CN103127903B - Normal-temperature dechlorinating agent - Google Patents
Normal-temperature dechlorinating agent Download PDFInfo
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- CN103127903B CN103127903B CN201310095160.4A CN201310095160A CN103127903B CN 103127903 B CN103127903 B CN 103127903B CN 201310095160 A CN201310095160 A CN 201310095160A CN 103127903 B CN103127903 B CN 103127903B
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- 230000000382 dechlorinating effect Effects 0.000 title abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 59
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 56
- 239000000292 calcium oxide Substances 0.000 claims abstract description 50
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 50
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 29
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 29
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 29
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 29
- 238000002360 preparation method Methods 0.000 claims abstract description 24
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 18
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 16
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004927 clay Substances 0.000 claims abstract description 12
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 239000011787 zinc oxide Substances 0.000 claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 39
- 238000002156 mixing Methods 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 25
- 238000004898 kneading Methods 0.000 claims description 23
- 239000000126 substance Substances 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 12
- 229960004643 cupric oxide Drugs 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 24
- 239000013078 crystal Substances 0.000 abstract description 13
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 8
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 3
- 229910001448 ferrous ion Inorganic materials 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 230000003247 decreasing effect Effects 0.000 abstract description 2
- 239000005751 Copper oxide Substances 0.000 abstract 1
- 229960000892 attapulgite Drugs 0.000 abstract 1
- 229910000431 copper oxide Inorganic materials 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 229910052625 palygorskite Inorganic materials 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 38
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 24
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 24
- 229940010698 activated attapulgite Drugs 0.000 description 18
- 238000009530 blood pressure measurement Methods 0.000 description 18
- 230000000704 physical effect Effects 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 15
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 description 13
- 239000007789 gas Substances 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000006298 dechlorination reaction Methods 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- -1 carbonate compound Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011143 downstream manufacturing Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 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
- 238000001833 catalytic reforming Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005262 decarbonization Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 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 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
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Abstract
The invention discloses a normal-temperature dechlorinating agent. The normal-temperature dechlorinating agent is mainly prepared from 20-30 parts of ferrous sulfate, 20-40 parts of CaO and 10-25 parts of attapulgite clay in parts by weight and further comprises 15-25 parts of waste catalyst, wherein active components of the waste catalyst include copper oxide and zinc oxide. According to the normal-temperature dechlorinating agent, the ferrous sulfate has weak acidity and can react with calcium carbonate impurity in calcium oxide to enable the crystal form of the calcium oxide to be more regular, and meanwhile, ferrous ions are continuously oxidized into iron oxide to enable the crystal forms of the calcium oxide and the iron oxide to be mutually doped, so that the dechlorinating effect of the dechlorinating agent is improved; and according to a preparation method of dechlorinating agent disclosed by the invention, a roasting process is not needed, the energy consumption is reduced, devices used in the preparation process are decreased, the preparation step is simplified, and the preparation cost is lowered.
Description
Technical field
The present invention relates to a kind of normal temperature antichlor, belong to gas purification technique field.
Background technology
In petrochemical industry, the reforming catalyst of catalytic reforming process in use activity can fail gradually, need timing regeneration active to recover it, and in the regenerative process of catalyst, regenerating medium organic chloride is needed to carry out oxychlorination to catalyst, during oxychlorination process carries out or terminate after, the organic chloride of portion of residual is converted into hydrogen chloride HCl under the high temperature conditions.HCl can flow into pipeline and the equipment of follow-up system with the gas after regeneration, cause corrosion to pipeline or equipment, or emptying after stain air.In addition, if containing ammonia NH in downstream process raw material
3, then can generate ammonium chloride, cause equipment blocking, the frequent incrustation of recycle compressor entrance, affect unit normal run; In addition, if HCl is by after the Catalyst Adsorption in downstream process, the acidity change of catalyst can be caused, affect the normal performance of catalyst, make technique be difficult to normal operation, bring very large economic loss to enterprise.
