CN110467952A - A kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent - Google Patents
A kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent Download PDFInfo
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- CN110467952A CN110467952A CN201910726639.0A CN201910726639A CN110467952A CN 110467952 A CN110467952 A CN 110467952A CN 201910726639 A CN201910726639 A CN 201910726639A CN 110467952 A CN110467952 A CN 110467952A
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- liquefied petroleum
- petroleum gas
- desulfurizing agent
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 47
- 230000003009 desulfurizing effect Effects 0.000 title claims abstract description 44
- 239000003915 liquefied petroleum gas Substances 0.000 title claims abstract description 40
- 230000003647 oxidation Effects 0.000 title claims abstract description 38
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000012798 spherical particle Substances 0.000 claims abstract description 24
- 239000011148 porous material Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 15
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 15
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002808 molecular sieve Substances 0.000 claims abstract description 15
- 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 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- LEVWYRKDKASIDU-QWWZWVQMSA-N D-cystine Chemical compound OC(=O)[C@H](N)CSSC[C@@H](N)C(O)=O LEVWYRKDKASIDU-QWWZWVQMSA-N 0.000 claims abstract description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 229960003067 cystine Drugs 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 239000002562 thickening agent Substances 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 18
- 239000002518 antifoaming agent Substances 0.000 claims description 17
- 235000019738 Limestone Nutrition 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- 210000002966 serum Anatomy 0.000 claims description 13
- HUAUNKAZQWMVFY-UHFFFAOYSA-M sodium;oxocalcium;hydroxide Chemical compound [OH-].[Na+].[Ca]=O HUAUNKAZQWMVFY-UHFFFAOYSA-M 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- -1 polyoxyethylene Polymers 0.000 claims description 9
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 239000001099 ammonium carbonate Substances 0.000 claims description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
- 239000006028 limestone Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 6
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 6
- 239000008394 flocculating agent Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000000320 mechanical mixture Substances 0.000 claims description 6
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 6
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 239000000230 xanthan gum Substances 0.000 claims description 6
- 229920001285 xanthan gum Polymers 0.000 claims description 6
- 229940082509 xanthan gum Drugs 0.000 claims description 6
- 235000010493 xanthan gum Nutrition 0.000 claims description 6
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- MDFFNEOEWAXZRQ-UHFFFAOYSA-N aminyl Chemical compound [NH2] MDFFNEOEWAXZRQ-UHFFFAOYSA-N 0.000 claims description 4
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 4
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 4
- 239000000839 emulsion Substances 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 238000001802 infusion Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 abstract description 8
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 abstract description 8
- 229910000037 hydrogen sulfide Inorganic materials 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 8
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 238000006722 reduction reaction Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000005979 thermal decomposition reaction Methods 0.000 abstract description 3
- 238000002485 combustion reaction Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000006477 desulfuration reaction Methods 0.000 description 8
- 230000023556 desulfurization Effects 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical group CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 239000001273 butane Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BKOOMYPCSUNDGP-UHFFFAOYSA-N 2-methylbut-2-ene Chemical group CC=C(C)C BKOOMYPCSUNDGP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/12—Liquefied petroleum gas
Abstract
The present invention relates to technical field of desulfurizer preparation, and in particular to a kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent；Molecular sieve, activated alumina, kaolin and active carbon in the present invention are porous material, effectively can carry out physical absorption to the sulfur dioxide generated after liquefied petroleum gas combustion；Pore creating material in the present invention is under conditions of 100~150 DEG C by thermal decomposition to generate bubble, bubble is at this time from the surface of spherical particle and internal evolution, so that spherome surface and a large amount of rough micropores of internal formation, increase the contact area of the hydrogen sulfide and mercaptan in oxidation desulfurizing agent and liquefied petroleum gas；When hydrogen sulfide and mercaptan flow to the micropore in oxidation desulfurizing agent, it occurs oxygen reduction reaction with the cystine having on the inner wall of oxidation desulfurizing agent outer wall and micropore and is removed, to achieve the purpose that oxidation sweetening, i.e. hydrogen sulfide and mercaptan in chemical method removing liquefied petroleum gas.
