CN115888804A - Dechlorinating agent and preparation method thereof - Google Patents
Dechlorinating agent and preparation method thereof Download PDFInfo
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- CN115888804A CN115888804A CN202211407901.3A CN202211407901A CN115888804A CN 115888804 A CN115888804 A CN 115888804A CN 202211407901 A CN202211407901 A CN 202211407901A CN 115888804 A CN115888804 A CN 115888804A
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- metal salt
- solution
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- molecular sieve
- dechlorinating
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- 230000000382 dechlorinating effect Effects 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 229910052751 metal Inorganic materials 0.000 claims abstract description 85
- 239000002184 metal Substances 0.000 claims abstract description 85
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 74
- 239000000243 solution Substances 0.000 claims abstract description 62
- 150000003839 salts Chemical class 0.000 claims abstract description 57
- 239000002808 molecular sieve Substances 0.000 claims abstract description 48
- 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 48
- 238000000034 method Methods 0.000 claims abstract description 35
- 239000002244 precipitate Substances 0.000 claims abstract description 30
- 239000012266 salt solution Substances 0.000 claims abstract description 28
- 239000012065 filter cake Substances 0.000 claims abstract description 26
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 20
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 19
- 239000000440 bentonite Substances 0.000 claims abstract description 18
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 18
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000047 product Substances 0.000 claims abstract description 18
- 239000011230 binding agent Substances 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 26
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 24
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 18
- 239000001099 ammonium carbonate Substances 0.000 claims description 18
- 238000006298 dechlorination reaction Methods 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000012716 precipitator Substances 0.000 claims description 13
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 229920002472 Starch Polymers 0.000 claims description 10
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 10
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 10
- 239000008107 starch Substances 0.000 claims description 10
- 235000019698 starch Nutrition 0.000 claims description 10
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 9
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 9
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 9
- 238000001125 extrusion Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 8
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 7
- 235000012438 extruded product Nutrition 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical class [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- 241000196324 Embryophyta Species 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical class [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 4
- 241000219793 Trifolium Species 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical class [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 239000011575 calcium Substances 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 235000013877 carbamide Nutrition 0.000 claims description 4
- 239000011777 magnesium Chemical class 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 4
- 229910052725 zinc Chemical class 0.000 claims description 4
- 239000011701 zinc Chemical class 0.000 claims description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims 2
- 244000275012 Sesbania cannabina Species 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims 1
- 235000017557 sodium bicarbonate Nutrition 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 19
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 15
- 239000000460 chlorine Substances 0.000 abstract description 15
- 229910052801 chlorine Inorganic materials 0.000 abstract description 15
- 238000000975 co-precipitation Methods 0.000 abstract description 9
- 239000011148 porous material Substances 0.000 abstract description 7
- 238000000465 moulding Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000035515 penetration Effects 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 30
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 11
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 10
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 10
- 239000002994 raw material Substances 0.000 description 10
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 230000000149 penetrating effect Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 241000219782 Sesbania Species 0.000 description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 3
- 239000013543 active substance Substances 0.000 description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- -1 alkaline earth metal carbonates Chemical class 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Classifications
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Catalysts (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a dechlorinating agent and a preparation method thereof, belonging to the technical field of dechlorinating agents, comprising a metal salt precipitate, alkali metal, a molecular sieve, bentonite, a binder and a pore-forming agent, wherein the preparation method of the dechlorinating agent comprises the following steps: (1) preparation of metal salt solution: (2) preparation of a precipitant solution: (3) preparation of metal salt precipitate: (4) Adding alkali metal, molecular sieve, bentonite, binder and pore-forming agent into the nano-scale metal salt filter cake in proportion, pouring the materials into a mixing bin, stirring uniformly, and extruding for molding; and (5) drying and roasting the product extruded by the extruder. The invention has the beneficial effects that: the metal salt precipitate is prepared by adopting a coprecipitation method, the pore size distribution of the dechlorinating agent is more concentrated, a filter cake is directly extruded and roasted without drying and parallel flow adding processes, the prepared dechlorinating agent has higher strength and penetration chlorine capacity, the powder is dropped and the breaking rate is lower in the using process, and the service time of the dechlorinating catalyst is prolonged.
