CN116459787A - Composite filtering agent for resisting siloxane and hydrogen sulfide poisoning and preparation method thereof - Google Patents
Composite filtering agent for resisting siloxane and hydrogen sulfide poisoning and preparation method thereof Download PDFInfo
- Publication number
- CN116459787A CN116459787A CN202310598721.6A CN202310598721A CN116459787A CN 116459787 A CN116459787 A CN 116459787A CN 202310598721 A CN202310598721 A CN 202310598721A CN 116459787 A CN116459787 A CN 116459787A
- Authority
- CN
- China
- Prior art keywords
- parts
- copper sulfate
- hydrogen sulfide
- siloxane
- sulfate solution
- 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
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 238000001914 filtration Methods 0.000 title claims abstract description 45
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 41
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 36
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 231100000572 poisoning Toxicity 0.000 title claims abstract description 31
- 230000000607 poisoning effect Effects 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical class [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 51
- 239000002808 molecular sieve Substances 0.000 claims abstract description 34
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 34
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000000839 emulsion Substances 0.000 claims description 11
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical group CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 5
- 229920001296 polysiloxane Polymers 0.000 claims 1
- 239000007789 gas Substances 0.000 abstract description 26
- 230000035945 sensitivity Effects 0.000 abstract description 10
- 238000001179 sorption measurement Methods 0.000 abstract description 8
- 238000007084 catalytic combustion reaction Methods 0.000 abstract description 5
- 230000002427 irreversible effect Effects 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 19
- 239000003463 adsorbent Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- 230000029087 digestion Effects 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- -1 Siloxanes Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 125000001183 hydrocarbyl group Chemical group 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000002238 attenuated effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 2
- 239000000413 hydrolysate Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 239000002594 sorbent Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002619 bicyclic group Chemical group 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 235000013980 iron oxide Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 125000002950 monocyclic group Chemical group 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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
- B01J20/10—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
- 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
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/116—Molecular sieves other than zeolites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/25—Coated, impregnated or composite adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/30—Sulfur compounds
- B01D2257/304—Hydrogen sulfide
-
- 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
- B01D2257/556—Organic compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention discloses a composite filtering agent for resisting siloxane and hydrogen sulfide poisoning and a preparation method thereof, which relate to the technical field of material compounding and comprise the following components in parts by weight: 5-100 parts of organic titanate, 5-100 parts of saturated copper sulfate solution and 10-20 parts of molecular sieve; the composite filtering agent prepared by the invention has the characteristics of high specific surface area of the existing physical adsorption type filtering agent and selective filtering of chemical reagents, can effectively remove siloxane and hydrogen sulfide contained in gas to be detected, and avoids the phenomenon of irreversible attenuation (i.e. poisoning) of sensitivity of a catalytic combustion type gas sensor.
Description
Technical Field
The invention relates to the technical field of material compounding, in particular to a composite filtering agent for resisting siloxane and hydrogen sulfide poisoning and a preparation method thereof.
Background
Siloxanes are a common organosilicon compound, and a typical representation of such siloxanes is Hexamethyldisiloxane (HMDS). Hydrogen sulfide is an inorganic compound with the chemical formula of H2S. These two substances are widely used in chemical production processes due to their variety of applications. However, for gas sensors, particularly catalytic combustion type gas sensors, if the two substances participate in the combustion process in the gas sensor, they are converted into solid substances which are difficult to decompose and deposited, and cause irreversible serious damage to the gas sensor, i.e. sensor poisoning phenomenon occurs. In the case of a detection gas containing siloxane or hydrogen sulfide, the sensitivity of the catalytic combustion gas sensor may drop to half or less within several hours. At this point the sensor no longer has the ability to monitor toxic and harmful gases and alarm. The prior patent discloses the following technology:
the patent publication KR100804241B1 entitled "method for removing Hydrogen sulfide and volatile siloxanes from a digestion gas" discloses the following: a method for removing hydrogen sulfide and volatile siloxanes from a digestion gas is provided using a refined digestion gas containing methane as a heat source for a power plant to prevent the discharge of air-shift limiting materials. The adsorption solution is prepared by mixing iron oxide into water. The hydrogen sulfide contained in the digestion gas is contacted with the adsorption solution at a gas-liquid contact ratio of 3 to 4, and is removed from the digestion gas. The digested gas from which hydrogen sulfide has been removed is dehumidified to a relative humidity of 30% by volume or less. The dehumidified digestion gas is moved to an activated carbon adsorption column to remove volatile siloxanes from the digestion gas.
