CN113797889A - Acetylene sludge molecular sieve composite adsorbent for purifying hydrogen cyanide and preparation method thereof - Google Patents
Acetylene sludge molecular sieve composite adsorbent for purifying hydrogen cyanide and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a carbide slag molecular sieve composite adsorbent for purifying hydrogen cyanide and a preparation method thereof, belonging to the technical field of adsorbents. According to the invention, a NaY molecular sieve is used as a carrier, and carbide slag is used as an active component; through high-temperature activation modification, the purification capacity of the composite adsorbent to HCN can be improved, the activity of the composite adsorbent is increased, and the adsorption effect is more stable. In an HCN adsorption activity test, the purification efficiency of the composite adsorbent provided by the invention can be maintained at more than 90% within 360 min. The carbide slag is solid waste with large stockpiling amount in China, and is used as an active component of an adsorbent to purify hydrogen cyanide in waste gas, so that the resource utilization of the carbide slag is solved, and a new method is provided for purifying the hydrogen cyanide.
Description
Technical Field
The invention belongs to the technical field of adsorbents, and particularly relates to a carbide slag molecular sieve composite adsorbent for purifying hydrogen cyanide and a preparation method thereof.
Background
Hydrogen Cyanide (HCN) is a highly toxic, corrosive, flammable and volatile compound, one of the cyanides, and is considered to be a primary intermediate precursor of nitrogen oxides in the conversion of nitrogen in coal. The sources of HCN are mainly: calcium carbide furnace tail gas, coal cracking and coal industry, automobile tail gas, yellow phosphorus tail gas, a nitrogen removal process of hydrocarbon selective catalytic reduction nitrogen oxide, manufacturing of polyacrylonitrile-based carbon fiber, combustion of nitrogen-containing substances, biomass fuel and the like. On the one hand, HCN can directly permeate into the human body through respiratory organs and skin and then react with intracellular components to cause asphyxia and hypoxia. Low concentrations of HCN can lead to symptoms such as nausea, vomiting, dyspnea, etc., while high concentrations of HCN can lead to acute toxicity and even death. On the other hand, HCN causes pollution to the ecological environment. With the increasing demand for health and environment, HCN purification is important.
The existing methods for purifying HCN mainly comprise absorption, combustion, adsorption, catalytic hydrolysis, catalytic oxidation and the like. The absorption method is to introduce waste gas containing HCN into alkali liquor to ionize to generate CN-, and then to carry out secondary treatment to recover cyanide. The combustion method is that HCN is combusted at high temperature to generate gases such as CO2, N2 and H2O, and the method has high energy consumption and cost. The catalytic hydrolysis is that HCN and H2O are subjected to hydrolysis reaction under the catalytic condition to generate gases such as NH3 and CO. The catalytic oxidation is that HCN is subjected to oxidation reaction on the surface of a catalyst under the aerobic condition to generate N2 or NOx. The catalytic hydrolysis/oxidation hydrolysis method has the characteristics of high efficiency, low energy consumption, less side reaction and the like, but has more strict requirements on the reaction and is not mature enough in application.
The adsorption method is to adsorb and fix HCN by an adsorbent to eliminate the HCN, mainly comprises physical adsorption and chemical adsorption, and has the advantages of simple operation, low required cost and energy consumption, easily obtained materials and the like. The traditional adsorption method adopts a single material to prepare the adsorbent, has low purification efficiency and is difficult to realize deep purification. The composite adsorbent prepared by the method has high HCN purification efficiency and long adsorption time, and can realize deep purification.
Chinese patent CN112675867A discloses a catalytic material synthesized by using cerium oxide material as carrier to load metal oxide and then using hydrothermal method and deposition precipitation method. Chinese patent CN107649176A discloses a method for preparing a catalyst by using a titanium-silicon molecular sieve TS-1 as a carrier, copper oxide or iron oxide as an active component, and yttrium oxide and magnesium oxide as auxiliaries, but the method has harsh preparation conditions, complex operation and high cost.
Disclosure of Invention
In order to effectively remove toxic and harmful gas HCN, the invention provides a carbide slag molecular sieve composite adsorbent for purifying hydrogen cyanide, wherein a carrier is as follows: the molecular sieve comprises the following active components: carbide slag. The invention effectively improves the purification capacity of the adsorbent to HCN by a high-temperature activation modification means.
