CN102784631A - Method for regenerating carbon molecular sieve - Google Patents
Method for regenerating carbon molecular sieve Download PDFInfo
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- CN102784631A CN102784631A CN2012103019373A CN201210301937A CN102784631A CN 102784631 A CN102784631 A CN 102784631A CN 2012103019373 A CN2012103019373 A CN 2012103019373A CN 201210301937 A CN201210301937 A CN 201210301937A CN 102784631 A CN102784631 A CN 102784631A
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Abstract
The invention discloses a method for regenerating a carbon molecular sieve. The method includes steps of acid pickling, washing, carbonizing, activating, pore adjusting and the like. By the method for regenerating the carbon molecular sieve, the carbon molecular sieve can be reused on the premise that the performance and the quality of the carbon molecular sieve are not degraded, and a new profit increasing point is found out for enterprises in the industry of carbon molecular sieves while resource waste and environmental pollution are reduced and environments are protected.
Description
Technical field
The invention belongs to the sieve technology field, particularly relate to a kind of renovation process of making the nitrogen molecular sieve.
Background technology
Carbon molecular sieve (CMS) is the high-efficiency adsorbent of transformation absorption nitrogen production by air separation, because carbon molecular sieve has stronger affinity to water, wet goods molecule, this just requires very cleaning of raw air, must do to purify preliminary treatment.Because factors such as air compressor are used in transformation absorption, just in air, bring water, oil vapour and other harmful chemical gas inevitably into simultaneously.Thereby cause the nitrogen-preparing carbon molecular sieves micropore to stop up, separating effect gradually falls, until the forfeiture effect, and promptly so-called nitrogen-preparing carbon molecular sieves " poisoning ".
At present; Fast development of China transformation absorption (PSA) technology, along with nitrogen is manufactured on the extensive use of each big industrial circle, nitrogen production by air separation (PSA) industry is constantly developed; The nitrogen-preparing carbon molecular sieves use amount increases greatly; And nitrogen-preparing carbon molecular sieves is as requisite high-efficiency adsorbent in the transformation absorption nitrogen production by air separation device since its service life 5-8 only, China has 5000 tons of " poisonings " nitrogen-preparing carbon molecular sieves to discard every year approximately according to incompletely statistics.If it is discarded to be taken as industrial refuse, not only China's ecological environment is polluted, also wasted resource, and this wasting of resources and environmental disruption can increase thereupon also along with the acceleration of industrial development.
And the enterprise of home and abroad and research institution have only carried out big quantity research to the production of carbon molecular sieve, the activating and regenerating of " poisoning " carbon molecular sieve are not all had the report of relevant research and production application.Therefore, the home and abroad does not still have effective, economic recycle method to this discarded object at present.
Summary of the invention
Based on this, the purpose of this invention is to provide a kind of renovation process of the carbon molecular sieve of poisoning.
Concrete technical scheme is following:
A kind of renovation process of carbon molecular sieve comprises the steps:
(1) pickling: place hydrochloric acid solution to stir fully, clean the poisoning carbon molecular sieve, with the inorganic impurities such as oxide in the dissolved carbon molecular sieve;
(2) washing: the carbon molecular sieve after step (1) pickling with clear water rinsing 2-3 time, with oxide and other impurity of abundant removal step (1) dissolving, is reduced it to later stage activation and the influence of transferring the hole process;
(3) carbonization: place nitrogen environment under 700-900 ℃, to carry out carbonization the carbon molecular sieve after step (2) washing, promptly get the carbon molecular sieve of regenerating;
(4) activation: place nitrogen environment to feed carbon dioxide down earlier the carbon molecular sieve after step (3) carbonization and carry out perforate, and then feeding steam carries out the pore volume increase at 500-800 ℃;
(5) transfer the hole: place nitrogen environment to feed down the carbon molecular sieve after step (4) activation and transfer the hole agent to transfer the hole, promptly get the carbon molecular sieve of regenerating at 600-750 ℃.
Among some embodiment, the concentration expressed in percentage by volume of hydrochloric acid solution is 5-20% in the said step (1) therein.
Among some embodiment, the time of 700-900 ℃ of carbonization of said step (3) is 2-6h therein.
Among some embodiment, the time of 500-800 ℃ of activation of said step (4) is 1-3h therein.
Among some embodiment, it is 650-750 ℃ that said step (5) is transferred the temperature in hole therein, and the hole agent of said accent is benzene or toluene.
Advantage of the present invention and beneficial effect are following:
The present invention provides a kind of regeneration technology of the carbon molecular sieve of poisoning, and makes carbon molecular sieve under the prerequisite that performance and quality do not descend, realize repeated use.The present invention will poison, lost efficacy, after the discarded carbon molecular sieve Regeneration Treatment, reuse, reduced the wasting of resources, alleviated environmental pollution, in the protection environment, for the enterprise of carbon molecular sieve industry has found new profit growth point.
