CN110813232A - Sulfur-resistant adsorbent for purifying yellow phosphorus tail gas and preparation method thereof - Google Patents
Sulfur-resistant adsorbent for purifying yellow phosphorus tail gas and preparation method thereof Download PDFInfo
- Publication number
- CN110813232A CN110813232A CN201911066917.0A CN201911066917A CN110813232A CN 110813232 A CN110813232 A CN 110813232A CN 201911066917 A CN201911066917 A CN 201911066917A CN 110813232 A CN110813232 A CN 110813232A
- Authority
- CN
- China
- Prior art keywords
- adsorbent
- sulfur
- tail gas
- yellow phosphorus
- tolerant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/55—Compounds of silicon, phosphorus, germanium or arsenic
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a sulfur-resistant adsorbent for purifying yellow phosphorus tail gas and a preparation method thereof. The total phosphorus in the yellow phosphorus tail gas can be adsorbed on a bed layer at the low temperature of not more than 200 ℃, and the yellow phosphorus tail gas is led out of an adsorbent bed layer after being oxidized by introducing air. The adsorbent has good capability of tolerating sulfur-containing impurities in the yellow phosphorus tail gas. The adsorbent can be desorbed under the condition of normal temperature, has good desorption performance, does not influence the dephosphorization performance of the yellow phosphorus tail gas due to the existence of hydrogen sulfide or other impurities, and can realize front-end dephosphorization and then desulfurization in industrial application. The total phosphorus of the purified gas is about 1ppm, and the requirement of preparing carbon chemical synthesis gas is met.
Description
Technical Field
The invention relates to an adsorbent, in particular to a sulfur-resistant adsorbent for purifying yellow phosphorus tail gas.
Background
During the production of yellow phosphorus, phosphate ore is reduced by coke in a high-temperature electric furnace, carbon is discharged from the electric furnace from the upper part in the form of CO and phosphorus mainly in the form of elemental phosphorus, and other species are discharged from the electric furnace from the lower part in the form of slag. After the high-temperature gas is sprayed and cooled by a plurality of stages of water, phosphorus steam enters a phosphorus receiving tank in a liquid state, and uncondensed furnace gas is called yellow phosphorus tail gas. The phosphorus ore has complex components, and the yellow phosphorus tail gas also contains a large amount of water vapor and impurities such as CH4, CO2, N2, O2, AsH3, HF, total sulfur, total phosphorus and the like besides a large amount of CO. The total sulfur is H2S and organic sulfur, wherein H2S is the main sulfur. The total phosphorus is elemental phosphorus and PH 3. The yellow phosphorus tail gas is rich in a large amount of CO, so that combustion heat of the yellow phosphorus tail gas can be utilized and the yellow phosphorus tail gas can be used as a carbon chemical synthesis raw material, but due to sulfur and phosphorus impurities contained in the yellow phosphorus tail gas, the yellow phosphorus tail gas is always difficult to reuse in an industrial mode. At present, most yellow phosphorus enterprises still adopt a simple and extensive emptying combustion mode for treating yellow phosphorus tail gas, resources are wasted, and the impurities such as total phosphorus and total sulfur are converted into phosphorus oxide and SO2 after combustion, and the like, which can cause serious pollution to the environment. 80% of yellow phosphorus in the world is produced in China. In recent years, the environmental protection requirement of China is increasingly strict, and the requirement on the purification of yellow phosphorus tail gas is urgent. If the yellow phosphorus tail gas can be purified and then combusted, the heat energy contained in CO is utilized, and even purified CO is used as the raw material gas for oxo synthesis, so that huge economic and environmental protection values are brought. However, the yellow phosphorus tail gas has complex composition and high purification difficulty, and especially, the removal of total phosphorus is the most difficult.