In order to realize the purpose, the invention is realized by the following technical scheme:
the invention provides a carbide slag/molecular sieve composite adsorbent for purifying hydrogen cyanide, which is obtained by taking a NaY molecular sieve as a carrier and carbide slag as an active ingredient through a high-temperature activation method.
The invention also provides a preparation method of the carbide slag molecular sieve composite adsorbent for purifying hydrogen cyanide, which comprises the following steps:
(1) mashing a NaY molecular sieve, grinding to 80-120 meshes, activating at high temperature, taking out, cooling to room temperature, and storing for later use;
(2) crushing and grinding the carbide slag to 20-40 meshes, calcining at high temperature to remove impurities, taking out, cooling to room temperature, and storing for later use;
(3) adding deionized water into the carbide slag obtained in the step (2) to digest the carbide slag into lime emulsion, standing for 24 hours, and taking saturated supernatant and filtering for later use;
(4) putting the NaY molecular sieve obtained in the step (1) into the saturated supernatant obtained in the step (3) for soaking for 24 hours, then putting the saturated supernatant into a drying oven for drying for 10 hours at 100 ℃, taking the saturated supernatant out, and cooling to room temperature;
(5) and (4) sieving the sample obtained in the step (4) to 20-40 meshes, and roasting at 300-500 ℃ for 3h to obtain the carbide slag/molecular sieve composite adsorbent.
Further, in the step (1), the high-temperature activation condition is 300-500 ℃ roasting for 3 h.
Further, in the step (2), the high-temperature calcination condition is 800 ℃ for 6 h.
Further, in the step (3), the slag-water ratio is 0.15g of carbide slag: 100ml of water.
Further, in the step (4), the liquid-solid ratio is 75mL of supernatant: 3g NaY molecular sieve.
Further, in the step (5), the calcination temperature is preferably 300 ℃.
The method for removing hydrogen cyanide by using the composite adsorbent comprises the following steps: the adsorption temperature of the adsorbent for removing hydrogen cyanide is 20-50 ℃, and the space velocity is 10000-15000 h-1。
The invention has the advantages that:
1. the molecular sieve is widely applied to the fields of catalysis, adsorption separation and the like in air pollution control, and has the characteristics of complex structure, unique holes, high activity, low price and the like. The invention takes the molecular sieve as a carrier and the carbide slag as an active component, and the activity of the carbide slag is increased and the adsorption effect is more stable through high-temperature modification. The invention not only solves the problem of resource utilization of the carbide slag, but also provides a new method for purifying the hydrogen cyanide.
2. In the adsorption activity test of hydrogen cyanide, the purification efficiency of the adsorbent can be maintained at more than 90% within 360 min.
3. The preparation and purification process of the adsorbent has the advantages of simple flow, simple operation and feasible technology.
Drawings
FIG. 1 is a graph of the purification efficiency of HCN by the adsorbent prepared in example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, preferred embodiments of the present invention will be described in detail below to facilitate understanding of the skilled person.
Example 1:
(1) taking 5g of NaY molecular sieve, mashing, grinding to 80 meshes, then placing into a muffle furnace, roasting at 500 ℃ for 3h, taking out, cooling to room temperature, and storing for later use.
(2) And (3) taking 5g of carbide slag, mashing, grinding to 20-40 meshes, then placing the carbide slag into a muffle furnace for high-temperature calcination and impurity removal (calcination is carried out for 6 hours at 800 ℃), taking out the carbide slag, cooling to room temperature, and storing for later use.
(3) And (3) adding deionized water into 0.15g of the carbide slag obtained in the step (2) to digest the carbide slag into lime emulsion, wherein the slag-water ratio is 0.15g of the carbide slag: 100mL of water, standing the lime emulsion for 24h, taking saturated supernatant and filtering for later use.
(4) And (3) putting 3g of the molecular sieve obtained in the step (1) into 75mL of saturated supernatant obtained in the step (3) for soaking for 24h, then putting into a drying oven for drying at 100 ℃ for 10h, taking out, cooling to room temperature, and storing for later use.
(5) And (4) sieving the sample obtained in the step (4) to 20-40 meshes, then placing the sample into a muffle furnace to be roasted for 3 hours at the temperature of 400 ℃, taking out the sample, and cooling the sample to room temperature to obtain the carbide slag/molecular sieve composite adsorbent.
Activity test of the adsorbent: 0.4g of the composite adsorbent prepared in the example was placed in a fixed bed adsorption column for dynamic adsorption performance testing, and simulated exhaust gas was introduced, wherein the HCN concentration in the simulated exhaust gas was 260mg/m3The adsorption temperature is 20 ℃, and the space velocity is 15000h-1The outlet concentration of HCN is measured every 10min in the initial stage of the test, and every 30min in the middle and later stages of the test.
