CN108311102B - Method for removing peculiar smell of sodium hydrosulfide solution - Google Patents
Method for removing peculiar smell of sodium hydrosulfide solution Download PDFInfo
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- CN108311102B CN108311102B CN201810092353.7A CN201810092353A CN108311102B CN 108311102 B CN108311102 B CN 108311102B CN 201810092353 A CN201810092353 A CN 201810092353A CN 108311102 B CN108311102 B CN 108311102B
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- sodium hydrosulfide
- hydrosulfide solution
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- crown ether
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
- C01B17/32—Hydrosulfides of sodium or potassium
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- Nanotechnology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for removing the peculiar smell of a sodium hydrosulfide solution, which is characterized in that a certain amount of composite adsorbent is added into the sodium hydrosulfide solution produced industrially, and after reaction for a period of time at a certain temperature, the sodium hydrosulfide solution without the peculiar smell can be obtained by filtering. The production method is simple to operate, and compared with the conventional adsorbent, the adsorbent has a better adsorption effect. The treated product has no peculiar smell, the quality is improved, the obtained product can meet the requirements of related industries, the purity of downstream products is improved, and the industrial treatment is easy.
Description
Technical Field
The invention belongs to the technical field of fine chemical engineering, and relates to a method for removing the peculiar smell of a sodium hydrosulfide solution.
Background
Sodium hydrosulfide solution is a very important chemical raw material. The fertilizer industry is used for removing sulphur in desulphurizing agents, the dye industry is mainly used for synthesizing organic intermediates and preparing auxiliaries of sulphur dyes, and the tanning industry is used for dehairing and tanning of hides and the like. It is also a raw material for preparing ammonium sulfide, ethanethiol, mercaptopropionic acid and polyphenylene sulfide, and plays an important role in organic synthesis, three-waste treatment and the like.
The synthesis of the sodium hydrosulfide solution is mainly prepared by absorbing hydrogen sulfide by liquid alkali. In order to make full use of the company resources, the absorbed hydrogen sulfide is mainly derived from acid gas discharged from petrochemical refineries. The off-flavors in the product result from some organic impurities contained in the acid gas. The sodium hydrosulfide solution with peculiar smell is difficult to sell, and influences the health condition of production workers to a certain extent. It also affects the purity of downstream products, and therefore its handling is a critical requirement.
In recent years, although there are a lot of reports on the improvement of the process and quality of sodium hydrosulfide, no odor removal has been reported so far.
Disclosure of Invention
The invention provides a method for removing the peculiar smell of a sodium hydrosulfide solution, aiming at preparing the sodium hydrosulfide by using industrial hydrogen sulfide, in particular to a process for preparing the sodium hydrosulfide by using industrial hydrogen sulfide derived from petrochemical acid gas. Industrial hydrogen sulfide, especially hydrogen sulfide from petrochemical acid gas, contains some odorous organic and inorganic impurities (such as aromatic hydrocarbon substances, saturated hydrocarbons, sulfur-containing compounds, etc.), which are difficult to remove, and sodium hydrosulfide prepared by using the hydrogen sulfide has an odor and affects the product quality. The method of the invention has simple process operation and low requirement on equipment, more importantly improves the quality of the industrial sodium hydrosulfide solution, further improves the practical value of the industrial sodium hydrosulfide solution, greatly meets the requirements of customers and markets, and has great social and economic values.
The invention relates to a method for removing the peculiar smell of a sodium hydrosulfide solution, which adopts the following specific technical scheme:
adding a composite adsorbent accounting for 0.5-1% of the mass of the sodium hydrosulfide solution into the industrially produced sodium hydrosulfide solution, stirring and reacting for 2-5h at the temperature of 30-60 ℃, and filtering after reaction to obtain odorless sodium hydrosulfide solution;
wherein, the composite adsorbent consists of the following components: the adsorbent comprises the following components in parts by weight: 1 part, modifier: 2-5 parts; the preparation method comprises the following steps: dispersing the adsorbent in the modifier, stirring at 30-40 deg.C for 30-60min, filtering, and drying at 30 deg.C to obtain the composite adsorbent.
The adsorbent is one or more of activated carbon, carbon fiber and industrial multi-walled carbon nano-tube;
the modifier is crown ether modifier selected from any one of 12-crown ether-4, 15-crown ether-5, 12-crown ether-4, 2, 2-dimethyl-15-crown ether-5.