To be the inventor obtain through a large amount of experiments, summary and conclusion the series of process parameter of carbon molecular sieve regeneration technology provided by the invention, and the regeneration of poisoning carbon molecular sieve is had very obvious effects.The poisoning carbon molecular sieve is handled through regeneration technology provided by the invention, and its quality can reach company standard Q/CSK03-2011 " activating and regenerating nitrogen-preparing carbon molecular sieves ".The company standard performance indications are following:
Description of drawings
Fig. 1 is a carbon molecular sieve regeneration technology schematic flow sheet of the present invention.
The specific embodiment
Below through embodiment the present invention is done further elaboration.
Embodiment 1
A kind of renovation process of carbon molecular sieve comprises the steps:
(1) pickling: it is that 8% hydrochloric acid solution stirs fully, cleans that the poisoning carbon molecular sieve is placed volumetric concentration, with the inorganic impurities such as oxide in the dissolved carbon molecular sieve;
(2) washing: the carbon molecular sieve after step (1) pickling with clear water rinsing 2-3 time, with oxide and other impurity of abundant removal step (1) dissolving, is reduced it to later stage activation and the influence of transferring the hole process;
(3) carbonization: place nitrogen environment at 700 ℃ of following carbonization 6h the carbon molecular sieve after step (2) washing, promptly get the carbon molecular sieve of regenerating.
Embodiment 2
A kind of renovation process of carbon molecular sieve comprises the steps:
(1) pickling: it is that 8% hydrochloric acid solution stirs fully, cleans that the poisoning carbon molecular sieve is placed volumetric concentration, with the inorganic impurities such as oxide in the dissolved carbon molecular sieve;
(2) washing: the carbon molecular sieve after step (1) pickling with clear water rinsing 2-3 time, with oxide and other impurity of abundant removal step (1) dissolving, is reduced it to later stage activation and the influence of transferring the hole process;
(3) carbonization: place nitrogen environment at 750 ℃ of following carbonization 3h the carbon molecular sieve after step (2) washing;
(4) activation: place nitrogen environment to feed carbon dioxide down earlier the carbon molecular sieve after step (3) carbonization and carry out perforate 30min, and then feeding steam carries out pore volume increase 40min at 600 ℃;
(5) transfer the hole: place nitrogen environment to feed toluene down the carbon molecular sieve after step (4) activation and transfer the hole, promptly get the carbon molecular sieve of regenerating at 650 ℃.
Embodiment 3
A kind of renovation process of carbon molecular sieve comprises the steps:
(1) pickling: it is that 15% hydrochloric acid solution stirs fully, cleans that the poisoning carbon molecular sieve is placed volumetric concentration, with the inorganic impurities such as oxide in the dissolved carbon molecular sieve;
(2) washing: the carbon molecular sieve after step (1) pickling with clear water rinsing 2-3 time, with oxide and other impurity of abundant removal step (1) dissolving, is reduced it to later stage activation and the influence of transferring the hole process;
(3) carbonization: place nitrogen environment at 800 ℃ of following carbonization 3h the carbon molecular sieve after step (2) washing;
(4) activation: place nitrogen environment to feed carbon dioxide down earlier the carbon molecular sieve after step (3) carbonization and carry out perforate 40min, and then feeding steam carries out pore volume increase 30min at 750 ℃;
(5) transfer the hole: place nitrogen environment to feed toluene down the carbon molecular sieve after step (4) activation and transfer the hole, promptly get the carbon molecular sieve of regenerating at 700 ℃.
The performance of the regenerative carbon molecular sieve of the foregoing description gained is following:
In the last table is the testing result to 3 embodiment products obtained therefroms, and data can find out that products obtained therefrom has all reached, exceeded the index that enterprise's mark requires, and can satisfy the instructions for use to carbon molecular sieve fully from table.
The above embodiment has only expressed several kinds of embodiments of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art under the prerequisite that does not break away from the present invention's design, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with accompanying claims.
Claims (5)
1. the renovation process of a carbon molecular sieve is characterized in that, comprises the steps:
(1) pickling: place hydrochloric acid solution to stir fully, clean the poisoning carbon molecular sieve;
(2) washing: with the carbon molecular sieve after step (1) pickling with clear water rinsing 2-3 time;
(3) carbonization: place nitrogen environment under 700-900 ℃, to carry out carbonization the carbon molecular sieve after step (2) washing;
(4) activation: place nitrogen environment to feed carbon dioxide down earlier the carbon molecular sieve after step (3) carbonization and carry out perforate, and then feeding steam carries out the pore volume increase at 500-800 ℃;
(5) transfer the hole: place nitrogen environment to feed down the carbon molecular sieve after step (4) activation and transfer the hole agent to transfer the hole, promptly get the carbon molecular sieve of regenerating at 600-750 ℃.
