CN105561981B - A kind of derived energy chemical spent lye processing high-efficiency desulfurization catalyst and preparation method thereof - Google Patents
A kind of derived energy chemical spent lye processing high-efficiency desulfurization catalyst and preparation method thereof Download PDFInfo
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- CN105561981B CN105561981B CN201510941070.1A CN201510941070A CN105561981B CN 105561981 B CN105561981 B CN 105561981B CN 201510941070 A CN201510941070 A CN 201510941070A CN 105561981 B CN105561981 B CN 105561981B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
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Abstract
The invention discloses a kind of derived energy chemical spent lye processing high-efficiency desulfurization catalyst, are made of active presoma, synergist, auxiliary agent, antifreezing agent, solvent etc..When preparing the desulphurization catalyst, active presoma, synergist, auxiliary agent and a small amount of solvent are added in synthesis reactor first and are stirred to react, it adds antifreezing agent and solvent makes dissolution completely and stirs evenly, finished product, when use can directly add in proportion according to spent lye treating capacity.The raw materials for production of high-efficiency desulfurization catalyst of the present invention are easy to get, and preparation process is simple, and product is uniform liquid, and good fluidity, catalytic activity is high, selectivity is good, and additive amount is few, and product is nontoxic, environmentally protective, have good economy.
Description
Technical field
The invention belongs to the preparation technical fields of chemical products, are related to a kind of derived energy chemical spent lye processing high-efficiency desulfurization
Catalyst and preparation method thereof.
Background technique
Derived energy chemical spent lye refers to the height generated in enterprises' productions such as petrochemical industry, New Coal Chemical and extraordinary chemical industry
Concentration pollutant alkaline waste liquor, typically contain in spent lye the sulfide of higher concentration, mercaptan, acylate, creosote, oil and
Other similar organic and inorganic compound has dark, stench and strong corrosive, belongs to hazardous waste.Spent lye is for example direct
Discharge can release intense irritation foul smell, cause seriously to pollute to atmosphere, waters and soil, therefore, such waste water is unsuitable
It is directly discharged into the wastewater reuse approach system of manufacturing enterprise, is typically necessary and is pre-processed before.
Sulfide removal method mainly has the precipitation method, vaporizing extract process, neutralisation, oxidation in well known spent lye both at home and abroad at present
Method, causticization regeneration sodium hydroxide, vulcanized sodium is produced in crystallization and spent lye is used for pulping and paper-making etc., wherein commonly oxidizing process,
It is to carry out catalytic oxidation treatment under certain temperature, pressure to spent lye using catalyst, finally convert sulphur for sulfide
Thiosulfate or sulfate.
A kind of method for oxidation as disclosed in US4855123 be using non-impregnated C catalyst 50~130 DEG C, 0~
The catalysis oxidation carried out under conditions of 980KPa, by oxidizing sodium sulphide at sodium polysulfide and sodium thiosulfate, but due to thio sulphur
Sour sodium is also unstable sulfur-containing compound, in acid condition, can be disproportionated generation elemental sulfur, therefore this method cannot be from basic
On sulfur-containing compound is converted to the form of stable sulfate.For another the patent of Publication No. US5207927, US5470486
The method addressed in text is under the conditions of 1000KPa or so, to be oxidation of the sulfide into sulfuric acid at 150 DEG C using metallic catalyst
Salt.Using high temperature, high-pressure oxidation method, although preferable oxidation processes effect can be obtained, the investment of the engineering equipment of device is big,
Operating cost is high, and system operatio, management are also extremely complex.