After the modification, the adsorption capacity of the composite adsorbent is more outstanding, the adsorption speed and the adsorption capacity are greatly improved, the treatment time and the using amount of the adsorbent are reduced, the content of sodium hydrosulfide is not influenced, other impurities are not introduced, and the composite adsorbent can be removed by filtering.
The dosage of the composite adsorbent in the illustrated steps is 0.5-1% of the mass of the industrial sodium hydrosulfide solution, and the preferred dosage is 0.6-0.9%. If the addition amount of the composite adsorbent is less than 0.5%, a good adsorption effect cannot be achieved. If the amount of the composite adsorbent added is more than 1%, the reagent is wasted.
The reaction treatment temperature in the reaction is 30-60 ℃. If the reaction temperature is too low, the reaction time is long, and the reaction rate is slow; if the reaction temperature is too high, other side reactions occur, and other impurities occur, which affect the quality of sodium hydrosulfide.
The reaction time is 2-5h, and if the reaction time is too short, the reaction is insufficient; too long a reaction time increases energy consumption and wastes a lot of time.
In conclusion, the method for removing the peculiar smell of the sodium hydrosulfide solution is simple to operate, compared with the conventional adsorbent, the method has the advantages that the adsorption effect is better, the treated product has no peculiar smell, the quality is improved, the obtained product can meet the requirements of related industries, the purity of downstream products is improved, the industrial treatment is easy, and the economic and use values are improved.
Detailed Description
The following further description of the present invention is provided in connection with specific embodiments to enable those skilled in the art to further understand the present invention, and not to limit the present invention, and all techniques based on the principles described herein are within the scope of the present invention. The industrial sodium hydrosulfide solution in the following examples is prepared from industrial hydrogen sulfide derived from petrochemical acid gas; the following examples are carried out using conventional techniques, except as otherwise indicated.
Example 1
Adding 0.7g of composite adsorbent into 100g of industrial sodium hydrosulfide solution, stirring at 40 ℃ for 3 hours, and filtering to obtain odorless sodium hydrosulfide solution.
Wherein, the composite adsorbent is prepared from 1 part of activated carbon and 3 parts of modifier 12-crown ether-4 by weight.
Dispersing 1 part of activated carbon in 3 parts of modifier under high-speed stirring, stirring for 50min at 30 ℃, filtering, and drying for 2h at 30 ℃ to obtain the composite adsorbent.
Example 2
Adding 0.5g of composite adsorbent into 100g of industrial sodium hydrosulfide solution, stirring at 50 ℃ for 2 hours, and filtering to obtain odorless sodium hydrosulfide solution.
The composite adsorbent is prepared from an industrial multi-walled carbon nanotube and 2 parts of a modifier 15-crown ether-5 in parts by weight.
Dispersing 1 part of industrial multi-walled carbon nano-tube in 2 parts of modifier under high-speed stirring, stirring for 30min at 40 ℃, filtering, and drying for 2h at 30 ℃ to obtain the composite adsorbent.
| NaSH content | Smell(s) | |
| Before treatment | 38.19％ | Has salty odor |
| After treatment | 38.12％ | Has no taste |
Example 3
Adding 0.9g of composite adsorbent into 100g of industrial sodium hydrosulfide solution, stirring at 60 ℃ for 4 hours, and filtering to obtain odorless sodium hydrosulfide solution.
Wherein, the composite adsorbent is prepared from 1 part of carbon fiber and 4 parts of modifier 12-crown ether-4 by weight.
Dispersing 1 part of carbon fiber in 4 parts of modifier under high-speed stirring, stirring for 60min at 30 ℃, filtering, and drying for 2h at 30 ℃ to obtain the composite adsorbent.
| NaSH content | Smell(s) | |
| Before treatment | 38.12％ | Has salty odor |
| After treatment | 38.1％ | Has no taste |
Example 4
Adding 1.0g of composite adsorbent into 100g of industrial sodium hydrosulfide solution, stirring at 40 ℃ for 3h, and filtering to obtain odorless sodium hydrosulfide solution.
The composite adsorbent is prepared from 0.5 part of activated carbon, 0.5 part of industrial multi-walled carbon nanotube and 3 parts of modifier 2, 2-dimethyl-15-crown ether-5 in parts by weight.