At present, the total phosphorus removal is mainly carried out by adopting an adsorption method, and the method is divided into a catalytic oxidation adsorption method and a temperature swing adsorption method. The catalytic oxidation adsorption method is classified into a liquid-phase catalytic oxidation method and a solid-phase catalytic oxidation method. In the early foreign countries, liquid-phase catalytic oxidation is mainly adopted for dephosphorization. For example, SU618124 discloses a liquid phase absorption process for the absorption of phosphine and hydrogen sulfide using an aqueous sulfuric acid solution of sodium sulfate, sodium chromate, copper sulfate. SU570386 discloses a method for absorbing phosphine and hydrogen sulfide in calcium carbide tail gas by using hydrochloric acid aqueous solution of ferrous chloride, cuprous chloride and mercuric chloride. The liquid phase method generally contains heavy metals such as Cr, Hg and the like which have great toxicity to human bodies, and brings serious environmental pollution. The solid-phase catalytic oxidation is an important research hotspot in the later period because the solid-phase catalytic oxidation is environment-friendly and does not need to process a large amount of solution. SU413968 reports a NaX supported copper-zirconium catalyst for removing phosphine by catalytic oxidation, but at temperatures as high as 700 ℃. CN101695653 discloses a preparation method of a modified activated carbon adsorbent capable of treating low-concentration phosphine, which adopts an activated carbon carrier after ultrasonic washing, and active components of copper and zinc are impregnated by ultrasonic, and promoters of cerium and lanthanum are added, but the adsorption capacity of the adsorbent is obviously reduced along with the prolonging of time. CN1398658A discloses a method for purifying yellow phosphorus tail gas by fixed bed catalytic oxidation, which is based on the principle that the strong reducibility of phosphine reacts with active components on an active carbon carrier in an aerobic atmosphere to generate phosphorus oxide which is adsorbed on active carbon to achieve the purification purpose. After the phosphorus oxide is adsorbed and saturated, the phosphorus oxide is eluted from the activated carbon in a steam washing mode, so that the catalyst can be regenerated. However, the regeneration process causes a gradual loss of active sites, and after repeated washing of the catalyst bed, the phosphorus content of the catalyst decreases rapidly and eventually leads to deactivation. In other adsorption methods, US5182088 reports that an adsorbent prepared by using copper and zinc oxides as active components and adding silver and mercury oxides as promoters by a coprecipitation method has a large increase in adsorption capacity, but has high cost and heavy metal toxicity.
In these more representative purification processes, either the catalyst or the adsorbent needs to be regenerated. Not only does the regeneration process add to the complexity of the equipment and operation, in the case of catalysts, repeated regenerations tend to cause a gradual deactivation of the active sites. The patent application No. 201110457379.5 describes a method for preparing a catalyst for continuous dephosphorization, which overcomes the disadvantages of the prior catalyst that needs to be regenerated, and realizes continuous dephosphorization without regeneration. However, because the catalyst selects the activated carbon carrier with high specific surface and a microporous structure as a main component, the phosphorus oxide as a reaction product must be transferred out of the system along with the reaction atmosphere at high temperature (300-400 ℃) and high water vapor (the preset volume percentage of the water vapor to the yellow phosphorus tail gas is 10: 90-50: 50), so that the effect of continuous dephosphorization can be achieved. Heating large volumes of gas to high temperatures increases energy consumption, and therefore one of the technical problems currently being addressed by researchers in this field is: the deep dephosphorization adsorbent for purifying the yellow phosphorus tail gas can deeply dephosphorize at a lower reaction temperature, such as 200 ℃, so that the operation energy consumption is reduced, the cost for purifying the yellow phosphorus tail gas is reduced, and the yellow phosphorus tail gas has a wider application space.
Disclosure of Invention
In view of the above-mentioned drawbacks and problems of the prior art, an object of the embodiments of the present invention is to provide a sulfur-tolerant adsorbent for purifying yellow phosphorus tail gas and a method for preparing the same.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a sulfur-resistant adsorbent for purifying yellow phosphorus tail gas,
s1: preparing a carrier; mixing the raw materials with an activated carbon molecular sieve, adding water to prepare a viscous paste, extruding and forming in a press, and drying to obtain a carrier;
s2: preparing a steeping fluid;
s3: dipping; putting the carrier into the impregnation liquid, impregnating for 4 hours under the vacuum-pumping condition, stopping vacuum-pumping, adding a precipitator, and adjusting the pH value to be alkaline;
s4: aging the precipitate, filtering and separating;
s5: drying and roasting;
s6: and obtaining a finished product.
