CN112755957A - High-efficiency dearsenic agent and preparation method thereof - Google Patents

High-efficiency dearsenic agent and preparation method thereof Download PDF

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CN112755957A
CN112755957A CN202110036606.0A CN202110036606A CN112755957A CN 112755957 A CN112755957 A CN 112755957A CN 202110036606 A CN202110036606 A CN 202110036606A CN 112755957 A CN112755957 A CN 112755957A
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agent
carrier
molecular sieve
dearsenization
drying
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CN112755957B (en
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陈凯
张先茂
王泽�
王瑜
王国兴
郑敏
王天元
金建涛
王栋斌
沈康文
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Wuhan Kelin Chemical Industry Group Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/18—Synthetic zeolitic molecular sieves
    • B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Catalysts (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

The invention discloses a high-efficiency dearsenization agent and a preparation method thereof, belonging to the technical field of dearsenization purification, wherein the dearsenization agent is composed of a 13x molecular sieve and a TS-1 titanium silicalite molecular sieve as a carrier I, an IVB group element as a carrier II, a VIII group fourth period element as a main agent I, a VIII group fifth and sixth period elements as a main agent II and a lanthanide as an auxiliary agent. The high-efficiency dearsenization agent provided by the invention has the advantages of high arsenic capacity, high dearsenization precision, good stability and long service life, and can be used for purification in the fields of natural gas, synthesis gas, flue gas, coal gas, blast furnace gas, coke oven gas, light gas liquid hydrocarbon, ethylene-rich gas and the like.