In recent years, generally adopt in commercial plant antichlor remove regeneration produce gas in hydrogen chloride gas, Chinese patent literature CN1088388C discloses a kind of refined antichlor and preparation method thereof, described antichlor is using the compound of sodium, calcium and zinc as the active component of antichlor, directly mix extruded moulding for carrier adds suitable quantity of water with kaolin or rectorite, bentonite, diatomite, then form through 350-400 DEG C of roasting.Above-mentioned technology employs the active material of ternary system, comprise the compound of sodium (sodium carbonate, NaOH or sodium acid carbonate), calcium (calcium carbonate, calcium hydroxide or calcium oxide) and zinc (zinc carbonate or zinc oxide), the serviceability temperature scope of this antichlor is room temperature to 400 DEG C, even and if the chlorosity when 300-400 DEG C also can only reach about 30%, cannot realize higher chlorosity under normal temperature.
For this reason, Chinese patent literature CN101269294A discloses a kind of Zincium-calcium dechlorinating agent at normal temperature and preparation method thereof, this antichlor can realize the dechlorination function of antichlor at normal temperatures, improve HCl content and the removal precision of original antichlor, but antichlor disclosed in prior art all needs the process of high-temperature roasting in preparation process, in order to the hydroxide used in raw material or carbonate compound be converted to the oxide of regular crystal forms or intrinsic contaminants in metal oxide removed the oxide obtaining regular crystal forms, realize dechlorination function, therefore for coordinating the roasting process of antichlor also to need to be equipped with corresponding equipment, such as roaster, add the preparation process of antichlor, improve the preparation cost of antichlor.
Summary of the invention
Technical problem to be solved by this invention be antichlor of the prior art in preparation process owing to there is roasting process, need to consume unnecessary energy, supporting equipment is set, increase the technical problem of preparation cost of antichlor, so provide that a kind of preparation method is simple, low cost and the high normal temperature antichlor of chlorosity.
For this reason, the technical scheme that the present invention takes is:
A kind of normal temperature antichlor, described normal temperature antichlor is made primarily of ferrous sulfate, calcium oxide and Concave-convex clay rod, wherein ferrous sulfate is 20-30 weight portion, calcium oxide is 20-40 weight portion, Concave-convex clay rod 10-25 weight portion, containing calcium carbonate impurity in described calcium oxide; Described normal temperature antichlor is prepared from by following steps:
(1) a certain amount of ferrous sulfate, calcium oxide and Concave-convex clay rod are mixed, and abundant kneading;
(2) in the material after described step (1) mixing, add binding agent, above-mentioned substance mixed grind is become paste, by described paste extruded moulding;
(3) the stripe shape thing of described step (2) is carried out drying at 150-200 DEG C, can antichlor be obtained.
In above-mentioned normal temperature antichlor, described normal temperature antichlor is made primarily of the agent of giving up of ferrous sulfate, calcium oxide, Concave-convex clay rod and catalyst; The catalyst also adding 15-25 weight portion in described step (1) gives up agent, and the give up active component of agent of described catalyst is cupric oxide and zinc oxide.
In above-mentioned normal temperature antichlor, the described catalyst content of cupric oxide in agent that gives up is 15-20wt%; The content of zinc oxide is 10-20wt%.
In above-mentioned normal temperature antichlor, the agent of giving up of described catalyst is that catalyst for methanol gives up agent.
In above-mentioned normal temperature antichlor, the give up particle diameter of agent of described catalyst is not more than 10nm.
In above-mentioned normal temperature antichlor, described binding agent is Ludox or CMC.
In above-mentioned normal temperature antichlor, the time of described kneading is 40-60 minute.
In above-mentioned normal temperature antichlor, the drying time of described bar is 2 hours.。
Compared with prior art, tool of the present invention has the following advantages:
(1) normal temperature antichlor of the present invention is made primarily of ferrous sulfate, calcium oxide and Concave-convex clay rod, wherein ferrous sulfate is 20-30 weight portion, calcium oxide is 20-40 weight portion, Concave-convex clay rod 10-25 weight portion, containing calcium carbonate impurity in described calcium oxide; Described normal temperature antichlor is prepared from by following steps: a certain amount of ferrous sulfate, calcium oxide and Concave-convex clay rod mix by (1), and abundant kneading; (2) in the material after described step (1) mixing, add binding agent, above-mentioned substance mixed grind is become paste, by described paste extruded moulding; (3) the stripe shape thing of described step (2) is carried out drying at 150-200 DEG C, can antichlor be obtained.Normal temperature antichlor of the present invention only just can obtain the oxide with regular crystal formation in preparation process in the process of drying, do not need the process of roasting, reduce energy ezpenditure, decrease the equipment used in preparation process, simplify preparation process, reduce preparation cost; Stripe shape thing carries out in dry process at 150-200 DEG C, because ferrous sulfate has faintly acid, can react with the impurity calcium carbonate in calcium oxide, make the crystal formation of calcium oxide more regular, meanwhile, ferrous ion is constantly oxidized to the oxide of iron, the crystal formation of calcium oxide and iron oxide is adulterated mutually, obtains regular CaO-Fe
2o
3crystal structure, improves the dechlorination effect of antichlor, and its disposable chlorosity that penetrates reaches more than 50%.