In the step S1, the raw material is one or more of kaolin, clay and bentonite.
Wherein, in the step S1, the specific surface area of the activated carbon molecular sieve is 800-1500 square meters per gram.
In step S2, the dipping solution is non-oxide metal salt with the concentration of 0.1-0.5 mol/L.
In step S3, the precipitating agent is an aqueous solution of potassium dihydrogen phosphate at a saturated concentration.
Wherein, in the step S4, the pH value of the solution is kept between 9 and 10 during precipitation and aging.
In step S4, the precipitation aging time is 12 hours.
In the step S5, the drying temperature is 100-150 ℃, and the drying time is 3 h; the roasting temperature is 220-280 ℃, and the roasting time is 2-4 h.
The invention also protects a sulfur-resistant adsorbent for purifying the yellow phosphorus tail gas, which is prepared by the preparation method.
The sulfur-resistant adsorbent for purifying the yellow phosphorus tail gas and the preparation method thereof provided by the invention have the advantages that the prepared adsorbent can deeply remove the total phosphorus in the yellow phosphorus tail gas under the condition of low temperature, the adsorption capacity is high, the desorption can be realized under the condition of normal temperature, the desorption performance is good, the dephosphorization performance of the yellow phosphorus tail gas is not influenced by the existence of hydrogen sulfide or other impurities in the yellow phosphorus tail gas, and the front-end dephosphorization and the desulfurization can be realized in the industrial application of the adsorbent. The main impurities left after the total phosphorus removal of the yellow phosphorus tail gas are hydrogen sulfide and organic sulfur, and can be conveniently removed by the existing mature desulfurization process in industry, the dephosphorization problem is solved by the most convenient process with the lowest cost, the core problem of yellow phosphorus tail gas purification is solved, and the utilization of the yellow phosphorus tail gas reaches the lowest purification cost. The total phosphorus of the purified gas is about 1ppm, and the requirement of preparing carbon chemical synthesis gas is met.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As an example, a method for preparing a sulfur-tolerant adsorbent for purifying yellow phosphorus tail gas,
s1: preparing a carrier; mixing the raw materials with an activated carbon molecular sieve, adding water to prepare a viscous paste, extruding and forming in a press, and drying to obtain a carrier; the raw material is one or more of kaolin, clay and bentonite. The specific surface area of the activated carbon molecular sieve is 800 plus 1500 square meters per gram. The carbon atoms on the activated carbon molecular sieve are positioned on the inner surface and the outer surface to form a unique adsorption structure, and the activated carbon molecular sieve is called as a surface solid. The pores of the adsorbent are directly opened on the surface of the particles and the pore size distribution is concentrated, so that the diffusion path of the adsorbent reaching the adsorption site is shorter than that of active carbon and has larger driving force. The 10-30 mu m ultra-fine particles are combined together to form rich spaces, and the size of the spaces and the ultra-fine particles are in the same order of magnitude, so that a larger specific surface area is created. The more developed specific surface area and narrower pore size distribution make it have faster adsorption and desorption speeds and larger adsorption capacity than activated carbon. The activated carbon molecular sieve has the characteristics, so that the activated carbon molecular sieve can be used as an adsorbent carrier, the efficiency of adsorption reaction can be increased, the loading capacity of active components is reduced, and the derivation of reaction products is facilitated. But the price is high, and the neutral price ratio is low in practical application. The kaolin, the clay or the bentonite have certain pore structure and adsorption effect, are low in price and easy to obtain, and tests show that the kaolin, the clay or the bentonite are resistant to hydrogen sulfide and organic sulfur in the yellow phosphorus tail gas, which is very important for purifying the yellow phosphorus tail gas.
S2: preparing a steeping fluid; the impregnation liquid is non-oxide metal salt with the concentration of 0.1-0.5 mol/L. The non-oxide metal salt is present as an active component of the adsorbent. Preferably, it is an iron or copper salt. Iron salts and are selected from ferric chloride or ferric nitrate. The copper salt may be selected from copper chloride or copper nitrate.