Description
The technical field is as follows:
the invention belongs to the technical field of dechlorinating agents, and particularly relates to a dechlorinating agent and a preparation method thereof.
Background art:
in the dechlorination technology developed at home and abroad at present, common dechlorinating agent systems comprise a CuO-ZnO series, a CaO-Al2O3 series, a NaO-Al2O3 series, a K2O-Fe2O3 series and a dechlorinating agent which is formed by using a molecular sieve and an active substance.
Chinese patent CN1064099A discloses a dechlorinating agent which uses alkali metal and alkaline earth metal as dechlorinating active components and natural inorganic clay as a binder, and can reduce the content of hydrogen chloride after dechlorination to below 0.50mg/L when the reaction temperature is lower than 280 ℃.
Chinese patent CN1079415A discloses a dechlorinating agent using alumina and alkali metal and alkaline earth metal carbonates, which can reduce the content of hydrogen chloride in the raw material to below 0.50 mg/L.
Chinese patent CN1178133A uses sodium carbonate, calcium carbonate and magnesium oxide as active components, uses natural inorganic clay as a carrier, and can reduce chlorine in raw materials to below 0.10mg/L when the reaction temperature is lower than 480 ℃, but the chlorine capacity can only reach 30%.
Chinese patent CN1539921A discloses a multifunctional dechlorinating agent composed of a molecular sieve and an active substance, wherein the dechlorinating agent is a multi-component compound and comprises, by mass, 0-30% of a binder, 5-20% of the molecular sieve, 30-90% of an alkali metal-alkaline earth metal oxide and 1-5% of a synergist, and can work at a wide temperature range of 100-550 ℃ but only can reduce chlorine in raw materials to about 1 mg/L.
U.S. Pat. No. 4,8978,893,897,897 discloses a dechlorinating agent, which is prepared by loading alkaline earth metal as an active substance on alumina, but the chlorine capacity can only reach 13.8%, and the chlorine content after dechlorination is about 1 mg/L. In summary, most of the dechlorinating agents known in the prior art are prepared by impregnating 17% or less of active components on a porous carrier, the chlorine capacity is generally not high, higher dechlorination effect cannot be achieved, and the dechlorinating agents can be generally used only at lower temperature of 500 ℃ or less.
The invention content is as follows:
in order to solve the problems and overcome the defects of the prior art, the invention provides the dechlorinating agent which can ensure that the dechlorinated coal gas can meet the subsequent processing requirements and reduce the corrosion of equipment and the poisoning of catalysts for subsequent hydrolysis, hydrogenation and the like; is particularly suitable for being applied to medium and low temperature dechlorinating agents in coal chemical industry,
the specific technical scheme for solving the technical problems comprises the following steps: the dechlorination agent is characterized in that: comprises metal salt precipitate, alkali metal, molecular sieve, bentonite, adhesive and pore-forming agent.
Further, the dechlorination agent comprises 100 parts of metal salt precipitate and alkali metal: 0.5-10 parts of molecular sieve: 0.5-10 parts of bentonite: 0.5-10 parts of binder: 0.5-10 parts of pore-forming agent: 0.5-10 parts.
A preparation method of a dechlorinating agent adopts the dechlorinating agent and comprises the following steps:
(1) Preparation of metal salt solution: dissolving metal salt in water to prepare a solution with the concentration of 50-200g/L and the temperature of 50-80 ℃;
(2) Preparation of precipitant solution: dissolving the precipitant in water, and mixing to obtain precipitant solution; the concentration of the solution is 200g/L, and the temperature of the solution is 50 ℃;
(3) Preparation of metal salt precipitate: adding a metal salt solution and a precipitant solution in a concurrent flow manner, controlling the reaction temperature at 40-80 ℃ and the pH value at 7.5-10.5, and filtering and washing to obtain a nano-scale metal salt filter cake;
(4) Adding alkali metal, molecular sieve, bentonite, binder and pore-forming agent into the nanoscale metal salt filter cake in proportion, pouring the materials into a mixing bin, stirring and uniformly mixing for 30min, immediately feeding into a strip extruder, and performing extrusion molding;
(5) Drying the product extruded by the extruder at 100-200 ℃ for 3h, and roasting at 500-700 ℃ for 2h to obtain the dechlorinating agent.