In addition to above-mentioned method for oxidation, this field, which also has, at present is used under room temperature, condition of normal pressure through traditional catalyst pair
The method that sulfide carries out airoxidation in spent lye, though these methods can improve oxidation reaction speed to a certain extent
Degree, but still sulfide or thiosulfate rapidly cannot be thoroughly oxidized to stable sulfate, and deposit in oxidation product
In a large amount of thiosulfate, oxidation reaction is not thorough；In addition, can also generate biggish stink in treatment process, atmosphere is polluted
Environment.Support type Cobalt Phthalocyanine catalytic oxidation desulfurization is used in technology as disclosed in CN101143746A patent text, uses tower
Formula reactor, though sulfide desulfuration efficiency can be made to be improved, product is only converted to thiosulfate, and unstable
State sulphur.It in the presence of for another example mentioning iron-containing catalyst in CN1579956A patent text, is stirred to react with compressed air, can make to vulcanize
Object is down to 45mg/L hereinafter, but being still to convert thiosulfate for most of sulphur, and be catalyzed in treatment process using this method
Agent dosage is big, is solidliquid mixture, and operation sequence is complicated.For another example method disclosed in CN10178068A patent text is to utilize three
The compound of valence bismuth makees catalyst, and sulfide or thiosulfate are completely oxidized to sulfate under room temperature, normal pressure, processes
The dosage of catalyst is larger in journey, and need to repeatedly adjust PH and introduce a large amount of water, also needs to increase filter device, and need to recycle and urge
Agent, process are partial to complexity.
Summary of the invention
It is an object of the invention to overcome defect of the existing technology, providing one kind can be under the conditions of synthesis under normal pressure by sulphur
Compound is completely oxidized to the derived energy chemical spent lye processing high-efficiency desulfurization catalyst of sulfate, while providing one kind and being exclusively used in this
The preparation method of high-efficiency desulfurization catalyst.
It is described that technical scheme is as follows.
A kind of derived energy chemical spent lye processing high-efficiency desulfurization catalyst, is made of the raw material of substance of following mass ratioes:
Wherein, the active presoma is the molysite being made of ferric sulfate, iron chloride or ferric nitrate and/or by sulfuric acid
The cobalt salt that cobalt, cobalt nitrate or cobalt chloride are constituted and/or the manganese being made of manganese sulfate, manganese acetate, manganese oxalate, manganese chloride or manganese nitrate
Salt；
The synergist is neopelex and/or lauryl sodium sulfate and/or polyacrylic acid and its salt
Class and/or ethyoxyl sodium alkyl sulfate and/or lauric acid amide of ethanol and/or ethyoxyl alkyl ammonium sulfate；
The auxiliary agent is sodium metasilicate and/or sodium sorbate and/or triethanolamine and/or polyphosphate sodium and/or Boratex
And/or ethylenediamine tetraacetic methene sodium phosphate and/or sodium citrate and/or sodium ethylene diamine tetracetate and/or diethylenetriamine pentacarboxylic acid
Sodium and/or heptose sodium sugar and/or sodium gluconate；
The antifreezing agent is methanol and/or ethyl alcohol and/or ethylene glycol and/or propylene glycol and/or glycerine；
The solvent is water.
The method for being used to prepare the high-efficiency desulfurization catalyst is: at normal temperature, first by active presoma, synergist, help
The solvent of agent and 7%~22% amount, which is added in synthesis reactor, is stirred to react 2~5h, after the completion, be added antifreezing agent and remaining 78%
The solvent of~93% amount completes dissolution, and continues 2~5h of stirring, finished product.Obtained finished product is colourless to faint yellow
Transparency liquid, 1.05 ± 0.1g/mL of density, < -5 DEG C of condensation point.
The technical solution that the present invention optimizes is: the active presoma is the molysite being made of ferric sulfate, ferric nitrate
And/or it the cobalt salt that is made of cobaltous sulfate, cobalt nitrate or cobalt chloride and/or is made of manganese sulfate, manganese acetate, manganese oxalate or manganese chloride
Manganese salt.
The technical solution that the present invention optimizes also resides in: the synergist is neopelex and/or dodecane
Base sodium sulphate.
The technical solution that the present invention optimizes also resides in: the auxiliary agent is Boratex and/or sodium gluconate and/or poly- phosphorus
Sour sodium and/or ethylenediamine tetraacetic methene sodium phosphate and/or sodium ethylene diamine tetracetate.