S3: dipping; putting the carrier into the impregnation liquid, adopting a vacuum impregnation method, impregnating for 4 hours under the vacuum condition, stopping vacuumizing, adding a precipitator which is a monopotassium phosphate aqueous solution with saturated concentration, and adjusting the pH value to be alkaline;
s4: and (3) precipitation aging, wherein a precipitation method is used, the pH value of the solution is kept between 9 and 10 during the precipitation aging, and the precipitation aging time is 12 hours, such as when iron salt or copper salt is used as non-oxide metal salt, the formed iron phosphate or copper phosphate is precipitated on the carrier. Filtering and separating to obtain the aged carrier.
S5: drying and roasting; and drying and roasting the carrier separated in the S4. The drying temperature is 100-150 ℃, and the drying time is 3 h; the roasting temperature is 220-280 ℃, and the roasting time is 2-4 h. The drying temperature is preferably 120 ℃.
S6: and obtaining the finished product adsorbent. The adsorbent can adsorb total phosphorus in the yellow phosphorus tail gas, including phosphine and elemental phosphorus, on the adsorbent, and when the adsorption is carried out, the total phosphorus is oxidized into phosphorus oxide to be adsorbed on a bed layer, and the phosphorus oxide is transferred out of the bed layer in a vacuumizing mode, so that the purpose of removing the total phosphorus in the yellow phosphorus tail gas is achieved; the adsorbent is able to withstand the presence of sulphur and other impurities in the yellow phosphorus tail gas atmosphere. And (3) adsorbing the total phosphorus in the tail gas on an adsorbent, replacing the bed layer with nitrogen after saturated adsorption is achieved, introducing air to oxidize the total phosphorus into phosphorus oxide, vacuumizing and guiding out the bed layer, and finishing regeneration of the adsorbent.
The steps have the advantages of simple preparation process, easy operation, low preparation cost and industrialization suitability.
A sulfur-resistant adsorbent for purifying yellow phosphorus tail gas is prepared by the preparation method. The adsorbent is suitable for removing total phosphorus impurities from yellow phosphorus tail gas. The total phosphorus is collected outside the reaction bed in the form of dilute phosphoric acid after catalytic conversion. The reaction temperature of the whole process is not more than 200 ℃, thereby reducing energy consumption. The adsorbent disclosed by the invention has high adsorption activity and lower required active components. In the adsorption process, total phosphorus in the yellow phosphorus tail gas, including phosphine and simple substance phosphorus, is adsorbed, and is vacuumized after being adsorbed to a certain degree, so that the pressure can be changed for desorption, and the desorbed adsorbent is regenerated and can be reused. And the effect of resisting sulfide is good, and the reaction with hydrogen sulfide does not occur in operation. The appearance shape is kept stable in the reaction atmosphere with total phosphorus and hydrogen sulfide, and the carrier and the active component are not changed before and after the reaction through XRD characterization.
Example 1:
weighing 800g of clay and 80g of activated carbon molecular sieve, granulating, physically mixing, adding water, blending into thick paste, extruding the paste in a press machine for molding, drying to remove water, and finally controlling the water content of the prepared strip-shaped carrier to be between 2 and 5 percent.
34.10g of copper nitrate was weighed out to prepare 2L of an aqueous solution, 800g of the carrier was added thereto, and the mixture was immersed for 4 hours under a vacuum condition. Stopping vacuumizing, slowly adding 500ml of potassium dihydrogen phosphate aqueous solution with saturated concentration, adjusting the pH value to 9, aging for 12h, filtering, drying at 120 ℃, and roasting at 240 ℃ to obtain the finished sulfur-resistant adsorbent.
The adsorbent was packed in a fixed bed reactor. The fixed bed catalytic reactor temperature was set at 180 ℃; the space velocity is set at 6000h-1. 770ppm of total phosphorus and 3500ppm of total sulfur before purifying the yellow phosphorus tail gas. After the yellow phosphorus tail gas is introduced into a fixed bed reactor for purification, the total phosphorus content in the yellow phosphorus tail gas is 1.1ppm, and the total sulfur content is unchanged. The condensed and washed collection after purification is only diluted phosphoric acid. The reaction is continued for 200h, and the adsorption activity is unchanged.