Further, the metal salt is one or a mixture of more than two of soluble metal salts of calcium, magnesium and zinc.
Furthermore, the precipitant is a mixture of more than two of ammonia water, ammonium carbonate, ammonium bicarbonate and urea.
Further, the alkali metal is one or a mixture of more than two of sodium carbonate, sodium bicarbonate, potassium carbonate, sodium hydroxide and potassium hydroxide.
Further, the binder is one or a mixture of more than two of hydroxymethyl cellulose, water, nitric acid and silicate.
Further, the pore-forming agent is one or a mixture of more than two of sesbania powder, plant starch and dihydric alcohol.
Further, the molecular sieve is one or a mixture of more than two of an A-type molecular sieve, a NaY molecular sieve and a ZSM-5 molecular sieve, and the silicon-aluminum ratio of the molecular sieve is more than 1.3.
Further, the appearance of the extrusion molding product is cylindrical, clover, butterfly and five gears; the diameter is 3-10mm, and the length is 2-40mm.
The invention has the beneficial effects that:
one advantage of the invention is that the metal salt precipitate is prepared by a coprecipitation method, so that the obtained dechlorinating agent has more concentrated pore size distribution and better catalytic dechlorination effect;
one advantage of the invention is that the metal salt precipitate is prepared by a coprecipitation method, and is directly extruded and roasted, and the prepared dechlorinating agent has higher strength and penetrating chlorine capacity.
One advantage of the invention is that the coprecipitation method is provided for preparing the metal salt precipitate, on the basis of which the filter cake is directly extruded and roasted without drying and cocurrent adding processes, and the prepared dechlorinating agent has higher strength and penetrating chlorine capacity, has lower powder dropping and breaking rate in the using process and prolongs the service time of the dechlorinating catalyst.
Description of the drawings:
FIG. 1 is a diagram showing the results of analysis by a fully automatic specific surface area and porosity analyzer in example 3 of the present invention;
FIG. 2 is the result of the full-automatic specific surface area and porosity analyzer of comparative example 1 of the present invention;
FIG. 3 shows the results of the full-automatic specific surface area and porosity analyzer of comparative example 2 of the present invention;
FIG. 4 shows the results of the full-automatic specific surface area and porosity analyzer of comparative example 3 of the present invention;
FIG. 5 shows the results of the full-automatic specific surface area and porosity analyzer of comparative example 4 of the present invention;
FIG. 6 shows the results of the full-automatic specific surface area and porosity analyzer of comparative example 5 of the present invention;
the specific implementation mode is as follows:
in the description of the invention, specific details are given only to enable a full understanding of the embodiments of the invention, but it should be understood by those skilled in the art that the invention is not limited to these details for the implementation. In other instances, well-known structures and functions have not been described or shown in detail to avoid obscuring the points of the embodiments of the invention. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The specific implementation mode of the invention is as follows:
in order to better understand the present invention, the specific embodiments are specifically illustrated, it is emphasized that the effects of the embodiments are not substantially different from the various embodiments within the scope of the present invention, including the respective reagents and the content ratios of the reagents, which can achieve the described effects of the present invention and solve the above problems, and other combinations are not described herein;
the first embodiment is as follows:
a dechlorinating agent is prepared from the deposit of metallic salt, alkali metal, molecular sieve, bentone, adhesive and pore-forming agent.
The dechlorinating agent comprises 100 parts of metal salt precipitate and alkali metal: 0.5 part, molecular sieve: 0.5 part, bentonite: 0.5 part, binder: 0.5 part of pore-forming agent: 0.5 part.