The technical solution that the present invention optimizes also resides in: the antifreezing agent is ethylene glycol and/or propylene glycol.
In above-mentioned high-efficiency desulfurization catalyst, active presoma is active raw material, and the effect of synergist is that enhancing system is molten
Oxygen effect, auxiliary agent are the raw materials of synthesizing activity object, promote oxygen atom activation, the effect of antifreezing agent is to reduce the freezing point of product, molten
The effect of agent is dilution component, makes final products liquid condition, is easy to add.
The mechanism of action of high-efficiency desulfurization catalyst of the present invention is: under normal pressure, low temperature, which can be effective
Ground promotes the dissolution of oxygen in air, activation, improves selectivity of product, to promote being rapidly completed for reaction, makes unstable sulphur
Compound is converted into the sulphur of stable state.
2Na2S+2O2+H2O→Na2S2O3+2NaOH
Na2S2O3+2O2+2NaOH→2Na2SO4+H2O
Compared with the prior art, the advantages of the present invention are as follows:
1, compared to previous desulphurization catalyst product, desulphurization catalyst of the present invention is uniform liquid, good fluidity, easily
In addition, and not blocking pipeline；
2, desulphurization catalyst of the present invention, which has, reduces surface tension, the activation for increasing dissolved oxygen, promoting oxygen atom, promotees
Carried out into rapid reaction, improve oxidation efficiency and other effects；
3, the selectivity of desulphurization catalyst of the present invention is good, additive amount is few, catalytic activity is high, S2-Conversion is thorough, product
It is nontoxic, it is environmentally protective；
4, the raw material of desulphurization catalyst of the present invention be easy to get, prepare it is simple, at low cost, can effectively reduce spent lye processing
Cost.
Specific embodiment
Derived energy chemical spent lye processing high-efficiency desulfurization catalyst of the present invention by active presoma, synergist, help
The raw material of substance such as agent, antifreezing agent, solvent composition.Wherein, described active presoma is by ferric sulfate, iron chloride or ferric nitrate structure
At molysite and/or the cobalt salt that is made of cobaltous sulfate, cobalt nitrate or cobalt chloride and/or by manganese sulfate, manganese acetate, manganese oxalate, chlorine
Change the manganese salt that manganese or manganese nitrate are constituted；Described synergist be neopelex and/or lauryl sodium sulfate and/or
Polyacrylic acid and its esters and/or ethyoxyl sodium alkyl sulfate and/or lauric acid amide of ethanol and/or ethyoxyl alkylsurfuric acid
Ammonium；Described auxiliary agent be sodium metasilicate and/or sodium sorbate and/or triethanolamine and/or polyphosphate sodium and/or Boratex and/or
Ethylenediamine tetraacetic methene sodium phosphate and/or sodium citrate and/or sodium ethylene diamine tetracetate and/or diethylenetriamine pentacarboxylic acid sodium and/
Or heptose sodium sugar and/or sodium gluconate；Described antifreezing agent is methanol and/or ethyl alcohol and/or ethylene glycol and/or propylene glycol
And/or glycerine；Described solvent is water.
The method for being used to prepare the high-efficiency desulfurization catalyst is: at normal temperature, first by active presoma, synergist, help
The solvent of agent and a small amount of (7%~22% amount), which is added in synthesis reactor, is stirred to react 2~5h, after the completion, antifreezing agent and its is added
The solvent of remaining (78%~93% amount) completes dissolution, and continues 2~5h of stirring, finished product.It can be according to spent lye when use
Treating capacity is directly added in proportion.
The content of present invention is furtherd elucidate below with reference to embodiment, but practical application form of the invention is not only
It is defined in following embodiments.
Embodiment 1
Manganese sulfate 10g, neopelex 2g, sodium metasilicate 5g, sodium citrate 10g, sodium gluconate 7g are taken respectively
It is added in synthesis reactor with water 10g, stirs 3h at normal temperature, then add ethylene glycol 5g, water 51g, continued to stir 2h, make
Fully dissolved is uniformly mixed, finished product.