Description

High-efficiency dearsenic agent and preparation method thereof
Technical Field
The invention belongs to the technical field of dearsenification and purification, and particularly relates to a high-efficiency dearsenification agent and a preparation method thereof.
Background
In the ethylene industry, hydrocarbon cracking, catalytic reforming, hydrogenation processes and the like all contain a very small amount of arsenide, and although the content of the arsenide is very low, the arsenide can cause catalyst poisoning, so that the catalyst in the subsequent processes is inactivated, and the product quality is directly influenced. Therefore, in order to avoid the above problems, it is necessary to remove as much arsenic as possible, otherwise it cannot be directly applied to the subsequent chemical production.
Currently, the dearsenization agents commonly used in industry are mainly classified into copper-based dearsenization agents, nickel-based dearsenization agents, lead-based dearsenization agents, and manganese-based dearsenization agents.
Chinese patent document CN101591556B discloses a modified dearsenic agent and a preparation method thereof, comprising 15-30 wt% of copper oxide, 15-30 wt% of zinc oxide and 20-28 wt% of VIII group metal oxide; 5-10 wt% of alumina and the balance of inactive substances, and is characterized in that the dearsenization efficiency is ensured, the content of metal copper with higher price is reduced, and the content of other high-activity metals with lower price is correspondingly increased, thereby reducing the cost of the dearsenization agent as a whole.
Chinese patent document CN1115382C discloses a dearsenization agent for petroleum hydrocarbons, a preparation method and an application thereof, wherein the dearsenization agent consists of 5-20 wt% of Ni, 0.5-5.0 wt% of Mo or W and the balance of a carrier, NiO in an oxidation state hardly has dearsenization activity, and the dearsenization activity is achieved only by reducing for 8-48 hours at 150-450 ℃.
Chinese patent document CN101591554A discloses a normal-temperature composite desulfurization and dearsenization agent and a preparation method thereof, the desulfurization and dearsenization agent consists of a carrier and active components, the active components comprise lead oxide, magnetic iron oxide and copper oxide, and the carrier is gamma-Al2O3The desulfurization and dearsenization agent needs to be activated for 4 to 8 hours at 350 to 650 ℃.
Chinese patent document 101485971B discloses a normal temperature dearsenic agent, which is composed of 20-55 wt% of manganese dioxide, 10-45 wt% of ferric oxide and 10-35 wt% of carrier, and utilizes the synergistic effect between manganese dioxide and ferric oxide, and adds proper carrier and pore-expanding agent to obtain high arsenic content and high dearsenic efficiency.
Disclosure of Invention
The invention aims to obtain the dearsenization agent with the advantages of high arsenic capacity, good water resistance, excellent dearsenization performance and the like. The dearsenization agent is composed of a 13x molecular sieve and a TS-1 titanium silicalite molecular sieve as a carrier I, an IVB group element as a carrier II, a VIII group fourth period element as a main agent I, a VIII group fifth and sixth period elements as a main agent II and a lanthanide series element as an auxiliary agent; the IVB group element is at least one of Ti and Zr; the VIII group fourth period element is one of Fe, Co and Ni, and the VIII group fifth period element and the VIII group sixth period element are one of Ru, Rh, Pd, Os, Ir and Pt; the lanthanide is at least one of La, Ce, Nd and Sm.
The preparation method of the dearsenic agent comprises the following steps:
(1) uniformly mixing the 13x molecular sieve, the carrier II, the binder and the pore-forming agent, forming a rolling ball, drying, coating the TS-1 titanium silicalite molecular sieve on the outermost layer in a rolling ball forming mode, drying and roasting;
(2) soaking the product roasted in the step (1) in a solution of a main agent I and a main agent II in equal volume, drying and roasting;
(3) soaking the product roasted in the step (2) in the solution of the auxiliary agent in the same volume, drying and roasting;
(4) activating the product roasted in the step (3) for 2-4 h at 400 ℃ in a mixed atmosphere of hydrogen, nitrogen and steam, wherein the gas volume space velocity is 1000-2000 h-1And cooling to room temperature in nitrogen to obtain the dearsenic agent.
Furthermore, the mass ratio of the 13x molecular sieve to the TS-1 titanium silicalite molecular sieve in the carrier I is 1 (0.3-0.5).
Further, the dosage of the carrier II in the step (1) is determined by that Ti and Zr elements account for 10-25% of the mass of the carrier I.
Further, the drying and roasting modes in the step (1) are drying at 80-150 ℃ for 2-6 h and roasting at 550-750 ℃ for 2-4 h.
Further, the dosage of the main agent I in the step (2) is determined by that Fe, Co and Ni elements account for 3-10% of the total mass of the carrier I and the carrier II, and the dosage of the main agent II is determined by that Ru, Rh, Pd, Os, Ir and Pt elements account for 0.1-0.8% of the total mass of the carrier I and the carrier II.