A preparation method of a dechlorinating agent comprises the following steps:
(1) Preparation of metal salt solution: dissolving metal salt in water to prepare a solution with the concentration of 50g/L and the temperature of 50 ℃;
(2) Preparation of precipitant solution: dissolving a precipitator in water, and mixing to prepare a precipitator solution; the concentration of the solution is 200g/L, and the temperature of the solution is 50 ℃;
(3) Preparation of metal salt precipitate: adding a metal salt solution and a precipitator solution in a concurrent flow manner, controlling the reaction temperature at 40 ℃ and the pH value at 7.5, and then filtering and washing to obtain a nano-scale metal salt filter cake;
(4) Adding alkali metal, molecular sieve, bentonite, binder and pore-forming agent into the nanoscale metal salt filter cake in proportion, pouring the materials into a mixing bin, stirring and uniformly mixing for 30min, immediately feeding into a strip extruder, and performing extrusion molding;
(5) And drying the product extruded by the extruder at 100 ℃ for 3h, and roasting at 500 ℃ for 2h to obtain the dechlorinating agent catalyst.
Wherein the metal salt is one or more nitrates of calcium, magnesium and zinc.
Wherein the precipitant is one or more of ammonia water, ammonium carbonate, ammonium bicarbonate and urea.
Wherein the alkali metal is one or more of sodium carbonate, sodium bicarbonate, potassium carbonate, sodium hydroxide and potassium hydroxide.
Wherein the binder is one or a mixture of more than two of hydroxymethyl cellulose, water, nitric acid and silicate.
The pore-forming agent is one or a mixture of more than two of sesbania powder, plant starch and dihydric alcohol.
The molecular sieve is one or a mixture of more than two of an A-type molecular sieve, a NaY molecular sieve and a ZSM-5 molecular sieve, and the silica-alumina ratio of the molecular sieve is more than 1.3.
Wherein the appearance of the extrusion molded product is a cylinder, clover, butterfly and five gears; the diameter is 3-10mm, and the length is 2-40mm.
The second embodiment:
a dechlorinating agent is prepared from the deposit of metallic salt, alkali metal, molecular sieve, bentone, adhesive and pore-forming agent.
The dechlorinating agent comprises 100 parts of metal salt precipitate and alkali metal: 10 parts of molecular sieve: 10 parts of bentonite: 10 parts of binder: 10 parts of pore-forming agent: 10 parts.
A preparation method of a dechlorinating agent comprises the following steps:
(1) Preparation of metal salt solution: dissolving metal salt in water to prepare a solution with the concentration of 200g/L and the temperature of 80 ℃;
(2) Preparation of precipitant solution: dissolving a precipitator in water, and mixing to prepare a precipitator solution; the concentration of the solution is 200g/L, and the temperature of the solution is 50 ℃;
(3) Preparation of metal salt precipitate: adding a metal salt solution and a precipitant solution in a concurrent flow manner, controlling the reaction temperature at 40-80 ℃ and the pH value at 7.5-10.5, and filtering and washing to obtain a nano-scale metal salt filter cake;
(4) Adding alkali metal, molecular sieve, bentonite, binder and pore-forming agent into the nanoscale metal salt filter cake in proportion, pouring the materials into a mixing bin, stirring and mixing uniformly for 30min, immediately entering a strip extruder, and performing extrusion molding;
(5) And drying the product extruded by the extruder at 200 ℃ for 3h, and roasting at 700 ℃ for 2h to obtain the dechlorinating agent catalyst.
Wherein the metal salt is one or more nitrates of calcium, magnesium and zinc.
Wherein the precipitant is a mixture of more than one of ammonia water, ammonium carbonate, ammonium bicarbonate and urea.
Wherein the alkali metal is one or a mixture of more than two of sodium carbonate, sodium bicarbonate, potassium carbonate, sodium hydroxide and potassium hydroxide.
Wherein the binder is one or a mixture of more than two of hydroxymethyl cellulose, water, nitric acid and silicate.
The pore-forming agent is one or a mixture of more than two of sesbania powder, plant starch and dihydric alcohol.
