume ratio of controlling the solid-liquid of described carrier and diluted acid is 1:2-1:3, to completing that described carrier after immersion carries out once or washing-baking step repeatedly, obtain pretreated carrier, wherein said bake out temperature is 100-110 DEG C.
Described diluted acid is rare nitric acid, and the concentration of described rare nitric acid is 8wt%.
In step (1), described soluble metallic salt is soluble ferric iron salt, and described inorganic alkaline solution is NaOH, potassium hydroxide.
The concentration of described maceration extract is 1-10g/mL, and the mass concentration of described inorganic alkaline solution is 1-5wt%.
Described carrier is porous carrier, and its specific area is greater than 1000m
2/ g.
Described carrier is one or more any combination in active carbon, titanium oxide, zirconia, molecular sieve.
In step (3), under stirring condition, drip described inorganic alkali lye.
In step (3), be 2-4h described drying time, and described baking temperature is 100-105 DEG C.
The hydrolytic catalyst of carbonyl sulfur preparing according to described method.
Technique scheme of the present invention has the following advantages compared to existing technology:
(1) preparation method of hydrolytic catalyst of carbonyl sulfur of the present invention, its by first by carrier impregnation in active metal salting liquid, make the surface that is dispersed in carrier of active metal salt uniform ion, dipping certain hour, the pickup of active metal salt ion reaches capacity, now slowly drip gradually inorganic alkali lye, control pH value well, metal ion and hydroxyl be combined be beneficial to form countless molecules be attached in the surface and pore passage structure of carrier, while preparing hydrolytic catalyst of carbonyl sulfur compared to art methods, the carrier of metallic compound on dip loading be impregnated in the process in alkali lye again, can cause metallic compound to run off serious, the load capacity of active component on final carrier is reduced greatly, cause the Sulfur capacity of hydrolytic catalyst of carbonyl sulfur lower, desulfuration efficiency is low, the hydrolytic catalyst of carbonyl sulfur that the inventive method prepares, on carrier surfaces externally and internally, the decentralization of active component and load capacity are all fine, Sulfur capacity is high, desulfuration efficiency is high.
(2) preparation method of hydrolytic catalyst of carbonyl sulfur of the present invention, also comprise carrier is carried out to pretreated step, by first carrier being immersed to rare nitric acid dousing, 100-110 DEG C of oven dry after washing, repeat described washing and baking step one or many, thereby not only utilize the impurity in dilute nitric acid dissolution carrier and removed, also help in carrier surface increase and adhere to acidic-group, provide oxy radical for further flooding active component, contribute to improve dipping efficiency.
(3) preparation method of hydrolytic catalyst of carbonyl sulfur of the present invention, preferred described soluble metallic salt is soluble ferric iron salt, described inorganic alkaline solution is NaOH, thereby pass through carrier impregnation in iron salt solutions, make iron ion be dispersed in carrier surface and reach capacity, slowly drip again sodium hydroxide solution, by regulating pH, iron ion is combined with hydroxyl and is formed countless FeOOH molecules and be attached to the surfaces externally and internally of carrier, this FeOOH and NaOH exist simultaneously, not only be conducive to strengthen the hydrolysis effect of COS, FeOOH can also be by the hydrolysate H of COS simultaneously
2s absorbs, and realizes the disposable cos that removes.
(4) preparation method of hydrolytic catalyst of carbonyl sulfur of the present invention, described being dried as close drying, thereby airtight at one, in the environment that temperature slowly raises, the moisture content containing in inorganic alkali lye on carrier gradually reduces, until dry, on carrier can there is not too large change in the dipping position of inorganic base all the time, the inorganic base finally obtaining can be dispersed in inside and the surface of carrier, the rapid evaporation due to steam in drying course in open environment compared to prior art, easily there is anti-alkali phenomenon in macro manifestations, the distribution uniform of inorganic base in catalyst carrier of the present invention, good to the removal effect of COS.