(2) catalyst employed in the raw material used in the present invention in industrial production gives up agent, the give up active component in agent and other active component in antichlor of catalyst is formed and acts synergistically, improve the removal precision of antichlor of the present invention, make described dechlorination catalyst disposable HCl content can up to 62% at normal temperatures simultaneously; Other composition in agent and catalyst gives up, improve the intensity of antichlor of the present invention on the whole, show after tested, the side pressure strength of this antichlor reaches more than 80N/cm.
(3) normal temperature antichlor of the present invention, utilization contains active component cupric oxide, the catalyst of zinc oxide gives up, and agent substitutes pure cupric oxide, zinc oxide, not only save cost but also achieved catalyst and to have given up the recycling of agent, avoid energy waste, the catalyst decreased in industrial production gives up the pollution that agent brings.
(4) normal temperature antichlor of the present invention, to give up agent owing to adding catalyst for methanol, thus makes it have very strong water resistance, its can when in unstripped gas, moisture content is less than 6% dechlorination unaffected.
(5) in the preparation process of antichlor of the present invention, by selecting the baking temperature be suitable for, ensure that antichlor smooth in appearance, avoiding cracking, thus ensure that good intensity, antichlor also can be made to form suitable pore canal system simultaneously.
(6) antichlor of the present invention is mainly used in removing of the impurity such as hydrogen chloride in petroleum and petrochemical sector, also can be applicable to smart dechlorination in the production technologies such as synthetic ammonia, methyl alcohol, connection alcohol, methanation, also the essence that can be applicable to the chlorine in the multiple gases such as gaseous hydrocarbon, hydrogen, hydrogen and nitrogen gas, semiwater gas, oven gas, decarbonization gas takes off, and is of wide application.
Detailed description of the invention
Embodiment 1
Take the ferrous sulfate of 25g, the calcium oxide of 40g, 15g activated attapulgite mixes, and carries out kneading 45min afterwards; By above-mentioned evenly after siccative add Ludox 35g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 180 DEG C, can antichlor be obtained.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity utilizing ZQJ-II Intelligent testing machine for particle (large connection intelligent testing machine factory manufactures) to record this antichlor is 79N/cm, and bulk density is 0.66g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 50%.
Embodiment 2
Take the ferrous sulfate of 25g, the calcium oxide of 40g, the catalyst of 15g activated attapulgite and 20g gives up agent mixing, carries out kneading 45min afterwards; By above-mentioned evenly after siccative add Ludox 35g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 180 DEG C, can antichlor be obtained.Wherein, described catalyst gives up the particle diameter of agent for being not more than 10 nanometers, is that the catalyst produced in the process of methanol provided by Yunnan petrochemical industry Co., Ltd of PetroChina Company Limited. gives up agent.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 89N/cm, and bulk density is 0.69g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 60%.
Embodiment 3
Take the ferrous sulfate of 30g, the calcium oxide of 40g, 25g activated attapulgite mixes, and carries out kneading 40min afterwards; By above-mentioned evenly after siccative add Ludox 40g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 180 DEG C, can antichlor be obtained.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 73N/cm, and bulk density is 0.68g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 55%.
Embodiment 4
Take the ferrous sulfate of 30g, the calcium oxide of 40g, the catalyst of 25g activated attapulgite and 20g gives up agent mixing, carries out kneading 40min afterwards; By above-mentioned evenly after siccative add Ludox 40g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 180 DEG C, can antichlor be obtained.Wherein, described catalyst gives up the particle diameter of agent for being not more than 10 nanometers, is that the catalyst produced in the process of methanol provided by east, Tengzhou City Oil Co., Ltd gives up agent.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 87N/cm, and bulk density is 0.70g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 62%.
Embodiment 5
Take the ferrous sulfate of 20g, the calcium oxide of 20g, 10g activated attapulgite mixes, and carries out kneading 50min afterwards; By above-mentioned evenly after siccative add CMC 30g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 200 DEG C, can antichlor be obtained.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 74N/cm, and bulk density is 0.71g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 48%.