The molecular sieve is one or a mixture of more than two of an A-type molecular sieve, a NaY molecular sieve and a ZSM-5 molecular sieve, and the silica-alumina ratio of the molecular sieve is more than 1.3.
Wherein the appearance of the extrusion molding product is a cylinder, clover, butterfly and five gears; the diameter is 3-10mm, and the length is 2-40mm.
Example three:
(1) Preparation of metal salt solution: preparing a metal salt solution from calcium nitrate, magnesium nitrate and zinc nitrate, wherein the concentration of the solution is 100g/L, and the temperature of the solution is 60 ℃;
(2) Preparation of precipitant solution: one or more of ammonium carbonate and ammonium bicarbonate are mixed to prepare a precipitator solution, the concentration of the solution is 200g/L, and the temperature of the solution is 50 ℃;
(3) Preparation of metal salt precipitate: adding the metal salt solution and the precipitant solution in a concurrent flow manner, controlling the reaction temperature to be 55-60 ℃ and the pH value to be 8.5-9.5; then filtering and washing to obtain a nano-scale metal salt filter cake;
(4) Pouring the raw materials into a mixing bin in proportion, uniformly stirring for 30min, immediately feeding into a strip extruding machine, and extruding and molding; the extruded product is 7.0mm cylinder in appearance and 3-20mm in length;
the metal salt-sodium carbonate composite material comprises 100 parts of metal salt precipitate and sodium carbonate: 2 parts of molecular sieve (silica-alumina ratio is 1.5): 3 parts of bentonite: 6 parts, hydroxymethyl cellulose: 4 parts, starch: 5 parts of (a) a mixture of (b),
(5) Drying the product extruded by the extruder at 100-200 ℃ for 3h, and roasting at 500-700 ℃ for 2h to obtain the final product of the dechlorinating agent catalyst.
In order to more intuitively show the process advantages of the invention, the preparation method of the dechlorination agent is compared with the equivalent replacement method adopted by the same process,
comparative example 1:
the procedure is as in example 3, except that: in the preparation process of the comparative example, the prepared metal salt precipitate is extruded and roasted after being dried;
specifically, the method comprises the following steps:
(1) Preparation of metal salt solution: preparing calcium nitrate, magnesium nitrate and zinc nitrate into a metal salt solution, wherein the concentration of the solution is 100g/L, and the temperature of the solution is 60 ℃;
(2) Preparation of precipitant solution: one or more of ammonium carbonate and ammonium bicarbonate are mixed to prepare a precipitator solution, the concentration of the solution is 200g/L, and the temperature of the solution is 50 ℃;
(3) Preparation of metal salt precipitate: adding the metal salt solution and the precipitant solution in a concurrent flow manner, controlling the reaction temperature to be 55-60 ℃ and the pH value to be 8.5-9.5; then filtering and washing to obtain a nano-scale metal salt filter cake;
(4) Drying and crushing the filter cake at 120 ℃ to obtain nano metal salt powder;
(5) Adding raw materials into the nano metal salt powder in proportion, pouring the mixture into a mixing bin, uniformly stirring the mixture for 30min, immediately feeding the mixture into a strip extruding machine, and performing extrusion molding; the extruded product is 7.0mm cylinder in appearance and 3-20mm in length;
the metal salt-sodium carbonate composite material comprises 100 parts of metal salt precipitate and sodium carbonate: 2 parts of molecular sieve (the ratio of silicon to aluminum is 1.5): 3 parts of bentonite: 6 parts, hydroxymethyl cellulose: 4 parts, starch: 5 parts of (a) a mixture of (b),
(6) Drying the product extruded by the extruder at 100-200 ℃ for 3h, and roasting at 500-700 ℃ for 2h to obtain the final product of the dechlorinating agent catalyst.