Embodiment 2
3 grams of ferric sulfate, manganese sulfate 5g, lauryl sodium sulfate 3g, triethanolamine 5g, ethylenediamine tetraacetic methene phosphoric acid are taken respectively
Sodium 5g, sodium citrate 5g and water 10g are added in synthesis reactor, stir 4h at normal temperature, then add ethylene glycol 7g, water 60g,
Continue to stir 2h, make to be completely dissolved, is uniformly mixed, finished product.
Embodiment 3
8 grams of manganese nitrate, cobaltous sulfate 8g, lauryl sodium sulfate 2g, triethanolamine 5g, sodium ethylene diamine tetracetate are taken respectively
15g, sodium citrate 15g and water 10g are added in synthesis reactor, stir 3h at normal temperature, then add propylene glycol 10g, water
37g continues to stir 3h, makes to be completely dissolved, is uniformly mixed, finished product.
Embodiment 4
3 grams of ferric sulfate, manganese nitrate 2g, ethyoxyl sodium alkyl sulfate 3g, sodium metasilicate 8g, sodium ethylene diamine tetracetate 8g are taken respectively
It is added in synthesis reactor with water 5g, stirs 3h at normal temperature, then add propylene glycol 5g, water 66g, continued to stir 2h, make
Fully dissolved is uniformly mixed, finished product.
Embodiment 5
Manganese acetate 5g, 3 grams of cobalt chloride, lauryl sodium sulfate 3g, sodium metasilicate 8g, diethylenetriamine pentacarboxylic acid sodium are taken respectively
18g and water 8g are added in synthesis reactor, stir 4h at normal temperature, then add ethylene glycol 10g, water 45g, continue to stir 2h,
Make to be completely dissolved, be uniformly mixed, finished product.
Embodiment 6
2 grams of iron chloride, manganese acetate 6g, lauryl sodium sulfate 4g, sodium ethylene diamine tetracetate 12g, sodium citrate are taken respectively
10g and water 10g are added in synthesis reactor, stir 4h at normal temperature, then add glycerine 10g, water 45g, continue to stir 2h,
Make to be completely dissolved, be uniformly mixed, finished product.
Embodiment 7
Take respectively manganese chloride 4g, 3 grams of cobalt chloride, lauric acid amide of ethanol 4g, triethanolamine 5g, polyphosphate sodium 15g and
Water 10g is added in synthesis reactor, stirs 3h at normal temperature, then adds ethylene glycol 5g, water 54g, is continued to stir 3h, be made completely
Dissolution is uniformly mixed, finished product.
Embodiment 8
Manganese oxalate 5g, lauryl sodium sulfate 6g, sodium citrate 5g, diethylenetriamine pentacarboxylic acid sodium 5g, grape are taken respectively
Sodium saccharate 5g and water 15g are added in synthesis reactor, stir 5h at normal temperature, are then added ethylene glycol 8g, water 51g, are continued to stir
2h is mixed, makes to be completely dissolved, is uniformly mixed, finished product.
With certain chemical plant spent lye (S2-Content is 9870mg/L) it is treatment fluid, it is catalyzed using air catalytic oxidation method
Agent evaluation and test, normal pressure, 50 DEG C of reaction temperature, desulphurization catalyst dosage is the 2 ‰ of spent lye, and parallel laboratory test, reaction is after a certain period of time
Sampling processing analysis, experimental result is shown in the following table 1.Preparing catalyst has good catalytic activity and selectivity, in normal pressure, compared with low temperature
Under degree, quickly by S2-Thoroughly conversion, and most of sulfate radical for generating stable state, obtain high temperature, the effect that high-pressure process has.