Embodiment 6
Take the ferrous sulfate of 20g, the calcium oxide of 20g, the catalyst of 10g activated attapulgite and 25g gives up agent mixing, carries out kneading 50min afterwards; By above-mentioned evenly after siccative add CMC 30g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 200 DEG C, can antichlor be obtained., wherein, described catalyst gives up the particle diameter of agent for being not more than 10 nanometers, is that the catalyst produced in the process of methanol provided by Yunnan petrochemical industry Co., Ltd of PetroChina Company Limited. gives up agent.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 88N/cm, and bulk density is 0.72g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 54%.
Embodiment 7
Take the ferrous sulfate of 28g, the calcium oxide of 30g, 20g activated attapulgite mixes, and carries out kneading 60min afterwards; By above-mentioned evenly after siccative add Ludox 35g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 150 DEG C, can antichlor be obtained.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 74N/cm, and bulk density is 0.71g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 52%.
Embodiment 8
Take the ferrous sulfate of 28g, the calcium oxide of 30g, the catalyst of 20g activated attapulgite and 15g gives up agent mixing, carries out kneading 60min afterwards; By above-mentioned evenly after siccative add Ludox 35g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 150 DEG C, can antichlor be obtained.Wherein, catalyst described in the present embodiment gives up the particle diameter of agent for being not more than 10 nanometers, is that the catalyst produced in the process of methanol provided by Yunnan petrochemical industry Co., Ltd of PetroChina Company Limited. and east, Tengzhou City Oil Co., Ltd gives up the mixture that agent is mixed to form by the mass ratio of 1:3.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 88N/cm, and bulk density is 0.82g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 58%.
Embodiment 9
Take the ferrous sulfate of 22g, the calcium oxide of 35g, 25g activated attapulgite mixes, and carries out kneading 55min afterwards; By above-mentioned evenly after siccative add CMC 35g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 160 DEG C, can antichlor be obtained.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 76N/cm, and bulk density is 0.72g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 53%.
Embodiment 10
Take the ferrous sulfate of 22g, the calcium oxide of 35g, the catalyst of 25g activated attapulgite and 18g gives up agent mixing, carries out kneading 55min afterwards; By above-mentioned evenly after siccative add CMC 35g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 160 DEG C, can obtain antichlor wherein, described catalyst gives up the particle diameter of agent for being not more than 10 nanometers, is that the catalyst produced in the process of methanol provided by east, Tengzhou City Oil Co., Ltd gives up agent.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 89N/cm, and bulk density is 0.83g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 57%.
Embodiment 11
Take the ferrous sulfate of 30g, the calcium oxide of 25g, 18g activated attapulgite mixes, and carries out kneading 40min afterwards; By above-mentioned evenly after siccative add CMC 30g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 170 DEG C, can antichlor be obtained.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 77N/cm, and bulk density is 0.73g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 50%.
Embodiment 12
Take the ferrous sulfate of 30g, the calcium oxide of 25g, the catalyst of 18g activated attapulgite and 22g gives up agent mixing, carries out kneading 40min afterwards; By above-mentioned evenly after siccative add CMC 30g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 170 DEG C, can antichlor be obtained.Wherein, described catalyst gives up the particle diameter of agent for being not more than 10 nanometers, is that the catalyst produced in the process of methanol provided by east, Tengzhou City Oil Co., Ltd gives up agent.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 89N/cm, and bulk density is 0.83g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 56%.
Comparative example 1
Take the di-iron trioxide of 25g, the calcium oxide of 40g, 15g activated attapulgite mixes, and carries out kneading 45min afterwards; By above-mentioned evenly after siccative add Ludox 35g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 180 DEG C, can antichlor be obtained.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 57N/cm, and bulk density is 0.53g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 10%.
Comparative example 2
Take the di-iron trioxide of 25g, the calcium oxide of 40g, the catalyst of 15g activated attapulgite and 20g gives up agent mixing, carries out kneading 45min afterwards; By above-mentioned evenly after siccative add Ludox 35g, by above-mentioned substance wet mixing 30 minutes, until mixed grind.Become paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 180 DEG C, can obtain antichlor, wherein, described catalyst gives up the particle diameter of agent for being not more than 10 nanometers, is that the catalyst produced in the process of methanol provided by Yunnan petrochemical industry Co., Ltd of PetroChina Company Limited. gives up agent.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 60N/cm, and bulk density is 0.56g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 18%.