Detailed description of the invention
Embodiment 1
The present embodiment provides a kind of hydrolytic catalyst of carbonyl sulfur, is greater than 1000m with specific area
2the porous activated carbon of/g is carrier, and taking Fe, Na as active component, it adopts preparation with the following method:
(1) by the water-soluble ferrous sulfate FeSO that is mixed with 1g/mL
4maceration extract;
(2) by 100g carrier impregnation in maceration extract described in 200mL, soak 20min at 25 DEG C;
(3) under stirring condition, in above-mentioned system, slowly drip the NaOH solution that mass concentration is 1%, after regulating pH to be 7.5,15min, filter and elimination filtrate, control is dry, and 100 DEG C of dry 4h, obtain described hydrolytic catalyst of carbonyl sulfur.
Embodiment 2
The present embodiment provides a kind of hydrolytic catalyst of carbonyl sulfur, and it is greater than 1000m with specific area
2the porous titanium oxide of/g is carrier, and taking Fe, Na as active component, it adopts preparation with the following method:
(1) volume ratio that carrier is immersed to the watery hydrochloric acid of 8wt% and control the solid-liquid of described carrier and watery hydrochloric acid is 1:3, soaks 12h, washes latter 100 DEG C and dries 2h, repeats described washing and baking step 3 times, obtains pretreated carrier;
(2) by the water-soluble ferrous sulfate FeSO that is mixed with 10g/mL
4maceration extract;
(3) by 100g carrier impregnation in maceration extract described in 300mL, soak 40min at 25 DEG C;
(4) under stirring condition, in above-mentioned system, slowly drip the NaOH solution that mass concentration is 5%, after regulating pH to be 7.5,20min, filter, under 105 DEG C of conditions, carry out close drying 2h, obtain described hydrolytic catalyst of carbonyl sulfur.
Embodiment 3
The present embodiment provides a kind of hydrolytic catalyst of carbonyl sulfur, and it is greater than 1000m with specific area
2the porous molecular screen of/g is carrier, and taking iron, potassium as active component, it adopts preparation with the following method:
(1) volume ratio that carrier is immersed to rare nitric acid of 8wt% and control the solid-liquid of described carrier and rare nitric acid is 1:3, soaks 18h, washes latter 100 DEG C and dries 2h, repeats described washing and baking step 1 time, obtains pretreated carrier;
(2) by the water-soluble ferrous sulfate iron FeSO that is mixed with 1g/mL
4maceration extract;
(3) by 100g carrier impregnation in maceration extract described in 200mL, soak 20min at 25 DEG C;
(4) under stirring condition, in above-mentioned system, slowly drip the KOH solution that mass concentration is 1%, after regulating pH to be 7.5,15min, filter and elimination filtrate, control is dry, and 110 DEG C of dry 4h, obtain described hydrolytic catalyst of carbonyl sulfur.
Embodiment 4
The present embodiment provides a kind of hydrolytic catalyst of carbonyl sulfur, and it is greater than 1000m with specific area
2the porous zirconia of/g is carrier, and taking iron, potassium as active component, it adopts preparation with the following method:
(1) by the water-soluble ferric nitrate FeSO that is mixed with 1g/mL
4maceration extract;
(2) by 100g carrier impregnation in maceration extract described in 300mL, soak 40min at 25 DEG C;
(3) under stirring condition, in above-mentioned system, slowly drip the KOH solution that mass concentration is 5%, after regulating pH to be 7.5,30min, filter and elimination filtrate, control is dry, and 100 DEG C of dry 4h, obtain described hydrolytic catalyst of carbonyl sulfur.
Comparative example
This comparative example provides a kind of preparation method of hydrolytic catalyst of carbonyl sulfur, and it comprises the steps:
(1) ZSM-5 molecular sieve carrier is heated to 24h at 200 DEG C;
(2) 12h in the FeSO4 that is 1mol/L by the carrier impregnation after activation processing in concentration, after filtration, 120 DEG C of dry carriers that obtain metallic iron compound for 8 hours;
(3) by the carrier impregnation of step (2) carried metal iron in the sodium hydroxide solution of 20wt%, dipping 12h, filters, and through 120 DEG C of dry 8 hours, 300 DEG C roastings 7 hours, obtains hydrolytic catalyst of carbonyl sulfur.