Description
Technical field
The present invention relates to technical field of desulfurizer preparation, and in particular to a kind of preparation side of liquefied petroleum gas oxidation desulfurizing agent
Method.
Background technique
Liquefied petroleum gas is mainly composed by hydrocarbon, and main component is propane, butane and other alkane
Hydrocarbon etc..It is easy for operation due to its calorific value height, smoke dust, without breeze when liquefied petroleum gas makees fuel, widely enter
People's lives field.In addition, liquefied petroleum gas is also used to cut metal, for the baking of agricultural product and the roasting of Industrial Stoves
Deng.
Liquefied petroleum gas is to carry out a kind of obtained nothing of pressurization cooling liquefaction by natural gas or petroleum in oil plant
Color volatile liquid.Its easily spontaneous combustion encounters open fire energy after its aerial content has reached certain concentration range
Explosion.Via the obtained liquefied petroleum gas main constituents of oil plant be one of propane, propylene, butane, butylene or
Two kinds of person, and it also adulterates a small amount of pentane, amylene and micro sulfide impurities.
If the sulfide of liquefied petroleum CNOOC is not sloughed, the sulfide contained can generate sulfur-containing oxide in burning
Atmosphere is polluted.But the bad desulfurization effects of existing desulfurizing agent, the sulfide in liquefied petroleum gas cannot be carried out
Removing well, i.e., desulfuration efficiency is lower.
Summary of the invention
In view of the above problems, the present invention provides a kind of preparation methods of liquefied petroleum gas oxidation desulfurizing agent, use
In solve background technique proposed in the technical issues of.
To achieve the above object, the following technical solution is employed by the present invention:
A kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent, includes the following steps:
S1, by weight 15~22 parts of molecular sieves of component precise, 10~16 parts of activated aluminas, 8~13 parts of kaolin,
10~15 parts of active carbons, 30~40 parts of lime stones, 20~26 parts of soda lime, 2.0~2.5 parts of complex thickeners, 1.3~1.8 parts
Pore creating material, 1.5~2.0 parts of defoaming agents, 2.6~3.2 parts of flocculants, suitable quantity of water and appropriate mixed liquor；
S2, respectively by the molecular sieve weighed in S1, activated alumina, kaolin, active carbon, lime stone and soda lime distinguish
It is placed in grinder and is ground, obtain each component fine powder, save respectively, it is spare；
S3, each component fine powder obtained in S2 is all placed in container, mixed component is denoted as obtained in container；Then
The mixed liquor of the water of addition 16~20wt.% of mixed component and 12~16wt.% into reaction kettle, mechanical mixture stirring 20~
After 30min, container is placed in progress 30~40min of ultrasonic disperse in ultrasonic device, obtains mixed serum；
S4, resulting mixed serum is transferred in reaction kettle, then complex thickener, defoaming agent and flocculant is added and mixed
In slurries, 75~85 DEG C are warming up to, while after 10~20min of ultrasonic agitation, standing naturally, obtaining mixture of viscous form；
S5, pore creating material is added into mixture of viscous form obtained in S4, uses mechanical equipment will after being mixed evenly
Be processed into diameter be 2~3mm spherical particle, then spherical particle is placed in drying box and is dried, drying temperature is
100~150 DEG C, until moisture content≤15% of spherical particle is to get liquefied petroleum gas oxidation desulfurizing agent finished product.
Further, the pore creating material selects one of ammonium hydrogen carbonate, ammonium carbonate.Pore creating material is at 100~150 DEG C
Under the conditions of by thermal decomposition to generate bubble, bubble is at this time from the surface of spherical particle and internal evolution, so that sphere table
Face and it is internal form a large amount of rough micropores, increase oxidation desulfurizing agent in liquefied petroleum gas hydrogen sulfide and mercaptan connect
Contacting surface product.
Further, the defoaming agent selects silicone emulsion, the one of which in polyoxyethylene polyoxy propyl alcohol amidogen ether.Disappear
The using of infusion can to mix between each raw material more uniform, guarantee the liquefied petroleum gas oxidation desulfurizing agent quality produced
Homogeneity.