Comparative example 3
Take the di-iron trioxide of 13.2g, the calcium oxide of 40g, 15g activated attapulgite mixes, and carries out kneading 45min afterwards; By above-mentioned evenly after siccative add Ludox 35g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 180 DEG C, can antichlor be obtained.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 55N/cm, and bulk density is 0.51g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 6%.
Comparative example 4
Take the di-iron trioxide of 13.2g, the calcium oxide of 40g, the catalyst of 15g activated attapulgite and 20g gives up agent mixing, carries out kneading 45min afterwards; By above-mentioned evenly after siccative add Ludox 35g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 180 DEG C, can antichlor be obtained.Wherein, described catalyst gives up the particle diameter of agent for being not more than 10 nanometers, is that the catalyst produced in the process of methanol provided by Yunnan petrochemical industry Co., Ltd of PetroChina Company Limited. gives up agent.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 58N/cm, and bulk density is 0.54g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 11%.
Comparative example 5
Take the di-iron trioxide of 13.2g, the calcium oxide of 40g, 15g activated attapulgite mixes, and carries out kneading 45min afterwards; By above-mentioned evenly after siccative add Ludox 35g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 180 DEG C, then in 350 DEG C of roastings 0.5 hour, can antichlor be obtained.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 58N/cm, and bulk density is 0.56g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 8%.
Comparative example 6
Take the di-iron trioxide of 13.2g, the calcium oxide of 40g, the catalyst of 15g activated attapulgite and 20g gives up agent mixing, carries out kneading 45min afterwards; By above-mentioned evenly after siccative add Ludox 35g, by above-mentioned substance wet mixing 30 minutes, until mixed grind becomes paste, above-mentioned paste is placed on small-sized banded extruder, extrudes Ф 4 stripe shape thing; Above-mentioned bar is carried out drying 2 hours at 180 DEG C, then in 350 DEG C of roastings 0.5 hour, can antichlor be obtained.Wherein, described catalyst gives up the particle diameter of agent for being not more than 10 nanometers, is that the catalyst produced in the process of methanol provided by Yunnan petrochemical industry Co., Ltd of PetroChina Company Limited. gives up agent.
Carry out physical property test to above-mentioned antichlor, the pressure measurement intensity of this antichlor is 60N/cm, and bulk density is 0.56g/ml; The above-mentioned antichlor prepared is shattered to 20-40 order, and at air speed 3000h
-1, its HCl content is evaluated under room temperature 23 DEG C of conditions, test result shows that the disposable chlorosity that penetrates of the antichlor prepared in this embodiment is 14%.
Can be found out by the contrast of embodiment 1-12, be added with catalyst give up agent antichlor and the same terms same materials do not add catalyst give up agent antichlor compared with, its side pressure strength and the disposable chlorosity that penetrates all are improved, in the quality of di-iron trioxide used in comparative example 1 and embodiment 1, ferrous sulfate raw material is identical in quality, the di-iron trioxide mole used in comparative example 3 is identical with the mole of di-iron trioxide in the antichlor that embodiment 1 prepares, but its chlorosity of antichlor of the comparative example 1 prepared under the same conditions and comparative example 3 is all well below the antichlor chlorosity in embodiment 1, show to adopt merely di-iron trioxide to mix with calcium oxide, the normal temperature antichlor of high chlorosity can not be obtained, namely di-iron trioxide and calcium oxide two kinds of crystalline structure simple superposition are made merely, the chlorosity of antichlor can not be improved, its reason is the calcium carbonate owing to usually all containing trace in commercially available calcium oxide, the crystal formation of calcium oxide is affected, and the contrast of comparative example 1 and comparative example 3 two kinds of antichlors shows, the simple amount improving di-iron trioxide can not significantly improve the chlorosity of normal temperature antichlor, antichlor in comparative example 5 is identical with the raw material of antichlor in comparative example 3, but the antichlor of comparative example 5 adds the process of high-temperature roasting in preparation process, but the chlorosity difference of two kinds of antichlors for preparing of distinct methods not obvious, show that the crystal formation of high-temperature calcination process on di-iron trioxide and calcium oxide does not produce significantly impact.