The patent with publication number KR1020170075262A, entitled "adsorbent for efficiently removing hydrogen sulfide and siloxane from ammonia water and ferric polysulfate" discloses the following: an adsorbent for removing hydrogen sulfide and siloxane with high efficiency by ammonia water and ferric polysulfate and a preparation method thereof. The production method of the adsorbent for removing hydrogen sulfide and siloxane according to the present invention comprises: water glass, ammonia water and iron oxide at a pH of 6 to 9 and water glass with ammonia at a pH of 1:2 to 1:6 weight ratio. Separating solid phase precipitate and liquid contained in the mixture; washing the precipitate with distilled water; and drying the precipitate.
Currently, in order to remove these substances harmful to the gas sensor, adsorption based on silica gel, alumina, zeolite or activated carbon as an adsorbent or the adsorbents disclosed in the above patents is used. However, using these materials is based on physical processes, the filtration effect is lost after adsorption-desorption reaches equilibrium, and the non-selective adsorption effect can affect accurate measurement of the target detection gas.
Disclosure of Invention
The invention aims at: the invention provides a composite filtering agent for resisting siloxane and hydrogen sulfide poisoning and a preparation method thereof, and aims to solve the technical problem that the existing absorbing effect of an absorbing agent for absorbing siloxane and hydrogen sulfide is poor.
The invention adopts the following technical scheme for realizing the purposes:
the invention provides a composite filtering agent for resisting siloxane and hydrogen sulfide poisoning, which comprises the following components in parts by weight: 5-100 parts of organic titanate, 5-100 parts of saturated copper sulfate solution and 10-20 parts of molecular sieve.
The composite filter agent has the characteristics of high specific surface area of the existing physical adsorption type filter agent and the selective filtering characteristic of chemical reagents, can effectively remove siloxane and hydrogen sulfide contained in gas to be detected, and avoids the phenomenon of irreversible attenuation (i.e. poisoning) of sensitivity of the catalytic combustion type gas sensor.
The composite filtering agent has the selective filtering performance on siloxane and hydrogen sulfide, and can remove the siloxane and the hydrogen sulfide without influencing the concentration of the gas to be detected. Has the advantage of strong pertinence.
In one embodiment, the composition comprises the following components in parts by weight: 100 parts of organic titanate, 100 parts of saturated copper sulfate solution and 20 parts of molecular sieve.
In one embodiment, the composition comprises the following components in parts by weight: 45 parts of organic titanate, 45 parts of saturated copper sulfate solution and 15 parts of molecular sieve.
In one embodiment, the composition comprises the following components in parts by weight: 5 parts of organic titanate, 5 parts of saturated copper sulfate solution and 10 parts of molecular sieve.
In one placeIn one embodiment, the organic titanate is Ti (OR) 4 。
In particular, the organotitanates have the formula Ti (OR) 4 Wherein each R independently represents hydrogen or a hydrocarbyl group having 1 to 10 carbon atoms, wherein each of these hydrocarbyl groups is optionally interrupted by one or more-O-, -NH-, -n=and/or-C (O) -and/or by one or more-OH and/or NH 2 Substituted and wherein optionally two or three of these hydrocarbyl groups are bonded to each other and form a mono-or bicyclic ring.
In one embodiment, the organic titanate is isopropyl titanate.
In particular, isopropyl titanate is the preferred material for the organic titanate.