Test case
The described hydrolytic catalyst of carbonyl sulfur number consecutively that above-described embodiment 1-4 and comparative example are prepared is A, B, C, D, E, carries out the mensuration of Sulfur capacity.
Condition determination is: the unstripped gas (all the other are high-purity N 2) that is 30～80ppm containing COS concentration, 25 DEG C of air speed 3000h-1, reaction temperatures, normal pressure.Described hydrolytic catalyst of carbonyl sulfur loadings 2mL, the control of desulphurization reaction terminal outlet tail gas sulfur content is 0.05ppm, in tail gas, analysis of sulfur content adopts chromatography determination.
The computing formula of Sulfur capacity S is: S%=V*C/M;
In formula, V represents the volume of unstripped gas, and C represents the concentration (mg/m3) of COS in unstripped gas, and M represents the loadings of hydrolytic catalyst of carbonyl sulfur.
The measurement result of Sulfur capacity is as shown in table 1.
The measurement result of the different hydrolytic catalyst of carbonyl sulfur Sulfur capacity of table 1-
| Numbering | Reaction temperature/DEG C | Penetrate Sulfur capacity/% | Outlet precision/ppm |
| A | Normal temperature | 14.59 | 0.05 |
| B | Normal temperature | 18.19 | 0.02 |
| C | Normal temperature | 15.56 | 0.05 |
| D | Normal temperature | 16.64 | 0.02 |
| E | Normal temperature | 10.78 | 0.05 |
Data from table 1, can find out, hydrolytic catalyst of carbonyl sulfur of the present invention, and Sulfur capacity is high, and desulfuration efficiency is high.
Obviously, above-described embodiment is only for example is clearly described, and the not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also giving exhaustive to all embodiments.And the apparent variation of being extended out thus or variation are still among the protection domain in the invention.
Claims (10)
1. a preparation method for hydrolytic catalyst of carbonyl sulfur, it comprises the steps:
(1) by the water-soluble soluble metallic salt maceration extract that is mixed with;
(2) by carrier impregnation in described maceration extract and the volume ratio of controlling solid-liquid be 1:2-1:3, soak 20-40min;
(3), to slowly dripping inorganic alkali solution in described maceration extract, until after pH value is 7.5,15-30min, after filtration, be dried, obtain described hydrolytic catalyst of carbonyl sulfur.
2. the preparation method of hydrolytic catalyst of carbonyl sulfur according to claim 1, it is characterized in that, front being also provided with of step (1), carrier is carried out to pretreated step, specifically comprise: carrier is immersed in diluted acid and soaks 12-18h, and the volume ratio of controlling the solid-liquid of described carrier and diluted acid is 1:2-1:3; To completing that described carrier after immersion carries out once or washing-baking step repeatedly, obtain pretreated carrier, wherein said bake out temperature is 100-110 DEG C.
3. the preparation method of hydrolytic catalyst of carbonyl sulfur according to claim 2, is characterized in that, described diluted acid is rare nitric acid, and the concentration of described rare nitric acid is 8wt%.
4. according to the preparation method of the arbitrary described hydrolytic catalyst of carbonyl sulfur of claim 1-3, it is characterized in that, in step (1), described soluble metallic salt is soluble ferric iron salt, and described inorganic alkaline solution is NaOH, potassium hydroxide.
5. according to the preparation method of the arbitrary described hydrolytic catalyst of carbonyl sulfur of claim 1-4, it is characterized in that, the concentration of described maceration extract is 1-10g/mL, and the concentration of described inorganic alkaline solution is 1-5wt%.
6. according to the preparation method of the arbitrary described hydrolytic catalyst of carbonyl sulfur of claim 1-5, it is characterized in that, described carrier is porous carrier, and its specific area is greater than 1000m
2/ g.