The applicant thinks in normal temperature antichlor of the present invention, required calcium oxide is all buied from domestic Chemical market, all containing impurity calcium carbonate in commercially available calcium oxide, because ferrous sulfate has faintly acid, can react with the impurity calcium carbonate in calcium oxide, make the crystal formation of calcium oxide more regular, meanwhile, ferrous ion is constantly oxidized to the oxide of iron, the crystal formation of calcium oxide and iron oxide is adulterated mutually, obtains regular CaO-Fe
2o
3crystal structure, thus improve the dechlorination effect of antichlor, the unexpected effect that ferrous sulfate plays in the process preparing normal temperature antichlor as raw material, create unexpected technique effect, the preparation method of normal temperature antichlor of the present invention, does not need the process of roasting simultaneously, reduce energy ezpenditure, decrease the equipment used in preparation process, simplified preparation process, reduced preparation cost.
Obviously, above-described embodiment is only for clearly example being described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of extending out or variation be still within the protection domain of the invention.
Claims (8)
1. a normal temperature antichlor, it is characterized in that, described normal temperature antichlor is made primarily of ferrous sulfate, calcium oxide and Concave-convex clay rod, wherein ferrous sulfate is 20-30 weight portion, calcium oxide is 20-40 weight portion, Concave-convex clay rod 10-25 weight portion, containing calcium carbonate impurity in described calcium oxide;
Described normal temperature antichlor is prepared from by following steps:
(1) a certain amount of ferrous sulfate, calcium oxide and Concave-convex clay rod are mixed, and abundant kneading;
(2) in the material after described step (1) mixing, add binding agent, above-mentioned substance mixed grind is become paste, by described paste extruded moulding;
(3) the stripe shape thing of described step (2) is carried out drying at 150-200 DEG C, can antichlor be obtained.
2. normal temperature antichlor according to claim 1, is characterized in that,
Described normal temperature antichlor is made primarily of the agent of giving up of ferrous sulfate, calcium oxide, Concave-convex clay rod and catalyst;
The catalyst also adding 15-25 weight portion in described step (1) gives up agent, and the give up active component of agent of described catalyst is cupric oxide and zinc oxide.
3. normal temperature antichlor according to claim 2, is characterized in that, the described catalyst content of cupric oxide in agent that gives up is 15-20wt%; The content of zinc oxide is 10-20wt%.
4. normal temperature antichlor according to claim 3, is characterized in that, the agent of giving up of described catalyst is that catalyst for methanol gives up agent.
5. normal temperature antichlor according to claim 4, is characterized in that, the give up particle diameter of agent of described catalyst is not more than 10nm.
6., according to the arbitrary described normal temperature antichlor of claim 1-5, it is characterized in that, described binding agent is Ludox or CMC.
7. the preparation method of normal temperature antichlor according to claim 6, is characterized in that, the time of described kneading is 40-60 minute.
8. the preparation method of normal temperature antichlor according to claim 7, is characterized in that, the drying time of described bar is 2 hours.
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| CN109248708A (en) * | 2017-07-15 | 2019-01-22 | 吴月兵 | A kind of room temperature antichlor and preparation method thereof |
| CN109382388B (en) * | 2017-08-07 | 2022-05-13 | 中国石化扬子石油化工有限公司 | Method for preparing fresh dechlorinating agent from waste dechlorinating agent |
| CN109453735B (en) * | 2017-09-06 | 2021-04-06 | 中国石化扬子石油化工有限公司 | Cellular liquid-phase dechlorinating agent, and preparation method and application thereof |
| CN110523368B (en) * | 2019-08-27 | 2022-04-19 | 万华化学（宁波）有限公司 | Preparation method of chlorine absorbent, chlorine absorbent and application thereof |
| CN110882683B (en) * | 2019-11-26 | 2020-07-07 | 青岛庄信恒瑞催化剂有限公司 | Dechlorination deoxidation catalyst and preparation method and application thereof |
| CN110803803A (en) * | 2019-11-27 | 2020-02-18 | 阳新鹏富矿业有限公司 | Treatment agent and treatment method for wet desulphurization wastewater |
| CN112940794A (en) * | 2021-02-23 | 2021-06-11 | 湖北华特尔净化科技股份有限公司 | Anti-toxin protective agent for blast furnace gas and preparation method thereof |
| CN115634563B (en) * | 2021-07-19 | 2025-12-02 | 中国石油化工股份有限公司 | A chlorine-fixing agent, its preparation method and application |
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