Further, the flocculant selects aluminium polychloride, the one of which in poly-ferric chloride.Flocculant makes
With the cementability that can enhance between each component, standard is carried out for the preparation of subsequent spherical particle with being used cooperatively for thickener is met
It is standby, it is ensured that the quality of spherical particle.
Further, the complex thickener is formed by the mass mixings such as sodium carboxymethylcellulose pyce and xanthan gum.Thickener
Use being gone on smoothly convenient for subsequent production spherical particle.
The mixed liquor the preparation method comprises the following steps: by cystine be dissolved in quality be its 4~6 sodium hydroxide solution in, warp
Mixed liquor finished product is remembered after being mixed evenly, wherein the concentration of sodium hydroxide solution is 0.5~0.8mol/L.Oxidation desulfurizing agent
Surface and it is internal generate a large amount of rough micropore, when in liquefied petroleum gas hydrogen sulfide and mercaptan enter in micropore,
It occurs oxygen reduction reaction with the cystine having on the inner wall of oxidation desulfurizing agent outer wall and micropore and is removed, to reach
The purpose of oxidation sweetening.
Further, the partial size of each component fine powder after grinding in the S2 is 200~300 mesh.
Further, the frequency being stirred by ultrasonic in the S4 is 20~28KHz, and ultrasonic power is 100~200W.It is super
Sound stirring is had reason abundant between each component and is equably mixed, to improve the quality of mixture of viscous form.
Using above-mentioned technical solution, the beneficial effect that the present invention reaches is:
The present invention is aoxidized using molecular sieve, activated alumina, kaolin, active carbon, lime stone and soda lime etc. as preparation
The raw material of desulfurizing agent.Wherein, molecular sieve, activated alumina, kaolin and active carbon are porous material, can be effectively to liquefaction
The sulfur dioxide generated after oil gas burning carries out physical absorption.In addition, item of the pore creating material at 100~150 DEG C in the present invention
By thermal decomposition to generate bubble under part, bubble is at this time from the surface of spherical particle and internal evolution, so that spherome surface
A large amount of rough micropores are formed with inside, increase the contact of oxidation desulfurizing agent and hydrogen sulfide and mercaptan in liquefied petroleum gas
Area (specific surface area of oxidation desulfurizing agent i.e. prepared by the present invention is larger).When hydrogen sulfide and mercaptan are flow in oxidation desulfurizing agent
When micropore, oxygen reduction reaction occurs with the cystine having on the inner wall of oxidation desulfurizing agent outer wall and micropore and is removed, from
And having achieved the purpose that oxidation sweetening, i.e., chemical method removes the hydrogen sulfide and mercaptan in liquefied petroleum gas.The present invention passes through object
The chemical method of reason absorption method and redox reaction improve desulfuration efficiency significantly with the use of energy.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described.Based on the embodiment of the present invention, the common skill in this field
Art personnel every other embodiment obtained without creative efforts belongs to the model that the present invention protects
It encloses.
Embodiment 1:
A kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent, includes the following steps:
S1, by weight 18 parts of molecular sieves of component precise, 10 parts of activated aluminas, 9 parts of kaolin, 10 parts of active carbons,
35 parts of lime stones, 2.2 parts of complex thickeners, 1.3 parts of pore creating materials, 1.7 parts of defoaming agents, 2.6 parts of flocculants, are fitted at 20 parts of soda lime
Measure water and appropriate mixed liquor；
S2, respectively by the molecular sieve weighed in S1, activated alumina, kaolin, active carbon, lime stone and soda lime distinguish
It is placed in grinder and is ground, obtain each component fine powder, save respectively, it is spare；
S3, each component fine powder obtained in S2 is all placed in container, mixed component is denoted as obtained in container；Then
The water of mixed component 16wt.% and the mixed liquor of 12wt.% are added into reaction kettle, after mechanical mixture stirs 20min, by container
It is placed in progress ultrasonic disperse 30min in ultrasonic device, obtains mixed serum；
S4, resulting mixed serum is transferred in reaction kettle, then complex thickener, defoaming agent and flocculant is added and mixed
In slurries, 75 DEG C are warming up to, while after 10min is stirred by ultrasonic, stand naturally, obtain mixture of viscous form；
S5, pore creating material is added into mixture of viscous form obtained in S4, uses mechanical equipment will after being mixed evenly
Be processed into diameter be 2mm spherical particle, then spherical particle is placed in drying box and is dried, drying temperature 100
DEG C, until the moisture content of spherical particle is 10% to get liquefied petroleum gas oxidation desulfurizing agent finished product.