The test result shows that the purification efficiency of the composite adsorbent to HCN can be maintained to be more than 90% within 20 min.
Example 2:
(1) taking 5g of NaY molecular sieve, mashing, grinding to 100 meshes, then placing into a muffle furnace, roasting at 500 ℃ for 3h, taking out, cooling to room temperature, and storing for later use.
(2) And (3) taking 5g of carbide slag, mashing, grinding to 20-40 meshes, then placing the carbide slag into a muffle furnace for high-temperature calcination and impurity removal (calcination is carried out for 6 hours at 800 ℃), taking out the carbide slag, cooling to room temperature, and storing for later use.
(3) And (3) adding deionized water into 0.15g of the carbide slag obtained in the step (2) to digest the carbide slag into lime emulsion, wherein the slag-water ratio is 0.15g of the carbide slag: 100mL of water, standing the lime emulsion for 24h, taking saturated supernatant and filtering for later use.
(4) And (3) putting 3g of the molecular sieve obtained in the step (1) into 75mL of saturated supernatant obtained in the step (3) for soaking for 24h, then putting into a drying oven for drying at 100 ℃ for 10h, taking out, cooling to room temperature, and storing for later use.
(5) And (4) sieving the sample obtained in the step (4) to 20-40 meshes, then placing the sample into a muffle furnace to be roasted for 3 hours at 500 ℃, taking out the sample, and cooling the sample to room temperature to obtain the carbide slag/molecular sieve composite adsorbent.
Activity test of the adsorbent: 0.4g of the composite adsorbent prepared in the example was placed in a fixed bed adsorption column for dynamic adsorption performance testing, and simulated exhaust gas was introduced, wherein the HCN concentration in the simulated exhaust gas was 260mg/m3The adsorption temperature is 20 ℃, and the space velocity is 15000h-1The outlet concentration of HCN is measured every 10min in the initial stage of the test, and every 30min in the middle and later stages of the test.
The test result shows that the purification efficiency of the composite adsorbent to HCN can be maintained to be more than 90% within 200 min.
Example 3:
(1) taking 5g of NaY molecular sieve, mashing, grinding to 120 meshes, then placing into a muffle furnace, roasting at 500 ℃ for 3h, taking out, cooling to room temperature, and storing for later use.
(2) And (3) taking 5g of carbide slag, mashing, grinding to 20-40 meshes, then placing the carbide slag into a muffle furnace for high-temperature calcination and impurity removal (calcination is carried out for 6 hours at 800 ℃), taking out the carbide slag, cooling to room temperature, and storing for later use.
(3) And (3) adding deionized water into 0.15g of the carbide slag obtained in the step (2) to digest the carbide slag into lime emulsion, wherein the slag-water ratio is 0.15g of the carbide slag: 100mL of water, standing the lime emulsion for 24h, taking saturated supernatant and filtering for later use.
(4) And (3) putting 3g of the molecular sieve obtained in the step (1) into 75mL of saturated supernatant obtained in the step (3) for soaking for 24h, then putting into a drying oven for drying at 100 ℃ for 10h, taking out, cooling to room temperature, and storing for later use.
(5) And (4) sieving the sample obtained in the step (4) to 20-40 meshes, then placing the sample into a muffle furnace to be roasted for 3 hours at the temperature of 600 ℃, taking out the sample, and cooling the sample to room temperature to obtain the carbide slag/molecular sieve composite adsorbent.
Activity test of the adsorbent: 0.4g of the composite adsorbent prepared in the example was placed in a fixed bed adsorption column for dynamic adsorption performance testing, and simulated exhaust gas was introduced, wherein the HCN concentration in the simulated exhaust gas was 260mg/m3The adsorption temperature is 20 ℃, and the space velocity is 15000h-1The outlet concentration of HCN is measured every 10min in the initial stage of the test, and every 30min in the middle and later stages of the test.
The test result shows that the purification efficiency of the composite adsorbent to HCN can be maintained to be more than 90% within 50 min.
Example 4:
(1) taking 5g of NaY molecular sieve, mashing, grinding to 120 meshes, then placing into a muffle furnace, roasting at 500 ℃ for 3h, taking out, cooling to room temperature, and storing for later use.