Comparative example 2:
the procedure is as in example 3, except that: in the preparation process of the comparative example, the prepared metal salt precipitate does not adopt a coprecipitation method, but adopts a direct addition method;
specifically, the method comprises the following steps:
1. adding sodium carbonate into the mixed powder of calcium hydroxide, magnesium oxide and zinc oxide: 2%, molecular sieve (silica to alumina ratio 1.5): 3% of bentonite: 6%, hydroxymethyl cellulose: 4%, starch: 5 percent and 40 percent of water are poured into the mixing bin according to the proportion, stirred and mixed uniformly for 30min, immediately enters a strip extruding machine, and is extruded and molded; the extruded product is 7.0mm cylinder in appearance and 3-20mm in length;
2. drying the product extruded by the extruder at 100-200 ℃ for 3h, and roasting at 500-700 ℃ for 2h to obtain the final finished catalyst.
Comparative example 3:
the procedure is as in example 3, except that: in the preparation process of the comparative example, the molecular sieve with the silicon-aluminum ratio of 1.0 is adopted in the comparative example 3;
specifically, the method comprises the following steps:
1. metal salt solution: preparing calcium nitrate, magnesium nitrate and zinc nitrate into a metal salt solution, wherein the concentration of the solution is 100g/L, and the temperature of the solution is 60 ℃;
2. precipitant solution: one or more of ammonium carbonate and ammonium bicarbonate are mixed to prepare a precipitator solution, the concentration of the solution is 200g/L, and the temperature of the solution is 50 ℃;
3. adding the metal salt solution and the precipitant solution in a concurrent flow manner, controlling the reaction temperature to be 55-60 ℃ and the pH value to be 8.5-9.5;
4. filtering and washing the precipitate to obtain a nano-scale metal salt filter cake;
5. adding sodium carbonate to the filter cake: 2%, molecular sieve (silica to alumina ratio 1): 3%, bentonite: 6%, hydroxymethyl cellulose: 4%, starch: 5 percent, pouring the raw materials into a mixing bin according to a proportion, uniformly stirring for 30min, immediately feeding into a strip extruding machine, and extruding and molding; the extruded product is 7.0mm cylinder in appearance and 3-20mm in length;
6. drying the product extruded by the extruder at 100-200 ℃ for 3h, and roasting at 500-700 ℃ for 2h to obtain the final product of the dechlorinating agent catalyst.
Comparative example 4:
the preparation method is the same as that of the embodiment 3, except that: in the preparation process of the comparative example, the metal salt solution and the precipitator solution are added in the comparative example 4 in sequence;
specifically, the method comprises the following steps:
1. metal salt solution: preparing calcium nitrate, magnesium nitrate and zinc nitrate into a metal salt solution, wherein the concentration of the solution is 100g/L, and the temperature of the solution is 60 ℃;
2. precipitant solution: one or more of ammonium carbonate and ammonium bicarbonate are mixed to prepare a precipitator solution, the concentration of the solution is 200g/L, and the temperature of the solution is 50 ℃;
3. adding a metal salt solution into a reactor, slowly adding a precipitant solution into the metal salt solution, controlling the reaction temperature to be 55-60 ℃, controlling the reaction time to be 30-45min, and controlling the end-point pH value to be 8.5-9.5;
4. filtering and washing the precipitate to obtain a nano-scale metal salt filter cake;
5. adding sodium carbonate to the filter cake: 2%, molecular sieve (silica to alumina ratio 1.5): 3% of bentonite: 6%, hydroxymethyl cellulose: 4%, starch: 5%, pouring the raw materials into a mixing bin in proportion, stirring and uniformly mixing for 30min, immediately feeding into a strip extruding machine, and extruding and molding; the extruded product is 7.0mm cylinder in appearance and 3-20mm in length;
6. drying the product extruded by the extruder at 100-200 ℃ for 3h, and roasting at 500-700 ℃ for 2h to obtain the final finished product of the dechlorinating agent catalyst.