The pore creating material selects ammonium hydrogen carbonate.
The defoaming agent selects silicone emulsion.
The flocculant selects aluminium polychloride.
The complex thickener is formed by the mass mixings such as sodium carboxymethylcellulose pyce and xanthan gum.
The mixed liquor the preparation method comprises the following steps: it is in its 4 times sodium hydroxide solution, through mixed that cystine, which is dissolved in quality,
Mixed liquor finished product is remembered in conjunction after mixing evenly, and wherein the concentration of sodium hydroxide solution is 0.5mol/L.
The partial size of each component fine powder after grinding in the S2 is 200 mesh.
The frequency being stirred by ultrasonic in the S4 is 20KHz, ultrasonic power 100W.
Embodiment 2:
A kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent, includes the following steps:
S1, by weight 15 parts of molecular sieves of component precise, 12 parts of activated aluminas, 8 parts of kaolin, 11 parts of active carbons,
30 parts of lime stones, 2.0 parts of complex thickeners, 1.5 parts of pore creating materials, 1.5 parts of defoaming agents, 2.8 parts of flocculants, are fitted at 22 parts of soda lime
Measure water and appropriate mixed liquor；
S2, respectively by the molecular sieve weighed in S1, activated alumina, kaolin, active carbon, lime stone and soda lime distinguish
It is placed in grinder and is ground, obtain each component fine powder, save respectively, it is spare；
S3, each component fine powder obtained in S2 is all placed in container, mixed component is denoted as obtained in container；Then
The water of mixed component 18wt.% and the mixed liquor of 14wt.% are added into reaction kettle, after mechanical mixture stirs 25min, by container
It is placed in progress ultrasonic disperse 35min in ultrasonic device, obtains mixed serum；
S4, resulting mixed serum is transferred in reaction kettle, then complex thickener, defoaming agent and flocculant is added and mixed
In slurries, 80 DEG C are warming up to, while after 15min is stirred by ultrasonic, stand naturally, obtain mixture of viscous form；
S5, pore creating material is added into mixture of viscous form obtained in S4, uses mechanical equipment will after being mixed evenly
Be processed into diameter be 2mm spherical particle, then spherical particle is placed in drying box and is dried, drying temperature 120
DEG C, until the moisture content of spherical particle is 12% to get liquefied petroleum gas oxidation desulfurizing agent finished product.
The pore creating material selects ammonium carbonate.
The defoaming agent selects polyoxyethylene polyoxy propyl alcohol amidogen ether.
The flocculant selects poly-ferric chloride.
The complex thickener is formed by the mass mixings such as sodium carboxymethylcellulose pyce and xanthan gum.
The mixed liquor the preparation method comprises the following steps: it is in its 5 times sodium hydroxide solution, through mixed that cystine, which is dissolved in quality,
Mixed liquor finished product is remembered in conjunction after mixing evenly, and wherein the concentration of sodium hydroxide solution is 0.6mol/L.
The partial size of each component fine powder after grinding in the S2 is 250 mesh.
The frequency being stirred by ultrasonic in the S4 is 25KHz, ultrasonic power 100W.