(2) And (3) taking 5g of carbide slag, mashing, grinding to 20-40 meshes, then placing the carbide slag into a muffle furnace for high-temperature calcination and impurity removal (calcination is carried out for 6 hours at 800 ℃), taking out the carbide slag, cooling to room temperature, and storing for later use.
(3) And (3) adding deionized water into 0.15g of the carbide slag obtained in the step (2) to digest the carbide slag into lime emulsion, wherein the slag-water ratio is 0.15g of the carbide slag: 100mL of water, standing the lime emulsion for 24h, taking saturated supernatant and filtering for later use.
(4) And (3) putting 3g of the molecular sieve obtained in the step (1) into 75mL of saturated supernatant obtained in the step (3) for soaking for 24h, then putting into a drying oven for drying at 100 ℃ for 10h, taking out, cooling to room temperature, and storing for later use.
(5) And (4) sieving the sample obtained in the step (4) to 20-40 meshes, then placing the sample into a muffle furnace to be roasted for 3 hours at 700 ℃, taking out the sample, and cooling the sample to room temperature to obtain the carbide slag/molecular sieve composite adsorbent.
Activity test of the adsorbent: 0.4g of the composite adsorbent prepared in the example was placed in a fixed bed adsorption column for dynamic adsorption performance testing, and simulated exhaust gas was introduced, wherein the HCN concentration in the simulated exhaust gas was 260mg/m3The adsorption temperature is 20 ℃, and the space velocity is 15000h-1The outlet concentration of HCN is measured every 10min in the initial stage of the test, and every 30min in the middle and later stages of the test.
The test result shows that the purification efficiency of the composite adsorbent to HCN can be maintained to be more than 90% within 110 min.
Example 5:
(1) taking 5g of NaY molecular sieve, mashing, grinding to 100 meshes, then placing into a muffle furnace, roasting at 500 ℃ for 3h, taking out, cooling to room temperature, and storing for later use.
(2) And (3) taking 5g of carbide slag, mashing, grinding to 20-40 meshes, then placing the carbide slag into a muffle furnace for high-temperature calcination and impurity removal (calcination is carried out for 6 hours at 800 ℃), taking out the carbide slag, cooling to room temperature, and storing for later use.
(3) And (3) adding deionized water into 0.1g of the carbide slag obtained in the step (2) to digest the carbide slag into lime emulsion, wherein the proportion of slag to water is 0.1g of the carbide slag to 100mL of water, standing the lime emulsion for 24 hours, taking saturated supernatant and filtering the saturated supernatant for later use.
(4) And (3) putting 3g of the molecular sieve obtained in the step (1) into 75mL of saturated supernatant obtained in the step (3) for soaking for 24h, then putting into a drying oven for drying at 100 ℃ for 10h, taking out, cooling to room temperature, and storing for later use.
(5) And (4) sieving the sample obtained in the step (4) to 20-40 meshes, then placing the sample into a muffle furnace to be roasted for 3 hours at 500 ℃, taking out the sample, and cooling the sample to room temperature to obtain the carbide slag/molecular sieve composite adsorbent.
Activity test of the adsorbent: the 0.4g of the composite adsorbent prepared in the example is put into a fixed bed adsorption column for dynamic adsorption performance test, simulated waste gas is introduced, the HCN concentration in the simulated waste gas is 260mg/m3, the adsorption temperature is 20 ℃, and the space velocity is 15000h-1At the beginning of the test, every 1And (3) measuring the outlet concentration of HCN once in 0min, and measuring the outlet concentration of HCN once every 30min in the middle and later periods of the test.
The test result shows that the purification efficiency of the composite adsorbent to HCN can be maintained to be more than 90% within 170 min.
Example 6:
(1) taking 5g of NaY molecular sieve, mashing, grinding to 100 meshes, then placing into a muffle furnace, roasting at 500 ℃ for 3h, taking out, cooling to room temperature, and storing for later use.
(2) And (3) taking 5g of carbide slag, mashing, grinding to 20-40 meshes, then placing the carbide slag into a muffle furnace for high-temperature calcination and impurity removal (calcination is carried out for 6 hours at 800 ℃), taking out the carbide slag, cooling to room temperature, and storing for later use.
(3) And (3) adding deionized water into 0.05g of the carbide slag obtained in the step (2) to digest the carbide slag into lime emulsion, wherein the proportion of slag to water is 0.05g of the carbide slag to 100mL of water, standing the lime emulsion for 24 hours, taking saturated supernatant and filtering the saturated supernatant for later use.