Comparative example 5:
the preparation method is the same as in comparative example 4, except that: in the preparation process of the comparative example, the filter cake is dried;
specifically, the method comprises the following steps:
1. metal salt solution: preparing calcium nitrate, magnesium nitrate and zinc nitrate into a metal salt solution, wherein the concentration of the solution is 100g/L, and the temperature of the solution is 60 ℃;
2. precipitant solution: one or more of ammonium carbonate and ammonium bicarbonate are mixed to prepare a precipitator solution, the concentration of the solution is 200g/L, and the temperature of the solution is 50 ℃;
3. adding a metal salt solution into a reactor, slowly adding a precipitant solution into the metal salt solution, controlling the reaction temperature to be 55-60 ℃, controlling the reaction time to be 30-45min, and controlling the end-point pH value to be 8.5-9.5;
4. filtering and washing the precipitate to obtain a nano-scale metal salt filter cake;
5. drying and crushing the filter cake at 120 ℃ to obtain nano metal salt powder;
6. adding sodium carbonate to the nano metal salt powder: 2%, molecular sieve (silica to alumina ratio 1.5): 3% of bentonite: 6%, hydroxymethyl cellulose: 4%, starch: 5 percent, pouring the raw materials into a mixing bin according to a proportion, uniformly stirring for 30min, immediately feeding into a strip extruding machine, and extruding and molding; the extruded product is a cylinder with the appearance of 7.0mm and the length of 3-20mm;
7. drying the product extruded by the extruder at 100-200 ℃ for 3h, and roasting at 500-700 ℃ for 2h to obtain the final finished product of the dechlorinating agent catalyst.
And (3) strength measurement: the strength of the sample was measured using a DL3 model smart particle Strength measuring apparatus manufactured by Lian Peng Bright science and technology development Ltd.
Penetration chlorine capacity test method: crushing the catalyst, screening 5mL of a 20-40-mesh sample, and filling the sample into an evaluation device; the temperature of the device is 150 +/-0.5 ℃; raw material gas component: 1000ppm of hydrogen chloride gas and the balance of nitrogen; the flow rate of the raw material gas is controlled by a mass flowmeter, and the airspeed is 1000h -1 . The chlorine content at the outlet was greater than 1ppm, i.e.breakthrough was considered. Breakthrough sulfur capacity = (mass of chlorine consumed in feed gas/mass of catalyst) × 100%.
Table 1: catalyst indexes of dechlorinating agents in different processes
From the data analysis in table 1, it can be seen that:
example 3 compared to comparative example 1: in the embodiment 3, the filter cake is not dried, the hydroxyl on the surface of the filter cake is not destroyed, and the particles connected by the hydroxyl after extrusion strip roasting are not destroyed, so that the prepared catalyst has higher strength, has lower powder falling and breaking rate in the using process, and prolongs the service time of the catalyst.
Example 3 compared to comparative example 2: example 3 the preparation of the calcium-magnesium mixture by the coprecipitation method has more concentrated pore size distribution and better catalytic dechlorination effect,
although comparative example 2 also did not proceed with drying, the strength of the catalyst was the worst after extrusion-calcination.
Example 3 in comparison to comparative example 3: the molecular sieve with the silicon-aluminum ratio of 1.5 is adopted in the example 3, the molecular sieve with the silicon-aluminum ratio of 1.0 is adopted in the comparative example 3, and the dechlorination effect of the molecular sieve with the silicon-aluminum ratio of more than 1.3 is higher than that of the molecular sieve with the silicon-aluminum ratio of less than 1.3.
Example 3 in comparison to comparative example 4: the catalyst prepared in the comparative example 4 has cracks after high-temperature roasting, has serious surface powder falling and can not be used;
this is probably due to the fact that example 3 employed: adding the metal salt solution and the precipitant solution in a concurrent flow manner, controlling the reaction temperature to be 55-60 ℃ and the pH value to be 8.5-9.5; therefore, the reaction system always keeps a stable pH value, the pore size distribution of the metal salt precipitate is more uniform and concentrated, and the finally formed product is easy to form and is difficult to fall off.