Embodiment 3:
A kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent, includes the following steps:
S1, by weight 22 parts of molecular sieves of component precise, 14 parts of activated aluminas, 13 parts of kaolin, 13 parts of active carbons,
40 parts of lime stones, 2.5 parts of complex thickeners, 1.6 parts of pore creating materials, 2.0 parts of defoaming agents, 3.0 parts of flocculants, are fitted at 24 parts of soda lime
Measure water and appropriate mixed liquor；
S2, respectively by the molecular sieve weighed in S1, activated alumina, kaolin, active carbon, lime stone and soda lime distinguish
It is placed in grinder and is ground, obtain each component fine powder, save respectively, it is spare；
S3, each component fine powder obtained in S2 is all placed in container, mixed component is denoted as obtained in container；Then
The water of mixed component 18wt.% and the mixed liquor of 15wt.% are added into reaction kettle, after mechanical mixture stirs 25min, by container
It is placed in progress ultrasonic disperse 40min in ultrasonic device, obtains mixed serum；
S4, resulting mixed serum is transferred in reaction kettle, then complex thickener, defoaming agent and flocculant is added and mixed
In slurries, 80 DEG C are warming up to, while after 15min is stirred by ultrasonic, stand naturally, obtain mixture of viscous form；
S5, pore creating material is added into mixture of viscous form obtained in S4, uses mechanical equipment will after being mixed evenly
Be processed into diameter be 3mm spherical particle, then spherical particle is placed in drying box and is dried, drying temperature 140
DEG C, until the moisture content of spherical particle is 14% to get liquefied petroleum gas oxidation desulfurizing agent finished product.
The pore creating material selects ammonium hydrogen carbonate.
The defoaming agent selects silicone emulsion.
The flocculant selects aluminium polychloride.
The complex thickener is formed by the mass mixings such as sodium carboxymethylcellulose pyce and xanthan gum.
The mixed liquor the preparation method comprises the following steps: it is in its 5 times sodium hydroxide solution, through mixed that cystine, which is dissolved in quality,
Mixed liquor finished product is remembered in conjunction after mixing evenly, and wherein the concentration of sodium hydroxide solution is 0.7mol/L.
The partial size of each component fine powder after grinding in the S2 is 300 mesh.
The frequency being stirred by ultrasonic in the S4 is 28KHz, ultrasonic power 200W.
Embodiment 4:
A kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent, includes the following steps:
S1, by weight 20 parts of molecular sieves of component precise, 16 parts of activated aluminas, 11 parts of kaolin, 15 parts of active carbons,
38 parts of lime stones, 2.3 parts of complex thickeners, 1.8 parts of pore creating materials, 1.9 parts of defoaming agents, 3.2 parts of flocculants, are fitted at 26 parts of soda lime
Measure water and appropriate mixed liquor；
S2, respectively by the molecular sieve weighed in S1, activated alumina, kaolin, active carbon, lime stone and soda lime distinguish
It is placed in grinder and is ground, obtain each component fine powder, save respectively, it is spare；
S3, each component fine powder obtained in S2 is all placed in container, mixed component is denoted as obtained in container；Then
The water of mixed component 20wt.% and the mixed liquor of 16wt.% are added into reaction kettle, after mechanical mixture stirs 30min, by container
It is placed in progress ultrasonic disperse 40min in ultrasonic device, obtains mixed serum；
S4, resulting mixed serum is transferred in reaction kettle, then complex thickener, defoaming agent and flocculant is added and mixed
In slurries, 85 DEG C are warming up to, while after 20min is stirred by ultrasonic, stand naturally, obtain mixture of viscous form；
S5, pore creating material is added into mixture of viscous form obtained in S4, uses mechanical equipment will after being mixed evenly
Be processed into diameter be 3mm spherical particle, then spherical particle is placed in drying box and is dried, drying temperature 150
DEG C, until the moisture content of spherical particle is 15% to get liquefied petroleum gas oxidation desulfurizing agent finished product.
The pore creating material selects ammonium carbonate.
The defoaming agent selects polyoxyethylene polyoxy propyl alcohol amidogen ether.
The flocculant selects poly-ferric chloride.
The complex thickener is formed by the mass mixings such as sodium carboxymethylcellulose pyce and xanthan gum.
The mixed liquor the preparation method comprises the following steps: it is in its 6 times sodium hydroxide solution, through mixed that cystine, which is dissolved in quality,
Mixed liquor finished product is remembered in conjunction after mixing evenly, and wherein the concentration of sodium hydroxide solution is 0.8mol/L.
The partial size of each component fine powder after grinding in the S2 is 300 mesh.