(4) And (3) putting 3g of the molecular sieve obtained in the step (1) into 75mL of saturated supernatant obtained in the step (3) for soaking for 24h, then putting into a drying oven for drying at 100 ℃ for 10h, taking out, cooling to room temperature, and storing for later use.
(5) And (4) sieving the sample obtained in the step (4) to 20-40 meshes, then placing the sample into a muffle furnace to be roasted for 3 hours at 500 ℃, taking out the sample, and cooling the sample to room temperature to obtain the carbide slag/molecular sieve composite adsorbent.
Activity test of the adsorbent: the 0.4g of the composite adsorbent prepared in the example is put into a fixed bed adsorption column for dynamic adsorption performance test, simulated waste gas is introduced, the HCN concentration in the simulated waste gas is 260mg/m3, the adsorption temperature is 20 ℃, and the space velocity is 15000h-1The outlet concentration of HCN is measured every 10min in the initial stage of the test, and every 30min in the middle and later stages of the test.
The test result shows that the purification efficiency of the composite adsorbent to HCN can be maintained to be more than 90% within 130 min.
Example 7:
(1) mashing 5g NaY molecular sieve, grinding to 100 mesh, and storing for use.
(2) 5g of carbide slag is smashed and ground to 20-40 meshes, and is stored for later use.
(3) 0.15g of the carbide slag obtained in the step (2) is added with deionized water and digested into lime emulsion, and the slag-water ratio is 0.15g of the carbide slag: 100mL of water, standing the lime emulsion for 24h, taking saturated supernatant and filtering for later use.
(4) And (3) putting 3g of the molecular sieve obtained in the step (1) into 75mL of saturated supernatant obtained in the step (3) for soaking for 24h, then putting into a drying oven for drying at 100 ℃ for 10h, taking out, cooling to room temperature, and storing for later use.
(5) And (4) sieving the sample obtained in the step (4) to 20-40 meshes to obtain the unmodified carbide slag/molecular sieve composite adsorbent.
Activity test of the adsorbent: 0.4g of the composite adsorbent prepared in the example was placed in a fixed bed adsorption column for dynamic adsorption performance testing, and simulated exhaust gas was introduced, wherein the HCN concentration in the simulated exhaust gas was 260mg/m3The adsorption temperature is 20-50 ℃, and the airspeed is 10000-15000 h-1The outlet concentration of HCN is measured every 10min in the initial stage of the test, and every 30min in the middle and later stages of the test.
The test result shows that the purification efficiency of the composite adsorbent to HCN is maintained to be more than 90% within 10 min.
Example 8:
taking 5g of NaY molecular sieve, mashing, grinding to 100 meshes, then placing into a muffle furnace, roasting at 500 ℃ for 3h, taking out, cooling to room temperature, and obtaining a blank molecular sieve adsorbent.
Activity test of the adsorbent: 0.4g of the adsorbent prepared in the example was placed in a fixed bed adsorption column for dynamic adsorption performance testing, and simulated exhaust gas was introduced, in which the HCN concentration was 260mg/m3The adsorption temperature is 20-50 ℃, and the airspeed is 10000-15000 h-1The outlet concentration of HCN is measured every 10min in the initial stage of the test, and every 30min in the middle and later stages of the test.
The test result shows that the purification efficiency of the adsorbent to HCN is maintained to be more than 90% within 30 min.
By comparing 8 examples, the modified carbide slag/molecular sieve composite adsorbent has better effect of removing carbonyl sulfide than unmodified carbide slag/molecular sieve composite adsorbent and single molecular sieve adsorbent; the preparation conditions of the adsorbent with the best removal effect are as follows: the roasting temperature is 500 ℃, and the slag-water ratio is 0.15g of carbide slag: 100mL of deionized water.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (8)
1. The carbide slag/molecular sieve composite adsorbent for purifying hydrogen cyanide is characterized in that: the acetylene sludge molecular sieve composite adsorbent for purifying hydrogen cyanide is obtained by using a NaY molecular sieve as a carrier and acetylene sludge as an active ingredient through a high-temperature activation method.