The invention also provides a preparation method of the composite filtering agent for resisting siloxane and hydrogen sulfide poisoning, which comprises the following steps:
step S01, preparing materials, namely preparing 0-100 parts of organic titanate, 0-100 parts of saturated copper sulfate solution and 10-20 parts of molecular sieve;
step S02, placing the saturated copper sulfate solution prepared in the step S01 into a reaction container for standby;
step S03, dropwise adding the organic titanate prepared in the step S01 into the saturated copper sulfate solution in the step S02, and then uniformly stirring, wherein the organic titanate is hydrolyzed in the saturated copper sulfate solution to obtain a composite material emulsion;
step S04, adding the composite emulsion obtained in the step S03 into the molecular sieve in the step S01;
and S05, drying the molecular sieve treated in the step S04 to obtain the composite filtering agent.
Specifically, 5-100 parts of organic titanate, 5-100 parts of saturated copper sulfate solution, 10-20 parts of molecular sieve and the content of components is a key point;
during preparation, saturated copper sulfate solution is prepared, and organic titanate is added dropwise, wherein the key of the reaction is that the organic titanate is hydrolyzed in the saturated copper sulfate solution to obtain a hydrolysate. In the scheme, the molecular sieve is used as a base material, so that a hydrolysate is formed on the surface of the molecular sieve by the saturated copper sulfate solution and the organic titanate. The siloxane and hydrogen sulfide in the gas are removed by using the water-soluble organic solvent as a filtering agent.
In one embodiment, in step S01, the method for preparing the saturated copper sulfate solution is as follows: adding excessive copper sulfate pentahydrate into distilled water, stirring for 30-45 min, and filtering to obtain saturated copper sulfate solution.
In one embodiment, in step S02, the reaction vessel is one of a beaker, flask, or erlenmeyer flask.
In one embodiment, in step S05, the molecular sieve is dried at 60-70 ℃ for 24-30 hours to obtain the composite filter.
In particular, this protocol discloses a subsequent drying treatment of the molecular sieve after addition of the composite emulsion, preferably divided into 60 ℃, preferably for 24 hours.
The beneficial effects of the invention are as follows:
1. the composite filtering agent has the characteristics of high specific surface area of the existing physical adsorption type filtering agent and the selective filtering characteristic of chemical agents, can effectively remove siloxane and hydrogen sulfide contained in gas to be detected, and avoids the phenomenon of irreversible attenuation (i.e. poisoning) of sensitivity of a catalytic combustion type gas sensor.
2. The filtering agent has the selective filtering performance on siloxane and hydrogen sulfide, and can remove the two gases without influencing the concentration of the gas to be detected.
Drawings
Fig. 1 is a graph comparing experimental results of hydrogen sulfide poisoning experiments of the sensors of example 1, example 2, example 3 and comparative example 1.
Fig. 2 is a graph comparing experimental results of the sensor siloxane poisoning experiments of example 1, example 2, example 3 and comparative example 2.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures. Furthermore, the terms "first," "second," and the like, are used merely to distinguish between descriptions and should not be construed as indicating or implying relative importance.
In describing embodiments of the present invention, it should be noted that the directions or positional relationships indicated by the terms "inner", "outer", "upper", etc. are directions or positional relationships based on those shown in the drawings, or those that are conventionally put in place when the inventive product is used, are merely for convenience of description and simplification of description, and are not indicative or implying that the apparatus or element in question must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
Example 1
The invention provides a composite filtering agent for resisting siloxane and hydrogen sulfide poisoning, which comprises the following components in parts by weight: 45 parts of isopropyl titanate, 45 parts of saturated copper sulfate solution and 15 parts of molecular sieve.
The preparation method of the composite filtering agent comprises the following steps:
step S01, preparing materials, namely 45 parts of isopropyl titanate, 45 parts of saturated copper sulfate solution and 15 parts of molecular sieve;
firstly, preparing a saturated copper sulfate solution, wherein the preparation method of the saturated copper sulfate solution comprises the following steps: adding excessive copper sulfate pentahydrate into distilled water, stirring for 30min, and filtering to obtain saturated copper sulfate solution.