Example 2:
weighing 200g of kaolin and 20g of activated carbon molecular sieve, granulating, physically mixing, adding water, blending into thick paste, extruding the paste in a press machine for molding, drying to remove water, and finally controlling the water content of the prepared strip-shaped carrier to be between 2 and 5 percent.
Weighing 13.52g of ferric chloride, preparing into 500ml of aqueous solution, adding 200g of carrier, soaking for 4h under the vacuum condition, stopping vacuumizing, slowly adding 100ml of potassium dihydrogen phosphate aqueous solution with saturated concentration, adjusting the pH value to 10, aging for 12h, filtering, drying at 120 ℃, and roasting at 240 ℃ to obtain the finished sulfur-resistant adsorbent.
The adsorbent was packed in a fixed bed reactor. The fixed bed catalytic reactor temperature was set at 170 ℃; the space velocity is set at 10000h-1. The total phosphorus is 890ppm and the total sulfur is 3000ppm before the yellow phosphorus tail gas is purified. After the yellow phosphorus tail gas is introduced into a fixed bed reactor for purification, the total phosphorus content in the yellow phosphorus tail gas is 0.9ppm, the total sulfur content is unchanged, and the condensed, washed and collected matter after purification is only dilute phosphoric acid. The reaction is continued for 150 hours, and the adsorption activity is unchanged.
Example 3:
preparation of the carrier: weighing 400g of bentonite and 40g of activated carbon molecular sieve, granulating, physically mixing, adding water, blending into thick paste, extruding the paste in a press machine for molding, drying to remove water, and finally controlling the water content of the prepared strip-shaped carrier to be between 2 and 5 percent.
The preparation process of the adsorbent comprises the following steps: 13.64g of copper chloride was weighed out to prepare 1L of an aqueous solution, 400g of the carrier was added thereto, and the mixture was immersed for 4 hours under a vacuum condition. Stopping vacuumizing, slowly adding potassium dihydrogen phosphate aqueous solution with saturated concentration, adjusting the pH value to 9, aging for 12h, filtering, drying at 120 ℃, and roasting at 240 ℃ to obtain the finished sulfur-resistant adsorbent.
The adsorbent was packed in a fixed bed reactor. The fixed bed catalytic reactor temperature was set at 190 ℃; the space velocity is set at 5000h-1. The total phosphorus content is 830ppm and the total sulfur content is 2000ppm before the yellow phosphorus tail gas is purified. Purifying by introducing into fixed bed reactorThen, the total phosphorus in the yellow phosphorus tail gas is 0.9ppm, and the total sulfur content is unchanged. The condensed and washed collection after purification is only diluted phosphoric acid. The reaction is continued for 180 hours, and the adsorption activity is unchanged.
Example 4:
preparation of the carrier: weighing 100g of kaolin, 100g of clay, 100g of bentonite and 30g of activated carbon molecular sieve, granulating, physically mixing, adding water, blending into a viscous paste, extruding in a press to form strips, drying to remove water, and finally controlling the water content of the prepared strip-shaped carrier to be 2-5%.
The preparation process of the adsorbent comprises the following steps: 48.48g of ferric nitrate was weighed out to prepare 1L of an aqueous solution, 300g of the carrier was added thereto, and the mixture was immersed for 4 hours under a vacuum condition. Stopping vacuumizing, slowly adding potassium dihydrogen phosphate aqueous solution with saturated concentration, adjusting pH value to about 10, aging for 12h, filtering, drying at 120 ℃, and roasting at 240 ℃ to obtain the finished sulfur-resistant adsorbent.
The adsorbent was packed in a fixed bed reactor. The fixed bed catalytic reactor temperature was set at 160 ℃; the space velocity is set at 5000h-1. The total phosphorus content before the purification of the yellow phosphorus tail gas is 770ppm and the total sulfur content is 1800 ppm. After the yellow phosphorus tail gas is introduced into a fixed bed reactor for purification, the total phosphorus content in the yellow phosphorus tail gas is 0.75ppm, and the total sulfur content is unchanged. The condensed and washed collection after purification is only diluted phosphoric acid. The reaction is continued for 220h, and the adsorption activity is unchanged.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. A preparation method of a sulfur-resistant adsorbent for purifying yellow phosphorus tail gas is characterized by comprising the following steps:
s1: preparing a carrier; mixing the raw materials with an activated carbon molecular sieve, adding water to prepare a viscous paste, extruding and forming in a press, and drying to obtain a carrier;
s2: preparing a steeping fluid;
s3: dipping; putting the carrier into the impregnation liquid, impregnating for 4 hours under the vacuum-pumping condition, stopping vacuum-pumping, adding a precipitator, and adjusting the pH value to be alkaline;
s4: aging the precipitate, filtering and separating;
s5: drying and roasting;
s6: and obtaining a finished product.