Furthermore, the dosage of the auxiliary agent in the step (3) is determined by taking La, Ce, Nd and Sm as elements to account for 0.05-0.1% of the mass of the carrier I and the carrier II.
Further, the drying and roasting modes in the step (2) and the step (3) are roasting for 2-6 h at 80-150 ℃ and roasting for 2-4 h at 350-450 ℃.
The high-efficiency dearsenic agent and the preparation method thereof provided by the invention have the following advantages:
a. the method is characterized in that a 13x molecular sieve and a TS-1 titanium silicalite molecular sieve are used as a carrier I, elements Ti and Zr in an IVB group are used as a carrier II, the molecular sieve has strong adsorption performance, the 13x molecular sieve is an alkali metal aluminosilicate and has certain alkalinity, and belongs to a solid alkali, the TS-1 titanium silicalite molecular sieve has strong hydrophobicity due to the fact that strong-acid Al ions do not exist in a framework structure, the two are compounded, competitive adsorption of water vapor is reduced, adsorption of arsenic-containing substances is facilitated, the molecular sieve carrier is mixed and kneaded with the Ti and the Zr for molding, high-temperature roasting is carried out at 550-750 ℃, structural stability of the carrier is enhanced, and service life of the dearsenizer is prolonged. Meanwhile, the TS-1 titanium silicalite molecular sieve is coated on the outermost layer in a rolling ball forming mode, so that the adsorption of the dearsenization agent on water vapor is effectively reduced, the dearsenization precision of the dearsenization agent can be enhanced, and the service life of the dearsenization agent can be prolonged.
b. The high arsenic content is provided by using VIII group fourth period elements Fe, Co and Ni as a main agent I and VIII group fifth and sixth period elements Ru, Rh, Pd, Os, Ir and Pt as a main agent II and utilizing the strong arsenic absorption performance of the cheap metal main agent I, and the main agent II supplements the arsenic removal precision of the main agent I.
c. Lanthanide elements La, Ce, Nd and Sm are adopted as auxiliary agents, and strong activity of the auxiliary agents is utilized, and a small amount of lanthanide elements are added to promote the arsenic absorption characteristics of the main agent I and the main agent II.
d. The dearsenization agent is activated in the mixed atmosphere of hydrogen, nitrogen and steam, so that the double effects of expanding pores of the molecular sieve and reducing and activating the dearsenization agent can be achieved, the preparation process is simplified, and the cost is saved.
Detailed Description
The technical solution of the present invention is further defined below with reference to the specific embodiments, but the scope of the claims is not limited to the description.
Example 1
Dearsenicating agent 1 was prepared as follows:
(1) uniformly mixing 100g of 13x molecular sieve, 54g of titanium dioxide, pseudo-boehmite and hydroxymethyl cellulose, rolling ball forming, drying at 150 ℃ for 2h, coating 30g of TS-1 titanium silicalite molecular sieve on the outermost layer in a rolling ball forming mode, drying at 150 ℃ for 2h, and baking at 550 ℃ for 4 h;
(2) soaking the roasted product in the step (1) in 57.07gNi (NO) solution in equal volume3)2And 0.39g K2PtCl4Then baking the solution at 80 ℃ for 6h, and baking the solution at 450 ℃ for 2 h;
(3) soaking the roasted product of the step (2) in a solution of 0.28gLa (NO) in equal volume3)3·6H2Baking the mixture in the solution of O at 80 ℃ for 6h, and baking the mixture at 450 ℃ for 2 h;
(4) activating the product roasted in the step (3) for 2h at 400 ℃ in the mixed atmosphere of hydrogen, nitrogen and water vapor, wherein the gas space velocity is 1600h-1. The dearsenization agent is obtained after being cooled to room temperature in nitrogen and is marked as dearsenization agent 1.
Example 2
Dearsenicating agent 2 was prepared as follows:
(1) uniformly mixing 100g of 13x molecular sieve, 36g of titanium dioxide, silica sol and hydroxymethyl cellulose, rolling ball forming, drying at 80 ℃ for 6h, coating 45g of TS-1 titanium silicalite molecular sieve on the outermost layer in a rolling ball forming mode, drying at 80 ℃ for 6h, and roasting at 650 ℃ for 4 h;
(2) soaking the roasted product in the step (1) in 70.40g of Fe (NO) dissolved in the same volume3)3And 1.70g of ruthenium nitrate, and then baking the mixture at 90 ℃ for 4 hours and at 360 DEG C3h；
(3) Soaking the roasted product of the step (2) in a solution of 0.28gLa (NO) in equal volume3)3·6H2O and 0.21gCe (NO)3)3Then baking the solution at 90 ℃ for 4h, and baking the solution at 360 ℃ for 3 h;
(4) activating the product roasted in the step (3) for 4h at 400 ℃ in the mixed atmosphere of hydrogen, nitrogen and water vapor, wherein the gas space velocity is 1800h-1. The dearsenization agent is obtained after being cooled to room temperature in nitrogen and is marked as dearsenization agent 2.
Example 3
Dearsenicating agent 3 was prepared as follows:
(1) uniformly mixing 100g of 13x molecular sieve, 25g of titanium dioxide, 20g of zirconium dioxide, alumina sol and sesbania powder, rolling the mixture into a ball, drying the ball at 120 ℃ for 4 hours, coating 50g of TS-1 titanium silicalite molecular sieve on the outermost layer in a rolling ball forming mode, drying the ball at 120 ℃ for 4 hours, and roasting the ball at 750 ℃ for 2 hours;
(2) soaking the roasted product of the step (1) in a solution containing 18.14g of Co (NO) in equal volume3)2And 2.18gRh (NO)3)3Then baking the solution at 110 ℃ for 3h, and baking the solution at 420 ℃ for 2 h;
(3) soaking the roasted product of the step (2) in a solution of 0.45gCe (NO) in equal volume3)3Then baking the solution at 110 ℃ for 3h, and baking the solution at 420 ℃ for 2 h;
(4) activating the product roasted in the step (3) for 3h at 400 ℃ in the mixed atmosphere of hydrogen, nitrogen and water vapor, wherein the gas space velocity is 1200h-1. The dearsenization agent is obtained after being cooled to room temperature in nitrogen and is marked as dearsenization agent 3.
Example 4
Dearsenicating agent 4 was prepared as follows:
(1) uniformly mixing 100g of 13x molecular sieve, 18g of zirconium dioxide, pseudo-boehmite and sesbania powder, rolling the mixture into balls, drying the balls at 100 ℃ for 5 hours, coating 35g of TS-1 titanium silicalite molecular sieve on the outermost layer in a rolling ball forming mode, drying the balls at 100 ℃ for 5 hours, and roasting the balls at 600 ℃ for 3 hours;
(2) soaking the roasted product in the step (1) in 37.96g of Co (NO) dissolved in the same volume3)2And 2.65gPd (NO)3)2In solution of (2), thenBaking at 150 deg.C for 2 hr, and baking at 350 deg.C for 4 hr;
(3) soaking the roasted product of the step (2) in a solution of 0.17gNd (NO) in equal volume3) 3And 0.17gSm (NO)3) 3Then baking the solution at 150 ℃ for 2h, and baking the solution at 350 ℃ for 4 h;
(4) activating the product roasted in the step (3) for 4h at 400 ℃ in the mixed atmosphere of hydrogen, nitrogen and water vapor, wherein the gas space velocity is 1500h-1. The dearsenization agent is obtained after being cooled to room temperature in nitrogen and is marked as dearsenization agent 4.
Example 5
Dearsenicating agent 5 was prepared as follows:
(1) uniformly mixing 100g of 13x molecular sieve, 35g of titanium dioxide, 19g of zirconium dioxide, pseudo-boehmite and hydroxymethyl cellulose, rolling ball forming, drying at 140 ℃ for 3h, coating 40g of TS-1 titanium silicalite molecular sieve on the outermost layer in a rolling ball forming mode, drying at 140 ℃ for 3h, and roasting at 700 ℃ for 2 h;
(2) soaking the roasted product in the step (1) in a solution of 42.12g of Ni (NO) in equal volume3)2And 1.04gH2IrCl6·6H2Baking the mixture in the solution of O at 120 ℃ for 4h, and baking the mixture at 380 ℃ for 3 h;
(3) soaking the roasted product of the step (2) in a solution of 0.26gSm (NO) in equal volume3)3Then baking the solution at 120 ℃ for 4h, and baking the solution at 380 ℃ for 3 h;
(4) activating the product roasted in the step (3) for 4h at 400 ℃ in the mixed atmosphere of hydrogen, nitrogen and water vapor, wherein the gas space velocity is 2000h-1. The dearsenization agent is obtained after being cooled to room temperature in nitrogen and is marked as dearsenization agent 5.
Example 6
The dearsenization agent 6 was prepared as follows:
(1) uniformly mixing 100g of 13x molecular sieve, 35g of zirconium dioxide, silica sol and sesbania powder, rolling the mixture into balls, drying the balls at 130 ℃ for 4 hours, coating 30g of TS-1 titanium silicalite molecular sieve on the outermost layer in a rolling ball forming mode, drying the balls at 130 ℃ for 4 hours, and roasting the balls at 720 ℃ for 2 hours;
(2) soaking the roasted product in the step (1) in a solution containing 42.78g of Fe (NO) in equal volume3)3And 1.95gNa2[OsCl6]Baking the solution at 100 ℃ for 5 hours and baking the solution at 400 ℃ for 4 hours;
(3) soaking the roasted product of the step (2) in a solution of 0.30gNd (NO) in equal volume3) 3Baking the solution at 100 ℃ for 5 hours and baking the solution at 400 ℃ for 4 hours;
(4) activating the product roasted in the step (3) for 3h at 400 ℃ in the mixed atmosphere of hydrogen, nitrogen and water vapor, wherein the gas space velocity is 1000h-1. The dearsenization agent is obtained after being cooled to room temperature in nitrogen and is marked as dearsenization agent 6.
The arsenic removal effect of the dearsenization agent prepared in the above example was evaluated: arsenic trioxide reacts with zinc material and sulfuric acid to prepare high-concentration arsine gas, and the high-concentration arsine gas is added into a glass steel cylinder to prepare feed gas with the arsine content reaching 1500 ppb. 3mL of 20-40 mesh particles obtained by grinding the dearsenic agent prepared in the embodiments 1-6 are respectively filled into a quartz reaction tube, and arsine gas is enabled to pass through the reaction tube at a space velocity of 1000h-1The dearsenification data of each dearsenification agent obtained after 72 hours of operation are shown in Table 1. Wherein the dearsenification rate = (inlet arsenic concentration-outlet arsenic concentration)/inlet arsenic concentration = 100%.
TABLE 1 dearsenification data for dearsenification agents of examples 1-6
Examples Dearsenification rate%
1 98.7
2 99.2
3 99.8
4 99.9
5 100
6 98.9