Dispersing 0.5 part of activated carbon and 0.5 part of industrial multi-walled carbon nanotube in 3 parts of modifier under high-speed stirring, stirring for 40min at 30 ℃, filtering, and drying for 2h at 30 ℃ to obtain the composite adsorbent.
| NaSH content | Smell(s) | |
| Before treatment | 38.05％ | Has salty odor |
| After treatment | 38.04％ | Has no taste |
From the above examples, it can be seen that the method of the present invention for treating sodium hydrosulfide has almost no influence on the content of sodium hydrosulfide, and at the same time, aromatic hydrocarbons, saturated hydrocarbons, sulfur-containing compounds and other odorous substances are effectively adsorbed, so that the obtained sodium hydrosulfide has no peculiar smell, and the use value of the industrial sodium hydrosulfide is improved.
Claims (3)
1. A method for removing the peculiar smell of a sodium hydrosulfide solution is characterized by comprising the following steps: adding a composite adsorbent accounting for 0.5-1% of the mass of the sodium hydrosulfide solution into the industrially produced sodium hydrosulfide solution, stirring and reacting at 30-60 ℃, and filtering after reaction to obtain odorless sodium hydrosulfide solution;
wherein, the composite adsorbent consists of the following components: the adsorbent comprises the following components in parts by weight: 1 part, modifier: 2-5 parts; the preparation method comprises the following steps: dispersing the adsorbent in a modifier, stirring at 30-40 deg.C for 30-60min, filtering, and drying at 30 deg.C to obtain composite adsorbent;
the modifier is crown ether modifier selected from any one of 12-crown ether-4, 15-crown ether-5, 12-crown ether-4, 2, 2-dimethyl-15-crown ether-5;
the adsorbent is one or more of activated carbon, carbon fiber and industrial multi-walled carbon nano-tube.
2. A method according to claim 1, wherein the method comprises the steps of: the dosage of the composite adsorbent is 0.6-0.9% of the mass of the sodium hydrosulfide solution.
3. A method according to claim 1, wherein the method comprises the steps of: the stirring and reaction time is 2-5 h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810092353.7A CN108311102B (en) | 2018-01-30 | 2018-01-30 | Method for removing peculiar smell of sodium hydrosulfide solution |
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| CN201810092353.7A CN108311102B (en) | 2018-01-30 | 2018-01-30 | Method for removing peculiar smell of sodium hydrosulfide solution |
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| CN108311102B true CN108311102B (en) | 2020-06-30 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1308557A (en) * | 1998-07-10 | 2001-08-15 | 高林环境技术公司 | Process and catalyst/sorber for treating sulfur compound containing effluent |
| CN106540663A (en) * | 2016-12-09 | 2017-03-29 | 南华大学 | A kind of preparation method of the crown ether modified carbon nano tube tube material for adsorption uranium |
| CN107029539A (en) * | 2017-04-07 | 2017-08-11 | 上海盛剑环境系统科技有限公司 | A kind of processing method of the waste gas containing oxynitrides |
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2018
- 2018-01-30 CN CN201810092353.7A patent/CN108311102B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1308557A (en) * | 1998-07-10 | 2001-08-15 | 高林环境技术公司 | Process and catalyst/sorber for treating sulfur compound containing effluent |
| CN106540663A (en) * | 2016-12-09 | 2017-03-29 | 南华大学 | A kind of preparation method of the crown ether modified carbon nano tube tube material for adsorption uranium |
| CN107029539A (en) * | 2017-04-07 | 2017-08-11 | 上海盛剑环境系统科技有限公司 | A kind of processing method of the waste gas containing oxynitrides |
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| CN108311102A (en) | 2018-07-24 |
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Effective date of registration: 20200717 Address after: 256500 Boxing Economic Development Zone, Binzhou, Shandong Patentee after: SHANDONG EFIRM BIOCHEMISTRY AND ENVIRONMENTAL PROTECTION Co.,Ltd. Address before: 256500 Boxing Economic Development Zone, Binzhou, Shandong Patentee before: YELLOW RIVER DELTA JINGBO RESEARCH INSTITUTE OF CHEMICAL INDUSTRY Co.,Ltd. |
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Address after: 256500 Boxing Economic Development Zone, Shandong, Binzhou Patentee after: Yifeng New Material Co.,Ltd. Address before: 256500 Boxing Economic Development Zone, Shandong, Binzhou Patentee before: SHANDONG EFIRM BIOCHEMISTRY AND ENVIRONMENTAL PROTECTION Co.,Ltd. |