2. the renovation process of carbon molecular sieve according to claim 1 is characterized in that, the concentration expressed in percentage by volume of hydrochloric acid solution is 5-20% in the said step (1).
3. the renovation process of carbon molecular sieve according to claim 1 is characterized in that, the time of 700-900 ℃ of carbonization of said step (3) is 2-6h.
4. the renovation process of carbon molecular sieve according to claim 1 is characterized in that, the time of 500-800 ℃ of activation of said step (4) is 1-3h.
5. the renovation process of carbon molecular sieve according to claim 1 is characterized in that, it is 650-750 ℃ that said step (5) is transferred the temperature in hole, and the hole agent of said accent is benzene or toluene.
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| CN2012103019373A CN102784631A (en) | 2012-08-23 | 2012-08-23 | Method for regenerating carbon molecular sieve |
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| CN2012103019373A CN102784631A (en) | 2012-08-23 | 2012-08-23 | Method for regenerating carbon molecular sieve |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103349973A (en) * | 2013-06-14 | 2013-10-16 | 湖州新奥利吸附材料有限公司 | Regeneration method of nitrogen-preparation carbon molecular sieve |
| CN103962095A (en) * | 2013-01-25 | 2014-08-06 | 江苏益茂纯电动汽车有限公司 | Regeneration process of glove box waste molecular sieve for lithium battery liquid injection |
| CN104307479A (en) * | 2014-11-07 | 2015-01-28 | 威海华泰分子筛有限公司 | Regeneration method of invalid carbon molecular sieve |
| CN105944674A (en) * | 2016-06-17 | 2016-09-21 | 湖州南浔展辉分子筛厂 | Regeneration method of poisoned carbon molecular sieve |
| CN106082207A (en) * | 2016-06-15 | 2016-11-09 | 湖州南浔展辉分子筛厂 | A kind of production system of carbon molecular sieve |
| CN106076921A (en) * | 2016-06-15 | 2016-11-09 | 湖州南浔展辉分子筛厂 | A kind of cleaning device of carbon molecular sieve |
| 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 |
| CN107649093A (en) * | 2016-07-26 | 2018-02-02 | 中国石化扬子石油化工有限公司 | A kind of renovation process of aromatic hydrocarbon refining carclazyte |
| CN112337321A (en) * | 2019-08-08 | 2021-02-09 | 中国石油天然气股份有限公司 | Carbon molecular sieve membrane structure remodeling method |
| CN114572984A (en) * | 2022-04-07 | 2022-06-03 | 浙江吉鑫空分材料科技有限公司 | Preparation method of high-adsorbability carbon molecular sieve |
-
2012
- 2012-08-23 CN CN2012103019373A patent/CN102784631A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103962095A (en) * | 2013-01-25 | 2014-08-06 | 江苏益茂纯电动汽车有限公司 | Regeneration process of glove box waste molecular sieve for lithium battery liquid injection |
| CN103349973A (en) * | 2013-06-14 | 2013-10-16 | 湖州新奥利吸附材料有限公司 | Regeneration method of nitrogen-preparation carbon molecular sieve |
| CN103349973B (en) * | 2013-06-14 | 2015-05-06 | 湖州新奥利吸附材料有限公司 | Regeneration method of nitrogen-preparation carbon molecular sieve |
| CN104307479A (en) * | 2014-11-07 | 2015-01-28 | 威海华泰分子筛有限公司 | Regeneration method of invalid carbon molecular sieve |
| CN104307479B (en) * | 2014-11-07 | 2016-04-20 | 威海华泰分子筛有限公司 | A kind of renovation process of the carbon molecular sieve that lost efficacy |
| CN106082207A (en) * | 2016-06-15 | 2016-11-09 | 湖州南浔展辉分子筛厂 | A kind of production system of carbon molecular sieve |
| CN106076921A (en) * | 2016-06-15 | 2016-11-09 | 湖州南浔展辉分子筛厂 | A kind of cleaning device of carbon molecular sieve |
| CN105944674A (en) * | 2016-06-17 | 2016-09-21 | 湖州南浔展辉分子筛厂 | Regeneration method of poisoned carbon molecular sieve |
| CN107649093A (en) * | 2016-07-26 | 2018-02-02 | 中国石化扬子石油化工有限公司 | A kind of renovation process of aromatic hydrocarbon refining carclazyte |
| 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 |
| CN112337321A (en) * | 2019-08-08 | 2021-02-09 | 中国石油天然气股份有限公司 | Carbon molecular sieve membrane structure remodeling method |
| CN112337321B (en) * | 2019-08-08 | 2022-11-04 | 中国石油天然气股份有限公司 | Carbon molecular sieve membrane structure remodeling method |
| CN114572984A (en) * | 2022-04-07 | 2022-06-03 | 浙江吉鑫空分材料科技有限公司 | Preparation method of high-adsorbability carbon molecular sieve |
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Application publication date: 20121121 |