2. The method for preparing the carbide slag molecular sieve composite adsorbent for purifying hydrogen cyanide according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
(1) mashing a NaY molecular sieve, grinding to 80-120 meshes, activating at high temperature, taking out, cooling to room temperature, and storing for later use;
(2) crushing and grinding the carbide slag to 20-40 meshes, calcining at high temperature to remove impurities, taking out, cooling to room temperature, and storing for later use;
(3) adding deionized water into the carbide slag obtained in the step (2) to digest the carbide slag into lime emulsion, standing for 24 hours, and taking saturated supernatant and filtering for later use;
(4) putting the NaY molecular sieve obtained in the step (1) into the saturated supernatant obtained in the step (3) for soaking for 24 hours, then putting the saturated supernatant into a drying oven for drying for 10 hours at 100 ℃, taking the saturated supernatant out, and cooling to room temperature;
(5) and (4) sieving the sample obtained in the step (4) to 20-40 meshes, and roasting at 300-500 ℃ for 3h to obtain the carbide slag/molecular sieve composite adsorbent.
3. The method for preparing the carbide slag molecular sieve composite adsorbent for purifying hydrogen cyanide according to claim 1, wherein the method comprises the following steps: in the step (1), the high-temperature activation condition is 300-500 ℃ roasting for 3 h.
4. The carbide slag molecular sieve composite adsorbent for purifying hydrogen cyanide and the preparation method thereof according to claim 1, wherein the composite adsorbent comprises: in the step (2), the high-temperature calcination condition is 800 ℃ for 6 h.
5. The method for preparing the carbide slag molecular sieve composite adsorbent for purifying hydrogen cyanide according to claim 1, wherein the method comprises the following steps: in the step (3), the slag-water ratio is 0.15g of carbide slag: 100ml of water.
6. The carbide slag molecular sieve composite adsorbent for purifying hydrogen cyanide and the preparation method thereof according to claim 1, wherein the composite adsorbent comprises: in the step (4), the liquid-solid ratio is 75mL of supernatant: 3g NaY molecular sieve.
7. The carbide slag molecular sieve composite adsorbent for purifying hydrogen cyanide and the preparation method thereof according to claim 1 or 5, wherein the composite adsorbent comprises: in the step (5), the calcination temperature is 300 ℃.
8. The method for removing hydrogen cyanide by using composite adsorbent according to any one of claims 1-7, characterized in that: the adsorption temperature of the adsorbent for removing hydrogen cyanide is 20-50 ℃, and the space velocity is 10000-15000 h-1。
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101982221A (en) * | 2010-10-27 | 2011-03-02 | 西安交通大学 | Method for desorbing hydrogen cyanide in gaseous phase products obtained by performing chemical machining on coals |
US20140241969A1 (en) * | 2013-02-22 | 2014-08-28 | Intercat, Inc. | Process of removing hcn from flue gas |
CN107626309A (en) * | 2017-09-04 | 2018-01-26 | 昆明理工大学 | A kind of method that hydrogen cyanide hydrolyst is prepared using sepiolite as carrier |
CN107649176A (en) * | 2017-09-22 | 2018-02-02 | 昆明理工大学 | A kind of catalyst and preparation method for hydrogen cyanide catalyzing hydrolysis |
CN108499515A (en) * | 2018-03-05 | 2018-09-07 | 昆明理工大学 | A kind of doping type CO2The preparation method of Ca-base adsorbent |
CN109135866A (en) * | 2018-08-29 | 2019-01-04 | 佛山市禅城区诺高环保科技有限公司 | A kind of highly effective fuel desulfurizing agent and preparation method thereof |
-
2021
- 2021-10-13 CN CN202111189574.4A patent/CN113797889B/en active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101982221A (en) * | 2010-10-27 | 2011-03-02 | 西安交通大学 | Method for desorbing hydrogen cyanide in gaseous phase products obtained by performing chemical machining on coals |
US20140241969A1 (en) * | 2013-02-22 | 2014-08-28 | Intercat, Inc. | Process of removing hcn from flue gas |
CN107626309A (en) * | 2017-09-04 | 2018-01-26 | 昆明理工大学 | A kind of method that hydrogen cyanide hydrolyst is prepared using sepiolite as carrier |
CN107649176A (en) * | 2017-09-22 | 2018-02-02 | 昆明理工大学 | A kind of catalyst and preparation method for hydrogen cyanide catalyzing hydrolysis |
CN108499515A (en) * | 2018-03-05 | 2018-09-07 | 昆明理工大学 | A kind of doping type CO2The preparation method of Ca-base adsorbent |
CN109135866A (en) * | 2018-08-29 | 2019-01-04 | 佛山市禅城区诺高环保科技有限公司 | A kind of highly effective fuel desulfurizing agent and preparation method thereof |
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