CN105944674A - Regeneration method of poisoned carbon molecular sieve - Google Patents
Regeneration method of poisoned carbon molecular sieve Download PDFInfo
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- CN105944674A CN105944674A CN201610430414.7A CN201610430414A CN105944674A CN 105944674 A CN105944674 A CN 105944674A CN 201610430414 A CN201610430414 A CN 201610430414A CN 105944674 A CN105944674 A CN 105944674A
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- molecular sieve
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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
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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Abstract
The invention provides a regeneration method of a poisoned carbon molecular sieve. The method comprises the following steps of S100, acid washing, wherein the poisoned carbon molecular sieve is put in a hydrochloric acid solution to be fully soaked; S200, water washing, wherein the poisoned carbon molecular sieve subjected to acid washing is rinsed 2-3 times with clear water; S300, solvent washing, wherein the poisoned carbon molecular sieve subjected to water washing is put in an organic solvent to be fully soaked; S400, hole regulating, wherein the poisoned carbon molecular sieve is put in a nitrogen environment to be subjected to hole regulating at 600 DEG C to 750 DEG C. The carbon molecular sieve obtained through the method is high in performance and quality, repeated utilization of the carbon molecular sieve is achieved, resource waste is reduced, the environment is protected, and environmental pollution is avoided.
Description
Technical field
The present invention relates to carbon molecular sieve field, particularly relate to the renovation process of a kind of carbon molecular sieve of being poisoned.
Background technology
Carbon molecular sieve (CMS) is a kind of carbonaceous adsorbent in a broad sense, to be the activated carbon that is evenly distributed of micropore in the narrow sense, it is to be made up of crystalline carbon and agraphitic carbon, there is highly developed pore structure and the atomic hole of wedge shape close to adsorbed molecular diameter, and even aperture distribution, it is possible to discrepant for stereochemical structure size molecule is separated.At present, carbon molecular sieve has been widely used for the every field such as environmental conservation, chemical industry, petroleum industry, food processing, hydrometallurgy, refined, the militarization protection of medicine.
Owing to carbon molecular sieve has stronger affinity, therefore it is required that raw air must be the cleanest to water, oil equimolecular.But using the reasons such as air compressor due to pressure-variable adsorption, bring water, oil vapour and other harmful chemicals gas the most in atmosphere into, thus cause nitrogen-preparing carbon molecular sieves blockage of the micro orifice, separating effect gradually drops, here it is the poisoning of so-called carbon molecular sieve.
China's pressure-variable adsorption (PSA) technology is fast-developing at present, and along with nitrogen preparation is in the extensive application of each big industrial circle, nitrogen production by air separation industry develops rapidly, and the usage amount of nitrogen-preparing carbon molecular sieves is greatly increased.According to statistics, discarded due to poisoning every year carbon molecular sieve there are about 5000 tons.If this sulfurization carbon molecular sieve is simply abandoned, on the one hand ecological environment is polluted, on the other hand cause the great wasting of resources.
Therefore it provides a kind of, can effectively to make carbon molecular sieve regeneration method be technical problem urgently to be resolved hurrily.
Summary of the invention
For the problems referred to above, it is an object of the invention to provide the renovation process of a kind of carbon molecular sieve of being poisoned.
Technical scheme is as follows:
The renovation process of a kind of carbon molecular sieve of being poisoned, it comprises the steps:
S100: pickling: poisoning carbon molecular sieve is placed in hydrochloric acid solution and fully soaks；
S200: washing: the clear water of the poisoning carbon molecular sieve after pickling is rinsed 2 ~ 3 times；
S300: solvent clean: carbon molecular sieve of being poisoned after washing is placed in organic solvent and fully soaks；
S400: adjust hole: by after solvent clean poisoning carbon molecular sieve be placed in nitrogen environment be passed through at 600 ~ 750 DEG C tune hole agent carry out adjust hole process.
Wherein, in step S100, the concentration of hydrochloric acid solution is 5% ~ 10%.
Wherein, in step S100, soak time is 30min ~ 80min.
Wherein, in step S300, organic solvent is toluene, dimethylbenzene or DMF.
Wherein, the time adjusting hole to process in step S400 is 10min ~ 50min.