2. The method for preparing the sulfur-tolerant adsorbent for purifying the yellow phosphorus tail gas according to claim 1, wherein the sulfur-tolerant adsorbent comprises the following components: in the step S1, the raw material is one or more of kaolin, clay and bentonite.
3. The method for preparing the sulfur-tolerant adsorbent for purifying the yellow phosphorus tail gas according to claim 2, wherein the sulfur-tolerant adsorbent comprises the following components: in the step S1, the specific surface area of the activated carbon molecular sieve is 800-1500 square meters per gram.
4. The method for preparing the sulfur-tolerant adsorbent for purifying the yellow phosphorus tail gas according to claim 3, wherein the sulfur-tolerant adsorbent comprises the following components in percentage by weight: in the step S2, the dipping solution is non-oxide metal salt with the concentration of 0.1-0.5 mol/L.
5. The method for preparing the sulfur-tolerant adsorbent for purifying the yellow phosphorus tail gas according to claim 4, wherein the sulfur-tolerant adsorbent comprises the following components in percentage by weight: in step S3, the precipitant is an aqueous solution of potassium dihydrogen phosphate with a saturated concentration.
6. The method for preparing the sulfur-tolerant adsorbent for purifying the yellow phosphorus tail gas according to claim 5, wherein the sulfur-tolerant adsorbent comprises the following components in percentage by weight: in the step S4, the pH value of the solution is kept between 9 and 10 during precipitation and aging.
7. The method for preparing the sulfur-tolerant adsorbent for purifying the yellow phosphorus tail gas according to claim 6, wherein the sulfur-tolerant adsorbent comprises the following components in percentage by weight: in the step S4, the precipitation aging time is 12 h.
8. The method for preparing the sulfur-tolerant adsorbent for purifying the yellow phosphorus tail gas according to claim 7, wherein the sulfur-tolerant adsorbent comprises the following components: in the step S5, the drying temperature is 100-150 ℃, and the drying time is 3 h; the roasting temperature is 220-280 ℃, and the roasting time is 2-4 h.
9. A sulfur-resistant adsorbent for purifying yellow phosphorus tail gas is characterized in that: the adsorbent is prepared by the preparation method of any one of claims 1 to 8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911066917.0A CN110813232A (en) | 2019-11-04 | 2019-11-04 | Sulfur-resistant adsorbent for purifying yellow phosphorus tail gas and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911066917.0A CN110813232A (en) | 2019-11-04 | 2019-11-04 | Sulfur-resistant adsorbent for purifying yellow phosphorus tail gas and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110813232A true CN110813232A (en) | 2020-02-21 |
Family
ID=69552295
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911066917.0A Pending CN110813232A (en) | 2019-11-04 | 2019-11-04 | Sulfur-resistant adsorbent for purifying yellow phosphorus tail gas and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110813232A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114471743A (en) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | Advanced oxidation catalyst containing ferric phosphate and preparation method thereof |
| CN114471634A (en) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | Catalytic material for catalytic oxidation and preparation method and application thereof |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86108921A (en) * | 1986-12-29 | 1988-07-20 | 山东省环境保护科学研究所 | Composite inorganic adsorbents and preparation method thereof |
| JP2007021318A (en) * | 2005-07-14 | 2007-02-01 | Japan Pionics Co Ltd | Treatment method and apparatus of exhaust gas |