Step S02, placing the saturated copper sulfate solution prepared in the step S01 into a reaction container for standby, wherein the reaction container is a beaker;
step S03, dropwise adding the organic titanate prepared in the step S01 into the saturated copper sulfate solution in the step S02, and then uniformly stirring, wherein the organic titanate is hydrolyzed in the saturated copper sulfate solution to obtain a composite material emulsion;
step S04, adding the composite emulsion obtained in the step S03 into the molecular sieve in the step S01;
and S05, drying the molecular sieve treated in the step S04 at 60 ℃ for 24 hours to obtain the composite filtering agent.
Example 2
The invention provides a composite filtering agent for resisting siloxane and hydrogen sulfide poisoning, which comprises the following components in parts by weight: 100 parts of isopropyl titanate, 100 parts of saturated copper sulfate solution and 20 parts of molecular sieve.
The preparation method of the composite filtering agent comprises the following steps:
step S01, preparing materials, namely 100 parts of isopropyl titanate, 100 parts of saturated copper sulfate solution and 20 parts of molecular sieve;
firstly, preparing a saturated copper sulfate solution, wherein the preparation method of the saturated copper sulfate solution comprises the following steps: adding excessive copper sulfate pentahydrate into distilled water, stirring for 30min, and filtering to obtain saturated copper sulfate solution.
Step S02, placing the saturated copper sulfate solution prepared in the step S01 into a reaction container for standby, wherein the reaction container is a beaker;
step S03, dropwise adding the organic titanate prepared in the step S01 into the saturated copper sulfate solution in the step S02, and then uniformly stirring, wherein the organic titanate is hydrolyzed in the saturated copper sulfate solution to obtain a composite material emulsion;
step S04, adding the composite emulsion obtained in the step S03 into the molecular sieve in the step S01;
and S05, drying the molecular sieve treated in the step S04 at 60 ℃ for 24 hours to obtain the composite filtering agent.
Example 3
The invention provides a composite filtering agent for resisting siloxane and hydrogen sulfide poisoning, which comprises the following components in parts by weight: 5 parts of isopropyl titanate, 5 parts of saturated copper sulfate solution and 10 parts of molecular sieve.
The preparation method of the composite filtering agent comprises the following steps:
step S01, preparing materials, namely 50 parts of isopropyl titanate, 50 parts of saturated copper sulfate solution and 15 parts of molecular sieve;
firstly, preparing a saturated copper sulfate solution, wherein the preparation method of the saturated copper sulfate solution comprises the following steps: adding excessive copper sulfate pentahydrate into distilled water, stirring for 30min, and filtering to obtain saturated copper sulfate solution.
Step S02, placing the saturated copper sulfate solution prepared in the step S01 into a reaction container for standby, wherein the reaction container is a beaker;
step S03, dropwise adding the organic titanate prepared in the step S01 into the saturated copper sulfate solution in the step S02, and then uniformly stirring, wherein the organic titanate is hydrolyzed in the saturated copper sulfate solution to obtain a composite material emulsion;
step S04, adding the composite emulsion obtained in the step S03 into the molecular sieve in the step S01;
and S05, drying the molecular sieve treated in the step S04 at 60 ℃ for 24 hours to obtain the composite filtering agent.
Comparative example 1
In this comparative example, the saturated copper sulfate solution was changed to distilled water as compared with example 1. Otherwise, the same as in example 1 was used.
Comparative example 2
In contrast to example 1, isopropyl titanate was not added. Otherwise, the same as in example 1 was used.
Table 1 shows the formulations of the filters of examples 1 to 3 and comparative examples 1 to 2, wherein the formulations of examples 1 to 3 are the first, last and middle three sets of data for the formulation range of the invention.