Comparative example 4 compared to comparative example 5: although the filter cake drying is not adopted in the later stage of the comparative example 4, the difference between the penetrating chlorine capacity and the average compressive strength is not large, because the comparative example 4 and the comparative example 5 do not adopt the concurrent flow addition, the PH value of the reaction system is changed, the pore diameter of the metal salt precipitate is not uniform, the pore structure is formed, and the strength of the product cannot be changed by adopting the filter cake drying in the later stage or not.
In conclusion: one advantage of the invention is that the metal salt precipitate is prepared by a coprecipitation method, so that the obtained dechlorinating agent has more concentrated pore size distribution and better catalytic dechlorination effect;
one advantage of the invention is that the metal salt precipitate is prepared by a coprecipitation method, and is directly extruded and roasted, and the prepared dechlorinating agent has higher strength and penetrating chlorine capacity.
One advantage of the invention is that the coprecipitation method is provided for preparing the metal salt precipitate, on the basis of which the filter cake is directly extruded and roasted without drying and cocurrent adding processes, and the prepared dechlorinating agent has higher strength and penetrating chlorine capacity, has lower powder dropping and breaking rate in the using process and prolongs the service time of the dechlorinating catalyst.
Claims (10)
1. A dechlorination agent, which is characterized in that: comprises metal salt precipitate, alkali metal, molecular sieve, bentonite, adhesive and pore-forming agent.
2. The dechlorination agent according to claim 1, characterized in that the components in the dechlorination agent comprise 100 parts of metal salt precipitates, alkali metal: 0.5-10 parts of molecular sieve: 0.5-10 parts of bentonite: 0.5-10 parts of binder: 0.5-10 parts of pore-forming agent: 0.5-10 parts.
3. A preparation method of a dechlorination agent adopts the dechlorination agent 1 or 2, and is characterized in that: the preparation method comprises the following steps:
(1) Preparation of metal salt solution: dissolving metal salt in water to prepare solution with the concentration of 50-200g/L and the temperature of 50-80 ℃;
(2) Preparation of precipitant solution: dissolving a precipitator in water, and mixing to prepare a precipitator solution; the concentration of the solution is 200g/L, and the temperature of the solution is 50 ℃;
(3) Preparation of metal salt precipitate: adding a metal salt solution and a precipitant solution in a concurrent flow manner, controlling the reaction temperature at 40-80 ℃ and the pH value at 7.5-10.5, and filtering and washing to obtain a nano-scale metal salt filter cake;
(4) Adding alkali metal, molecular sieve, bentonite, binder and pore-forming agent into the nanoscale metal salt filter cake in proportion, pouring the materials into a mixing bin, stirring and uniformly mixing for 30min, immediately feeding into a strip extruder, and performing extrusion molding;
(5) Drying the product extruded by the extruder at 100-200 ℃ for 3h, and roasting at 500-700 ℃ for 2h to obtain the dechlorinating agent.
4. The process for producing a dechlorinating agent according to claim 3, wherein the metal salt is one or a mixture of two or more soluble metal salts of calcium, magnesium and zinc.
5. The process for preparing dechlorinating agent according to claim 3, wherein the precipitant is a mixture of two or more of ammonia water, ammonium carbonate, ammonium bicarbonate and urea.
6. The process for producing a dechlorinating agent according to claim 3, wherein the alkali metal is one or a mixture of two or more of sodium carbonate, sodium hydrogen carbonate, potassium carbonate, sodium hydroxide and potassium hydroxide.
7. The method of claim 3, wherein the binder is one or a mixture of two or more of hydroxymethyl cellulose, water, nitric acid, and silicate.
8. The method of claim 3, wherein the pore-forming agent is one or a mixture of two or more of sesbania powder, plant starch, and glycol.
9. The method for preparing dechlorinating agent according to claim 3, characterized in that the molecular sieve is one or a mixture of more than two of A type molecular sieve, naY molecular sieve and ZSM-5 molecular sieve, and the silicon-aluminum ratio of the molecular sieve is more than 1.3.
10. The process for the preparation of a dechlorination agent according to claim 3, characterized in that the extruded product has the appearance of a cylinder, clover, butterfly, five-wheel gear; the diameter is 3-10mm, and the length is 2-40mm.
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