| US20110185899A1 (en) * | 2010-02-02 | 2011-08-04 | Battelle Memorial Institute | Methods for Abatement of Arsenic and Phosphorous Contaminants From Fuel Gases Prior to Gasification |
| CN102775018A (en) * | 2012-07-25 | 2012-11-14 | 华南理工大学 | Phosphorus removing and coupling process of sewage sludge treatment |
| CN103182316A (en) * | 2011-12-30 | 2013-07-03 | 北京北大先锋科技有限公司 | Catalyst for dephosphorizing yellow phosphorus tail gas and preparation method thereof |
| CN103316624A (en) * | 2013-06-08 | 2013-09-25 | 华烁科技股份有限公司 | Dephosphorization agent and preparation method thereof |
| CN104069734A (en) * | 2013-03-26 | 2014-10-01 | 北京北大先锋科技有限公司 | Dephosphorization catalytic reaction process and catalyst for yellow phosphorus tail gas |
| CN104098094A (en) * | 2014-07-26 | 2014-10-15 | 淮北市森化碳吸附剂有限责任公司 | Active carbon for adsorbing phosphine and preparation method of active carbon |
| CN104338432A (en) * | 2013-07-30 | 2015-02-11 | 湖南华望熏蒸消毒有限公司 | Phosphine gas treatment agent and preparation method thereof |
| CN104492375A (en) * | 2014-12-15 | 2015-04-08 | 西南化工研究设计院有限公司 | Adsorbent for recovering CO from industrial exhaust gas as well as preparation method and application of adsorbent |
| CN108993400A (en) * | 2018-09-14 | 2018-12-14 | 河南环宇石化装备科技股份有限公司 | A kind of preparation method of the high-efficiency adsorbent of separation of nitrogen-methane |
| CN109603741A (en) * | 2019-01-16 | 2019-04-12 | 武汉禾谷环保有限公司 | A kind of Dephosphorising agent and preparation method thereof |
| CN209076673U (en) * | 2018-09-13 | 2019-07-09 | 河南环宇石化装备科技股份有限公司 | A kind of yellow phosphoric tail gas adsorbent preparation facilities |
-
2019
- 2019-11-04 CN CN201911066917.0A patent/CN110813232A/en active Pending
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86108921A (en) * | 1986-12-29 | 1988-07-20 | 山东省环境保护科学研究所 | Composite inorganic adsorbents and preparation method thereof |
| JP2007021318A (en) * | 2005-07-14 | 2007-02-01 | Japan Pionics Co Ltd | Treatment method and apparatus of exhaust gas |
| US20110185899A1 (en) * | 2010-02-02 | 2011-08-04 | Battelle Memorial Institute | Methods for Abatement of Arsenic and Phosphorous Contaminants From Fuel Gases Prior to Gasification |
| CN103182316A (en) * | 2011-12-30 | 2013-07-03 | 北京北大先锋科技有限公司 | Catalyst for dephosphorizing yellow phosphorus tail gas and preparation method thereof |
| CN102775018A (en) * | 2012-07-25 | 2012-11-14 | 华南理工大学 | Phosphorus removing and coupling process of sewage sludge treatment |
| CN104069734A (en) * | 2013-03-26 | 2014-10-01 | 北京北大先锋科技有限公司 | Dephosphorization catalytic reaction process and catalyst for yellow phosphorus tail gas |
| CN103316624A (en) * | 2013-06-08 | 2013-09-25 | 华烁科技股份有限公司 | Dephosphorization agent and preparation method thereof |
| CN104338432A (en) * | 2013-07-30 | 2015-02-11 | 湖南华望熏蒸消毒有限公司 | Phosphine gas treatment agent and preparation method thereof |
| CN104098094A (en) * | 2014-07-26 | 2014-10-15 | 淮北市森化碳吸附剂有限责任公司 | Active carbon for adsorbing phosphine and preparation method of active carbon |
| CN104492375A (en) * | 2014-12-15 | 2015-04-08 | 西南化工研究设计院有限公司 | Adsorbent for recovering CO from industrial exhaust gas as well as preparation method and application of adsorbent |
| CN209076673U (en) * | 2018-09-13 | 2019-07-09 | 河南环宇石化装备科技股份有限公司 | A kind of yellow phosphoric tail gas adsorbent preparation facilities |
| CN108993400A (en) * | 2018-09-14 | 2018-12-14 | 河南环宇石化装备科技股份有限公司 | A kind of preparation method of the high-efficiency adsorbent of separation of nitrogen-methane |
| CN109603741A (en) * | 2019-01-16 | 2019-04-12 | 武汉禾谷环保有限公司 | A kind of Dephosphorising agent and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| TANYOL M ET AL.: "removal of phosphate from aqueous solutions by chemical and thermal modified bentonite clay", 《WATER AIR AND SOIL POLLUTION》 * |
| 蒋明等: "改性活性炭净化PH3实验研究", 《环境科学与技术》 * |