The invention has the beneficial effects as follows: the renovation process of the poisoning carbon molecular sieve of the present invention removes the oxide etc. in carbon molecular sieve hole first with pickling; then organic solvent is utilized to remove the organic compound in carbon molecular sieve hole; last carrying out carbon molecular sieve again adjusts hole to process; the carbon molecular sieve performance finally obtained and quality are the highest; achieve the recycling of carbon molecular sieve; decrease the wasting of resources, protect environment, it is to avoid environmental pollution.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with specific embodiment, the present invention is further elaborated.
It should be noted that in the case of not conflicting, the embodiment in the application and the feature in embodiment can be mutually combined.
The raw material and the equipment that use in following example are commercially available if not otherwise indicated.
Embodiment one
The renovation process of a kind of carbon molecular sieve of being poisoned, it comprises the steps:
S100: pickling: being placed in the hydrochloric acid solution that concentration is 5% by poisoning carbon molecular sieve and fully soak to remove the oxide etc. in carbon molecular sieve hole, soak time is preferably 30min ~ 80min；Preferably it is stirred during immersion；
S200: washing: the clear water of the poisoning carbon molecular sieve after pickling is rinsed 2 ~ 3 times；Washing can remove hydrochloric acid solution and other solutees of pickling；
S300: solvent clean: being placed in toluene by carbon molecular sieve of being poisoned after washing and fully soak, soak time is 10min ~ 20min；In this step, the dissolving of the Organic substance in carbon molecular sieve hole in organic solvent thus removes the Organic substance of deposition in hole；
S400: adjust hole: by after solvent clean poisoning carbon molecular sieve be placed in nitrogen environment carry out at 600 DEG C adjust hole process, the time is 20min.Adjust hole after having processed, i.e. can obtain the carbon molecular sieve of regeneration.
Owing to adding solvent cleaning step in regeneration methods of the invention, on the one hand solvent clean can remove the organic compound in carbon molecular sieve, and on the other hand solvent is also used as follow-up tune hole agent use.Owing to clearly ratio more thoroughly, therefore can save the steps such as the carbonization in other renovation process, activation, it is only necessary to carry out hole adjusting hole to process.Can use as adjusting hole agent additionally, due to the organic solvent used during solvent clean, therefore this step need not additionally be passed through tune hole agent.Furthermore owing to adjusting hole agent to be well dispersed in carbon molecular sieve when soaking, the time therefore adjusting hole to process can suitably shorten.
Embodiment two
The renovation process of a kind of carbon molecular sieve of being poisoned, it comprises the steps:
S100: pickling: poisoning carbon molecular sieve is placed in the hydrochloric acid solution that concentration is 8% and soaks 40min to remove the oxide etc. in carbon molecular sieve hole；Preferably it is stirred during immersion；
S200: washing: the clear water of the poisoning carbon molecular sieve after pickling is rinsed 2 ~ 3 times；Washing can remove hydrochloric acid solution and other solutees of pickling；The washing hydromining water containing micro-nano bubble in the present embodiment, a diameter of 0.1 ~ 10 micron of the micro-nano bubble contained in water, the micro-nano bubble contained in water can enter hole thus the solute of taking away in hole, thus clean more thorough；
S300: solvent clean: carbon molecular sieve of being poisoned after washing is placed in dimethylbenzene immersion 15min；
S400: adjust hole: being placed in nitrogen environment by the poisoning carbon molecular sieve after solvent clean and carry out adjusting hole to process at 650 DEG C, the time is 10min.Adjust hole after having processed, i.e. can obtain the carbon molecular sieve of regeneration.