7. according to the preparation method of the arbitrary described hydrolytic catalyst of carbonyl sulfur of claim 1-6, it is characterized in that, described carrier is one or more any combination in active carbon, titanium oxide, zirconia, molecular sieve.
8. according to the preparation method of the arbitrary described hydrolytic catalyst of carbonyl sulfur of claim 1-7, it is characterized in that, in step (3), under stirring condition, drip described inorganic alkali solution.
9. according to the preparation method of the arbitrary described hydrolytic catalyst of carbonyl sulfur of claim 1-8, it is characterized in that, in step (3), be 2-4h described drying time, and described baking temperature is 100-105 DEG C.
10. the hydrolytic catalyst of carbonyl sulfur preparing according to the arbitrary described method of claim 1-9.
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Cited By (6)
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|---|---|---|---|---|
| CN110711555A (en) * | 2019-11-13 | 2020-01-21 | 中化工程集团环保有限公司 | Deodorizing agent for treating sulfur-containing malodorous gas and preparation method thereof |
| CN110813229A (en) * | 2019-11-25 | 2020-02-21 | 中冶南方都市环保工程技术股份有限公司 | Modification method and application of modified microcrystalline material desulfurizing agent based on ZSM-5 molecular sieve |
| CN113426289A (en) * | 2021-06-29 | 2021-09-24 | 松山湖材料实验室 | Hydrolysis adsorbent, blast furnace gas desulfurization method and desulfurization equipment |
| CN114405536A (en) * | 2022-01-27 | 2022-04-29 | 上海绿强新材料有限公司 | Hydrolysis catalyst for high-concentration carbon disulfide in steel plant gas and preparation and application thereof |
| CN116212625A (en) * | 2023-05-09 | 2023-06-06 | 明硕环境科技集团股份有限公司 | High-strength ferric hydroxide desulfurizing agent and preparation method thereof |
| CN117563631A (en) * | 2024-01-16 | 2024-02-20 | 陕西驭腾化学控股发展有限公司 | Titanium dioxide-silicon dioxide aerogel catalyst and preparation method and application thereof |
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Cited By (9)
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|---|---|---|---|---|
| CN110711555A (en) * | 2019-11-13 | 2020-01-21 | 中化工程集团环保有限公司 | Deodorizing agent for treating sulfur-containing malodorous gas and preparation method thereof |
| CN110813229A (en) * | 2019-11-25 | 2020-02-21 | 中冶南方都市环保工程技术股份有限公司 | Modification method and application of modified microcrystalline material desulfurizing agent based on ZSM-5 molecular sieve |
| CN113426289A (en) * | 2021-06-29 | 2021-09-24 | 松山湖材料实验室 | Hydrolysis adsorbent, blast furnace gas desulfurization method and desulfurization equipment |
| CN114405536A (en) * | 2022-01-27 | 2022-04-29 | 上海绿强新材料有限公司 | Hydrolysis catalyst for high-concentration carbon disulfide in steel plant gas and preparation and application thereof |
| CN114405536B (en) * | 2022-01-27 | 2024-05-28 | 上海绿强新材料有限公司 | Hydrolysis catalyst for high-concentration carbon disulfide in steel mill gas and preparation and application thereof |
| CN116212625A (en) * | 2023-05-09 | 2023-06-06 | 明硕环境科技集团股份有限公司 | High-strength ferric hydroxide desulfurizing agent and preparation method thereof |
| CN116212625B (en) * | 2023-05-09 | 2023-09-05 | 明硕环境科技集团股份有限公司 | High-strength ferric hydroxide desulfurizing agent and preparation method thereof |
| CN117563631A (en) * | 2024-01-16 | 2024-02-20 | 陕西驭腾化学控股发展有限公司 | Titanium dioxide-silicon dioxide aerogel catalyst and preparation method and application thereof |
| CN117563631B (en) * | 2024-01-16 | 2024-03-26 | 陕西驭腾化学控股发展有限公司 | Hydrolysis catalyst for blast furnace gas fine desulfurization, preparation method and application |
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