| 韩长日等: "《电子与信息化学品制造技术》", 31 October 2001 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114471743A (en) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | Advanced oxidation catalyst containing ferric phosphate and preparation method thereof |
| CN114471634A (en) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | Catalytic material for catalytic oxidation and preparation method and application thereof |
| CN114471634B (en) * | 2020-10-27 | 2023-10-10 | 中国石油化工股份有限公司 | Catalytic material for catalytic oxidation and preparation method and application thereof |
| CN114471743B (en) * | 2020-10-27 | 2024-01-09 | 中国石油化工股份有限公司 | Advanced oxidation catalyst containing ferric phosphate and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102049257B (en) | Catalyst for simultaneously reducing SO2 and NO with CO as well as preparation and application of catalyst | |
| CN101653690B (en) | Sulfur and mercury removing agent | |
| CN102357364A (en) | Preparation of activated carbon-based catalyst used for selective reduction desulphurization of flue gas | |
| CN105289476A (en) | Metal-modified 13X molecular sieve desulphurization adsorbent and its preparation method and use | |
| CN112708477A (en) | Method for increasing combustion heat value of blast furnace gas and simultaneously removing organic sulfur and inorganic sulfur | |
| CN102500362A (en) | Catalyst for removing H2S from gas by catalytic oxidation, preparation method and application | |
| CN110813232A (en) | Sulfur-resistant adsorbent for purifying yellow phosphorus tail gas and preparation method thereof | |
| CN101804289A (en) | Preparation of flue gas desulfurizer and use and regeneration method thereof | |
| CN1175920C (en) | Catalytic yellow phosphorus tail gas oxidizing and purifying method in fixed bed | |
| CN101091869A (en) | Method for cleansing exhaust gas of sulfureted hydrogen in low concentration | |
| CN104888692A (en) | Method for preparing adsorbent capable of simultaneously removing hydrogen sulfide, hydrogen phosphide and arsenic hydride | |
| CN101544914A (en) | Method and device for thermally desulfurizing by synthesis gas dry method and reclaiming sulfur | |
| CN104667861A (en) | Desulfurization adsorption agent used for gasoline and gasoline desulfurization method | |
| CN114835142A (en) | Method for recovering carbon dioxide from industrial kiln tail gas and producing lithium carbonate | |
| CN109550521B (en) | Catalyst for treating waste amine liquid, preparation method and application thereof | |
| CN112086298B (en) | Modified activated carbon/ferroferric oxide composite material and preparation method and application thereof | |
| CN101318124A (en) | Method for preparing molecular sieve adsorption agent for low-concentration hydrogen phosphide purification | |
| CN105080487B (en) | Load active carbon desulfurization adsorbent of phthalocyanine cobalt sulfonate and copper and preparation method thereof | |
| CN101402020B (en) | Method for purifying arsenic hydride gas in industrial waste gas | |
| CN1308985A (en) | Process for using iron-series metal oxide as desulfurizing agent | |
| CN1237472A (en) | Method for recovering sulfur dioxide from gas and its equipment | |
| CN101564684A (en) | Method for preparing transitional metal ion Co modified adsorbent for purifying low-concentration phosphine | |
| WO2013134910A1 (en) | Process for purifying tail gas from ore-smelting electrical furnace by catalytic oxidization | |
| CN101590354B (en) | Dephosphorization agent for removing PH3 in yellow phosphorus tail gas, preparation method and application thereof | |
| CN104069734B (en) | A kind of dephosphorization catalytic reaction technique of yellow phosphoric tail gas and catalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200221 |
|
| RJ01 | Rejection of invention patent application after publication |