Embodiment three
The renovation process of a kind of carbon molecular sieve of being poisoned, it comprises the steps:
S100: pickling: poisoning carbon molecular sieve is placed in the hydrochloric acid solution that concentration is 10% and soaks 80min to remove the oxide etc. in carbon molecular sieve hole；
S200: washing: the clear water of the poisoning carbon molecular sieve after pickling is rinsed 2 ~ 3 times；Washing can remove hydrochloric acid solution and other solutees of pickling；The washing hydromining water containing micro-nano bubble in the present embodiment, a diameter of 0.1 ~ 10 micron of the micro-nano bubble contained in water, the micro-nano bubble contained in water can enter hole thus the solute of taking away in hole, thus clean more thorough；Water scouring water containing micro-nano bubble is that carbon molecular sieve is carried out by spurting, and carbon molecular sieve can be more effectively carried out by the current of spurting；
S300: solvent clean: carbon molecular sieve of being poisoned after washing is placed in DMF immersion 20min；
S400: adjust hole: being placed in nitrogen environment by the poisoning carbon molecular sieve after solvent clean and carry out adjusting hole to process at 700 DEG C, the time is 50min.Adjust hole after having processed, i.e. can obtain the carbon molecular sieve of regeneration.
The performance of the regenerative carbon molecular sieve that above-described embodiment obtains is as follows:
| Project | Poisoning carbon molecular sieve | Embodiment one | Embodiment two | Embodiment three |
| Bulk density, kg/L | 0.64 | 0.65 | 0.65 | 0.66 |
| Rich nitrogen concentration, % | 99.4 | 99.4 | 99.5 | 99.4 |
| Denitrification production rate, L/h*kg | ＜ 100 | 260 | 265 | 268 |
By above-mentioned experimental data it is found that carbon molecular sieve function admirable after Zai Sheng, comply fully with use requirement.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that, for the person of ordinary skill of the art, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claim.
Claims (5)
1. the renovation process of a carbon molecular sieve of being poisoned, it is characterised in that comprise the steps:
S100: pickling: poisoning carbon molecular sieve is placed in hydrochloric acid solution and fully soaks；
S200: washing: the clear water of the poisoning carbon molecular sieve after pickling is rinsed 2 ~ 3 times；
S300: solvent clean: carbon molecular sieve of being poisoned after washing is placed in organic solvent and fully soaks；
S400: adjust hole: be placed in the poisoning carbon molecular sieve after solvent clean in nitrogen environment to be passed through at 600 ~ 750 DEG C and adjust hole agent to carry out adjusting hole to process.
The renovation process of poisoning carbon molecular sieve the most according to claim 1, it is characterised in that in step S100, the concentration of hydrochloric acid solution is 5% ~ 10%.
The renovation process of poisoning carbon molecular sieve the most according to claim 1, it is characterised in that in step S100, soak time is 30min ~ 80min.
The renovation process of poisoning carbon molecular sieve the most according to claim 1, it is characterised in that in step S300, organic solvent is toluene, dimethylbenzene or DMF.
The renovation process of poisoning carbon molecular sieve the most according to claim 1, it is characterised in that the time adjusting hole to process in step S400 is 10min ~ 50min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107175091A (en) * | 2017-06-10 | 2017-09-19 | 湖州知维技术服务有限公司 | A kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way |
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2016
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| EP0680783A2 (en) * | 1994-05-05 | 1995-11-08 | Dow Corning Corporation | Two-step thermal regeneration of adsorbents |
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| CN107175091A (en) * | 2017-06-10 | 2017-09-19 | 湖州知维技术服务有限公司 | A kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way |
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Denomination of invention: A regeneration method of poisoned carbon molecular sieve Effective date of registration: 20210730 Granted publication date: 20190305 Pledgee: Zhejiang Nanxun Rural Commercial Bank Co.,Ltd. Hefu Changchao sub branch Pledgor: HUZHOU NANXUN ZHANHUI MOLECULAR SIEVE PLANT Registration number: Y2021330001044 |
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Date of cancellation: 20220805 Granted publication date: 20190305 Pledgee: Zhejiang Nanxun Rural Commercial Bank Co.,Ltd. Hefu Changchao sub branch Pledgor: HUZHOU NANXUN ZHANHUI MOLECULAR SIEVE PLANT Registration number: Y2021330001044 |
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Denomination of invention: A regeneration method of poisoned carbon molecular sieve Effective date of registration: 20221006 Granted publication date: 20190305 Pledgee: Zhejiang Nanxun Rural Commercial Bank Co.,Ltd. Hefu Changchao sub branch Pledgor: HUZHOU NANXUN ZHANHUI MOLECULAR SIEVE PLANT Registration number: Y2022330002449 |
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