1 embodiment 1-8 desulphurization catalyst catalytic oxidation effect of table
Claims (5)
1. a kind of derived energy chemical spent lye processing high-efficiency desulfurization catalyst, it is characterised in that: the desulphurization catalyst is by following matter
The raw material of substance of amount ratio is made:
Wherein, the active presoma is the molysite being made of ferric sulfate, iron chloride or ferric nitrate and/or by cobaltous sulfate, nitre
Sour cobalt or the cobalt chloride cobalt salt constituted and/or the manganese salt being made of manganese sulfate, manganese acetate, manganese oxalate, manganese chloride or manganese nitrate；
The synergist be neopelex and/or lauryl sodium sulfate and/or polyacrylic acid and its esters and/
Or ethyoxyl sodium alkyl sulfate and/or lauric acid amide of ethanol；
The auxiliary agent is sodium metasilicate and/or sodium sorbate and/or triethanolamine and/or polyphosphate sodium and/or ethylenediamine tetramethyl
Pitch sodium phosphate and/or sodium citrate and/or sodium ethylene diamine tetracetate and/or diethylenetriamine pentacarboxylic acid sodium and/or gluconic acid
Sodium；
The antifreezing agent is ethylene glycol and/or propylene glycol and/or glycerine；
The solvent is water；
The method for being used to prepare the desulphurization catalyst is: at normal temperature, first by active presoma, synergist, auxiliary agent and 7%~
The solvent of 22% amount, which is added in synthesis reactor, is stirred to react 2~5h, after the completion, antifreezing agent and remaining 78%~93% amount is added
Solvent completes dissolution, and continues 2~5h of stirring, finished product.
2. derived energy chemical spent lye processing high-efficiency desulfurization catalyst according to claim 1, it is characterised in that: described
Active presoma is the molysite being made of ferric sulfate, ferric nitrate and/or the cobalt salt being made of cobaltous sulfate, cobalt nitrate or cobalt chloride
And/or the manganese salt being made of manganese sulfate, manganese acetate, manganese oxalate or manganese chloride.
3. derived energy chemical spent lye processing high-efficiency desulfurization catalyst according to claim 1, it is characterised in that: described
Synergist is neopelex and/or lauryl sodium sulfate.
4. derived energy chemical spent lye processing high-efficiency desulfurization catalyst according to claim 1, it is characterised in that: described
Auxiliary agent is sodium gluconate and/or polyphosphate sodium and/or ethylenediamine tetraacetic methene sodium phosphate and/or sodium ethylene diamine tetracetate.
5. derived energy chemical spent lye processing high-efficiency desulfurization catalyst according to claim 1, it is characterised in that: described
Antifreezing agent is ethylene glycol and/or propylene glycol.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5244576A (en) * | 1991-02-05 | 1993-09-14 | Stone & Webster Engineering Limited | Spent caustic treatment |
| CN102151476A (en) * | 2011-03-29 | 2011-08-17 | 武汉国力通化工环保科技有限公司 | Method for removing hydrogen sulfide in gas phase through oxidization under high gravity field |
| CN103194296A (en) * | 2013-04-25 | 2013-07-10 | 兰州新星中性清洗技术有限公司 | Coal washing and desulfurizing agent composition and preparation method thereof |
| CN105056719A (en) * | 2015-07-30 | 2015-11-18 | 福州大学化肥催化剂国家工程研究中心 | Preparation method of FeOOH low-temperature desulfurizer and desulfurizer prepared through same |
-
2015
- 2015-12-16 CN CN201510941070.1A patent/CN105561981B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5244576A (en) * | 1991-02-05 | 1993-09-14 | Stone & Webster Engineering Limited | Spent caustic treatment |
| CN102151476A (en) * | 2011-03-29 | 2011-08-17 | 武汉国力通化工环保科技有限公司 | Method for removing hydrogen sulfide in gas phase through oxidization under high gravity field |
| CN103194296A (en) * | 2013-04-25 | 2013-07-10 | 兰州新星中性清洗技术有限公司 | Coal washing and desulfurizing agent composition and preparation method thereof |
| CN105056719A (en) * | 2015-07-30 | 2015-11-18 | 福州大学化肥催化剂国家工程研究中心 | Preparation method of FeOOH low-temperature desulfurizer and desulfurizer prepared through same |
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