Table 1 formulation tables of examples 1 to 3 and comparative examples 1 to 2
| Group of | Isopropyl titanate | Saturated copper sulfate solution | Molecular sieve | Water and its preparation method |
| Example 1 | 45 | 45 | 15 | / |
| Example 2 | 100 | 100 | 20 | / |
| Example 3 | 5 | 5 | 10 | / |
| Comparative example 1 | 45 | / | 15 | 45 |
| Comparative example 2 | / | 45 | 15 | / |
Table 2 shows experimental data of hydrogen sulfide poisoning of the sensor after the sorbents of examples 1 to 3 and comparative example 1 absorbed, and it can be seen that the sorbents prepared by the invention have better absorption effect. Specifically, the prepared adsorbent still keeps the sensor sensitivity above 90% after 8 hours and 16 hours of experiment, while the sensor sensitivity of comparative example 1 is fast attenuated, the sensor sensitivity of comparative example 1 is attenuated to 65.7% after 16 hours, and the sensor is in a semi-failure state.
Table 2 table of hydrogen sulfide poisoning test data of examples 1 to 3 and comparative example 1
Table 3 shows the experimental data of the siloxane poisoning of the sensor after the adsorbents of examples 1 to 3 and comparative example 2 were absorbed, respectively, and it can be seen that the adsorbents prepared by the present invention have better absorption effect. Specifically, the adsorbents prepared by the invention still maintain the sensor sensitivity above 90% after 8 hours and 16 hours of experiment, while the sensor sensitivity of comparative example 2 decays rapidly, especially the sensor sensitivity of comparative example 2 decays to 2% after 8 hours, at which time the sensor is hardly operational.
Table 3 table of the siloxane poisoning test data of examples 1 to 3 and comparative example 2
Fig. 1 is a graph comparing experimental results of hydrogen sulfide poisoning experiments of the sensors of example 1, example 2, example 3 and comparative example 1. Fig. 2 is a graph comparing experimental results of the sensor siloxane poisoning experiments of example 1, example 2, example 3 and comparative example 2.
Claims (10)
1. The composite filtering agent for resisting siloxane and hydrogen sulfide poisoning is characterized by comprising the following components in parts by weight: 5-100 parts of organic titanate, 5-100 parts of saturated copper sulfate solution and 10-20 parts of molecular sieve.
2. The composite filtering agent for resisting siloxane and hydrogen sulfide poisoning according to claim 1, which is characterized by comprising the following components in parts by weight: 100 parts of organic titanate, 100 parts of saturated copper sulfate solution and 20 parts of molecular sieve.
3. The composite filtering agent for resisting siloxane and hydrogen sulfide poisoning according to claim 1, which is characterized by comprising the following components in parts by weight: 45 parts of organic titanate, 45 parts of saturated copper sulfate solution and 15 parts of molecular sieve.
4. The composite filtering agent for resisting siloxane and hydrogen sulfide poisoning according to claim 1, which is characterized by comprising the following components in parts by weight: 5 parts of organic titanate, 5 parts of saturated copper sulfate solution and 10 parts of molecular sieve.
5. The composite filter of claim 1, wherein the organic titanate is Ti (OR) 4 。
6. The silicone and hydrogen sulfide poisoning resistant composite filter of claim 1, wherein the organic titanate is isopropyl titanate.
7. A method for preparing a composite filtering agent for resisting siloxane and hydrogen sulfide poisoning, which is characterized by comprising the following steps of:
step S01, preparing materials, namely preparing 5-100 parts of organic titanate, 5-100 parts of saturated copper sulfate solution and 10-20 parts of molecular sieve;
step S02, placing the saturated copper sulfate solution prepared in the step S01 into a reaction container for standby;
step S03, dropwise adding the organic titanate prepared in the step S01 into the saturated copper sulfate solution in the step S02, and then uniformly stirring, wherein the organic titanate is hydrolyzed in the saturated copper sulfate solution to obtain a composite material emulsion;
step S04, adding the composite emulsion obtained in the step S03 into the molecular sieve in the step S01;
and S05, drying the molecular sieve treated in the step S04 to obtain the composite filtering agent.