Claims (7)

1. The high-efficiency dearsenization agent is characterized in that the dearsenization agent is composed of a 13x molecular sieve and a TS-1 titanium silicalite molecular sieve as a carrier I, an IVB group element as a carrier II, a VIII group fourth period element as a main agent I, a VIII group fifth and sixth period elements as a main agent II and a lanthanide series element as an auxiliary agent; the IVB group element is at least one of Ti and Zr; the VIII group fourth period element is one of Fe, Co and Ni, and the VIII group fifth period element and the VIII group sixth period element are one of Ru, Rh, Pd, Os, Ir and Pt; the lanthanide is at least one of La, Ce, Nd and Sm; the preparation method comprises the following steps:
(1) uniformly mixing the 13x molecular sieve, the carrier II, the binder and the pore-forming agent, forming a rolling ball, drying, coating the TS-1 titanium silicalite molecular sieve on the outermost layer in a rolling ball forming mode, drying and roasting;
(2) soaking the product roasted in the step (1) in a solution of a main agent I and a main agent II in equal volume, drying and roasting;
(3) soaking the product roasted in the step (2) in the solution of the auxiliary agent in the same volume, drying and roasting;
(4) activating the product roasted in the step (3) for 2-4 h at 400 ℃ in a mixed atmosphere of hydrogen, nitrogen and steam, wherein the gas volume space velocity is 1000-2000 h-1And cooling to room temperature in nitrogen to obtain the dearsenic agent.
2. The method of claim 1, wherein the mass ratio of the 13x molecular sieve to the TS-1 titanium silicalite molecular sieve in the carrier I is 1 (0.3-0.5).
3. The method according to claim 1, wherein the amount of the carrier II is determined by that Ti and Zr account for 10-25% of the mass of the carrier I.
4. The method according to claim 1, wherein the amount of the base compound I is determined by the amount of Fe, Co and Ni elements accounting for 3-10% of the total mass of the carrier I and the carrier II, and the amount of the base compound II is determined by the amount of Ru, Rh, Pd, Os, Ir and Pt elements accounting for 0.1-0.8% of the total mass of the carrier I and the carrier II.
5. The method according to claim 1, wherein the amount of the auxiliary agent is determined by taking La, Ce, Nd and Sm as elements accounting for 0.05-0.1% of the mass of the carrier I and the carrier II.
6. The method as claimed in claim 1, wherein the drying and baking in step (1) is performed at 80-150 ℃ for 2-6 h and at 550-750 ℃ for 2-4 h.
7. The method as claimed in claim 1, wherein the drying and roasting in step (2) and step (3) are carried out at 80-150 ℃ for 2-6 h and at 350-450 ℃ for 2-4 h.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004082000A (en) * 2002-08-27 2004-03-18 Toyota Motor Corp Exhaust gas cleaning catalyst
CN104624223A (en) * 2015-02-09 2015-05-20 北京北大先锋科技有限公司 Continuous arsenic removal catalyst for industrial tail gas purification and preparation method thereof
CN110639466A (en) * 2019-09-30 2020-01-03 四川润和催化新材料股份有限公司 Dearsenic adsorbent and preparation method thereof
CN111672533A (en) * 2020-06-28 2020-09-18 北京化工大学 Dearsenifying catalyst and its prepn

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004082000A (en) * 2002-08-27 2004-03-18 Toyota Motor Corp Exhaust gas cleaning catalyst
CN104624223A (en) * 2015-02-09 2015-05-20 北京北大先锋科技有限公司 Continuous arsenic removal catalyst for industrial tail gas purification and preparation method thereof
CN110639466A (en) * 2019-09-30 2020-01-03 四川润和催化新材料股份有限公司 Dearsenic adsorbent and preparation method thereof
CN111672533A (en) * 2020-06-28 2020-09-18 北京化工大学 Dearsenifying catalyst and its prepn

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