The frequency being stirred by ultrasonic in the S4 is 28KHz, ultrasonic power 200W.
Testing result:
Desulfurization test is carried out to desulfurizing agent prepared by the present invention, as a result see the table below:
Note: 1, in 500 milliliters of stainless steel closed containers, desulfurizing agent prepared by the present invention, In sulfur method: are previously added
Sulfur content 1120mg/m is injected under pressurized state3100 milliliters of liquefied petroleum gas (with percent by volume), after container closure is good, In
Oscillating reactions 4 hours at 20 DEG C, the liquefied petroleum gas after refining desulfurization is released in decompression, and measures sulfur content therein.
2, comparative example is progress desulfurization using presently commercially available DSM desulfurizing agent as desulfurizing agent.
The desulfurization effect that can be seen that the desulfurizing agent prepared through the invention from the data in table is substantially better than commercially available
DSM desulfurizing agent shows that the desulfuration efficiency of desulfurizing agent prepared by the present invention is higher, more conducively promotes.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (8)
1. a kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent, which comprises the steps of:
S1, by weight 15~22 parts of molecular sieves of component precise, 10~16 parts of activated aluminas, 8~13 parts of kaolin, 10~
15 parts of active carbons, 30~40 parts of lime stones, 20~26 parts of soda lime, 2.0~2.5 parts of complex thickeners, 1.3~1.8 parts of pore-creating
Agent, 1.5~2.0 parts of defoaming agents, 2.6~3.2 parts of flocculants, suitable quantity of water and appropriate mixed liquor；
S2, the molecular sieve weighed in S1, activated alumina, kaolin, active carbon, lime stone and soda lime is respectively placed in respectively
It is ground in grinder, obtains each component fine powder, save respectively, it is spare；
S3, each component fine powder obtained in S2 is all placed in container, mixed component is denoted as obtained in container；Then to anti-
The mixed liquor of water and 12~16wt.% that 16~20wt.% of mixed component is added in kettle is answered, mechanical mixture stirs 20~30min
Afterwards, container is placed in progress 30~40min of ultrasonic disperse in ultrasonic device, obtains mixed serum；
S4, resulting mixed serum is transferred in reaction kettle, then mixed serum is added in complex thickener, defoaming agent and flocculant
In, 75~85 DEG C are warming up to, while after 10~20min of ultrasonic agitation, standing naturally, obtaining mixture of viscous form；
S5, pore creating material is added into mixture of viscous form obtained in S4, is added it using mechanical equipment after being mixed evenly
Work at diameter be 2~3mm spherical particle, then spherical particle is placed in drying box and is dried, drying temperature be 100~
150 DEG C, until moisture content≤15% of spherical particle is to get liquefied petroleum gas oxidation desulfurizing agent finished product.
2. a kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent according to claim 1, it is characterised in that: described to make
One of ammonium hydrogen carbonate, ammonium carbonate are selected in hole agent.
3. a kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent according to claim 1, it is characterised in that: described to disappear
One of which in infusion selection silicone emulsion, polyoxyethylene polyoxy propyl alcohol amidogen ether.
4. a kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent according to claim 1, it is characterised in that: the wadding
One of which in solidifying agent selection aluminium polychloride, poly-ferric chloride.
5. a kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent according to claim 1, it is characterised in that: described multiple
Thickener is closed to be formed by the mass mixings such as sodium carboxymethylcellulose pyce and xanthan gum.
6. a kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent according to claim 1, which is characterized in that described mixed
Close liquid the preparation method comprises the following steps: by cystine be dissolved in quality be its 4~6 sodium hydroxide solution in, after being mixed evenly
Remember mixed liquor finished product, wherein the concentration of sodium hydroxide solution is 0.5~0.8mol/L.
7. a kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent according to claim 1, it is characterised in that: the S2
The partial size of each component fine powder after middle grinding is 200~300 mesh.
8. a kind of preparation method of liquefied petroleum gas oxidation desulfurizing agent according to claim 1, it is characterised in that: the S4
The frequency of middle ultrasonic agitation is 20~28KHz, and ultrasonic power is 100~200W.
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