8. The method for preparing the siloxane-resistant and hydrogen sulfide poisoning-resistant composite filtering agent according to claim 7, wherein in the step S01, the preparation method of the saturated copper sulfate solution is as follows, adding excessive copper sulfate pentahydrate into distilled water, stirring for 30-45 min, and filtering to obtain the saturated copper sulfate solution.
9. The method for preparing a composite filtering agent for siloxane and hydrogen sulfide poisoning resistance according to claim 7, wherein in step S02, the reaction vessel is one of a beaker, a flask, or an erlenmeyer flask.
10. The method for preparing the composite filtering agent for resisting siloxane and hydrogen sulfide poisoning according to claim 7, wherein in the step S05, the molecular sieve is dried for 24-30 hours at 60-70 ℃ to obtain the composite filtering agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310598721.6A CN116459787A (en) | 2023-05-25 | 2023-05-25 | Composite filtering agent for resisting siloxane and hydrogen sulfide poisoning and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310598721.6A CN116459787A (en) | 2023-05-25 | 2023-05-25 | Composite filtering agent for resisting siloxane and hydrogen sulfide poisoning and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116459787A true CN116459787A (en) | 2023-07-21 |
Family
ID=87177214
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310598721.6A Pending CN116459787A (en) | 2023-05-25 | 2023-05-25 | Composite filtering agent for resisting siloxane and hydrogen sulfide poisoning and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116459787A (en) |
-
2023
- 2023-05-25 CN CN202310598721.6A patent/CN116459787A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0794240A1 (en) | Mercury adsorbent | |
| CN107376673B (en) | Loaded with TiO2PES ultrafiltration membrane of nanotube and preparation method and application thereof | |
| CN112029106B (en) | Preparation method and application of modified HKUST-1 sulfur-resistant adsorbent for adsorbing n-hexane | |
| Chen et al. | Antenna-protected metal–organic squares for water/ammonia uptake with excellent stability and regenerability | |
| JPH07185317A (en) | Granular adsorbent, method for preparation thereof and method for adsorbing and drying neutral gas | |
| Khataei et al. | Applications of porous frameworks in solid‐phase microextraction | |
| CN114588879B (en) | IL@MOFs composite material and preparation method and application thereof | |
| Seredych et al. | Desulfurization of digester gas on wood-based activated carbons modified with nitrogen: importance of surface chemistry | |
| CN100548878C (en) | A kind of preparation method of hydrophobic silica gel | |
| CN108201877A (en) | A kind of graphene filtering material and its preparation method and application | |
| CN108160056B (en) | Preparation method of nylon membrane for adsorbing heavy metals | |
| US8500880B2 (en) | Amino acid salt articles and methods of making and using them | |
| Xu et al. | The aminosilane functionalization of cellulose nanocrystal aerogel via vapor‐phase reaction and its CO2 adsorption characteristics | |
| US5512262A (en) | Process for cleaning harmful gas | |
| US20190091653A1 (en) | Magnetic adsorbent for organic pollutant removal | |
| Li | Research progress of hydrogen sulfide adsorption based on MOFs | |
| CN116459787A (en) | Composite filtering agent for resisting siloxane and hydrogen sulfide poisoning and preparation method thereof | |
| CN1078236C (en) | Organic sulphur eliminating agent with normal temperature modified active carbon and its preparation | |
| CN115873265A (en) | Amination modified ZIF-8 material and preparation method thereof | |
| CN103894148B (en) | A kind of modifying method of activated carbon effectively removing trace acidic gas in air | |
| JP7004611B2 (en) | Carbon dioxide adsorbent and its manufacturing method | |
| WO1999055620A1 (en) | Reactive matrix for removing moisture from a fluorine containing gas and process | |
| KR20020043387A (en) | Manufacturing Method for Glass Fiber Reinforced Activated Carbon/Zeolite Composite Adsorbent with Waste Water Treatment Using Mixture of Zeolite and Phenolic Resin | |
| Attia et al. | The effect of activation method on the adsorption performance of saw-dust activated carbon | |
| Shakir et al. | Adsorptive Removal of Furfural from Wastewater on Prepared Activated Carbon from Sawdust |
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 |